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Ceramics, Volume 6, Issue 4 (December 2023) – 30 articles

Cover Story (view full-size image): This study highlights the effect of rare-earth ion doping on the magnetic and magnetocaloric properties of the ferrimagnetic garnet compound Gd1-xRExFe5O12 (RE = Nd, Sm, Dy, and Y). The rare-earth ion substitution resulted in site-to-site bond lengths and bond angle alterations, thereby influencing the magnetic exchange interaction among site ions. The variation in maximum magnetic entropy change (−∆SMmax) was enhanced via Dy3+ and Sm3+ substitution but decreased with Nd3+ and Y3+ substitution. A first-principal density function theory (DFT) technique was used to shed light on the observed magnetic behavior of the substituted compound. The study shows that the magnetic moments of the doped rare-earth ions play a vital role in tuning the magnetocaloric properties of the garnet compound. View this paper
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13 pages, 5233 KiB  
Article
Effects of Composition Variations on Mechanochemically Synthesized Lithium Metazirconate-Based Ceramics and Their Resistance to External Influences
by Bauyrzhan K. Abyshev, Sholpan G. Giniyatova and Artem L. Kozlovskiy
Ceramics 2023, 6(4), 2394-2406; https://doi.org/10.3390/ceramics6040147 - 15 Dec 2023
Viewed by 1541
Abstract
The study examines the influence of variations in the compositions of components for the production of lithium-containing ceramics based on lithium metazirconate obtained by the method of mechanochemical grinding and subsequent thermal sintering. For component variation, two compositions were used, consisting of zirconium [...] Read more.
The study examines the influence of variations in the compositions of components for the production of lithium-containing ceramics based on lithium metazirconate obtained by the method of mechanochemical grinding and subsequent thermal sintering. For component variation, two compositions were used, consisting of zirconium dioxide (ZrO2) and two distinct types of lithium-containing materials: lithium perchlorate (LiClO4·3H2O) and lithium carbonate (Li2CO3). Adjusting the concentration of these components allowed for the production of two-phase ceramics with varying levels of impurity phases. Using X-ray phase analysis methods, it was determined that the use of LiClO4·3H2O results in the formation of a monoclinic phase, Li2ZrO3, with impurity inclusions in the orthorhombic phase, LiO2. On the other hand, when Li2CO3 is used, the resulting ceramics comprise a mixture of two phases, Li2ZrO3 and Li6Zr2O7. During the studies, it was established that the formation of impurity inclusions in the composition of ceramics leads to an increase in the stability of strength properties with varying mechanical test conditions, as well as stabilization of thermophysical parameters and a decrease in thermal expansion during long-term high-temperature tests. It has been established that in the case of two-phase ceramics Li2ZrO3/Li6Zr2O7 in which the dominance of the Li6Zr2O7 phase is observed during high-temperature mechanical tests, a more pronounced decrease in resistance to cracking is observed, due to thermal expansion of the crystal lattice. Full article
(This article belongs to the Special Issue Mechanical Behavior and Reliability of Engineering Ceramics)
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<p>Results of X-ray phase analysis of the studied samples of lithium-containing ceramics depending on the variation in the concentration of the initial components.</p>
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<p>Results of X-ray phase analysis of the studied samples of lithium-containing ceramics depending on the variation in the concentration of the initial components.</p>
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<p>Results of changes in the strength parameters of lithium-containing ceramics depending on the concentration of the lithium-containing component: (<b>a</b>) results of changes in hardness and (<b>b</b>) results of changes in resistance to single compression at a compression speed of 0.1 mm/min.</p>
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<p>Results of strengthening depending on the concentration of impurity phases: (<b>a</b>) when changing the concentration of LiO<sub>2</sub> and (<b>b</b>) when changing the concentration of Li<sub>6</sub>Zr<sub>2</sub>O<sub>7</sub>.</p>
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<p>Results of tests on the crack resistance of ceramics when changing the rate of single compression in the case of varying ceramic compositions: (<b>a</b>) composition 1 and (<b>b</b>) composition 2.</p>
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<p>Results of changes in cracking resistance with changes in compression rate: (<b>a</b>) composition 1 and (<b>b</b>) composition 2.</p>
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<p>Results of changes in the thermal conductivity coefficient of the studied ceramics depending on changes in the concentration of lithium-containing components.</p>
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<p>Results of a study of resistance to single compression at different temperatures of lithium-containing ceramics: (<b>a</b>) composition 1 and (<b>b</b>) composition 2.</p>
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<p>(<b>a</b>) Results of changes in the coefficient of volumetric thermal expansion and (<b>b</b>) results of changes in hardness values of ceramic samples after thermal stability tests.</p>
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8 pages, 2232 KiB  
Communication
Oxygen-Bonding State and Oxygen-Reduction Reaction Mechanism of Pr0.7Ca0.3Mn1−xCoxO3−d (x = 0, 0.1, 0.2, 0.3)
by Kanghee Jo, Seungjae Lee and Heesoo Lee
Ceramics 2023, 6(4), 2386-2393; https://doi.org/10.3390/ceramics6040146 - 15 Dec 2023
Cited by 1 | Viewed by 1523
Abstract
We investigated the effects of Co doping on Pr0.7Ca0.3MnO3−d in the perspective of an oxygen-bonding state change. In all compositions, Pr0.7Ca0.3Mn1−xCoxO3−d (PCMCx, x = 0, 0.1, 0.2, 0.3) showed [...] Read more.
We investigated the effects of Co doping on Pr0.7Ca0.3MnO3−d in the perspective of an oxygen-bonding state change. In all compositions, Pr0.7Ca0.3Mn1−xCoxO3−d (PCMCx, x = 0, 0.1, 0.2, 0.3) showed an orthorhombic structure, and the lattice gradually contracted with increasing Co content. The doped Co was mostly present as 2+ and 3+, which decreased the average oxidation value of the B site and created oxygen vacancies for charge compensation. However, as the Co content increased, the proportion of Co3+ increased, and the content of oxygen vacancies gradually decreased. In addition, the ratio of adsorbed oxygen in PCMC0.1 was the highest, and the B-O covalency was enhanced. Accordingly, the electrochemical reaction of oxygen with the cathode material in PCMC0.1 could occur most easily, showing the smallest polarization resistance among the Co-doped Pr0.7Ca0.3MnO3−d. We can confirm the formation of oxygen vacancies via Co doping and the effect of B-O covalency on the oxygen-reduction reaction of Pr0.7Ca0.3MnO3−d. Full article
(This article belongs to the Special Issue Advances in Electronic Ceramics)
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<p>X-ray diffraction pattern and (112) peak of Co-doped Pr<sub>0.7</sub>Ca<sub>0.7</sub>MnO<sub>3−d</sub>.</p>
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<p>X-ray photoelectron spectra of PCMCx and peak deconvolution result: (<b>a</b>–<b>d</b>) O 1s core level spectra, (<b>e</b>–<b>h</b>) Mn 2p 3/2 core level spectra of PCM and PCMC0.1–0.3, and (<b>i</b>–<b>k</b>) Co 2p 1/2 core level spectra of PCMC0.1–0.3.</p>
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<p>(<b>a</b>) Electrochemical impedance spectra of PCMCx. Rohm was subtracted to emphasize the polarization resistance and (<b>b</b>) fitting result at 550 °C.</p>
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<p>Distribution of relaxation time spectra of PCMCx via temperature: (<b>a</b>) 550 °C, (<b>b</b>) 650 °C, and (<b>c</b>) 750 °C.</p>
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19 pages, 4618 KiB  
Article
Assessing the Effects of Refuse-Derived Fuel (RDF) Incorporation on the Extrusion and Drying Behavior of Brick Mixtures
by Ioannis Makrygiannis, Athena Tsetsekou, Orestis Papastratis and Konstantinos Karalis
Ceramics 2023, 6(4), 2367-2385; https://doi.org/10.3390/ceramics6040145 - 14 Dec 2023
Viewed by 1760
Abstract
This study explores the potential benefits of incorporating Recycled Demolition Waste (RDF) as an additive in ceramic mass for the brick industry, with a focus on applications such as thermoblocks. The research underscores the significance of sustainable waste management practices and environmental conservation [...] Read more.
This study explores the potential benefits of incorporating Recycled Demolition Waste (RDF) as an additive in ceramic mass for the brick industry, with a focus on applications such as thermoblocks. The research underscores the significance of sustainable waste management practices and environmental conservation by diverting waste from landfills. RDF, exhibiting combustion properties above 550 °C, emerges as a valuable candidate for enhancing clay-based materials, particularly in the brick production process where firing temperatures exceed 850 °C. Conducted in two phases, the research initially concentrated on RDF preparation, RDF integration with clay materials, and its influence on extrusion and drying phases. Employing innovative techniques involving brick and tile industry machinery coupled with sand incorporation yielded promising results. The grounding of RDF particles to less than 1 mm not only facilitated the mixing process but also ensured stable grinding temperatures within the hammer mill, reducing operational costs. During extrusion, challenges associated with unprocessed RDF material were addressed by utilizing ground RDF, leading to a more efficient and cost-effective process with enhanced plasticity and reduced water requirements. Practical implications for brick plant operations were identified, promoting resource and energy savings. Drying behavior analysis revealed the positive impact of RDF integration, showcasing reduced sensitivity, decreased drying linear shrinkage, and improved density properties. RDF’s role as an inert additive resulted in a 5% reduction in density, enhancing porosity and thermal insulation properties, particularly in thermoblock applications. In the brick industry, where durability, thermal performance, and cost-efficiency are paramount, this study emphasizes the potential benefits of incorporating RDF into clay-based materials. While further research is needed to address the firing procedure of RDF as a brick mass additive, the initial findings underscore the promise of this approach for sustainable and environmentally responsible brick production. This study contributes to the literature by shedding light on the advantages and challenges of integrating RDF into clay-based products, supporting sustainability and waste reduction in construction and manufacturing. The findings provide valuable insights into the performance and feasibility of these mixtures, offering crucial information for industries striving to adopt eco-conscious production methods. This article not only outlines the applied methodology and experimental setup but also presents results related to the behavior of RDF-inclusive clay block mixtures in the production environment. Anticipated to exert considerable influence on future practices and policies, this research contributes to the growing body of knowledge concerning eco-friendly and sustainable manufacturing processes. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>Materials used in the current study.</p>
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<p>Drying circle and each of the 3 phases followed for the tests.</p>
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<p>(<b>Left</b>): mixture with unprocessed RDF (TZRDF10). (<b>Right</b>): mixture of processed RDF (TZRDF10P).</p>
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<p>(<b>Left</b>): 100% clay after cutting. <b>Middle</b>: Processed RDF mix after cutting. (<b>Right</b>): Unprocessed RDF mix after cutting.</p>
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<p>Plasticity by Pfefferkorn and necessary extrusion water for all mixtures.</p>
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<p>Drying linear shrinkage and drying sensitivity of the dried samples.</p>
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<p>Drying bending strength and density of the dried samples.</p>
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<p>Re-absorption of dry products over 24 h in room conditions.</p>
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<p>(<b>a</b>) Surface of dry sample from 100%. (<b>b</b>) Surface of dry sample from TZRDF10 (unprocessed RDF). (<b>c</b>) Surface of dry sample from TZRDF10P. (<b>d</b>) Side view from the cutting area of dry sample from TZ. (<b>e</b>) Side view from the cutting area of dry sample from TZRDF10. (<b>f</b>) Side view from the cutting area of dry sample from TZRDF10P.</p>
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15 pages, 4240 KiB  
Article
Optimizing the Fly Ash/Activator Ratio for a Fly Ash-Based Geopolymer through a Study of Microstructure, Thermal Stability, and Electrical Properties
by Meenakshi Yadav, Lalit Kumar, Vikas Yadav, Karthikeyan Jagannathan, Vidya Nand Singh, Surinder P. Singh and V. Ezhilselvi
Ceramics 2023, 6(4), 2352-2366; https://doi.org/10.3390/ceramics6040144 - 12 Dec 2023
Cited by 1 | Viewed by 2150
Abstract
Fly ash (FA)-based geopolymer was prepared using sodium hydroxide and sodium silicate (in 2.5ratio) as an alkali activator liquid (AL). The condition of FA/AL was optimized for achieving 1.00, 1.25, 1.5, and 1.75 ratios by varying the alkali concentrations, which are referred to [...] Read more.
Fly ash (FA)-based geopolymer was prepared using sodium hydroxide and sodium silicate (in 2.5ratio) as an alkali activator liquid (AL). The condition of FA/AL was optimized for achieving 1.00, 1.25, 1.5, and 1.75 ratios by varying the alkali concentrations, which are referred to as GP1, GP2, GP3, and GP4, respectively. The influence of slight variations in the FA/AL ratio on microstructure, morphology, functional groups, and composition was investigated by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), X-ray fluorescence (XRF), and Fourier transform infrared spectroscopy (FTIR). FESEM detected a homogeneous fused matrix of fly ash and alkali activator solution up to 1.5 ratios; GP3 showed a dense morphology. FTIR confirmed that the formation of aluminosilicate gel induced a shift in the T–O (T = Si or Al) asymmetric stretching band, nearing a lower frequency. XRD showed an amorphous structure with phases, including quartz, mullite, hematite, and sodalite. The thermogravimetry and differential thermal analysis (TGA–DTA) indicated that the geopolymer samples were thermally stable. The electrical study concluded that the geopolymer possessed insulating properties. Full article
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<p>Surface morphology of fly ash.</p>
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<p>SEM images of geopolymer prepared at different ratios of FA/AL: (<b>a</b>) 1.00 (GP1), (<b>b</b>) 1.25 (GP2), (<b>c</b>) 1.50 (GP3), and (<b>d</b>) 1.75 (GP4), respectively.</p>
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<p>XRD spectra of fly ash.</p>
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<p>XRD spectra of geopolymer samples prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4), respectively.</p>
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<p>Structures of (<b>a</b>) quartz, (<b>b</b>) mullite, and (<b>c</b>) hematite (VESTA-Visualization for electronic and structural analysis).</p>
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<p>FTIR spectra of fly ash.</p>
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<p>FTIR spectra of geopolymers prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4).</p>
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<p>TGA curves of geopolymers prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4).</p>
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<p>DTA curves of geopolymers prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4).</p>
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<p>Conductivity versus frequency plot of geopolymers prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4).</p>
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<p>Permittivity/dielectric constant versus frequency plot of geopolymers prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4).</p>
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<p>D factor versus frequency plot of geopolymers prepared at different ratios of FA/AL: (a) 1.00 (GP1), (b) 1.25 (GP2), (c) 1.50 (GP3), and (d) 1.75 (GP4).</p>
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19 pages, 52581 KiB  
Article
Investigation of Porous Ceramic Structures Based on Hydroxyapatite and Wollastonite with Potential Applications in the Field of Tissue Engineering
by Andreia Cucuruz, Cristina-Daniela Ghițulică, Georgeta Voicu, Cătălina-Alexandra Bogdan, Vasilica Dochiu and Roxana Cristina Popescu
Ceramics 2023, 6(4), 2333-2351; https://doi.org/10.3390/ceramics6040143 - 8 Dec 2023
Cited by 1 | Viewed by 1876
Abstract
Bioceramics are the most promising materials used for hard tissue reconstruction. In this study, wollastonite/hydroxyapatite (HAp/WS)-type composite ceramic structures were synthesized with the aim of reaching a material with improved properties for use in bone tissue regeneration. The scaffolds were synthesized using a [...] Read more.
