Range Of Crystal Sizes Research Articles

Photocatalytic activity for degradation of methylene blue dye-mediated nanocomposite-copper oxide/graphene oxide preparation from blood solution via hydrothermal method with laser irradiation

Blood solution contains an abundant supply of metals, natural polysaccharides, and protein. Copper oxide/graphene oxide nanocomposite (CuO/GO NCs) was created by the hydrothermal method of mixing a blood solution with copper nitrate (Cu2NO3) salt and graphene (G) material, followed by irradiation with a pulse laser ablation (PLA) (Nd-YAG) technique at 250 Mj, 532 nm, 5 cm, and 900 pulses. Paper filters were used to investigate the methylene blue (MB) dye degradation of CuO-GO NCs produced via the PLA process. The structure and optical properties of CuO-GO-NCs were studied and analyzed using X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM) images, transmission electron microscopy (TEM) images, and UV–visible spectra. CuO/GO NCs have a cubic shape with an average crystal size range of 11–52 nm, according to XRD research. An average particle size of 40 nm is created in the surface morphology investigated with FE-SEM, indicating the form of small grains in the nanoparticle. Inside cell morphology examined by TEM, a grain particle size of 40 nm is produced, suggesting that the nanoparticle has a tiny spherical form for CuO NPs, while the morphology of GO NPs has a nanosheet-like structure. CuO/GO NCs have an optical band edge value of 2.5 eV and a wavelength of 352 nm, according to the UV–visible spectrum. Using filter paper containing CuO/GO NCs, the degradation efficiency of MB dye after 50 min in the presence of ambient light in the environment was 99 %. This is a brand-new, rapid, and safe technique that has never been used before.

The Biological Crystals in Chamid Bivalve Shells: Diversity in Morphology and Crystal Arrangement Pattern

Chamid bivalves are marine organisms that live in high-energy environments and are cemented to hard substrates. To avoid shell damage, the organisms form thick, densely ornamented shells. Shell material consists of aragonite, and the ornamentation may be either aragonitic or calcitic. The latter can be developed as scaly spines, rows of blades, or comarginal, radial arched lamellae. We investigated biological crystal morphology and mode of assembly of Chama arcana and Chama gryphoides shells. Structural characteristics were obtained from electron backscatter diffraction (EBSD) measurements, complemented with laser confocal and BSE imaging. We found a wide range of crystal morphologies and sizes, ranging from irregularly shaped calcite and/or aragonite prisms to tiny and thin aragonite laths. We observed four different modes of crystal assembly patterns: 1. strongly interlocked dendritic calcite units forming the ornamentation blades; 2. aragonite laths arranged to lamellae forming the outer shell layer, the layer adjacent to the calcite; 3. aragonite laths arranged into blocks comprising inner shell layers or aragonitic ornamentations; and 4. shell portions consisting of aragonite prisms, structured in size and crystal orientation, at muscle attachment sites. These four different types of crystal arrangements were observed for the shells of the investigated chamid species; however, they had slightly different strengths of structuring and slight variations in crystal organisation. Additionally, we observed unique microstructural features in Chama shells: We report ornamentation crystals resembling idiomorphic calcite and novel, twinned entities found at the changeover between the aragonitic layers. We highlight and discuss these differences and anomalies in this contribution.

Facile Synthesis and Characterization of Zirconia Nanoparticles in Dental Applications

Scientists and dentists use tiny particles called ZrO2/Nps (Zirconia Nanoparticles) in medicine. In addition, zirconia particles are commonly used in the realm of medicine and dentistry. They are ideal for tooth structure because of their beneficial properties. The objective of this research is to prepare zirconium oxide nanoparticles in a simple and easy way. Nano-zirconium oxide is prepared using the co-precipitation method. The produced powder was diagnosed using tools like X-ray diffraction, microscopy, and spectroscopy, which also analyzed its properties such as X-ray spectroscopy and density measurement. The XRD results confirmed that the powder product has high purity. The crystal size range is 27.97nm. The results match the (JCPDS (ZrO2) sheet No.79-1769). The EDX test revealed the presence of the following elements (Zr–O). The test of SEM (Scanning Electron Microscope) show that the particles nearly spherical and the size was 74.03nm. The Zr–O stretching modes and the Zr–O2–Zr bending modes were confirmed by the FTIR (Fourier transform infrared). The density of ZrO2/Np was measured several times and determined it to be (5.07±0.12 g/cm3).

