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16 pages, 18440 KiB  
Article
Microstructural Evolution and Mechanical Properties of Extruded AZ80 Magnesium Alloy during Room Temperature Multidirectional Forging Based on Twin Deformation Mode
by Rou Wang, Fafa Yan, Jiaqi Sun, Wenfang Xing and Shuchang Li
Materials 2024, 17(20), 5055; https://doi.org/10.3390/ma17205055 - 16 Oct 2024
Abstract
This study investigates the preparation of ultrahigh-strength AZ80 magnesium alloy bulks using room temperature multidirectional forging (MDF) at different strain rates. The focus is on elucidating the effects of multidirectional loading and strain rates on grain refinement and the subsequent impact on the [...] Read more.
This study investigates the preparation of ultrahigh-strength AZ80 magnesium alloy bulks using room temperature multidirectional forging (MDF) at different strain rates. The focus is on elucidating the effects of multidirectional loading and strain rates on grain refinement and the subsequent impact on the mechanical properties of the AZ80 alloy. Unlike hot deformation, the alloy subjected to room temperature MDF exhibits a lamellar twinned structure with multi-scale interactions. The key to achieving effective room temperature MDF of the alloy lies in combining multidirectional loading with small forging strains per pass (6%). This approach not only maximizes the activation of twinning to accommodate deformation but ensures sufficient grain refinement. Microstructural analysis reveals that the evolution of the grain structure in the alloy during deformation results from the competition between {101¯2} twinning or twinning variant interactions and detwinning. Increasing the forging rate effectively activates more twin variants, and additional deformation passes significantly enhance twin interaction levels and dislocation density. Furthermore, at a higher strain rate, more pronounced dislocation accumulation facilitates the transformation of twin structures into high-angle grain boundaries, promoting texture dispersion and suppressing detwinning. The primary strengthening mechanisms in room temperature MDF samples are grain refinement and dislocation strengthening. While increased dislocation density raises yield strength, it reduces post-yield work hardening capacity. After two passes of MDF at a higher strain rate, the alloy achieves an optimal balance of strength and ductility, with a tensile strength of 462 MPa and an elongation of 5.1%, significantly outperforming hot-deformed magnesium alloys. Full article
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Figure 1

Figure 1
<p>Schematic diagram of the MDF process (where ED represents the extrusion direction of the extruded bar, while TD and RD represent the transverse directions).</p>
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<p>(<b>a</b>) The IPF coloring map, (<b>b</b>) texture, and (<b>c</b>) XRD pattern of as-extruded AZ80 Mg alloy after ST.</p>
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<p>Microstructures and grain size distributions of AZ80 Mg alloy processed at room temperature MDF with different parameters.</p>
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<p>GB characteristics are highlighted with inserted GB rotation axis distribution and corresponding misorientation angle distributions of AZ80 Mg alloy processed at room temperature MDF with different parameters.</p>
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<p>Texture characteristics of room temperature MDF samples with different parameters.</p>
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<p>KAM maps and distribution histograms of room temperature MDF samples with different parameters. (<b>a</b>–<b>c</b>) Group 1, 0.006 s<sup>−1</sup> and (<b>d</b>–<b>f</b>) Group 2, 0.06 s<sup>−1</sup>.</p>
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<p>XRD patterns of room temperature MDF samples under different parameters (1: Group 1, 0.006 s<sup>−1</sup>, 2: Group 2, 0.06 s<sup>−1</sup>).</p>
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<p>The microstructural evolution characteristics of typical grains in the A1–A4 regions of <a href="#materials-17-05055-f003" class="html-fig">Figure 3</a>. (<b>a</b>,<b>e</b>,<b>i</b>,<b>m</b>) IPF coloring maps, (<b>b</b>,<b>f</b>,<b>j</b>,<b>n</b>) GB maps, (<b>c</b>,<b>g</b>,<b>k</b>,<b>o</b>) KAM maps, and (<b>d</b>,<b>h</b>,<b>l</b>,<b>p</b>) discrete (0001) PFs.</p>
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<p>Engineering stress–strain curves of AZ80 alloys under different MDF parameters at room temperature (1: Group 1, 0.006 s<sup>−1</sup>, 2: Group 2, 0.06 s<sup>−1</sup>).</p>
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<p>Comparison of mechanical properties of samples prepared in this study with some typical thermomechanically processed AZ80 or AZ91 Mg alloys [<a href="#B22-materials-17-05055" class="html-bibr">22</a>,<a href="#B23-materials-17-05055" class="html-bibr">23</a>,<a href="#B24-materials-17-05055" class="html-bibr">24</a>,<a href="#B25-materials-17-05055" class="html-bibr">25</a>,<a href="#B26-materials-17-05055" class="html-bibr">26</a>].</p>
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<p>Comparison of SF for basal &lt;a&gt; slip when ED loading of AZ80 alloy samples after different room temperature MDF processes and ST.</p>
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18 pages, 2818 KiB  
Article
Study on the Changes in the Microbial Community in Rhizosphere Soil of Blueberry Plants at Different Growth Stages
by Jinying Li, Xuanrong Wu, Xiongxiong Lu, Dekang Hou, Haiguang Liu, Ying Wang and Lin Wu
Agronomy 2024, 14(10), 2393; https://doi.org/10.3390/agronomy14102393 - 16 Oct 2024
Abstract
In order to clarify the relationship between mineral nutrients and rhizosphere microorganisms at different growth and development stages of blueberry (Vaccinium spp.), this work studied the dynamic changes in element content and microbial quantity in different parts of blueberry plants. The test [...] Read more.
In order to clarify the relationship between mineral nutrients and rhizosphere microorganisms at different growth and development stages of blueberry (Vaccinium spp.), this work studied the dynamic changes in element content and microbial quantity in different parts of blueberry plants. The test material was a 12-year-old half-highbush blueberry variety (‘Beilu’). The changes in the mineral nutrient elements in leaves, branches and the soil of blueberry plants were studied at the full bloom stage (T1), green fruit stage (T2), mature stage (T3) and late mature stage (T4), and the correlations of the average contents of mineral elements in the four periods were studied. The bacterial community in the rhizosphere soil was determined and analyzed using 16S rRNA high-throughput sequencing technology. The results showed that the changes in other mineral elements in various parts of blueberry plants varied in different periods. Nitrogen (N) showed a downward trend in branches, leaves and soil, especially in leaves (p < 0.05). The N contents in T2, T3 and T4 decreased by 9.9%, 26.4% and 29.9%, respectively. The N contents in the leaves and branches showed a downward trend at different growth stages, especially in leaves. The phosphorus (P) content in leaves showed a trend of increasing first and then decreasing, while it continued to increase in branches. The content of potassium (K) in leaves changed significantly, where it increased first and then decreased. The content of calcium (Ca) in leaves decreased first and then increased, while the content of magnesium (Mg) in branches and leaves decreased first and then increased, and the relative change was significant. The contents of iron (Fe) and zinc (Zn) in leaves decreased first and then increased, while the contents of manganese (Mn) and copper (Cu) were relatively stable. Cu decreased first and then increased in leaves and soil, and it increased first and then decreased in branches. The mineral nutrients in different growth stages of blueberry showed significant correlation in leaves, branches and soil. Mn in leaves was significantly positively correlated with P, Ca, Mg, Mn, Cu and Zn in soil (p < 0.01). Nitrogen and calcium in leaves were significantly correlated with manganese and phosphorus in soil, respectively. Ca in branches was significantly positively correlated with N and K in soil and was significantly positively correlated with Zn in soil (p < 0.01). Magnesium was significantly negatively correlated with iron in soil. The bacterial community structure of the blueberry rhizosphere soil changed significantly over time (p < 0.05), and the relative abundance showed the following trend: T4 > T2 > T3 > T1. At the phylum level, Proteobacteria, Acidobacteria, Actinobacteria, Chloroflexi and Verrucomicrobia were the dominant bacteria in different periods. Candidatus solibacter and Bryobacter were significantly higher in T1 and T3 than in T1 and T4. Bradyrhizobium flora increased significantly at T3. Sphingomonas increased significantly at T1 (p < 0.05). Full article
(This article belongs to the Section Horticultural and Floricultural Crops)