Bioceramics are the most promising materials used for hard tissue reconstruction. In this study, wollastonite/hydroxyapatite (HAp/WS)-type composite ceramic structures were synthesized with the aim of reaching a material with improved properties for use in bone tissue regeneration. The scaffolds were synthesized using a foam replica method, starting from ceramic powders with different mass ratios. These were subsequently studied and compared to identify the ideal mass ratio in terms bioactive character, appropriate mechanical properties, but also microstructural influence. The results indicate that all of the samples showed a highly porous microstructure with interconnected pores and high mineralization after 21 days of immersion in SBF. The porous structures with 90% and 70% mass contents of hydroxyapatite presented a well-defined structure and the highest values of mechanical compressive strength. Biocompatibility evaluation showed that osteoblast-like cells are able to penetrate the inner volume of the structures, exhibiting a biocompatible behavior in terms of morphological features and viability following 7 days of incubation. All results show that the porous composite ceramics with 90% and 70% mass contents of hydroxyapatite are promising materials for bone tissue regeneration. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>Schematic representation of the obtained ceramic powders with different weight ratios.</p>
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<p>Schematic representations of the polyurethane sponge, sponge immersed in ceramic suspension and porous ceramic structures after thermal treatment at a temperature of 1200 °C.</p>
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<p>(<b>a</b>) X-ray diffractograms recorded for the composite ceramic powders, with different mass ratios Hap/WS, thermally treated at a temperature of 1000 °C and (<b>b</b>) zoom made on region 2θ:29–35.</p>
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<p>Derivatogram of the polyurethane sponge.</p>
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<p>SEM images of porous structures: (<b>A</b>–<b>C</b>) 1 Hap/9 WS, (<b>D</b>–<b>F</b>) 3 Hap/7 WS, (<b>G</b>–<b>I</b>) 5 Hap/5 WS, (<b>J</b>–<b>L</b>) 7 Hap/3 WS and (<b>M</b>–<b>O</b>) 9 Hap/1 WS, at magnifications of 100×, 1000×, and 10,000×, respectively.</p>
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<p>SEM images of porous structures: (<b>A</b>–<b>C</b>) 1 Hap/9 WS, (<b>D</b>–<b>F</b>) 3 Hap/7 WS, (<b>G</b>–<b>I</b>) 5 Hap/5 WS, (<b>J</b>–<b>L</b>) 7 Hap/3 WS and (<b>M</b>–<b>O</b>) 9 Hap/1 WS, at magnifications of 100×, 1000×, and 10,000×, respectively.</p>
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<p>SEM images of porous structures: (<b>A</b>) 1 HAp/9 WS, (<b>B</b>) 3 HAp/7 WS, (<b>C</b>) 5 HAp/5 WS, (<b>D</b>) 7 HAp/3 WS and (<b>E</b>) 9 HAp/1 WS after 21 days in SBF.</p>
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<p>Cell viability profile of MG-63 osteoblast-like cells following 7 days of incubation on HAp/WS scaffolds. Results are represented as mean ± STDEV (<span class="html-italic">n</span> = 3); statistical significance: * <span class="html-italic">p</span> &lt; 0.05, ** <span class="html-italic">p</span> &lt; 0.01.</p>
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<p>SEM micrographs of porous structures with osteoblast-like cells on (<b>A</b>) 1 HAp/9 WS, (<b>B</b>) 3 HAp/7 WS, (<b>C</b>) 5 HAp/5 WS, (<b>D</b>) 7 HAp/3 WS and (<b>E</b>) 9 HAp/1 WS after 7 days.</p>
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13 pages, 5438 KiB  
Article
Analysis of the Structure and Durability of Refractory Castables Impregnated with Sodium Silicate Glass
by Jurgita Malaiškienė, Valentin Antonovič, Renata Boris, Andrius Kudžma and Rimvydas Stonys
Ceramics 2023, 6(4), 2320-2332; https://doi.org/10.3390/ceramics6040142 - 4 Dec 2023
Cited by 1 | Viewed by 2394
Abstract
This study examines the impact of the impregnation of fireclay-based conventional (CC) and medium-cement castables (MCCs) with liquid sodium silicate glass under vacuum conditions. The goal is to assess how this treatment affects the physical and mechanical properties and durability (alkali and thermal [...] Read more.
This study examines the impact of the impregnation of fireclay-based conventional (CC) and medium-cement castables (MCCs) with liquid sodium silicate glass under vacuum conditions. The goal is to assess how this treatment affects the physical and mechanical properties and durability (alkali and thermal shock resistance) of these castables used in biomass combustion boilers, where they are exposed to temperatures up to 1100 °C. The research work employs standard test methods to evaluate the physical and mechanical properties. Additionally, advanced techniques such as scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray diffraction (XRD), and specific tests for alkali resistance and thermal shock resistance are used. The research findings suggest that impregnation with sodium silicate glass under vacuum significantly enhances the alkali resistance of both CC and MCCs. This improvement is primarily due to the reduction in porosity and the increase in density. SEM images reveal that the impregnated samples are coated with a glassy layer and the pores are partially filled with sodium silicate. Tests for alkali resistance demonstrate the formation of a protective glassy layer (with a thickness of 0.9–1.5 mm) on the castable surfaces, thereby reducing the further penetration of alkali into deeper layers of the samples. However, it is important to mention that the impregnated refractory castables have reduced resistance to thermal shock cycles. Full article
(This article belongs to the Special Issue Innovative Manufacturing Processes of Silicate Materials)
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<p>The scheme of the “crucible method” of a test sample (<b>a</b>) and a polished samples for SEM–EDS tests (<b>b</b>).</p>
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<p>Xray analysis of control (<b>a</b>) and impregnated (<b>b</b>) samples. (1—CC-1, 2—CC-2, 3—MCC-1, 4—MCC-2).</p>
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<p>The images of control and impregnated samples (P—pore, BSS—blown sodium silicate, TPM—typical porous matrix): (<b>a</b>) CC-1- impregnated, (<b>b</b>) CC-2- impregnated, (<b>c</b>) MCC-1- impregnated, (<b>d</b>) MCC-2- impregnated, (<b>e</b>) CC-1 control, (<b>f</b>) CC-2 control, (<b>g</b>) MCC-1 control, (<b>h</b>) MCC-2 control.</p>
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<p>Results of density and <span class="html-italic">UPV</span> of control and impregnated samples.</p>
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<p>Porosity of control and impregnated samples.</p>
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<p>CCS of control and impregnated samples.</p>
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<p>Images of impregnated refractory castable samples after 20 cycles of alkaline exposure (dashed line—zone of protestive glassy barrier formation): (<b>a</b>) CC-1 control, (<b>b</b>) CC-2 control, (<b>c</b>) MCC-1 control, (<b>d</b>) MCC-2 control, (<b>e</b>) CC-1- impregnated, (<b>f</b>) CC-2- impregnated, (<b>g</b>) MCC-1- impregnated, (<b>h</b>) MCC-2- impregnated.</p>
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<p>Relative content of potassium at different penetration distances: (<b>a</b>) control samples; (<b>b</b>) impregnated samples.</p>
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<p>Modulus of elasticity of control and impregnated samples.</p>
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<p>The comparison of thermal shock resistance of control and impregnated samples.</p>
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13 pages, 2368 KiB  
Article
Fabrication and Characterization of Narrow-Wavelength Phosphors of Tb-Doped Yttrium-Silicon-Aluminum Oxynitride Using Spray Pyrolysis
by Bramantyo Bayu Aji, Yu-Hsiuan Huang, Masatsugu Oishi, Toshihiro Moriga and Shao-Ju Shih
Ceramics 2023, 6(4), 2307-2319; https://doi.org/10.3390/ceramics6040141 - 3 Dec 2023
Viewed by 1931
Abstract
Selective emission of green light phosphor powder Y4SiAlO8N as the host material and Tb3+ as the activator was successfully achieved using spray pyrolysis (SP). Samples synthesized with various calcination temperatures and precursor concentrations indicated that the most suitable [...] Read more.
Selective emission of green light phosphor powder Y4SiAlO8N as the host material and Tb3+ as the activator was successfully achieved using spray pyrolysis (SP). Samples synthesized with various calcination temperatures and precursor concentrations indicated that the most suitable parameter for the synthesized powder is the calcination of 0.05 M Y3.92SiAlO8N:0.08Tb3+ at a temperature of 1600 °C. The effect of the selected parameters was substantiated by the high purity of the Y3.92SiAlO8N:0.08Tb3+ phase, as confirmed by X-ray diffraction (XRD) analysis. The Scherrer equation was used to calculate grain size. In addition, scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometry (EDS) confirmed the presence of micron-sized particles, which matched well with the theoretical chemical composition. The specific surface area of the phosphor powder was determined using the Brunauer–Emmett–Teller method. Finally, fluorescence spectrometry was used to determine the luminescence properties. The correlation between the crystallinity of the phosphor powder and narrowing emission is also discussed. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>XRD patterns of as-received powder and the Y<sub>3.92</sub>SiAlO<sub>8</sub>N:0.08Tb<sup>3+</sup> powders calcined at the temperatures of 1300, 1400, 1500, 1600, and 1650 °C.</p>
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<p>Crystallite sizes of as-received powder and the Y<sub>3.92</sub>SiAlO<sub>8</sub>N:0.08Tb<sup>3+</sup> powders calcined at the temperatures of 1300, 1400, 1500, 1600, and 1650 °C.</p>
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<p>SEM images of (<b>a</b>) as-received powder and the Y<sub>3.92</sub>SiAlO<sub>8</sub>N:0.08Tb<sup>3+</sup> powders calcined at the temperatures of (<b>b</b>) 1300, (<b>c</b>) 1400, (<b>d</b>) 1500, (<b>e</b>) 1600, and (<b>f</b>) 1650 °C.</p>
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<p>EDS spectra of (<b>a</b>) as-received powder and the Y<sub>3.92</sub>SiAlO<sub>8</sub>N:0.08Tb<sup>3+</sup> powders calcined at the temperatures of (<b>b</b>) 1300, (<b>c</b>) 1400, (<b>d</b>) 1500, (<b>e</b>) 1600, and (<b>f</b>) 1650 °C.</p>
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<p>(<b>a</b>) Excitation (λem = 543 nm) and (<b>b</b>) emission spectra (λex = 251 nm) of Y<sub>3.92</sub>SiAlO<sub>8</sub>N:0.08Tb<sup>3+</sup> phosphor powders calcined at the temperatures of 1300, 1400, 1500, 1600, and 1650 °C.</p>
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<p>Correlation between photoluminescence intensity (<sup>5</sup>D<sub>4</sub> → <sup>7</sup>F<sub>5</sub>) and crystalline size for Y<sub>3.92</sub>SiAlO<sub>8</sub>N:0.08Tb<sup>3+</sup> powders.</p>
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12 pages, 1107 KiB  
Article
Features of Structures and Ionic Conductivity of Na3Fe2(PO4)3 Polycrystals Obtained by Solid Phase and Melt Methods
by A. S. Nogai, A. A. Nogai, D. E. Uskenbaev, A. B. Utegulov, E. A. Nogai and D. D. Toleugulov
Ceramics 2023, 6(4), 2295-2306; https://doi.org/10.3390/ceramics6040140 - 29 Nov 2023
Cited by 3 | Viewed by 1659
Abstract
This article investigates the structures and conductive properties of polycrystals of Na3Fe2(PO4)3 obtained by solid-state and melt synthesis methods using concentrated optical radiation. It has been established that in the melt synthesis method, the material is [...] Read more.
This article investigates the structures and conductive properties of polycrystals of Na3Fe2(PO4)3 obtained by solid-state and melt synthesis methods using concentrated optical radiation. It has been established that in the melt synthesis method, the material is synthesized under significantly non-equilibrium thermodynamic conditions, leading to the creation of deformations in the sample, which contribute to the enhancement of ionic conductivity. Additionally, the synthesis duration is reduced by half. Through a comparative assessment of the structural parameters and conductive properties of these materials, it is demonstrated that polycrystals obtained by the melt method exhibit better texture and higher ionic conductivity. The occurrence of deformations during the synthesis of α-Na3Fe2(PO4)3 under high temperature-gradient conditions indicates the elasticity of the crystalline framework {[Fe2(PO4)]3−}3∞. It is concluded that the non-equilibrium thermodynamic conditions of α-Na3Fe2(PO4)3 synthesis promote the formation of deformations in the crystalline structure of polycrystals, leading to a partial increase in symmetry and ionic conductivity. Full article
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<p>Diffraction patterns of Na<sub>3</sub>Fe<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub> polycrystals obtained by solid-phase (Type 1) and melt (Type 2) methods.</p>
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<p>Microstructures of polycrystals and percentage of elemental composition for Na<sub>3</sub>Fe<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub> (at a scale of 30 μm), obtained by the solid-phase method: (<b>a</b>) sample Type 1; and melt method (<b>b</b>) Type 2 sample.</p>
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<p>Percentage of elemental composition for Na<sub>3</sub>Fe<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub> polycrystals obtained by the solid-phase method: (<b>a</b>) sample Type 1; melt method (<b>b</b>) Type 2 sample.</p>
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<p>Temperature dependences of the ionic conductivity of Na<sub>3</sub>Fe<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub> polycrystals obtained by solid-phase (Type 1) and melt (Type 2) methods.</p>
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13 pages, 3303 KiB  
Article
Hydroxyapatite-Resin Composites Produced by Vat Photopolymerization and Post-Processing via In Situ Hydrolysis of Alpha Tricalcium Phosphate
by Carolina Oliver-Urrutia, Lenka Drotárová, Sebastián Gascón-Pérez, Karel Slámečka, Simona Ravaszová, Ladislav Čelko and Edgar B. Montufar
Ceramics 2023, 6(4), 2282-2294; https://doi.org/10.3390/ceramics6040139 - 24 Nov 2023
Viewed by 2171
Abstract
Vat photopolymerization is an additive manufacturing technique that utilizes photosensitive resins to fabricate 3D polymeric objects with high precision. However, these objects often lack mechanical strength. This study investigated the strengthening of a resin based on epoxidized soybean oil acrylate, specifically designed for [...] Read more.
Vat photopolymerization is an additive manufacturing technique that utilizes photosensitive resins to fabricate 3D polymeric objects with high precision. However, these objects often lack mechanical strength. This study investigated the strengthening of a resin based on epoxidized soybean oil acrylate, specifically designed for vat photopolymerization, by the in situ formation of hydroxyapatite nanocrystals. First, a stable alpha tricalcium phosphate (α-TCP)-resin feedstock mixture was developed (~30 vol.% α-TCP), which proved suitable for fabricating monoliths as well as complex triply periodic minimal surface (gyroid, diamond, and Schwarz) porous structures through vat photopolymerization. The results demonstrated that the incorporation of α-TCP particles led to a significant mechanical improvement of the resin. Second, post-printing hydrothermal treatments were utilized to transform the α-TCP particles into hydroxyapatite crystals within the resin. It was observed that the space between hydroxyapatite crystals within the composites was occupied by the cured resin, resulting in a more compact, stronger, and mechanically more reliable material than the porous hydroxyapatite produced by the hydrolysis of α-TCP mixed with water. Moreover, water absorption during the hydrothermal treatments caused the plasticization of the cured resin. As a consequence, the hydroxyapatite-resin composites displayed slightly lower mechanical properties compared to the as-printed α-TCP-resin composite. Full article
(This article belongs to the Special Issue Innovative Research on Calcium Phosphates Based Ceramics)
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<p>STL models and VPP CDHA/R-90 porous structures.</p>
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<p>Microstructure of VPP composites. (<b>a</b>) α-TCP/R monolith (left) and cured resin without ceramic powder (right). (<b>b</b>) Hydrothermally treated CDHA-resin composites.</p>
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<p>XRD patterns of composites fabricated by VPP. Composite components (Resin and CDHA-ctrl) are included for comparison. Right hand plot is a detailed view of the patterns in the range 20–41°.</p>
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<p>ATR-FTIR spectra of composites fabricated by VPP. Composite components (Resin and CDHA-ctrl) are included for comparison.</p>
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<p>Results of compression tests of composite monoliths and composite components. (<b>a</b>) Compressive stress–strain curves with the highest and lowest values. (<b>b</b>) Yield strength and compressive strength. The compressive strength of the Resin corresponds to the stress at 20% strain. (<b>c</b>) Young’s modulus. Bar plots show average ± SD values (<span class="html-italic">n</span> = 5).</p>
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<p>Images of CDHA/R-90 porous structures. (<b>a</b>) Schwarz lateral view, (<b>b</b>) Schwarz top view, (<b>c</b>) gyroid lateral view, and (<b>d</b>) diamond lateral view.</p>
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<p>Mechanical behavior of CDHA/R-90 porous structures. (<b>a</b>) Compressive stress–strain curves, and images of fracture surfaces in (<b>b</b>) gyroid and (<b>c</b>) diamond TPMS porous structures. Thin arrows point to the cup and cone fractures and dash ellipses show examples of the periodic rough surface.</p>
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13 pages, 2818 KiB  
Article
Inorganic Green Pigments Based on LaSr2AlO5
by Kazuki Yamaguchi, Akari Takemura, Saki Furumoto, Ryohei Oka and Toshiyuki Masui
Ceramics 2023, 6(4), 2269-2281; https://doi.org/10.3390/ceramics6040138 - 22 Nov 2023
Viewed by 1918
Abstract
La1.03Sr1.97Al0.97M0.03O5 (M = Fe, Co, Ni, and Cu) samples were synthesized using a citrate sol–gel method to develop a novel environmentally friendly inorganic green pigment. Among them, the Co-doped sample exhibited a vivid [...] Read more.