The Synthesis of Y-zeolite-modified CaCO3-ZnO Nanocomposites as an Antibacterial Agent

The ability of inorganic antibacterial agents like metal oxides and nanoscale inorganic materials to inhibit bacterial growth rates has yet to receive much research attention. In this study, CaCO3-ZnO/Y-zeolite nanocomposites were created utilizing coprecipitation and impregnation techniques with Ca(CH3COO)2, Zn(CH3COO)2 2H2O, Y-zeolite precursors. Physical and chemical characteristics of nanocomposites have been investigated using XRD, FTIR, and SEM-EDX characterizations. The agar-well diffusion method tested the substance for antibacterial activity against gram-positive and gram-negative bacteria. Nanocomposites have a crystal size range of 35.46-36.53 nm and a crystallinity of 35-37 %, according to the results of XRD analysis. The carbonate groups are visible in FTIR data at wave numbers 1433, 875, and 712 cm-1. The Zn-O absorption band was verified at wave numbers 600-400 cm-1. The Y-zeolite absorption bands at wave numbers 1012-997 cm-1 and 745-746 cm-1 were confirmed. The particle morphology is cube-shaped with irregular sizes. The EDX result showed that the composition consists of 35.92 % calcium, 1.68 % zinc, 44.81 % oxygen, and 13.79 % carbon as elements. With the addition of 2.5 % Y-zeolite, the antibacterial activity of nanocomposites showed the best results, with an inhibition zone diameter of 7.62 mm against Escherichia coli and 6.56 mm against Staphylococcus aureus bacteria.

A new approach to crystal habit retrieval from far-infrared spectral radiance measurements

Abstract. To generate reliable climate predictions, global models need accurate estimates of all the energy fluxes contributing to the Earth's radiation budget (ERB). Clouds in general, and more specifically ice clouds, play a key role in the determination of the ERB as they may exert either a feedback or a forcing action, depending on their optical and microphysical properties and physical state (solid/liquid). To date, accurate statistics and climatologies of cloud parameters are not available. Specifically, the ice cloud composition in terms of ice crystal shape (or habit) is one of the parameters with the largest uncertainty. The Far-infrared Outgoing Radiation Understanding and Monitoring (FORUM) experiment, foreseen to be the ninth Earth Explorer mission of the European Space Agency, will measure, for the first time spectrally resolved from space, the entire upwelling spectrum emitted by the Earth from 100 to 1600 cm−1. The far-infrared portion of the Earth spectrum, especially from 200 to 600 cm−1, is very sensitive to cloud ice crystal shapes; thus, FORUM measurements could also represent an opportunity to study the ice cloud composition in terms of ice crystal habit mixtures. To investigate this possibility, we developed an accurate and advanced scheme allowing us to model ice cloud optical properties – also in cases of clouds composed of mixed ice crystal habits. This feature is in fact necessary because in situ measurements acquired over the years also point out that the shape of ice cloud crystals varies depending on the crystal size range. In our model, the resulting cloud optical properties are also determined by the input habit fractions. Thus, the retrieval of these fractions from spectral radiance measurements can be attempted. Using 375 different cloudy scenarios, we assess the performance of our retrieval scheme in the determination of crystal habit mixtures starting from FORUM-simulated measurements. The most relevant error components affecting the retrieved cloud parameters are not very large and are of random nature; thus, FORUM measurements will allow us to set up an accurate climatology of cloud parameters. To provide an example of the benefit that one could get from the habit mixture retrievals, we also show the improved accuracy of the thermal outgoing fluxes calculations compared to using assumed mixtures.

