ZnSe-based heterostructures grown on GaAs substrates have been investigated for use in pin-diode LED applications. In this study, a conventional Bragg-Brentano diffractometer (BBD) has been used to screen samples for phase identification, crystallite size, presence of polycrystalline ZnSe, and initial rocking curve (RC) analysis. A limitation of the conventional diffractometer is that the smallest RC full width at half maximum (FWHM) that can be achieved is 500 to 600 arc sec. As deposition parameters are optimized and the RC limit of the conventional diffractometer is reached, analysis is moved to a four-bounce high-resolution diffractometer (HRD). Although more time for analysis is required, using the HRD has a RC resolution advantage, where RCs of <20 arc sec are obtained for neat GaAs wafers. Combining the BBD and HRD instruments for analysis of ZnSe films grown on GaAs substrates allows for an efficient means of high sample throughput combined with an accurate measurement of film alignment.

X-ray powder diffraction (XRD) is utilized for the determination of polymorphism in crystalline organic materials. Though convenient to use in a laboratory setting, XRD is not easily adapted to in situ monitoring of synthetic chemical production applications or thin film depositions. Near-infrared spectroscopy (NIR) can be adapted to in situ manufacturing schemes by use of a source/detector probe. Conversely, NIR is unable to conclusively define the existence of polymorphism in crystalline materials. By combining the two techniques, a novel simultaneous NIR/XRD instrument has been developed. During material’s analysis, results from XRD allowed for the determination of the existence of polymorphic phases, and NIR data were collected as a fingerprint for each of the observed polymorphs. These NIR fingerprints allowed for the development of a library, which can be referenced during the use of a NIR probe in manufacturing settings. The NIR/XRD instrument was also used to monitor materials during exposure to ambient air. XRD can detect crystalline phase changes and NIR can monitor solvent loss and/or water uptake.

Six A-type zeolites: NaA, MnNaA, CoNaA, NiNaA, ZnNaA, CdNaA have been characterized by X-ray powder diffraction. The zeolites with selected divalent cations have been synthesized by a very careful ion-exchange process using very high quality NaA zeolite. Experimental 2θ peak positions, relative peak intensities, values of d and Miller indices as well as a unit cell parameter are reported.

A new ternary compound Dy5Co6Sn18 was synthesized and studied. The crystal structure of Dy5Co6Sn18 was determined using the Rietveld refinement method. The compound was found to crystallize in tetragonal space group I41/acd, Tb5Rh6Sn18-type structure, with a=13.5598(3) Å, c=7.1470(5) Å, Z=8, and Dcalc=8.789 g/cm3. Measurements of magnetic susceptibility and electrical resistivity on polycrystalline samples were also performed. The Curie–Weiss law was followed, with θp=−15.7 K and μeff=10.61μB. Dy5Co6Sn18 is a spin-glass with a freezing temperature of 6.5 K.

Nanostructuring is one of the effective approaches to lower the thermal conductivity of thermoelectric materials for improving its figure of merit. The nano-sized uniform skutterudite Co1−xNixSb3 (x = 0, 0.05, 0.075, 0.125, 0.15, and 0.25) thermoelectric powders were synthesized in triethylene glycol solution by using CoCl2, NiCl2, and SbCl3 as precursors and NaBH4 as the reductant. Different synthesis conditions were studied to pursue pure and uniform skutterudite CoSb3 powders. The powders were characterized by X-ray diffraction, field emission scanning electron microscope, and energy-dispersive X-ray analysis. Experimental results show that a Ni-doped skutterudite Co1−xNixSb3 single phase was obtained at 290 °C for 12 h. The powders are spherical, small, and uniform. As x increases from 0 to 0.25, the unit-cell parameter a increases from 0.9044 to 0.9065 nm and the particle size increases from 10 to 30 nm.

Variation of structural parameters of dimethylammonium manganese formate [(CH3)2NH2]Mn[(HCOO)3] upon substitution by the transition elements Zn, Co, and Ni is studied by powder X-ray diffraction (PXRD) technique. These metal–organic framework (MOF) crystals were grown by solvothermal method. The PXRD patterns of all MOFs exhibited rhombohedral structure. PXRD patterns of MOFs were analyzed using Rietveld refinement method. While the parent Mn-MOF and Mn0.9Zn0.1MOF are found to have similar structural parameters, Co and Ni substituted Mn-MOFs have smaller structural parameters than that of parent Mn-MOF. The reason for this variation in the lattice parameters is explained based on the Shannon ionic radii.

