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The fashion industry's reliance on dyes contributes significantly to environmental pollution, which disturbs the ecological balance. To address this issue, we used ZnO/Mg combined with activated carbon (AC) at various concentrations (0.1 g, 0.5 g, and 1 g), which were synthesized via sol-gel and mechanical alloying processes. The analysis of X-ray diffraction shows reduced crystallite size, with d-spacing change ( → d ← ) for ZnO/Mg/AC (0.5 g) and ( ← d → ) for ZnO/Mg/AC (1 g), respectively. The results of the IR spectrum indicated the main vibrations is MgO and Zn-O bonds at wave numbers 673 cm -1 and 467 cm -1 . It was found that ZnO/Mg/AC (1 g) shows high degradation performance D % : 86.15% as a consequence of reduced crystallite size: 22.67 nm, decreased skin depth: 0.002 cm, widening of optical phonon vibration ( Δ ( LO - TO ) ): 252 cm -1 and increased E g : 4.6 eV as a function AC variation. Moreover, the finding of high photocatalytic performance ≥  80% for 0.25 mL MB dissolved in 250 mL distilled water is obtained from all composites. Based on these results, ZnO/Mg/AC shows potential as a photocatalyst to solve the MB waste problem., (© 2024. The Author(s), under exclusive licence to the European Photochemistry Association, European Society for Photobiology.)

This study investigates the antibacterial activity and spectral characteristics of Cu-doped ZnO nanoparticles synthesized via the gelatin-based sol-gel method, focusing on their potential biomedical applications. Zn₁₋ₓCuₓO nanoparticles (x = 0.0, 0.01, 0.03, and 0.05) were fabricated using this method. The incorporation of copper dopants into the ZnO matrix significantly influences both the crystalline structure and spectral properties of the nanoparticles. X-ray diffraction analysis confirms the presence of a wurtzite structure without any pyrochlore phase. The broadening of spectral features indicates modifications in lattice parameters and elastic constants. XRD results reveal that adding Cu to the ZnO lattice causes a decrease in crystallite size from 32 to 18 nm. Transmission electron microscopy shows spherical-shaped ZnO nanoparticles with sizes ranging from 30 to 40 nm. Moreover, Cu-doped ZnO nanoparticles exhibit considerable inhibition against bacterial growth. Adding Cu enhances the antibacterial activity of ZnO nanoparticles, suggesting their potential in biomedical applications. Overall, these findings highlight the promising prospects of sol-gel synthesized Cu-doped ZnO nanoparticles in the biomedical field., Competing Interests: The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2024 The Authors.)

A series ofCd0.45Co0.55Fe2-yEuyO4( y = 0.0, 0.1, 0.2, 0.3) spinel nanoferrites (SNFs) were synthesized using a self-igniting process and employed as electrode materials for supercapacitor applications. The results demonstrated the formation of a single SNFs phase, as shown by the XRD data. The crystallite size lies between the range of 29.30-51.12 nm. The porosity percentage is within the range of 31.37%-32.99%. Rietveld refinement of XRD and Raman analysis revealed the pure spinel phase and no secondary phase was observed. The saturation magnetization and magnetic anisotropy were also decreased with the addition of Eu 3+ in Cd-Co SNFs. The high coercive field was enhanced for Eu 3+ doping as compared to pure Cd-Co SNFs. The dielectric constant was improved with the substitution of Eu 3+ in Cd-Co SNFs. The dielectric tangent loss was reduced with the doping of Eu 3+ . The electrochemical performance of the Eu 3+ doped Cd-Co SNFs achieved an impressive maximum specific capacitance at a lower scan rate. Based on these findings, the outstanding electrochemical performance of the Eu 3+ doped Cd-Co SNFs suggests their potential as promising materials for high-frequency, magnetic ferrofluid, and supercapacitor electrodes., (© 2024 IOP Publishing Ltd.)

This research investigates the structural, morphological, and optical properties of Cadmium Selenide (CdSe) thin films deposited via the Chemical Bath Deposition (CBD) Technique, focusing on the impact of Iron (Fe) doping. Using Cadmium Chloride (CdCl 2 ) and Ferrous chloride (FeCl 2 ) as precursor materials, the research investigates how Fe doping affects the structural and photoelectric characteristics of the films. Employing various characterization methods including X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Fourier-Transform Infrared Spectroscopy (FTIR), and UV-Vis NIR spectroscopy, the study provides a comprehensive analysis of the films. XRD analysis confirms the formation of a cubic structure with a predominant orientation along the (111) plane, consistent with XRD peaks. Additionally, XRD data reveals the degradation of thin films post-annealing. Crystalline size and strain are determined using the Debye-Scherrer and Wilson formulae, while lattice constant and Size-strain plots are derived from X-ray line broadening. The average crystallite size ranges from 12 to 21 nm. Optical band gaps are found to be 2.25 eV, 2.91 eV, 2.87 eV, and 2.85 eV for the samples. Interestingly, a decrease in crystal size with increasing doping concentration correlates with a reduction in bandgap. This investigation offers valuable insights into the fabrication and characterization of CdSe thin films, particularly highlighting the impact of Fe doping on their structural and optical properties. Overall, this study provides valuable insights into the fabrication and characterization of CdSe thin films, emphasizing the importance of precise doping control for tailoring material properties and advancing their applications in photovoltaic and optoelectronic devices., Competing Interests: The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2024 The Authors.)

The supercritical hydrothermal synthesis of nanomaterials has gained significant attention due to its straightforward operation and the excellent performance of the resulting products. In this study, the supercritical hydrothermal method was used with Zn(CH 3 COO) 2 ·2H 2 O as the precursor and deionized water and ethanol as the solvent. Nano-ZnO was synthesized under different reaction temperatures (300~500 °C), reaction times (5~15 min), reaction pressures (22~30 MPa), precursor concentrations (0.1~0.5 mol/L), and ratios of precursor to organic solvent (C 2 H 5 OH) (2:1~1:4). The effects of synthesis conditions on the morphology and size of ZnO were studied. It was found that properly increasing hydrothermal temperature and pressure and extending the hydrothermal time are conducive to the more regular morphology and smaller size of ZnO particles, which is mainly achieved through the change of reaction conditions affecting the hydrothermal reaction rate. Moreover, the addition of ethanol makes the morphology of nano-zno more regular and significantly inhibits the agglomeration phenomenon. In addition to the change in physical properties of the solvent, this may also be related to the chemical bond established between ethanol and ZnO. The results show that the optimum synthesis conditions of ZnO are 450 °C, 26 MPa, 0.3 mol/L, 10 min, and the molar ratio of precursor to ethanol is 1:3.

The layered double hydroxides (LDHs) of transition metals are of great interest as building blocks for the creation of composite photocatalytic materials for hydrogen production, environmental remediation and other applications. However, the synthesis of most LDHs is reported only by the conventional coprecipitation method, which makes it difficult to control the catalyst's crystallinity. In the present study, ZnCr- and NiCr-LDHs have been successfully prepared using a facile hydrothermal approach. Varying the hydrothermal synthesis conditions allowed us to obtain target products with a controllable crystallite size in the range of 2-26 nm and a specific surface area of 45-83 m 2 ∙g -1 . The LDHs synthesized were investigated as photocatalysts of hydrogen generation from aqueous methanol. It was revealed that the photocatalytic activity of ZnCr-LDH samples grows monotonically with the increase in their average crystallite size, while that of NiCr-LDH ones reaches a maximum with intermediate-sized crystallites and then decreases due to the specific surface area reduction. The concentration dependence of the hydrogen evolution activity is generally consistent with the standard Langmuir-Hinshelwood model for heterogeneous catalysis. At a methanol content of 50 mol. %, the rate of hydrogen generation over ZnCr- and NiCr-LDHs reaches 88 and 41 μmol∙h -1 ∙g -1 , respectively. The hydrothermally synthesized LDHs with enhanced crystallinity may be of interest for further fabrication of their nanosheets being promising components of new composite photocatalysts.

