THE DEGREE OF CRYSTALLINITY OF MULTICOMPONENT POLYMERS BY X-RAY DIFFRACTION ANALYSIS

Based on the X-ray scattering intensity theory,the correction factors of the degree of crystallinity formulae of the multicomponent polymers have been clearly defined.The formula of degree of erystallinity of the multicomponent polymers was derived in terms of the WAXD theory ahd improved graphic multipeak resolution methods.The results calculated are compatible with the density measurement.

Investigation of Changes in the Fine Structure of Graphitizing Carbon Materials during Heat Treatment by X-Ray Diffraction Analysis

The properties of synthetic graphite materials, widely used in advanced fields, are determined by their structure, which is formed in the process of high-temperature (~2500°C) heat treatment. The fine structure of a graphitizing carbon material based on petroleum coke containing 1.3 wt% S at various stages of graphitization was studied by X-ray diffraction analysis. Some of the samples contained the addition of dispersed Fe2O3. It is shown that the heat-treated material in the range 1200°C - 2600°C is heterogeneous, its component composition is determined by the processing temperature and the presence of Fe2O3 additive. The observed dependence of the component composition on the heat treatment temperature suggests that the process of graphitization of the carbon material, apparently, develops through a number of metastable states.

X-ray diffraction analysis of cold-worked Cu-Ni-Si and Cu-Ni-Si-Cr alloys by Rietveld method

Cold worked and annealed supersaturated Cu-2.65Ni-0.6Si and Cu-2.35Ni-0.6Si-0.6Cr alloys were studied. The microstructural parameters evolution, including crystallite size, root mean square strain and dislocation density was analyzed using Materials Analysis Using Diffraction software （MAUD）. The parameters for both alloys have typical values of cold deformed and subsequently annealed copper based alloy. A net change of the crystallite size, root mean square strain and dislocation density values of the alloys aged at 450 °C for 2.5-3 h seems corresponding to the recovery and recrystallization processes. Addition of Cr as quaternary element did not lead to any drastic changes of post deformation or ageing microstructural parameters and hence of recovery-recrystallization kinetics.

Operando X-ray diffraction analysis of the degradation mechanisms of a spinel LiMn2O4 cathode in different voltage windows

The understanding of reaction mechanisms of electrode materials is of significant importance for the development of advanced batteries.The LiMn2O4 cathode has a voltage plateau around 2.8 V(vs.Li^+/Li),which can provide an additional capacity for Li storage,but it suffers from a severe capacity degradation.In this study,operando X-ray diffraction is carried out to investigate the structural evolutions and degradation mechanisms of LiMn2O4 in different voltage ranges.In the range of 3.0-4.3 V(vs.Li^+/Li),the LiMn2O4 cathode exhibits a low capacity but good cycling stability with cycles up to 100 cycles and the charge/discharge processes are associated with the reversible extraction/insertion of Li^+from/into LixMn2O4(0≤x≤1).In the range of 1.4-4.4 V(vs.Li^+/Li),a capacity higher than 200 mAh/g is achieved,but it rapidly decays during the cycling.The voltage plateau around 2.8 V(vs.Li^+/Li)is related to the transformation of the cubic LiMn2O4 phase to the tetragonal Li2Mn2O4 phase,which leads to the formation of cracks as well as the performance degradation.

Preparation, crystallization and preliminary X-ray diffraction analysis of PH1948, predicted RNA methyltransferase from Pyrococcus horikoshii

RNA methyltransferase is responsible for transferring methyl and resulting in methylation on the bases or ribose ring of RNA, which existed widely but mostly remains an open question. A recombinant protein PH1948 predicting RNA methyl- transferase from Pyrococcus horikoshii OT3 has been crystallized. The crystals of selenomethionyl PH1948 belong to space group C2, with unit-cell parameters a=207.0 ?, b=43.1 ?, c=118.2 ?, β=92.1°, and diffract X-rays to 2.2 ? resolution. The VM value was determined to be 2.8 ?3/Da, indicating the presence of four protein molecules in the asymmetric unit.

Application of methods of X-ray diffraction analysis and acoustic emission on research of plastic deformation in steels

Results of researches on plastic deformation of steels were obtained by acoustic emission and X-ray methods.The new numerical-analytical method of the thin structure parameter determination on one diffraction line was offered.It is supposed that with a growth of the deformation the cubic lattice will be transformed in the orthorhombic lattice.It is shown that changes of a condition of crystal structure of austenitic steel occur in four stages and of carbonaceous steel occur in six stages.Existence of two types of acoustic emission sources in carbonaceous steel and one type of acoustic emission source in austenitic steel was proposed.

Evaluation method of coal rank based on X-ray diffraction analysis an example from SE Qinshui Basin

Based on analysis on X-ray diffraction, the metamorphic grade of coal in southeast Qinshui Basin was discussed, and a precise evaluation of coal rank through XRD analysis was made, in addition, the correlation of coal rank and vitrinite reflectance （Ro） was compared. XRD spectra of coal shows （002）-band and γ-band, and based on fitting calculation and multi-peak separation methods, the values of 2θ002 and 2θγ can be obtained, as well as corresponding intensities I002 and Iγ, consequently the coal rank can be quantized as the ratio of I002 and Iγ, that is coal rank=I002/Iγ. The research shows that the values of θ002 and θγ increase with the metamorphic grade, and a very good linear positive correlation exists between calculated Coal Rank and Ro.

