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It was experimentally observed that in polycrystalline materials under low macro loading of the specimen the first sites of failure initiation take place in the specific clusters of few grains. In some grains of these extreme clusters, the local (meso-) strains and stresses are high enough to cause first damages or plastic slips. In the stochastic microstructure of polycrystals, the formation of an extreme cluster is random and rare. Nevertheless, they govern the failure process initiation and can severely affect the reliability of polycrystalline machine parts. It is time and resource consuming to search and investigate extreme clusters on the real specimens of polycrystalline materials experimentally. A theoretical tool is desirable. Here we present the powerful computational method to look for extreme clusters, to investigate their possible patterns, and to evaluate the absolute maximums of local strains/stresses that can be achieved in these clusters. The experimentally observed clusters consist of few (3-4) preferably oriented neighboring grains or even of one big supergrain. The strain and stress bursts arise due to an interaction of the grains. One can expect that in bigger clusters, larger local bursts of fields can be generated. We found the typical forms of the extreme clusters (small and big) in four different polycrystals with grains of a weak and strong anisotropy for the case of uniaxial tension. In all regarded cases, the extreme clusters have the forms of the symmetrical patterns. In big clusters of highly anisotropic grains, the maximum of mesostrain exceeds the macrostrain by several times. In clusters of weakly anisotropic grains, the local strain concentration is rather moderate (tens of percents).

This research work aims to investigate the mechanically alloyed Fe15Co2P3. Parametric Rietveld refinement method, of the obtained X-ray patterns, was performed for qualitative and quantitative phase analysis, structural, microstructural and mechanical properties. The ball-milled powder mixture crystallized within the face-centred cubic α-Fe(P) solid solution in equilibrium with Co75Fe25 phase. The crystallite size decreases reaching 100 and 200 nm respectively after 3h of milling. The highest values of the dislocation density, microstain and stored energy are registered for the α-Fe(P) solid solution. The studied mechanical properties manifest the brittle nature of the α-Fe(P) solid solution compared to the Co75Fe25 phase. The squareness ratio Mr/Ms and the coercivity values of the milled powders increase with increasing milling time and reach steady state after 2 h. The hysteresis loss energy and maximum permeability reach minimal values of 45*10− 4 W/m3 and 49*10− 3 H/m respectively, after 1 h of milling at the opposite of the switching field distribution.

Aluminum, boron, and magnesium are one of the most common aerospace infrastructure materials. Therefore it is important to know their effectiveness in radiation shielding. In this study, Al–B–Mg powder alloy with a nominal composition of Al50B25Mg25 was synthesized by using a mechanical alloying (MA) process under an argon gas atmosphere for potential use as a aluminum based engineering material. Microstructural evolution, thermal behaviour, and mechanical properties of the mechanically alloyed powders as a function of milling time were investigated by means of X-ray diffraction (XRD), differential scanning calorimetry, transmittance electron microscopy and scanning electron microscopy (SEM). The XRD and SEM results revealed that the microstructure of the powders materials changed during MA. The crystallite size of Al–B–Mg powders decreased with increasing milling time. The average crystallite size was determined. The results also showed that after 100 h of milling time nanostructured α-Al (Mg, B) solid solution phase whose crystallite sizes are below 17 nm were obtained. Also, radiation shielding parameters have been investigated using NaI (Tl) γ-ray spectrometry at 662 and 1173 keV energies obtained via 137Cs and 60Co radioactive point sources. The obtained experimental data have been compared with XCOM theoretical data. The experimental data was utilized to calculate the half-value layer, tenth-value layer, and mean free path values. According to the obtained data, Al50Mg25B25 alloy powder prepared and annealed at 300 °C has been shown to provide better protection against radiation.

Neutral three-dimensional Eu3+- and Tb3+-based metal-organic frameworks (MOFs) with 4-fold interpenetration can be produced by seeding with anionic Cd2+-based MOF crystallites of identical connectivity. In the absence of these crystallites, two-dimensional networks are formed.

Background In this work biologically active CuO nanoparticle were discussed. The literature suggests that CuO shows very good antibacterial activity on both Gram positive and Gram-negative bacterial strains. Further, it is used in antibacterial coatings on various substrates to prevent various kinds of medical equipment’s. Here CuO NPs was prepared via greener approach and almond gum is used as a reducing agent. Almond gum is nontoxic and contains huge amount of polysaccharides. Hence, the gum mediated CuO NPs can be used to treat urinary tract infection (UTI). Method The CuO NPs were characterized using UV, FTIR, XRD and HESEM with EDX analysis. The antibacterial (both Gram positive and Gram negative) effects of CuO NPs were determined with agar well diffusion method. Results The CuO NPs were characterized by X-ray diffraction pattern result indicates that the monoclinic structure with average crystallite size about 12.91 nm. Straight line model in Scherrer method results found to be crystallite size. The crystallite size and microstrain were estimated in W–H analysis. Lorentz polarization factor, size-strain plot (SSP), morphological index (M-I) and dislocation density were calculated based on x-ray diffraction data. The FTIR analysis confirms presence of Cu and O band. From the absorption spectrum of CuO NPs, it was found to be cutoff wavelength of 230 nm and direct bandgap was found to be 4.97 eV. Morphology analysis shows that the synthesized of CuO NPs reveals agglomerated and spherical in shape. It was found to be 16 nm–25 nm. Energy dispersive spectroscopy (EDX) result indicates percentages of Cu and O element present in the sample. Antimicrobial studies reveal zone of inhibition of CuO NPs. This was used in different pathogens such as gram-positive and Gram-negative bacteria. This study shows exhibit excellent antimicrobial effects of CuO NPs. Conclusion Hence, in this article the novel and cost-effective method to prepare CuO NPs was discussed. The prepared CuO NPs can be used as an antifungal and antibacterial reagent.

Due to the dominance of non-densifying sintering mechanisms (surface diffusion and evaporation condensation) pure tin oxide ceramics exhibit unusual sintering behavior that allows sintering without shrinkage, i.e. without changes in porosity. It is therefore ideally suited for fundamental studies. In this paper we study the crystallite size and its changes as a function of temperature and dwell time via X-ray diffraction (XRD) line broadening. It is shown that, although the contribution of microstrain broadening is negligibly small, the difference between the different evaluation methods (Scherrer equation, Williamson-Hall plots, Halder-Wagner plot) is quite large. Nevertheless similar qualitative conclusions can be drawn irrespective of the specific evaluation method used (although Halder-Wagner analysis is most reasonable). Significant crystallite growth can be expected for pure tin oxide ceramics from nanosized powders only at temperatures above 1000 °C. Prolonging the dwell times beyond 3 h does not affect the crystallite size to any significant degree.

