[go: up one dir, main page]

 
 
Sign in to use this feature.

Years

Between: -

Subjects

remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline

Journals

remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline

Article Types

Countries / Regions

remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline
remove_circle_outline

Search Results (4,278)

Search Parameters:
Keywords = SEM-EDS

Order results
Result details
Results per page
Select all
Export citation of selected articles as:
17 pages, 3569 KiB  
Article
A Cippus from Turris Libisonis: Evidence for the Use of Local Materials in Roman Painting on Stone in Northern Sardinia
by Roberta Iannaccone, Stefano Giuliani, Sara Lenzi, Matteo M. N. Franceschini, Silvia Vettori and Barbara Salvadori
Minerals 2024, 14(10), 1040; https://doi.org/10.3390/min14101040 (registering DOI) - 17 Oct 2024
Abstract
The ancient Roman town of Turris Libisonis was located on the northern coast of Sardinia and was known in the past as an important naval port. Located in the Gulf of Asinara, it was a Roman colony from the 1st century BCE and [...] Read more.
The ancient Roman town of Turris Libisonis was located on the northern coast of Sardinia and was known in the past as an important naval port. Located in the Gulf of Asinara, it was a Roman colony from the 1st century BCE and became one of the richest towns on the island. Among the archaeological finds in the area, the cippus exhibited in the Antiquarium Turritano is of great interest for its well-preserved traces of polychromy. The artefact dates back to the early Imperial Age and could have had a funerary or votive function. The artefact was first examined using a portable and non-invasive protocol involving multi-band imaging (MBI), portable X-ray fluorescence (p-XRF), portable FT-IR in external reflectance mode (ER FT-IR) and Raman spectroscopy. After this initial examination, a few microfragments were collected and investigated by optical microscopy (OM), X-ray powder diffraction (XRPD), Fourier-transform infrared spectroscopy in ATR mode (ATR FT-IR) and micro-ATR mode (μATR FT-IR) and Scanning Electron Microscopy/Energy Dispersive Spectroscopy (SEM-EDS) to improve our knowledge and characterize the materials and to determine their provenience. The results contribute to a better understanding of the provenance of materials and shed light on pigments on stone and their use outside the Italian peninsula and, in particular, Roman Sardinia. Full article
(This article belongs to the Special Issue Geomaterials and Cultural Heritage)
Show Figures

Figure 1

Figure 1
<p>(<b>a</b>) The position of the cippus in the Antiquarium of Porto Torres (SS) and the two sides analyzed: (<b>b</b>) side A; (<b>c</b>) side B (courtesy of Ministero della Cultura–Direzione Regionale Musei Sardegna).</p>
Full article ">Figure 2
<p>(<b>a</b>) Raking light detail of flaking areas; (<b>b</b>) High magnification image (60×) of the area in the red square; (<b>c</b>) SEM image in BSE from the sample (red point) and (<b>d</b>) EDS analysis results of a point on recrystallized salt.</p>
Full article ">Figure 3
<p>(<b>a</b>) Raman spectrum of point corresponding to (<b>a</b>) a black area and (<b>b</b>) a yellow area, respectively. On the right, the optical microscopic details of the points (60×). In (<b>b</b>) Raman spectrum of yellow area, in black, and goethite reference spectrum in yellow (RRUFF mineral database).</p>
Full article ">Figure 4
<p>(<b>a</b>) p-XRF spectra of point 8 in black, point 10 in dotted black and the reference background in red; (<b>b</b>) the locations of measured points 8 and 10 are shown (<b>c</b>) Raman spectra of green earth pigment at point 8 (in green) and point 10 (in gray).</p>
Full article ">Figure 5
<p>Microphotographs of thin sections of the carbonate rock of the cippus (<b>a</b>,<b>b</b>) and of the mortar covering the cippus (<b>c</b>,<b>d</b>) (using a polarized light microscope): (<b>a</b>,<b>c</b>) parallel nicols; (<b>b</b>,<b>d</b>) crossed nicols.</p>
Full article ">Figure 6
<p>Geological map of Porto Torres and its surrounding area. Modified from [<a href="#B46-minerals-14-01040" class="html-bibr">46</a>].</p>
Full article ">Figure 7
<p>Macro-photo of carbonate rock of the cippus. Various fossils were observed in the carbonatic rock of the cippus: (<b>a</b>) gastropods; (<b>b</b>) ammonites; (<b>c</b>) algae tallus.</p>
Full article ">Figure 8
<p>Fragment analyzed by SEM−EDS. (<b>a</b>) Optical microscope image at 50×; (<b>b</b>) backscattered details at 127×; and (<b>c</b>) EDS analysis results.</p>
Full article ">Figure 9
<p>(<b>a</b>) FT-IR micro-ATR spectrum obtained from the green sample using point analysis with a TE-MCT detector and (<b>b</b>) FT-IR FPA-ATR spectrum extracted from the chemical map shown above. The arrow indicates the position of the spectrum.</p>
Full article ">
14 pages, 3628 KiB  
Article
Tackling Microbial Contamination: Safesink Solution with Silver-Coated Microspheres
by Eulalia Zumaquero, David Terrado, Rosa de Llanos, Marina Puerta, Rocío Cejudo and María Pilar Gómez-Tena
Bacteria 2024, 3(4), 344-357; https://doi.org/10.3390/bacteria3040023 - 16 Oct 2024
Viewed by 175
Abstract
Ceramic and vitreous materials can be functionalized to exhibit biocidal activity. This research evaluates the biocidal properties of silver-modified vitreous microspheres designed to be included in water endpoints and siphons to prevent nosocomial diseases produced in hospital environments. The microspheres obtained from a [...] Read more.
Ceramic and vitreous materials can be functionalized to exhibit biocidal activity. This research evaluates the biocidal properties of silver-modified vitreous microspheres designed to be included in water endpoints and siphons to prevent nosocomial diseases produced in hospital environments. The microspheres obtained from a coating and heat treatment process at 650 °C have been chemically and microstructurally characterized using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Wavelength Dispersive X-ray Fluorescence (WD-XRF), Scanning Electron Microscopy (FEG-SEM) and Energy-dispersive X-ray Microanalysis (EDS) to determine how silver particles are distributed in the glassy matrix and to relate their bactericidal capacity by means of leaching tests. Microbiological tests have been performed against microorganisms such as Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, and Candida auris. The results revealed that these silver-coated microspheres had significant bactericidal activity, with a significant reduction in the population of E. coli, C. auris, and P. aeruginosa, with no cytotoxic effect of these microspheres. Full article
(This article belongs to the Collection Feature Papers in Bacteria)
Show Figures

Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>SEM micrograph and EDS analyzed areas of silver-coated glass beads (cross-section).</p>
Full article ">Figure 2
<p>SEM micrograph of silver-coated glass beads (glassy matrix) (50,000×).</p>
Full article ">Figure 3
<p>SEM micrograph and coating thickness measurements in cross-section of the silver-coated glass beads. The white arrows indicate the silver coating on the glass bead. The numbers inside the beads are shown in <a href="#bacteria-03-00023-t002" class="html-table">Table 2</a>.</p>
Full article ">Figure 4
<p>Cross-section of the silver-coated glass beads after the lixiviation process as seen with the stereo-microscope (<b>left</b>) and SEM (<b>right</b>).</p>
Full article ">Figure 5
<p>SEM micrograph and EDS analysis (% weight) of the cross-section of silver-coated glass beads after the lixiviation process.</p>
Full article ">Figure 6
<p>Antimicrobial activity of silver-coated glass beads against a known microbial population of <span class="html-italic">S. aureus</span> ATCC 29213 (<b>A</b>), <span class="html-italic">E. coli</span> CECT 101 (<b>B</b>), <span class="html-italic">P. aeruginosa ATCC 27853</span> (<b>C</b>), and <span class="html-italic">C. auris CJ 207</span> (<b>D</b>). Experimental condition comparing the effect of silver-coated glass beads and positive control (no beads).</p>
Full article ">Figure 7
<p>Antimicrobial activity of lixiviation extractions against a known microbial population of <span class="html-italic">S. aureus</span> ATCC 29213 (<b>A</b>), <span class="html-italic">E. coli</span> CECT 101 (<b>B</b>), <span class="html-italic">P. aeruginosa ATCC 27853</span> (<b>C</b>), and <span class="html-italic">C. auris CJ 207</span> (<b>D</b>). Experimental condition comparing the effect of silver-coated glass beads (blue line) and positive control (no beads) (black line).</p>
Full article ">Figure 8
<p>Representation of the average rates of cell viability for the three technical replicates.</p>
Full article ">
20 pages, 15874 KiB  
Article
Study on the Performance of High-Performance Mortar (HPM) Prepared Using Sodium-Silicate-Modified Graphite Tailing Sand
by Ruixin Jiang, Zhengjun Wang, Yingxin Du and Yajing Wen
Buildings 2024, 14(10), 3269; https://doi.org/10.3390/buildings14103269 (registering DOI) - 15 Oct 2024
Viewed by 289
Abstract
In order to rationalize the consumption of graphite tailing sand and reduce its pollution of the environment—with sodium silicate being a commonly used activator for improving the strength of concrete composites—in this study, the joint effects of sodium silicate (SS) and graphite tail [...] Read more.
In order to rationalize the consumption of graphite tailing sand and reduce its pollution of the environment—with sodium silicate being a commonly used activator for improving the strength of concrete composites—in this study, the joint effects of sodium silicate (SS) and graphite tail sand (GT) on the strength and frost resistance of graphite tail sand high-performance mortar (GT-HPM) were investigated. Experiments were conducted to evaluate the bulk density, water absorption, compressive strength, speed of sound, and working performance status of GT-HPM before and after freezing and thawing at different SS dosages and different GT substitution rates. The microstructural properties of GT-HPM were also analyzed by X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM/EDS). The results showed that 4% SS doping improved the performance of GT-HPM more obviously. Moreover, with an increase in the GT substitution rate, the mechanical properties and frost resistance of GT-HPM increased firstly and then decreased, and the best performance of GT-HPM was obtained when the GT substitution rate was 20%. At 6% SS doping, the performance of GT-HPM gradually decreased with the increase in the graphite tailing sand substitution rate. FT-IR testing showed that there was no significant change with the type of hydration products used, and the Si–O–T absorption peak and average bond length of GT-4 were the largest. SS and GT promoted the generation of hydration products. Microstructural analysis showed that 4% SS promoted the hydration reaction; in addition, an appropriate amount of GT improved the pore structure of HPM, increased the strength and frost resistance, and provided fundamental insights for the subsequent comprehensive utilization of graphite tailing sand. Full article
Show Figures