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Figure 1

Figure 1
<p>Mineral element contents in different parts of blueberry plants at different growth stages. T1. full bloom stage; T2. green fruit stage; T3. mature stage; T4. late mature stage. (<b>A</b>): The total N contents of leaves, branches and rhizosphere soil; (<b>B</b>): total P contents in leaves, branches and rhizosphere soil; (<b>C</b>): total K contents of leaves, branches and rhizosphere soil; (<b>D</b>): total Ca contents in leaves and branches and available Ca content in rhizosphere soil; (<b>E</b>): total Mg contents in leaves and branches and available Mg content in rhizosphere soil; (<b>F</b>): total Fe contents in leaves and branches and available Fe content in rhizosphere soil; (<b>G</b>): total Mn contents in leaves and branches and available Mn content in rhizosphere soil; (<b>H</b>): total Cu contents in leaves and branches and available Cu content in rhizosphere soil; (<b>I</b>) total Zn contents in leaves and branches and available Zn content in rhizosphere soil. The lower-case letters indicate a significant difference (<span class="html-italic">p</span> &lt; 0.05) among different samples for each treatment.</p>
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<p>Venn distribution of rhizosphere soil bacteria in blueberry plants at different developmental periods. T1. full bloom stage; T2. green fruit stage; T3. mature stage; T4. late mature stage.</p>
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<p>Analysis of rhizosphere soil bacterial communities PCoA in blueberry plants at different developmental periods. T1. full bloom stage; T2. green fruit stage; T3. mature stage; T4. late mature stage.</p>
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<p>Relative abundance of bacteria (phylum level) at different developmental periods of blueberry plants. T1. full bloom stage; T2. green fruit stage; T3. mature stage; T4. late mature stage.</p>
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<p>Relative abundance of bacteria (genus level) at different developmental periods of blueberry plants. T1. full bloom stage; T2. green fruit stage; T3. mature stage; T4. late mature stage.</p>
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<p>RDA of the top ten dominant bacterial genera and soil environmental factors. (Note: Each point represents a sample; the blue arrows represent the environmental factors, the red arrows represent the dominant bacteria, and the length of the arrows represents the degree of association with the bacteria, where a long length of the arrows indicates a high degree of association. The angle between the environmental factors and the dominant bacteria represents the size of the correlation between them. An acute angle indicates that the two factors are positively correlated, a right angle means they are not correlated, and an obtuse angle means they are negatively correlated. The <span class="html-italic">p</span>-value represents the value obtained by the random permutation nonparametric test. The smaller the <span class="html-italic">p</span>-value, the more significant the effect of the influencing factors on the composition of the flora. The percentage in the coordinate axis brackets represents the proportion of the differences in the data that the corresponding coordinate axis can explain.).</p>
Full article ">Figure A1
<p>High-quality sample sequence distribution map.</p>
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<p>Rhizosphere soil bacterial dilution curves of blueberry fruits at different developmental periods. T1. full bloom period; T2. green fruit period; T3. maturation period; T4. late maturation stage.</p>
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20 pages, 5211 KiB  
Article
Perspectives of Hydrogen Generation in Cavitation–Jet Hydrodynamic Reactor
by G. K. Mamytbekov, I. V. Danko, Zh. I. Beksultanov, Y. R. Nurtazin and A. Rakhimbayev
Appl. Sci. 2024, 14(20), 9415; https://doi.org/10.3390/app14209415 (registering DOI) - 15 Oct 2024
Viewed by 283
Abstract
The article investigates the potential for producing hydrogen by combining the methods of water splitting under cavitation and the chemical activation of aluminum in a high-speed cavitation–jet flow generated by a specialized hydrodynamic reactor. The process of cavitation and water spraying causes the [...] Read more.
The article investigates the potential for producing hydrogen by combining the methods of water splitting under cavitation and the chemical activation of aluminum in a high-speed cavitation–jet flow generated by a specialized hydrodynamic reactor. The process of cavitation and water spraying causes the liquid heating itself until it reaches saturated vapor pressure, resulting in the creation of vapor–gaseous products from the splitting of water molecules. The producing of vapor–gaseous products can be explained through the theory of non-equilibrium low-temperature plasma formation within a high-speed cavitation–jet flow of fluid. Special focus is also given to the interactions occurring at the interface boundary phase of aluminum and liquid under cavitation condition. The primary solid products formed on aluminum surfaces are bayerite, copper oxides (I and II), iron carbide, and a compound of magnesium oxides and aluminum hydroxide. A high hydrogen yield of 60% was achieved when using a 0.1% sodium hydroxide solution as a working liquid compared to demineralized water. Moreover, hydrogen methane was also detected in the volume of the vapor–gas mixture, which could be utilized to address the challenges of decarbonization and the recycling of aluminum-containing solid industrial and domestic waste. This work provides a contribution to the study of the mechanism of hydrogen generation by cavitation–jet processing of water and aqueous alkali solutions, in which conditions are created for double cavitation in the cavitation–jet chamber of the hydrodynamic reactor. Full article
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Figure 1

Figure 1
<p>General view of the cavitation–jet reactor: 1—cavitation–jet chamber; 2—liquid receiver vessel; 3—frequency converter; 4—centrifugal pump; 5, 6, 7, and 8—digital manometers.</p>
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<p>Schematic Diagram of the Mass Spectrum Analysis Stand for Residual Gases: MS—mass spectrometer, TP—turbomolecular pump, SP—spiral dry pump, V—vacuum valves, P—pressure sensor, BO—storage tank, and R—gas containing chamber.</p>
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<p>The sections of cavitation–jet chamber.</p>
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<p>Dependence of pH and temperature of water on of cavitation–jet processing time (<b>a</b>) and the increase in water temperature in relation to the frequency of the current supplied to the centrifugal pump via the frequency converter (<b>b</b>).</p>
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<p>Dependence of concentration of four metals on temperature and time of cavitation–jet processing of demineralized water (<b>a</b>) and aqueous solution of 0.1 wet % NaOH (<b>b</b>).</p>
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<p>Accumulation of gaseous products as a function of temperature during cavitation–jet processing of a 0.1% solution in a cavitation–jet reactor.</p>
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<p>Hydrogen accumulation data from gas chromatography during the cavitation–jet processing of 0.1% solution of NaOH in CJR.</p>
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<p>XRD (<b>a</b>), SEM (<b>bI</b>,<b>bII</b>) and EDA (<b>bIII</b>) data of the suspension formed during the cavitation–jet treatment of demineralized water. The colors of the lines indicate the element: calcium—brown line, carbon—turquoise line, oxygen—green line.</p>
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<p>XRD data of the powder formed during the cavitation–jet treatment of 0.1% NaOH solution on the surface of Al<sub>disc/foil</sub> and working part (Screw, Reflector and Splitter) of the cavitation–jet chamber.</p>
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<p>SEM data of the powder formed during the cavitation–jet treatment of 0.1% NaOH solution on the surface of working parts of cavitation–jet chamber, * means an increase in the scale of particle size measurement.</p>
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<p>Hydrogen generation on the reflector surface of the CJR.</p>
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14 pages, 2218 KiB  
Article
Synthesis and Characterization of Extremely Bulky Aminopyridinate Ligands and a Series of Their Groups 1 and 2 Metal Complexes
by Arif M. Earsad, Albert Paparo, Matthew J. Evans and Cameron Jones
Inorganics 2024, 12(10), 270; https://doi.org/10.3390/inorganics12100270 (registering DOI) - 15 Oct 2024
Viewed by 427
Abstract
High-yielding synthetic routes to five new extremely bulky aminopyridine pro-ligands were developed, viz. (C5H3N-6-Ar1)N(H)Ar2-2; Ar1 = Trip, Ar2 = TCHP (HAmPy1), Ar* (HAmPy2) or Ar (HAmPy3); [...] Read more.