La1.03Sr1.97Al0.97M0.03O5 (M = Fe, Co, Ni, and Cu) samples were synthesized using a citrate sol–gel method to develop a novel environmentally friendly inorganic green pigment. Among them, the Co-doped sample exhibited a vivid yellow, but not green. Then, (La0.94Ca0.06)Sr2(Al0.97Mn0.03)O5 was synthesized and characterized with respect to the crystal structure, optical properties, and color. The sample was obtained in a single-phase form and the lattice volume was smaller than that of the (La0.94Ca0.06)Sr2AlO5 sample, indicating that Mn ions in the lattice of the sample were pentavalent. The sample exhibited optical absorption at a wavelength below 400 nm and around 650 nm. These absorptions were attributed to the ligand, the metal charge transfer (LMCT), and d-d transitions of Mn5+. Because the green light corresponding to 500 to 560 nm was reflected strongly, the synthesized sample exhibited a bright green color. (La0.94Ca0.06)Sr2(Al0.97Mn0.03)O5 showed high brightness (L* = 50.1) and greenness (a* = −20.8), and these values were as high as those of the conventional green pigments such as chromium oxide and cobalt green. Therefore, the (La0.94Ca0.06)Sr2(Al0.97Mn0.03)O5 pigment is a potential candidate for a novel environmentally friendly inorganic green pigment. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>XRD patterns of the LaSr<sub>2</sub>AlO<sub>5</sub>, LaSr<sub>2</sub>(Al<sub>0.97</sub>Fe<sub>0.03</sub>)O<sub>5</sub>, and La<sub>1.03</sub>Sr<sub>1.97</sub>(Al<sub>0.97</sub><span class="html-italic">M</span><sub>0.03</sub>)O<sub>5</sub> (<span class="html-italic">M</span>: Co, Ni, and Cu) samples. The standard data of LaSr<sub>2</sub>AlO<sub>5</sub> is based on the literature reported by Im, W.B et al. (2009) [<a href="#B15-ceramics-06-00138" class="html-bibr">15</a>].</p>
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<p>UV-Vis reflectance spectra for the LaSr<sub>2</sub>AlO<sub>5</sub>, LaSr<sub>2</sub>(Al<sub>0.97</sub>Fe<sub>0.03</sub>)O<sub>5</sub>, and La<sub>1.03</sub>Sr<sub>1.97</sub>(Al<sub>0.97</sub><span class="html-italic">M</span><sub>0.03</sub>)O<sub>5</sub> (<span class="html-italic">M</span>: Co, Ni, and Cu) samples.</p>
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<p>Photographs of the LaSr<sub>2</sub>AlO<sub>5</sub>, LaSr<sub>2</sub>(Al<sub>0.97</sub>Fe<sub>0.03</sub>)O<sub>5</sub>, and La<sub>1.03</sub>Sr<sub>1.97</sub>(Al<sub>0.97</sub><span class="html-italic">M</span><sub>0.03</sub>)O<sub>5</sub> (<span class="html-italic">M</span>: Co, Ni, and Cu) samples.</p>
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<p>Photographs of the La<sub>1+<span class="html-italic">x</span></sub>Sr<sub>2−<span class="html-italic">x</span></sub>(Al<sub>1−<span class="html-italic">x</span></sub>Co<span class="html-italic"><sub>x</sub></span>)O<sub>5</sub> (<span class="html-italic">x</span> = 0, 0.03, 0.05, and 0.10) samples.</p>
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<p>XRD patterns of the (La<sub>1−2<span class="html-italic">x</span></sub>Ca<sub>2<span class="html-italic">x</span></sub>)Sr<sub>2</sub>(Al<sub>1−<span class="html-italic">x</span></sub>Mn<span class="html-italic"><sub>x</sub></span>)O<sub>5</sub> (<span class="html-italic">x</span> = 0 and 0.03) and (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>AlO<sub>4.97</sub> samples. The standard data of LaSr<sub>2</sub>AlO<sub>5</sub> is based on the literature reported by Im, W.B et al. (2009) [<a href="#B15-ceramics-06-00138" class="html-bibr">15</a>].</p>
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<p>Rietveld refinement profiles of the XRD patterns for the (<b>a</b>) LaSr<sub>2</sub>AlO<sub>5</sub>, (<b>b</b>) (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>AlO<sub>4.97</sub>, and (<b>c</b>) (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>(Al<sub>0.97</sub>Mn<sub>0.03</sub>)O<sub>5</sub> samples. The black cross symbols and the solid red lines represent the observed and calculated intensities, respectively. The difference profiles between the observed and calculated patterns are depicted as a blue line at the bottom. The green vertical bars show the Bragg reflection peaks.</p>
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<p>(<b>a</b>) Crystal structure obtained via the Rietveld analysis for (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>(Al<sub>0.97</sub>Mn<sub>0.03</sub>)O<sub>5</sub>. (<b>b</b>) The octahedral coordination environment of La/Sr(1)O<sub>8</sub>, the decahedral coordination environment of Sr(2)O<sub>10</sub>, and the tetrahedral coordination environment of AlO<sub>4</sub>.</p>
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<p>UV-Vis reflectance spectra for the LaSr<sub>2</sub>AlO<sub>5</sub>, (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>AlO<sub>4.97</sub>, and (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>(Al<sub>0.97</sub>Mn<sub>0.03</sub>)O<sub>5</sub> samples.</p>
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<p>Photographs of the pellets of LaSr<sub>2</sub>AlO<sub>5</sub>, (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>AlO<sub>4.97</sub>, and (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>(Al<sub>0.97</sub>Mn<sub>0.03</sub>)O<sub>5</sub> powders.</p>
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<p>Photographs of the pellets of (La<sub>0.94</sub>Ca<sub>0.06</sub>)Sr<sub>2</sub>(Al<sub>0.97</sub>Mn<sub>0.03</sub>)O<sub>5</sub>, chromium oxide, cobalt green deep, and cobalt green pale powders.</p>
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13 pages, 7705 KiB  
Article
Effect of Ferrule Design on Stress Distribution of Maxillary Incisor Rehabilitated with Ceramic Crown and PEEK Post–Core Material: A 3D Finite Element Analysis
by Laura H. J. Alberto, Zhaoxu Zhang and Yuanyuan Duan
Ceramics 2023, 6(4), 2256-2268; https://doi.org/10.3390/ceramics6040137 - 20 Nov 2023
Cited by 1 | Viewed by 2233
Abstract
Endodontic-treated teeth with massive degrees of coronal tissue loss usually require rehabilitation with post-retained unitary crowns. This study aimed to evaluate the effect of ferrule design on the stress distribution of maxillary incisors rehabilitated with zirconia crowns using finite element analysis. Six three-dimensional [...] Read more.
Endodontic-treated teeth with massive degrees of coronal tissue loss usually require rehabilitation with post-retained unitary crowns. This study aimed to evaluate the effect of ferrule design on the stress distribution of maxillary incisors rehabilitated with zirconia crowns using finite element analysis. Six three-dimensional models were generated according to the presence and location of ferrule (No Ferrule, Buccal Ferrule, Lingual Ferrule, Buccolingual Ferrule, and Full Ferrule). The post–core materials tested were Nickel–chromium (NiCr) and Polyetheretherketone (PEEK). A static load of 100 N at a 45-degree angle on the Lingual surface, in a region 2 mm below the incisive ridge, was applied. Von Mises stresses and contour plots of all of the models were collected and analyzed. A lower and more uniform stress distribution was observed in the Full Ferrule model compared with the remaining models. A reduction of 72% in the von Mises peak stresses was observed in the root when comparing the Full Ferrule and No Ferrule models, both with PEEK post–core material. In conclusion, the presence of an incomplete ferrule is beneficial to the stress distribution in restored post-retained crowns. The use of PEEK for post–core structures reduces the stress concentration on the posts, reducing the predisposition to irreparable root fracture. Full article
(This article belongs to the Special Issue Ceramic Materials in Oral Applications)
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<p>Standard right central incisor for root canal treatment training. (<b>A</b>) Tomographic image produced using micro-CT; (<b>B</b>) resultant image after importing slices to Simpleware.</p>
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<p>Three-dimensional models generated with different ferrule designs (represented in blue colors and indicated with an asterisk). (<b>A</b>) No Ferrule model; (<b>B</b>) Buccal Ferrule model; (<b>C</b>) Lingual Ferrule model; (<b>D</b>) Buccolingual (BL) Ferrule model; and (<b>E</b>) Full Ferrule model.</p>
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<p>Models meshed with tetrahedron quadratic elements. (<b>A</b>) Frontal view; (<b>B</b>) lateral view.</p>
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<p>Boundary and load conditions. Constricted nodes are represented in orange, while the load direction and location are represented by yellow arrows. (<b>A</b>) Lingual view; (<b>B</b>) lateral view.</p>
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<p>Convergence test data.</p>
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<p>Peak stress values of all models’ component layers expressed in von Mises stress (MPa).</p>
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<p>Contour plot for stress distribution on the crown. The top row represents the buccolingual cross-section view and the bottom row represents the transverse plane view. Models: (<b>A</b>) No Ferrule (NiCr); (<b>B</b>) No Ferrule (PEEK); (<b>C</b>) Buccal Ferrule; (<b>D</b>) Lingual Ferrule; (<b>E</b>) Buccolingual Ferrule; and (<b>F</b>) Full Ferrule.</p>
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<p>Transverse plane view of stress distribution contour plots of ferrule and root model components. Models: (<b>A</b>) No Ferrule (NiCr); (<b>B</b>) No Ferrule (PEEK); (<b>C</b>) Buccal Ferrule; (<b>D</b>) Lingual Ferrule; (<b>E</b>) Buccolingual Ferrule; and (<b>F</b>) Full Ferrule.</p>
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<p>Contour plot for stress distribution on the buccolingual cross-section of the root and ferrule. Models: (<b>A</b>) No Ferrule (NiCr); (<b>B</b>) No Ferrule (PEEK); (<b>C</b>) Buccal Ferrule; (<b>D</b>) Lingual Ferrule; (<b>E</b>) Buccolingual Ferrule; and (<b>F</b>) Full Ferrule.</p>
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<p>Contour plot for stress distribution on the post–core layers of models without ferrule. (<b>A</b>) Lingual view of the No Ferrule model (PEEK); (<b>B</b>) Buccal view of the No Ferrule model (PEEK); (<b>C</b>) Lingual view of the No Ferrule model (NiCr); and (<b>D</b>) Buccal view of the No Ferrule model (NiCr).</p>
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13 pages, 6209 KiB  
Article
Coextrusion of Clay-Based Composites: Using a Multi-Material Approach to Achieve Gradient Porosity in 3D-Printed Ceramics
by Julian Jauk, Hana Vašatko, Lukas Gosch, Kristijan Ristoski, Josef Füssl and Milena Stavric
Ceramics 2023, 6(4), 2243-2255; https://doi.org/10.3390/ceramics6040136 - 17 Nov 2023
Cited by 1 | Viewed by 1959
Abstract
3D printing of ceramics has started gaining traction in architecture over the past decades. However, many existing paste-based extrusion techniques have not yet been adapted or made feasible in ceramics. A notable example is coextrusion, a common approach to extruding multiple materials simultaneously [...] Read more.
3D printing of ceramics has started gaining traction in architecture over the past decades. However, many existing paste-based extrusion techniques have not yet been adapted or made feasible in ceramics. A notable example is coextrusion, a common approach to extruding multiple materials simultaneously when 3D-printing thermoplastics or concrete. In this study, coextrusion was utilized to enable multi-material 3D printing of ceramic elements, aiming to achieve functionally graded porosities at an architectural scale. The research presented in this paper was carried out in two consecutive phases: (1) The development of hardware components, such as distinct material mixtures and a dual extruder setup including a custom nozzle, along with software environments suitable for printing gradient materials. (2) Material experiments including material testing and the production of exemplary prototypes. Among the various potential applications discussed, the developed coextrusion method for clay-based composites was utilized to fabricate ceramic objects with varying material properties. This was achieved by introducing a combustible as a variable additive while printing, resulting in a gradient porosity in the object after firing. The research’s originality can be summarized as the development of clay-based material mixtures encompassing porosity agents for 3D printing, along with comprehensive material-specific printing parameter settings for various compositions, which collectively enable the successful creation of functionally graded architectural building elements. These studies are expected to broaden the scope of 3D-printed clay in architecture, as it allows for performance optimization in terms of structural performance, insulation, humidity regulation, water absorption and acoustics. Full article
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<p>Pore structures visualized using an lCT40 micro-computed tomography device from Scanco, Switzerland. (<b>a</b>) 10 vol.-% paper sludge, (<b>b</b>) 10 vol.-% sawdust—both on 6 × 5 × 15 mm<sup>3</sup> samples. (<b>c</b>) Micropores in fired clay as captured using scanning electron microscopy.</p>
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<p>Cubic samples, unfired and fired, of material mixtures of wood sawdust and clay ranging from weight ratios of 2:7 (<b>left</b>) to the printable maximum of 1:3 (<b>center</b>) and 1:1 (<b>right</b>).</p>
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<p>The custom nozzle to enable coextrusion being designed in 3D (<b>left</b>), schematic drawing of the hardware setup (<b>center</b>) and the dual extruder setup (<b>right</b>).</p>
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<p>Test specimens exhibiting distinct material distribution within individual printed objects comprising standard extrusion with only the primary material (<b>left</b>), with a continuous coextrusion of primary and secondary material (<b>center</b>) and switching between standard extrusion and coextrusion according to printing path information (<b>right</b>) without affecting the overall geometry of the test specimens.</p>
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<p>Sanded test specimens comparing consistent printing settings (<b>left</b>) with the successful positioning of the inside material according to multiple user-defined patterns such as circular arrangement (<b>center</b>) and crossed arrangement (<b>right</b>).</p>
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<p>Cross-sections of different material compositions within one extrusion. From <b>left</b> to <b>right</b>, Mixtures 1, 2, 3, 4 and 5 as described in <a href="#ceramics-06-00136-t002" class="html-table">Table 2</a>.</p>
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<p>Concept drawing visualizing the cooling effect (<b>left</b>), printing process of the architectural prototype (<b>center</b>) and a mockup of printed objects exhibiting varying water absorption (<b>right</b>).</p>
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30 pages, 8746 KiB  
Article
High-Lead Glazed Ceramic Production in Western Iberia (Gharb al-Andalus) between the 10th and Mid-13th Centuries: An Approach from the City of Évora (Portugal)
by Carlos Andrés Camara, María José Gonçalves, José Antonio Paulo Mirão, Susana Gómez Martínez and Massimo Beltrame
Ceramics 2023, 6(4), 2213-2242; https://doi.org/10.3390/ceramics6040135 - 15 Nov 2023
Viewed by 2388
Abstract
In the present study an archaeometry programme has been developed on a limited number of coarse wares, monochrome, and bichrome glazed ceramics retrieved in the cities of Évora, Mértola, and Silves, located in Western Iberia, Portugal (Gharb al-Andalus during the Islamic period). [...] Read more.