Figure 1

Figure 1
<p>Particle size distribution of materials in GT-HPM.</p>
Full article ">Figure 2
<p>Flowchart of the test.</p>
Full article ">Figure 3
<p>Velocity of sound test principle.</p>
Full article ">Figure 4
<p>Freeze–thaw test chamber temperature–time curve.</p>
Full article ">Figure 5
<p>Water absorption and wet-packing density.</p>
Full article ">Figure 6
<p>GT-HPM compressive damage section.</p>
Full article ">Figure 7
<p>Variation in GT-HPM compressive strength and sound velocity values at different ages.</p>
Full article ">Figure 8
<p>Graphite tailing substitution rate versus compressive strength and sound velocity fit.</p>
Full article ">Figure 9
<p>Changes in GT-HPM performance before and after freeze–thaw cycles. (<b>a</b>) The mass loss of GT-HPM after freeze–thaw test; (<b>b</b>) the RDME of GT-HPM after freeze–thaw test; (<b>c</b>) the change in the strength of GT-HPM before and after freeze–thaw; (<b>d</b>) the strength change of GT-HPM after freeze–thaw test.</p>
Full article ">Figure 10
<p>GT-HPM reaction mechanism diagram. (<b>a</b>) Freeze–thaw cycle damage mechanism diagram; (<b>b</b>) alkali exciter reaction mechanism diagram.</p>
Full article ">Figure 11
<p>FTIR spectra of GT-HPM after freezing and thawing.</p>
Full article ">Figure 12
<p>XRD pattern of GT-HPM samples after freeze–thaw cycles.</p>
Full article ">Figure 13
<p>SEM images of GT-HPM samples after freeze–thaw cycles.</p>
Full article ">Figure 14
<p>EDS results of GT-HPM samples after freeze–thaw cycles.</p>
Full article ">
16 pages, 3835 KiB  
Article
Isolation and Characterization of Nanocellulose from Polypodiophyta Fern Using Chemo-Mechanical Method
by Katja Vasić, Monika Dokl, Željko Knez and Maja Leitgeb
Biomimetics 2024, 9(10), 624; https://doi.org/10.3390/biomimetics9100624 (registering DOI) - 14 Oct 2024
Viewed by 406
Abstract
Nanocellulose is considered a promising and sustainable biomaterial, with excellent properties of biorenewability with improved mechanical properties. As a unique natural biopolymer, it has been applied to many different industries, where efficient and environmentally friendly productions are in demand. For the first time, [...] Read more.
Nanocellulose is considered a promising and sustainable biomaterial, with excellent properties of biorenewability with improved mechanical properties. As a unique natural biopolymer, it has been applied to many different industries, where efficient and environmentally friendly productions are in demand. For the first time, ferns from the class Polypodiopsida were used for the isolation of cellulose fibers, which was performed using a chemo-mechanical method. As chemical treatment plays a crucial role in the isolation of nanocellulose, it affects the efficiency of the extraction process, as well as the properties of the resulting nanocellulose. Therefore, mechanical fibrillation was performed via grinding, while the chemical process consisted of three different treatments: alkali treatment, bleaching, and acid hydrolysis. In three different experiments, each treatment was separately prolonged to investigate the differing properties of isolated nanocellulose. Structural analysis and morphological analysis were investigated by SEM, EDS, FT-IR, and DLS. The thermal stability of cellulose fibers was investigated by TGA/DSC. The morphology of obtained nanocellulose was confirmed via SEM analysis for all samples, with particles ranging from 20 nm up to 600 nm, while the most consistent sizes were observed for NC3, ranging from 20 to 60 nm. FT-IR spectra showed prominent absorption peaks corresponding to cellulose, as well as the absence of absorption peaks, corresponding to lignin and hemicellulose. The EDS confirmed the elemental purity of nanocellulose, while TGA/DSC indicated higher thermal stability of nanocellulose, compared to untreated fern, which started to degrade earlier than nanocellulose. Such characteristics with unique properties make nanocellulose a versatile biomaterial for the industrial production of cellulosic materials. Full article
(This article belongs to the Special Issue Advances in Biomaterials, Biocomposites and Biopolymers 2024)
Show Figures

Figure 1

Figure 1
<p>Isolation process of nanocellulose from <span class="html-italic">Polypodiophyta</span> fern.</p>
Full article ">Figure 2
<p>SEM of samples NC1 (<b>a</b>–<b>e</b>), NC2 (<b>f</b>–<b>j</b>), and NC3 (<b>k</b>–<b>o</b>) at various magnification levels.</p>
Full article ">Figure 3
<p>Scanning electron micrographs and line scanning EDS profiles of isolated cellulose samples: (<b>a</b>) NC1, (<b>b</b>) NC2, and (<b>c</b>) NC3.</p>
Full article ">Figure 4
<p>FTIR spectra of the isolated nanocellulose samples: (<b>a</b>) NC1, (<b>b</b>) NC2, (<b>c</b>) NC3, and (<b>d</b>) raw untreated material.</p>
Full article ">Figure 5
<p>TGA profiles of the isolated cellulose samples: (<b>a</b>) NC1, (<b>b</b>) NC2, (<b>c</b>) NC3, and (<b>d</b>) untreated raw material.</p>
Full article ">Figure 6
<p>DSC profile curves of the isolated cellulose samples: (<b>a</b>) NC1, (<b>b</b>) NC2, (<b>c</b>) NC3, and (<b>d</b>) untreated raw material.</p>
Full article ">Figure 7
<p>Particle size distribution profiles of isolated cellulose samples.</p>
Full article ">
32 pages, 26302 KiB  
Article
Development of Novel Biocomposites with Antimicrobial-Activity-Based Magnesium-Doped Hydroxyapatite with Amoxicillin
by Carmen Cimpeanu, Daniela Predoi, Carmen Steluta Ciobanu, Simona Liliana Iconaru, Krzysztof Rokosz, Mihai Valentin Predoi, Steinar Raaen and Monica Luminita Badea
Antibiotics 2024, 13(10), 963; https://doi.org/10.3390/antibiotics13100963 - 12 Oct 2024
Viewed by 729
Abstract
Background/Objectives: A biocomposite based on magnesium-doped hydroxyapatite and enriched with amoxicillin (MgHApOx) was synthesized using the coprecipitation method and is presented here for the first time. Methods: The stability of MgHAp and MgHApOx suspensions was evaluated by ultrasound measurements. The structure [...] Read more.
Background/Objectives: A biocomposite based on magnesium-doped hydroxyapatite and enriched with amoxicillin (MgHApOx) was synthesized using the coprecipitation method and is presented here for the first time. Methods: The stability of MgHAp and MgHApOx suspensions was evaluated by ultrasound measurements. The structure of the synthesized MgHAp and MgHApOx was examined with X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The crystalline structure was determined by X-ray diffraction. The FTIR data were collected in the range of 4000–400 cm−1. The morphology of the nanoparticles was evaluated by scanning electron microscopy (SEM). Furthermore, the biocompatible properties of MgHAp, MgHApOx and amoxicillin (Ox) suspensions were assessed using human fetal osteoblastic cells (hFOB 1.19 cell line). The antimicrobial properties of the MgHAp, MgHApOx and Ox suspension nanoparticles were assessed using the standard reference microbial strains Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922 and Candida albicans ATCC 10231. Results: X-ray studies have shown that the biocomposite retains the characteristics of HAp and amoxicillin. The SEM assessment exhibited that the apatite contains particles at nanometric scale with acicular flakes morphology. The XRD and SEM results exhibited crystalline nanoparticles. The average crystallite size calculated from XRD analysis increased from 15.31 nm for MgHAp to 17.79 nm in the case of the MgHApOx sample. The energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analysis highlighted the presence of the constituent elements of MgHAp and amoxicillin. Moreover, XPS confirmed the substitution of Ca2+ ions with Mg2+ and the presence of amoxicillin constituents in the MgHAp lattice. The results of the in vitro antimicrobial assay demonstrated that MgHAp, MgHApOx and Ox suspensions exhibited good antimicrobial activity against the tested microbial strains. The results showed that the antimicrobial activity of the samples was influenced by the presence of the antibiotic and also by the incubation time. Conclusions: The findings from the biological assays indicate that MgHAp and MgHApOx are promising candidates for the development of new biocompatible and antimicrobial agents for biomedical applications. Full article
Show Figures