High-yielding synthetic routes to five new extremely bulky aminopyridine pro-ligands were developed, viz. (C5H3N-6-Ar1)N(H)Ar2-2; Ar1 = Trip, Ar2 = TCHP (HAmPy1), Ar* (HAmPy2) or Ar (HAmPy3); Ar1 = TCHP, Ar2 = Ar* (HAmPy4) or Ar (HAmPy5) (Trip = 2,4,6-triisopropylphenyl, TCHP = 2,4,6-tricyclohexylphenyl, Ar* = C6H2(CHPh2)2Me-2,6,4, Ar = C6H2(CHPh2)2Pri-2,6,4. Four of these were deprotonated with LiBun in diethyl ether to give lithium aminopyridinate complexes which were dimeric for the least bulky ligand, [{Li(AmPy1)}2] or monomeric for the bulkier aminopyridinates, i.e., in [Li(AmPy2−4)(OEt2)]. One aminopyridine was deprotonated with MeMgI to give monomeric [Mg(AmPy3)I(OEt2)2]. When treated with sodium or potassium mirrors or 5% w/w Na/NaCl, over-reduction occurred, leading to the alkali metal aminopyridinates, [M(AmPy3)(η6-toluene)] (M = Na or K) or [{Na(AmPy3)}]. An attempted reduction of [Mg(AmPy3)I(OEt2)2] with a dimagnesium(I) compound led only to partial loss of diethyl ether and the formation of [(AmPy3)Mg(μ-I)2Mg(AmPy3)(OEt2)]. All prepared complexes have potential as ligand transfer reagents in salt metathesis reactions with metal halide complexes. Full article
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Figure 1

Figure 1
<p>The bulky aminopyridinate ligand <b>I</b> (Trip = 2,4,6-triisopropylphenyl and Dip = 2,6-diisopropylphenyl).</p>
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<p>Molecular structure of HAmPy<sup>3</sup> (25% thermal ellipsoids are shown; hydrogen atoms, except the amine proton, omitted). Selected bond lengths (Å) and angles (°): N(1)-C(1) 1.342(2), C(1)-N(2) 1.380(2), N(1)-C(1)-N(2) 114.24(13).</p>
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<p>Molecular structures of <b>1</b> (<b>top</b>) and <b>4</b> (<b>bottom</b>) (25% thermal ellipsoids are shown; hydrogen atoms omitted; TCHP, Trip, C(H)Ph<sub>2</sub> and/or cyclohexyl groups shown as wireframe for clarity). See <a href="#inorganics-12-00270-t001" class="html-table">Table 1</a> for relevant metrical parameters.</p>
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<p>Molecular structure of compound <b>5</b> (25% thermal ellipsoids are shown; hydrogen atoms omitted; isopropyl, ethyl and C(H)Ph<sub>2</sub> groups shown as wireframe for clarity). Selected bond lengths (Å) and angles (°): I(1)-Mg(1) 2.741(1), Mg(1)-O(2) 2.064(3), Mg(1)-N(2) 2.091(3), Mg(1)-O(1) 2.126(3), Mg(1)-N(1) 2.185(3), N(1)-C(1) 1.364(5), N(2)-C(1) 1.348(5), N(2)-Mg(1)-N(1) 63.64(13), N(2)-C(1)-N(1) 112.6(3).</p>
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<p>Molecular structures of the monomer unit of compound <b>6</b> (<b>top</b>), and compound <b>8</b> (<b>bottom</b>) (25% thermal ellipsoids are shown; hydrogen atoms omitted; isopropyl, and C(H)Ph<sub>2</sub> groups shown as wireframe for clarity). Selected bond lengths (Å) and angles (°) for <b>6</b>: Na(1)-N(2) 2.299(2), Na(1)-N(1) 2.4254(19), N(1)-C(1) 1.380(3), C(1)-N(2) 1.329(3), Na(1)-C(16)’ 2.828(3), Na(1)-C(17)’ 3.014(3), N(2)-Na(1)-N(1) 57.65(7), N(2)-C(1)-N(1) 114.66(19). Selected bond lengths (Å) and angles (°) for <b>8</b>: K(1)-N(2) 2.612(4), K(1)-N(1) 2.777(4), N(1)-C(1) 1.393(6), C(1)-N(2) 1.321(6), K(1)-toluene cent. 2.988(5), N(2)-K(1)-N(1) 50.41(11), N(2)-C(1)-N(1) 115.8(4).</p>
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<p>Molecular structure of compound <b>9</b> (25% thermal ellipsoids are shown; hydrogen atoms omitted; isopropyl and C(H)Ph<sub>2</sub> groups shown as wireframe for clarity). Selected bond lengths (Å) and angles (°): N(1)-C(1) 1.372(6), C(1)-N(2) 1.350(7), N(3)-C(60) 1.374(6), N(4)-C(60) 1.341(6), Mg(1)-N(2) 2.009(4), Mg(1)-N(1) 2.155(4), Mg(2)-N(4) 2.011(4), Mg(2)-N(3) 2.066(4), Mg(1)-O(1) 2.014(4), I(1)-Mg(2) 2.7123(19), I(1)-Mg(1) 2.7531(16), I(2)-Mg(2) 2.6782(18), N(2)-Mg(1)-N(1) 65.46(16), N(2)-C(1)-N(1) 111.9(4), N(4)-Mg(2)-N(3) 67.03(15), N(4)-C(60)-N(3) 112.0(4).</p>
Full article ">Scheme 1
<p>Synthesis of aminopyridine pro-ligands HAmPy<sup>1−5</sup> (dba = dibenzylideneacetone; dppp = 1,3-bis(dipehylphospino)propane; TCHP = 2,4,6-tricyclohexylphenyl; Ar* = C<sub>6</sub>H<sub>2</sub>(CHPh<sub>2</sub>)<sub>2</sub>Me-2,6,4; Ar<sup>†</sup> = C<sub>6</sub>H<sub>2</sub>(CHPh<sub>2</sub>)<sub>2</sub>Pr<span class="html-italic"><sup>i</sup></span>-2,6,4).</p>
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<p>Synthesis of compounds <b>1</b>–<b>4</b> (delocalization within the aminopyridinate ligands is not depicted).</p>
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<p>Synthesis of compounds <b>5</b>–<b>8</b>.</p>
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16 pages, 4343 KiB  
Article
Structural Evolution of Olivine during Mechanochemically Assisted Mineral Carbonation under CO2 Flow
by Costantino Cau, Alessandro Taras, Gabriele Masia, Laura Caggiu, Stefano Enzo, Sebastiano Garroni, Fabrizio Murgia and Gabriele Mulas
Inorganics 2024, 12(10), 269; https://doi.org/10.3390/inorganics12100269 (registering DOI) - 15 Oct 2024
Viewed by 434
Abstract
The mechanism of the mechanically assisted mineral carbonation of commercial olivine under the flow of a carbon dioxide (CO2)/nitrogen (N2) mixture has been elucidated by ex situ powder X-ray diffraction and Fourier-transform infrared spectroscopy. The overall CO2 conversion [...] Read more.
