Thermal expansion of kyanite at ambient pressure:An X-ray powder diffraction study up to 1000℃

The thermal expansion coefficients of kyanite at ambient pressure have been investigated by an X-ray powder diffraction technique with temperatures up to 1000 ℃. No phase transition was observed in the experimental temperature range. Data for the unit-cell parameters and temperatures were fitted empirically resulting in the following thermal expansion coefficients： αa = 5.8（3） × 10^-5, αb = 5.8 （1）× 10^-5, αc = 5.2（1）× 10^-5, and αv = 7.4（1） × 10^-3 ℃ 1 in good agreement with a recent neutron powder diffraction study. On the other hand, the variation of the unit-cell angles α, β and γ of kyanite with increase in temperature is very complicated, and the agreement among all studies is poor. The thermal expansion data at ambient pressure reported here and the compression data at ambient temperature from the literature suggest that, for the kyanite lattice, the most and least thermally expandable directions correspond to the most and least compressible directions, respectively.

Ab initio Structure Determination of [Co(NH_3)_5Br]Br_2 Using Conventional X-ray Powder Diffraction

The crystal structure of [Co(NH3)5Br]Br2 has been determined ab initio from the conventional X-ray powder diffraction data. The approximate structure with all 7 indeyendent non-H atoms was solved by direct methods. The final orthorhombic unit-cell parameters after Rietveld refinement are: a=13.6927, b=10.7071, c=6.9400A, V=1017.47A3, F30=93(0.0075,43), M20=49, Z=4. Space group is Pnma. The structure agreement factors are: Rp=0.066,Rwp=0.090, RF=0.041, RB=0.042.

Neutron powder diffraction and high-pressure synchrotron x-ray diffraction study of tantalum nitrides

Tantalum nitride （TAN） compact with a Vickers hardness of 26 GPa is prepared by a high-pressure and high- temperature （HPHT） method. The crystal structure and atom occupations of WC-type TaN have been investigated by neutron powder diffraction, and the compressibility of WC-type TaN has been investigated by using in-situ high-pressure synchrotron x-ray diffraction. The third-order Birch-Murnaghan equation of state fitted to the x-ray diffraction pressure- volume （P-V） sets of data, collected up to 41 GPa, yields ambient pressure isothermal bulk moduli of B0 = 369（2） GPa with pressure derivatives of B~ = 4 for the WC-type TaN. The bulk modulus of WC-type TaN is not in good agreement with the previous result （Bo = 351 GPa）, which is close to the recent theoretical calculation result （Bo = 378 GPa）. An analysis of the experiment results shows that crystal structure of WC-type TaN can be viewed as alternate stacking of Ta and N layers along the c direction, and the covalent Ta-N bonds between Ta and N layers along the c axis in the crystal structure play an important role in the incompressibility and hardness of WC-type TaN.

Rietveld Refinement and X-ray Powder Diffraction Data of GdAlSi

The X-ray powder diffraction data of the compound GdAlSi was studied by means of X-ray diffraction technique and refined by Rietveld method. The compound GdAlSi has tetragonal α-ThSi_2-type structure, space group I4_1/amd (No.141), Z=4, the lattice parameters a=041234 (1) nm, c=1.44202(1) nm. The Smith and Snyder figure of merit [5] F_N is F_ 30=2521(36). The R-factors of Rietveld refinement are R_p=0.098 and R_ wp=0.128. The X-ray powder diffraction data are given. The field dependence of the magnetization measured at room temperature and the temperature variation of the inverse magnetic susceptibility of the compound GdAlSi were also presented.

X-ray Powder Diffraction Data and Rietveld Refinement for NdCoGe_3

オ-ray powder diffraction data and crystal structure of RE compound NdCoGe3 were studied by using X-ray powder diffraction and refined by the Rietveld profile fitting method. The compound has the tetragonal BaNiSn3type structure, space group I4mm (No.107) a=0.42961(2) nm, c=098147(4) nm, V=0.018114 nm3, Z=2 and Dx=7.717 g·cm-3. The figure of merit FN for the powder data is F30=623 (0.0107, 45). Structure refinement was performed with 110 reflections and led to Rp=11.78% and Rwp=16.56%.