Impact of the crystal size of crystalline active pharmaceutical compounds on loading into microneedles

Microneedle (MN) technology offers a promising platform for the delivery of a wide variety of active pharmaceutical compounds into and/or through the skin. Yet, the low loading capacity of MNs limits their clinical translation. The solid state of loaded compounds, crystallinity versus amorphousness and crystal size of the former, could greatly affect their loading. Here, we investigated the effect of the crystal size of crystalline compounds on their loading into dissolving MNs, prepared using the solvent-casting technique. A model crystalline compound was subjected to crystal size reduction via wet bead milling and loaded into dissolving MNs. A range of crystal sizes, from micro to nano, was obtained via different milling periods. The obtained crystals were characterized for their size, morphology, and sedimentation behavior. Besides, their content, solid state inside the MNs, and impact on the MN mechanical strength were assessed. The crystals exhibited size-dependent sedimentation, which dramatically affected their loading inside the MNs. However, crystal size and sedimentation demonstrated a negligible effect on the mechanical strength and sharpness of the needles, hence no anticipated impact on the MNs’ drug delivery efficiency. The elucidation of the correlation between the crystal size and MN loading opens new potentials to address a major drawback in MN technology.

Design of highly active Ni catalysts supported on carbon nanofibers for the hydrolytic hydrogenation of cellobiose.

The direct transformation of cellulose into sugar alcohols (one-pot conversion) over supported nickel catalysts represents an attractive chemical route for biomass valorization, allowing the use of subcritical water in the hydrolysis step. The effectiveness of this process is substantially conditioned by the hydrogenation ability of the catalyst, determined by design parameters such as the active phase loading and particle size. Herein, mechanistic insights into catalyst design to produce superior activity were outlined using the hydrolytic hydrogenation of cellobiose as a model reaction. Variations in the impregnation technique (precipitation in basic media, incipient wetness impregnation, and the use of colloidal-deposition approaches) endowed carbon-nanofiber-supported catalysts within a wide range of Ni crystal sizes (5.8–20.4 nm) and loadings (5–14 wt%). The link between the properties of these catalysts and their reactivity has been established using characterization techniques such as X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and inductively coupled plasma-optical emission spectroscopy (ICP-OES). A fair compromise was found between the Ni surface area (3.89 m2/g) and its resistance against oxidation for intermediate crystallite sizes (∼11.3 nm) loaded at 10.7 wt%, affording the hydrogenation of 81.2% cellobiose to sorbitol after 3 h reaction at 190°C and 4.0 MPa H2 (measured at room temperature). The facile oxidation of smaller Ni particle sizes impeded the use of highly dispersed catalysts to reduce the metal content requirements.

Pore-Scale Mechanisms for Spectral Induced Polarization of Calcite Precipitation Inferred from Geo-Electrical Millifluidics.

Spectral induced polarization (SIP) has the potential for monitoring reactive processes in the subsurface. While strong SIP responses have been measured in response to calcite precipitation, their origin and mechanism remain debated. Here we present a novel geo-electrical millifluidic setup designed to observe microscale reactive transport processes while performing SIP measurements. We induced calcite precipitation by injecting two reactive solutions into a porous medium, which led to highly localized precipitates at the mixing interface. Strikingly, the amplitude of the SIP response increased by 340% during the last 7% increase in precipitate volume. Furthermore, while the peak frequency in SIP response varied spatially over 1 order of magnitude, the crystal size range was similar along the front, contradicting assumptions in the classical grain polarization model. We argue that the SIP response of calcite precipitation in such mixing fronts is governed by Maxwell-Wagner polarization due to the establishment of a precipitate wall. Numerical simulations of the electric field suggested that spatial variation in peak frequency was related to the macroscopic shape of the front. These findings provide new insights into the SIP response of calcite precipitation and highlight the potential of geoelectrical millifluidics for understanding and modeling electrical signatures of reactive transport processes.

Influence of ettringite on the crack self-repairing of cement-based materials in a hydraulic environment

Abstract As a green and environmental protection method, the self-repairing technology has great expectations to be met. In this study, the influence of ettringite on the crack self-repairing of cement-based materials in a hydraulic environment was systematically analyzed. First, the composition and pore characteristics of the self-repairing carrier was studied by XRD, XRF, and the mercury injection method. The composition was basically consistent with cement-based materials, and the structure of the self-repairing carrier was relatively dense. Second, the products were analyzed by SEM and EDS, and it was found that the distribution range of crystal size was from 1 to 20 µm, the cube and flocculent accumulation was calcite, while the rod and flake crystals were ettringite. Finally, the repair effect on the surface and inside of the crack was demonstrated by the crack area repair rate and water permeability resistance. Compared with single microbial mineralization, the synergistic repair effect of microbial mineralization and ettringite formation was better in water permeability resistance. With the further increase of water pressure, its advantages would be more obvious.