The mechanism of the mechanically assisted mineral carbonation of commercial olivine under the flow of a carbon dioxide (CO2)/nitrogen (N2) mixture has been elucidated by ex situ powder X-ray diffraction and Fourier-transform infrared spectroscopy. The overall CO2 conversion depends on the rotational frequency of the mill’s engine, and it reaches 85% within 90 min of mechanical treatment at a flow rate of 2.5 L min−1. By tuning the frequency of rotation, the kinetics of CO2 conversion unveil a complex reaction pathway involving subsequent steps. Structural analyses suggest that clinochlore, a magnesium (Mg-)- and iron (Fe-)-containing aluminosilicate gathered among the components of olivine, is formed and consumed in different stages, thus promoting the CO2 sequestration that eventually results in the formation of hydrated and anhydrous Mg-based carbonates. Full article
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Graphical abstract

Graphical abstract
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<p>(<b>Top</b>): P-XRD pattern of the pristine olivine. Rietveld refinement reveals that the main component is Mg<sub>1.8</sub>Fe<sub>0.2</sub>SiO<sub>4</sub>, forsterite, ~92.5 wt.%, followed by Mg<sub>0.8</sub>Fe<sub>0.2</sub>SiO<sub>3</sub>, ferrous enstatite, ~5 wt.%, and (Mg,Fe(II))<sub>5</sub>Al(Si<sub>3</sub>Al)O<sub>10</sub>(OH)<sub>8</sub>, clinochlore, ~2.5 wt.%. (<b>Bottom</b>): structural models of forsterite, enstatite, and clinochlore, indicated by (<b>a</b>), (<b>b</b>), and (<b>c</b>), respectively.</p>
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<p>(<b>A</b>): SEM micrography of pristine olivine particles, showing a narrow distribution of faceted micrometric particles ((<b>B</b>): detail of a selected particle) and EDX analysis showcasing a homogeneous distribution of O, Mg, Si, Al, and Fe, which are the main elements of the crystallographic phases composing olivine, flanked by some minor inclusions of Ca, Mn, and Ni.</p>
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<p>CO<sub>2</sub> conversion kinetics as a function of the grinding time. Milling conditions: continuous flow of CO<sub>2</sub>/N<sub>2</sub> 10:90, 2.5 mL min<sup>−1</sup>; rotational speed of the mill was set at 745 (green scatters), 875 (blue scatters), and 1000 rpm (red scatters). Dotted lines are added for the sake of clarity, and they are intended only to help follow the conversion trends at each of the rpms investigated. The highest CO<sub>2</sub> conversion rate was reached after 40 min of milling at 1000 rpm (red scatters, 85% of injected CO<sub>2</sub>), remaining stable up to the end of the investigated timeframe.</p>
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<p>From bottom to top: P-XRD analyses on pristine and reacted olivine at different milling times (745 rpm, 2.5 mL min<sup>−1</sup> of mixture gas containing 10% <span class="html-italic">v</span>/<span class="html-italic">v</span> CO<sub>2</sub>).</p>
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<p>FTIR analyses at different milling times (745 rpm, 10% <span class="html-italic">v</span>/<span class="html-italic">v</span> CO<sub>2</sub> concentration, 2.5 mL min<sup>−1</sup>). Vibrations of the skeleton of the Si-O silicate matrix of olivine are also found, identifiable in the characteristic bands in the range 1000–500 cm<sup>−1</sup>.</p>
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<p>XRD patterns (data points) and Rietveld refinement analyses (continuous lines) of olivine undergoing mechanical grinding in a commercial Spex-type mill for times increasing from 1 to 10 h.</p>
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<p>Experimental setup for the mechanochemical process under continuous flow of reactive gas mixture.</p>
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15 pages, 2041 KiB  
Article
Assessment of the Response to Fertilization for the Sustainable Management of Native Grasses from Flooded Savannah Ecosystem Arauca, Colombian Orinoquia
by Arcesio Salamanca-Carreño, Otoniel Pérez-López, Mauricio Vélez-Terranova, Oscar Mauricio Vargas-Corzo, Pere M. Parés-Casanova and Andrés F. Castillo-Pérez
Sustainability 2024, 16(20), 8915; https://doi.org/10.3390/su16208915 - 15 Oct 2024
Viewed by 305
Abstract
The native grasses of the flooded savannah ecosystem are produced under natural conditions and there is little information on the productive and nutritional response to the application of fertilizers. They are proposed as a strategy for adaptation to climate change and for the [...] Read more.
The native grasses of the flooded savannah ecosystem are produced under natural conditions and there is little information on the productive and nutritional response to the application of fertilizers. They are proposed as a strategy for adaptation to climate change and for the sustainable development of livestock farming. The aim of the study was to evaluate the response to low doses of fertilization of native grasses (“bank” grasses: Paspalum plicatulum, Panicum versicolor, and Paspalum sp. “Low” grasses: Leersia hexandra and Hymenachne amplexicaulis) in flooded savannah conditions. The green forage samples were taken in a 1 m2 frame at 28-, 35-, and 42-day cutting intervals and biomass production was estimated with and without fertilization. After 35 days, the nutritional composition was analyzed by near-infrared reflectance spectroscopy (NIRS). The effect of fertilization and the grasses × cutting interval interaction influenced (p < 0.05) green forage (GF, t/ha) and dry matter (DM, t/ha). The effect of fertilization and the grasses × fertilization interaction on the nutritional composition only influenced the content of calcium (Ca2+) and magnesium (Mg2+) in the “low” grasses, while in the “bank” grasses, it influenced the sodium (Na) content (p < 0.05). The application of fertilizers generated significant differences in forage yield, but not in the general nutritional composition of grasses. However, some numerical variations were observed in favor of fertilized grasses. According to these results, the application of fertilizers will not be required to increase the value of the nutritional composition. Native grasses constitute an important sustainable food resource for livestock in flooded savannah ecosystems. This study constitutes the first approximation to understanding the behavior of native grasses for sustainable management in the flooded savannah ecosystem. Full article
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<p>Red color: Arauca department, located in eastern Colombia. Red circle: flooded savannah ecosystem where the experiment was carried out. Photographs to the right: flooded savannah ecosystem of Arauca.</p>
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<p>Grasses native to the physiographic position “low”: (<b>a</b>) <span class="html-italic">Leersia hexandra</span> and (<b>b</b>) <span class="html-italic">Hymenachne amplexicaulis</span>; and “bank”: (<b>c</b>) <span class="html-italic">Paspalum plicatulum</span>, (<b>d</b>) <span class="html-italic">Panicum versicolor</span>, and (<b>e</b>) <span class="html-italic">Paspalum</span> sp., in the Araucana flooded savannah.</p>
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<p>Yield of green forage (<b>a</b>) and dry matter (<b>b</b>) of grasses with and without fertilization evaluated in the “bank” physiographic position of flooded savannahs of the Colombian Orinoquia. WTF = Without fertilization; WF = with fertilization.</p>
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<p>Yield of green forage (<b>a</b>) and dry matter of grasses (<b>b</b>) with and without fertilization evaluated in the “low” physiographic position of flooded savannahs of the Colombian Orinoquia. WTF = Without fertilization; WF = With fertilization.</p>
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15 pages, 2896 KiB  
Article
The Synergistic Effects of Different Phosphorus Sources: Ferralsols Promoted Soil Phosphorus Transformation and Accumulation
by Long Zhou, Tilei Zhao, Nyeinnyein Thu, Hongmin Zhao, Yi Zheng and Li Tang
Agronomy 2024, 14(10), 2372; https://doi.org/10.3390/agronomy14102372 - 14 Oct 2024
Viewed by 308
Abstract
Phosphorus (P) application can enhance soil P availability and alter P fractions. However, the P accumulation and transformation of different P sources in low-phosphorus red soil remain unclear. Two-year (2018–2019) field experiments were conducted to investigate the effects of five P source treatments [...] Read more.