In the present study an archaeometry programme has been developed on a limited number of coarse wares, monochrome, and bichrome glazed ceramics retrieved in the cities of Évora, Mértola, and Silves, located in Western Iberia, Portugal (Gharb al-Andalus during the Islamic period). The goals were to shed light on glazed ceramics provenance, technology, trading, and on the glaze technology applied. For this purpose, a multi-analytical approach was employed to characterize ceramic pastes and glazes using optical microscopy (OM), X-ray diffraction (XRD), X-ray fluorescence (XRF), and a Scanning Electron Microscope coupled to an Energy Dispersive Spectrometer (SEM-EDS). Results evidenced that over the Islamic rule, coarse wares were locally produced at Évora. On the contrary, monochrome and bichrome glazed ceramics were imported from the city of Silves, Mértola, and from unidentified workshops, probably located in southern Iberia. The analysis of decorations evidenced that despite the provenance of the samples, the glaze technology applied was rather uniform over time, depicting a widespread technological transfer in the al-Andalus. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>The Iberian Peninsula and the geographical location of Évora, Mértola, and Silves (elaborated by Massimo Beltrame).</p>
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<p>Adapted geological maps of the cities of Évora, Mértola, and Silves. Maps were downloaded from the website of the National Laboratory of Energy and Geology (Geoportal-LNEG-Portugal). The scale is 1:500,000 (elaborated by Massimo Beltrame).</p>
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<p>Picture of each unglazed and glazed ceramic sample included in the present study.</p>
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<p>Technical drawings of each ceramic sample (elaborated by Carlos Camara).</p>
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<p>Representative microphotographs of each pottery fabric collected in cross polarized light (XPL) (scale 750 µm): PF1 with an amphibole in the centre of the picture (EVR 1 sample), PF2 with angular to sub-rounded crystals of quartz and feldspars (EVR 15 sample), PF3 with and unmixed clay nodule (SIL 26 sample), PF4 with a buffy coloured ceramic paste and a small fragment of schist (EVR 12 sample), PF5 with thermally altered limestone fragments (EVR 16 sample) and PF6 very small crystals of muscovite mixed in the ceramic paste and a fragment of chert in the centre of the picture (EVR 2 sample).</p>
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<p>Unglazed and glazed ceramic samples plotted on the Paste-Temper-Porosity ternary plot.</p>
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<p>Samples ternary plots. Unglazed and glazed ceramic samples from Évora (<b>top</b>), Mértola (<b>bottom</b>) are plotted inside the (CaO + MgO) − Al<sub>2</sub>O<sub>3</sub> − SiO<sub>2</sub> ternary system.</p>
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<p>Samples ternary plots. Unglazed and glazed ceramic samples from Silves are plotted inside the (CaO + MgO) − Al<sub>2</sub>O<sub>3</sub> − SiO<sub>2</sub> ternary system.</p>
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<p>Samples binary plots. Identified pottery fabrics plotted inside the Na<sub>2</sub>O/CaO vs. CaO binary space (<b>top</b>), and inside the SiO<sub>2</sub> vs. CaO binary space (<b>bottom</b>).</p>
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<p>Samples of binary plots. Identified pottery fabrics plotted inside the Al<sub>2</sub>O<sub>3</sub>/K<sub>2</sub>O vs. CaO + MgO binary space.</p>
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<p>Inner and outer glazed surfaces plotted inside PbO/SiO<sub>2</sub> ratio vs. Na<sub>2</sub>O+K<sub>2</sub>O binary plots.</p>
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<p>Inner and outer glazed surfaces plotted inside PbO/SiO<sub>2</sub> ratio vs. Na<sub>2</sub>O+K<sub>2</sub>O binary plots.</p>
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<p>Inner and outer glazed surfaces plotted inside FeO vs. Al<sub>2</sub>O<sub>3</sub> (<b>top</b>) and SiO<sub>2</sub> vs. Al<sub>2</sub>O<sub>3</sub> (<b>bottom</b>) binary plots. Sample EVR 9 is not included in binary plots.</p>
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<p>Inner and outer glazed surfaces plotted inside FeO vs. Al<sub>2</sub>O<sub>3</sub> (<b>top</b>) and SiO<sub>2</sub> vs. Al<sub>2</sub>O<sub>3</sub> (<b>bottom</b>) binary plots. Sample EVR 9 is not included in binary plots.</p>
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<p>BSE and SE images and elemental mapping distribution of the SIL 29 sample (inner side) displaying a limited ceramic body–glaze interface made up of acicular and euhedral crystals (<b>A</b>), which, correspondingly, are composed of lead–potassium feldspar and calcium-rich pyroxene (<b>B</b>,<b>C</b>).</p>
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<p>Binary plot of Al<sub>2</sub>O<sub>3</sub> (ceramic paste vs. glaze) of the inner (<b>top</b>) and outer (<b>bottom</b>) glaze surfaces, evidencing that there was no diffusion of Al<sub>2</sub>O<sub>3</sub> from the ceramic body toward the glaze.</p>
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<p>Binary plot of SiO<sub>2</sub> (ceramic paste vs. glaze) of the inner (<b>top</b>) and outer (<b>bottom</b>) glaze surfaces, evidencing that there was no diffusion of SiO<sub>2</sub> from the ceramic body to the glaze.</p>
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<p>(<b>A</b>) BSE picture of black/brown decoration of sample MER 19 showing a rather homogeneous glaze. (<b>B</b>) BSE picture of black/brown decoration of sample EVR 11 showing different crystallites on the top surface of the glaze.</p>
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<p>(<b>A</b>–<b>C</b>) BSE picture and elemental mapping distribution of the black/brown decoration of sample EVR 2. (<b>B</b>–<b>D</b>) BSE picture and elemental mapping distribution of the black/brown decoration of sample EVR 11.</p>
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<p>(<b>A</b>–<b>C</b>) BSE picture and elemental mapping distribution of the black/brown decoration of sample SIL 25. (<b>B</b>–<b>D</b>) BSE picture and elemental mapping distribution of the black/brown decoration of sample SIL 26.</p>
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35 pages, 107018 KiB  
Article
Non-Invasive On-Site XRF and Raman Classification and Dating of Ancient Ceramics: Application to 18th and 19th Century Meissen Porcelain (Saxony) and Comparison with Chinese Porcelain
by Philippe Colomban, Gulsu Simsek Franci, Mareike Gerken, Michele Gironda and Viviane Mesqui
Ceramics 2023, 6(4), 2178-2212; https://doi.org/10.3390/ceramics6040134 - 12 Nov 2023
Cited by 4 | Viewed by 2223
Abstract
The authentication and dating of rare ceramics is generally carried out using subjective criteria, mainly based on visual interpretation. However, the scientific study and evaluation of the materials used could contribute objectively. The analytical data relating to the major and minor elements of [...] Read more.
The authentication and dating of rare ceramics is generally carried out using subjective criteria, mainly based on visual interpretation. However, the scientific study and evaluation of the materials used could contribute objectively. The analytical data relating to the major and minor elements of the coloring agents of the decoration or the base marks, and the characteristics of the raw materials (related to geology and ore processing), can be obtained on the conservation site non-invasively using a pXRF instrument and the phases formed may be identified using Raman microspectroscopy. This approach is applied to 28 objects assigned to the production of the Meissen Factory, from the collection of the Musée National de Céramique, Cité de la Céramique, Sèvres. They have polychromic or blue-and-white decorations and are supposed to have been produced in the 18th and 19th centuries. Some have a production date that has been perfectly established, others may have been produced using an earlier mold, or even have been decorated on an unknown date different from that of the firing of the biscuit. The combination of several classification criteria concerning the type of glaze, previously identified in the study of French and Chinese 17th and 18th centuries productions, i.e., the elements associated with cobalt present in the mark or the blue decoration and the relative levels of impurities of the glaze matrix, both characteristic of the raw materials and giving a strong XRF signal, leads to the identification of groups of homogeneous objects (respectively, counting seven, three, two and two objects for which at least four out of five criteria are identical); the other objects present too many differences to be considered as having been produced with the same raw materials. The first group brings together almost all the objects with a reliable pedigree made before ~1750, but includes two objects with decoration types closer to those of the 1800s. The comparison of the pXRF signals confirms the possibility of identifying the use of European ingredients for the production of painted enamels in the Qing dynasty. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>Cumulative number of factories established in Western countries up to 1826. In blue, the production of soft-paste; in black, the production of hard-paste (phosphatic English pastes are included in this class).</p>
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<p>Examples of pXRF spectra showing the main types of signatures (peaks marked with * arise from the instrument) of MNC 469.5.1, 2274.9, MNC 8322, MNC 22298.1, MNC 2274.38 and MNC 19032.2 artifacts. Main elements at the origin of transition peak are given. Visible images of the analyzed spot (~1 mm diameter) are shown. All XRF spectra are presented in <a href="#app1-ceramics-06-00134" class="html-app">Figure S1 (Supplementary Materials)</a>.</p>
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<p>Examples of Raman spectra (recorded from MNC 14234, MNC 8322, MNC 23181 and MNC 9638 artifacts). The color of the analyzed area is given.</p>
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<p>Ternary diagrams of the relative intensities of the signal of the elements constituting fluxes: Pb, Ca, K (<b>a</b>) and Ba-Ca-K (<b>b</b>). The inventory numbers MNCx of the objects and the area analyzed (color, mark, glaze) are indicated (see <a href="#ceramics-06-00134-t001" class="html-table">Table 1</a>).</p>
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<p>Ternary diagrams of the relative intensities for the elements Y, Rb, Sr (<b>a</b>) and Zr, Rb, Sr (<b>b</b>). The inventory numbers of the objects and the area analyzed (color, mark, glaze) are indicated (see <a href="#ceramics-06-00134-t001" class="html-table">Table 1</a>).</p>
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<p>Comparison of the relative intensities of the signal of (<b>a</b>) the elements Ag, Cu and Bi (normalized by the signal of Co), Ni, Zn and As in the blue zones (mark and decorations) and (<b>b</b>) Sn, Zn and As (Groups 1 to 3 are discussed throughout the text).</p>
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<p>Diagrams of hierarchical similarity constructed with the variables indicated for the colorless glaze (<b>a</b>), blue areas (<b>b</b>) and the marks; (<b>c</b>) Sn-Zn-As signal diagram for all areas (<b>d</b>).</p>
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<p>Diagrams of hierarchical similarity constructed with the variables indicated for the colorless glaze (<b>a</b>), blue areas (<b>b</b>) and the marks; (<b>c</b>) Sn-Zn-As signal diagram for all areas (<b>d</b>).</p>
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<p>Comparison of the relative intensity of the characteristics peak of the Cu-Au-Ag (<b>a</b>), Sn-Au-As, (<b>b</b>), Co-Au-Fe (<b>c</b>), Co-U-Mn (<b>d</b>), Co-Ni-Cr (<b>e</b>) and Co-Mn-Cr (<b>f</b>) element signal diagrams for colored areas.</p>
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<p>Comparison of the relative intensity of the characteristics peak of the Cu-Au-Ag (<b>a</b>), Sn-Au-As, (<b>b</b>), Co-Au-Fe (<b>c</b>), Co-U-Mn (<b>d</b>), Co-Ni-Cr (<b>e</b>) and Co-Mn-Cr (<b>f</b>) element signal diagrams for colored areas.</p>
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<p>Comparison of representative Raman spectra recorded on blue (blue line), green/light green (green and light-green line) and yellow (orange line) areas of MNC 2530, MNC 11205, MNC 19014, MNC 190322, MNC 14201 (<b>a</b>) and MNC 2274.38, MNC 469.5.1, MNC 11064 and MNC 11205 artifacts (violet line: light blue area); (<b>b</b>) zoom of the 0-1300 cm<sup>-1</sup> spectral range Lines are a guide for the eye.</p>
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<p>Comparison of the present data relative to Y-Rb-Sr (<b>a</b>), Zr-Rb-Sr (<b>b</b>),Pb-Ca-K (<b>c</b>) and Ba-Ca-K (<b>d</b>) signal with those previously recorded for red Böttger paste (<span class="html-italic">boccaro</span> ware, red open circle; see previous figures for the explanation of other labels) references [<a href="#B6-ceramics-06-00134" class="html-bibr">6</a>,<a href="#B7-ceramics-06-00134" class="html-bibr">7</a>].</p>
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<p>Comparison of pXRF signals relative to Y, Rb and Sr content for Meissen (<b>a</b>,<b>c</b>) and for Qing Chinese porcelain glazes from the 18th century (<b>b</b>,<b>d)</b>; collections of the museums of Paris (Musée des Arts Asiatiques-Guimet and Musée du Louvre) and Geneva (Musée de l’Ariana and Musée de la Fondation Baur) and French porcelain glazes from the end of the 17th and beginning of the 18th century (Por. Fr., Collection Cité de la Céramique, Sèvres) (<b>c</b>,<b>d</b>) according to data from references [<a href="#B26-ceramics-06-00134" class="html-bibr">26</a>,<a href="#B51-ceramics-06-00134" class="html-bibr">51</a>]. For comparison, data on blue-and-white porcelains from the earlier Yuan and Ming dynasties (including Vietnamese productions) are also indicated. Blue areas: (<b>c</b>,<b>d</b>); other colors: (<b>a</b>,<b>b</b>). (<b>d</b>) Graphical conclusion.</p>
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16 pages, 3143 KiB  
Article
Biomechanical Behavior of Lithium-Disilicate-Modified Endocrown Restorations: A Three-Dimensional Finite Element Analysis
by Fatien I. Al-naqshabandi, Bahar Jaafar Selivany and Abdulsalam Rasheed Al-zahawi
Ceramics 2023, 6(4), 2162-2177; https://doi.org/10.3390/ceramics6040133 - 11 Nov 2023
Cited by 1 | Viewed by 1942
Abstract
This study aimed to assess the biomechanical behavior of endocrown-restored mandibular molars according to “margin design” and “coverage extent” using finite element analysis (FEA). Six 3D solid models were fabricated, namely, those with complete occlusal coverage: A (butt joint), B (anatomic margin); partial [...] Read more.
This study aimed to assess the biomechanical behavior of endocrown-restored mandibular molars according to “margin design” and “coverage extent” using finite element analysis (FEA). Six 3D solid models were fabricated, namely, those with complete occlusal coverage: A (butt joint), B (anatomic margin); partial coverage (two mesial cusps): C (butt joint), D (anatomic margin); and partial coverage with mesial class II cavity: E (butt joint), F (anatomic margin). All models received lithium disilicate endocrowns (2.0 mm thickness and 4.0 mm central retainer cavity depth). A 300 N vertical load was applied to the occlusal surface, while a 250 N oblique load was applied at 45° to the lingual inclined planes of the buccal cusps. The maximum von Mises stress (VMS) distribution patterns were calculated for the endocrown, tooth structure, and cement layer. The VMS on the prepared teeth and cement layer showed subtle differences between the tested models under vertical loads. The anatomic margin (partial and complete coverage) exhibited a more homogeneous stress distribution and offered a more adhesive area of the tooth structure. Under oblique loading, the anatomic margin (complete and partial), except Model D, exhibited the lowest VMS in the cement layer. An anatomically based endocrown could be a promising alternative to the butt joint design, providing better-devised endocrown restorations, which could potentially yield a more benign stress dissipation. Full article
(This article belongs to the Special Issue Ceramic Materials in Oral Applications)
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<p>Schematic illustration of different modified endocrowns. (<b>A</b>) Complete flat butt joint. (<b>B</b>) Complete anatomic margin. (<b>C</b>) Partial flat butt joint. (<b>D</b>) Partial anatomic margin. (<b>E</b>) Partial flat butt joint with MO class II cavity. (<b>F</b>) Partial anatomic margin with MO class II cavity. The endocrown was modeled with a 2.0 mm occlusal thickness and a 4.0 mm pulp chamber extension depth.</p>
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<p>Distribution of the stresses (MPa) according to different margin design and occlusal coverage extent endocrowns under vertical load (sectioned lingual side view). (<b>A</b>) Complete flat butt joint. (<b>B</b>) Complete anatomic margin. (<b>C</b>) Partial flat butt joint. (<b>D</b>) Partial anatomic margin. (<b>E</b>) Partial flat butt joint with MO class II cavity. (<b>F</b>) Partial anatomic margin with MO class II cavity.</p>
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<p>Stress distribution in dental tissue remnants according to different margin designs and occlusal coverage extent under vertical load. (<b>A</b>) Complete flat butt joint. (<b>B</b>) Complete anatomic margin. (<b>C</b>) Partial flat butt joint. (<b>D</b>) Partial anatomic margin. (<b>E</b>) Partial flat butt joint with MO class II cavity. (<b>F</b>) Partial anatomic margin with MO class II cavity. (1) Occlusal dentinal side view. (2) Mesio-occlusal side view (enamel). (3) Lingual dentinal side view. The color scale with red to blue colors corresponds to high- to low-stress areas. The top figure shows the enamel layer orientation.</p>
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<p>Von Mises stresses (VMS) in the cement layer in six FEA models under vertical load (occlusal side view). Showing maximum VMS at the pulp chamber floor in models (<b>A</b>,<b>B</b>,<b>D</b>,<b>F</b>) and at the interface of the endocrown margin and unreduced occlusal dental surface in partial coverage butt joint margin design models (<b>C</b>,<b>E</b>).</p>
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<p>Distribution of the stresses (MPa) according to different margin designs and occlusal-coverage-extended endocrowns under oblique load (sectioned lingual side view). (<b>A</b>) Complete flat butt joint. (<b>B</b>) Complete anatomic margin. (<b>C</b>) Partial flat butt joint. (<b>D</b>) Partial anatomic margin. (<b>E</b>) Partial flat butt joint with MO class II cavity. (<b>F</b>) Partial anatomic margin with MO class II cavity.</p>
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<p>Stress distribution in dental tissue remnants according to different margin and occlusal reduction designs under oblique load. (<b>A</b>) Complete flat butt joint. (<b>B</b>) Complete anatomic margin. (<b>C</b>) Partial flat butt joint. (<b>D</b>) Partial anatomic margin. (<b>E</b>) Partial flat butt joint with MO class II cavity. (<b>F</b>) Partial anatomic margin with MO class II cavity. (1) Occlusal dentinal side view. (2) Internal side of buccal enamel side view. (3) buccal dentinal side view. The color scale with red to blue colors corresponds to high- to low-stress areas. The top figure shows the enamel layer orientation.</p>
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<p>Von Mises stresses (VMS) in the cement layer in six FEA models under oblique load (occlusal side view). Showing maximum VMS at the pulp chamber floor in complete coverage endocrown simulation models (<b>A</b>,<b>B</b>) and at the interface between the occlusal endocrown margin and the unreduced occlusal dental surface in partial coverage butt joint margin design models (<b>C</b>–<b>F</b>).</p>
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14 pages, 9585 KiB  
Article
Preparation and Characterization of Freeze-Dried β-Tricalcium Phosphate/Barium Titanate/Collagen Composite Scaffolds for Bone Tissue Engineering in Orthopedic Applications
by Dwi Fortuna Anjusa Putra, Bramantyo Bayu Aji, Henni Setia Ningsih, Ting-Wei Wu, Akihiro Nakanishi, Toshihiro Moriga and Shao-Ju Shih
Ceramics 2023, 6(4), 2148-2161; https://doi.org/10.3390/ceramics6040132 - 11 Nov 2023
Cited by 1 | Viewed by 2025
Abstract
The freeze-drying method creates a scaffold with a composite mesoporous structure with many advantages. However, everyday materials such as β-tricalcium phosphate (β-TCP) have been used as an orthopedic implant for canine tribal bone defects for decades, for instance, for grafting material of even [...] Read more.