Correlating Surface Structures and Electrochemical Activity Using Shape-Controlled Single-Pt Nanoparticles.

We report a method for synthesizing and studying shape-controlled, single Pt nanoparticles (NPs) supported on carbon nanoelectrodes. The key advance is that the synthetic method makes it possible to produce single, electrochemically active NPs with a vast range of crystal structures and sizes. Equally important, the NPs can be fully characterized, and, therefore, the electrochemical properties of the NPs can be directly correlated to the size and structure of a single shape. This makes it possible to directly correlate experimental results to first-principles theory. Because just one well-characterized NP is analyzed at a time, the difficulty of applying a theoretical analysis to an ensemble of NPs having different sizes and structures is avoided. In this article, we report on two specific Pt NP shapes having sizes on the order of 200 nm: concave hexoctahedral (HOH) and concave trapezohedral (TPH). The former has {15 6 1} facets and the latter {10 1 1} facets. The electrochemical properties of these single NPs for the formic acid oxidation (FAO) reaction are compared to those of a single, spherical polycrystalline Pt NP of the same size. Finally, density functional theory, performed prior to the electrochemical studies, were used to interpret the experimental results of the FAO experiments.

On the contribution of Pair Distribution Function (PDF) to the characterization of nanocrystalline MOFs: The case of M-MOF-74

Nanoporous Metal-Organic Frameworks (MOFs) have a great potential in so many industrial applications including heterogeneous catalysis and gas storage/capture/separation. MOF-74 is one of the most interesting MOFs in an academic context, as it contains open metal sites, possesses high versatility in metal nature, and can be prepared with so small crystal size. As a consequence, the catalytic activity of these nanocrystalline materials is superior to that given by their conventional counterparts. However, their characterization by conventional X-ray diffraction (XRD) is insufficient. In this work, we present a joint study of XRD and Pair Distribution Function (PDF) -both acquired under synchrotron radiation- of a series of nanocrystalline M-MOF-74 materials (M = Mg, Co, Ni, Cu or Zn) prepared at room temperature. Whereas the XRD continues being lacking for an adequate structural characterization, PDF provides key structural information at medium and short range and, therefore, is ideal for studying such nano-domains. It was confirmed that these materials are exclusively composed by MOF-74 phase and that their poor ability to diffract is due solely to their eminent nanocrystallinity, which resulted to be even more pronounced than it has been previously estimated. Beyond Scherrer-like approaches, PDF can give direct information about the range of crystal size in nanocrystalline materials. Moreover, the technique is also able to detect slight structural deviations in short-range environments, just like it is made clear in the case of Cu-MOF-74 compared with the rest of M-MOF-74 materials, which possesses a marked Jahn-Teller effect in the octahedral coordination of Cu.

Energy spectra due to the intrinsic radiation of LYSO/LSO scintillators for a wide range of crystal sizes.