Phosphorus (P) application can enhance soil P availability and alter P fractions. However, the P accumulation and transformation of different P sources in low-phosphorus red soil remain unclear. Two-year (2018–2019) field experiments were conducted to investigate the effects of five P source treatments (CK—no phosphorus; SSP—superphosphate; MAP—calcium–magnesium phosphate; DAP—monoammonium phosphate; and CMP—diammonium phosphate) on the P accumulation of maize and soil P fractions in low-P red soil using the Hedley Sequential Method. The results showed that P application significantly increased P uptake, Olsen-P, total phosphorus, and most of the soil P fractions. Compared to the CMP, MAP, and DAP treatments, SSP had a relatively higher P accumulation and labile P pool, with a slightly lower moderately labile P pool. The SSP treatment mainly increased soil-available P content and crop P uptake by increasing the labile P pool (resin-P and NaHCO3-Pi) and reducing the moderately labile P pool and non-labile P pool. The P activation coefficient (PAC%) and Olsen-P were positively correlated with labile P (resin-P, NaHCO3-Pi, and NaHCO3-Po) and moderately labile P (NaOH-Pi and 1 M HCl-Pi) and negatively correlated with Fe2O3 and Al2O3. The results suggest that SSP has a priority effect on the crop P uptake and soil P availability in low-P red soil. Full article
(This article belongs to the Section Soil and Plant Nutrition)
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<p>Sequential P fractions based on the Hedley method modified by Tiessen and Moir [<a href="#B30-agronomy-14-02372" class="html-bibr">30</a>].</p>
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<p>Effect of different P sources (CK, SSP, MAP, DAP, and CMP) on the P uptake of maize in 2018 and 2019. Values are means ± standard deviation (<span class="html-italic">n</span> = 3). Values with the same lower-case letters are not significantly different among different P sources and years at the 5% level by the LSD. Y represents the year, P represents the P sources and Y × P represents the interaction between the year and the P sources. *** <span class="html-italic">p</span> &lt; 0.001, * <span class="html-italic">p</span> &lt; 0.05. CK is no P fertilizer, SSP is single superphosphate (90 kg ha<sup>−1</sup>), CMP is calcium magnesium phosphate (90 kg ha<sup>−1</sup>), MAP is monoammonium phosphate (90 kg ha<sup>−1</sup>), and DAP is diammonium phosphate (90 kg ha<sup>−1</sup>).</p>
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<p>Changes in the soil Olsen-P (<b>a</b>), total P (<b>b</b>) and PAC% (<b>c</b>) to 20 cm depth as affected by different P sources. Values are means ± standard deviation (<span class="html-italic">n</span> = 3). Values with the same lower-case letters are not significantly different among different P sources and years at the 5% level by the LSD. Y represents the year, P represents the P sources and Y × P represents the interaction between the year and the P sources. *** <span class="html-italic">p</span> &lt; 0.001, ** <span class="html-italic">p</span> &lt; 0.01, * <span class="html-italic">p</span> &lt; 0.05. CK is no P fertilizer, SSP is single superphosphate (90 kg ha<sup>−1</sup>), CMP is calcium magnesium phosphate (90 kg ha<sup>−1</sup>), MAP is monoammonium phosphate (90 kg ha<sup>−1</sup>), and DAP is diammonium phosphate (90 kg ha<sup>−1</sup>).</p>
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<p>Effect of different P sources (CK, SSP, MAP, DAP, and CMP) on the total inorganic P (<b>a</b>), total organic P (<b>b</b>) in 2018 and 2019. Values are means ± standard deviation (<span class="html-italic">n</span> = 3). Values with the same lower-case letters are not significantly different among different P fertilizer sources and years at the 5% level by the LSD. Y represents the year, P represents the P sources and Y × P represents the interaction between the year and the P sources. *** <span class="html-italic">p</span> &lt; 0.001, ** <span class="html-italic">p</span> &lt; 0.01, ns <span class="html-italic">p</span> &gt; 0.05. CK is no P fertilizer, SSP is single superphosphate (90 kg ha<sup>−1</sup>), CMP is calcium magnesium phosphate (90 kg ha<sup>−1</sup>), MAP is monoammonium phosphate (90 kg ha<sup>−1</sup>), and DAP is diammonium phosphate (90 kg ha<sup>−1</sup>).</p>
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<p>Effect of different P sources (CK, SSP, MAP, DAP, and CMP) on the labile P pools (<b>a</b>), moderately-labile P pools (<b>b</b>) and non-labile P pools (<b>c</b>) in 2018 and 2019. Values are means ± standard deviation (<span class="html-italic">n</span> = 3). Values with the same lower-case letters are not significantly different among different P sources and years at the 5% level by the LSD. Y represents the year, P represents the P sources and Y × P represents the interaction between the year and the P sources. *** <span class="html-italic">p</span> &lt; 0.001, ** <span class="html-italic">p</span> &lt; 0.01, ns <span class="html-italic">p</span> &gt; 0.05. CK is no P fertilizer, SSP is single superphosphate (90 kg ha<sup>−1</sup>), CMP is calcium magnesium phosphate (90 kg ha<sup>−1</sup>), MAP is monoammonium phosphate (90 kg ha<sup>−1</sup>), and DAP is diammonium phosphate (90 kg ha<sup>−1</sup>).</p>
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<p>Effect of different P sources (CK, SSP, MAP, DAP, and CMP) on the labile P fractions in 2018 and 2019. Values are means ± standard deviation (<span class="html-italic">n</span> = 3). For each soil P fraction, values followed by the same lower-case letter are not significantly different among different P fertilizer sources and years at the 5% level by the LSD. Y represents the year, P represents the P sources and Y × P represents the interaction between the year and the P sources. *** <span class="html-italic">p</span> &lt; 0.001, ** <span class="html-italic">p</span> &lt; 0.01. CK is no P fertilizer, SSP is single superphosphate (90 kg ha<sup>−1</sup>), CMP is calcium magnesium phosphate (90 kg ha<sup>−1</sup>), MAP is monoammonium phosphate (90 kg ha<sup>−1</sup>), and DAP is diammonium phosphate (90 kg ha<sup>−1</sup>).</p>
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<p>Effect of different P sources (CK, SSP, MAP, DAP, and CMP) on the proportions of labile P pool, moderately-labile P pool and non-labile P pool in 2018 and 2019. Values are means ± standard deviation (<span class="html-italic">n</span> = 3). Values with the same lower-case letters are not significantly different among different P sources and years at the 5% level by the LSD. CK refers to no P application, SSP refers to P application for calcium superphosphate, MAP refers to P application for calcium magnesium phosphate, DAP refers to P application for monoammonium phosphate, and CMP refers to P application for diammonium phosphate.</p>
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<p>Correlations between the soil chemical properties and soil P pools were determined by the redundancy analysis. The red arrow indicates the explanatory variable, and the black arrow indicates the response variable.</p>
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<p>Correlations between the soil P fractions and P uptake, Olsen-P and PAC% as determined by the redundancy analysis. The red arrow indicates the explanatory variable, and the black arrow indicates the response variable.</p>
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<p>Random forest analyses to identify the main predictors of the P uptake, Olsen-P, and PAC% among all P fractions. Percentage increases in the MSE (mean squared error) of variables were used to estimate the importance of these predictors, and higher MSE% values imply more important predictors. Significance levels are as follows: * <span class="html-italic">p</span> &lt; 0.05 and ** <span class="html-italic">p</span> &lt; 0.01.</p>
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13 pages, 2299 KiB  
Article
Soil Recycling of Waste Biomass in the Production of Malus domestica Fruit Tree Seedlings
by Natalia Matłok, Małgorzata Szostek and Maciej Balawejder
Agriculture 2024, 14(10), 1806; https://doi.org/10.3390/agriculture14101806 - 14 Oct 2024
Viewed by 583
Abstract
The production of fruit tree seedlings generates waste wood biomass, which results from the pruning of budded rootstocks in the first year of the two-year production cycle. This study proposes a new method of managing this biomass by recycling the wood chips (2, [...] Read more.