Figure 1

Figure 1
<p>Time evolution of the recorded signals of MgHAp suspension from left to right over 5000 s (<b>a</b>); Recorded signals amplitudes during the experiment for MgHAp suspension (<b>b</b>).</p>
Full article ">Figure 2
<p>Time evolution of the recorded signals of MgHApOx suspension from left to right over 4500 s (<b>a</b>); Recorded signals amplitudes during the experiment for MgHApOx suspension (<b>b</b>).</p>
Full article ">Figure 3
<p>Spectral amplitudes of all recorded signals (<b>a</b>), time-averaged attenuation for the investigated frequency range (<b>b</b>) and relative spectral amplitudes vs. time (<b>c</b>) of MgHAp sample.</p>
Full article ">Figure 4
<p>Spectral amplitudes of all recorded signals (<b>a</b>), time-averaged attenuation for the investigated frequency range (<b>b</b>) and relative spectral amplitudes vs. time (<b>c</b>) of MgHApOx sample.</p>
Full article ">Figure 5
<p>XRD patterns of MgHAp (<b>b</b>), MgHApOx (<b>c</b>) and Ox (<b>d</b>) samples. The JCPDS # 09-0432 of HAp (<b>a</b>) and JCPDS # 39-1832 of Ox (<b>e</b>). The * indicates the maxima associated with amoxicillin structure.</p>
Full article ">Figure 6
<p>XRD patterns of MgHAp (<b>a</b>), MgHApOx (<b>b</b>) relative shift on 2θ range of 25–35°. The * indicates the maxima associated with amoxicillin structure.</p>
Full article ">Figure 7
<p>(<b>a</b>,<b>b</b>) SEM micrographs obtained at ×100,000 and at ×200,000 for MgHAp sample; (<b>d</b>,<b>e</b>) SEM micrographs obtained at ×100,000 and at ×200,000 for MgHApOx sample. (<b>c</b>,<b>f</b>) particle size distribution obtained for MgHAp and MgHApOx.</p>
Full article ">Figure 8
<p>Energy-dispersive X-ray spectroscopy spectra of (<b>a</b>) MgHAp and (<b>b</b>) MgHApOx.</p>
Full article ">Figure 9
<p>FTIR general spectra of MgHAp, MgHApOx and Ox.</p>
Full article ">Figure 10
<p>FTIR spectra of MgHAp, MgHApOx and Ox obtained between 900 and 1200 cm<sup>−1</sup> and their second derivative curve.</p>
Full article ">Figure 11
<p>Deconvoluted FTIR spectra of the MgHAp, Ox and MgHApOx obtained in the 900–1200 cm<sup>−1</sup> spectral domain.</p>
Full article ">Figure 12
<p>General XPS spectra of MgHAp (<b>a</b>) and MgHApOx (<b>b</b>) samples.</p>
Full article ">Figure 13
<p>High-resolution XPS spectra and curve-fitting results of C 1s for MgHAp (<b>a</b>) and MgHApOx (<b>b</b>); O1s for MgHAp (<b>c</b>) and MgHApOx (<b>d</b>); Ca2p for MgHAp (<b>e</b>) and MgHApOx (<b>f</b>); P2p for MgHAp (<b>g</b>) and MgHApOx (<b>h</b>).</p>
Full article ">Figure 14
<p>High-resolution XPS spectra and curve-fitting results of Mg 2p for MgHAp (<b>a</b>) and MgHApOx (<b>b</b>).</p>
Full article ">Figure 15
<p>High-resolution XPS spectra and curve-fitting results of N1s (<b>a</b>) and S 2p (<b>b</b>) for MgHApOx sample.</p>
Full article ">Figure 16
<p>Percentage hemolysis of sheep red blood cells (RBCs) exposed to different concentrations of MgHAp, MgHApOx and Ox suspensions. The statistical analysis of the data was performed using one-way ANOVA. The calculated <span class="html-italic">p</span>-values were <span class="html-italic">p</span> &lt; 0.002.</p>
Full article ">Figure 17
<p>MTT assay of hFOB 1.19 cells incubated with MgHAp, MgHApOx and Ox suspensions for 24, 48 and 72 h. The results are represented as mean ± standard deviation (SD) and are expressed as percentages of control (100% viability). The statistical analysis of the data was performed using one-way ANOVA. The <span class="html-italic">p</span>-values indicated are * <span class="html-italic">p</span> ≤ 0.002, ** <span class="html-italic">p</span> ≤ 0.001, *** <span class="html-italic">p</span> ≤ 0.0001.</p>
Full article ">Figure 18
<p>Lactate dehydrogenase (LDH) activity released in the culture medium of hFOB 1.19 cells after the treatment with MgHAp, MgHApOx and Ox suspensions for 24, 48 and 72 h. The results are represented as mean ± standard deviation (SD). The statistical analysis of the data was performed using one-way ANOVA. The <span class="html-italic">p</span>-values indicated are * <span class="html-italic">p</span> ≤ 0.002, ** <span class="html-italic">p</span> ≤ 0.001, *** <span class="html-italic">p</span> ≤ 0.0001.</p>
Full article ">Figure 19
<p>Graphical representation of the logarithmic values of colony forming units (CFU)/mL of <span class="html-italic">S. aureus</span> ATCC 25923 (<b>a</b>), <span class="html-italic">E. coli</span> ATCC 25922 (<b>b</b>) and <span class="html-italic">C. albicans</span> ATCC 10231 (<b>c</b>) microbial strains after 24, 48 and 72 h of exposure to MgHAp, MgHApOx and Ox suspensions. #—depicts the bactericidal properties of the samples. The results are represented as mean ± standard error. Ordinary one-way ANOVA was used for the statistical analysis. The <span class="html-italic">p</span>-values indicated are * <span class="html-italic">p</span> ≤ 0.002, ** <span class="html-italic">p</span> ≤ 0.001, *** <span class="html-italic">p</span> ≤ 0.0001.</p>
Full article ">Figure 20
<p>The schematic representation (<b>a</b>) and the image (<b>b</b>) of US experimental setup [<a href="#B95-antibiotics-13-00963" class="html-bibr">95</a>].</p>
Full article ">
17 pages, 19564 KiB  
Article
Effects of ZrO2 Nano-Particles’ Incorporation into SnAgCu Solder Alloys: An Experimental and Theoretical Study
by Agata Skwarek, Halim Choi, Tamás Hurtony, Jaeduk Byun, Ahmad Azmin Mohamad, David Bušek, Karel Dušek and Balázs Illés
Nanomaterials 2024, 14(20), 1636; https://doi.org/10.3390/nano14201636 - 12 Oct 2024
Viewed by 344
Abstract
This study investigates the mechanism and effects of incorporating different ZrO2 nano-particles into SAC0307 solder alloys. ZrO2 nano-powder and nano-fibers in 0.25–0.5 wt% were added to the SAC0307 alloy to prepare composite solder joints by surface mount technology. The solder joints [...] Read more.
This study investigates the mechanism and effects of incorporating different ZrO2 nano-particles into SAC0307 solder alloys. ZrO2 nano-powder and nano-fibers in 0.25–0.5 wt% were added to the SAC0307 alloy to prepare composite solder joints by surface mount technology. The solder joints were shear tested before and after a 4000 h long 85 °C/85% RH corrosive reliability test. The incorporation of ZrO2 nano-particles enhanced the initial shear force of the solder joint, but they decreased the corrosion resistance in the case of 0.5 wt%. SEM, EDS, and FIB analysis revealed intensive growth of SnO2 on the solder joint surfaces, leading to the formation of Sn whiskers. Density functional theory (DFT) simulations showed that, despite Sn being able to bond to the surface of ZrO2, the binding energy was weak, and the whole system was therefore unstable. It was also found that ZrO2 nano-particles refined the microstructure of the solder joints. Decreased β-Sn grain size and more dispersed intermetallic compounds were observed. The microstructural refinement caused mechanical improvement of the ZrO2 composite solder joints by dispersion strengthening but could also decrease their corrosion resistance. While ZrO2 nano-particles improved the solder joint mechanical properties, their use is recommended only in non-corrosive environments, such as microelectronics for space applications. Full article
(This article belongs to the Section Nanocomposite Materials)
Show Figures

Figure 1

Figure 1
<p>Statistics of the shear forces.</p>
Full article ">Figure 2
<p>SEM micrograph of the surface of the joints after 4000 h TH test: (<b>a</b>) ref. SAC; (<b>b</b>) SAC-0.25ZrO<sub>2</sub>(np); (<b>c</b>) SAC-0.5ZrO<sub>2</sub>(np).</p>
Full article ">Figure 3
<p>SEM micrograph of the surface of the solder joints after 4000 h TH test: (<b>a</b>) SAC-0.25ZrO<sub>2</sub>(nf); (<b>b</b>) SAC-0.5ZrO<sub>2</sub>(nf).</p>
Full article ">Figure 4
<p>Sn whiskers on the solder joints: (<b>a</b>) reference SAC; (<b>b</b>) SAC-0.25ZrO<sub>2</sub>(np); (<b>c</b>) SAC-0.5ZrO<sub>2</sub>(np); (<b>d</b>) SAC-0.25ZrO<sub>2</sub>(nf); (<b>e</b>) SAC-0.5ZrO<sub>2</sub>(nf); (<b>f</b>) EDS spectra of S5.</p>
Full article ">Figure 5
<p>Cross-section of the solder joints after 4000 h TH test: (<b>a</b>) ref. SAC; (<b>b</b>) SAC-0.25ZrO<sub>2</sub>(np); (<b>c</b>) SAC-0.5ZrO<sub>2</sub>(np); (<b>d</b>) SAC-0.25ZrO<sub>2</sub>(nf); (<b>e</b>) SAC-0.5ZrO<sub>2</sub>(nf).</p>
Full article ">Figure 6
<p>Spatial corrosion depth (d<span class="html-italic"><sub>SC</sub></span>) in the solder joints.</p>
Full article ">Figure 7
<p>Microstructure of the solder joints: (<b>a</b>) Ref. SAC, 0 h TH test; (<b>b</b>) SAC-0.5ZrO<sub>2</sub>(np), 0 h TH test; (<b>c</b>) SAC-0.5ZrO<sub>2</sub>(nf), 0 h TH test; (<b>d</b>) ref. SAC, 4000 h TH test; (<b>e</b>) SAC-0.25ZrO<sub>2</sub>(np), 4000 h TH test; (<b>f</b>) SAC-0.25ZrO<sub>2</sub>(nf), 4000 h TH test.</p>
Full article ">Figure 8
<p>DFT calculation of the Sn cluster on the ZrO<sub>2</sub> crystal, the initial position is left, and the optimized position is right.</p>
Full article ">Figure 9
<p>Investigation of localized corrosion in a SAC-ZrO<sub>2</sub> solder joint: (<b>a</b>) SEM-BSE of SAC-0.5ZrO<sub>2</sub>(np); (<b>b</b>) EDS spectra (M1-M4); (<b>c</b>) SEM-BSE of FIB cut 1; (<b>d</b>) SEM-BSE of SAC-0.5ZrO<sub>2</sub>(nf); (<b>e</b>) SEM-BSE of FIB cut 2; (<b>f</b>) EDS spectra (M5–M8).</p>
Full article ">Figure 10
<p>Corrosion of the solder joints: (<b>a</b>) simple corrosion in SAC solder joints; (<b>b</b>) enhanced corrosion in SAC-0.5ZrO<sub>2</sub>(np/nf) composite solder joints.</p>
Full article ">
25 pages, 11394 KiB  
Article
Electroanalytical Studies on Codeposition of Cobalt with Ruthenium from Acid Chloride Baths
by Iwona Dobosz and Ewa Rudnik
Coatings 2024, 14(10), 1301; https://doi.org/10.3390/coatings14101301 - 11 Oct 2024
Viewed by 506
Abstract
The aim of this study was to systematically analyze the influence of potential and the Co(II)–Ru(III) molar ratio on the electrochemical behavior of the Co–Ru system during codeposition from acidic chloride electrolytes. The equilibrium speciation of the baths was investigated spectrophotometrically and compared [...] Read more.
The aim of this study was to systematically analyze the influence of potential and the Co(II)–Ru(III) molar ratio on the electrochemical behavior of the Co–Ru system during codeposition from acidic chloride electrolytes. The equilibrium speciation of the baths was investigated spectrophotometrically and compared with theoretical calculations based on the stability constants of Co(II) and Ru(III) complexes. The codeposition of the metals was characterized using electroanalytical methods, including cyclic voltammetry, chronoamperometry, and anodic stripping linear voltammetry. The alloys obtained at different potentials were analyzed for their elemental composition (EDS, mapping), phase composition (XRD), and surface morphology (SEM). The morphology and composition of the alloys were mainly dependent on the deposition potential, which controlled the cobalt incorporation. Ruthenium–rich alloys were produced at potentials of −0.6 V and −0.7 V (vs. SCE). In these conditions, cobalt anomalously codeposited due to the formation of the CoOH+ intermediate, triggered by the intense hydrogen evolution on the ruthenium sublayer. Bulk cobalt electrodeposition began at a potential of around −0.8 V, resulting in the formation of cobalt-rich alloys. The early stages of the electrodeposition were investigated using different nucleation models. A transition from 2D progressive nucleation to 3D instantaneous nucleation at around −0.8 V was identified as being caused by cobalt incorporation. This was well correlated with electroanalytical data, partial polarization curves of alloy deposition, elemental mapping analysis, and the structure of the deposits. Full article
Show Figures