Enamel and dentin are susceptible to acids from food sources leading to dental erosion, a global problem affecting millions of individuals. Particulate hydroxyapatite (HAP) on the tooth surface can influence the effects of acid attacks. Standardized bovine enamel and dentin samples with artificial saliva are used in an in vitro cyclic demineralization–remineralization protocol to analyze the structural changes experienced by tooth surfaces using high-resolution scanning electron microscopy and to evaluate the potential of a HAP-based oral care gel in the protection of teeth from erosive attacks. The interfaces between HAP particle and enamel HAP crystallites are investigated using focused ion beam preparation and transmission electron microscopy. The results show that erosion with phosphoric acid severely affects enamel crystallites and dentin tubules, while artificial saliva leads to remineralization effects. The HAP-gel forms a microscopic layer on both enamel and dentin surfaces. Upon acid exposure, this layer is sacrificed before the native tooth tissues are affected, leading to significantly lower degrees of demineralization compared to the controls. This demonstrates that the use of particulate HAP as a biomaterial in oral care formulations can help protect enamel and dentin surfaces from erosive attacks during meals using a simple and effective protection principle.

Nanostructure of chromium oxide (Cr2O3-NPs) with rhombohedral structure were successfully prepared by spray pyrolysis technique using Aqueous solution of Chromium (III) chloride CrCl3 as solution. The films were deposited on glass substrates heated to 450°C using X-ray diffraction (XRD) shows the nature of polycrystalline samples. The calculated lattice constant value for the grown Cr2O3 nanostructures is a = b = 4.959 Å & c = 13.594 Å and the average crystallize size (46.3-55.6) nm calculated from diffraction peaks, Spectral analysis revealed FTIR peak characteristic vibrations of Cr-O Extended and Two sharp peaks present at 630 and 578 cm-1 attributed to Cr-O “stretching modes”, are clear evidence of the presence of crystalline Cr2O3. The energy band gap (3.4 eV) for the chromium oxide nanostructures was measured using the UV-VIS-NIR Optical Spectrophotometer. It was found that by scanning electron microscopy (SEM) and image results, there is a large amount of nanostructure with an average crystal size of 46.3-55.6 nm, which indicates that our synthesis process is a successful method for preparing Cr2O3 nanoparticles.

MoS2 is an attractive sulfur-resistant catalyst for directly converting sulfur-containing syngas to high value-added chemicals. However, the effect of the layered structure on the catalytic activity for CO hydrogenation reactions is far from clear. Herein, MoS2/carbon composite catalysts with 1–8 stacking layers in MoS2 crystallites are synthesized, and the impact of the layer numbers on the catalytic performance is probed for the low-temperature methanation of sulfur-containing syngas. The results indicate that the turnover frequency of CO methanation increases from 2.4 × 10-3 to 3.7 × 10-3 s−1 with decreasing layer numbers of MoS2 crystallites from 8.3 to 1.1. This result is thoroughly explained by the fact that the higher ratio of rim sites in MoS2 crystallites with fewer layer numbers enhances the catalytic activity, which originates from the facilitated activation of CO and H2. These understandings are important for the rational design and development of more efficient MoS2-based catalysts for CO hydrogenation.

Bio-ingredients (animal urine and honey) assisted synthesis of Fe doped ZnO nanostructures has been reported. The structural, optical, morphological, and thermal properties of Fe–ZnO nanostructures were investigated using XRD, FTIR, FESEM, TEM, and TGA. The average crystallite size of Fe–ZnO nanostructures made with animal urine is 34.2 nm, while those made with honey have an average crystallite size of 8.8 nm. It indicates that the size of Fe–ZnO nanostructure crystallites was determined in part by reaction time. FESEM was used to verify the nanostructures of the spherical shaped nanoparticles, and the honey Fe–ZnO sample showed a uniform distribution of particles. EDX analysis confirmed the existence of Zinc (Zn), Iron (Fe), and Oxygen (O) in the synthesized sample. According to TEM photos of Fe–ZnO nanostructures, the particle size of the samples is well correlated with the crystallite size determined by XRD. The thermal stability of Fe–ZnO nanostructures, as well as the effect of these natural ingredients on thermal stability, has been investigated. The surface charge and Zeta potential value of Fe doped ZnO nanoparticles using honey and Animal urine have been analyzed. The obtained values confirm the honey used Fe–ZnO nanoparticles has higher stability (−22.7 mV) than the animal urine assisted sample (−10.1 mV).

Strontium (Sr)-doped La0.67K0.33-xSrxMnO3 (LKSMO) ceramics were obtained by traditional sol-gel method. With increasing Sr content, full width at half maximum (FWHM) for temperature-dependent resistivity curves increased, resistivity decreased, and peak resistivity temperature (TP) shifted toward high temperature. Microstructure of LKSMO ceramics was characterized by X-ray diffraction, scanning electron microscopy, X-ray photoemission spectroscopy, energy dispersive spectrometry, and Fourier transform infrared spectroscopy, etc. Connection between microstructure and properties of ceramics was studied by combining double exchange mechanism, Jahn-Teller effect, and phenomenological percolation model. Electrical transport mechanism of ferromagnetic metal (FMM) and paramagnetic insulator (PMI) regions was employed to explain temperature coefficient of resistivity (TCR) and magnetoresistance (MR) behaviors of as-obtained samples. Various scattering factors, effective mass of itinerant electron, and energy difference between FMM and PMI phases affected FWHM of ρ-T curves in Sr-doped LKSMO ceramics. In sum, these findings provide physical mechanism and experimental guidance for synthesis of high-TCR and MR polycrystalline ceramics at room temperature.

Pure manganese titanate (MnTiO3) powder was successfully synthesized by means of the molten salt method, at 1000 °C for 3 h. The effect of salts used during the synthesis process was evidenced by X-ray diffraction (XRD). Structural parameters were calculated by the Rietveld refinement, where a crystallite size of 292 nm was estimated. Ultraviolet–Visible (UV–Vis) spectroscopy showed that MnTiO3 displays a wide light absorption range, from 200 nm to 800 nm. Through first-principles calculations, the band structure and density of states for ilmenite-type MnTiO3 were estimated, where an indirect band gap of 3.4 eV was obtained. Atomic composition and chemical bonds were determined by X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FT-IR), respectively. Electrochemical properties of MnTiO3 were analyzed using the Mott-Schottky curve, where an n-type semiconducting behavior and a flat band potential ( E f b ) of 1.41 V (vs NHE at pH = 0) were observed.

Multifunctional materials have gained huge attention owing to their great possibility in device applications. However, producing single-phase multifunctional materials, associated with various novel properties, has been proved to be a serious challenge. A simple yet effective way to overcome this barrier, is therefore of great importance. Here, we report the evolution of temperature- and magnetic field-dependent novel multifunctional phenomena in polycrystalline La2-xTbxCoMnO6. Substitution of Tb in ferromagnetic La2CoMnO6, induces antiferromagnetic ordering through development of antisite disorder and antiphase boundaries, and results in a phase separation between ferromagnetic/antiferromagnetic layers. This originates the coexistence of conventional and inverse magnetocaloric effects in this system. The switching between them, with its tunability with temperature and magnetic field, suggests a huge potential of this compound. In addition, a clear correlation is established between the magnetocaloric switching and field-induced metamagnetic transitions. Furthermore, the discovery of tunable giant exchange bias (~1.8 kOe) at very low cooling field (500 Oe), a reasonable self-exchange bias (270 Oe), and a large negative magnetoresistance (~14%), makes this system enormously attractive for practical applications and fundamental research. The present study proposes a novel and effective route for successfully preparing essential multifunctional compounds to open a new pathway toward room-temperature applications.