The production of fruit tree seedlings generates waste wood biomass, which results from the pruning of budded rootstocks in the first year of the two-year production cycle. This study proposes a new method of managing this biomass by recycling the wood chips (2, 3 and 5 t ha−1) back into the soil. The impact of different wood chip doses on selected physicochemical soil properties after the production process (especially soil organic carbon content (SOC), as well as the quantity and quality of the produced Malus domestica fruit tree seedlings, was determined. The recycling of waste biomass contributed to enriching the soil with additional components, mainly organic carbon with the potential for biotransformation into humic substances. The applied doses of wood chips, in amounts of 2, 3, and 5 t ha−1, resulted in an increase in SOC content compared to the control by 21.5%, 22.5%, and 35.8%, respectively. Additionally, the recycling of waste biomass introduced other compounds important for plant growth and development into the soil, particularly iron, zinc, magnesium, and manganese. It should be noted that the proposed method of managing waste biomass generated during the apple tree seedling production stage resulted in reduced production costs while maintaining high production indices. Full article
(This article belongs to the Section Agricultural Soils)
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<p>Technology for producing one-year-old apple trees with consideration of the soil’s incorporation of biomass waste generated from cutting rootstocks.</p>
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<p>Average pH value (1 mol KCl dm<sup>−3</sup>) depending on the applied dose of chips from waste biomass. Mean values ± standard deviation. Identical super-scripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post hoc Tukey HSD test. (a) Identical superscripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post hoc Tukey HSD test.</p>
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<p>(<b>A</b>–<b>D</b>) Concentration of the available nitrogen, phosphorus, potassium, and magnesium in soil depending on the applied dose chips from waste biomass (Mean ± SD). Mean values ± standard deviation. Identical super-scripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post hoc Tukey HSD test. (a, b) Identical superscripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post-hoc Tukey HSD test.</p>
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<p>Content of soil organic carbon (SOC) in soil depending on the applied dose chips from waste biomass (Mean ± SD). Mean values ± standard deviation. Identical super-scripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post hoc Tukey HSD test. (a) Identical superscripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post hoc Tukey HSD test.</p>
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<p>Concentration of soluble Fe (<b>A</b>), Mn (<b>B</b>), Zn (<b>C</b>) and Cu (<b>D</b>) in soil depending on the applied dose chips from waste biomass (Mean ± SD). Mean values ± standard deviation. Identical super-scripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post-hoc Tukey HSD test. (a, b) Identical superscripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post hoc Tukey HSD test.</p>
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<p>Average amount [%] of accepted apple budding chips depending on the applied dose of chips waste biomass. (a, b) Identical superscripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post-hoc Tukey HSD test.</p>
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<p>Part of the apple tree I and II selection depending on the applied dose of chips from waste biomass. (a, b) Identical superscripts denote no significant (<span class="html-italic">p</span> &lt; 0.05) differences between the experimental objects according to the post-hoc Tukey HSD test.</p>
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16 pages, 272 KiB  
Article
Presence of Trace Elements in Edible Insects Commercialized through Online E-Commerce Platform
by Nadia San Onofre, David Vie, Jose M. Soriano and Carla Soler
Toxics 2024, 12(10), 741; https://doi.org/10.3390/toxics12100741 - 12 Oct 2024
Viewed by 368
Abstract
This study aimed to evaluate the presence of various elements in edible insect-based food products available for human consumption. Several products were analyzed using atomic spectroscopy, and descriptive statistical analysis was conducted with IBM SPSS Statistics 27. The results revealed the presence of [...] Read more.
This study aimed to evaluate the presence of various elements in edible insect-based food products available for human consumption. Several products were analyzed using atomic spectroscopy, and descriptive statistical analysis was conducted with IBM SPSS Statistics 27. The results revealed the presence of elements such as arsenic, cadmium, copper, magnesium, nickel, silver, lead, tungsten, uranium, mercury, platinum, aluminum, beryllium, bismuth, lithium, antimony, and thallium. Significant differences were found based on product type, insect species, and country of origin. The findings underscore the need to assess each insect species for its potential as a food source, taking into account element bioaccumulation factors. A comprehensive, global approach is essential for ensuring the food safety of edible insects as a sustainable protein source. Further research is needed to address these safety concerns. Full article
(This article belongs to the Section Agrochemicals and Food Toxicology)
15 pages, 1393 KiB  
Article
The Impact of Activated Carbon–MexOy (Me = Bi, Mo, Zn) Additives on the Thermal Decomposition Kinetics of the Ammonium Nitrate–Magnesium–Nitrocellulose Composite
by Zhanerke Yelemessova, Ayan Yerken, Dana Zhaxlykova and Bagdatgul Milikhat
J. Compos. Sci. 2024, 8(10), 420; https://doi.org/10.3390/jcs8100420 - 12 Oct 2024
Viewed by 388
Abstract
This research investigates the impact of additives such as activated carbon (AC) combined with metal oxides (Bi2O3, MoO3, and ZnO) on the thermal decomposition kinetics of ammonium nitrate (AN), magnesium (Mg), and nitrocellulose (NC) as a basic [...] Read more.
This research investigates the impact of additives such as activated carbon (AC) combined with metal oxides (Bi2O3, MoO3, and ZnO) on the thermal decomposition kinetics of ammonium nitrate (AN), magnesium (Mg), and nitrocellulose (NC) as a basic AN–Mg–NC composite. To study the thermal properties of the AN–Mg–NC composite with and without the AC–MexOy (Me = Bi, Mo, Zn) additive, a differential scanning calorimetry (DSC) analysis was conducted. The DSC results show that the AC–MexOy (Me = Bi, Mo, Zn) additive catalytically affects the basic AN–Mg–NC composite, lowering the peak decomposition temperature (Tmax) from 534.58 K (AN–Mg–NC) to 490.15 K (with the addition of AC), 490.76 K (with AC–Bi2O3), 492.17 K (with AC–MoO3), and 492.38 K (with AC–ZnO) at a heating rate of β equal to 5 K/min. Based on the DSC data, the activation energies (Ea) for the AN–Mg–NC, AN–Mg–NC–AC, and AN–Mg–NC–AC–MexOy (Me = Bi, Mo, Zn) composites were determined using the Kissinger method. The results suggest that incorporating AC and AC–MexOy (Me = Bi, Mo, Zn) additives reduce the decomposition temperatures and activation energies of the basic AN–Mg–NC composite. Specifically, Ea decreased from 99.02 kJ/mol (for AN–Mg–NC) to 93.63 kJ/mol (with addition of AC), 91.45 kJ/mol (with AC–Bi2O3), 91.65 kJ/mol (with AC–MoO3), and 91.76 kJ/mol (with AC–ZnO). These findings underscore the potential of using AC–MexOy (Me = Bi, Mo, Zn) as a catalytic additive to enhance the performance of AN–Mg–NC-based energetic materials, increasing their efficiency and reliability for use in solid propellants. Full article
(This article belongs to the Special Issue Theoretical and Computational Investigation on Composite Materials)
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<p>DSC curve of an AN–Mg–NC basic composite heated at <span class="html-italic">β</span> = 5 K/min.</p>
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<p>DSC curves of (<b>a</b>) AN–Mg–NC–AC; (<b>b</b>) AN–Mg–NC–AC–Bi<sub>2</sub>O<sub>3</sub>; (<b>c</b>) AN–Mg–NC–AC–MoO<sub>3</sub>; (<b>d</b>) AN–Mg–NC–AC–ZnO composites heated at <span class="html-italic">β</span> = 5 K/min.</p>
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<p>Kissinger plot of the basic AN–Mg–NC composite.</p>
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<p>Kissinger plot of the AN–Mg–NC–AC composite.</p>
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<p>Kissinger plot of the AN–Mg–NC–AC–Bi<sub>2</sub>O<sub>3</sub> composite.</p>
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<p>Kissinger plot of the AN–Mg–NC–AC–MoO<sub>3</sub> composite.</p>
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<p>Kissinger plot of the AN–Mg–NC–AC–ZnO composite.</p>
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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 (registering DOI) - 12 Oct 2024
Viewed by 689
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
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<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>
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<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>
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<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>
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<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>
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<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>
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<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>
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<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>
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<p>Energy-dispersive X-ray spectroscopy spectra of (<b>a</b>) MgHAp and (<b>b</b>) MgHApOx.</p>
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<p>FTIR general spectra of MgHAp, MgHApOx and Ox.</p>
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<p>FTIR spectra of MgHAp, MgHApOx and Ox obtained between 900 and 1200 cm<sup>−1</sup> and their second derivative curve.</p>
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<p>Deconvoluted FTIR spectra of the MgHAp, Ox and MgHApOx obtained in the 900–1200 cm<sup>−1</sup> spectral domain.</p>
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<p>General XPS spectra of MgHAp (<b>a</b>) and MgHApOx (<b>b</b>) samples.</p>
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<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>
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<p>High-resolution XPS spectra and curve-fitting results of Mg 2p for MgHAp (<b>a</b>) and MgHApOx (<b>b</b>).</p>
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<p>High-resolution XPS spectra and curve-fitting results of N1s (<b>a</b>) and S 2p (<b>b</b>) for MgHApOx sample.</p>
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<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>
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<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>
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<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>
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<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>
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<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>
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15 pages, 11845 KiB  
Article
Study on the Influence of Injection Velocity on the Evolution of Hole Defects in Die-Cast Aluminum Alloy
by Hanxue Cao, Qiang Zhang, Weikai Zhu, Sheng Cui, Qin Yang, Zhibai Wang and Bin Jiang
Materials 2024, 17(20), 4990; https://doi.org/10.3390/ma17204990 - 12 Oct 2024
Viewed by 251
Abstract
Aluminum alloy die casting has achieved rapid development in recent years and has been widely used in all walks of life. However, due to its high pressure and high-speed technological characteristics, avoiding hole defects has become a problem of great significance in aluminum [...] Read more.