The freeze-drying method creates a scaffold with a composite mesoporous structure with many advantages. However, everyday materials such as β-tricalcium phosphate (β-TCP) have been used as an orthopedic implant for canine tribal bone defects for decades, for instance, for grafting material of even shapes to form an implant for our teeth. However, this material is still not entirely expected to be the best implant due to its high biodegradability. Besides that, using the piezoelectric effect on the bone can lead to more efficiency in cell growth and a faster healing time for patients. Based on this phenomenon, a scaffold composite with a piezoelectric material such as barium titanate (BaTiO3/BT) has been tested. Based on the BT/β-TCP ratio, the scaffold composite of BT and β-TCP produces a porous structure with porosity ranging from 30.25 ± 11.28 to 15.25 ± 11.28 μm. The BT/β-TCP ratio influences the samples’ pore type, which affects each sample’s mechanical properties. In our result, the scaffold of 45.0 wt% BT/45.0 wt% β-TCP/10.0 wt% collagen has achieved a significant value of 0.5 MPa for maximum stress with a sufficient pore size of 25.32 ± 8.05 μm. Finally, we performed a viability test to see the sample’s piezoelectric effect, which showed that the piezoelectric effect does increase bone healing time when tested by growing MC3T3-E1 cells on the samples. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>SEM images of (<b>a</b>) commercial barium titanate and (<b>b</b>) SP-derived ꞵ-TCP particles.</p>
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<p>XRD patterns of various compositions for the BT/β-TCP/collagen composite scaffolds.</p>
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<p>SEM images of (<b>a</b>) 90.0 wt% BT/10.0 wt% collagen, (<b>b</b>) 67.5 wt% BT/22.5 wt% β-TCP/10.0 wt% collagen, (<b>c</b>) 45.0 wt% BT/45.0 wt% β-TCP/10.0 wt% collagen, (<b>d</b>) 22.5 wt% BT/67.5 wt% β-TCP/10.0 wt% collagen, and (<b>e</b>) 90.0 wt% β-TCP/10.0 wt% collagen composite scaffolds.</p>
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<p>(<b>a</b>) Stress-strain curve of various compositions of BT/β-TCP/collagen composite scaffolds under continuous load and (<b>b</b>) compressive modulus of various compositions of BT/β-TCP/collagen composite scaffolds.</p>
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<p>The porosity measurement of BT/β-TCP/collagen composite scaffolds with different wt%.</p>
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<p>(<b>a</b>) In vitro biodegradation of various compositions of BT/β-TCP/collagen composite scaffolds after soaking in SBF solution from 0 to 28 d and (<b>b</b>) weight loss after 28 days of biodegradation of all composites.</p>
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<p>Cell viability of MC3T3-E1 cells in contact with BT/β-TCP/collagen composite scaffolds by MTT assay (* <span class="html-italic">p</span> &lt; 0.05 as compared to control).</p>
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<p>Correlation between (<b>a</b>) β-TCP concentration and pore size of composite scaffolds and (<b>b</b>) porosity percentage and pore size of composite scaffolds.</p>
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<p>Correlation between weight loss and pore size of composite scaffolds.</p>
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14 pages, 3195 KiB  
Article
Ceramic Filters for the Efficient Removal of Azo Dyes and Pathogens in Water
by Marvellous Oaikhena, Abimbola E. Oluwalana-Sanusi, Puseletso P. Mokoena, Nonhlangabezo Mabuba, Themba Tshabalala and Nhamo Chaukura
Ceramics 2023, 6(4), 2134-2147; https://doi.org/10.3390/ceramics6040131 - 9 Nov 2023
Cited by 1 | Viewed by 2078
Abstract
Overcoming the scarcity of safe and sustainable drinking water, particularly in low-income countries, is one of the key challenges of the 21st century. In these countries, the cost of centralized water treatment facilities is prohibitive. This work examines the application of low-cost ceramic [...] Read more.
Overcoming the scarcity of safe and sustainable drinking water, particularly in low-income countries, is one of the key challenges of the 21st century. In these countries, the cost of centralized water treatment facilities is prohibitive. This work examines the application of low-cost ceramic filters as point-of-use (POU) devices for the removal of methylene blue, o-toluidine blue, Staphylococcus aureus, and Staphylococcus typhi from contaminated water. The ceramic filters had typical kaolinite functional groups, making them suitable for the removal of dyes and pathogens. Surface charge measurements indicated strongly anionic filters, while thermal properties confirmed the carbonization of the biowaste additive leaving behind a porous kaolinite structure which subsequently dehydroxylated into meta kaolinite. In addition, morphological data showed heterogeneous filter surfaces. Increased biomass content improved the permeability, water adsorption, flow rate, and apparent porosity of the filter. The ceramic filter removed methylene blue (42.99–59.74%), o-toluidine (79.95–92.71%), Staphylococcus aureus (98–100%), and Staphylococcus typhi (75–100%). Overall, the study demonstrated the effectiveness of POU ceramic filters in removing organic pollutants in contaminated water while serving as disinfectants. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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Graphical abstract

Graphical abstract
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<p>The fabrication process of ceramic filters.</p>
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<p>(<b>a</b>) FTIR, (<b>b</b>) XRD spectra, for clay, coffee bean residue, and ceramic filters, and (<b>c</b>) BET isotherms for CF-25, CF-30, CF-35, and CF-40.</p>
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<p>SEM images and the corresponding EDX spectra and elemental maps (inserts) for (<b>a</b>) CF-25, (<b>b</b>) CF-30, (<b>c</b>) CF-35, and (<b>d</b>) CF-40.</p>
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<p>Thermal stability of (<b>a</b>) CF-25, (<b>b</b>) CF-30, (<b>c</b>) CF-35, and (<b>d</b>) CF-40.</p>
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<p>Zeta potential variation of ceramic filters.</p>
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<p>Recyclability of ceramic filters for (<b>a</b>) <span class="html-italic">o</span>-TB and (<b>b</b>) MB.</p>
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<p>An illustration of <span class="html-italic">S. aureus</span> and <span class="html-italic">S. typhi</span> removal.</p>
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17 pages, 4520 KiB  
Review
Bioinspired Mechanical Materials—Development of High-Toughness Ceramics through Complexation of Calcium Phosphate and Organic Polymers
by Tadashi Mizutani and Yui Okuda
Ceramics 2023, 6(4), 2117-2133; https://doi.org/10.3390/ceramics6040130 - 30 Oct 2023
Cited by 2 | Viewed by 1974
Abstract
Inspired by the process of bone formation in living organisms, many studies have been conducted to develop organic–inorganic composite materials by preparing calcium phosphate crystals within solutions or dispersions of polymers with appropriate functional groups. Bones are composite materials consisting of organic polymers [...] Read more.
Inspired by the process of bone formation in living organisms, many studies have been conducted to develop organic–inorganic composite materials by preparing calcium phosphate crystals within solutions or dispersions of polymers with appropriate functional groups. Bones are composite materials consisting of organic polymers (mainly type I collagen), carbonated apatite, and water, with volume fractions of 35–45%, 35–45%, and 15–25%, respectively. Carbonated apatite in bone contributes to rigidity, while organic polymers and water contribute to toughness. The inorganic crystal, carbonated apatite, is a plate-shaped crystal with dimensions of 50 nm × 25 nm × 1–4 nm, generating a significant organic–inorganic interface, due to its nanoscale size. This interface is believed to absorb externally applied forces to dissipate mechanical energy to thermal energy. Creating such nanometer-scale structures using top-down approaches is challenging, making bottom-up methods, such as the coprecipitation of polymer and inorganic crystals, more suitable. In this account, efforts to develop eco-friendly mechanical materials using biomass, such as cellulose and starch, based on the bottom-up approach to bone-like composites are described. Full article
(This article belongs to the Special Issue Innovative Research on Calcium Phosphates Based Ceramics)
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<p>Brick-and-mortar structure of bone and polymer–HAP composites prevent fragile fracture.</p>
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<p>Comparison of bending strength, elastic modulus, and strain at failure, evaluated by three-point bending tests of tapioca starch (TS)–hydroxyapatite, phosphorylated tapioca starch (PTS)–hydroxyapatite, and TEMPO-oxidized cellulose nanofibers (TCNF)–hydroxyapatite composites containing 70 wt% of hydroxyapatite [<a href="#B88-ceramics-06-00130" class="html-bibr">88</a>,<a href="#B89-ceramics-06-00130" class="html-bibr">89</a>].</p>
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<p>Comparison of bending strength, elastic modulus, and strain at failure, evaluated by three-point bending tests of tapioca starch (TS)–hydroxyapatite, phosphorylated tapioca starch (PTS)–hydroxyapatite, and TEMPO-oxidized cellulose nanofibers (TCNF)–hydroxyapatite composites containing 70 wt% of hydroxyapatite [<a href="#B88-ceramics-06-00130" class="html-bibr">88</a>,<a href="#B89-ceramics-06-00130" class="html-bibr">89</a>].</p>
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<p>Plot of elastic moduli of phosphorylated tapioca starch (PTS)–HAP composites and tapioca starch (TS)–HAP composites against the volume fraction of HAP.</p>
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<p>Schematic representation of TEMPO-oxidized cellulose nanofibers [<a href="#B90-ceramics-06-00130" class="html-bibr">90</a>].</p>
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<p>Fracture surface of the compact of the TCNF-HAP composite, coprecipitated at 90 °C (<b>left</b>), and that of the compact of the phosphorylated starch–HAP composite, coprecipitated at 70 °C (<b>right</b>). In the three-point bending test of the TCNF-HAP compacts, the compacts only bent, so the fracture surface was produced by pulling the compact using bare hands.</p>
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<p>Schematic representation of the coprecipitation of TCNF and HAP. At an intermediate concentration of TCNF, heterogeneous nucleation of HAP on TCNF is the major pathway to produce an aligned composite. At a low concentration of TCNF, both heterogeneous and homogeneous nucleations occur to prevent the formation of the fibrous structure.</p>
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<p>Acylation of the composites of starch and hydroxyapatite.</p>
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<p>Water absorption of the compacts of PTS-HAP composites containing 66 wt% HAP, acylated with acetyl (Ac), lauroyl (Lau), and benzoyl (Bz) groups.</p>
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<p>The ratios of bending strength and elastic modulus after water immersion to those before water immersion of the acylated PTS-HAP composite compacts.</p>
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<p>Stress–strain curves of the phosphorylated starch–HAP composite containing 50 wt% of the inorganic phase and its acylated composites.</p>
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<p>Stress–strain curves of the acylated composites of phosphorylated starch–HAP after immersion in water at 25 °C for 24 h.</p>
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<p>Water absorption of the compacts of TCNF-HAP composites containing 62 wt% HAP acylated with acetyl (Ac), hexanoyl (Hex), octanoyl (Oct), lauroyl (Lau), and benzoyl (Bz) groups.</p>
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<p>The ratios of bending strength and elastic modulus after water immersion to those before water immersion of the acylated TCNF-HAP composite compacts.</p>
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<p>Schematic representation of the water resistance of the composites of hydroxyapatite and hydrophilic and hydrophobic polymers. Appropriate hydrophilic/hydrophobic balance of the polymer is necessary for the water resistance of the composite.</p>
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19 pages, 9392 KiB  
Article
Electron-Beam Processing of Aluminum-Containing Ceramics in the Forevacuum Pressure Range
by Aleksandr Klimov, Ilya Bakeev and Aleksey Zenin
Ceramics 2023, 6(4), 2098-2116; https://doi.org/10.3390/ceramics6040129 - 23 Oct 2023
Cited by 1 | Viewed by 1784
Abstract
Aluminum–ceramic materials based on Al2O3 and AlN are widely used in the electronics industry and, according to a number of electrophysical and technical and economic parameters, are among the most suitable for the production of electrical and radio engineering products. [...] Read more.
Aluminum–ceramic materials based on Al2O3 and AlN are widely used in the electronics industry and, according to a number of electrophysical and technical and economic parameters, are among the most suitable for the production of electrical and radio engineering products. In this study, it is shown that the treatment of ceramics based on Al2O3 with an electron beam with a power of 200–1100 W and a current of 10–50 mA leads to heating of the ceramic surface to a temperature of 1700 °C. When heated to a temperature of 1500 °C and kept at this temperature for no more than 10 s, an increase in the roughness of the ceramic surface is observed by more than an order of magnitude. At the same time, for ceramic substrates based on aluminum nitride, an increase in the temperature of electron beam treatment from 1300 to 1700 °C leads to an increase in thermal conductivity from 1.5 to 2 times. The edge angle of water wetting of the AlN surface can vary from 20 to 100 degrees depending on the processing temperature, which allows one to control the transition of the material from a hydrophilic to a hydrophobic state. At the same time, electron beam exposure to Al2O3 does not change the wettability of this material so much. Electron beam processing in the forevacuum pressure region allows controlled changes in the electrophysical properties of ceramic materials based on Al2O3 and AlN. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>SEM surface images of original substrates: (<b>a</b>) Policor (Al<sub>2</sub>O<sub>3</sub>), (<b>b</b>) INC-AN180 (AlN).</p>
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<p>Schematic diagram of the experimental setup: 1—plasma-cathode electron source; 2—vacuum chamber; 3—beam deflection system; 4—electron beam; 5—beam-plasma; 6—sintered sample; 7—computer; 8—pyrometer.</p>
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<p>Thermal regime of electron-beam irradiation of samples. The holding temperature was 1700 °C.</p>
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<p>Dependence of sample temperature on electron beam power for different ceramics and holding temperatures: 1, 3—Al<sub>2</sub>O<sub>3</sub>; 2, 4—AlN.</p>
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<p>Surface of aluminum oxide ceramic samples processed at different holding temperatures: (<b>a</b>) 1300 °C, (<b>b</b>) 1500 °C, (<b>c</b>) 1600 °C, (<b>d</b>) 1700 °C.</p>
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<p>Roughness of Al<sub>2</sub>O<sub>3</sub> ceramics: (<b>a</b>) original sample; (<b>b</b>) irradiated at 1300 °C; (<b>c</b>) irradiated at 1500 °C.</p>
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<p>Surface of AlN samples processed at different temperatures: (<b>a</b>) original, (<b>b</b>) 1300 °C, (<b>c</b>) 1400 °C, (<b>d</b>) 1500 °C, (<b>e</b>) 1600 °C, (<b>f</b>) 1700 °C. The gray elements in the images are AlN grains. The bright areas are supposedly yttrium aluminate.</p>
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<p>Formation of an aluminum–yttrium structure on the AlN surface processed at temperatures of 1500 °C (<b>a</b>) and 1700 °C (<b>b</b>).</p>
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<p>Histogram of elemental composition over the irradiated AlN surface. The isothermal holding temperature is 1700 °C.</p>
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<p>X-ray diffraction patterns of AlN + Y<sub>2</sub>O<sub>3</sub> samples; original, and at temperatures of 1600 °C and 1700 °C.</p>
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<p>Dependence of AlN hardness measured by the Vickers method on processing temperature.</p>
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<p>Dependence of thermal conductivity on processing temperature. The temperature at which the measurements were carried out: 1—50 °C, 2—500 °C.</p>
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<p>Photographs of water droplets on the surface of Al<sub>2</sub>O<sub>3</sub> substrates: (<b>a</b>) original sample; (<b>b</b>) after processing at a temperature of 1600 °C; (<b>c</b>) after processing at a temperature of 1700 °C.</p>
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<p>Photographs of water droplets on the surface of AlN substrates: (<b>a</b>) original sample; (<b>b</b>) after processing at a temperature of 1600 °C; (<b>c</b>) after processing at a temperature of 1700 °C.</p>
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<p>Contact angles of Al<sub>2</sub>O<sub>3</sub> and AlN surfaces. A temperature of 1200 °C corresponds to non-irradiated material.</p>
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12 pages, 3695 KiB  
Article
One-Step Microwave Synthesis of New Hybrid Phosphor (CSSC) for White Light-Emitting Diodes
by Maxim Sychov, Mariia Keskinova, Andrey Dolgin, Igor Turkin, Kazuhiko Hara and Hiroko Kominami
Ceramics 2023, 6(4), 2086-2097; https://doi.org/10.3390/ceramics6040128 - 19 Oct 2023
Viewed by 1478
Abstract
The possibility of synthesizing a new hybrid phosphor CSSC (mixture of 0.5 CaSrSiO4:Eu2+: 0.29 Ca6Sr4Si6O21Cl2:Eu2+: 0.21 Ca10Si6O21Cl2:Eu2+) [...] Read more.
