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Article
Multidimensional Separation by Magnetic Seeded Filtration: Experimental Studies
Powders 2023, 2(3), 588-606; https://doi.org/10.3390/powders2030037 - 01 Aug 2023
Viewed by 396
Abstract
The current state of separation technology often neglects the multidimensional nature of real particle systems, which are distributed not only in terms of size, but also in terms of other properties, such as surface charge. Therefore, the aim of this study is to [...] Read more.
The current state of separation technology often neglects the multidimensional nature of real particle systems, which are distributed not only in terms of size, but also in terms of other properties, such as surface charge. Therefore, the aim of this study is to experimentally investigate the applicability of magnetic seeded filtration as a multidimensional separation process. Magnetic seed particles are added to a multisubstance suspension, and a selective heteroagglomeration with the nonmagnetic target particles is induced, allowing for an easy subsequent magnetic separation. The results show that high separation efficiencies can be achieved and that the parameters pH and ionic strength govern the agglomeration process. Selective separation based on surface charge was observed, but undesirable heteroagglomeration processes between the target particles lead to a loss of selectivity. Particle size was clearly identified as a second relevant separation feature, and its partially opposite influence on collision frequency and collision efficiency was discussed. Finally, experimental data of multidimensional separation are presented, in which a size-distributed two-substance suspension is separated into defined size and material fractions in a single process step. This study highlights the need for multidimensional evaluation in general and the potential of magnetic seeded filtration as a promising separation technique. Full article
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Article
Dielectric Performance of UHMWPE-MgFe2O4 Composites Depending on Polymer Crystallinity, and the Concentration and Size of Mechanochemically Synthesized Ferrite Particles
Powders 2023, 2(3), 578-587; https://doi.org/10.3390/powders2030036 - 01 Aug 2023
Viewed by 266
Abstract
Mechanochemically synthesized particles of two types of magnesium ferrites, one of which with structural distortions and an average size of 170 nm, and another that is highly crystalline with an average size of 900 nm, were introduced into a matrix of ultra-high-molecular-weight polyethylene [...] Read more.
Mechanochemically synthesized particles of two types of magnesium ferrites, one of which with structural distortions and an average size of 170 nm, and another that is highly crystalline with an average size of 900 nm, were introduced into a matrix of ultra-high-molecular-weight polyethylene via the milling processing. The final material has been formed by hot pressing mechanocomposites based on ultra-high-molecular-weight polyethylene and magnesium ferrite particles of various fineness and concentration. Structural characteristics were studied using scanning electron microscopy, differential scanning calorimetry and X-ray diffraction analysis. The dielectric properties of the obtained composites were analyzed by testing the frequency dependence of the permeability, dielectric losses, and conductivity. The effect of filler concentration and particle size, as well as the crystallinity of the polymer, on the dielectric properties of the composite material were studied. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Mechanosynthesis, Structure and Photoluminescent Properties of the Pr3+ Doped LiNbO3, LiNbO3:Mg, LiTaO3 Nanopowders
Powders 2023, 2(3), 562-577; https://doi.org/10.3390/powders2030035 - 21 Jul 2023
Viewed by 188
Abstract
In the current work, nanocrystalline powders with different compositions, namely Li0.98Pr0.02NbO3, Li0.93Pr0.02Mg0.05NbO3 and Li0.98Pr0.02TaO3 were synthesized for the first time using the method of high-energy [...] Read more.
In the current work, nanocrystalline powders with different compositions, namely Li0.98Pr0.02NbO3, Li0.93Pr0.02Mg0.05NbO3 and Li0.98Pr0.02TaO3 were synthesized for the first time using the method of high-energy ball milling of the starting materials (Li2CO3, Nb2O5, Ta2O5, MgO, Pr6O11), followed by high-temperature annealing. XRD data analysis confirmed the absence of parasitic phases in the obtained nanocrystalline compounds. The estimated particle sizes ranged from 20 to 80 nm. From the obtained nanopowders, ceramic samples were prepared using specially developed equipment, which allowed for pressing at elevated temperatures with a simultaneous application of a constant electric field. The obtained photoluminescence spectra exhibit characteristic features of Pr3+ ions in the crystal structure of LiNbO3 and LiTaO3 and are most efficiently excited by UV light. Samples pressed with an electric field application show higher intensity of photoluminescence. Investigations of the temperature dependence of electrical conductivity of the Li0.98Pr0.02NbO3 sample, pressed with the application of an electric field, indicate that the conductivity mechanism is similar to that of LiNbO3 single crystals and, at high temperatures, is attributed to the lithium conduction mechanism. Full article
(This article belongs to the Special Issue Feature Papers in Powders 2023)
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Article
Mechanochemical Synthesis and DC Electrical Conductivity of PANI-Based MWCNT Containing Nanocomposites with Te0 and Bi2Te3 Thermoelectric Nanophase
Powders 2023, 2(3), 540-561; https://doi.org/10.3390/powders2030034 - 14 Jul 2023
Viewed by 308
Abstract
Nowadays, the search for the coupled polymer nanocomposite thermoelectrics that exhibit a high value of thermoelectric figure of merit (ZT) and similar behaviour of physical properties for the use as legs of thermoelectric cells is a current challenge. The direct current (DC) conductivity [...] Read more.