This paper aims to explore the influence of solvent effects on the crystal habit of venlafaxine hydrochloride using the modified attachment energy (MAE) model by molecular dynamics (MD) simulation. Solvent effects were investigated based on the different morphologies of venlafaxine hydrochloride acquired by simulation and experimental technology from the solvents of isopropanol, dimethyl sulfoxide, and acetonitrile. Firstly, morphologically dominant crystal faces were obtained through the prediction of crystal habit in vacuum by the attachment energy (AE) model. Subsequently, the MAEs were calculated by the MD simulation to modify the crystal shapes in a real solvent environment, and the simulation results were in agreement with the experimental ones. Meanwhile, in order to have a better understanding of the solvent effects, the surface structure was introduced to analyze the solvent adsorption behaviors. The results show that the crystal habits of venlafaxine hydrochloride are affected by the combination of the AE and surface structures. Finally, the flowability of the obtained crystal powders from different solvents was investigated by measurement and analysis of the angle of repose and compressibility. The above results verify that the physical properties are closely related to the morphologies of the crystals.

The crystal structure of bumetanide has been solved and refined using synchrotron X-ray powder diffraction data, and optimized using density functional techniques. Bumetanide crystallizes in space group P-1 (#2) with a = 5.00168(4), b = 9.22649(3), c = 19.59924(14) Å, α = 80.7941(5), β = 82.8401(7), γ = 86.8148(7)°, V = 885.268(9) Å3, and Z = 2. The crystal structure is layered with the double layers parallel to the ab plane. The exterior of the layer is composed of hydrocarbon portions of the molecule, both phenyl rings and butyl side chains. The central portion of the bilayer contains the hydrogen-bonding regions, both the carboxylic acid dimers and the hydrogen bonds involving the sulfonamide groups. The molecular conformations of bumetanide in this current triclinic structure and the previously-determined monoclinic polymorph FEDGON are very similar, as are the energies of the two polymorphs. The powder pattern is included in the Powder Diffraction File™ as entry 00-066-1609.

X-ray powder diffraction data, unit-cell parameters, and space group for deoxyschisandrin, C24H32O6, are reported [a = 13.083(3) Å, b = 19.563(9) Å, c = 8.805(6) Å, β = 90.472(0)°, unit-cell volume V = 2253.82 Å3, Z = 4, and space group P21]. All measured lines were indexed and are consistent with the P21 space group. No detectable impurity was observed.

The crystal structure of pazopanib hydrochloride Form 1 has been refined using synchrotron X-ray powder diffraction data and optimized using density functional theory techniques. Pazopanib hydrochloride crystallizes in space group P-1 (#2) with a = 8.45008(6), b = 8.71310(12), c = 16.05489(35) Å, α = 79.5996(9), β = 86.4784(5), γ = 87.3764(3)°, V = 1159.724(9) Å3, and Z = 2. The crystal structure is essentially identical to that of CSD Refcode CEVYEK. There are four strong N–H⋯Cl hydrogen bonds to the chloride anion. Several additional weaker N–H⋯Cl and C–H⋯Cl hydrogen bonds are also present. A variety of C–H⋯O, C–H⋯N, and N–H⋯S hydrogen bonds also contribute to the lattice energy. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™.

Nitinol is a shape memory alloy based on the inter-atomic compound having a composition of 50  at% each of Ni and Ti, NiTi. The shape memory effect results from a reversible martensitic phase transformation. An increasing solubility range with temperature on the Ni-rich side can produce a precipitation reaction resulting in a slight matrix composition adjustment with appropriate heat treatment. Electrolytic phase extraction (Andrews and Hughes, 1957) is used to evaluate the secondary phases in the alloy and Ti2Ni and TiC are positively identified using powder wide-angle X-ray diffraction procedures. Two samples of an Ni-rich alloy at 57 and 60 at% are also analyzed. These Ni-rich samples show Ti2Ni and an additional phase, Ni3Ti.

The stereoselective synthesis of 7-fluoro-2-exo-(2-methylpropen-1-yl)-2,3,4,5-tetrahydro-1,4-epoxybenzo[b]azepine was developed by intramolecular 1,3-dipolar cycloaddition of the nitrone derived from the corresponding 2-allyl-4-fluoro-N-(3-methylbut-2-enyl)aniline. The X-ray powder diffraction (XRPD) pattern for the new compound was analyzed and found to crystallize in a monoclinic system with space group P21/m (No. 11) and refined unit-cell parameters a = 11.655(5) Å, b = 5.850(2) Å, c = 18.314(4) Å, β = 104.27(3) and V = 1210.1 (6) Å3.