Most detectors in current positron emission tomography (PET) scanners and prototypes use lutetium oxyorthosilicate (LSO) or lutetium yttrium oxyorthosilicate (LYSO) scintillators. The aim of this work is to provide a complete set of background energy spectra, due to the scintillator intrinsic radioactivity, for a wide range of crystal sizes. An analytical model, developed and validated in a previous work, was used to obtain the background energy spectra of square base cuboids of different dimensions. The model uses the photon absorption probabilities of the three gamma rays (88, 202, and 307keV) emitted following the beta decay of 176 Lu to 176 Hf excited states. These probabilities were obtained for each crystal size considered in this work from Monte Carlo simulations using the PENELOPE code. The probabilities are then used to normalize and shift the beta spectrum to the corresponding energy value of the simultaneous detection of one, two, or three gamma rays in the scintillator. The simulated cuboids had side lengths of 5, 10, 20, 30, 40, 50, and 60mm and crystal thickness T=2.5, 5, 10, 15, and 20mm. From these results a complete set of energy spectra, including intermediate dimensions, were obtained. In addition, LYSO and LSO were compared in terms of their analytical background energy spectra for two crystal sizes. The analytical spectra were convolved using a variable Gaussian kernel to account for the energy resolution of a typical detector. A parameterization of the photon absorption probabilities for each gamma ray energy as a function of the cuboid volume to surface area ratio was obtained. A data set of L(Y)SO background energy spectra was obtained and is available for the reader as 2D histograms. The model accurately predicts the structure of the energy spectra including the relative peak and valley intensities. The data allow visualizing how the structure evolves with increasing crystal length and thickness. Lutetium yttrium oxyorthosilicate and LSO present very similar background energy spectra for the range of sizes studied in this work and therefore the data generated can be confidently used for both scintillator materials. The filtered spectra showed a variable shift in the main peaks, depending on crystal size, alerting that to achieve a correct detector calibration using the background spectrum is not straight forward and requires precise data analysis and measurements. In addition, we found that square base L(Y)SO cuboids with same volume to surface area ratio have background spectra with the same structure. We present the energy spectra of L(Y)SO crystal of different sizes which will be very useful for industry and research groups developing and simulating detectors for positron imaging applications in terms of calibration, quality assurance, crystal maps, detector fine gain tuning, background reduction and other applications using the long-lived 176 Lu source. We analyzed the data produced in this work and found that crystal cuboids with equal volume to surface area ratio produce the same background energy spectra, a conclusion that simplifies its calculation and clarifies why the same energy spectrum is observed under different experimental setups.

High performance single-mode vertical cavity surface emitting lasers based on CsPbBr3 nanocrystals with simplified processing

• A simple ligand-assisted reprecipitation strategy is developed for applications in CsPbBr 3 PNCs-based VCSELs. • The fabricated VCSELs exhibit excellent single-mode lasing without mode competition. • Low lasing threshold (8 μJ/cm 2 ), high Q (~1425) and SE coupling factor (~0.24) are achieved. • The ultrafast decay of ~10 ps indicate a high modulation bandwidth (~GHz) of the VCSELs. Perovskite nanocrystals (PNCs) have emerged as highly promising optical gain materials for laser applications. Despite the recent surge of reports on their lasing performance, it remains a challenge to achieve PNCs-based single-mode vertical cavity surface emitting lasers (VCSELs) because of their inhomogeneous gain saturation. Here, we successfully demonstrate high performance single-mode VCSELs using CsPbBr 3 PNCs that were synthesized via a facile ligand-assisted reprecipitation strategy. The optical gain medium with wide crystal size range was fabricated, and the dense assembly of each individual PNCs was expected to offer a homogeneous optical continuum to reduce gain saturation inhomogeneity. The fabricated VCSELs exhibit excellent single-mode lasing at ~541 nm without mode hopping and high spontaneous emission coupling factor of ~0.24, which is one order of magnitude higher than those of nitride-based VCSELs. Through streak camera direct observations, the stimulated emission of the laser device exhibits an ultrafast decay of ~10 ps, and the electron hole plasma (EHP) mechanism is considered responsible for stimulated emission in the VCSELs. This work paves the way toward next-generation high performance PNC-based single-mode laser devices with reduced fabrication cost for practical application.

Green-Synthesized Silver Nanoparticles Induced Apoptotic Cell Death in MCF-7 Breast Cancer Cells by Generating Reactive Oxygen Species and Activating Caspase 3 and 9 Enzyme Activities.

Silver nanoparticles are among the most significant diagnostic and therapeutic agents in the field of nanomedicines. In the current study, the green chemistry approach was made to optimize a cost-effective synthesis protocol for silver nanoparticles from the aqueous extract of the important anticancer plant Fagonia indica. We investigated the anticancer potential and possible involvement of AgNPs in apoptosis. The biosynthesized AgNPs are stable (zeta potential, -16.3 mV) and spherical with a crystal size range from 10 to 60 nm. The MTT cell viability assay shows concentration-dependent inhibition of the growth of Michigan Cancer Foundation-7 (MCF-7) cells (IC50, 12.35 μg/mL). In addition, the fluorescent microscopic analysis shows activation of caspases 3 and 9 by AgNPs that cause morphological changes (AO/EB assay) in the cell membrane and cause nuclear condensation (DAPI assay) that eventually lead to apoptotic cell death (Annexin V/PI assay). It was also observed that AgNPs generate reactive oxygen species (ROS) that modulate oxidative stress in MCF-7 cells. This is the first study that reports the synthesis of a silver nanoparticle mediated by Fagonia indica extract and evaluation of the cellular and molecular mechanism of apoptosis.