Nowadays, the search for the coupled polymer nanocomposite thermoelectrics that exhibit a high value of thermoelectric figure of merit (ZT) and similar behaviour of physical properties for the use as legs of thermoelectric cells is a current challenge. The direct current (DC) conductivity is one of the three important components of thermoelectric figure of merit. The aim of this study was to obtain PANI-based nanothermoelectrics with Te0 and Bi2Te3 nanoparticles and MWCNT by mechanochemical methodology and to investigate the dependency of their DC electrical conductivity on temperature in the 298–353 K range using the Arrhenius and Mott’s variable range hopping (VRH) models. Inorganic Te0 and Bi2Te3 nanoparticles were pre-synthesized by the available and environmentally friendly method using a commercial tellurium powder. The samples obtained were characterized by X-ray diffractometry (XRD), IR and UV-Vis spectroscopy. The XRD study of ES-PANI/Te0 (4.4 wt% Te0) and ES-PANI/Bi2Te3 (2.9 wt% Bi2Te3) nanocomposites found that the nanoparticle average size was 32 nm and 17 nm, respectively. The DC conductivity study of the samples with different nanophase content (2.1, 4.4, 10.2 wt% Te0, 1.5, 2.9, 7.3 wt% Bi2Te3, 1.5 wt% MWCNT) by the two points measurement method reveals the following: (a) the presence of inorganic nanophase reduces the conductivity compared to the matrix, (b) the addition of MWCNT in ES-PANI increases its electrical conductivity, (c) the conductivity of ES-PANI/Te0 as well as ES-PANI/Bi2Te3 nanocomposite rises with the increasing inorganic nanophase content, (d) the observed increase in the electrical conductivity of MWCNT-based nanocomposites with increasing inorganic nanophase content is interrupted by a characteristic area of decrease in its value at average values of inorganic nanoparticles content (at Te0 content of 4.4 wt%, at Bi2Te3 content of 2.9 wt%), (e) a similar DC conductivity behaviour in ES-PANI/Te0—ES-PANI/Bi2Te3 and ES-PANI/Te0-MWCNT—ES-PANI/Bi2Te3-MWCNT nanocomposite pairs is observed. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Effects of Process Parameters on Cold Spray Additive Manufacturing of Quasicrystalline Al93Fe3Cr2Ti2 Alloy
Powders 2023, 2(3), 525-539; https://doi.org/10.3390/powders2030033 - 14 Jul 2023
Viewed by 343
Abstract
Quasicrystalline Al93Fe3Cr2Ti2 (at.%) gas-atomized powders, which exhibit a metastable composite microstructure, were used to produce coatings by cold spray additive manufacturing processing (CSAM) using different processing parameters. The metastable composite microstructure provides the Al93Fe [...] Read more.