Tricalcium aluminate is an important phase of Portland clinker. In this paper, three polymorphs of C 3 A were prepared by means of the solid-state synthesis method using intensive milling of the raw material mixture which was doped with various amounts of Na 2 O and sintered at a temperature of 1300 °C for 2 h. The final products were evaluated through X-ray diffraction using Rietveld analysis. The effect of the Na dopant content on the change in the crystalline structure of tricalcium aluminate was studied. It was proven that the given preparation procedure, which differed from other studies, was close to the real conditions of the formation of Portland clinker, and it was possible to prepare a mixture of different polymorphs of calcium aluminate. Fundamental changes in the crystal structure occurred in the range of 3-4% Na, when the cubic structure changes to orthorhombic. At a dosage of Na dopant above 4%, the orthorhombic structure changes to a monoclinic structure. There are no clearly defined boundaries for the existence of individual C 3 A phases; these phases arise at the same time and overlap each other in the areas of their formation at different Na doses.

Lactose crystallization during storage deteriorates reconstitution performance of milk powders, but the relationship between lactose crystallization and reconstitution is inexplicit. The objective of this study is to characterize crystalline lactose in the context of formulation and elucidate the complex relationship between lactose crystallization and powder functionality. Lactose in Skim Milk Powder (SMP), Whole Milk Powder (WMP) and Fat-Filled Milk Powder (FFMP) stored under 23 %, 53 % and 75 % Relative Humidity (RH) at 25  ℃ for four months was compared. Lactose, surface chemistry and microstructure of FFMP stored at 25 ℃ and 40 ℃ at 23 % to 75 % RH for four months were also analyzed and interpreted. At the same RH, FFMP crystallized in the same pattern as WMP. At 53 % RH, FFMP and WMP differentiated from SMP in terms of lactose morphology as well as the ratio between anhydrous α-lactose and anhydrous β-lactose. Lactose remained amorphous at 23 % RH, crystallized predominantly to α/β-lactose (1:4) at 40 to 58 % RH and to α-lactose monohydrate at 75 % RH. The crystallinity index was similar for all powders containing crystalline lactose. The estimated crystallite size increased from approx. 0.1 to 20 µm with increasing RH and temperature. When amorphous lactose crystallized into crystals below approx. 0.1 µm at 25 °C and 43 % RH, the microstructure and surface lipid were comparable to that of the reference powder. This powder reconstituted into a stable suspension system comparable to that of reference (well performing) powders. These results demonstrate that crystallite size is the key property linking lactose crystallization and reconstitution. Our finding thus indicates limiting crystallite size is important for maintaining desired product quality., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 The Authors. Published by Elsevier Ltd.. All rights reserved.)

Hydroxyapatite (HAp) [Ca 10 (PO 4 ) 6 (OH) 2 ] is remarkably similar to the hard tissue of the human body and the uses of this material in various fields in addition to the medical sector are increasing day by day. In this research, mustered oil, soybean oil, as well as coconut oil were employed as liquid media for synthesizing nanocrystalline HAp using a wet chemical precipitation approach. The X-ray diffraction (XRD) study verified the crystalline phase of the HAp in all the indicated media and discovered similarities with the standard database. Several prominent models such as the Scherrer's Method (SM), Halder-Wagner Method (HWM), linear straight-line method (LSLM), Williamson-Hall Method (W-M), Monshi Scherrer Method (MSM), Size-Strain Plot Method (SSPM), Sahadat-Scherrer Method (S-S) were applied for the determination of crystallite size. The stress, strain, and energy density were also computed from the above models. All the models, without the Linear straight-line technique of Scherrer's equation, resulted in an appropriate value of crystallite size for synthesized products. The calculated crystallite sizes were 6.5 nm for HAp in master oil using Halder-Wagner Method, and 143 nm for HAp in coconut oil using the Scherrer equation which were the lowest and the largest, respectively., Competing Interests: The authors declare the following financial interests/personal relationships which may be considered as potential competing interests:There is nothing to declare If there are other authors, they declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2024 The Authors.)

Experiments were conducted to reveal the nanostructure evolution in additively manufactured (AMed) 316L stainless steel due to severe plastic deformation (SPD). SPD-processing was carried out using the high-pressure torsion (HPT) technique. HPT was performed on four different states of 316L: the as-built material and specimens heat-treated at 400, 800 and 1100 °C after AM-processing. The motivation for the extension of this research to the annealed states is that heat treatment is a usual step after 3D printing in order to reduce the internal stresses formed during AM-processing. The nanostructure was studied by X-ray line profile analysis (XLPA), which was completed by crystallographic texture measurements. It was found that the as-built 316L sample contained a considerable density of dislocations (10 15 m -2 ), which decreased to about half the original density due to the heat treatments at 800 and 1100 °C. The hardness varied accordingly during annealing. Despite this difference caused by annealing, HPT processing led to a similar evolution of the microstructure by increasing the strain for the samples with and without annealing. The saturation values of the crystallite size, dislocation density and twin fault probability were about 20 nm, 3 × 10 16 m -2 and 3%, respectively, while the maximum achievable hardness was ~6000 MPa. The initial <100> and <110> textures for the as-built and the annealed samples were changed to <111> due to HPT processing.

The influence of milling time and volume fraction of reinforcement on the morphology, microstructure, and mechanical behaviors of SiC p -reinforced AA2017 composite powder produced by high-energy ball milling (HEBM) was investigated. AA2017 + SiC p composite powder with different amounts of SiC particles (5, 10, and 15 vol%) was successfully prepared from gas-atomized AA2017 aluminum alloy powder with a particle size of <100 μm and silicon carbide (SiC) powder particles with an average particle size of <1 μm. An optical microscope (OM), X-ray diffraction (XRD), and scanning electron microscope (SEM) were utilized to characterize the microstructure of the milled composite powder at different milling periods. The results indicated that the SiC particles were homogeneously distributed in the AA2017 matrix after 5 h of HEBM time. The morphology of the particles transformed from a laminar to a nearly spherical shape, and the size of the milled powder particles reduced with increasing the content of SiC particles. The XRD analysis was carried out to characterize the phase constituents, crystallite size, and lattice strain of the composite powders at different milling periods. It was found that with increasing milling time and SiC volume fraction, the crystallite size of the aluminum alloy matrix decreased while the lattice strain increased. The average crystallite sizes were reduced from >300 nm to 68 nm, 64 nm, and 64 nm after 5 h of milling, corresponding to SiC contents of 5, 10, and 15 vol%, respectively. As a result, the lattice strain increased from 0.15% to 0.5%, which is due to significant plastic deformation during the ball milling process. XRD results showed a rapid decrease in crystallite size during the early milling phase, and the minimum grain size was achieved at a higher volume fraction of SiC particles. Microhardness tests revealed that the milling time has a greater influence on the hardness than the amount of SiC reinforcements. Therefore, the composite powder milled for 5 h showed an average microhardness three times higher than that of the unmilled powder particles.

This work is concerned with fabricating ferrite nanoparticles of nickel-zinc with the chemical formula: Ni 0.55 Zn 0.45 Fe 2-x Ce x O 4 , 0 ≤ x ≤ 0.011 by co-deposition technique and modifying their electrical, microscopic, spectroscopic, optical, electrical and dielectric properties as advanced engineering materials through doping with the cerium (Ce) element. XRD patterns displayed that the samples have a monophasic Cerium-Nickel-zinc (CNZ) spinel structure without other impurities for cerium concentration (x) ≤ 0.066. Both values of crystallite size and lattice parameters decrease from 33.643 to 23.137 nm and from 8.385 to 8.353 nm, respectively, with the increasing Ce ions substitution content from 0 to 0.066. SEM images indicate that grains of the fabricated compounds are smaller, more perfect, more homogeneous, and less agglomeration than those of the un-doped Ni-Zn nano-ferrites. The maximum intensity of first-order Raman spectral peaks (E g , F2g(2), A1g(2), and A1g(1)) of CNZ ferrite nanoparticles are observed at about (330, 475, 650, 695) cm -1 , respectively, that confirms the CNZ samples have the cubic spinel structure. The direct and indirect optical energy bandgaps of CNZ samples have a wide spectrum of values from semiconductors to insulators according to cerium concentration. The results showed that the values of dielectric constant, dielectric loss factor, and Ac conductivity and the conductivity transition temperature are sensitive to cerium ions content. AC conductivity exhibited by the CNZ samples has the semiconductor materials behavior, where the AC conductivity increases due to temperature or doping concentration. The results indicate that Ni 0.55 Zn 0.45 Fe 1.944 Ce 0.066 O 4 ferrite nanoparticles may be selected for optoelectronic devices, high-frequency circuits, and energy storage applications., (© 2023. The Author(s).)