Aluminum alloy die casting has achieved rapid development in recent years and has been widely used in all walks of life. However, due to its high pressure and high-speed technological characteristics, avoiding hole defects has become a problem of great significance in aluminum alloy die casting production. In this paper, the filling visualization dynamic characterization experiment was innovatively developed, which can directly study and analyze the influence of different injection rates on the formation and evolution of alloy flow patterns and gas-induced defects. As the injection speed increased from 1.0 m/s to 1.5 m/s, the average porosity increased from 7.49% to 9.57%, marking an increase in the number and size of the pores. According to the comparison with Anycasting, simulation results show that a liquid metal injection speed of 1.5 m/s when filling the flow front vs. the previous injection rate of 1.0 m/s caused fractures when filling at the same filling distance. Therefore, the degree of the broken splash at the flow front is more serious. Combined with the analysis of transport mechanics, the fracturing is due to the wall-attached jet effect of the liquid metal in the filling process. It is difficult for the liquid metal to adhere to the type wall in order to fuse with subsequent liquid metal to form cavity defects. With an increase in injection velocity, the microgroup volume formed via liquid breakage decreases; thus the volume of air entrapment increases, finally leading to an increase in cavity defects. Full article
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<p>(<b>a</b>) DCC630 horizontal cold chamber die casting machine, (<b>b</b>) Visual platform diagram.</p>
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<p>Opening position and size of windows. (<b>a</b>) Front view of mold; (<b>b</b>) Isometric side view of mold; (<b>c</b>) Schematic diagram of test sample; (<b>d</b>) Window Size Diagram.</p>
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<p>Three-dimensional model of the sample and sampling location (S1, S2, S3, S4). (<b>a</b>) Sampling location diagram; (<b>b</b>) specimen size.</p>
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<p>Image-Pro Plus marks the location and size of the hole. (<b>a</b>) Original image; (<b>b</b>) Coloring image; (<b>c</b>) Processed image.</p>
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<p>Flow characteristics at different velocities of injection: (<b>a1</b>–<b>a6</b>) 1.0 m/s, (<b>b1</b>–<b>b6</b>) 1.5 m/s.</p>
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<p>Simulation results of filling flow at different speeds: (<b>a1</b>(<b>1</b>)–<b>a6</b>(<b>6</b>)) 1.0 m/s, (<b>b1</b>(<b>1</b>)–<b>b6</b>(<b>6</b>)) 1.5 m/s.</p>
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<p>Cross-sectional morphology of specimens with an inner gate thickness of 3.0 mm and an injection velocity of 1.0 m/s.</p>
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<p>Cross-sectional morphology of specimens with an inner gate thickness of 3.0 mm and an injection velocity of 1.5 m/s.</p>
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<p>Porosity at different injection velocities at a 3.0 mm inner gate.</p>
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<p>Flow pattern of liquid metal at S2 position at injection velocity of 1.0 m/s. (<b>a</b>) t1; (<b>b</b>) t2; (<b>c</b>) t3.</p>
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<p>Flow pattern of liquid metal at S2 position at injection velocity of 1.5 m/s. (<b>a</b>) t1; (<b>b</b>) t2; (<b>c</b>) t3.</p>
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<p>Wall jet model.</p>
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<p>Diagram between Oh and Re.</p>
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14 pages, 7759 KiB  
Article
SLM Magnesium Alloy Micro-Arc Oxidation Coating
by Xuejie Yue, Kangning Xu, Shuyi Wang, Hengyan Liu, Shiyue Guo, Rusheng Zhao, Gaopeng Xu, Hao Wang and Xuezheng Yue
Materials 2024, 17(20), 4988; https://doi.org/10.3390/ma17204988 - 12 Oct 2024
Viewed by 336
Abstract
In this study, we utilized Selective Laser Melting (SLM) technology to fabricate a magnesium alloy, and subsequently subject it to micro-arc oxidation treatment. We analyzed and compared the microstructure, elemental distribution, wetting angle, and corrosion resistance of the SLM magnesium alloy both before [...] Read more.
In this study, we utilized Selective Laser Melting (SLM) technology to fabricate a magnesium alloy, and subsequently subject it to micro-arc oxidation treatment. We analyzed and compared the microstructure, elemental distribution, wetting angle, and corrosion resistance of the SLM magnesium alloy both before and after the micro-arc oxidation process. The findings indicate that the SLM magnesium alloy exhibits surface porosity defects ranging from 2% to 3.2%, which significantly influence the morphology and functionality of the resulting film layer formed during the micro-arc oxidation process. These defects manifest as pores on the surface, leading to an uneven distribution of micropores with varying sizes across the layer. The surface roughness of the 3D-printed magnesium alloy exhibits a high roughness value of 180 nanometers. The phosphorus (P) content is lower within the film layer compared to the surface, suggesting that the Mg3(PO4)2 phase predominantly resides on the surface, whereas the interior is primarily composed of MgO. The micro-arc oxidation process enhances the hydrophilicity and corrosion resistance of the SLM magnesium alloy, thereby potentially endowing it with bioactivity. Additionally, the increased surface roughness post-treatment promotes cell proliferation. However, certain inherent defects present in the SLM magnesium alloy samples negatively impact the improvement of their corrosion resistance. Full article
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<p>AZ91D magnesium alloy powder.</p>
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<p>XRD patterns of AZ91 magnesium alloy powder and printed samples.</p>
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<p>Microstructural images of 3D-printed magnesium alloy and analysis of surface porosity defects and density.</p>
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<p>SEM surface morphology of SLM magnesium alloy micro-arc oxide film.</p>
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<p>EDS spectra of SLM magnesium alloy micro-arc oxide coating.</p>
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<p>SEM cross-sectional view of the micro-arc oxide coating layer of SLM magnesium alloy. (The red dotted line shows the position of the cut material and the orange dotted line shows the membrane outline).</p>
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<p>Cross-sectional EDS spectra of SLM magnesium alloy micro-arc oxide coating.</p>
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<p>XRD pattern of micro-arc oxide coating layer on SLM magnesium alloy.</p>
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<p>Wetting angle (<b>a</b>) of SLM magnesium alloy before and after micro-arc oxidation treatment; (<b>b</b>) post-processing; (<b>c</b>) Comparison of wetting angle.</p>
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<p>Kinetic polarization curves measured in SBF simulated body fluids before and after microarc oxidation of SLM magnesium alloys.</p>
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<p>AFM image of 3D-printed magnesium alloy micro-arc oxide coating.</p>
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<p>The infrared spectroscopy analysis of the MAO coating after immersion in SBF for 21 days.</p>
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18 pages, 6591 KiB  
Article
Bioactive-Glass-Incorporated Plasma Electrolytic Oxidation Coating on AZ31 Mg Alloy: Preparation and Characterization
by Syed Ahmed Uzair, Fayaz Hussain and Muhammad Rizwan
Ceramics 2024, 7(4), 1459-1476; https://doi.org/10.3390/ceramics7040094 (registering DOI) - 12 Oct 2024
Viewed by 529
Abstract
Magnesium alloys, despite having a number of attractive properties, encounter difficulties in clinical applications due to their rapid degradation rate in the physiological environment. In this work, a Bioglass (BG)-incorporated plasma electrolytic oxidation (PEO) coating was applied on the AZ31 Mg alloy to [...] Read more.