The possibility of synthesizing a new hybrid phosphor CSSC (mixture of 0.5 CaSrSiO4:Eu2+: 0.29 Ca6Sr4Si6O21Cl2:Eu2+: 0.21 Ca10Si6O21Cl2:Eu2+) using a one-step microwave synthesis method is demonstrated. The concentrations of europium and calcium in the synthesized phosphors were optimized at 1 and 10 mol. %, respectively, to achieve maximum brightness and color rendering index. The optimal conditions for the synthesis of phosphors in a microwave furnace were determined as 750 °C for 10 min. The resulting phosphor exhibited a wide luminescence spectrum that covered the entire visible region, resulting in a high color rendering index and a warm white luminescence when used as a light source. It is shown that the sol–gel method for preparing the charge mixture for the new phosphor allows for a 35% higher luminescence brightness compared to the solid-phase method, due to a more uniform distribution of the activator. Full article
(This article belongs to the Special Issue Composite Nanopowders: Synthesis and Applications)
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<p>Emission spectra of CaSrSiO<sub>4</sub>:Eu<sup>2+</sup> (green), Ca<sub>6</sub>Sr<sub>4</sub>Si<sub>6</sub>O<sub>21</sub>Cl<sub>2</sub>:Eu<sup>2+</sup> (yellow), and Ca<sub>10</sub>Si<sub>6</sub>O<sub>21</sub>Cl<sub>2</sub>:Eu<sup>2+</sup> (blue) phosphors.</p>
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<p>The custom-made microwave furnace: 1—power supply unit and magnetron, 2—reaction chamber, 3—sensor of supplied microwave energy, 4—sensor of reflected microwave energy, 5—circulator, 6—load, 7—optical radiometer. Arrows—the direction of movement of electromagnetic waves.</p>
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<p>Model of the reaction chamber: 1—diaphragm, 2—movable wall, 3—antinodes of the electric field energy.</p>
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<p>Designs of thermostats for synthesis of phosphors in microwave furnace: (<b>a</b>)—oxidizing atmosphere, with a susceptor; (<b>b</b>,<b>d</b>)—reducing atmosphere, soot in the charge, without susceptor; (<b>c</b>)—reducing atmosphere, soot above and below the charge, without susceptor; (<b>e</b>)—reducing atmosphere, soot in the charge, with a susceptor; (<b>f</b>)—reducing atmosphere, soot above and below the charge, with a susceptor.</p>
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<p>Brightness of samples in reference units (y.e.) synthesized in different facilities.</p>
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<p>Photoluminescence spectra of hybrid phosphor (CaSrSiO<sub>4</sub>:Eu<sup>2+</sup>, Ca<sub>6</sub>Sr<sub>4</sub>Si<sub>6</sub>O<sub>21</sub>Cl<sub>2</sub>:Eu<sup>2+</sup>, Ca<sub>10</sub>Si<sub>6</sub>O<sub>21</sub>Cl<sub>2</sub>:Eu<sup>2+</sup>) synthesized in microwave and muffle furnaces. Unmarked curves are components of the photoluminescence spectrum bands of the developed phosphors (presented in <a href="#ceramics-06-00128-t001" class="html-table">Table 1</a>).</p>
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<p>Luminescence of samples synthesized in muffle and microwave ovens in color coordinates.</p>
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<p>Electron microphotographs of the samples.</p>
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<p>The brightness of the samples was influenced by two factors: (<b>a</b>) the duration of synthesis at a temperature of 700 °C and (<b>b</b>) the temperature of synthesis.</p>
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<p>Photoluminescence spectra of synthesized samples with different concentrations of Ca<sup>2+</sup>.</p>
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<p>Brightness hybrid phosphor (0.5 CaSrSiO<sub>4</sub>:Eu<sup>2+</sup>, 0.29 Ca<sub>6</sub>Sr<sub>4</sub>Si<sub>6</sub>O<sub>21</sub>Cl<sub>2</sub>:Eu<sup>2+</sup>, 0.21 Ca<sub>10</sub>Si<sub>6</sub>O<sub>21</sub>Cl<sub>2</sub>:Eu<sup>2+</sup>) at different concentrations of europium.</p>
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<p>Dependence of the brightness of cathodoluminescence on anode voltage.</p>
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<p>Photoluminescence spectra of sunlight, WLED based on YAG:Ce, and mixed phosphor.</p>
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16 pages, 2462 KiB  
Article
The Effect of the Addition of Aluminum Nitride to the Composition of NiAl2O4 Ceramics on Hydrogenation Processes and the Increase in Resistance to Swelling and Degradation
by Artem L. Kozlovskiy
Ceramics 2023, 6(4), 2070-2085; https://doi.org/10.3390/ceramics6040127 - 19 Oct 2023
Cited by 1 | Viewed by 1563
Abstract
This work examines the effects of the formation of impurity inclusions in the structure of NiAl2O4 ceramics when aluminum nitride is added to them and the occurrence of a reinforcement effect that prevents hydrogenation processes and the subsequent destruction of [...] Read more.
This work examines the effects of the formation of impurity inclusions in the structure of NiAl2O4 ceramics when aluminum nitride is added to them and the occurrence of a reinforcement effect that prevents hydrogenation processes and the subsequent destruction of conductive and thermophysical characteristics. The appeal of ceramics possessing a spinel crystal structure lies in their potential use as ceramic fuel cells for both hydrogen generation and storage. Simultaneously, addressing the challenges related to ceramic degradation during hydrogenation, a critical aspect of hydrogen production, can enhance the efficiency of these ceramics while lowering electricity production costs. The selection of aluminum nitride as an additive for ceramic modification is based on its remarkable resistance to structural damage accumulation, its potential to enhance resistance to high-temperature degradation, and its ability to bolster strength properties. Moreover, an examination of the alterations in the strength characteristics of the examined samples subjected to hydrogenation reveals that the stability of two-phase ceramics is enhanced by more than three to five times compared to the initial ceramics (those without the addition of AlN). Additionally, it was noted that the most significant alterations in both structure and strength become apparent at irradiation fluences exceeding 1014 proton/cm2, where atomic displacements in the damaged ceramic layer reach over 5 dpa. During the evaluation of thermophysical properties, it was discerned that ceramics featuring an impurity phase in their composition exhibit the highest stability. These ceramics demonstrated a reduction in the thermal conductivity coefficient of less than 1% at the peak irradiation fluence. Full article
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<p>(<b>a</b>) Graph of the change in the value of ionization losses of incident protons along the trajectory of motion in the near-surface layer; (<b>b</b>) dependence of plotting the value of atomic displacements along the trajectory of proton motion in the near-surface layer of ceramics.</p>
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<p>The results of X-ray diffraction of the studied ceramic samples depending on the variation in AlN concentration upon its addition (red dotted lines indicate the formation of inclusions in the form of the Al<sub>7</sub>O<sub>3</sub>N<sub>8</sub> orthorhombic phase).</p>
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<p>The results of morphological features of synthesized ceramics depending on alterations in AlN concentration in the composition: (<b>a</b>) pristine; (<b>b</b>) 0.01 M; (<b>c</b>) 0.03 M; (<b>d</b>) 0.05 M; (<b>e</b>) 0.10 M; (<b>f</b>) 0.15 M.</p>
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<p>The results of morphological features of synthesized ceramics depending on alterations in AlN concentration in the composition: (<b>a</b>) pristine; (<b>b</b>) 0.01 M; (<b>c</b>) 0.03 M; (<b>d</b>) 0.05 M; (<b>e</b>) 0.10 M; (<b>f</b>) 0.15 M.</p>
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<p>The results of changes in the structural parameters of ceramics subject to hydrogenation: (<b>a</b>) the assessment results of the change in the crystal lattice volume depending on the value of atomic displacements; (<b>b</b>) the results of alterations in the value of the structural ordering factor depending on the value of atomic displacements.</p>
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<p>The dependence of changes in structural parameters at maximum irradiation fluence in the case of variation in AlN concentration in the composition of ceramics.</p>
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<p>The results of changes in strength characteristics: (<b>a</b>) change in hardness depending on irradiation fluence (value of atomic displacements); (<b>b</b>) change in the maximum pressure that ceramics can withstand during a single compression.</p>
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<p>The results of changes in strength characteristics: (<b>a</b>) decrease in hardness (softening); (<b>b</b>) reduction in crack resistance.</p>
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<p>The results of changes in the thermal conductivity coefficient of ceramics depending on the value of atomic displacements.</p>
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17 pages, 3884 KiB  
Article
Size-Independent Flexure Test Technique for the Mechanical Properties of Geocomposites Reinforced by Unidirectional Fibers
by Hung Tran Doan, Dora Kroisova and Oleg Bortnovsky
Ceramics 2023, 6(4), 2053-2069; https://doi.org/10.3390/ceramics6040126 - 17 Oct 2023
Viewed by 1388
Abstract
In assessing the bending attributes for geopolymer composites augmented with uni-directional fibers, methodologies aligned with the established American and European standards yield quantifiable values for flexural strength, denoted as σm*, and its corresponding elasticity modulus, E*. Notably, these values exhibit [...] Read more.
In assessing the bending attributes for geopolymer composites augmented with uni-directional fibers, methodologies aligned with the established American and European standards yield quantifiable values for flexural strength, denoted as σm*, and its corresponding elasticity modulus, E*. Notably, these values exhibit a pronounced dependency on the size of the testing parameters. Specifically, within a judicious range of support span L relative to specimen height H, spanning a ratio of 10 to 40, these metrics can vary by a factor between 2 and 4. By conducting evaluations across an extensive array of H/L ratios and adhering to the protocols set for comparable composites with a plastic matrix, it becomes feasible to determine the definitive flexural elastic modulus E and shear modulus G, both of which can be viewed as size-neutral material traits. A parallel methodology can be employed to deduce size-agnostic values for flexural strength, σm. The established linear relationship between the inverse practical value E* (1/E*) and the squared ratio (H/L)2 is acknowledged. However, a congruent 1/σm* relationship has been recently corroborated experimentally, aligning primarily with Tarnopolsky’s theoretical propositions. The parameter T, defined as the inverse gradient of 1/σm* about (H/L)2, is integral to these findings. Furthermore, the significance of the loading displacement rate is underscored, necessitating a tailored consideration for different scenarios. Full article
(This article belongs to the Special Issue The Production Processes and Applications of Geopolymers)
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<p>Ratio of the effective value <span class="html-italic">E</span> to the virtual value <span class="html-italic">E</span>*; ratios of <span class="html-italic">E</span>*/<span class="html-italic">G</span> in the legend.</p>
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<p>Theoretical size dependences of <math display="inline"><semantics> <mrow> <mrow> <mrow> <msub> <mrow> <mi>σ</mi> </mrow> <mrow> <mi>m</mi> </mrow> </msub> </mrow> <mo>/</mo> <mrow> <msubsup> <mrow> <mi>σ</mi> </mrow> <mrow> <mi>m</mi> </mrow> <mrow> <mo>*</mo> </mrow> </msubsup> </mrow> </mrow> </mrow> </semantics></math> ratios at different <span class="html-italic">E/G</span> (in the legend).</p>
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<p>Reciprocal effective elasticity modulus vs. <span class="html-italic">(H/L)</span><sup>2</sup> ratio.</p>
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<p>Reciprocal effective flexural strength vs. <span class="html-italic">(H/L)</span><sup>2</sup> ratio.</p>
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<p>Reciprocal effective flexural properties ((<b>a</b>,<b>c</b>,<b>e</b>) for flexural modulus and (<b>b</b>,<b>d</b>,<b>f</b>) for flexural strength) of composites carbon HTS 5631 1600tex 24k-M1 matrix at different temperatures of curing in legends.</p>
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<p>Correlation of flexural modulus for geopolymer M2-basalt; rate of deformation in mm/min in the legend.</p>
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<p>Correlation of flexural strength for geopolymer M2-basalt; rate of deformation in mm/min in the legend.</p>
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<p>Comparison of <span class="html-italic">E</span> in carbon-woven (twill) and unidirectional fabrics, last numbers in the legend: days of cooled matrix storage.</p>
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<p>Comparison of <span class="html-italic">σ<sub>m</sub></span> in carbon-woven (twill) and unidirectional fabrics, last numbers in the legend: days of cooled matrix storage.</p>
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<p>Comparison of <span class="html-italic">E</span> in E-glass-woven (twill) and unidirectional fabrics, last numbers in the legend: days of cooled matrix storage.</p>
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<p>Comparison of <span class="html-italic">σ<sub>m</sub></span> in E-glass-woven (twill) and unidirectional fabrics, last numbers in the legend: days of cooled matrix storage.</p>
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17 pages, 6325 KiB  
Article
The Feature Resolution and Dimensional Control in Freeform Solidification of Alumina Systems by Stereolithography
by Mustafa K. Alazzawi, Chawon Hwang, Victoria R. Tsarkova and Richard A. Haber
Ceramics 2023, 6(4), 2036-2052; https://doi.org/10.3390/ceramics6040125 - 17 Oct 2023
Cited by 1 | Viewed by 1485
Abstract
Controlling the feature resolution and dimension of printed products using stereolithography requires a comprehensive understanding of compositional and printing variables. Balancing these variables adds more complexity to manufacturing near net shape products. In this study, the compositional variables examined include particle size and [...] Read more.