Chromium (Cr)-doped cobalt ferrite nanoparticles were synthesized using a sol-gel autocombustion method, with the chemical formula CoCr x Fe 2x O 4 . The value of x ranged from 0.00 to 0.5 in 0.1 increments. X-ray diffraction analysis confirmed the development of highly crystalline cubic spinel structures for all samples, with an average crystallite size of approximately 40 to 45 nm determined using the Scherrer equation. Pellets were prepared using a traditional ceramic method. The magnetic and magnetostrictive properties of the samples were tested using strain gauge and VSM (vibrating sample magnetometer) techniques. The results of the magnetic and magnetostrictive tests showed that the chromium-substituted cobalt ferrites exhibited higher strain derivative magnitudes than pure cobalt ferrite. These findings indicated that the introduction of chromium into the cobalt ferrite structure led to changes in the material's magnetic properties. These changes were attributed to anisotropic contributions, resulting from an increased presence of Co 2+ ions at B-sites due to the chromium substitutions. In summary, this study concluded that introducing chromium into the cobalt ferrite structure caused alterations in the material's magnetic properties, which were explained by changes in the cationic arrangement within the crystal lattice. This study successfully explained these alterations using magnetization and coercivity data and the probable cationic dispersion.

Crystalline solid dispersions (CSDs) represent a thermodynamically stable system capable of effectively reducing the crystallite size of drugs, thereby enhancing their solubility and bioavailability. This study uses flavonoid drugs with the same core structures but varying numbers of hydroxyl groups as model drugs and poloxamer 188 as a carrier to explore the intrinsic relationships between drug-polymer interactions, crystallite size, and in vitro dissolution behavior in CSDs. Initially, we investigate the interactions between flavonoid drugs and P188 by calculating Hansen solubility parameters, determination of Flory-Huggins interaction parameters, and other methods. Subsequently, we explore the crystallization kinetics of flavonoid drugs and P188 in CSD systems using polarized optical microscopy and powder X-ray diffraction. We monitor the domain size and crystallite size of flavonoids in CSDs through powder X-ray diffraction and a laser-particle-size analyzer. Finally, we validate the relationship between crystallite size and in vitro dissolution behavior through powder dissolution. The results demonstrate that, as the number of hydroxyl groups increases, the interactions between drugs and polymers become stronger, making drug crystallization in the CSD system less likely. Consequently, reductions in crystalline domain size and crystallite size become more pronounced, leading to a more significant enhancement in drug dissolution.

Zinc Oxide (ZnO) nanoparticles (NPs) have been synthesized by a simple chemical precipitation method. The effect of monoethanolamine (MEA) content in different solvents on ZnO NPs synthesis and their structural properties has been investigated. The NPs synthesized by using isopropanol (IPA) with 15 ml MEA as a stabilizer under the most favorable conditions (deposition time, t d  = 120 min, temperature = 60 °C) showed good structural properties. Synthesized NPs exhibited beneficial structural properties after annealing. The hexagonal wurtzite crystal structure of ZnO NPs was verified by XRD. Different models were used to calculate structural parameters such as crystallite size, strain, stress, and energy density for all the reflection peaks of XRD corresponding to ZnO lying in the range 2θ = 15⁰-80⁰. The crystallite size of the ZnO nanoparticles was found to be 50-60 nm. FTIR and EDX confirmed the presence of ZnO NPs in the samples. SEM micrograph of all the samples revealed that the grain sizes decrease gradually with the increase of the amount of MEA. UV-Visible diffuse reflectance spectroscopy results provide evidence that the ZnO NPs possess broader absorption bands, together with high band gap energy. The ZnO NPs synthesized with IPA solvent have the highest transmittance and band gap energy of 3.3eV. According to DLS data, various content of MEA stabilizer in solvent affects the hydrodynamic size of ZnO NPs., Competing Interests: The authors declare the following financial interests/personal relationships which may be considered as potential competing interests: Kazi Hanium Maria reports administrative support, equipment, drugs, or supplies, and statistical analysis were provided by Department of Physics, University of Dhaka and Experimental Physics Division, Atomic Energy Centre, Dhaka. Kazi Hanium Maria reports a relationship of 10.13039/501100006523University of Dhaka with Centre for Advanced Research in Sciences, 10.13039/501100009500Bangladesh University of Engineering and Technology, Bangladesh Atomic Energy Centre, 10.13039/501100005999Bangladesh Council of Scientific and Industrial Research that includes: non-financial support., (© 2023 The Authors. Published by Elsevier Ltd.)

The focus of this investigation was to determine the mechanism of effective glass transition temperature (T g ) on the crystallization behavior and microstructure of drugs in crystalline solid dispersion (CSD). CSDs were prepared by rotary evaporation using ketoconazole (KET) as a model drug and the triblock copolymer poloxamer 188 as a carrier. The pharmaceutical properties of CSDs, such as crystallite size, crystallization kinetics, and dissolution behavior, were investigated to provide a foundation for studying the crystallization behavior and the microstructure of drugs in CSDs. According to classical nucleation theory, the relationship of treatment temperature-drug crystallite size-T E of CSD was investigated. Voriconazole, a compound that is structurally similar to KET but with different physicochemical properties, was used to verify the conclusions. The dissolution behavior of KET was significantly enhanced compared to the raw drug due to smaller crystallite size. Crystallization kinetic studies revealed a two-step crystallization mechanism for KET-P188-CSD, in which P188 crystallized first and KET crystallized later. When the treatment temperature was near T g , the drug crystallite size was smaller and more numerous, which suggests nucleation and slow growth. With the increase of temperature, the drug changed from nucleation to growth, and the number of crystallites decreased and the size of the drug increased. This result suggests it is possible to prepare CSDs with higher drug loading and smaller crystallite size by adjusting the treatment temperature and T E , so as to maximize the drug dissolution rate. The VOR-P188-CSD maintained a relationship between treatment temperature, drug crystallite size, and T g E and the treatment temperature can be used to regulate the drug crystallite size and improve the drug solubility and dissolution rate.g E , so as to maximize the drug dissolution rate. The VOR-P188-CSD maintained a relationship between treatment temperature, drug crystallite size, and T g E . The findings of our study demonstrate that T g E and the treatment temperature can be used to regulate the drug crystallite size and improve the drug solubility and dissolution rate., (© 2023. Controlled Release Society.)

The small nanoparticle size and long-chain ligands in colloidal metal halide perovskite quantum dots (PeQDs) cause charge confinement, which impedes exciton dissociation and carrier extraction in PeQD solar cells, so they have low short-circuit current density J sc , which impedes further increases in their power conversion efficiency (PCE). Here, a re-assembling process (RP) is developed for perovskite nanocrystalline (PeNC) films made of colloidal perovskite nanocrystals to increase J sc in PeNC solar cells. The RP of PeNC films increases their crystallite size and eliminates long-chain ligands, and thereby overcomes the charge confinement in PeNC films. These changes facilitate exciton dissociation and increase carrier extraction in PeNC solar cells. By use of this method, the gradient-bandgap PeNC solar cells achieve a J sc = 19.30 mA cm -2 without compromising the photovoltage, and yield a high PCE of 16.46% with negligible hysteresis and good stability. This work provides a new strategy to process PeNC films and pave the way for high performance PeNC optoelectronic devices., (© 2023 Wiley-VCH GmbH.)