Magnesium alloys, despite having a number of attractive properties, encounter difficulties in clinical applications due to their rapid degradation rate in the physiological environment. In this work, a Bioglass (BG)-incorporated plasma electrolytic oxidation (PEO) coating was applied on the AZ31 Mg alloy to overcome this major limitation. PEO treatment was carried out in constant current mode with and without the addition of BG particles. The effects of BG particles on the coating’s morphology, composition, adhesion, electrochemical corrosion resistance and bioactivity were analyzed. SEM micrographs revealed that BG submicron particles were well adhered to the surface and the majority of them were entrapped in the micropores. Furthermore, the adhesion strength of the coated layer was adequate—a maximum value of 22.5 N was obtained via a micrometer scratch test. Potentiodynamic polarization (PDP) and electrochemical impedance spectroscopy (EIS) results revealed that the degradation rate of the Mg alloy was slowed down by up to 100 times, approximately. Moreover, the PEO–BG layer considerably enhanced the in vitro bioactivity of the Mg alloy in a simulated body fluid (SBF) environment; a prominent apatite layer was witnessed through SEM imaging. Consequently, the BG-incorporated PEO layer on Mg AZ31 alloy exhibited some promising outcomes and, therefore, can be considered for biomedical applications. Full article
(This article belongs to the Special Issue Research Progress in Ceramic Coatings)
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<p>SEM images of (<b>a</b>,<b>b</b>) synthesized BG particles (before milling), (<b>c</b>) BG particles after milling and (<b>d</b>) EDS analysis of milled BG particles.</p>
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<p>(<b>a</b>) XRD pattern of synthesized 58S BG. (<b>b</b>) Particle size distribution of 58S BG powder (after milling).</p>
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<p>Voltage–time response of PPEO, PEO–BG-50 and PEO–BG-100 coatings.</p>
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<p>Optical images of uncoated and coated samples (immersed part).</p>
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<p>(<b>a</b>,<b>b</b>) SEM images of PPEO surface morphologies, (<b>d</b>,<b>e</b>) PEO–BG-50 surface morphologies, (<b>g</b>,<b>h</b>) PEO–BG-100 surface morphologies, (<b>c</b>,<b>f</b>,<b>i</b>) backscattered SEM (BSEM) images of cross-sectioned morphologies.</p>
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<p>EDS analysis of (<b>a</b>) PPEO and (<b>b</b>) PEO–BG-50 coatings.</p>
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<p>XRD patterns of (<b>a</b>) AZ31 substrate, (<b>b</b>) PPEO, (<b>c</b>) PEO–BG.</p>
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<p>The optical micrographs and critical loads of scratch tracks of all PEO coatings.</p>
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<p>Potentiodynamic behavior of the AZ31 substrate and PEO-coated samples.</p>
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<p>The schematic diagram of the corrosion mechanism. (<b>a</b>,<b>b</b>) PEO coating without BG particles, the substrate is easily corroded. (<b>c</b>,<b>d</b>) PEO with BG particles on surface results in compact layer and better corrosion resistance.</p>
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<p>(<b>a</b>) Nyquist plots. (<b>b</b>) Bode curves: frequency vs. impedance. (<b>c</b>) Bode curves: frequency vs. phase angle.</p>
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<p>Equivalent electric circuit for fitting EIS data.</p>
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<p>SEM and EDS analyses of samples immersed in SBF. (<b>a</b>,<b>b</b>) 7 days PEO–BG. (<b>c</b>,<b>d</b>) 14 days PEO–BG. (<b>e</b>,<b>f</b>) 14 days PPEO.</p>
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16 pages, 9355 KiB  
Article
Enhancing Magnesium Bioactivity for Biomedical Applications: Effects of Laser Texturing and Sandblasting on Surface Properties
by Marjetka Conradi, Aleksandra Kocijan and Bojan Podgornik
Materials 2024, 17(20), 4978; https://doi.org/10.3390/ma17204978 - 11 Oct 2024
Viewed by 282
Abstract
Magnesium and its alloys, valued for their lightweight and durable characteristics, have garnered increasing attention for biomedical applications due to their exceptional biocompatibility and biodegradability. This work introduces a comparison of advanced and basic methods—laser texturing and sandblasting—on magnesium surfaces to enhance bioactivity [...] Read more.
Magnesium and its alloys, valued for their lightweight and durable characteristics, have garnered increasing attention for biomedical applications due to their exceptional biocompatibility and biodegradability. This work introduces a comparison of advanced and basic methods—laser texturing and sandblasting—on magnesium surfaces to enhance bioactivity for biomedical applications. Employing a comprehensive analysis spanning surface morphology, hardness, wettability, tribological performance, and corrosion behavior, this study elucidates the intricate relationship between varied surface treatments and magnesium’s performance. Findings reveal that both laser texturing and sandblasting induce grain refinement. Notably, sandblasting, particularly with a duration of 2 s, demonstrates superior wear resistance and reduced corrosion rates compared to untreated magnesium, thereby emerging as a promising approach for enhancing magnesium bioactivity in biomedical contexts. This investigation contributes to a deeper understanding of the nuanced interactions between diverse surface treatments and their implications for magnesium implants in chloride-rich environments, offering valuable insights for prospective biomedical applications. Full article
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<p>SEM image of Al<sub>2</sub>O<sub>3</sub> particles used for sandblasting.</p>
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<p>SEM images of magnesium surfaces under investigation: diamond-polished (<b>a</b>), laser-textured (<b>b</b>), sandblasted for 2 s (<b>c</b>), sandblasted for 5 s (<b>d</b>), sandblasted for 10 s (<b>e</b>), and sandblasted for 30 s (<b>f</b>). The inset images show the details of the surfaces’ morphology at higher magnification.</p>
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<p>Surface profiles of diamond-polished (<b>a</b>), laser-textured (<b>b</b>), sandblasted for 2 s (<b>c</b>), sandblasted for 5 s (<b>d</b>), sandblasted for 10 s (<b>e</b>), and sandblasted for 30 s (<b>f</b>).</p>
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<p>EBSD band contrast image overlapping with the EBSD phase map for diamond-polished (<b>a</b>), laser-textured (<b>b</b>), and sandblasted 30 s (<b>c</b>) magnesium surface.</p>
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<p>EDS mapping of laser textured surface indicating increased surface oxidation of the ablated area.</p>
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<p>Hardness (GPa) variation with the distance from the sample’s surface into the bulk for diamond-polished (<b>a</b>), laser-textured (<b>b</b>), and sandblasted surfaces from 2 s–30 s (<b>c</b>–<b>f</b>).</p>
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<p>XPS spectra C 1 s, O 1 s, and Mg 1 s from polished (DP), laser-textured (LT), and sandblasted for 5 s (SB 5 s) magnesium samples.</p>
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<p>Comparison of friction curves for untreated (DP), laser-textured (LT), and sandblasted (SB) surfaces measured in air (black ○) and under lubrication with Hank’s solution (red □).</p>
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<p>Comparison of steady-state coefficient of friction (COF) for untreated (DP), laser-textured (LT), and sandblasted (SB) magnesium surfaces measured in air and under lubrication with Hank’s solution.</p>
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<p>Wear scar SEM micrographs in air for untreated (<b>a</b>), laser-textured (<b>b</b>), and sandblasted (<b>c</b>–<b>f</b>) magnesium surfaces. The insets show the wear scar on the counter body, Al<sub>2</sub>O<sub>3</sub> ball.</p>
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<p>SEM micrographs of wear scars under lubrication in Hank’s solution for untreated (<b>a</b>), laser-textured (<b>b</b>), and sandblasted (<b>c</b>–<b>f</b>) magnesium surfaces. The insets show the wear scar on the counter body, Al<sub>2</sub>O<sub>3</sub> ball.</p>
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<p>Wear volumes of untreated, laser-textured, and sandblasted magnesium surfaces in air and under lubrication in Hank’s solution.</p>
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<p>Potentiodynamic curves for polished (DP), laser-textured (LT), and sandblasted for 2–30 s (SB 2 s, SB 5 s, SB 10 s, and SB 30 s) magnesium samples measured in simulated physiological Hank’s solution at pH = 7.8 and room temperature.</p>
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