Controlling the feature resolution and dimension of printed products using stereolithography requires a comprehensive understanding of compositional and printing variables. Balancing these variables adds more complexity to manufacturing near net shape products. In this study, the compositional variables examined include particle size and solid content using two resins, and printing variables include layer thickness and energy dose. Choosing the energy dose for curing depends on compositional variables and consequently affects the degree of scattering. The results shows that light scattering determines the changes in the feature resolution and lateral dimensions. The layer thickness only affects the feature resolution and not the lateral dimensions. The vertical dimension does not significantly change with the chosen variables. In this study, fine-tuning the variables is shown to produce parts with high precision and resolution. Both compositional and printing variables play a key role in achieving near net shape products. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>Schematic of the tape casting-based printer, Admaflex 130. The printer uses a digital light processing system for curing and a doctor blade for spreading the materials. The z coordinate is the building direction, and the x and y coordinates are the casting substrate.</p>
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<p>(<b>a</b>) The viscosity and (<b>b</b>) shear stress of suspensions measured within a shear rate of (0.1–300.0) s<sup>−1</sup> at 25.0 °C.</p>
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<p>Analyzed images of the automated FOG gauge surface of the suspensions. (<b>a</b>) Suspensions composed of Resin1 and AA07 powder with different solid contents. (<b>b</b>) Suspension composed of Resin2 and AA07 powder. (<b>c</b>) Suspension composed of Resin2 and AA3 powder. The solid content is indicated underneath the images. AA07 powder was finer than AA3 powder.</p>
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<p>Cure depth (Cd) as a function of energy dose. (<b>a</b>) Three suspensions with a solid content of 75.0 %wt.; one suspension consisted of Resin1 with fine powder, and two others consisted of Resin2 with fine and coarse powders. (<b>b</b>) The suspensions consisted of Resin1 with fine powder, and the solid content varied (75.0–82.0 %wt).</p>
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<p>Cure width changes in lateral dimensions (x and y) as a function of energy dose. (<b>a</b>) Three suspensions with a solid content of 75.0 %wt.; one suspension consisted of Resin1 with fine powder, and two others consisted of Resin2 with fine and coarse powders. (<b>b</b>) The suspensions consisted of Resin1 with fine powder, and the solid content varied (75.0–82.0 %wt).</p>
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<p>Optical microscope images of as-printed ceramics perpendicular to the printing direction (z axis). The effects of layer thickness and energy dose on feature resolution and flaws are shown using samples with two different particle sizes. They contained a solid content of 75.0 %wt. The samples with fine alumina, AA07, were printed under the conditions of (<b>a</b>) low energy dose and 50.0 µm layer thickness, (<b>b</b>) high energy dose and 50.0 µm layer thickness, and (<b>c</b>) low energy dose and 20.0 µm layer thickness. The samples with coarse alumina, AA3, were printed under the conditions of (<b>d</b>) low energy dose and 50.0 µm layer thickness, (<b>e</b>) high energy dose and 50.0 µm layer thickness, and (<b>f</b>) low energy dose and 20.0 µm layer thickness.</p>
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<p>Optical microscope images of as-printed ceramics perpendicular to the printing direction (z axis). The effects of the solid content on feature resolution and flaws are shown using samples composed of AA07 and Resin1. The solid content was (<b>a</b>) 75.0 %wt. and (<b>b</b>) 82.0 %wt. They were printed using a low energy dose and 20.0 µm layer thickness.</p>
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<p>Scanning electron microscope images show the effect of layer thickness and energy dose using samples with two different particle sizes. They contained a solid content of 75.0 %wt. The as-printed samples with fine alumina, AA07, were printed under the conditions of (<b>a</b>) low energy dose and 50.0 µm layer thickness, (<b>b</b>) high energy dose and 50.0 µm layer thickness, and (<b>c</b>) low energy dose and 20.0 µm layer thickness. The as-debound samples with coarse alumina, AA3, were printed under the conditions of (<b>d</b>) low energy dose and 50.0 µm layer thickness as well as (<b>e</b>) high energy dose and 50.0 µm layer thickness. (<b>f</b>) Schematic shows how the stair-wise pattern is formed.</p>
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<p>Scanning electron microscope images show the effect of solid content using as-printed samples composed of AA07 and Resin1. The solid content was (<b>a</b>) 75.0 %wt. and (<b>b</b>) 82.0 %wt. They were printed using low energy dose and 20.0 µm layer thickness.</p>
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<p>The dimensional changes of as printed samples as a function of (<b>a</b>) energy dose and (<b>b</b>) layer thickness. Three samples with a solid content of 75.0 %wt., one sample consisted of Resin1 with fine powder, and two others consisted of Resin2 with fine and coarse powders.</p>
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<p>The dimensional changes of as printed samples as a function of solid content. The samples composed of AA07 and Resin1. They were printed using 20.0 µm layer thickness and a low energy dose.</p>
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<p>The changes in layer thickness across the prints and their microstructure images. Images were taken at three locations which were near the base, middle layers, and last layers. The layers near the base were printed first. The samples and print conditions varied. (<b>a</b>) Sample (Resin1 and 75.0 %wt. AA07 powder) was printed using 20.0 µm layer thickness and low energy dose conditions. (<b>b</b>) Sample (Resin2 and 75.0 %wt. AA07 powder) was printed using 20.0 µm layer thickness and low energy dose conditions. (<b>c</b>) Sample (Resin2 and 75.0 %wt. AA07 powder) was printed using 50.0 µm layer thickness and low energy dose conditions.</p>
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<p>Sintered samples composed of Resin1 and (<b>a</b>) 75.0 %wt. and (<b>b</b>) 82.0 %wt. AA07 powder. (<b>c</b>) Sintered sample composed of Resin2 and 75.0 %wt. AA07 powder. They were printed using 20.0 µm layer thickness and low energy dose conditions.</p>
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<p>The dimensional changes of sintered samples as a function of solid content using two resins.</p>
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18 pages, 11760 KiB  
Article
Dynamic Extrusion Control in Spot Deposition Modeling for Porous 3D Clay Structures
by Vesela Tabakova, Christina Klug and Thomas H. Schmitz
Ceramics 2023, 6(4), 2018-2035; https://doi.org/10.3390/ceramics6040124 - 6 Oct 2023
Viewed by 2027
Abstract
The dynamic state of the viscous clay in Liquid Deposition Modeling (LDM) often leads to discrepancies between the digital model and the resulting physical object. This emergent behavior can be harnessed to produce complex physical structures that would not be possible with other [...] Read more.
The dynamic state of the viscous clay in Liquid Deposition Modeling (LDM) often leads to discrepancies between the digital model and the resulting physical object. This emergent behavior can be harnessed to produce complex physical structures that would not be possible with other methods. This study takes advantage of the viscous state and tensile strength of the extruded clay strand to explore the impact of dynamic extrusion and deformations through travel paths in LDM to manufacture complex porous physical structures. The effects of these parameters are discussed in two case studies: (1) regular and semi-random Spot Deposition surfaces with either open or thickened regions, and (2) porous 3D lattice structures created through the controlled bending of vertical extrusions. The achieved higher geometrical complexity of objects through the algorithmically programmed alternations in the sequence and rate of material deposition allows for a wide range of buildup approaches that expand the production spectrum of sustainable small- and large-scale elements. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>Water content (wt.%) of the clay paste compared to the wet and dry sample weights.</p>
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<p>Scheme of the used Delta 3D Printer Actuator.</p>
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<p>Layered SD: (<b>a</b>) Isometric model; (<b>b</b>) Frontal elevation; (<b>c</b>) Geometric goal points and alternating tool-path direction.</p>
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<p>Semi-random SD: (<b>a</b>) Isometric model; (<b>b</b>) Frontal elevation; (<b>c</b>) Geometric goal points and tool-path direction.</p>
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<p>(<b>a</b>) Vertical SD scheme; (<b>b</b>) Deflection scheme; (<b>c</b>) Vertical SDs with constant extrusion; (<b>d</b>) Tapered vSDs with additional deformation though travel paths.</p>
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<p>Print success of vSD of different heights with decreasing extrusion: (<b>a</b>) Extrusion factor (f<sub>base</sub>) as % of h<sub>VSD</sub>; (<b>b</b>) Segment height (s).</p>
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<p>Horizontal SD: (<b>a</b>) layered SD scheme; (<b>b</b>) h<sub>L</sub> = 2 mm, d = 4 mm; (<b>c</b>) h<sub>L</sub> = 2 mm, d = 7.5 mm; (<b>d</b>) h<sub>L</sub> = 4 mm, d = 7.5 mm.</p>
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<p>Semi-random SD: (<b>a</b>) semi-random SD scheme; (<b>b</b>) Curved surface produced through semi-random SDs; (<b>c</b>) Surface close-up.</p>
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<p>Porous surfaces created through the modification of extrusion factors: (<b>a</b>) source image; (<b>b</b>) horizontal SD; (<b>c</b>) semi-random SD; (<b>d</b>) continuous deposition.</p>
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<p>Surfaces with over-extrusion: (<b>a</b>) semi-random SD; (<b>b</b>) continuous deposition; (<b>c</b>) continuous deposition.</p>
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<p>Vertical SD and deflection: (<b>a</b>) Curved surface produced through vSDs; (<b>b</b>) Surface close-up.</p>
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<p>Maximum bent height at the base of vSD for: (<b>a</b>) Bending scheme; (<b>b</b>) Bending angle; (<b>c</b>) Segment height.</p>
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<p>Interlocking patterns: (<b>a</b>) Horizontal interlocking; (<b>b</b>) Vertical interlocking; (<b>c</b>) Collage horizontal interlocking; (<b>d</b>) Collage vertical interlocking.</p>
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<p>Closed one-shelled lattice structures: (<b>a</b>,<b>d</b>) Horizontal interlocking with same direction of rotation; (<b>b</b>,<b>e</b>) Horizontal interlocking with alternating direction of rotation of the strand pairs; (<b>c</b>,<b>f</b>) Vertical interlocking.</p>
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<p>Isometric scheme of the parameters for horizontal interlocking: (<b>a</b>) vSD; (<b>b</b>) bending of vSD; (<b>c</b>) second vSD with horizontal interlocking; (<b>d</b>) second layer of vSD; (<b>e</b>) alternated bending direction of second-layer vSDs.</p>
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<p>Physical geometry of the single-plane horizontal interlocking produced with the parameters from <a href="#ceramics-06-00124-t004" class="html-table">Table 4</a>.</p>
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<p>Two-shelled linear lattice structure with horizontal overlapping: (<b>a</b>) Digital model; (<b>b</b>) Front view; (<b>c</b>) Diagonal view.</p>
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<p>Two-shelled linear lattice structure with vertical overlapping: (<b>a</b>) Digital model; (<b>b</b>) Front view; (<b>c</b>) Diagonal view.</p>
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<p>Two-shelled curved lattice structure with horizontal overlapping: (<b>a</b>) Front view; (<b>b</b>) Diagonal view.</p>
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10 pages, 2624 KiB  
Article
Chemical Compositions of Chinese Glazed Tiles from an Imperial Mausoleum of the Liao Dynasty
by Lan Zhao, Xiongfei Wan, Baoqiang Kang and He Li
Ceramics 2023, 6(4), 2008-2017; https://doi.org/10.3390/ceramics6040123 - 5 Oct 2023
Viewed by 1782
Abstract
Glazed tiles are characteristic architectural ceramics traditionally used in ancient Chinese royal buildings. Studies on their chemical compositions have provided valuable information regarding their compositional classifications and the provenances of their raw materials. Existing studies have mainly focused on the Yuan dynasty (1271–1368 [...] Read more.
Glazed tiles are characteristic architectural ceramics traditionally used in ancient Chinese royal buildings. Studies on their chemical compositions have provided valuable information regarding their compositional classifications and the provenances of their raw materials. Existing studies have mainly focused on the Yuan dynasty (1271–1368 AD) or later. Research on earlier ages is limited because of a lack of samples. In this study, we used an energy-dispersive X-ray fluorescence spectrometer to analyze the chemical compositions of 18 glazed tiles unearthed from an imperial mausoleum (the Xinli site) from the Liao dynasty (969–982 AD). The glazes of the tiles had a SiO2–Al2O3–PbO ternary oxidic system and the bodies of the tiles had a SiO2–Al2O3 binary oxidic system. Certain compositional differences were observed among the samples with different types of decorations. Compared with samples from the Yuan dynasty and later periods, the Xinli samples had higher SiO2 and Al2O3 contents and lower PbO and CuO contents in the tile glazes. The tile bodies of the Xinli samples had compositions similar to those of tile bodies from the Qing dynasty (1616–1912 AD). We speculated that the Xinli samples with different decorations came from different kiln sites. Full article
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<p>Photographs of the samples representing different types of glazed-tile decorations in this study: (<b>A</b>) example of type-A animal-face decoration; (<b>B</b>) example of type-B animal-face decoration; (<b>C</b>) example of type-C animal-face decoration; (<b>D</b>) sample with lotus-flower decoration.</p>
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<p>Plots of chemical compositions of the tile glazes from the Xinli site with different types of animal-face decorations. Dashed lines represent the corresponding element contents of the lotus-flower-decorated sample from the Xinli site.</p>
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<p>Plots of chemical compositions of the body samples from the Xinli site with different types of animal-face decorations. Dashed lines represent the corresponding element contents of the lotus-flower-decorated sample from the Xinli site.</p>
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<p>Comparison of chemical compositions of the tile glazes from different time periods. XL: Xinli site; YSD: Yuanshangdu site; MZD: Mingzhongdu site; FC: Forbidden City. (<b>A</b>) Contents of SiO<sub>2</sub>; (<b>B</b>) contents of PbO; (<b>C</b>) contents of Al<sub>2</sub>O<sub>3</sub>; (<b>D</b>) contents of CuO.</p>
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<p>Scatterplots of the SiO<sub>2</sub> and Al<sub>2</sub>O<sub>3</sub> contents of tile bodies from different time periods. Each dot represents a tile-body sample. XL: Xinli; YSD: Yuanshangdu; MZD: Mingzhongdu; FC: Forbidden City.</p>
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<p>Scatterplots of the SrO and Rb<sub>2</sub>O contents of the tile bodies from different kiln sites of the Liao dynasty. Each dot represents a tile-body sample.</p>
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17 pages, 5190 KiB  
Article
Frequency Characteristics of High Strain Rate Compressions of Cf-MWCNTs/SiC Composites
by Kun Luan, Chen Ming, Xiaomeng Fang and Jianjun Liu
Ceramics 2023, 6(4), 1991-2007; https://doi.org/10.3390/ceramics6040122 - 5 Oct 2023
Cited by 1 | Viewed by 1638
Abstract
The incorporation of ductile reinforcements into ceramics helps restrain crack deflection, which can enhance ceramics’ toughness and overcome the matrix’s brittleness. In this paper, we produced a ceramic composite reinforced by carbon fibers coated by multi-wall carbon nanotubes (shortened by Cf-MWCNT/SiC [...] Read more.
The incorporation of ductile reinforcements into ceramics helps restrain crack deflection, which can enhance ceramics’ toughness and overcome the matrix’s brittleness. In this paper, we produced a ceramic composite reinforced by carbon fibers coated by multi-wall carbon nanotubes (shortened by Cf-MWCNT/SiC composites) for enhanced impact resistance at a high strain rate that commonly occurs in composite materials used in astronautics, marine, and other engineering fields. The fabrication process involves growing multi-wall carbon nanotubes (MWCNTs) on a carbon fiber woven fabric (Cf) to create the fibril/fabric hybrid reinforcement. It is then impregnated by polymer solution (precursor of the ceramics), forming composites after the pyrolysis process, known as the liquid polymer infiltration and pyrolysis (PIP) technique. To assess the impact resistance of the Cf-MWCNT/SiC under high-strain rate compressions, the split Hopkinson pressure bar (SHPB) technique is employed. Since the failure behavior of the Cf-MWCNT/SiC composites in the absence of the ductile phase is not well understood, the study employs the Hilbert–Huang transform (HHT) to analyze the stress–time curves obtained from the SHPB experiments. By applying the HHT, we obtained the frequency–time spectrum and the marginal Hilbert spectrum of the stress signals. These analyses reveal the frequency characteristics of the Cf-MWCNT/SiC composite and provide insights into the relationship between transformed signal frequency and fracture behavior. By understanding the dynamic fracture behavior and frequency response of the Cf-MWCNT/SiC, it becomes possible to enhance its impact resistance and tailor its performance for specific protective requirements. Therefore, the findings of this study can guide the future design and optimization of Cf-MWCNT/SiC structures for various protective applications, such as body armor, civil structures, and protections for vehicles and aircraft. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>The structure and preparation of the C<sub>f</sub>-MWCNT/SiC composites: (<b>a</b>) Woven fabric made of carbon yarns; (<b>b</b>) Pyrolytic SiC layer coated on the fabric; (<b>c</b>) Synthesizing MWCNTs on fabric surface; (<b>d</b>) Impregnate fabrics with phenolic resin; (<b>e</b>) PIP treatment; (<b>f</b>) SEM image of Cf-MWCNT/SiC composites at a micro-scale.</p>
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<p>Schematic illustration of strength and fracture behavior in terms of intrinsic (brown color text) versus extrinsic (black color text) toughening mechanisms.</p>
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<p>Schematic illustration of the SHPB working principle.</p>
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<p>Typical input and output wave signals of C<sub>f</sub>-MWCNT/SiC composites tested at the strain rate of 1500 s<sup>−1</sup> in the out-of-plane direction.</p>
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<p>Process of Hilbert–Huang transform <sup>†</sup>: (<b>a</b>) Original stress/voltage–time signal collected by the SHPB; (<b>b</b>) The ensemble empirical mode decomposition: breaking down the original signal with an envelope (brown dot lines) for obtaining a mean value (blue dot line) which stands for the intrinsic mode function at a certain frequency level; (<b>c</b>) IMFs (intrinsic mode functions); (<b>d</b>) Frequency–time spectrum; (<b>e</b>) Marginal spectrum integrated from Hilbert spectrum that shows frequency distribution of fracture modes. <sup>†</sup> Note: the curves in (<b>a</b>–<b>c</b>) are not real experimental data, which are only examples illustrating the procedure of data processing. Please find the experimental data in <a href="#sec3dot2-ceramics-06-00122" class="html-sec">Section 3.2</a>.</p>
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<p>Stress–strain curves of C<sub>f</sub>-MWCNT/SiC composites tested at different impact strain rates in (<b>a</b>) in-plane direction; and (<b>b</b>) out-of-plane direction [<a href="#B19-ceramics-06-00122" class="html-bibr">19</a>].</p>
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<p>IMFs of the C<sub>f</sub>-MWCNT/SiC composites tested at different impact strain rates: (<b>a</b>–<b>e</b>) results in in-plane direction; (<b>f</b>–<b>j</b>) results in out-of-plane direction. The strain rate is labeled at the right bottom of each sub-figure.</p>
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<p>Frequency–time spectrum of the C<sub>f</sub>-MWCNT/SiC composites tested at different impact strain rates in (<b>a</b>–<b>e</b>) in-plane direction, and (<b>f</b>–<b>j</b>) out-of-plane direction.</p>
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<p>Marginal Hilbert spectrum of C<sub>f</sub>-MWCNT/SiC composites tested in (<b>a</b>–<b>e</b>) in-plane direction, and (<b>b</b>–<b>j</b>) out-of-plane direction.</p>
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<p>Fracture morphology and mapped marginal Hilbert spectrum. (<b>a</b>) SEM image of fracture in sample tested at 1200 s<sup>−1</sup> in an in-plane direction; (<b>b</b>) SEM image of fracture in the sample tested at 1500 s<sup>−1</sup> in an out-of-plane direction; (<b>c</b>) frequency distribution in an in-plane direction; (<b>d</b>) frequency distribution in an out-of-plane direction.</p>
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14 pages, 4142 KiB  
Article
Microstructure, Mechanical and Thermal Properties of ZTA/Al2TiO5 Ceramic Composites
by A. M. Hassan, Hamada Elsayed, M. Awaad, A. M. Saleh and S. M. Naga
Ceramics 2023, 6(4), 1977-1990; https://doi.org/10.3390/ceramics6040121 - 4 Oct 2023
Viewed by 2215
Abstract
Zirconia-toughened alumina (ZTA)/Al2TiO5 composites were prepared via a sol–gel route. The prepared samples were uniaxially pressed and pressurelessly sintered at 1650–1700 °C for 1 h. The microstructure, densification, and X-ray diffraction patterns of the sintered ZTA/Al2TiO5 composites [...] Read more.