In this study, the effect of microstructure under various dose rates of plasma immersion ion implantation on 8Cr4Mo4V steel has been investigated for crystallite size, lattice strain and dislocation density. The phase composition and structure parameters including crystallite size, dislocation density and lattice strain have been investigated by X-ray diffraction (XRD) measurements and determined from Scherrer's equation and three different Williamson-Hall (W-H) methods. The obtained results reveal that a refined crystallite size, enlarged microstrain and increased dislocation density can be obtained for the 8Cr4Mo4V steel treated by different dose rates of ion implantation. Compared to the crystallite size (15.95 nm), microstrain (5.69 × 10 -3 ) and dislocation density (8.48 × 10 15 ) of the dose rate of 2.60 × 10 17 ions/cm 2 ·h, the finest grain size, the largest microstrain and the highest dislocation density of implanted samples can be achieved when the dose rate rises to 5.18 × 10 17 ions/cm 2 ·h, the effect of refining is 26.13%, and the increment of microstrain and dislocation density are 26.3% and 45.6%, respectively. Moreover, the Williamson-Hall plots are fitted linearly by taking βcosθ along the y-axis and 4sinθ or 4sinθ/Y hkl or 4sinθ(2/Y hkl ) 1/2 along the x-axis. In all of the W-H graphs, it can be observed that some of the implanted samples present a negative and a positive slope; a negative and a positive slope in the plot indicate the presence of compressive and tensile strain in the material.

The paper studies the changes in physicochemical properties of three types of hydroxyapatite (HAp): HAp-HB (from bovine sources), HAp-SC (chemically synthesized), and bioinspired HAp-SE (synthesized using eggshells) calcined under identical thermally controlled conditions from room temperature to 400, 500, 600, 650, 680, 700, 720, 750, 800, and 900 °C in furnace air. The thermogravimetric analysis (TGA) indicated distinct thermal transitions and coalescence phenomena at different temperatures for these samples due to their sources and mineral composition differences. Inductively coupled plasma (ICP) showed that HAp-H (human), HAp-HB (bovine), and HAp-SE (bioinspired) have similar Ca, P, and Mg contents. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed that the coalescence phenomena increased in the crystallite size as the temperature increased. X-Ray diffraction (XRD) patterns revealed partial phase changes in the bioinspired sample (HAp-SE) and crystallite growth in all samples, resulting in full width at the half maximum (FWHM) and peak position alterations. Fourier-transform infrared spectroscopy (FTIR) showed that HAp-SE exhibited a partial phase change due to dehydroxylation and the presence of functional groups (PO 4 3- , OH, and CO 3 2- ) with varying vibrational modes influenced by the obtained method and calcination temperature. Raman spectra of the HAp-SE samples exhibited fluorescence at 400 °C and revealed vibrational modes of surface P-O. It observed the bands of the internal phosphates of the crystal lattice and shifts in the band positions at higher temperatures indicated phosphorus interacting with carbon and oxygen, triggering dehydroxylation.

The desire of producing marketable green bio-composites displaying good functional properties has increased. Biodegradable composites are a subject of interest as they respond to ecological concerns. In this study, an eco-friendly alkali-laccase modification was used to improve the interfacial adhesion of mukwa wood fiber and polylactic acid (PLA) matrix. The untreated and treated mukwa-PLA composites were fabricated via extrusion and compression molding technique and investigated. The mukwa wood fibers and mukwa-PLA composites were characterized by chemical composition, crystallite size, Fourier transform infrared spectroscope (FTIR), mechanical properties, and scanning electron microscope (SEM) respectively. The cellulose content was found to increase, while the hemicellulose, lignin, and extractives reduced after the surface modifications. The alkali-laccase, laccase, and alkali modifications increased the tensile strength of the untreated/PLA composites by 12.3 %, 5.2 %, and 3.8 % respectively. The flexural strength of the composites reached a maximum of 95.1 MPa following the alkali-laccase treatment. The alkali-laccase treated composites showed increased impact strength of 53.9 % on the untreated/PLA composites. Good correlations between the crystallite size and the mechanical properties were reported, with the highest R-square (R 2 ) value of 1 found between the impact strength and crystallite size. The modifications strengthened the interaction between mukwa and PLA as more voids, fiber pull-outs, and debonding characteristics were observed on SEM microstructures of untreated/PLA., (Copyright © 2022 Elsevier B.V. All rights reserved.)

In this study, an abundant and eco-friendly photocatalytic material, Fe 2 O 3 particles were synthesized by sonochemical method. Morphological and microstructural investigations of synthesized undoped and Ni, Co-doped Fe 2 O 3 particles were performed. The effect of particle morphology and microstructure on its photocatalytic performance was further investigated. Comparative studies for evaluating particle crystallite sizes were conducted by Williamson-Hall (W-H) method and modified Debye-Scherrer (MDS). Crystallite sizes and lattice strains of Fe 2 O 3 induced by process parameters were calculated by W-H method based on uniform deformation model (UDM). The crystallite sizes of the synthesized powders were calculated in the range of 200 nm and 76 nm by Williamson-Hall analysis. In addition to structural investigation, dislocation density of the synthesized particles was calculated by Williamson-Smallman relation. Afterwards, photocatalytic performance of Fe 2 O 3 particles was investigated in detail. The photodegradation of methylene blue solutions in the presence of light in 20 min with samples 3,4, and 5 in 20 min were 0.937, 0.896, and 0.855, respectively. Moreover, the photodegradation of methylene blue solution with sample 5 for 15, 30, and 45 min were 0.9, 0.828, and 0.757, respectively. A photocatalytic activity of 24.25% has been observed under optimum conditions for the time interval of 45 min., (© TÜBİTAK.)

Sputtering technique involves the use of plasma that locally heats surfaces of substrates during the deposition of atoms or molecules. This modifies the microstructure by increasing crystallinity and the adhesive properties of the substrate. In this study, the effect of sputtering on the microstructure of parylene-C was investigated in an aluminum nitride (AlN)-rich plasma environment. The sputtering process was carried out for 30, 45, 90 and 120 min on a 5 μm thick parylene-C film. Topography and morphology analyses were conducted on the parylene-C/AlN bilayers. Based on the experimental data, the results showed that the crystallinity of parylene-C/AlN bilayers was increased after 30 min of sputtering and remained saturated for 120 min. A scratch-resistance test conducted on the bilayers depicted that a higher force is required to delaminate the bilayers on top of the substrate. Thus, the adhesion properties of parylene-C/AlN bilayers were improved on glass substrate by about 17% during the variation of sputtering time.

Introduction: Polymer materials used in medical devices and treatments invariably encounter cellular networks. For the device to succeed in tissue engineering applications, the polymer must promote cellular interactions through adhesion and proliferation. To predict how a polymer will behave in vitro , these material-cell interactions need to be well understood., Methods: To study polymer structure-property relationships, microparticles of four chemically distinct tyrosol-derived poly(ester-arylate) polymers and a commercially available poly(lactic acid- co -glycolic acid) (PLGA) copolymer were prepared and their interactions with cells investigated. Cell loading concentration was optimized and cell adhesion and proliferation evaluated. Particles were also tested for their ability to adsorb bone morphogenetic protein-2 (BMP-2) and differentiate a myoblast cell line towards an osteoblast lineage through BMP-2 loading and release., Results: While cell adhesion was observed on all particles after 24 h of incubation, the highest degree of cell adhesion occurred on polymers with smaller crystallites. At longer incubation times, cells proliferated on all particle formulations, regardless of the differences in polymer properties. High BMP-2 loading was achieved for all particle formulations and all formulations showed a burst release. Even with the burst release, cells cultured on all formulations showed an upregulation in alkaline phosphatase (ALP) activity, a measure of osteoblast differentiation., Conclusions: As with cell adhesion, the polymer with the smaller crystallite showed the most ALP activity. We suggest that smaller crystallites serve as a proxy for topographical roughness to elicit the observed responses from cells. Furthermore, we have drawn a correlation between the polymer crystallite with the hydration potential using surface analysis techniques., Supplementary Information: The online version contains supplementary material available at 10.1007/s12195-022-00729-9., (© The Author(s) under exclusive licence to Biomedical Engineering Society 2022.)