X-ray Powder Diffraction Pattern of Bi_4(SiO_4)_3

In cooperation with figure-of-merits the Rietveld analysis can appraise both angular and intensity data of powder diffraction. In this work, X-ray diffraction pattern of Bi4(SiO4)3 was redetermined with intensity figure-of-merits, which qualify agreement between observed and calculated relative intensities. F30 is 158.90 (0.0059, 32), intensity figure of merit Rint is 8.7, I20(17), 8.0. The values of figure-of-merits show that the data of JCPDS cards are distorted. Both the experimental and calculated peak positions and heights are listed in detail.

IDENTIFICATION AND SIMULATION OF X-RAY POWDER DIFFRACTION PATTERN

A new method for pattern identification and simulation of X-ray powder diffraction data is described, which can give definite phase composition of the unknown rapidly and correctly. The method is implemented in Microsoft Fortran 77 for the IBM PC/XT/AT personal computer or their compatibles.

MY RESEARCH ACHIEVEMENTS IN POWDER X-RAY DIFFRACTION & PHASE DIAGRAMS

I graduated from the Department of Chemistry, Xiamen University in 1955, majoring in physical chemistry. I went to the Institute of Metallurgy under the Soviet Academy of Sciences in 1956 as a Ph.D.candidate in thermochemistry and crystal chemistry of metal alloys,and got my Ph.D.degree in 1960.In the following 30 years, I did basic and applied research in interdisciplines,including crystal chemistry,materials science and solid state physics.My main achievements can be listed in two aspects as follows:

X-Ray and Neutron Diffraction Studies on Thermal Parameters of Thalous Bromide

Thermal parameters of TIBr were determined using both X-ray and neutron diffraction techniques. The data was analysed by Rietveld profile refinement procedure. From the neutron diffraction data, due to weak odd-order reflections, it was not possible to determine the individual thermal parameters. TheX-ray diffraction measurements yielded BT1=0.296(5) nm2 and BBr=0.162(5) nm2. The overall isotropic value, B was 0.252(7) nm2 which is in good agreement with B=0.230(8) nm2 obtained from present neutron diffraction measurements. The present values are also in good agreement with theoretical estimates obtained from the shell models.

Crystallographic Characteristic of Intermetallic Compounds in Al-Si-Mg Casting Alloys Using Electron Backscatter Diffraction

The Al-Si-Mg alloy which can be strengthened by heat treatment is widely applied to the key components of aerospace and aeronautics. Iron-rich intermetallic compounds are well known to be strongly influential on mechanical properties in Al-Si-Mg alloys. But intermetallic compounds in cast Al-Si-Mg alloy intermetallics are often misidentified in previous metallurgical studies. It was described as many different compounds, such as AlFeSi, Al8Fe2Si, Al5（Fe, Mn）3Si2 and so on. For the purpose of solving this problem, the intermetallic compounds in cast Al-Si alloys containing 0.5% Mg were investigated in this study. The iron-rich compounds in Al-Si-Mg casting alloys were characterized by optical microscope（OM）, scanning electron microscope（SEM）, energy dispersive X-ray spectrometer（EDS）, electron backscatter diffraction（EBSD） and X-ray powder diffraction（XRD）. The electron backscatter diffraction patterns were used to assess the crystallographic characteristics of intermetallic compounds. The compound which contains Fe/Mg-rich particles with coarse morphologies was Al8FeMg3Si6 in the alloy by using EBSD. The compound belongs to hexagonal system, space group P6_2m, with the lattice parameter a=0.662 nm, c=0.792 nm. The β-phase is indexed as tetragonal Al3FeSi2, space group I4/mcm, a=0.607 nm and c=0.950 nm. The XRD data indicate that Al8FeMg3Si6 and Al3FeSi2 are present in the microstructure of Al-7Si-Mg alloy, which confirms the identification result of EBSD. The present study identified the iron-rich compound in Al-Si-Mg alloy, which provides a reliable method to identify the intermetallic compounds in short time in Al-Si-Mg alloy. Study results are helpful for identification of complex compounds in alloys.