We present a comprehensive comparative analysis of acid textured and MACE (Metal Assisted Chemical Etching) nano-textured multi crystalline silicon (mc-Si) solar cells processed in an industrial cell line in terms of performance parameters. The batch average open circuit voltage of nano-textured solar cells was marginally lower and the measures for improving the same are discussed. Batch average short circuit current (J S C ) and fill factor (FF) were respectively 0.65 mA-cm−2 and 0.7% (absolute) higher for MACE nano-textured solar cells. Significantly lower surface reflectance in MACE nano-textured cells in the blue and near infrared regions are found to be the reason for the enhancement in J S C . The main component of FF gain is identified as the lower series resistance in MACE cells. The contact formation mechanism in screen printed mc-Si solar cells, investigated using scanning electron microscopy, revealed that the elevated portions at the boundaries of the textures act as favorable sites for silver crystallite precipitation. A larger areal density of such sites is observed on the MACE nano-textured surface than in case of acid textured solar cells, leading to a much lower series resistance. The results suggest the potential for the application of MACE in the more popular mono-crystalline silicon cell technology for further reduction of contact resistance. Alternatively, MACE may be used to obtain similar contact resistance with lower amount of silver paste, compared to iso- and pyramid textured solar cells.

Graphical abstract, Highlights • Nano-silver synthesized via solution evaporation method with octahedral crystal structure and crystallite size of 28 to 39 nm. • Irregular and non-uniform surface morphology. • Different functional on the surface of nano-silver included CH, CH2, OH, alkyne, and an alkyl halide. • Nano-silver synthesized at 70 °C and a dose of 3.0 g/L caused effective inhibition of E. coli., The modulation of antimicrobial properties of nanomaterials can be achieved through various physical and chemical processes, which ultimately affect subsequent properties. In this study, the antibacterial potential of nano-silver was investigated at 0.5, 1.0, 2.0, and 3.0 g/L, and its differential temperature synthesis was achieved at 20, 50, and 70 °C using the solvent evaporation method. Nano-silver particles exhibited FCC (octahedral) crystalline structure with crystallite sizes ranging between 28 and 39 nm calculated using XRD analysis. Moreover, irregular and non-uniform surface morphology was evident from SEM micrographs. The UV–Vis absorbance spectrum of nano-silver exhibited wave maxima at 433 nm, while the FTIR analysis depicted different modes of vibration indicating the CH, OH, C≡C, C-Cl, and CH2 functional groups attached to the surface. Lastly, nano-silver caused prominent inhibition (12.5 mm) in the Escherichia coli growth, particularly at 70 °C synthesis temperature and 3.0 g/L dose. It is concluded that both the nano-silver crystal growth temperature and dose contributed substantially to bacterial growth inhibition linked with subsequent size, shape-dependent properties.

Cr-doped zinc-lanthanum nanoferrites Zn1-xCrxLa0.1Fe1.9O4 (x = 0.09, 0.18, 0.27, and 0.36) were successfully synthesized using sonochemical reactors. Effect of powder production parameters were extensively studied and powder characterization was performed. Existence of cubic spinel structures in the prepared nanoferrites with the average crystallite size ranging from 35 to 51 nm was confirmed by X-ray diffraction studies. An electrochemical impedance analyzer was used to measure the dielectric constant (e′), loss tangent (tan δ), and complex dielectric constant (e") with respect to frequency and composition ratio. Maxwell–Wagner polarization and hopping mechanism were calculated to distinguish the variations in e′, tan δ, and e". The Nyquist impedance plots for nanoferrites revealed the pseudocapacitance as well as resistive behavior. Vibrating sample magnetometer studies reveled the ferromagnetic behavior of nanoferrites. Substantially increased saturation magnetization and decreased coercivity were noted with respect to increased Cr2+ ions in the prepared nanoferrites. It was found that the addition of chromium in Zn1-xCrxLa0.1Fe1.9O4 nanoferrites enhances the optical, electrical, and magnetic properties of the nanoferrites.

Zirconium Carbide (ZrCx) was irradiated with 10 MeV Au3+ ions to a dose of 10 displacements per atoms (dpa) and subsequently with 100 and 300 keV electrons in a transmission electron microscope (TEM). After ion irradiation, dislocation loops were observed in the microstructure and an increase in the number of carbon vacancies was revealed by Raman spectroscopy. Grazing incidence X-ray diffraction (GIXRD) analysis showed that neither amorphization nor oxidation occurred during ion irradiation of the specimen. Subsequent electron irradiation of the pre-implanted ZrCx foil led to formation of nanosized tetragonal ZrO2 precipitates (5−10 nm diameter) on the surface of the TEM lamella. The formation of the new oxide phase was not related to the electron beam-induced heating of the specimen, but to electron stimulated oxidation caused by the residual oxygen inside the transmission electron microscope. Changes in size and density of ZrO2 crystallites were observed between the pristine and ion irradiated ZrCx regions following electron irradiation, suggesting that the initial microstructure of the ZrCx substrate played a key role in the nucleation and growth of the oxide islands. The obtained results provide insights into the microstructural response of ZrCx to different types of radiation and the inadvertent effects of the electron beam during TEM analysis of in-situ and ex-situ ion irradiated ZrCx. Additionally, the findings of this work suggest a method to prepare local ZrO2 nanoprecipitates within ZrCx grains by selective electron beam irradiation.

In this work, Ni-M-Al (M = K, Na, and Li) LDH-derived catalysts were evaluated for the biogas dry reforming. The catalysts were prepared by co-precipitation and characterized by SBET, XRD, TPR, NH3-TPD, CO2-TPD, SEM and TPO. Reactions were carried out in a fixed bed reactor with online GC analysis in step-wise mode in the range of 500–750 °C and the stability tests were performed at 700 °C. All prepared samples exhibited hydrotalcite-type structure. Differences in reducibility and in the acidity of oxides were observed. The acidity of the catalyst was in the order: NiLi > NiNa > NiK, which is in the opposite order of monovalent cation size. The NiLi catalyst showed the highest resistance to sintering during the reactions due to the higher reduction temperature of mixed oxides (Ni2AlO4 and NiAl2O4) which results in smaller Ni° crystallite size after reduction. The results at 700 °C showed that NiLi catalyst deactivation occurs mainly by carbon deposition, whereas the deactivation of NiK and NiNa catalyst occurs mainly by sintering. TPO results indicated different carbon species produced depending on how the reaction is performed. All the catalysts produced carbon nanotubes at 700 °C.