The effect of neodymium (Nd +3 ) on ZnO thin films has been studied with varying Nd doping percentage ranging from 1 to 5 wt%. XRD graphs confirmed that Nd ions have incorporated into the ZnO lattice without any structural modification. The increase of crystallite size was observed to vary from 27.5 to 31.90 nm with the increment in Nd amount. The optical spectra exhibited transparency in the visible region. The higher transmission was possessed at 1 wt at% Nd concentration. The band gap of Nd-doped ZnO thin films showed variation with the increase in Nd dopant concentration. The increment in dielectric constant and tangent loss was observed with the increase in Nd doping. The change in DC conductivity with frequency was measured by using Jonscher's power law while AC conductivity was explained with the hopping-barrier mechanism. The effects of Nd concentration on antibacterial efficiency against four different bacterial strains Escherichia coli (E. coli), Pseudomonas aeruginosa (P. aeruginosa), Klebsiella Pneumonia (K. Pneumonia), and Staphylococcus aureus (S. aureus) were investigated whereas antifungal activity of Nd-ZnO was done against Aspergillus fumigate by using agar disc-diffusion method. ZnO with 4 wt % Nd demonstrated the best photo-catalytic property., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

In this study, the effect of heat treatment on the structural, magnetic and electrical properties of La 2 FeMnO 6 prepared via the sol-gel and sintering method were investigated. The heat-treatment conditions, i.e., the calcination temperature (1023 K and 1173 K), sintering temperature and time (1273 K for 1 and 3 h) were carried out. X-ray diffraction (XRD) revealed orthorhombic pnma (62) symmetry without any impurity phase for all samples. X-ray photoelectron spectroscopy confirmed the presence of Fe 2+ -Fe 3+ -Fe 4+ and Mn 3+ -Mn 4+ mixed states, and lanthanum and oxygen vacancies resulting in various magnetic exchange interactions. Furthermore, the magnetisation hysteresis showed enhanced hysteresis loops accompanied by an increase in magnetisation parameters with calcination temperature. The Raman phonon parameters induced a redshift in the phonon modes, alongside an increase in the intensity and compression of the linewidth, reflecting a decrease in lattice distortion, which was confirmed by XRD. The temperature-dependent conductivity showed that the conduction mechanism is dominated by p-type polaron hopping, and the lowest activation energy was approximately 0.237 ± 0.003 eV for the minimum heat-treatment conditions. These results show that varying heat-treatment conditions can significantly affect the structural, magnetic and electrical properties of the La 2 FeMnO 6 system.

In the last few decades, there has been a trend involving the use of nanoscale fillers in a variety of applications. Significant improvements have been achieved in the areas of their preparation and further applications (e.g., in industry, agriculture, and medicine). One of these promising materials is magnesium oxide (MgO), the unique properties of which make it a suitable candidate for use in a wide range of applications. Generally, MgO is a white, hygroscopic solid mineral, and its lattice consists of Mg2+ ions and O2- ions. Nanostructured MgO can be prepared through different chemical (bottom-up approach) or physical (top-down approach) routes. The required resultant properties (e.g., bandgap, crystallite size, and shape) can be achieved depending on the reaction conditions, basic starting materials, or their concentrations. In addition to its unique material properties, MgO is also potentially of interest due to its nontoxicity and environmental friendliness, which allow it to be widely used in medicine and biotechnological applications.

Various crystallite size estimation methods were used to analyze X-ray diffractograms of spherical cerium dioxide and titanium dioxide anatase nanoparticles aiming to evaluate their reliability and limitations. The microstructural parameters were estimated from several integral breadth methods such as Scherrer, Monshi, Williamson-Hall, and their variants: (i) uniform deformation model, (ii) uniform strain deformation model, and (iii) uniform deformation energy density model. We also employed the size-strain plot and Halder-Wagner method. For this purpose, an instrumental resolution function of an Al 2 O 3 standard was used to subtract the instrumental broadening to estimate the crystallite sizes and strain, and the linear regression analysis was used to compare all the models based on the coefficient of determination. The Rietveld whole powder pattern decomposition method was introduced for comparison purposes, being the best candidate to fit the X-ray diffraction data of metal-oxide nanoparticles. Refined microstructural parameters were obtained using the anisotropic spherical harmonic size approach and correlated with the above estimation methods and transmission electron microscopy images. In addition, μ-Raman spectra were recorded for each material, estimating the mean crystallite size for comparison by means of a phonon confinement model.

In the present study, CaZrO 3 nanophosphors were sensitized with lanthanum (La) at different concentrations (0.5, 1.0, 1.5, 2.0, and 2.5) prepared using polyvinyl alcohol as the chelating agent through the sol-gel method. To study their structural and optical properties, samples were characterized by X-ray diffractometry (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM) and photoluminescence (PL). The XRD results revealed that samples were well crystallized and average crystallite sizes were calculated. The average crystallite size value was in good agreement with the value obtained from TEM analysis. Energy dispersive spectroscopy and FE-SEM confirmed the existence of La in the prepared samples. In the PL spectra, La-sensitized samples exhibited three bands at 402 nm, 438 nm, and 463 nm in the visible range when excited at the 260 nm wavelength. As the proportion of La increased, the intensity of bands at 438 nm and 463 nm decreased, whereas the band at 402 nm remained stable. Time-resolved PL spectra illustrated the lifetime of the samples. Corresponding CIE co-ordinates for La-sensitized CaZrO 3 were calculated., (© 2020 John Wiley & Sons, Ltd.)

Nickel oxide (NiO) is a wide band gap semiconductor material that is used as an electrochromic layer or an ion storage layer in electrochromic devices. In this work, the effect of annealing temperature on sol-gel NiO films was investigated. Fourier transform infrared spectroscopy (FTIR) showed that the formation of NiO via decomposition of the precursor nickel acetate occurred at about 300 °C. Meanwhile, an increase in roughness was observed by Atomic force microscope (AFM), and precipitation of a large number of crystallites was observed at 500 °C. X-ray Diffraction (XRD) showed that the NiO film obtained at such a temperature showed a degree of crystallinity. The film crystallinity and crystallite size also increased with increasing annealing temperature. An ultraviolet spectrophotometer was used to investigate the optical band gap of the colored NiO films, and it was found that the band gap increased from 3.65 eV to 3.74 eV with the increase in annealing temperature. An electrochromic test further showed that optical modulation density and coloring efficiency decreased with the increase in crystallite size. The electrochromic reaction of the nickel oxide film is more likely to occur at the crystal interface and is closely related to the change of the optical band gap. An NiO film with smaller crystallite size is more conducive to ion implantation and the films treated at 300 °C exhibit optimum electrochromic behavior.

Supramolecular structure is the critical factor that affects the properties of cellulosic fibers. This article studied the action of Papirindustriens forskningsinstitut (PFI) refining on the molecular aggregation and hydrogen bonding network, and tried to explore the relationship between the crystal packing and hydrogen-bonding network in cellulosic fibers. The results showed that the polymorph, H-bonding distance, and H-bonding energy of various H-bonds remained almost unchanged, while the crystalline index, crystallite size, and content of various H-bonds changed with refining. Therein, the content of the inter-molecular O(6)H⋯O(3') H-bonds was significantly correlated with the crystalline index that was obtained in intensities of the XRD peaks. The Pearson correlation coefficient between them was 0.888 ( p < 0.05) for softwood fibers and 0.889 ( p < 0.05) for hardwood fibers, respectively. It can be concluded that the variations of accessibility, swelling, and fibrillation were closely related to the supramolecular structure and the intermolecular H-bonds play an important role in the crystal packing of cellulose.