A clear understanding of the solid-state reaction of kaolinite (Kln), quartz (Qtz), and sodium carbonate (Na2CO3) is of great significance for the process optimization of coal gangue calcined with Na2CO3. In this work, a comparative study of the isothermal solid-state reaction systems of Kln–Na2CO3 and Kln–Qtz–Na2CO3 was performed by means of X-ray diffraction (XRD), scanning electron microscope, and energy dispersion spectroscopy (SEM-EDS). The results showed that the calcined products both for these reaction systems mainly contain different kinds of sodium aluminum silicates (e.g., NaAlSiO4, Na1.55Al1.55Si0.45O4, and Na1.95Al1.95Si0.05O4) and various kinds of sodium silicates (e.g., Na2Si3O7, Na2SiO3, and Na6Si2O7). The mass percentage of Na2CO3 played a key role in the phase transformation, determining the Na/Al/Si molar ratio of the formed sodium aluminum silicates. Compared with the reaction system of Kln–Na2CO3, the existence of Qtz inhibited the formation of sodium aluminum silicates in the reaction system of Kln–Qtz–Na2CO3. It should be noted that the formed phases both for these reaction systems were slightly different from that of the thermodynamical calculated results of Na2O–SiO2–Al2O3 using FactSage™ software. According to both the experimental and calculated results, a reasonable batching area for coal gangue activation was proposed that the addition of Na2CO3 should be in the range of 20–50% of the total mass of Kln, Qtz, and Na2CO3.

The ferroic phase transition in LaEr(MoO4)3 has been analyzed for the first time. It has been confirmed that this compound undergoes a phase transition from a tetragonal system (paraelectric-paraelastic phase), with space group P-421 m [β-Gd2(MoO4)3 averaged phase] to an orthorhombic system (ferroelectric-ferroelastic phase), with space group Pba2 [β'-Gd2(MoO4)3 phase] in a reversible process. This phenomenon, together with the observed demixing at high temperature has been studied using different techniques. LaEr(MoO4)3 samples have been obtained by the conventional solid-state synthesis. The thermal dependence of the crystal structure was studied by powder X-ray and neutron diffraction, following a new refining procedure in which the symmetry modes of atomic displacements from the paraelectric-paraelastic structure were analyzed. Dielectric spectroscopy measurements have confirmed the structural results, showing a very smooth phase transition. Finally, calculations within the framework of Density Functional Theory show a behavior of the lattice parameters similar to that observed in our experiments.

In present investigation, effect of modulation and machining parameters on deformation level of the chips produced during modulation assisted machining (MAM) has been studied. It is shown that disruption in tool-chip contact during modulation assisted machining helps in the formation of discrete chips. Size and shape of the particles produced in MAM can be controlled by varying modulation and machining conditions. Particulates of different shapes and sizes ranging from 100 µm to 5 mm with an aspect ratio of ~10 were produced using MAM. The morphology of the particulates produced was characterized by scanning electron microscope (SEM). Deformation in chip particulates was investigated using X-Ray diffraction. The crystallite size and internal strain in particulates were evaluated using Scherrer and Williamson-Hall methods respectively. The crystallite size of the particulates was found to decrease with decrease in their size, whereas internal strain in particulates was observed to increase with decrease in their size. Furthermore, the length of particulates was observed to decrease with an increase in the ratio of frequency of modulation (fm) to frequency of workpiece rotation (fw). However, the corresponding change in microstrain and crystallite size was insignificant with change in this ratio.

The effect of Dy3+ doping at A-site in hexagonal YMnO3 on the microstructure and magnetic properties was studied. Polycrystalline Y1−xDyxMnO3 samples with x ranging from 0 to 1 were synthesized by the solid-state reaction method. The microstructures of all the samples were studied by X-ray diffraction, which shows that Y1−xDyxMnO3 with a low concentration (x ≤ 0.5) of Dy3+ retains a hexagonal symmetry. The crystal structure refinements of the hexagonal Y1−xDyxMnO3 using the Rietveld method show that the unit-cell parameters of a, c, and unit-cell volume increase with increasing Dy doping, while the MnO5 trigonal bipyramids remain almost unchanged. The remarkable increasing of magnetic moment at a low temperature with increasing the Dy3+ doping concentration is ascribed to the spin order of Dy3+ and the increasing Dy3+–Mn3+ coupling and Mn3+–O–O–Mn3+ interaction.

The crystal structure of K2Zn(PO3)4 was determined and refined using the Rietveld method based on the isostructure model of K2Cu(PO3)4. This compound belongs to the monoclinic system with space group Cc and lattice parameters of a=11.0941(2) Å, b=12.5215(3) Å, c=7.6597(2) Å, and β=102.47(2)°. The chemical formula unit per unit cell is Z=4 and the calculated density is 2.938(3) g∕cm3. Zigzag [PO3]∞ chains formed along the a axis, and their period contains eight PO4 tetrahedrons.

Diffraction patterns were recorded, and unit cell dimensions refined by the least-squares method, for lactitol and lactitol monohydrate. Refined unit cell parameters for lactitol are: a =7.622(1) Å, b = 10.764(2) Å, c = 9.375(1) Å, β= 108.25(1)° in space group P21, and those for lactitol monohydrate a =7.844(1) Å, b = 12.673(2) Å, c = 15.942(2) Å in space group P212121.