Figure 1

Figure 1
<p>Structures of some Co(II) (<b>a</b>) and Ru(III) (<b>b</b>) complexes. Actual structures based on [<a href="#B27-coatings-14-01301" class="html-bibr">27</a>,<a href="#B32-coatings-14-01301" class="html-bibr">32</a>].</p>
Full article ">Figure 2
<p>UV–Vis absorption spectra of Co(II)–Ru(III) (<b>a</b>), Ru(III) (<b>b</b>), and Co(II) (<b>c</b>) acid chloride solutions. Co(II)–Ru(III) molar concentration ratio 10:1.</p>
Full article ">Figure 3
<p>Fractions of Co(II) and Ru(III) species in acid chloride solutions (3 M Cl<sup>−</sup>, pH 1): (<b>a</b>) 1 M Co(II) + 0.01 M Ru(III) and (<b>b</b>) 0.1 M Co(II) + 0.01 M Ru(III). For simplicity, water molecules are omitted in the complex formulas.</p>
Full article ">Figure 4
<p>Cyclic voltammetry curves registered in (<b>a</b>) Ru(III), (<b>b</b>) Co(II), and (<b>c</b>) Co(II)–Ru(III) acid chloride solutions: 1 M Co(II) and/or 0.01 M Ru(III).</p>
Full article ">Figure 5
<p>Cyclic voltammetry curves registered in (<b>a</b>) Ru(III), (<b>b</b>) Co(II), and (<b>c</b>) Co(II)–Ru(III) acid chloride solutions: 0.1 M Co(II) and/or 0.01 M Ru(III).</p>
Full article ">Figure 6
<p>Cyclic voltammetry curves for different switch potentials (from −0.8 V to −1.3 V) registered in Co(II)–Ru(III) acid chloride solutions with (<b>a</b>) 1 M Co(II) and (<b>b</b>) 0.1 M Co(II).</p>
Full article ">Figure 7
<p>Chronoamperometric curves registered in Co(II)–Ru(III) acid chloride solutions with (<b>a</b>) 1 M Co(II) and (<b>b</b>) 0.1 M Co(II). Lower plots show details for deposition potentials between −0.60 V and −0.85 V.</p>
Full article ">Figure 8
<p>Anodic sweep linear voltammetry curves registered in Co(II)–Ru(III) acid chloride solutions with (<b>a</b>) 1 M Co(II) and (<b>b</b>) 0.1 M Co(II).</p>
Full article ">Figure 9
<p>Anodic to cathodic charge ratios in Co(II)–Ru(III) solutions registered during cathodic accumulation step (40 s) and anodic sweep linear voltammetry.</p>
Full article ">Figure 10
<p>Schemes of nuclei formation and growth: (<b>a</b>) two-dimensional nuclei and (<b>b</b>) three-dimensional nuclei.</p>
Full article ">Figure 11
<p>Normalized i–t curves for 2D (upper) and 3D (lower) instantaneous IN and progressive PN nucleation and growth for deposition from Co(II)–Ru(III) acid chloride solutions with (<b>a</b>) 1 M Co(II) and (<b>b</b>) 0.1 M Co(II). Dashed and dotted lines represent model reference lines.</p>
Full article ">Figure 12
<p>Influence of deposition potential on metal content in deposits: (<b>a</b>) ruthenium and (<b>b</b>) cobalt.</p>
Full article ">Figure 13
<p>Influence of deposition potential on (<b>a</b>) deposit mass and (<b>b</b>) cathodic current efficiency.</p>
Full article ">Figure 14
<p>Morphology of deposits produced from 1 M Co(II)–Ru(III) bath at potentials (<b>a</b>) −0.8 V, (<b>b</b>) −1.1 V, and (<b>c</b>) −1.3 V.</p>
Full article ">Figure 15
<p>Morphology of deposits produced from 0.1 M Co(II)–Ru(III) bath at potentials (<b>a</b>) −0.6 V, (<b>b</b>) −0.7 V, (<b>c</b>) −0.8 V, (<b>d</b>) −0.9 V, (<b>e</b>) −1.0 V, (<b>f</b>) −1.1 V, and (<b>g</b>) −1.3 V.</p>
Full article ">Figure 16
<p>Distribution of elements (mapping) on surface of deposit produced from 0.1 M Co(II)–Ru(III) bath at potentials (<b>a</b>) −0.7 V, (<b>b</b>) −0.9 V, and (<b>c</b>) −1.1 V.</p>
Full article ">Figure 17
<p>X-ray diffraction patterns of deposits produced at different potentials from Co(II)–Ru(III) baths: (<b>a</b>) 0.1 M Co(II), (<b>b</b>) 1 M Co(II), and (<b>c</b>) substrates Au—glass covered with gold layer; H—aluminum holder. XRD standard cards: Co—03–065–9722, Ru—00–001–1256, and Co–Ru—01–071–7425.</p>
Full article ">Figure 18
<p>Partial polarization curves calculated for alloy deposition from the 0.1 M Co(II)–Ru(III) bath shown in two coordination systems: (<b>a</b>) E–I and (<b>b</b>) E–log I.</p>
Full article ">
18 pages, 32054 KiB  
Article
Study on the Process of Preparing Aluminum Foam Sandwich Panel Precursor by Friction Stir Welding
by Yu Zhang and Qiu Pang
Materials 2024, 17(20), 4981; https://doi.org/10.3390/ma17204981 - 11 Oct 2024
Viewed by 325
Abstract
In recent years, high-performance lightweight and multifunctional aluminum foam sandwiches (AFSs) can be successfully applied to spacecraft, automobiles, and high-speed trains. Friction stir welding (FSW) has been proposed as a new method for the preparation of AFS precursors in order to improve the [...] Read more.
In recent years, high-performance lightweight and multifunctional aluminum foam sandwiches (AFSs) can be successfully applied to spacecraft, automobiles, and high-speed trains. Friction stir welding (FSW) has been proposed as a new method for the preparation of AFS precursors in order to improve the cost-effectiveness and productivity of the preparation of AFS. In this study, the AFS precursors were prepared using the FSW process. The distribution of foaming agents in the AFS precursors and the structure and morphology of AFS were observed using optical microscopy (OM), scanning electron microscopy (SEM), and X-ray energy dispersive spectroscopy (EDS). The effects of the temperature and material flow on the distribution of the foaming agent during the FSW process were analyzed through experimental study and numerical simulation using ANSYS Fluent 19.0 software. The results show that the uniform distribution of the foaming agent in the matrix and excellent densification of AFS precursor can be prepared when the rotation speed is 1500 r/min, the travel speed is 25 mm/min, the tool plunge depth is 0.2 mm, and the tool moves along the retreating side (RS). In addition, the experimental and numerical simulations show that increasing the welding temperature improves the uniformity of foaming agent distribution and the area of AFS precursor prepared by single welding, shortening the thread length inhibits the foaming agent from reaching the upper sandwich plate and moving along the RS leads to a more uniform distribution of the foaming agent. Finally, the AFS with porosity of 74.55%, roundness of 0.97, and average pore diameter of 1.192 mm is prepared. Full article
Show Figures