Herein, nanocomposites films were prepared via the facile casting method by incorporating cellulose nanocrystals (CNCs) with arabinogalactan (AG), galactomannan (GM) or konjac glucomannan (KGM) respectively. The introduced polysaccharides maintained the transparency of CNCs films and promoted the UV blocking properties. In addition, mechanical strength of the nanocomposite films was greatly improved after the combination of polysaccharides. The interactions of hydroxyl-abundant macromolecules, smoother and tighter morphological structures, as well as the disturbed crystal structure were proved to be responsible for the improved properties. Hydrophilic lattice planes of cellulose crystallites were determined to interact with polysaccharides resulting in lower crystallite sizes and crystallinity. The cell culture assay revealed that the films had no cytotoxicity and presented a satisfactory cytocompatibility, because of the polysaccharides from plant cell walls introduced into the films. Therefore, the biocompatible nanocomposites films can be tuned by the addition of polysaccharides, which show great potentials for materials modification in optical, packaging and biomedical fields.

Cr3+-doped α-Al2O3 nanoparticles (Al2−xCrxO3, 0.005 ≤ x ≤ 0.05) were synthesized by co-precipitation method. X-ray diffraction (XRD) patterns of Cr3+:Al2O3 nanoparticles revealed the crystallite size of ∼53 nm and electron microscopy (SEM & TEM) confirmed the spherical nanoparticle formation. Diffuse reflectance spectra (DRS) displayed peaks at 406 and 558 nm corresponding to the Cr3+ transitions which became prominent with the increase in Cr3+ concentration which was also evidenced by the gradually increasing pink coloration of the samples. Photoluminescence (PL) studies showed the sharp red emission at 694 nm (ruby line) which was observed for all samples. The Dq/B value for all samples was found to be greater than 2.3 confirming the presence of Cr3+ ions in the octahedral sites. Chromaticity diagrams displayed the maximum red appearance for the sample with x = 0.01 and a lifetime of 4 ms. The synthesized Cr3+:Al2O3 nanoparticles with smaller crystallite sizes and narrow near monochromatic emission can be used in various applications including sensing, lasing, and bioimaging applications.

WOS:000707779000002 This study was conducted to investigate the impact of Calcium (Ca) and Manganese (Mn) dopants on the optical and surface properties of Titanium dioxide (TiO2) nanomaterial. Ca and Mn doped TiO2 thin films were fabricated by sol–gel spin-coating method. By keeping the doping ratio of Ca constant, Mn was doped at the ratios of 1, 3, and 5%. The morphological, structural and optical properties of the fabricated samples were taken by Atomic Force Microscope (AFM), Scanning Electron Microscope (SEM), Energy Dispersive X-Ray Analysis (EDX), X-Ray Diffraction Method (XRD) and UV–VIS spectroscopy. AFM and SEM analysis revealed that the morphological properties of TiO2 changed depending on the increase in doping ratio of Mn. XRD values obtained from the samples showed that the increases of crystallite size with manganese ions doping into the TiO2 the optical band gap of the samples increased with Ca and Mn dopants. As a result of the investigations, it was determined that Mn doping has significant effects on the morphological and optical properties of TiO2 films and the produced samples can be used in transparent conductive electrode applications, optoelectronic devices, and sensor production.

Introduction of artificial pinning centres in different morphology is a beneficial way to improve the flux pinning properties of a YBCO compound. In the present study, we report the effect of addition of sodium niobate (NaNbO3) nanostructures in two different form i.e. nanorods (NRs) and nanoparticles (NPs) with a varied wt% (0, 0.5, and 1 wt%) on the pinning capabilities of bulk YBCO polycrystalline samples. The orthorhombic crystal structure of YBCO was confirmed by the XRD spectra even in the nanocomposite samples. The existence of NPs or NRs on the surface and between the superconducting grains of YBCO was confirmed by morphological analysis. The critical temperature (Tc) remains almost unchanged as compared to pure YBCO on addition of NaNbO3 nanostructure in YBCO compound upto 1 wt% concentration. Even at higher fields (upto 6 T) and higher temperatures (upto 75 K), the addition of NaNbO3 NPs or NRs in YBCO nanocomposite resulted in a significant increase of ~2.6 times in the critical current density as compared to pure YBCO. In comparison to NRs added YBCO nanocomposite samples, NPs added YBCO nanocomposite samples showed higher improvement. Throughout the entire investigated range of applied field, the maximum pinning force was found for 0.5 wt% NPs added composite sample.

A series of Hafnium dioxide (HfO2) thin films with nominal thickness of 5–350 nm were reactively deposited on silicon（100）substrates at 200 °C using electron-beam evaporation. Based on the measurement and characterization techniques of spectroscopic ellipsometry, X ray diffraction, scanning electron microscopy and atomic force microscopy, the effect of growth thickness on the refractive index and crystallization of HfO2 film grown under the same conditions was studied. The results indicate that the change of refractive index of HfO2 film is closely related to the change of microstructure i.e., grain size and crystallization which change obviously with the increasing growth thickness. The average refractive index at 633 nm decreases about from 1.97 to 1.84 with the increase of the average size about from 0.5 nm to 7~8 nm and the crystallinity from zero to 74% when the thickness of HfO2 film increases from 5 nm to 350 nm. Meanwhile, a critical growth thickness of HfO2 film, somewhere on order of 130 nm, is confirmed at which the film transforms from an amorphous to a polycrystalline monoclinic structure. The sharp change of microstructure near the critical thickness value of HfO2 film leads to the abrupt change of optical properties of HfO2 film, such as the turning behaviors of the refractive index curve. The correlation between phase transformation, size and orientation of crystallite, packing density and hence the refractive index is established. The possible interpretations are proposed to well understand the underlying mechanism of the evolution of optical properties in HfO2 film-forming process.

Due to the inherent moisture instability problem of hybrid lead halide perovskites, polymer additives have to turn out to be a significant research area to enhance the moisture stability of these materials. It has been found that polymer engineering on the absorber layer of solar cells significantly improves chemical stability and overall device performance. This work reports the fabrication of pristine and polyvinylpyrrolidone (PVP) polymer capped methylammonium lead chloride (CH3NH3PbCl3) perovskite film via the electrospinning method. A structural study using an X-ray diffractometer shows a sharp fall in average crystallite size from 66.05 nm to 39.69 nm when PVP is used in the synthesis procedure. A similar trend is also seen in the microscopic analysis, which depicts that the particle size has decreased for PVP added CH3NH3PbCl3 perovskite film in comparison to CH3NH3PbCl3 pristine film. The surface coverage and uniformity of the film is much more in the presence of PVP. It has been noted from energy dispersive X-ray analysis that the oxygen content is ∼16% more in the pure film, i.e. PVP hinders the effect of moisture in perovskite film, which is the prime objective of this work. Moreover, the optical properties have been analyzed using diffuse reflectance mode of UV–Vis-NIR spectroscope. Finally, the use of CH3NH3PbCl3 as the electron transport layer has been demonstrated in Glass/FTO/CH3NH3PbCl3/CH3NH3SnI3/Spiro-OMeTAD/Au structured perovskite solar cell using the SCAPS-1D simulator. The above-mentioned cell exhibits a power conversion efficiency (PCE) of 21.65%, fill factor (FF) of 72.21%, 32.44 mA/cm2 of short circuit current density (Jsc), and 0.924 V open-circuit voltage (Voc).