Quasicrystalline Al93Fe3Cr2Ti2 (at.%) gas-atomized powders, which exhibit a metastable composite microstructure, were used to produce coatings by cold spray additive manufacturing processing (CSAM) using different processing parameters. The metastable composite microstructure provides the Al93Fe3Cr2Ti2 alloy with excellent mechanical properties. At the same time, the metastability of its microstructure, achieved by the high cooling rates of the gas atomization process, limits the processability of the Al93Fe3Cr2Ti2 powder. The purpose of this study was to investigate the effect of process parameters on the CSAM of quasicrystalline Al93Fe3Cr2Ti2 powder. The powder was sieved and classified to a size range of −75 µm. Using N2 carrier gas combined with different temperatures, pressures, nozzle apertures, and deposition substrate conditions, cold-sprayed coatings were produced. The porosity and thickness of the coatings were evaluated by image analyses. By SEM, XRD, DSC, and TEM, the microstructure was identified, and by Vickers microhardness, the mechanical properties of the coatings were investigated. Dense (≤0.50% porosity) and thick (~185.0 µm) coatings were obtained when the highest pressure (4.8 MPa), highest temperature (475 °C), and lowest nozzle aperture (A) were used in combination with an unblasted substrate. The SEM, XRD, and DSC data showed that the composite powder’s microstructure was retained in all coatings with no decomposition of the metastable i-phase into equilibrium crystalline phases. Supporting these microstructural results, all coatings presented a high and similar hardness of about 267 ± 8 HV. This study suggests that the CSAM process could, therefore. produce metastable quasicrystalline Al93Fe3Cr2Ti2 coatings with a composite microstructure and high hardness. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Cu-10 wt.% Al Alloys Produced by Spark Plasma Sintering of Powder Blends and a Mechanically Alloyed Mixture: A Comparative Investigation
Powders 2023, 2(3), 515-524; https://doi.org/10.3390/powders2030032 - 10 Jul 2023
Viewed by 343
Abstract
Cu–Al bronzes are interesting metallic materials, demonstrating higher hardness, higher wear resistance, higher corrosion resistance and a lower friction coefficient as compared with unalloyed copper. The powder metallurgy approach to the fabrication of these alloys presents opportunities to tailor their phase composition and [...] Read more.
Cu–Al bronzes are interesting metallic materials, demonstrating higher hardness, higher wear resistance, higher corrosion resistance and a lower friction coefficient as compared with unalloyed copper. The powder metallurgy approach to the fabrication of these alloys presents opportunities to tailor their phase composition and grain size. In the present work, the structural characteristics, phase composition and properties of Cu-10 wt.% Al alloys obtained by spark plasma sintering (SPS) of powder blends and a powder obtained by mechanical alloying (based on Cu(Al) solid solution) are reported. Alloys with different interaction degrees between the metals were obtained by SPS. The blends demonstrated better sinterability than the mechanically alloyed powder: a nearly fully dense alloy was obtained by SPS of the blend at 480 °C, whereas a temperature of 800 °C was necessary to consolidate the mechanically alloyed powder. The hardness and electrical conductivity of the sintered alloys were comparatively analyzed. It was shown that the Cu-10 wt.% Al alloys obtained without the mechanical alloying stage possess hardness and electrical conductivity comparable to those of the alloys obtained from the mechanically milled powder. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Wet Ball Milling Applied to Production of Composites and Coatings Based on Ti, W, and Nb Carbides
Powders 2023, 2(2), 499-514; https://doi.org/10.3390/powders2020031 - 15 Jun 2023
Viewed by 463
Abstract
The paper demonstrates the potential of wet ball milling of metals for the synthesis of various carbides and carbohydrides. The work reports on multicomponent carbides formed in Ti-(Cu/Fe/Si)-C, W-Fe-C, and Nb-(Cu/Fe/Si/Al)-C systems, as well as metastable or high-temperature intermetallics formed in Ti-Si, Nb-Si, [...] Read more.
The paper demonstrates the potential of wet ball milling of metals for the synthesis of various carbides and carbohydrides. The work reports on multicomponent carbides formed in Ti-(Cu/Fe/Si)-C, W-Fe-C, and Nb-(Cu/Fe/Si/Al)-C systems, as well as metastable or high-temperature intermetallics formed in Ti-Si, Nb-Si, Nb-Al, and Nb-Cu-Fe systems, which are stabilized with interstitial carbon. The formation of phase composition of powders fabricated under mechanochemical synthesis and subsequent thermal treatment has been studied. The as-fabricated powders have been used to produce bulk compacts and to apply wear-resistant coatings on steel (iron). Full article
(This article belongs to the Special Issue Particle Technologies)
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Communication
Conceptual Design of a Pilot Process for Manufacturing Aluminum-Based Intermetallic Compound Powders
Powders 2023, 2(2), 493-498; https://doi.org/10.3390/powders2020030 - 15 Jun 2023
Viewed by 330
Abstract
The FeAl intermetallic compound is of great interest for industry due to its low density, low cost and high mechanical and corrosion resistance, so it can replace stainless steels and nickel-based alloys for some applications. In previous publications, the concept (principle) test for [...] Read more.