A Complex Assemblage of Crystal Habits of Pyrite in the Volcanic Hot Springs from Kamchatka, Russia: Implications for the Mineral Signature of Life on Mars

In this study, the crystal habits of pyrite in the volcanic hot springs from Kamchatka, Russia were surveyed using scanning electron microscopy. Pyrite crystals occur either as single euhedral crystals or aggregates with a wide range of crystal sizes and morphological features. Single euhedral crystals, with their sizes ranging from ~200 nm to ~40 µm, exhibit combinations of cubic {100}, octahedral {111}, and pyritohedral {210} and {310} forms. Heterogeneous geochemical microenvironments and the bacterial activities in the long-lived hot springs have mediated the development and good preservation of the complex pyrite crystal habits: irregular, spherulitic, cubic, or octahedral crystals congregating with clay minerals, and nanocrystals attaching to the surface of larger pyrite crystals and other minerals. Spherulitic pyrite crystals are commonly covered by organic matter-rich thin films. The coexistence of various sizes and morphological features of those pyrite crystals indicates the results of secular interactions between the continuous supply of energy and nutritional elements by the hot springs and the microbial communities. We suggest that, instead of a single mineral with unique crystal habits, the continuous deposition of the same mineral with a complex set of crystal habits results from the ever-changing physicochemical conditions with contributions from microbial mediation.

New synthesis routes and catalytic applications of ferrierite crystals. Part 2: The effect of OSDA type on zeolite properties and catalysis

Tailoring of physicochemical properties of synthetic zeolites is of paramount importance when these materials are applied as heterogenous catalysts. In this work, the effect of the synthesis system and in particular of the organic structure directing agent (OSDA) on acidity, crystal morphology, and catalytic behaviour of FER-type materials is studied. FER-type zeolites with similar Si/Al ratio and crystal size range 0.3–15 μm are synthesised by changing OSDA type or by adding surfactant. A crystallization kinetic analysis shows that the stability of the zeolitic phase strongly depends on the OSDA type. In particular, the crystallization time strongly affects the purity of the FER phase when tetrahydrofuran is used as a template. Furthermore, it is found that long amines as 1,8-diaminooctane can play a role of OSDA obtaining highly crystalline FER-type crystals and with a high Lewis acid sites concentration. FT-IR and 27Al-NMR analyses show that all of the synthesised samples possess different Lewis acid sites concentration associated with extra-framework Al–OH species that are not detected by NMR analysis. Catalytic tests in methanol-to-dimethyl ether reaction reveal that synthesised samples exhibit different catalytic behaviour. In particular, large (10–15 μm) FER-type catalyst synthesised with tetrahydrofuran suffer deactivation caused by a higher carbon deposit level. On the contrary, nano-sized FER-type crystals, prepared by using pyrrolidine as OSDA and a surfactant, exhibits high selectivity and considerable resistance to coke deposition.

Residual stress effect on the fracture toughness of lithium disilicate glass‐ceramics

AbstractIn glass‐ceramics (GCs), on cooling from the crystallization temperature, internal residual stresses are generated due to the difference between the thermal expansion coefficient (TEC) of the crystal phase(s) and the residual glass. These stresses could degrade or promote their mechanical properties. In this work, we varied the magnitude of the residual stresses in lithium silicate GCs by designing their microstructures. The level of internal stresses was measured using (Synchrotron) X‐ray diffraction. The effects of anisotropy of thermal expansion, crystal shape, and intensity of the residual stresses were analyzed and compared using theoretical models. We extended the Hsueh‐Becher model to include the thermal expansion anisotropy of the orthorhombic lithium disilicate (LS2) crystals. We found that the average residual stresses within the LS2 crystals are compressive or null (−100 to ~0) and highly anisotropic. Most importantly, within the limits of this study, we found no evidence for the influence of (compressive or null) residual stresses on the fracture toughness of the studied GCs. Within the crystal size range from 1 to 5 μm, a highly crystallized volume fraction coupled to relatively large crystals (5 μm) of high elastic modulus improved the glass‐ceramic fracture toughness. This result can guide the microstructural design of novel tough GCs.