Figure 1

Figure 1
<p>Schematic diagram of the process of preparing AFS by FSW.</p>
Full article ">Figure 2
<p>Geometry, boundary definition, model mesh of the numerical model.</p>
Full article ">Figure 3
<p>Comparison of the metallographic organization of AFS precursors at the travel speed of 25 mm/min and different rotation speeds: (<b>a</b>) 1000 r/min, (<b>b</b>) 1500 r/min, (<b>c</b>) 2000 r/min.</p>
Full article ">Figure 4
<p>Comparison of metallographic organization of AFS precursor at the rotation speed of 25 mm/min and different travel speeds: (<b>a</b>) 25 mm/min, (<b>b</b>) 50 mm/min, (<b>c</b>) 100 mm/min.</p>
Full article ">Figure 5
<p>Comparison of metallographic organization of AFS precursors at different tool plunge depths: (<b>a</b>) 0.05 mm, (<b>b</b>) 0.20 mm, (<b>c</b>) 0.40 mm.</p>
Full article ">Figure 6
<p>The schematic diagram of tool movement along different directions and comparison of metallography: (<b>a</b>) the metallography of AS, (<b>b</b>) the metallography of RS, (<b>c</b>) the schematic diagram of AS, (<b>d</b>) the schematic diagram of RS.</p>
Full article ">Figure 7
<p>The formability experiment of AFS precursor under different welding tracks: (<b>a</b>) true stress-strain curves at different welding track, (<b>b</b>) Erikson formability test.</p>
Full article ">Figure 8
<p>Comparison of metallographic organization of AFS precursors at different pin thread lengths: (<b>a</b>) 4.00 mm, (<b>b</b>) 4.85 mm.</p>
Full article ">Figure 9
<p>Comparison of experimentally measured and numerically calculated temperature at 1500 r/min rotational speed and 25 mm/min travel speed: (<b>a</b>) experimentally measured schematic, (<b>b</b>) experimentally measured temperature curve, (<b>c</b>) numerically calculated temperature.</p>
Full article ">Figure 10
<p>Numerical simulation of the temperature distribution on the top surface of the workpiece for different parameters: (<b>a</b>) 25 mm/min travel speed and 1000 r/min rotational speed, (<b>b</b>) 100 mm/min travel speed and 1500 r/min rotational speed, (<b>c</b>) 25 mm/min travel speed and 1500 r/min rotational speed, (<b>d</b>) 25 mm/min travel speed and 2000 r/min rotational speed.</p>
Full article ">Figure 11
<p>The SEM morphology and EDS analysis of precursors at rotational speed 1500 r/min and tool movement along RS: (<b>a</b>) the metallographic organization of travel speed 100 mm/min, (<b>b</b>) SEM image of the rectangular region in (<b>a</b>), (<b>c</b>,<b>d</b>) the EDS maps corresponding to (<b>b</b>), (<b>e</b>) the metallographic organization of travel speed 25 mm/min, (<b>f</b>) SEM image of the rectangular region in (<b>e</b>), (<b>g</b>,<b>h</b>) the EDS maps corresponding to (<b>f</b>).</p>
Full article ">Figure 12
<p>Material flow in cross-section at different locations around the pin: (<b>a</b>) the cross-section schematic at different locations around the pin, (<b>b</b>) the metallographic organization of WZ, (<b>c</b>) the weld metal flow of cross-section I, (<b>d</b>) the weld metal flow of cross-section II, (<b>e</b>) the weld metal flow of cross-section III. The red arrows represent the material flow caused by the pin, the blue arrows represent the material flow caused by the tool shoulder, the yellow arrows represent the material flow caused by the material buildup, and the purple arrow represents material flowing out of the shoulder to form weld flash.</p>
Full article ">Figure 13
<p>The SEM morphology and EDS analysis of AFS precursor welded along the AS at travel speed 25 mm/min and rotational speed 1500 r/min: (<b>a</b>) metallographic organization, (<b>b</b>) SEM image of the rectangular region in (<b>a</b>), (<b>c</b>,<b>d</b>) the EDS maps corresponding to (<b>b</b>).</p>
Full article ">Figure 14
<p>SEM morphology and EDS analysis of AFS precursor under optimal welding parameters and methods (<b>a</b>) metallic organization of the precursor; (<b>b</b>) SEM image of the rectangular region in (<b>a</b>); (<b>c</b>) enlarged image of the rectangular region in (<b>b</b>); (<b>d</b>) EDS spectra of region A in (<b>c</b>); (<b>e</b>) EDS spectra of region B in (<b>c</b>); (<b>f</b>) EDS spectra of region C in (<b>c</b>); (<b>h</b>–<b>j</b>) EDS maps corresponding to (<b>c</b>).</p>
Full article ">Figure 15
<p>The foam microstructure of AFS precursors was prepared with pins of different thread lengths at 680 °C for different foaming times: (<b>a</b>,<b>b</b>) 4.00 mm (<b>c</b>,<b>d</b>) 4.85 mm.</p>
Full article ">Figure 16
<p>The bubble hole statistics and data comparison: (<b>a</b>) schematic of the bubble being counted, (<b>b</b>) comparison of bubble porosity, circularity, and diameter. Reprinted with permission from ref. [<a href="#B44-materials-17-04981" class="html-bibr">44</a>]. Copyright 2014 Elsevier. Reprinted with permission from ref. [<a href="#B45-materials-17-04981" class="html-bibr">45</a>]. Copyright 2018 J-Stage.</p>
Full article ">
23 pages, 17209 KiB  
Article
Application of Soft Magnetic Composite in XEV Motor Core Manufacturing: Process Effects and Performance Analysis
by Seongsu Kang and Seonbong Lee
Metals 2024, 14(10), 1163; https://doi.org/10.3390/met14101163 - 11 Oct 2024
Viewed by 320
Abstract
This study explores the application of AncorLam HR (Höganäs, Sweden), a soft magnetic composite material, in the stator core of an axial flux permanent magnet drive motor. Building on previous research that provided mechanical and thermal properties of the material, the focus is [...] Read more.
This study explores the application of AncorLam HR (Höganäs, Sweden), a soft magnetic composite material, in the stator core of an axial flux permanent magnet drive motor. Building on previous research that provided mechanical and thermal properties of the material, the focus is on analyzing how the manufacturing process affects the motor core’s shape. A bulk prototype was created based on case 3, which demonstrated the least deviation in density and internal stress. The prototypes were produced under the conditions of SPM 7 and 90 °C, and a heat treatment in a nitrogen atmosphere for 1 h, resulting in an average density error of 0.54%, confirming process effectiveness. A microstructural analysis using scanning electron microscopy (SEM) on Sample 2, with the highest density, confirmed consistency between simulation and prototype trends. Electron backscatter diffraction (EBSD) and X-ray diffraction (XRD) analyses revealed that the internal phase structure remained unchanged. Energy-dispersive spectroscopy (EDS) and transmission electron microscopy (TEM) identified the elimination of phosphorus (P) during molding, affecting the insulating layer, a critical factor for SMC materials. In motor simulations and actual measurements, the average torque was recorded as 37.7 N·m and 34.7 N·m at 1500 rpm and 27.7 N·m and 25.1 N·m at 2000 rpm, respectively. The torque comparison observed in the actual measurements compared to the simulation results indicates that the output loss increases in the actual measurements due to the deterioration of the insulation performance judged based on the microstructure evaluation. This study confirms the viability of using AncorLam HR in motor cores for electric vehicles and provides key data for improving the performance. Full article
(This article belongs to the Section Powder Metallurgy)
Show Figures

Figure 1

Figure 1
<p>The flow chart of the study.</p>
Full article ">Figure 2
<p>Strain–stress curve of AncorLam HR [<a href="#B17-metals-14-01163" class="html-bibr">17</a>].</p>
Full article ">Figure 3
<p>XRD measurement result of AncorLam HR powder.</p>
Full article ">Figure 4
<p>FIB Specimen Shape: (<b>a</b>) cross-section view 1, (<b>b</b>) cross-section view 2.</p>
Full article ">Figure 5
<p>AncorLam HR powder TEM measurement results: (<b>a</b>) cross-section view 1, (<b>b</b>) cross-section view 2, (<b>c</b>) EDS results for view 1, and (<b>d</b>) EDS results for view 2.</p>
Full article ">Figure 6
<p>FEA stator core model feature: (<b>a</b>) upper view and (<b>b</b>) isotropic view.</p>
Full article ">Figure 7
<p>FEA simulation model feature: (<b>a</b>) initial feature meshing, (<b>b</b>) die, (<b>c</b>) upper and lower punch, and (<b>d</b>) assembly.</p>
Full article ">Figure 8
<p>AFPM motor shape and dimensions.</p>
Full article ">Figure 9
<p>Relative density results of DOE: cases (<b>a</b>) 1, (<b>b</b>) 2, (<b>c</b>) 3, (<b>d</b>) 4, (<b>e</b>) 5, (<b>f</b>) 6, (<b>g</b>) 7, (<b>h</b>) 8, and (<b>i</b>) 9.</p>
Full article ">Figure 10
<p>Effective stress results of DOE: cases (<b>a</b>) 1, (<b>b</b>) 2, (<b>c</b>) 3, (<b>d</b>) 4, (<b>e</b>) 5, (<b>f</b>) 6, (<b>g</b>) 7, (<b>h</b>) 8, and (<b>i</b>) 9.</p>
Full article ">Figure 11
<p>Mean stress results of DOE: cases (<b>a</b>) 1, (<b>b</b>) 2, (<b>c</b>) 3, (<b>d</b>) 4, (<b>e</b>) 5, (<b>f</b>) 6, (<b>g</b>) 7, (<b>h</b>) 8, and (<b>i</b>) 9.</p>
Full article ">Figure 12
<p>Shape of specimen for density measurement: (<b>a</b>) specimen 1, (<b>b</b>) specimen 2, and (<b>c</b>) specimen 3.</p>
Full article ">Figure 13
<p>(<b>a</b>) The relative density at three height points of the motor stator core, (<b>b</b>) the SEM of the upper point, (<b>c</b>) the SEM of the middle point, (<b>d</b>) the SEM of the lower point.</p>
Full article ">Figure 14
<p>(<b>a</b>) SEM of upper point, (<b>b</b>) Fe results among EDS results, (<b>c</b>) Si results among EDS results, (<b>d</b>) Cr results among EDS results, and (<b>e</b>) Mo results among EDS results.</p>
Full article ">Figure 15
<p>(<b>a</b>) SEM upper point, (<b>b</b>) EBSD result of IPF, and (<b>c</b>) EBSD result of phases.</p>
Full article ">Figure 16
<p>XRD measurement result of AncorLam HR bulk prototype.</p>
Full article ">Figure 17
<p>(<b>a</b>) AncorLam HR bulk prototype TEM measurement results: (<b>b</b>) Fe, O, Zn results among EDS results.</p>
Full article ">Figure 18
<p>Torque simulation result over time at 140 A conditions of 1500 rpm.</p>
Full article ">Figure 19
<p>Torque simulation result over time at 100 A conditions of 2000 rpm.</p>
Full article ">Figure 20
<p>Core loss result with frequency.</p>
Full article ">Figure 21
<p>Core loss results over time.</p>
Full article ">Figure 22
<p>Motor dynamometer test equipment feature: (<b>a</b>) dynamometer and (<b>b</b>) test setup view.</p>
Full article ">Figure 23
<p>Torque measurement result over time at 140 A conditions of 1500 rpm.</p>
Full article ">Figure 24
<p>Torque measurement result over time at 100 A conditions of 2000 rpm.</p>
Full article ">
12 pages, 5852 KiB  
Article
Development of Cost-Effective Sn-Free Al-Bi-Fe Alloys for Efficient Onboard Hydrogen Production through Al–Water Reaction
by Rui Deng, Mingshuai Wang, Hao Zhang, Ruijun Yao, Kai Zhen, Yifei Liu, Xingjun Liu and Cuiping Wang
Materials 2024, 17(20), 4973; https://doi.org/10.3390/ma17204973 - 11 Oct 2024
Viewed by 485
Abstract
Leveraging the liquid-phase immiscibility effect and phase diagram calculations, a sequence of alloy powders with varying Fe content was designed and fabricated utilizing the gas atomization method. Microstructural characterizations, employing SEM, EDS, and XRD analyses, revealed the successful formation of an incomplete shell [...] Read more.
Leveraging the liquid-phase immiscibility effect and phase diagram calculations, a sequence of alloy powders with varying Fe content was designed and fabricated utilizing the gas atomization method. Microstructural characterizations, employing SEM, EDS, and XRD analyses, revealed the successful formation of an incomplete shell on the surfaces of Al-Bi-Fe powders, obviating the need for Sn doping. This study systematically investigated the microstructure, hydrolysis performance, and hydrolysis process of these alloys in deionized water. Notably, Al-10Bi-7Fe exhibited the highest hydrogen production, reaching 961.0 NmL/g, while Al-10Bi-10Fe demonstrated the peak conversion rate at 92.99%. The hydrolysis activation energy of each Al-Bi-Fe alloy powder was calculated using the Arrhenius equation, indicating that a reduction in activation energy was achieved through Fe doping. Full article
(This article belongs to the Collection Materials and Technologies for Hydrogen and Fuel Cells)
Show Figures