This study evaluated the effect of amylases on the formation, and characteristics of retrograded starches using sweet potato (SPS), cassava (CAS) and high amylose maize (HAS) starches. The starches were gelatinized, hydrolyzed with fungal or maltogenic α-amylase, de-branched and retrograded. The modified starches were then analyzed for digestibility, chain size distribution, relative crystallinity and crystallite size, thermal properties and the proportion of double helices. CAS was the most susceptible and HAS the most resistant to the action of both enzymes. Amylolysis was efficient in forming resistant starch type 3 (RS3) and high levels (> 60%) were found for all starches. RS3 content was highly correlated with the proportion of chains with degrees of polymerization between 13 and 30 for all starches, especially for the root starches, while for HAS, the high amylose content and reduction in the size of amylose chains and very long amylopectin chains also deeply contributed for the RS3 formation. These sizes (DP 13-30) are best suited for the formation of a more crystalline, more perfect, and more strongly bonded structure, composed of larger crystallites, and with a higher concentration of double helices. High correlation coefficients were found between RS3, relative crystallinity, crystallites size, and enthalpy change., (Copyright © 2020 Elsevier B.V. All rights reserved.)

Herein, Pt/HZSM-5 zeolite catalysts with different crystallite sizes ranging from nanosheet (~2 nm) to bulk crystals (~1.5 μm) have been prepared for the hydrodeoxygenation of guaiacol, and their effects on the reaction pathway and product selectivity were explored. HZSM-5 zeolites prepared by seeding (Pt/Z-40: ~40 nm) or templating (Pt/NS-2: ~2 nm) fabricated intra-crystalline mesopores and thus enhanced the reaction rate by promoting the diffusion of various molecules, especially the bulky ones such as guaiacol and 2-methoxycyclohexanol, leading to a higher cyclohexane selectivity of up to 80 wt % (both for Pt/Z-40 and Pt/NS-2) compared to 70 wt % for bulky HZSM-5 (Pt/CZ: ~1.5 μm) at 250 °C and 120 min. Furthermore, decreased crystallite sizes more effectively promoted the dispersion of Pt particles than bulky HZSM-5 (Pt/Z-400: ~400 nm and Pt/CZ). The relatively low distance between Pt and acidic sites on the Pt/Z-40 catalyst enhanced the metal/support interaction and induced the reaction between the guaiacol molecules adsorbed on the acidic sites and the metal-activated hydrogen species, which was found more favorable for deoxygenation than for hydrogenation of oxygen-containing molecules. In addition, Pt/NS-2 catalyst with a highly exposed surface facilitated more diverse reaction pathways such as alkyl transfer and isomerization.

Type 2 diabetes (T2D) adversely affects the normal functioning, intrinsic material properties, and structural integrity of many tissues, and bone fragility is one of them. To simulate human T2D and to investigate diabetic bone fragility, many rodent diabetic models have been developed. Still, an outbred genetically normal nonobese diabetic rat model is not available that can better simulate the disease characteristics of nonobese T2D patients, who have a high prevalence in Asia. In this study, we used a combination treatment of high-fat diet (4 weeks, 58% kcal as fat) and low-dose streptozotocin (STZ; 35 mg/kg i.p. at the end of the fourth week) to develop T2D in female Sprague-Dawley (SD) rats. After 8 weeks of the establishment of the T2D model, the femoral bones were excised after euthanizing rats (animal age approximately 21 to 22 weeks; n = 10 with T2D, n = 10 without diabetes). The bone microstructure (μCT), mechanical, and material properties (three-point bending, cyclic reference point indentation, nanoindentation), mean mineral crystallite size (XRD), bone composition (mineral-to-matrix ratio, nonenzymatic cross-link ratio [NE-xLR], Fourier transform-infrared microspectroscopy), and total fluorescent advanced glycation end products were analyzed. We found that diabetic bone had reduced whole-bone strength and compromised structural properties (μCT). The NE-xLRs were elevated in the T2D group, and strongly and negatively correlated with postyield displacement, which suggests bone fragility was caused by a lack of glycation control. Along with that, the decreased mineral-to-matrix ratio and modulus, increased indentation distance increase, and wider mineral crystallite size in the T2D group were evidence that the diabetic bone composition and material properties had changed, and bone became weaker with a tendency to easily fracture. Altogether, this model simulates the natural history and metabolic characteristics of late-stage T2D (insulin resistance and as disease progress develops, hypoinsulinemia) for nonobese young (and/or adolescent) T2D patients (Asians) and provides potential evidence of diabetic bone fragility at various organization levels. © 2020 The Authors. JBMR Plus published by Wiley Periodicals, Inc. on behalf of American Society for Bone and Mineral Research., (© 2020 The Authors. JBMR Plus published by Wiley Periodicals, Inc. on behalf of American Society for Bone and Mineral Research.)

Tricalcium silicate phase is one of the main components of modern Portland cements. One of the major industrial challenges in the field of cement production is mapping the influence of individual clinker minerals and their polymorphs on the properties of industrially produced clinkers. The primary goal of this work is to improve the fundamental knowledge of understanding the process of alite formation and development from a crystallographic point of view. This study focuses on the observation of the crystallization process of triclinic alite during the firing process, which to date has not been thoroughly described. The effects of a wide range of temperatures and sintering periods on crystallinity were assessed on samples fired in platinum crucibles in a laboratory furnace. X-ray analysis-together with calculation of crystallinity using Scherrer's equation-was used for observing the crystallite size changes of T1 alite polymorph. According to the acquired results, among the most technologically and economically advantageous regimes of production of a high-quality triclinic alite is the temperature of 1450 °C and sintering time of two hours. The most significant changes in the crystallite size occurred within the first hour of sintering for the whole investigated temperature range.

This rather long-standing project has resulted in a National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) for the analysis of crystallite size from a consideration of powder diffraction line profile broadening. It consists of two zinc oxide powders, one with a crystallite size distribution centered at approximately 15 nm, and a second centered at about 60 nm. These materials display the effects of stacking faults that broaden specific hkl reflections and a slight amount of microstrain broadening. Certification data were collected on the high-resolution powder diffractometer located at beamline 11-BM of the Advanced Photon Source, and on a NIST-built laboratory diffractometer equipped with a Johansson incident beam monochromator and position sensitive detector. Fourier transforms were extracted from the raw data using a modified, two-step profile fitting procedure that addressed the issue of accurate background determination. The mean column lengths, 〈 L 〉 area and 〈 L 〉 vol , were then computed from the Fourier transforms of the specimen contribution for each reflection. Data were also analyzed with fundamental parameters approach refinements using broadening models to yield 〈 L 〉 area and 〈 L 〉 vol values. These values were consistent with the model-independent Fourier transform results; however, small discrepancies were noted for the 〈 L 〉 area values from both machines and both crystallite size ranges. The fundamental parameters approach fits to the laboratory data yielded the certified lattice parameters.

The data presented in this manuscript showed the effects of the sodium sources on the morphology, crystallite size and carbon content of NaTi 2 (PO 4 ) 3 /C composite obtained after heat treatment under N 2 atmosphere of the as-spraydried powders. The morphology, crystalline size and carbon content of three products with different sodium sources were investigated. The data are related to "Synthesis of NaTi 2 (PO 4 ) 3 @C microspheres by an in situ process and their electrochemical properties" (Mao et al.,2020)., Competing Interests: The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (© 2020 The Authors.)