We report the synthesis of Mo2CTx MXene from the Mo–In–C non-MAX phase using UV-assisted safe etching in phosphoric acid followed by ultrasonic exfoliation. The EDX and XPS spectra confirm the selective etching of indium from the non-MAX phase stoichiometry and formation of Mo2CTx MXene. The structural characterization using X-Ray diffraction revealed the Mo–In–C non-MAX phase and Mo2CTx MXene with crystallite sizes 37.26 ± 0.56 nm and 46.89 ± 0 .70 nm, respectively. The morphology of the samples analyzed using FESEM, confirmed the formation of the multilayered and monolayer 2D Mo2CTx. A slight increase in the interplanar spacing (~0.921 A) was observed in HRTEM images for Mo2CTx with respect to Mo–In–C. The synthesis of Mo2C MXene from a non- MAX phase using a hydrogen fluoride-free safe etching root unlocks the wide opportunity for the industrial bulk production of MXenes.

The outstanding photocatalytic activity of metal sulphide based photocatalysts have much attention in environmental remediation due to utilization of wide spectrum range. In present paper, the photocatalytic activity of NiS and NiS-CNTs (carbon nanotubes) nanocomposite has been investigated. The hydrothermal technique was used for synthesis of NiS and NiS/CNTs nanocomposite. Structural elucidation of NiS and NiS/CNTs nanocomposite was conducted by X-ray diffraction (XRD) and Fourier transform infra-red (FTIR) techniques. These characterization techniques verified the formation and purity of samples as extra peaks of impurities were not observed in the obtained data. Scherer formula was used to examine the crystallite size of NiS NPs and NiS/CNTs reported that 9.5 nm and 10.2 nm are sizes of NiS and NiS/CNTs respectively. Scanning electron microscopic (SEM) analysis revealed the reduction in the aggregation of NiS and improved the surface area to assist the redox reactions due to presence of CNTs. Current-voltage (I–V) measurements studied the electrical behaviour of photocatalysts. Optical measurements of synthesized samples were analysed by UV–Visible spectrophotometry. The improvement in bandgap energy of nanocomposite was main reason of excellent photocatalytic activity. About 96% degradation of methylene blue was recorded via NiS/CNTs nanocomposite within 50 min. Photocatalytic performance of nanocomposite is faster than individual metal sulphide due to production of more free radicals, Ni–S–C bond development, surface defects and availability of more reaction sites. These features improved the photocatalytic activity of NiS/CNTs and provide an evidence to use carbon nanotubes for the formation of metal sulphide nanocomposites. Antibacterial property of sample was investigated by four Gram negative bacteria (Proteus vulgaris, Klebsiella pneumonia, Escherichia coli and Pseudomonas aeruginosa) and one Gram positive bacteria (Staphylococcus aureus) at different concentrations using disc diffusion method. The possible mechanism for degradation of Methylene blue under UV–Visible illuminations has been discussed. The upgraded degradation of methylene blue by NiS/CNTs nanocomposite supported that it is promising material for treatment of wastewater.

The effects of pH of the reaction solution and the concentration of phosphoric acid on the crystal growth behavior of LaPO4 crystallites were investigated and the mechanical properties of rare-earth phosphates were compared. As a result, the concentration of phosphoric acid of 10% was beneficial to the crystal growth of LaPO4 nanocrystalline. When the pH value of the reaction solution was 2, the size of LaPO4 crystallites increased gradually with the increasing reaction temperature, and the smallest crystallite size of 43.27 nm was obtained after heat-treatment at 1000 °C. Simultaneously, the activation energy for crystal growth of LaPO4 nanocrystalline was relatively lower (26.82 kJ mol−1). With the decreasing radii of rare-earth ions, the hardness, Young's modulus and fracture toughness of the bulk rare-earth phosphates exhibited a reduced tendency, resulted from the increase of porosity under the same preparation process.

The grains of oriented W-type hexaferrite BaNi2GdxFe16-xO27 (BaW) where x = 0.0, 0.1, 0.2, 0.3, 0.4 and 0.5 grew uniformly along their c-axis perpendicular to the sample plane, which meant high remanence ratio of BaW. When Gd3+ substitution content was x = 0.0, the corresponding remanence ratio reached as high as 0.90. When x = 0.2, the oriented BaW simultaneously possessed high saturation magnetization (Ms= 58.36 emu/g), high coercivity (Hc = 1527 Oe), high remanence ratio (Mr/Ms = 0.85), relatively low magnetocrystalline anisotropy field (Ha = 10,253 Oe) and low ferromagnetic resonance linewidth (ΔH = 624 Oe). These characteristics indicated the material was suitable for the design of self-biased circulator operated at K band. Based on the BaW material, self-biased double Y-junction microstrip circulator was designed and realized well circulatory function at K band.

Thin-film transistor (TFT) applications of GeSn have attracted attention as a means of improving the performance of electronic devices. Based on our advanced solid-phase crystallization and TFT process technologies, we comprehensively studied the relationship between the film properties and TFT characteristics of polycrystalline GeSn. The initial Sn concentration ${x}_{\mathrm {i}}$ significantly changed the crystal and electrical properties of the GeSn layer. Excess Sn ( ${x}_{\mathrm {i}} \ge 4.5$ %) precipitated in GeSn and degraded its properties, whereas the appropriate amount of Sn effectively passivated defects in Ge and reduced the density of defect-induced acceptors and grain boundary traps while maintaining a high Hall hole mobility (>200 cm 2 V −1 s −1 ). The performance of the accumulation-mode TFTs fabricated under 400 °C also strongly depended on $\boldsymbol {x}_{\mathrm {i}}$ , achieving both a high field-effect mobility (170 cm 2 V −1 s −1 ) and on/off ratio (10 3 ) at ${x}_{\mathrm {i}} = 1.6$ %. This performance was shown to be the highest among Ge-based TFTs with grain boundaries in the channel.

Dysprosium compounds with high magnetic anisotropy are widely studied as single molecule magnets (SMMs). Here the anisotropic magnetocaloric effect in a Dy(III) SMM, {[Dy(OSiMe3)2(4-Mepy)5(BPh4)] 0.5Toluene}, was studied by single crystals. Angular dependent magnetization can be observed at 300 K because of its high magnetic anisotropy. SMM behavior measured along the easy axis direction is identical to that of the polycrystalline sample. Rotating magnetization from the easy axis to the hard plane gives a maximum magnetic entropy change (–ΔSR) of 3.05 J/(kg∙K) at 19 K at ΔB = 5 T, which enables the Dy(III) SMM to be used as a low-temperature rotating magnetic refrigerant.

The recrystallization behaviour of micron-sized cubic boron nitride (cBN) was studied by analysing the grain size and morphology of samples treated at 8−16 GPa/1500–2200 °C. The results show that the recrystallization temperature of cBN under a pressure of 8 GPa is approximately 1650 °C and increases by approximately 100 °C with every 2 GPa increase in pressure. Once grain recrystallization starts, the grains grow abnormally quickly as the temperature rises, and the strengthening effects of grain refinement and defect structure are greatly weakened. The recrystallization behaviour of cBN at high pressure is helpful to understand the sintering mechanism and control the microstructure and mechanical properties of sintered polycrystalline cBN compacts. In addition, the melting curve for cBN under high pressure is inferred according to the empirical relationship between recrystallization temperature and melting temperature, and the phase diagram for boron nitride is revised based on this new melting curve.