SYNTHESIS AND X-RAY POWDER STUDY OF A NEW COMPOUND:Ba_6Ti_7Nb_9O_(42)

A new compound Ba6Ti7Nb9O42 was prepared for the first time by solid state reaction in BaO-TiO2-Nb2O5, ternary system. The X-ray powder diffraction data of the title compound was determined. Ba6Ti7Nb9O42 crystallizes in the hexagonal system -with unit cell parameters a=9.0527(4) A,c=11.790(1) A,and space group P63/mcm(193),z=1. The calculated and measured densities are 5. 293 g/cm3 and 5.285 g/cm3, respectively.

Quantification of flupirtine maleate polymorphs using X-ray powder diffraction

Flupirtine maleate, a pharmaceutical compound for treating psychotic disease in clinics, has seven polymorphs. Form A, with better crystal stability and bioavailability, has been widely used as the pharmaceutical crystal form. Unfortunately, it is usually found in a polymorphic mixture with form B. In this study, pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction （XRPD）, Fourier transform infrared spectroscopy （FT-IR） and thermal analysis. An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters. The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0- 100% （w/w）, good linear relationship, with R2= 0.999, excellent repeatability and precision and low limits of detection （LoD） of 0.15% （w/w） and quantification （LoQ） of 0.5% （w/w）. The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation, but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good, repeatable, sensitive, and accurate method. This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs （forms A and B） quantitatively and control the quality of the bulk drug.

The determination of the crystal struoure of tetra-potassium uranyl tricarbonate by powder X-ray diffraction method

A uranyl compound, K_4UO_2(CO_3)_3 has been characterized by powder X-ray diffraction method. M. W.=606.46, monoclinic, C2/c (No. 15), a=1.0240(7), b=0.9198(4), c=1.2222(12)nm, β=95.12(4)°,V=1.1466(5)nm^3, Z=4, D_m=3.468g/cm^3, D_c=3.513g/cm~, λ(Cu Kα_1)=O.1540598nm, T=298K. The structure was solved by heavy atom method and Fourier synthesis, and refined by full- matrix least-squares method to R=0.1185 for 275 reflections. The uranium (Ⅵ) atom is in an eight-coordinate distorted hexagonal-bipyramidal environment with creasy fan shape. The linear uranyl group approaches to perpendicular to the equatorial plane in which three carbonate groups are chelated. U(Ⅵ) has two linear oxygen atoms closer to it (U-O=0.1767 (5) nm) than six other neighbours (U-O ranging from 0.2516 to 0.2568nm). The distances between carbon atoms and uncoordinated oxygen atoms are 0.122 (1) and 0.123(1) nm, which are distinctly different from those between carbon and coordinated oxygen atoms (mean 0.134(6) nm). This fact reveals the non-eq- uivalence of one oxygen atom to the other two in each carbonate. In K_4UO_2(CO_3)_3, the O-O dis- tance for the adjacent carbonate groups is 0.2794(4)nm approaching to the sum of Van der Waals radii of two oxygen atoms. The K-O distances vary between 0.2667 and 0.3131nm, and each anion is immediately surrounded by six potassium ions, only four of which can be considered to belong to the same structural formula unit, and they are symmetrically located above and below the equatorial plane.

Silicon assistant carbothermal reduction for SiC powders

The silicon assistant method to increase the reaction yield of carbothermal reduction of silica at a lower temperature is reported. The effect of silicon on the carbothermal reduction process has been investigated in detail. Compared with traditional reduction, the introduction of silicon can change the reaction path and further increase the conversion of silicon carbide at a lower temperature. It is considered that the assistant reduction consists of three steps： vaporizing and melting of silicon, formation of silicon monoxide, and synthesis of silicon carbide. The morphology of the synthesized SiC powders through the silicon assistant method can be affected apparently by the experimental temperature.