In this research, the influence of microstructure parameters on the residual stresses of ultrafine-grained sheets was investigated. For this purpose, the constrained groove pressing (CGP) process was carried out on the copper sheets with 3 mm thickness, and residual stresses of the CGPed sheets was measured using the contour method. Microstructure of the CGPed specimens was evaluated by the optical microscopy, micro x-ray diffraction (micro-XRD), and transmission electron microscopy (TEM) experiments. Microstructure parameters including crystallites size, dislocations density, and lattice strain were calculated using Williamson-Hall and Williamson-Smallman equations, and the calculated results were validated by the TEM images. The influence of these parameters on the residual stresses was investigated by analysis of variance (ANOVA) method, and two approaches were considered in this way. According to the results, the CGP process can create nanostructures in the CGPed sheets, and with increasing number of CGP passes, grains size, crystallites size, lattice strain, and residual stresses decrease, and density of dislocations increases. Microstructure parameters have a significant effect on the macro-residual stresses, and strain is the most effective parameter. Also, in the ultrafine-grained sheets, micro-parameters have an undeniable contribution, which is the same as that of macro-parameters on the macro-residual stresses., Competing Interests: Declaration of Competing Interest The authors declared no potential conflicts of interest with respect to the research, authorship and/or publication of this article., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

La, Cu dual doped ZnO with Cu = 0%-4% were prepared by co-precipitation route. The XRD pattern optimized the Cu content as 2% which restrict the secondary phase formation. The new phase at 38.7° corresponding to CuO (111) and the another phase at 42.3° related to Zn (101) came from un-reacted Zn 2+ ions appeared in Cu = 4% doped sample. Zeta potential measurements confirms the stability of the particles. The blue shift of absorption edge and the energy gap from 3.66 eV to 3.99 eV by Cu doping was discussed by the shape of the particles, the distortion of the host lattice and generation of defect concentrations. The characteristic IR peaks around 470-489 cm -1 was related to the octahedral sites of Zn-O for Cu = 0 and 2% which is shifted to 616 cm -1 corresponding to the tetrahedral site at Cu = 4%. The shift in frequency was originated from the dissimilarity in the volume and bond lengths by the substitution of La and Cu in Zn-O. Based on the antibacterial report, it can be concluded that the Cu-doped Zn-La-O solid solution compose an effectual antimicrobial agent against pathogenic microorganisms. Cu = 4% doped sample possessed highest bacterial killing capacity because of the enhanced crystallite size and high density of oxygen vacancies which led the higher ROS values. Tuning of crystallite size and energy gap and the enhanced bactericial killing capacity by Cu addition is useful for opto-electronic device and medical applications., (Copyright © 2019 Elsevier B.V. All rights reserved.)

A single-beam optical-trap sample holder for X-ray diffraction measurements with synchrotron radiation has been developed. The sample holder was used to obtain an X-ray diffraction image of a single ZnO particle levitated in air, without mechanical contact, by the optical gradient force exerted by a focused laser beam. The diffraction image showed a Debye ring pattern, which was similar to a powder diffraction pattern of an assemblage of ZnO particles. While the ZnO particle is held by the optical trap in air, it rotates irregularly. Therefore, the Debye ring pattern of the ZnO particle can be clearly obtained even if the ZnO particle is a single grain. Lattice parameters and crystallite size of the single ZnO particle were determined simultaneously. The lattice parameters were determined to be a = 3.2505 ± 0.0005 Å and c = 5.207 ± 0.006 Å, which are consistent with those of the assemblage of ZnO particles. The crystallite size determined by the Scherrer method was 193.4 ± 26.2 nm.

The data presented in this manuscript showed the effect of the carbon sources on the morphology and crystallite size of Fe/C composite microspheres obtained after reduction of the as spray-dried powders. Each morphology, phase, and crystalline size of powders obtained after spray-drying and subsequent heat-treatment were investigated., (© 2019 The Author(s).)

Majority of organic matter is bound to clay minerals to form stable colloidal organo-mineral fraction (COMF) in soil. Stability of carbon (C) in COMF is crucial for long-term C sequestration in soil. However, information on the effect of long-term fertilization and manuring with various organic sources on C stability in such fraction in soils with varying clay mineralogy is scarce. The present study was, therefore, carried out to assess the effect of thirty-one years of continuous fertilization and manuring with different organics on C-stability in COMF extracted from an Inceptisol, a Vertisol, a Mollisol, and an Alfisol. The treatments comprised of control (no fertilization), 100% NPK (100% of recommended N, P and K through fertilizer), 50% NPK+ 50% of recommended N supplied through either farm yard manure (FYM) or cereal residue (CR) or green manure (GM). The stability of C (1/k) in COMF was determined from desorption rate constant (k) of humus-C by sequential extraction and correlated with extractable amorphous Fe-Al-Si-oxides, and crystallite size of illite minerals. Long-term fertilization and manuring with the above sources of organic altered the contents of amorphous Fe-Al-Si-oxides, and decreased the crystallite size of illite in all the soil orders. Fifty percent substitution of fertilizer N by various organics significantly increased C-stability in COMF by 27-221% (mean 111%) over full dose of NPK (100% NPK). Smectite dominating Vertisol exhibited highest stability of C followed by the Mollisol, the Inceptisol and the Alfisol. Stability of such C in soil was correlated positively with the amount of amorphous Fe and Al oxides but negatively with crystallite size of illite (r = -0.46, P < 0.01). Application of NPK + GM or NPK + FYM in Inceptisol, Vertisol and Mollisol and NPK + GM or NPK + CR in Alfisol emerged as the best management practices for higher stabilization of C in COMF for long-term C sequestration., (Copyright © 2019 Elsevier B.V. All rights reserved.)

Dissolution of cortical bone mineral under demineralization in 0.1 M HCl and 0.1 M EDTA solutions is studied by X-ray diffraction (XRD). The bone specimens (in the form of planar oriented pieces) were cut from a diaphysial fragment of a mature mammal bone so that a cross-section surface and a longitudinal section surface could be analyzed individually. This permitted to compare the dissolution behavior of bone apatite of different morphologies: crystals having the c-axis of the hexagonal unit-cell generally parallel to the long axis of the bone (major morphology) and those having the c-axis almost perpendicular to the bone axis (minor morphology). For these two types of morphology, the crystallite sizes in two mutually perpendicular directions (namely, [002] and [310]) were estimated by Scherrer formula in the initial and the stepwise-demineralized specimens. The data obtained reveal that the crystals belonging to the minor morphology dissolve faster than the crystals of the major morphological type, despite the fact that the crystallites of the minor morphology seem to be only a little smaller than those of the major morphology; the apatite crystallites irrespective of the morphology type are elongated in the c-axis direction. We hypothesize that the revealed difference in solubility may be caused by diverse chemical modifications of apatite of these two morphological types, since the solubility of apatite is strictly regulated by anionic and cationic substitutions in the lattice. The anisotropy effect in solubility of bone mineral seems to be functionally predetermined and this should be a crucial factor in the resorption and remodeling behavior of a bone. Some challenges arising at XRD examination of partially decalcified cortical bone blocks are discussed, as well as the limitations of estimation of bone crystallite size by XRD line-broadening analysis.

Solid oxide fuel cells need a diffusion barrier layer to protect the zirconia-based electrolyte if a cobalt-containing cathode material like lanthanum strontium cobalt ferrite (LSCF) is used. This protective layer must prevent the direct contact and interdiffusion of both components while still retaining the oxygen ion transport. Gadolinium-doped ceria (GDC) meets these requirements. However, for a favorable cell performance, oxide ion conducting films that are thin yet dense are required. Films with a thickness in the sub-micrometer to micrometer range were produced by the dry room temperature spray-coating technique, aerosol deposition. Since commercially available GDC powders are usually optimized for the sintering of screen printed films or pressed bulk samples, their particle morphology is nanocrystalline with a high surface area that is not suitable for aerosol deposition. Therefore, different thermal and mechanical powder pretreatment procedures were investigated and linked to the morphology and integrity of the sprayed films. Only if a suitable pretreatment was conducted, dense and well-adhering GDC films were deposited. Otherwise, low-strength films were formed. The ionic conductivity of the resulting dense films was characterized by impedance spectroscopy between 300 °C and 1000 °C upon heating and cooling. A mild annealing occurred up to 900 °C during first heating that slightly increased the electric conductivity of GDC films formed by aerosol deposition.