Figure 1

Figure 1
<p>The schematic experimental setup for the hydrolysis test.</p>
Full article ">Figure 2
<p>(<b>a</b>) Calculated vertical phase diagrams of Al-10Bi-Fe (wt.%); (<b>b</b>–<b>d</b>) calculated phase fractions diagrams of Al-10Bi-(3, 7, 10) Fe (wt.%).</p>
Full article ">Figure 3
<p>SEM images at various magnifications of as-atomized Al-Bi-Fe alloy powders: (<b>a</b>–<b>a<sub>2</sub></b>) Al-10Bi-3Fe (wt.%); (<b>b</b>–<b>b<sub>2</sub></b>) Al-10Bi-7Fe (wt.%); and (<b>c</b>–<b>c<sub>2</sub></b>) Al-10Bi-10Fe (wt.%).</p>
Full article ">Figure 4
<p>EDS analysis of the cross-section of the Al-Bi-Fe alloy powders: (<b>a</b>) Al-10Bi-3Fe, with element distributions: (<b>a<sub>1</sub></b>) Al; (<b>a<sub>2</sub></b>) Bi; (<b>a<sub>3</sub></b>) Fe; (<b>b</b>) Al-10Bi-7Fe (wt.%), with element distributions: (<b>b<sub>1</sub></b>) Al; (<b>b<sub>2</sub></b>) Bi; (<b>b<sub>3</sub></b>) Fe; (<b>c</b>) Al-10Bi-10Fe (wt.%), with element distributions: (<b>c<sub>1</sub></b>) Al; (<b>c<sub>2</sub></b>) Bi; (<b>c<sub>3</sub></b>) Fe.</p>
Full article ">Figure 5
<p>XRD patterns of the as-atomized Al-Bi-Fe alloy powders (<b>a</b>) separated XRD patterns; (<b>b</b>) stacked patterns focusing on the Al (111) peak.</p>
Full article ">Figure 6
<p>Charts of the hydrolysis of Al-Bi-Fe variations using deionized water at different reaction temperatures ranging from 30 to 50 °C: (<b>a</b>) the hydrogen yield vs. time curve; (<b>b</b>) the conversion rate.</p>
Full article ">Figure 7
<p>Cost and hydrolysis performance for various active Al alloys: (1) red area indicates Ga, In, Sn doping alloys; (2) yellow area indicates Ga, In-free alloys; and (3) green area indicates Sn-free alloys. The data are drawn from references [<a href="#B23-materials-17-04973" class="html-bibr">23</a>,<a href="#B24-materials-17-04973" class="html-bibr">24</a>,<a href="#B26-materials-17-04973" class="html-bibr">26</a>,<a href="#B27-materials-17-04973" class="html-bibr">27</a>,<a href="#B29-materials-17-04973" class="html-bibr">29</a>,<a href="#B30-materials-17-04973" class="html-bibr">30</a>].</p>
Full article ">Figure 8
<p>Plots of the hydrolysis of the Al-Bi-Fe variations using deionized water at different reaction temperatures ranging from 30 to 50 °C (<b>a</b>) hydrogen yield rates vs. time curves, (<b>b</b>) the Arrhenius plots.</p>
Full article ">Figure 9
<p>SEM images of the hydrolysis products of Al-Bi-Fe variations using deionized water at different reaction temperatures ranging from 30 to 50 °C.</p>
Full article ">Figure 10
<p>The morphological changes on the surface of Al-Bi-Fe alloy powders at different stages of the hydrolysis process, along with a schematic representation of the reaction mechanism.</p>
Full article ">
22 pages, 6834 KiB  
Article
Tomographic and Electron Microscopy Description of Two Bone-Substitute Xenografts for the Preservation of Dental Alveoli
by Lemy Vanessa Barba-Rosado, Maria-Fernanda Realpe, Carlos-Humberto Valencia-Llano, Diego López-Tenorio, Ismael Enrique Piñeres-Ariza and Carlos David Grande-Tovar
Int. J. Mol. Sci. 2024, 25(20), 10942; https://doi.org/10.3390/ijms252010942 - 11 Oct 2024
Viewed by 377
Abstract
After tooth extraction, bone levels in the alveoli decrease. Using a bone substitute can help minimize this bone loss. The substitute can be sourced from a human or animal donor or synthetically prepared. In this study, we aimed to address the following PICOS [...] Read more.
After tooth extraction, bone levels in the alveoli decrease. Using a bone substitute can help minimize this bone loss. The substitute can be sourced from a human or animal donor or synthetically prepared. In this study, we aimed to address the following PICOS question: In patients needing dental alveolar preservation for implant placement, how does alveolar preservation using a bovine hydroxyapatite bone xenograft with collagen compare to a xenograft without collagen in terms of changes in alveolar height and width, bone density, and the characteristics of the bone tissue observed in biopsies taken at 6 months? We evaluated two xenograft-type bone substitutes for preserving post-extraction dental sockets using tomography and microscopy to answer that question. A total of 18 dental alveoli were studied: 11 preserved with a xenograft composed of apatite (InterOss) and 7 with a xenograft composed of apatite–collagen (InterOss Collagen). Tomographic controls were performed at 1 and 6 months, and microscopic studies were performed on 13 samples. The biopsies were examined with scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS). A Multivariate Analysis of Variance (MANOVA) was conducted in the statistical analysis, revealing a significant increase in bone density over time (p = 0.04). Specifically, bone density increased from an average of 526.14 HU at 30 days to 721.96 HU at 60 days in collagen-free samples. However, no statistically significant differences in height or width were found between groups. The MANOVA results indicated that the overall model had a low predictive ability for height, width, and density variables (R-squared values were low), likely due to sample size limitations and the complexity of bone tissue dynamics. On the other hand, FTIR analysis revealed the presence of phosphate groups, carbonates, and amides I, II, and III, indicative of inorganic (hydroxyapatite) and organic (type I collagen) materials in the xenografts. TGA and DSC showed high thermal stability, with minimal mass loss below 150 °C. Finally, both xenografts were influential in alveolar bone regeneration after extraction without significant differences. The trend of increasing collagen density suggests an effect that requires further investigation. However, it is recommended that the sample size be increased to enhance the validity of the results. Full article
(This article belongs to the Section Materials Science)
Show Figures

Figure 1

Figure 1
<p>Surgical procedure to preserve the dental socket. (<b>A</b>) Post-extraction alveolus area. (<b>B</b>) Xenograft placement in the dental socket. (<b>C</b>) Placement of the barrier (membrane) protecting the graft. (<b>D</b>) Repositioned soft tissues in the grafted area. White oval: Area of the dental socket. Yellow arrow: An area of bone loss on the vestibular surface of the bony ridge. Yellow star: Mucous tissue on the vestibular surface of the bony ridge. Blue arrow: Socket grafted with xenograft material. Green arrow: Collagen membrane in position. White circles: Areas of suture of the tissues.</p>
Full article ">Figure 2
<p>Tomographic images of grafted alveoli in cross-sections. Yellow arrow: The vestibular surface of the ridge. Blue arrow: The palatal surface of the flange. <b>1</b>: Area of the alveolus made up of remnant or native bone. <b>2:</b> Area of the socket where the graft was placed. Blue stars: Radiopaque appearance zone. Yellow star: Area of radiolucent appearance. White circle: Grafted area of the alveolus. (<b>A</b>) Alveolus grafted with apatite–collagen at 1 month. (<b>B</b>) Alveolus grafted with apatite–collagen at 1 month. (<b>C</b>) Alveolus grafted with apatite at 1 month. (<b>D</b>) Alveolus grafted with apatite at 6 months.</p>
Full article ">Figure 3
<p>Taking the biopsy. (<b>A</b>) Trephine drill bit with a bone fragment inside. (<b>B</b>) Area of the ridge where the biopsy was taken. White oval: Trephine drill bit. Red arrow: Bone biopsy inside the trephine. White circle: Bone rim. Purple arrow: A remnant cavity where the biopsy was taken.</p>
Full article ">Figure 4
<p>FTIR spectra of apatite (black line) and apatite–collagen (red line).</p>
Full article ">Figure 5
<p>TGA and DTG of apatite and apatite–collagen: (<b>A</b>) TGA and DTG of apatite; (<b>B</b>) TGA and DTG of apatite–collagen.</p>
Full article ">Figure 6
<p>DSC thermograms for apatite (black line) and apatite–collagen (red line).</p>
Full article ">Figure 7
<p>Sample of dental alveoli grafted with apatite material, 6 months after implantation. SEM. Yellow arrows: Osteoblast-like cells. Blue arrows: Deposits of extracellular bone matrix. White circle: Area of histological interest.</p>
Full article ">Figure 8
<p>Sample of dental alveoli grafted with apatite material, 6 months after implantation. SEM technique/EDS technique. (<b>A</b>) Image of a cross-section of the biopsy. (<b>B</b>,<b>C</b>) Biopsy surface in cross section with extracellular matrix deposition. (<b>D</b>–<b>F</b>) Image of a longitudinal section of another biopsy with osteoblast-like cells. (<b>G</b>) Spectral analysis of the section shown in (<b>E</b>). (<b>H</b>) Spectral analysis of the section shown in (<b>F</b>)<b>.</b> Red circle: Cavity inside the sample. Yellow arrows: Osteoblast-like cells. Blue arrows: Deposits of extracellular bone matrix. Red arrows: Resorption lagoons. White circles: Areas of histological interest. Spectrum 1 to 5: Analysis zones. C: Carbon. O: Oxygen. P: Phosphorus. Ca: Calcium.</p>
Full article ">Figure 9
<p>Sample of dental socket grafted with apatite–collagen. SEM technique/SEM technique. (<b>A</b>) SEM technique. (<b>B</b>) SEM technique. (<b>C</b>) SEM technique. (<b>D</b>) SEM technique. (<b>E</b>) SEM technique (<b>F</b>) SEM technique. (<b>G</b>) Spectral analysis of sample F, using the EDS technique. (<b>H</b>) Spectral analysis of sample F, using the EDS technique. Yellow arrows: Osteoblast-like cells. Blue arrows: Deposits of extracellular bone matrix. Red arrows: Resorption lagoons. Purple arrows: Remnant fragments of grafted material. Spectrum 1 to 4: Analysis zones. C: Carbon. O: Oxygen. P: Phosphorus. Ca: Calcium.</p>
Full article ">
11 pages, 10750 KiB  
Article
Effect of Tempering Temperature on the Aqueous Corrosion Resistance of 9Cr Series Heat-Resistant Steel
by Hui Li and Hao Bai
Materials 2024, 17(20), 4960; https://doi.org/10.3390/ma17204960 - 11 Oct 2024
Viewed by 558
Abstract
In this investigation, the aqueous corrosion resistance of 9Cr series heat-resistant steel during tempering was investigated. Optical Microscopy (OM), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectrometer (EDS) were used to analyze the effect of tempering temperature on the microstructure and precipitation behavior [...] Read more.
In this investigation, the aqueous corrosion resistance of 9Cr series heat-resistant steel during tempering was investigated. Optical Microscopy (OM), Scanning Electron Microscopy (SEM), and Energy Dispersive Spectrometer (EDS) were used to analyze the effect of tempering temperature on the microstructure and precipitation behavior of precipitates. The heat-resisting steel was heated to 1150 °C for 1 h, and then tempered at different temperatures between 680 °C and 760 °C for 2 h. The microstructure of the heat-resistant steel after tempering was composed of lath-tempered martensite and fine precipitates. The hardness decreased with increasing tempering temperature, ranging from HBW 261 to HBW 193. The aqueous corrosion resistance improved as the tempering temperatures increased from 680 °C to 720 °C but deteriorated at higher temperatures, such as 760 °C, which was obtained by an electrochemical corrosion performance test. The aqueous corrosion resistance was affected by the decrease in dislocation density and the decrease in Cr solution in the tempered martensite. With the increase in the tempering temperature, the aqueous corrosion potential first increases and then decreases, the self-corrosion current density first decreases and then increases, and the polarization resistance first increases and then decreases. Furthermore, the increase in corrosion resistance is attributed to the reduction in dislocation density and chromium depletion in the martensitic structure as the tempering temperature approaches 720 °C. This paper reveals the effect of tempering temperature on the corrosion resistance of 9Cr series heat-resistant steel, which is a further exploration of a known phenomenon. Full article
Show Figures