The FeAl intermetallic compound is of great interest for industry due to its low density, low cost and high mechanical and corrosion resistance, so it can replace stainless steels and nickel-based alloys for some applications. In previous publications, the concept (principle) test for a novel FeAl powder manufacturing process has been shown. It consists mainly of the following stages: (a) metallic strip manufacture through rapid solidification, (b) water vapor exposure of these metallic strips for their disintegration and powder generation and (c) powder drying. Experimental tests were performed for 2 g of the FeAl intermetallic compound. However, this process can be extended to manufacture any other intermetallic compound containing aluminum, such as TiAl, NiAl, CoAl or any other that can be obtained from every element that can combine with aluminum, if the aluminum content is between 55 and 60 at.%. Nowadays, this process is at technology readiness level (TRL) 3. Therefore, in this paper, a process equipment up-scaling configuration for producing up to 15 kg powder is proposed. This manufacturing process is an industrial alternative to those commonly used to produce powders of this type of intermetallic compounds, such as mechanical alloying (MA). Moreover, several alternatives for employing renewable energy sources are given, making it even more environmentally sustainable. Full article
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Article
Hot Consolidation of Titanium Powders
Powders 2023, 2(2), 484-492; https://doi.org/10.3390/powders2020029 - 13 Jun 2023
Viewed by 312
Abstract
A novel method of the hot consolidation metal powders with shear deformation is proposed. The powders were encapsulated into tight containers and compacted after short-term heating in a furnace preheated to 900 °C. The method prevents powder oxidation, peripheral spalling and ensures the [...] Read more.
A novel method of the hot consolidation metal powders with shear deformation is proposed. The powders were encapsulated into tight containers and compacted after short-term heating in a furnace preheated to 900 °C. The method prevents powder oxidation, peripheral spalling and ensures the removal of the oxide films from the powder surfaces. Commercial titanium powders of different dispersivities and impurity concentrations were hot-compacted. The microstructure, hardness and bending strength of the compacts were investigated. The compacts from fine PTOM-1 powder, containing 0.32% of hydrogen, reveal the greatest values of the hardness and bending strength. Additional annealing results in 60% increase in the bending strength. Full article
(This article belongs to the Special Issue Feature Papers in Powders 2023)
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Article
Exploring the Effects of Cramped-Impact-Type Mechanical Action on Active Pharmaceutical Ingredient (Levofloxacin)—Prospects for Pharmaceutical Applications
Powders 2023, 2(2), 464-483; https://doi.org/10.3390/powders2020028 - 09 Jun 2023
Viewed by 624
Abstract
Mechanochemistry is one of the ten great discoveries of green chemistry methods for synthesizing new substances. A drug substance from the fluoroquinolone group was exposed to high-intensity mechanical impacts using a laboratory knife mill for 21 min and constantly monitored by analyzing samples [...] Read more.
Mechanochemistry is one of the ten great discoveries of green chemistry methods for synthesizing new substances. A drug substance from the fluoroquinolone group was exposed to high-intensity mechanical impacts using a laboratory knife mill for 21 min and constantly monitored by analyzing samples extracted every 3 min with DLS, SLS, LALLS, 2D-LS, optical and digital microscopy, FTIR, and Spirotox methods. A dispersity phenomenon was detected in an area where catastrophic dislocations formed and multiplied via laser methods. The positive correlation between the temperature of deformation and stress was demonstrated, similar to a typical stress–strain curve of a Bochvar–Oding curve and Young’s modulus: the angular coefficient of the straight section to OX was tgα = 10 min−1. Z-Average, ζ-potential, and polydispersity index dependences were represented as discontinuous periodic oscillations analogous to the defect and impurity transitions near the dislocation core. Deformation r from the high-intensity mechanical impact resulted in covalent bonds showing hyper- and hypochromic effects under FTIR spectra, a bathochromic shift of the maximum, and an oscillation emission at 3240 cm−1. A 2D-LS fingerprint diagram obtained via the topological convolution of the light scattering matrix made it possible to distinguish the off-loading samples from the native substance. The investigation of the dissolution kinetics in water via laser diffraction led to conclusions about the limiting diffusion stage and the acceleration of the mechanoactivation of the solid body’s dissolution under both linear and plastic deformation. The acceleration of obsEa of the cell death process in the temperature range from 296 to 302 K indicated a significant (2.5-fold) decrease in the toxicity of the aqueous 9 mM (1:3) sample solution at 21 min compared to that of the native levofloxacin. Adherence to the mechanochemistry laws provides an opportunity for drug repositioning to change their brand status by identifying new physicochemical and biological properties. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Interaction of Polyphenylsilsesquioxane with Various β-Diketonate Complexes of Titanium by Mechanochemical Activation
Powders 2023, 2(2), 445-463; https://doi.org/10.3390/powders2020027 - 08 Jun 2023
Viewed by 365
Abstract
In the present work, we studied the interaction of polyphenylsilsesquioxane with various β-diketonate complexes of titanium by mechanochemical activation. Polyphenylsilsesquioxane, bis-(2,4-pentanedionate) titanium dichloride, bis-(1-phenyl-1,3-butanedionate) titanium dichloride, and bis-(1,3-diphenyl-1,3-propanedionate) titanium dichloride were used as starting reagents. Various chemical and physicochemical methods of analysis were [...] Read more.