Three commercially available artificial bone substitutes with different compositions, hydroxyapatite (HAp; Neobone ® ), carbonate apatite (CO₃Ap; Cytrans ® ), and β-tricalcium phosphate (β-TCP; Cerasorb ® ), were compared with respect to their physical properties and tissue response to bone, using hybrid dogs. Both Neobone ® (HAp) and Cerasorb ® (β-TCP) were porous, whereas Cytrans ® (CO₃Ap) was dense. Crystallite size and specific surface area (SSA) of Neobone ® (HAp), Cytrans ® (CO₃Ap), and Cerasorb ® (β-TCP) were 75.4 ± 0.9 nm, 30.8 ± 0.8 nm, and 78.5 ± 7.5 nm, and 0.06 m²/g, 18.2 m²/g, and 1.0 m²/g, respectively. These values are consistent with the fact that both Neobone ® (HAp) and Cerasorb ® (β-TCP) are sintered ceramics, whereas Cytrans ® (CO₃Ap) is fabricated in aqueous solution. Dissolution in pH 5.3 solution mimicking Howship's lacunae was fastest in CO₃Ap (Cytrans ® ), whereas dissolution in pH 7.3 physiological solution was fastest in β-TCP (Cerasorb ® ). These results indicated that CO₃Ap is stable under physiological conditions and is resorbed at Howship's lacunae. Histological evaluation using hybrid dog mandible bone defect model revealed that new bone was formed from existing bone to the center of the bone defect when reconstructed with CO₃Ap (Cytrans ® ) at week 4. The amount of bone increased at week 12, and resorption of the CO₃Ap (Cytrans ® ) was confirmed. β-TCP (Cerasorb ® ) showed limited bone formation at week 4. However, a larger amount of bone was observed at week 12. Among these three bone substitutes, CO₃Ap (Cytrans ® ) demonstrated the highest level of new bone formation. These results indicate the possibility that bone substitutes with compositions similar to that of bone may have properties similar to those of bone.

Wet chemical synthesis of hydroxyapatite (HAp) nanostructures was carried out with different solution pH values (9, 10 and 11) and sintering temperatures (300°C, 500°C, 700°C and 900°C). The effects of pH and sintering temperature on the structural and morphological properties of nanocrystalline HAp powders were presented. Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM) analysis were performed to obtain the crystalline structure, chemical composition, morphology and particle size of the HAp powders. The TEM analysis is used in order to observe the rod- and flake-like HAp structures. XRD confirms the presence of both HAp hexagonal and monetite phases, although the monetite phase was less abundant in the resultant powders. Increase in pH reduced the monetite phase and enhanced Ca/P ratio from 1.7 to 1.83. Additionally, an increment in sintering temperature increased the crystallite size from 20 to 56 nm. The SEM analysis revealed the formation of semi-spherical and flake-like HAp structures with preferential flake morphology. An increase in pH and sintering temperature resulted in the growth and coalescence of crystals resulting in a porous capsular morphology. The FTIR analysis confirmed the reduction of carbonate stretching modes with an increase in pH and H-O-H antisymmetric stretching mode is eliminated for powders sintered at 900°C confirming the formation of stable and porous HAp powders., Competing Interests: The authors declare that they have no competing interests.

The Aerosol Deposition (AD) method has the unique property to allow for manufacturing dense ceramic films at room temperature. As found in many publications, the deposition process is very sensitive to powder properties. In particular, powders of nano-sized particles and grains, e.g., from precipitation, are usually beyond the conventional size range of AD processability, yielding chalk-like films of low mechanical stability. Thus, the conventional AD process is limited in applicability. In this study, we try to overcome this problem by adapting the standard milling treatment of powders for improved deposition by additional temperature pre-treatment. Using commercial tin dioxide and including a temperature treatment for grain growth, makes the powder accessible to deposition. In this way, we achieve optically translucent and conductive SnO₂ thick films. With the application such as a gas sensitive film as one of many possible applications for SnO₂ thick-films, the sensors show excellent response to various reducing gases. This study shows one exemplary way of extending the range of adequate powder and applications for the AD method.

We discussed the influence of Ag doping on the crystallite size of ZnO and enhanced Raman spectroscopy properties. We reported optical and vibrational properties of Ag-doped ZnO microrods which have been prepared through reflux method. Dopant induced shift and asymmetric broadening of Raman modes have been discussed. In Raman spectra, silver doping induces a lower wavenumber shift in E 2H mode. Moreover, the appearance of some additional peaks after Ag-doping were successfully studied and the doping is confirmed by the local vibration modes obtained at 230 and 390cm -1 . Effect of doping is studied by calculating the crystallite size and we discussed the variations in full width half maximum (FWHM), phonon lifetime with respect to varying crystallite size. Phonon lifetime decreases with increasing Ag concentration. The asymmetric broadening in Raman modes E 2H and E 2L with the addition of Ag are analysed with Fano fitting., (Copyright © 2018 Elsevier B.V. All rights reserved.)

The production and crystallinity of 13 C bacterial cellulose (BC) was examined in static culture of Komagataeibacter xylinus with different chemical and physical stimuli: the addition of NaCl or cloramphenicol as well as exposure to a magnetic field or to UV light. Crystalline BC biosynthesized under each stimulus was studied by XRD and solid state 13 C NMR analyses. All treatments produced BC with enhanced crystallinity over 90% (XRD) and 80% (NMR) compared to the control (83 and 76%, respectively) or to Avicel (77 and 62%, respectively). The XRD data indicated that the crystallite size was 80-85 Å. Furthermore, changes on the allomorphs (I α and I β ) ratio tendency of BC samples addressed to the stimuli were estimated using the C4 signal from 13 C NMR data. These results showed a decrease of the allomorph I α (3%) when BC was biosynthesized with UV light and chloramphenicol compared to control (58.79%). In contrast, the BC obtained with NaCl increased up to 60.31% of the I α allomorph ratio., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Samarium-doped ceria (SDC) carbonate has become an attractive electrolyte for fuel cells because of its remarkable ion conductivity and high performance. Different doped ceria-carbonate (single-carbonate SDC, binary-carbonate SDC, and ternary-carbonate SDC) electrolytes were synthesized by the coprecipitation/oxalate method, to optimize the electrochemical performance. The structure; morphology; and thermal, optical, and surface properties have been studied using a variety of techniques. The X-ray diffraction results confirmed the successful incorporation of samarium into ceria as a crystalline structure and inclusion of carbonate, which is amorphous in nature. To analyze the conduction mechanism, direct current conductivity was measured in a H 2 /O 2 atmosphere. Doped ceria-binary carbonate ((Li/Na)CO 3 -SDC) showed the best conductivity of 0.31 S cm -1 and power density of 617 mW cm -2 , at 600 °C. The enhancement in the ionic conductivity and performance of the composites is due to the contribution of hybrid ions (O 2- , H + ). The crystallite size of the composites was in the range 21-41 nm. For the calculation of band gaps, optical absorption spectra of the synthesized powders were analyzed, and they showed a red shift with the band gap energy in the range 2.6-3.01 eV, when compared to that of pure ceria (3.20 eV).

Soil vestiges might provide information about a crime scene. The Rietveld method with X-ray diffraction data (RM-XRD) is a nondestructive technique that makes it possible to characterize minerals present in the soils. Soil clays from the metropolitan region of Curitiba (Brazil) were submitted to DCB treatment and analyzed using XRD with CuK α radiation in the step-scan mode (0.02° 2θ/5 s). The GSAS+EXPGUI software was used for RM refinement. The RM-XRD results, together with the principal component analysis (PCA) (52.6% total variance), showed the kaolinite predominance in most analyzed samples and the highest quartz contents in "site 1." Higher anatase, and gibbsite and muscovite contents influenced discrimination, mainly in "site 3" and "site 1," respectively. These results were enough to discriminate clays of four sites and two horizons using a reduced amount of sample showing that the technique can be applied to the investigation into soil vestiges., (© 2017 American Academy of Forensic Sciences.)