Crystal growth promotion for CuGaSe2 (CGSe) photovoltaic absorber by silver (Ag)-addition is demonstrated, enhancing device performance for wide-gap CGSe solar cells. By introducing Ag precursor, the grain size in the polycrystalline CGSe films deposited by the three-stage process is increased, and a residual Ga2Se3 phase during the growth is suppressed. Photoluminescence intensity is enhanced with Ag-addition, indicating reduced non-radiative recombination, which is related to the suppression of Ga2Se3 phase and reduction of undesirable deep defect levels. For the Ag-alloyed CGSe solar cells, Urbach energy defined from the sub-gap tail in exponential external quantum efficiency is monotonically reduced from 25.5 to 21.1 meV, suggesting the improvement of CGSe bulk quality by Ag-alloying. Open-circuit voltage is enhanced since carrier recombination in Ag-alloyed CGSe bulk is suppressed. Short-circuit current density is also enhanced as carrier collection efficiency is improved by widened depletion width due to the reduction of carrier concentration by Ag-alloying. On the other hand, excess Ag-addition leads to increased series resistance and deterioration of the built-in potential in the solar cells due to the reduced carrier concentration in the Ag-alloyed CGSe absorber. Finally, the conversion efficiency is maximized to 5.3% at [Ag] / ([Ag] + [Cu]) ratio of 0.07 for the Ag-alloyed CGSe solar cells. These findings will help the performance enhancement for the wide-gap CGSe solar cells.

The authors would like to thank R. Dittmann for useful discussions, T. Kocourek, O. Pacherova, S. Cichon, V. Vetokhina, and P. Babor for their contributions to sample preparation and characterization. The authors (M.T., A.D.) acknowledge support from the Czech Science Foundation (Grant No. 19-09671S), the European Structural and Investment Funds and the Ministry of Education, Youth and Sports of the Czech Republic through Programme “Research, Development and Education” (Project No. SOLID21 CZ.02.1.01/0.0/0.0/16-019/0000760). This study was partly supported by FLAG-ERA JTC project To2Dox (L.R. and E.K.). Calculations have been performed on the LASC Cluster in the Institute of Solid State Physics (ISSP), University of Latvia, and at the HLRS supercomputer centre, Stuttgart (Project DEFTD). The ISSP has received funding as a Centre of Excellence through the EU Horizon 2020 Programme H2020-WIDESPREAD-01-2016-2017-Teaming-Phase2 (CAMART2, Grant No. 739508)., The electronic properties, including bandgap and conductivity, are critical for nearly all applications of multifunctional perovskite oxide ferroelectrics. Here we analysed possibility to induce semiconductor behaviour in these materials, which are basically insulators, by replacement of several percent of oxygen atoms with nitrogen, hydrogen, or vacancies. We explored this approach for one of the best studied members of the large family of ABO3 perovskite ferroelectrics — strontium titanate (SrTiO3). The atomic and electronic structure of defects were theoretically investigated using the large-scale first-principles calculations for both bulk crystal and thin films. The results of calculations were experimentally verified by studies of the optical properties at photon energies from 25 meV to 8.8 eV for in-situ prepared thin films. It was demonstrated that substitutions and vacancies prefer locations at surfaces or phase boundaries over those inside crystallites. At the same time, local states in the bandgap can be produced by vacancies located both inside the crystals and at the surface, but by nitrogen substitution only inside crystals. Wide-bandgap insulator phases were evidenced for all defects. Compared to pure SrTiO3 films, bandgap widening due to defects was theoretically predicted and experimentally detected. © 2021, The Author(s). Published under the CC BY 4.0 license., This article was funded by FLAG-ERA JTC project To2Dox, Czech Science Foundation (Grant no. 19-09671S), Ministry of Education, Youth and Sports of the Czech Republic, programme “Research, Development and Education” (Grant no. SOLID21 CZ.02.1.01/0.0/0.0/16-019/0000760); the ISSP has received funding as a Centre of Excellence through the EU Horizon 2020 Programme H2020-WIDESPREAD-01-2016-2017-Teaming-Phase2 (CAMART2, Grant No. 739508).

Surface modification of Zirconium (Zr) with Zirconia (ZrO2) nanotubes (NTs) was performed using a two-step electrochemical anodization to investigate the role of such a modified surface in apatite formation and the inhibition of bacterial growth on Zr implants. Pore size at the surface of the NT arrays was controlled, along with the NT length, by varying the 2nd-step anodizing time duration. Nearly four-fold changes in the pore size were achieved by varying the anodization at the second anodizing step. The apatite formation on the implant surfaces plays an important role in the osteointegration process, which can be greatly influenced by the morphology and crystalline structure of the surface. XRD analysis of the anodized surfaces identified a mixed phase of monoclinic and tetragonal ZrO2 NTs with the crystallite size decreasing with increased 2nd anodizing time duration. Surface roughness of the ZrO2 NTs decreased with an increase in anodizing time duration. The ZrO2 NTs with the largest pore sizes, and the smallest crystallite sizes (ZrO2-15 m) favoured the deposition of a Ca-rich compound on their surfaces following 24 days of soaking in SBF, and showed the highest apatite-forming ability among all studied samples. Antibacterial tests showed that the ZrO2-15 m sample exhibited antibacterial properties with 1log10 CFU/mL reduction of S. aureus and E. coli incubated in a buffer solution for 4 h. Loading the NT layer with antibacterial drug led to a complete inhibition of both bacterial species. The rate of drug release was slowed down by dip coating the drug loaded NTs in a PLGA solution. A higher number of dip-coating steps not only slowed down the release of the drug, it also led to a higher suppression of growth in both bacteria. Longer antibiotic exposure and optimized dosage of the drug released from ZrO2 NTs can therefore be managed by modifying the NT morphology and the number of PLGA dip-coating steps.