Structural Investigation of Silicon Carbide X Grains: Constraints on Condensation in Supernova Ejecta

Abstract We analyzed seven presolar SiC grains of supernova origin (average diameter: 1–2 μm) with transmission electron microscopy. Five grains are polycrystalline, whereas two grains are single crystals. Individual crystal domains of polycrystalline grains are in epitaxial relationship, with two grains consisting almost entirely of twinned crystal domains. Most grains are free of inclusions (only one TiC inclusion and one iron- and nickel-rich inclusion were found in two separate grains). Almost all crystals have cubic symmetry (3C polytype), but we found hexagonal SiC (6H polytype) in two grains. The large range of crystal domain sizes (average diameter: 50–970 nm), as well as the larger fraction of noncubic SiC polytypes in supernova grains relative to SiC grains that crystallized in the winds of asymptotic giant branch (AGB) stars, suggest that SiC condensation in supernova ejecta occurs at a larger range of chemical and physical conditions, including supersaturation, than in the winds of AGB stars. Modeling condensation of SiC struggles to produce SiC grains as large as, or bigger than, observed here, if condensation of large (i.e., several μm in diameter) graphite grains is to precede that of SiC, which is suggested by the presolar grain record and published equilibrium condensation models. We propose that future models of graphite and SiC condensation in SN ejecta explore higher ejecta densities than before, as well as gas compositions that are more silicon- and carbon-rich. Furthermore, we infer that some supernova SiC grains may have formed without prior condensation of graphite from their parent gas.

Single crystal fragmentation: Visualizing breakage model performance for pharmaceutical processes

The development of accurate crystal breakage kinetics is paramount to extending the capability of optimization and modelling methods within the pharmaceutical drug-product sector. However, there exists little experimental data on the performance on typical breakage models when applied to small-scale pharmaceutical crystals. Therefore, experimental investigations of crystal impacts on a steel target were carried out across a range of crystal sizes and impact velocities in order to determine critical breakage parameters for a given model. Direct observation of each impact was captured via a high-speed Shadowgraphy imaging technique, capable of 1μm crystal size resolution and up to a 125,000 frames-per-second capture rate. Crystals of Darunavir Ethanolate between a nominal 100→500μm size range were subject to impact velocities of 1→10m/s normal to the target surface. Furthermore, upon collision crystals were classified into one of three breakage modes: intact (Mode I), chipped (Mode II), or split/disintegrated (Mode III). The resulting data was then combined with a post-processing methodology utilizing a bi-variate histogram function and Kernel Density Estimation (KDE). This in turn enabled the extraction of experimentally observed crystal failure velocities, breakage modes, and selection functions detailing how crystal breakage varies with both crystal size and impact velocity. This data was then used to evaluate the performance of current literature in describing crystal breakage within pharmaceutical applications. Furthermore, the methodology implemented in this work can be applied to a range of particulate systems, yielding a flexible tool for pharmaceutical modelling capabilities.

Preparation of Fine-Grained Corundum Powders with Given Properties: Crystal Size and Habit Control

The processes of obtaining fine-grained corundum with a given crystal size and habit are considered. It is shown that thermocouple treatment in aqueous supercritical fluid allows one to obtain corundum from various precursors in a wide range of crystal sizes (0.01–500 μm). Powders with a crystal size in the range 20–500 μm can be obtained directly from hydrargillite prepared in the course of the Bayer Process. The size and habit of the crystals are determined by the parameters of the thermocouple treatment and properties of the process activators used. Powders with a crystal size falling in the range 30–1000 nm can be obtained by using synthesized or commercially available boehmite as a precursor for the thermocouple treatment. The crystal habit is determined by the habit of the boehmite crystals used. New methods of boehmite synthesis have been developed that allow one to obtain nonaggregated crystals with a size of 10 nm with a narrow distribution curve.