In the present work, we studied the interaction of polyphenylsilsesquioxane with various β-diketonate complexes of titanium by mechanochemical activation. Polyphenylsilsesquioxane, bis-(2,4-pentanedionate) titanium dichloride, bis-(1-phenyl-1,3-butanedionate) titanium dichloride, and bis-(1,3-diphenyl-1,3-propanedionate) titanium dichloride were used as starting reagents. Various chemical and physicochemical methods of analysis were used to study the synthesis products. The composition of the obtained compounds has been determined. It is shown that under conditions of mechanochemical activation, high-molecular-weight products with a Si/Ti ratio different from the specified ones are formed. In addition, under the action of mechanical stresses, the initial titanium complexes (except for acetylacetonate complex) polymerize with the formation of coordination of high-molecular-weight compounds, which are destroyed by the addition of ethyl alcohol. It has been established that with an increase in the volume of the organic ligand, titanium atoms enter the polymer siloxane chain to a lesser extent. This work is aimed at finding efficient and environmentally friendly methods for the synthesis and modification of organometallic macromolecular compounds. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Morphological Changes in Betulin Particles as a Result of Polymorphic Transformations, and Formation of Co-Crystals under Heating
Powders 2023, 2(2), 432-444; https://doi.org/10.3390/powders2020026 - 05 Jun 2023
Viewed by 523
Abstract
Changes in the morphology of betulin crystals during heating at selected temperatures corresponding to polymorphic transformations were investigated. It was shown that the prismatic crystals of starting betulin form III were converted into needles at 120 °C after water removal, followed by the [...] Read more.
Changes in the morphology of betulin crystals during heating at selected temperatures corresponding to polymorphic transformations were investigated. It was shown that the prismatic crystals of starting betulin form III were converted into needles at 120 °C after water removal, followed by the III→II polymorphic transformation. During further heating up to 180 °C, the whiskers of betulin form I were grown. Experiments on betulin heating in the presence of dicarboxylic acids, adipic or suberic showed that the morphological changes can serve as a test for the formation of cocrystals. According to morphological changes, the formation of cocrystals of betulin with adipic acid under heating was identified. The interaction of adipic acid vapor with the surface of betulin crystals was suggested. In contrast, morphological changes in the mixture of betulin and suberic acid under heating provided only the evidence of polymorphic transformations of the components. The results on cocrystal formation by heating were compared with the preparation of cocrystals by the liquid-assistance grinding method. Despite the fact that polymorphic forms with a high surface area were formed when betulin was heated, dissolution studies showed that the starting betulin polymorph III exhibited the highest dissolution rate in comparison with betulin polymorphs obtained under heating. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Mechanochemically Assisted Synthesis of Cu–Ag Microflakes
Powders 2023, 2(2), 421-431; https://doi.org/10.3390/powders2020025 - 01 Jun 2023
Viewed by 447
Abstract
In this work, a simple, inexpensive, and eco-friendly synthesis method of Cu−Ag microflakes has been developed. Firstly, Cu nanoparticles were synthesized by the reduction of copper nitrate in ethylene glycol at 180 °C in the presence of NaOH. The as-synthesized Cu powder was [...] Read more.