Control on the size of copper oxide (CuO) in the nano range is a highly motivating approach to study its multifunctional nature. The present investigation reports a sol-gel derived Ni doped CuO nanoparticles (Cu1-xNixO). Rietveld refinement of the XRD spectra confirms the formation of single monoclinic phase of Cu1-xNixO nanoparticles having crystallite size within the range of 19–21 nm. Raman spectra show the presence of characteristics Raman active modes and vibrational bands in the Cu1-xNixO samples that corroborate the monoclinic phase of the samples as revealed by refinement of XRD data. The estimated band gap of pure CuO is found to be ∼1.43 eV, which decreases with the increase of dopant concentration into CuO matrix. This result is in line with estimated crystallite size. Magnetization curves confirm the weak ferromagnetic nature of Cu1-xNixO nanoparticles which reveal the DMS phase. This weak magnetic nature may be induced in the samples due to the exchange interaction between the localized magnetic d-spins of Ni ions and carriers (holes or electrons) from the valence band of pristine CuO lattice. Replacement of Cu+2 by Ni+2 ions into the host CuO lattice induces the magnetization. The quantified value of squareness ratio (S

We apply silver nanoparticles (Ag NPs) as catalysts of CO2 reduction in a zero-gap gas-flow electrolyser. Ag NPs stabilized by different ligands —branched polyethylenimine (BPEI), polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), and citrate— are used in the experiments. The as-prepared NPs have almost identical initial size distributions, yet their catalytic performance, in terms of achievable current and CO selectivity, is different. During electrolysis all Ag NPs exhibit unambiguous morphology changes; the degradation pathway they follow, however, markedly depends on the chemical nature of the capping agent stabilizing them. Scanning electron micrographs obtained before and after constant-charge electrolyses carried out at different potentials reveal that amongst the studied ligands, BPEI seems to be the most effective stabilizer of Ag NPs; in turn, however, BPEI also limits CO formation the most. In case of PVP, mostly corrosion (particle shrinkage) is observed at practically relevant electrolysing potentials, while the application of PEG leads more to particle coalescence. Ostwald ripening seems to appear only at high applied (H2 forming) potentials in case of the three afore-mentioned ligands while in case of citrate it becomes significant already at mild (CO forming) voltages. By studying the effects of capping agent removal and exchange we demonstrate that apart from ligands directly attached to the Ag NPs, also the excess of capping agents (adsorbed on the electrode surface) plays a decisive role in determining the extent and mode of catalyst degradation. The results of SEM-based particle sizing are also confirmed by synchrotron based wide-angle X-ray scattering measurements that provide further insight into the evolution of crystallite size and lattice strain in the applied Ag NPs during electrolysis.

Ferroelectric nanostructured e phase tungsten trioxide (e- W O 3 ) is emerging as an important functional material with unique gas sensing and optoelectronic properties. However, e- W O 3 phase is typically unstable in the bulk at room temperature (RT) and it has only been produced at ambient conditions by rapid solidification processes, such as Flame Spray Pyrolysis (FSP). This work aims to assess the overall stability of the e phase at the nanoscale by studying its transformation from the stable γ phase to upon cooling. In-situ Raman spectroscopy has explored the effect of crystallite size on the solid-solid phase transformation from the symmetric γ (monoclinic) phase into the acentric e (monoclinic) phase. The phase transformation onset temperature ( T o n s e t ) ranges from −43 °C for bulk state to −150 °C for crystallites of 68 nm in size and varies linearly with the inverse of the crystallite size radius ( 1 r ) .

This work reports the preparation of nanocrystalline Ni-Gd0.1Ce0.9O1.95 (NiO-GDC) anode powders using a novel single-step co-precipitation synthesis method (carboxylate route) based on ammonium tartrate as a low-cost green precipitant. The thermogravimetric analysis (TGA) of the synthesised powder showed the complete calcination/crystallisation of the resultant precipitates to take place at 500 °C. The prepared NiO-GDC powder was coated on a GDC electrolyte disc and co-sintered at 1300 °C. A mixture of La0.6Sr0.4Co0.2Fe0.8O3−δ and GDC was used as the cathode material and subsequently coated onto the anode-electrolyte bilayer, resulting in the fabrication of a NiO-GDC|GDC|La0.6Sr0.4Co0.2Fe0.8O3−δ-GDC cell. The crystallite size of both NiO and CeO2 phases were estimated using the X-ray powder diffraction (XRD) profiles and were calculated to be ~14 nm. Applied H2 temperature-programmed reduction (H2-TPR) analysis indicated a synergetic effect among different anode composites' constituents, where an intense interaction between the dispersed NiO nanocrystalline particles and the GDC crystallite phase had weakened the metal-oxygen bonds in the synthesised anode composites, resulting in a strikingly high catalytic activity at temperatures as low as 300 °C. The electrochemical impedance spectroscopy (EIS) and the electrochemical performance of the fabricated cells were measured over a broad range of operating temperatures (500–750 °C) and H2/Ar-ratios of the anode fuel (e.g. 100%–15%). Quantitative analysis from the EIS data and the application of the distribution of relaxation times (DRT) method allowed for the estimation of the activation energies of the anodic high and intermediate frequency processes that were 0.45 eV and 0.76 eV, respectively. This is the first report of a NiO-GDC synthesis, where a considerable improvement in activation energy is observed at the low-temperature region. Such low activation energies were later associated with the adsorption/desorption process of water molecules at the surface of NiO-GDC composite, indicating a high activity towards hydrogen oxidation.

Cd1-xZnxS thin films were deposited by chemical bath deposition (CBD) technique, which is simple and cost effective, in a chemical bath containing appropriate amount of cadmium acetate, zinc acetate, and thiourea as precursors, in a clean glass substrate. The deposition was carried out by varying the bath temperatures (70 °C, 75 °C, 80 °C, and 85 °C) of the precursor solution. The XRD results indicate the existence of hexagonal structures of Cd1-xZnxS with an average crystallite size of ∼ 27–41 nm. EDX studies confirm the presence of Cd, Zn, and S in the films. HRTEM and SAED patterns show the crystalline nature of the films with the coexistence of the hexagonal phase. The optical constants viz; optical band gap, Urbach energy, static refractive index, and optical conductivity were studied by using UV- Vis transmission spectra as a function of CBD temperature. It was observed that with the increase of bath temperature in the above range, there were concomitant decreases in optical band gap from ∼3.3 to 2.8 eV. The Urbach energy, optical conductivity, and static refractive index of the films increase with the increase in bath deposition temperature. FTIR studies confirm the formation of ternary Cd1-xZnxS thin films.

In this study, Eu3+ doped natural fluorapatites [Ca10(PO4)6F2:xEu3+ (x = 0.1, 0.3 and 0.5)] were produced from a natural waste by solid-state powder synthesis, conventional sintering, and spark plasma sintering techniques. The effects of doping content and crystallite size on luminescence properties of fluorapatite were investigated by XRD, SEM, and PL analysis. The obtained results showed that luminescence emission's intensity significantly increased with doping content, but no effect was observed on the density and crystallite size. For the samples produced with different methods, emission intensity was the lowest for sintered samples by SPS (1150 °C, 10 min, 50 MPa) with the smallest crystalline size. In contrast, emission intensity was found much higher for synthesized powders with the largest crystallite size. Furthermore, upon excitation under UV radiation, the Eu doped fluorapatites demonstrated the characteristic 5D0–7F2 and 5D0–7F4 emission lines of Eu3+ at 618 nm and 704 nm (red region) with an ultrahigh intensity that has been firstly observed in the literature. Therefore, Eu doped fluorapatites, quickly produced from a natural waste in an eco-friendly and cost-effective way, carry a potential to be used in biological applications and lightning applications. © 2021 Elsevier Ltd and Techna Group S.r.l.