Characteristics of mechanical alloyed Ni-Al powder for sintering

Mechanical alloying was employed to obtain high-activity Ni-AI powder. The effects of mechanical alloying on the microstructure and characteristics of milled powder with a normal composition of Ni-22.89 at.% AI-0.5 at.% B were investigated by X-ray diffraction （XRD）, scanning electron microscopy （SEM）, and transmission electron microscopy （TEM）. The results show that a solution Ni （AI） was obtained after milling. During mechanical alloying, the milled powder obtains extra surface energy and crystalline energy because the crystallite size becomes free and the lattice strain increases with the milling time prolonging. Furthermore, about 0.5 mol% oxide in the particles were formed after milling, and this kind of dis- persed oxide is effective to improve the properties of the sintered alloy by dispersion strengthening. It is confirmed that Ni3AI alloy with outstanding properties has been prepared with mechanical alloyed powders.

Microstructural origins of high strength of Al-Si alloy manufactured by laser powder bed fusion:In-situ synchrotron radiation X-ray diffraction approach

The microstructural factors contributing to the high strength of additive-manufactured Al-Si alloys us-ing laser-beam powder bed fusion(PBF-LB)were identified by in-situ synchrotron X-ray diffraction in tensile deformation and transmission electron microscopy.PBF-LB and heat treatment were employed to manufacture Al-12%Si binary alloy specimens with different microstructures.At an early stage of de-formation prior to macroscopic yielding,stress was dominantly partitioned into the α-Al matrix,rather than the Si phase in all specimens.Highly concentrated Si solute(~3%)in the α-Al matrix promoted the dynamic precipitation of nanoscale Si phase during loading,thereby increasing the yield strength.After macroscopic yielding,the partitioned stress in the Si phase monotonically increased in the strain-hardening regime with an increase in the dislocation density in the α-Al matrix.At a later stage of strain hardening,the flow curves of the partitioned stress in the Si phase yielded stress relaxation owing to plastic deformation.Therefore,Si-phase particles localized along the cell walls in the cellular-solidified microstructure play a significant role in dislocation obstacles for strain hardening.Compared with the results of the heat-treated specimens with different microstructural factors,the dominant strengthening factors of PBF-LB manufactured Al-Si alloys were discussed.

Reactivity of Recycled Glass Powder in a Cementitious Medium

The reactivity of the recycled glass powder (GP) in a cementitious medium has been studied over time by means of X-ray diffraction and thermal gravimetric analysis. Two different mixtures based on cement/glass powder (0 or 20 wt% GP) and lime/glass powder (70 wt% GP) were considered. Analysis revealed the coexistence of both hydration and pozzolanic reaction during the hardening of the mortars. At young age, the cement hydration would prevail over the pozzolanic one resulting in a decrease of physico-chemical and mechanical properties of the material due to the dilution effect. The pozzolanic reaction that predominates from 91 days, would induce the formation of supplementary C-S-H leading to improve the material properties.

PREPARATION OF ULTRAFINE ALLOY POWDER BY REDUCTION OF COMPLEX OXIDE

The ultrafine alloy powders,CuRh,γ-Ni_(0.33)Fe_(0.66) and α-Fe_(0.66)Co_(0.33) of size less than 35 nm were prepared by reduction of complex metallic oxides under atmosphere of 15% H_2 and 85%Ar.

Thermal expansion of lattice parameter of (powder) silicon up to 1473 K

The XRPD (X-ray powder diffxactometry) patterns of silicon powder with a unit cell structure of diamond were determined from 298 to 1473 K. Lattice parameters of Si linearly increase with temperature. The thermal shifts of the positions of all reflection peaks are linearly correlated with the temperature. The coefficients of the intrinsic linear thermal expansion and volumetric thermal expansion were determined as 3.87×10-6/K and 1.16×10-5/K respectively. It indicates that Si is still a suitable standard in the XRPD method at high temperatures.

X-RAY RIETVELD STRUCTURE REFINEMENT OF ErNiSb

The crystal structure of compound ErNiSb has been refined by the Rietveld wholepatternfitting method from X-ray powder diffraction data.The compound ErNiSb is cubic, space group F43m and the structure parameters and reliability factors were refined to be a=6.268 3(1), V=246.29^(3), Z=4, D_(x)=9.377 g/cm^3, R_(B)=3.57%, R_(F)=3.64%, R_(p)=6.63%, R_(WP)=8.80%.