Figure 1

Figure 1
<p>SEM image of heat-resistant steel before tempering. (<b>a</b>) SEM; (<b>b</b>) EDS.</p>
Full article ">Figure 2
<p>OM image after different tempering temperatures of heat-resistant steel: (<b>a</b>) 680 °C; (<b>b</b>) 700 °C; (<b>c</b>) 720 °C; (<b>d</b>) 740 °C; (<b>e</b>) 760 °C.</p>
Full article ">Figure 3
<p>SEM image of heat-resistant steel after tempering at different temperatures (<b>a</b>) 680 °C; (<b>b</b>) 700 °C; (<b>c</b>) 720 °C; (<b>d</b>) 740 °C; (<b>e</b>) 760 °C; (<b>f</b>) EDS.</p>
Full article ">Figure 4
<p>Hardness of heat-resistant steel after different tempering.</p>
Full article ">Figure 5
<p>Polarization curve diagram of heat-resistant steel after different tempering.</p>
Full article ">Figure 6
<p>Impedance diagram of heat-resistant steel after treatment with different tempering.</p>
Full article ">Figure 7
<p>Macro image of heat-resistant steel samples after 30 days.</p>
Full article ">Figure 8
<p>SEM image of heat-resistant steel surface after neutral salt spray aqueous corrosion: (<b>a</b>) day 10; (<b>b</b>) day 20; (<b>c</b>) day 30; (<b>d</b>) EDS.</p>
Full article ">Figure 9
<p>Effect of the tempering temperature on the precipitate and element content in the heat-resistant steel: (<b>a</b>) the amount of precipitates; (<b>b</b>) the solid solution amount of Cr; (<b>c</b>) the amount of C precipitation; (<b>d</b>) the average size of the precipitates.</p>
Full article ">
23 pages, 16247 KiB  
Article
Sol–Gel Derived Alumina Particles for the Reinforcement of Copper Films on Brass Substrates
by Samah Sasi Maoloud Mohamed, Marija M. Vuksanović, Dana G. Vasiljević-Radović, Ljiljana Janković Mandić, Radmila M. Jančić Heinneman, Aleksandar D. Marinković and Ivana O. Mladenović
Gels 2024, 10(10), 648; https://doi.org/10.3390/gels10100648 - 11 Oct 2024
Viewed by 515
Abstract
The aim of this study is to provide tailored alumina particles suitable for reinforcing the metal matrix film. The sol–gel method was chosen to prepare particles of submicron size and to control crystal structure by calcination. In this study, copper-based metal matrix composite [...] Read more.
The aim of this study is to provide tailored alumina particles suitable for reinforcing the metal matrix film. The sol–gel method was chosen to prepare particles of submicron size and to control crystal structure by calcination. In this study, copper-based metal matrix composite (MMC) films are developed on brass substrates with different electrodeposition times and alumina concentrations. Scanning electron microscopy (FE-SEM) with energy-dispersive spectroscopy (EDS), TEM, and X-ray diffraction (XRD) were used to characterize the reinforcing phase. The MMC Cu-Al2O3 films were synthesized electrochemically using the co-electrodeposition method. Microstructural and topographical analyses of pure (alumina-free) Cu films and the Cu films with incorporated Al2O3 particles were performed using FE-SEM/EDS and AFM, respectively. Hardness and adhesion resistance were investigated using the Vickers microindentation test and evaluated by applying the Chen–Gao (C-G) mathematical model. The sessile drop method was used for measuring contact angles for water. The microhardness and adhesion of the MMC Cu-Al2O3 films are improved when Al2O3 is added. The concentration of alumina particles in the electrolyte correlates with an increase in absolute film hardness in the way that 1.0 wt.% of alumina in electrolytes results in a 9.96% increase compared to the pure copper film, and the improvement is maximal in the film obtained from electrolytes containing 3.0 wt.% alumina giving the film 2.128 GPa, a 134% hardness value of that of the pure copper film. The surface roughness of the MMC film increased from 2.8 to 6.9 times compared to the Cu film without particles. The decrease in the water contact angle of Cu films with incorporated alumina particles relative to the pure Cu films was from 84.94° to 58.78°. Full article
Show Figures