⍺-alumina powder with an average particle size of 180 nm was dispersed into a photosensitive resin to prepare slurry with a solid content of 40 vol% in this study. The main defects in fabricating high-performance alumina ceramics using digital light processing (DLP) 3D printing are crossing cracks resulting from the tensile stress induced by constrained shrinkage during polymerization and delamination arising from insufficient adhesion between the printed layers. The different photocurable resin systems and different amounts of plasticizer, PEG400, effects on the defect formation, sintered density, and mechanical strength were investigated. It was observed that the optimal resin composition was made up of monomer (1,6-hexanediol diacrylate) and oligomer (Bisphenol A epoxy acrylate) at the ratio of 4:1. For the slurry with binder/plasticizer of 8:2, the sintered body defects can be completely eliminated and the sintered density and average flexural strength can reach 94% and 340 MPa, respectively.

Pure (x = 0.0 wt%) superconducting YBa2Cu3O7−δ (YBCO) sample and added YBCO sample with 0.1 wt% artificial barium titanate (BTO) and 0.1 wt% tungsten trioxide (WO3) nanoparticles were prepared using the solid-state reaction route. Phase purity was analyzed via the X-rays diffraction technique. Scanning electron microscopy showed a high density of isolated W-rich secondary phases embedded within the YBCO added sample. Furthermore, both WO3 and BTO nanoparticles tend to reside at the grain boundaries and play the role of bridges connecting the YBCO superconducting granules. Quantitative analysis performed on the areas where nanosized entities induced by BTO and WO3 phases was evidenced by EDX analysis equipped with SEM instrument. The values of Hc2 increased from 1.6 T for pristine to 3.4 T for BTO/WO3 added samples. The superconducting parameters determined by AC susceptibility measurements also showed an improvement with WO3 and BTO nanoparticles co-addition. The value of Jcinter(0) increases from 1.18 kA/cm2 for the pristine sample to 5.10 kA/cm2 for BTO/WO3 co-added sample. Hence, the incorporation of artificial BTO and WO3 nanoparticles into the YBCO superconducting phase could be a useful way to make such compounds available in practical applications.

The lamellar structure of (Bi,Sb)2(Te,Se)3 alloys makes it difficult to achieve isotropic thermoelectric properties in the directions along and perpendicular to the c-axis, especially for n-type samples. In this work, by introducing Cu in polycrystalline n-type CuxBi2Te2.7Se0.3 and applying the traditional synthesis process of high-energy ball milling and hot pressing, substantial enhancement of the thermoelectric figure of merit zT is obtained in both in-plane and out-of-plane directions. The intercalated Cu not only provides electron transport media for mobility improvement but also reduces the lattice thermal conductivity owing to the strain fluctuation. Typically, the van der Waals gap in the out-of-plane direction leads to relatively slower mobility and lower lattice thermal conductivity. Taking into account the same average density-of-state effective mass (mavg* ∼ 1.5me) predicted based on a single parabolic model, the obtained quality factor β is comparable in both directions. As a result, a peak zT ∼ 1.05 at 420 K and the average zT approaching to 1.0 in the temperature range 300-500 K are obtained in both directions for the Cu0. 02Bi2Te2.7Se0.3 sample. The simple synthesis process and isotropic thermoelectric properties in this work make n-type Bi2Te3 more convenient for potential production and application.

Progress in understanding crystallization pathways depends on the ability to unravel relationships between intermediates and final crystalline products at the nanoscale, which is a particular challenge at elevated pressure and temperature. Here we exploit a high-pressure atomic force microscope to directly visualize brucite carbonation in water-bearing supercritical carbon dioxide (scCO2) at 90 bar and 50 °C. On introduction of water-saturated scCO2, in situ visualization revealed initial dissolution followed by nanoparticle nucleation consistent with amorphous magnesium carbonate (AMC) on the surface. This is followed by growth of nesquehonite (MgCO3·3H2O) crystallites. In situ imaging provided direct evidence that the AMC intermediate acts as a seed for crystallization of nesquehonite. In situ infrared and thermogravimetric–mass spectrometry indicate that the stoichiometry of AMC is MgCO3·xH2O (x = 0.5–1.0), while its structure is indicated to be hydromagnesite-like according to density functional theory and X-ray pair distribution function analysis. Our findings thus provide insight for understanding the stability, lifetime and role of amorphous intermediates in natural and synthetic systems. Non-classical crystallization may proceed through formation of intermediate phases, but it is not known whether these are linked to the final crystallization. Here, using an atomic force microscope at 90 bar, brucite carbonation is directly observed, with an amorphous intermediate acting as the seed for crystalline nesquehonite.

Million tons of cellulosic paper have been used for insulating coils in oil-filled electrical power transformers, thereby assuring the electricity supply for our societies. The high working temperatures in transformers constantly degrade paper insulators throughout their service life of up to 40 years. We approached the structural changes in oil-immersed cellulosic paper samples upon thermal stress in a study that compared unbleached softwood Kraft paper used as insulator paper with pure cotton cellulose paper. The model experiments used a thermal treatment in transformer oil at 170 °C for up to 14 days. The samples were characterized by means of 13C CP/MAS NMR spectroscopy, mainly based on deconvolution of the C4 resonance. An automated, fast, and reproducible C4 resonance deconvolution employing the “Peak Analyzer” tool of OriginPro 2020 (OriginLab Corporation, USA) was developed and used to exploit 13C CP/MAS NMR spectroscopy for the characterization of thermally stressed paper samples. Our results show that thermally induced structural changes depend heavily on the composition of paper, that hornification and coalescence of fibrils take place, and that the allomorph composition of cellulose crystallites is altered under the given conditions. Graphical abstract

Synthesis, optical, mechanical, and structural characterization of organic–inorganic nanocomposite thin films based on polyethylene oxide and poly(vinyl alcohol) (PVA) polymers incorporated with (1:0), (0.75:0.25), (0.5:0.5), (0.25:0.75), and (0:1) content percentage ratios of ZnO-NPs: Al2O3-NPs nanoparticles are reported. The optical properties, including the absorption coefficient, refractive index, extinction coefficient, dielectric function, and optical band gap for the films, are investigated from the measured transmittance and reflectance using a newly derived mathematical model. The as-grown PVA-PEO polymeric thin films exhibit transmittance of 87% while it decreases down to 75% with ZnO-NPs and decreases in between by the addition of Al2O3-NPs. However, the refractive index increases from 2.0 with ZnO-NPs to 2.7 with Al2O3-NPs. The band gap energy is from 3.98 to 3.89 eV accordingly. The dislocation density $$,$$ crystallite size, and average internal strain obtained from the X-ray diffraction patterns exhibit abnormal behavior for equal ratio (0.5:0.5) of the two types of NPs compared with other ratios. Fourier transform infrared (FTIR) spectroscopy measurements to elucidate the major vibrational modes and bonding in the nanocomposite thin films. A redshift of the major peaks has been observed for all investigated compositional ratios indicating a shift of the absorption edge confirming the band gap reduction. The SEM micrographs show a clear form of nanocomposites with PVA-PEO/ZnO-NPs compared to those when Al2O3-NPs or a combination of the two kinds of NPs are introduced to the complex matrix. Our detailed analysis of the physical properties of PVA-PEO/ZnO-Al2O3 indicates their potential to be candidate materials for modern optical and optoelectronic devices.