In this work, a simple, inexpensive, and eco-friendly synthesis method of Cu−Ag microflakes has been developed. Firstly, Cu nanoparticles were synthesized by the reduction of copper nitrate in ethylene glycol at 180 °C in the presence of NaOH. The as-synthesized Cu powder was then dispersed in a mixture of ethyl alcohol and a dispersant followed by the mechanochemical treatment of the dispersion in a ball mill resulting in the formation of Cu flakes of approximately 0.2 μm thick and 2.7 μm lateral size. Next, by adding AgNO3 dissolved in H2O into the Cu particle dispersion, the bimetallic Cu−Ag microflakes were prepared. The particles so prepared were investigated by X-ray phase analysis and electron microscopy. It was shown that the Cu−Ag bimetallic particles were also flake-like in shape and similar in size to the original Cu microflakes. The effect of synthesis conditions, including parameters of mechanochemical processing, on thickness, size, and uniformity of the bimetallic microflakes was studied. The results obtained in this study were compared with those obtained by wet chemical synthesis alone. The flake-like Cu–Ag particles are supposed to be used in the manufacture of conductive pastes, adhesives, and composites for printed electronics. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Mechanical Alloying of Copper- or Iron-Based Metallic Binders for Diamond Tools
Powders 2023, 2(2), 403-420; https://doi.org/10.3390/powders2020024 - 22 May 2023
Viewed by 521
Abstract
Powder mixtures based on copper or iron are used as metal binder materials in the manufacturing of abrasive and cutting tools. This article discusses some aspects and possibilities of using a high-energy ball milling process to modify the structure and properties of Cu-Sn, [...] Read more.
Powder mixtures based on copper or iron are used as metal binder materials in the manufacturing of abrasive and cutting tools. This article discusses some aspects and possibilities of using a high-energy ball milling process to modify the structure and properties of Cu-Sn, Cu-Sn-Ti and Fe-Ti powders, their sintered materials and composites with diamond. The structures of powders and sintered materials, as well as the binder-to-diamond interfaces in metal matrix composites with diamond fillers, were studied by XRD analysis, scanning electron microscopy and X-ray spectroscopy. Tribological properties and thermal stability of materials in the temperature range of 250–800 °C were investigated. Various mechanisms of dispersion strengthening during the heating of sintered materials are described. It is shown that due to the grain boundary distribution of titanium, it is possible to obtain single-phase powders in the form of a supersaturated solid solution of CuSn20Ti5 and FeTi20, which ensure the formation of thermally hardened alloys with a microhardness of 357–408 HV and 561–622 HV, respectively, in the temperature range of 350–800 °C. The wear resistance of sintered powder alloys increases more than twice. Furthermore, the simultaneous enhancement in both the strength and ductility of metal–diamond titanium-containing composites is achieved through the nanostructural state and the formation of a thin layer (up to 2 μm) of titanium carbide at the interface between the metal matrix and diamond. The developed alloy shows great potential as a binder in diamond tools which are designed for machining abrasive materials. Full article
(This article belongs to the Special Issue Particle Technologies)
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Article
Orthorhombic Crystal Structure of Grossular Garnet (Suva Česma, Western Serbia): Evidence from the Rietveld Refinement
Powders 2023, 2(2), 387-402; https://doi.org/10.3390/powders2020023 - 18 May 2023
Viewed by 674
Abstract
The grossular garnet from rodingite-type rock from the Suva Česma area in western Serbia is characterized with its weak anisotropic nature. Because its anisotropy could indicate a non-cubic lower symmetry, SEM-EDS and Rietveld powder refinement methods were used. The SEM-EDS results have shown [...] Read more.
The grossular garnet from rodingite-type rock from the Suva Česma area in western Serbia is characterized with its weak anisotropic nature. Because its anisotropy could indicate a non-cubic lower symmetry, SEM-EDS and Rietveld powder refinement methods were used. The SEM-EDS results have shown that the garnet has a (Ca3.00Mn0.01)3.01(Al1.82Fe0.15Ti0.02)1.99(Si2.97Al0.03)3.00O12 chemical composition (i.e., Grs91Adr08), which can be more specifically explained as ferric iron containing grossular. The next step further used Rietveld powder refinements of the various crystal structures in the Ia‾3d, R‾3c, R‾3, I41/a, Fddd, C2/c, and I‾1 space groups as well as a single mixture, which was followed by a comparative analysis of the R-values, site occupancy factors, and bond lengths and angles. The synthesis of these results showed both that the studied grossular garnet is not cubic and that it crystallized in the disordered Fddd space group with the final RB = 5.29% and RF = 1.75%. It was presumed that the grossular formed at temperatures between 150 and ~600 °C. Full article
(This article belongs to the Special Issue Feature Papers in Powders)
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