Graphical abstract

Graphical abstract
Full article ">Figure 1
<p>Particle morphology of alumina: (<b>a</b>) FE-SEM picture, (<b>b</b>) diameter size, (<b>c</b>) TEM micrographs, and (<b>d</b>) corresponding histogram of particles.</p>
Full article ">Figure 1 Cont.
<p>Particle morphology of alumina: (<b>a</b>) FE-SEM picture, (<b>b</b>) diameter size, (<b>c</b>) TEM micrographs, and (<b>d</b>) corresponding histogram of particles.</p>
Full article ">Figure 2
<p>(<b>a</b>) SEM images of alumina particles, (<b>b</b>) elemental mapping, (<b>c</b>) Al, (<b>d</b>) O, and (<b>e</b>) EDS spectra.</p>
Full article ">Figure 3
<p>X-ray diffractogram of alumina powder obtained by sol–gel method.</p>
Full article ">Figure 4
<p>The three-dimensional (3D) images of the brass substrate obtained on an AFM device: (<b>a</b>) brass surface after mechanical grinding and (<b>b</b>) after chemical etchings in a mixture of acids (HNO<sub>3</sub>:H<sub>3</sub>PO<sub>4</sub>:CH<sub>3</sub>COOH = 4:11:5 vol.%) at 10 s.</p>
Full article ">Figure 5
<p>Mechanical properties of brass substrate after chemical etching: (<b>a</b>) calculation of Meyer’s index and evaluation ISE, and (<b>b</b>) calculation hardness of substrate with application PSR model.</p>
Full article ">Figure 6
<p>Surface morphology analyses of electrodeposited alumina-free Cu and MMC Cu-Al<sub>2</sub>O<sub>3</sub> films electrodeposited/co-electrodeposited on the brass substrate with/without constant wt.% of alumina particles (1.0 wt.%) and with different thicknesses of the films: (<b>a</b>) 2 μm, Cu; (<b>b</b>) 2 μm, Cu-Al<sub>2</sub>O<sub>3</sub>; (<b>c</b>) 22 μm, Cu; (<b>d</b>) 22 μm, Cu-Al<sub>2</sub>O<sub>3</sub>; (<b>e</b>) 52 μm, Cu; and (<b>f</b>) 52 μm, Cu-Al<sub>2</sub>O<sub>3</sub>. The magnification was ×10,000 for all pictures.</p>
Full article ">Figure 6 Cont.
<p>Surface morphology analyses of electrodeposited alumina-free Cu and MMC Cu-Al<sub>2</sub>O<sub>3</sub> films electrodeposited/co-electrodeposited on the brass substrate with/without constant wt.% of alumina particles (1.0 wt.%) and with different thicknesses of the films: (<b>a</b>) 2 μm, Cu; (<b>b</b>) 2 μm, Cu-Al<sub>2</sub>O<sub>3</sub>; (<b>c</b>) 22 μm, Cu; (<b>d</b>) 22 μm, Cu-Al<sub>2</sub>O<sub>3</sub>; (<b>e</b>) 52 μm, Cu; and (<b>f</b>) 52 μm, Cu-Al<sub>2</sub>O<sub>3</sub>. The magnification was ×10,000 for all pictures.</p>
Full article ">Figure 7
<p>Element mapping of films: (<b>a</b>) alumina-free Cu film and (<b>b</b>) 5.0 wt.% of alumina particles. Film thickness was 22 μm.</p>
Full article ">Figure 8
<p>Element mapping of the Cu-Al<sub>2</sub>O<sub>3</sub> films co-electrodeposited with a constant concentration of alumina powder (1.0 wt.%) in electrolytes with film thickness variation: (<b>a</b>) 2 μm and (<b>b</b>) 52 μm alumina powder.</p>
Full article ">Figure 8 Cont.
<p>Element mapping of the Cu-Al<sub>2</sub>O<sub>3</sub> films co-electrodeposited with a constant concentration of alumina powder (1.0 wt.%) in electrolytes with film thickness variation: (<b>a</b>) 2 μm and (<b>b</b>) 52 μm alumina powder.</p>
Full article ">Figure 9
<p>The 3D AFM images of all deposition Cu and Cu-Al<sub>2</sub>O<sub>3</sub> films: (<b>a</b>) 2 μm Cu; (<b>b</b>) 2 μm Cu-Al<sub>2</sub>O<sub>3</sub>—1 wt.%; (<b>c</b>) 22 μm Cu; (<b>d</b>) 22 μm Cu-Al<sub>2</sub>O<sub>3</sub>—1 wt.%; (<b>e</b>) 52 μm Cu; (<b>f</b>) 52 μm Cu-Al<sub>2</sub>O<sub>3</sub>—1 wt.%; (<b>g</b>) 2 μm Cu-Al<sub>2</sub>O<sub>3</sub>—3%; and (<b>h</b>) 22 μm Cu-Al<sub>2</sub>O<sub>3</sub>—5 wt.%. The scan size was 50 × 50 μm<sup>2</sup>.</p>
Full article ">Figure 10
<p>The microhardness analysis of Cu (normal line) and Cu-Al<sub>2</sub>O<sub>3</sub> (dash line) MMC films applied to the C-G model: (<b>a</b>) with variations in the thickness of the films, (<b>b</b>) variations in the concentration of alumina particles in the suspension, and histograms with calculated values of an absolute hardness of the films (<b>c</b>) with different thicknesses, and (<b>d</b>) with 22 µm thickness and different concentrations of alumina particles.</p>
Full article ">Figure 11
<p>Adhesion properties of the films without/with reinforced alumina. Values of the adhesion parameter, called “critical reduced depth” for Cu (normal line) and Cu-Al<sub>2</sub>O<sub>3</sub> (dashed line) are also given.</p>
Full article ">Figure 12
<p>The values of static contact angles measured on the surface of Cu and Cu-Al<sub>2</sub>O<sub>3</sub> composite films: (<b>a</b>) with varying thicknesses and 1 wt.% of alumina particles, (<b>b</b>) with variations in the concentration of alumina particles in ABSEs, (<b>c</b>) with the appearance of a water droplet on a particle-free copper film, and (<b>d</b>) with 5.0 wt.% of alumina particles.</p>
Full article ">
13 pages, 4386 KiB  
Article
Reductive Sequestration of Chromate with Pyrite-Loaded nZVI@biochar Composites
by Min Sun, Yuechuan Feng, Yao Zhao and Xingrun Wang
Water 2024, 16(20), 2883; https://doi.org/10.3390/w16202883 - 10 Oct 2024
Viewed by 490
Abstract
Various green materials like biochar and Fe0 (nano-scale zerovalent iron, nZVI) have been applied to remediate aqueous Cr(VI) contamination, but few studies have tried to further improve the performance of nZVI and/or biochar composites with different sulfidation methods. Here, we modified a [...] Read more.
Various green materials like biochar and Fe0 (nano-scale zerovalent iron, nZVI) have been applied to remediate aqueous Cr(VI) contamination, but few studies have tried to further improve the performance of nZVI and/or biochar composites with different sulfidation methods. Here, we modified a hybrid material of nZVI@biochar with Na2S and pyrite (FeS2), applied it to remove aqueous Cr(VI) under different experimental conditions, and revealed key factors influencing Cr(VI) removal performance. The results show that pyrite loading is an effective sulfidation method to increase the Fe and S contents in composites. FeSx-nZVI@BC (1:1) had a Cr(VI) removal efficiency of ~95% with 5 mg/L Cr(VI) loaded, which was much higher than other hybrid composites. The Cr(VI) removal efficiency of FeSx-nZVI@BC showed a decreasing trend under pH conditions that increased from pH 3 to pH 9. The presence of dissolved oxygen and aqueous Cu2+ and Cd2+ could significantly suppress the removal of aqueous Cr(VI), while humic acids at different concentrations did not suppress Cr(VI) removal. After the reaction, it was observed with an energy-dispersive spectrometer (SEM-EDS) that most Cr in the solid phase was closely associated with pyrite minerals. X-ray photoelectron spectroscopy (XPS) spectra, together with the Fe2+-quenching method, confirmed that Fe (Fe2+ or Fe0) acted as the main electron donor, contributing to ~90% of the Cr(VI) reduction. Our study indicates that pyrite loading could further improve the performance of remediation materials and that the pyrite-loaded nZVI@BC composite is a green material with strong potential to be applied in the remediation of water contaminated by Cr(VI). Full article
(This article belongs to the Section Wastewater Treatment and Reuse)
17 pages, 5545 KiB  
Article
Effects of Samarium Doping on the Dielectric Properties of BaBi2Nb2O9 Aurivillius Ceramics
by Michał Rerak, Jolanta Makowska, Tomasz Goryczka, Beata Wodecka-Duś, Katarzyna Osińska, Grzegorz Tytko and Małgorzata Adamczyk-Habrajska
Materials 2024, 17(20), 4952; https://doi.org/10.3390/ma17204952 - 10 Oct 2024
Viewed by 436
Abstract
This study investigates the influence of samarium (Sm3+) doping on the structural, microstructural, mechanical, and dielectric properties of BaBi2Nb2O9 (BBN) ceramics. Using the solid-state reaction method, samples of BaBi2-xSmxNb2O9 [...] Read more.
This study investigates the influence of samarium (Sm3+) doping on the structural, microstructural, mechanical, and dielectric properties of BaBi2Nb2O9 (BBN) ceramics. Using the solid-state reaction method, samples of BaBi2-xSmxNb2O9 with varying concentrations of Sm (x = 0.01; 0.02; 0.04; 0.06; 0.08; 0.1) were prepared. Thermal analysis, microstructure characterization via SEM and EDS, X-ray diffraction, mechanical testing, and dielectric measurements were conducted. The results revealed that increasing Sm3+ concentration led to the formation of single-phase materials with a tetragonal structure at room temperature. Mechanical properties, such as Young’s modulus and stiffness, improved with Sm doping, indicating stronger atomic bonding. Dielectric properties showed that low concentrations of Sm3+ slightly increased electrical permittivity, while higher concentrations reduced it. The presence of Sm3⁺ also affected the relaxor properties, evidenced by changes in the freezing temperature and activation energy. Overall, the study concludes that samarium doping enhances the structural and functional properties of BBN ceramics, making them promising candidates for high-temperature piezoelectric and dielectric applications. The findings provide valuable insights into tailoring ceramic materials for advanced technological applications. Full article
(This article belongs to the Special Issue Properties of Ceramic Composites)
Show Figures

Figure 1

Figure 1
<p>Results of thermal analysis of stoichiometric substrate mixture BaCO<sub>3</sub>+(1−x)Bi<sub>2</sub>O<sub>3</sub>+Nb<sub>2</sub>O<sub>5</sub>+<span class="html-italic">x</span>/2Sm<sub>2</sub>O<sub>3</sub> of BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> material doped with Sm<sup>3+</sup> ions. (<b>a</b>) DTA—differential thermal analysis, (<b>b</b>) DTG—derivative thermogravimetry, (<b>c</b>) TG—thermogravimetric analysis.</p>
Full article ">Figure 2
<p>Graphical examples of the Rietveld refinement done for BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> ceramics doped with Sm<sup>3+</sup> ions.</p>
Full article ">Figure 3
<p>SEM image of BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> ceramics doped with Sm<sup>3+</sup> at concentrations of <span class="html-italic">x</span> = 0, <span class="html-italic">x</span> = 0.02, <span class="html-italic">x</span> = 0.06, and <span class="html-italic">x</span> = 0.1, magnified 15,000×. Next to it are grain size distribution diagrams.</p>
Full article ">Figure 4
<p>EDS spectrum of BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> ceramics doped with Sm<sup>3+</sup> ions.</p>
Full article ">Figure 5
<p>Temperature dependence of the real part of electric permittivity, with BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> ceramics modified with Sm<sup>3+</sup> ions obtained for a measuring field frequency equal to 100 kHz.</p>
Full article ">Figure 6
<p>The temperature dependence of the inverse of the real part of the electrical permittivity determined for the cooling process in a measurement field with a frequency of f = 100 kHz for the BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> ceramic modified with samarium ions for concentrations of x = 0.04.</p>
Full article ">Figure 7
<p>Dependence of the temperature <span class="html-italic">T</span><sub>dev</sub> (starting from which the classical Curie–Weiss law is applied) on the concentration of samarium admixture.</p>
Full article ">Figure 8
<p>Graph of the dependence of ln (1/<span class="html-italic">ε</span> − 1/<span class="html-italic">ε<sub>max</sub></span>) as a function of ln (<span class="html-italic">T</span> − <span class="html-italic">T</span><sub>m</sub>)) for BBN ceramics doped with samarium in the amount of <span class="html-italic">x</span> = 0.04.</p>
Full article ">Figure 9
<p>Temperature dependence. The real part of the electric permittivity component of BaBi<sub>2</sub>Nb<sub>2</sub>O<sub>9</sub> ceramics doped with Sr<sup>3+</sup> ions for the measurement field in the range f = 0.1 kHz–1 MHz (The arrow in the figures shows the direction of increasing frequency of the measurement field).</p>
Full article ">Figure 10
<p>An exemplary dependence of <span class="html-italic">f</span>(<span class="html-italic">T</span><sub>m</sub>) obtained for BBN ceramic doped with samarium at a concentration of x = 0.04. The red line indicates the fitting to the Vogel–Fulcher equation.</p>
Full article ">Figure 11
<p>Dependence of the freezing temperature <span class="html-italic">T</span><sub>f</sub> and the activation energy <span class="html-italic">E</span><sub>a</sub> on the concentration of samarium admixture.</p>
Full article ">
Back to TopTop