Zirconia-toughened alumina (ZTA)/Al2TiO5 composites were prepared via a sol–gel route. The prepared samples were uniaxially pressed and pressurelessly sintered at 1650–1700 °C for 1 h. The microstructure, densification, and X-ray diffraction patterns of the sintered ZTA/Al2TiO5 composites were investigated, and their mechanical properties, thermal coefficient, and shock resistance were characterized. The addition of Al2TiO5 hindered the grain growth of the alumina particles and enhanced the relative density, Vickers hardness, and bending strength of the composites compared with pure ZTA samples. The fracture toughness was improved by 19% upon the addition of 40 wt% Al2TiO5. Moreover, increasing the Al2TiO5 content resulted in an improvement in the thermal shock resistance. Full article
(This article belongs to the Special Issue Composite Nanopowders: Synthesis and Applications)
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<p>XRD patterns for (<b>a</b>) PSZ and (<b>b</b>) Al<sub>2</sub>TiO<sub>5</sub> calcined at 900 °C.</p>
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<p>Densification parameters for AT/ZTA composites sintered at different sintering temperatures in terms of (<b>a</b>) bulk density g/cm<sup>3</sup> and (<b>b</b>) apparent porosity %.</p>
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<p>Relative density of AT/ZTA composites sintered at 1700 °C.</p>
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<p>XRD diffraction pattern for the samples sintered at 1700 °C.</p>
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<p>SEM micrographs of the polished, thermally etched sintered samples, (<b>a</b>) 10% AT, (<b>b</b>) 20% AT, (<b>c</b>) 30% AT, and (<b>d</b>) 40% AT.</p>
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<p>SEM micrograph of Z4 (40 mass % AT) sintered samples (<b>a</b>) and the EDS spectra (<b>b</b>–<b>e</b>) of the different AT shapes marked on subfigure (<b>a</b>).</p>
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<p>Effect of Al<sub>2</sub>TiO<sub>5</sub> wt% content on the bending strength of AT/ZTA composite.</p>
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<p>Effect of Al<sub>2</sub>TiO<sub>5</sub> wt% content on the Vicker’s hardness of AT/ZTA composite.</p>
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<p>Effect of Al<sub>2</sub>TiO<sub>5</sub> wt% content on the fracture toughness of AT/ZTA composite.</p>
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<p>Thermal expansion of the AT/ZTA composites as a function of Al<sub>2</sub>TiO<sub>5</sub> content.</p>
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<p>Reduction % in bending strength of AT/ZTA samples after 5, 10, 15, and 20 cycles of thermal shock.</p>
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40 pages, 15195 KiB  
Article
Rare-Earth Doped Gd3−xRExFe5O12 (RE = Y, Nd, Sm, and Dy) Garnet: Structural, Magnetic, Magnetocaloric, and DFT Study
by Dipesh Neupane, Noah Kramer, Romakanta Bhattarai, Christopher Hanley, Arjun K. Pathak, Xiao Shen, Sunil Karna and Sanjay R. Mishra
Ceramics 2023, 6(4), 1937-1976; https://doi.org/10.3390/ceramics6040120 - 22 Sep 2023
Viewed by 2503
Abstract
The study reports the influence of rare-earth ion doping on the structural, magnetic, and magnetocaloric properties of ferrimagnetic Gd3−xRExFe5O12 (RE = Y, Nd, Sm, and Dy, x = 0.0, 0.25, 0.50, and 0.75) garnet compound [...] Read more.
The study reports the influence of rare-earth ion doping on the structural, magnetic, and magnetocaloric properties of ferrimagnetic Gd3−xRExFe5O12 (RE = Y, Nd, Sm, and Dy, x = 0.0, 0.25, 0.50, and 0.75) garnet compound prepared via facile autocombustion method followed by annealing in air. X-Ray diffraction (XRD) data analysis confirmed the presence of a single-phase garnet. The compound’s lattice parameters and cell volume varied according to differences in ionic radii of the doped rare-earth ions. The RE3+ substitution changed the site-to-site bond lengths and bond angles, affecting the magnetic interaction between site ions. Magnetization measurements for all RE3+-doped samples demonstrated paramagnetic behavior at room temperature and soft-ferrimagnetic behavior at 5 K. The isothermal magnetic entropy changes (−ΔSM) were derived from the magnetic isotherm curves, M vs. T, in a field up to 3 T in the Gd3−xRExFe5O12 sample. The maximum magnetic entropy change (SMmax) increased with Dy3+ and Sm3+substitution and decreased for Nd3+ and Y3+ substitution with x content. The Dy3+-doped Gd2.25Dy0.75Fe5O12 sample showed SMmax~2.03 Jkg−1K−1, which is ~7% higher than that of Gd3Fe5O12 (1.91 Jkg−1K−1). A first-principal density function theory (DFT) technique was used to shed light on observed properties. The study shows that the magnetic moments of the doped rare-earths ions play a vital role in tuning the magnetocaloric properties of the garnet compound. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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<p>Different polyhedral arrangements of cations in Gd<sub>3</sub>Fe<sub>5</sub>O<sub>12</sub> (<b>a</b>) dodecahedral, (<b>b</b>) octahedral, and (<b>c</b>) tetrahedral.</p>
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<p>(<b>a</b>) The arrangement of different polyhedral cells in a unit cell of Gd<sub>3</sub>Fe<sub>5</sub>O<sub>12</sub>. (<b>b</b>) The crystal structure of Gd<sub>3</sub>Fe<sub>5</sub>O<sub>12</sub> with eight formula units per unit cell.</p>
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<p>XRD pattern of the Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound. The inset shows an expanded view of the XRD pattern between 31–33°.</p>
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<p>(<b>a</b>–<b>d</b>): Rietveld refinement profile for Gd<sub>3-<span class="html-italic">x</span></sub>Dy<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>): Rietveld refinement profile for the Gd<sub>3−<span class="html-italic">x</span></sub>Nd<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>d</b>): Rietveld refinement profile for the Gd<sub>3-<span class="html-italic">x</span></sub>Sm<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>d</b>): Rietveld refinement profile for the Gd<sub>3-<span class="html-italic">x</span></sub>Y<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>Position of the oxygen and magnetic ions at the (<b>a</b>) octahedral, (<b>b</b>) tetrahedral, and (<b>c</b>) dodecahedral sites.</p>
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<p>(<b>a</b>) Lattice parameter and (<b>b</b>) Gd–Fe2 bond length of the Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>Bond angle (<b>a</b>) Fe1–O–Fe2 and (<b>b</b>) Gd–O–Fe2 for Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>d</b>): HWL plots for the Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>j</b>) SEM images and corresponding length distribution of the Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>j</b>) SEM images and corresponding length distribution of the Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>The partial and total density of states of pure Gd<sub>3</sub>Fe<sub>5</sub>O<sub>12</sub>: (<b>a</b>) TDOS and (<b>b</b>–<b>d</b>) orbital contributions of individual elements to the total DOS. Both the spin-up and spin-down components are shown.</p>
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<p>The magnetic moment of Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> as a function of doping content, <span class="html-italic">x</span>, was derived from the DFT study.</p>
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<p>(<b>a</b>–<b>d</b>) Thermogravimetric curves of Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>d</b>) FC/ZFC magnetization vs. temperature curves for the Gd<sub>3-<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>Schematic of three sublattice magnetizations as a function of temperature for RE<sub>3</sub>Fe<sub>5</sub>O<sub>12</sub> garnet compound.</p>
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<p>(<b>a</b>–<b>d</b>) Magnetization vs. field (<span class="html-italic">M</span> vs. <span class="html-italic">H</span>) curves for RE<sup>3+</sup> doped Gd<sub>3−<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds at 5 K.</p>
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<p>(<b>a</b>–<b>d</b>) M vs. H plots for the Gd<sub>3-x</sub>RE<sub>x</sub>O<sub>12</sub> compound measured at 300 K.</p>
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<p>(<b>a</b>–<b>d</b>) Isothermal magnetization curves for the Gd<sub>3-x</sub>Dy<sub>x</sub>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>) Isothermal magnetization curves for the Gd<sub>3-<span class="html-italic">x</span></sub>Nd<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>) Isothermal magnetization curves for the Gd<sub>3-<span class="html-italic">x</span></sub>Sm<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>) Isothermal magnetization curves for the Gd<sub>3-<span class="html-italic">x</span></sub>Y<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>): Change in magnetic entropy −ΔS<sub>M</sub>, as a function of temperature up to 3 T fields for the Gd<sub>3-<span class="html-italic">x</span></sub>Dy<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>): Change in magnetic entropy −ΔS<sub>M</sub>, as a function of temperature up to 3 T fields for the Gd<sub>3-<span class="html-italic">x</span></sub>Nd<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>): Change in magnetic entropy −ΔS<sub>M</sub>, as a function of temperature up to 3 T fields for the Gd<sub>3-<span class="html-italic">x</span></sub>Sm<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compounds.</p>
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<p>(<b>a</b>–<b>d</b>): Change in magnetic entropy −ΔS<sub>M</sub>, as a function of temperature up to 3 T fields for the Gd<sub>3-<span class="html-italic">x</span></sub>Y<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>ΔS<sub>M</sub><sup>max</sup> vs. field for the Gd<sub>3-<span class="html-italic">x</span></sub>RE<span class="html-italic"><sub>x</sub></span>Fe<sub>5</sub>O<sub>12</sub> compound.</p>
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<p>(<b>a</b>–<b>d</b>): Relative cooling power (RCP) of the Gd<sub>3-x</sub>RE<sub>x</sub>Fe<sub>5</sub>O<sub>12</sub> compound as a function of the applied field.</p>
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11 pages, 2630 KiB  
Article
Characterization and Heat Transfer Assessment of CuO-Based Nanofluid Prepared through a Green Synthesis Process
by Suresh Kumar Shanmugam, Ajithram Arivendan, Samy Govindan Selvamani, Thangaraju Dheivasigamani, Thirumalai Kumaran Sundaresan and Saood Ali
Ceramics 2023, 6(4), 1926-1936; https://doi.org/10.3390/ceramics6040119 - 22 Sep 2023
Cited by 2 | Viewed by 2038
Abstract
The manufacturing of copper oxide (CuO) nanoparticles has been accomplished utilizing a green technique that relies on biologically reliable mechanisms. Aqueous solutions of copper nitrate and Ixora Coccinea leaf extract are used in an environmentally safe process for creating CuO nanoparticles. The characterization [...] Read more.
The manufacturing of copper oxide (CuO) nanoparticles has been accomplished utilizing a green technique that relies on biologically reliable mechanisms. Aqueous solutions of copper nitrate and Ixora Coccinea leaf extract are used in an environmentally safe process for creating CuO nanoparticles. The characterization of the synthesized CuO nanoparticles involves the utilization of techniques such as X-ray diffractometry (XRD), scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), and thermogravimetricanalysis (TGA). CuO nanoparticles are confirmed by XRD and FTIR peak results. When the particles are measured, they range between 93.75 nm and 98.16 nm, respectively. The produced CuO nanoparticles are used to prepare the nanofluid. While conventional water exhibits a 3 °C temperature difference, nanofluid achieves a considerable temperature differenceof 7 °C. As a result, it is clear that the nanofluid performs better at dispersing heat into the environment. The experiment’s overall findings support the possibility of ecologically friendly, green-synthesized CuO nanoparticle-induced nanofluid as an effective heattransfer fluid that can be applied to heattransfer systems. Full article
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<p>Process involved in the eco-friendly green synthesis of CuO nanoparticles.</p>
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<p>XRD analysis.</p>
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<p>(<b>a</b>) FTIR analysis; (<b>b</b>) expanded view of FTIR to confirm CuO formation.</p>
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<p>Microstructure.</p>
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<p>EDAX spectrum analysis.</p>
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<p>(<b>a</b>) DTA analysis, (<b>b</b>) TGA analysis, and(<b>c</b>) expanded view of TGA.</p>
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<p>Heat transfer apparatus.</p>
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13 pages, 17693 KiB  
Article
Dielectric Properties of Compacts Sintered after High-Pressure Forming of Lithium Fluoride
by Pavel Ctibor, Libor Straka, Josef Sedláček and František Lukáč
Ceramics 2023, 6(4), 1913-1925; https://doi.org/10.3390/ceramics6040118 - 22 Sep 2023
Cited by 1 | Viewed by 1347
Abstract
High-pressure forming at 300 MPa and room temperature was applied before the sintering of a lithium fluoride (LiF) powder. The as-fired samples were tested as dielectrics and showed very interesting characteristics. The best sample, sintered at 750 °C for 8 h, had a [...] Read more.
High-pressure forming at 300 MPa and room temperature was applied before the sintering of a lithium fluoride (LiF) powder. The as-fired samples were tested as dielectrics and showed very interesting characteristics. The best sample, sintered at 750 °C for 8 h, had a relative permittivity of 12.1 and a loss tangent of 0.0006, both of them frequency-independent and temperature-independent up to at least 150 °C, and moreover, the volume DC resistivity was 27.4 × 1012 Ωm at room temperature. These parameters are comparable with oxide ceramics, processed at temperatures over 1300 °C, as for example, aluminum dioxide (Al2O3) or Y3Al5O12 (YAG). LiF material is advantageous because of its very low sintering temperature, which is only about one-half of typical oxide ceramic dielectrics. Full article
(This article belongs to the Special Issue Advances in Ceramics, 2nd Edition)
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Graphical abstract
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<p>Sample 700-2, relative permittivity versus changing frequency for three varying temperatures.</p>
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<p>Sample 700-2, loss tangent versus changing frequency for three varying temperatures.</p>
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<p>Sample 750-8, relative permittivity versus changing frequency for three varying temperatures.</p>
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<p>Sample 750-8, loss tangent versus changing frequency for three varying temperatures.</p>
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<p>Cross-sections of (<b>a</b>) sample 650-2; (<b>b</b>) sample 700-8; (<b>c</b>) sample 750-8 (with microindents); SEM-BSE.</p>
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<p>Cross-sections of (<b>a</b>) sample 650-2; (<b>b</b>) sample 700-8; (<b>c</b>) sample 750-8 (with microindents); SEM-BSE.</p>
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<p>Sample 750-8, cross-section; OM.</p>
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<p>Sample 700-2, cross-section; OM; scale is the same as for <a href="#ceramics-06-00118-f006" class="html-fig">Figure 6</a>.</p>
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<p>XRD pattern of LiF sintered at 675 °C.</p>
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<p>Band gap estimation for three LiF samples.</p>
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<p>Arrhenius plot of AC conductivity as a function of the absolute temperature, sample 700-2.</p>
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<p>Arrhenius plot of AC conductivity as a function of the absolute temperature, sample 835-8.</p>
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