Getting and X-Ray Diffraction Analysis of the Uranium Catalyst SAPO-U, Nd, Sb, Bi on the Basis of Natural Zeolite Deposits Chankanayskoe

To study the physical and chemical properties of uranium catalyst by impregnation and calcination us was first obtained uranium catalyst SAPO-U, Nd, Sb, Bi. The method of X-ray structure has been studied of the uranium catalyst SAPO-U, Nd, Sb, Bi.

Getting and X-ray Diffraction Analysis of the Microsphere Catalyst U, Nd on the Basis Fly Ash of Thermal Power Plants

To study the physical and chemical properties of aluminosilicate microsphere catalyst by impregnation and calcination us was first obtained aluminosilicate microsphere catalyst U, Nd for petrochemical processes. The method of X-ray structure has been studied for the microsphere catalyst U, Nd.

Purification, Crystallization and Preliminary X-Ray Diffraction Analysis of Exodeoxyribonuclease III from Crenarchaeon <i>Sulfolobus tokodaii</i>Strain 7

Exodeoxyribonuclease III (EXOIII) acts as a 3’→5’ exonuclease and is homologous to purinic/apyrimidinic (AP) endonuclease (APE), which plays an important role in the base excision repair pathway. To structurally investigate the reaction and substrate recognition mechanisms of EXOIII, a crystallographic study of EXOIII from Sulfolobus tokodaii strain 7 was carried out. The purified enzyme was crystallized by using the hanging-drop vapor-diffusion method. The crystals belonged to space group C2, with unit-cell parameters a = 154.2, b = 47.7, c = 92.4 ?, β = 125.8° and diffracted to 1.5 ? resolution.

Leaching behavior of phosphorous compounds from sewage sludge ash based on quantitative X-ray diffraction analysis

Phosphorus(P)is an essential and limited resource.Incineration sewage sludge ash(ISSA)contains a high amount of P,which can be recovered using chemical leaching methods.However,the recovery ratio depends on the speciation of P and the leaching conditions.In this study,hydrochloric acid was used as a leaching agent,and the effects of the hydrochloric acid concentration,leaching time,temperature,and liquid-solid ratio on the P leaching ratio were investigated.Furthermore,the co-leaching of macro-metals Ca,Al,Fe,and Mg was analyzed.The results showed that P leached rapidly within 30 min,where the leaching rate reached more than 80%and then gradually stabilized.The leaching concentrations of Ca and Mg had a significant correlation(correlation coefficient r^(2)>0.90),and both were leached completely.Al and P had similar leaching patterns,where the leaching rates increased initially and then decreased with time at 0.2 mol/L HCl.According to X-ray diffraction analysis and Rietveld refinement,the P in ISSA was mainly present in the forms of Mg_(3)Ca_(3)(PO_(4))_(4) and AlPO_(4).When leached using 0.2 mol/L HCl at 55℃ with a liquid-to-solid ratio of 20 L/kg,the AlPO_(4) and Fe_(3)(H_(2)O)_(3)(PO_(4))_(2) in ISSA dissolved initially and then precipitated on the surface of the solid phase,thereby impeding further P leaching.

In situ analysis of multi-twin morphology and growth using synchrotron polychromatic X-ray microdiffraction

Synchrotron polychromatic X-ray microdiffraction（micro-XRD） was applied to study in situ deformation twinning of commercially AZ31（Mg-3Al-1Zn） strip subjected to uniaxial tension.The morphology and growth of twins were analyzed in situ under the load level from 64 to 73 MPa.The X-ray microdiffraction data,collected on beamline 12.3.2 at the Advanced Light Source,were then used to map an area of 396μm x 200μm within the region of interest.The experimental set-up and X-ray diffraction microscopy with a depth resolution allow the position and orientation of each illuminated grain to be determined at the submicron size.A list of parent grains sorted by crystallographic orientation were selected to examine their twinning behavior.The results depict twin variant selection,local misorientation fluctuation and mosaic spread for multi-twins within the same parent grain.As load increases,the amplitude of misorientation fluctuation along twin trace keeps increasing.This is attributable to the accumulation of geometrically necessary dislocations.

MULTI-PEAK MATCH INTENSITY RATIO METHOD OF QUANTI-TATIVE X-RAY DIFFRACTION PHASE ANALYSIS

A new method for quantitative phase analysis is proposed by using X-ray diffraction multi-peak match intensity ratio. This method can obtain the multi-peak match intensity ratio among each phase in the mixture sample by using all diffraction peak data in the mixture sample X-ray diffraction spectrum and combining the relative intensity distribution data of each phase standard peak in JCPDS card to carry on the least square method regression analysis. It is benefit to improve the precision of quantitative phase analysis that the given single line ratio which is usually adopted is taken the place of the multi-peak match intensity ratio and is used in X-ray diffraction quantitative phase analysis of the mixture sample. By analyzing four-group mixture sample, adopting multi-peak match intensity ratio and X-ray diffraction quantitative phase analysis principle of combining the adiabatic and matrix flushing method, it is tested that the experimental results are identical with theory.

Analysis of surface orange peel of aluminum-alloy automobile sheet by using of EBSD and X-ray diffraction

The formation cause of orange peel of aluminum-alloy automotive sheet after tensile deformation was analysed by using X-ray diffraction and electron back-scattered diffraction(EBSD).The test results showed that formation cause of surface orange peel after tensile deformation related to product texture and nonuniform deformation during the tensile process.The grain size has significant effect on deformation uniform and texture formation.Coarse grains were easy to produce nonuniform deformation and texture,which would produce surface orange peel after tensile deformation.

In situ X-ray diffraction and thermal analysis of LiNi0.8Co0.15Al0.05O2 synthesized via co-precipitation method

LiNi0.9Co0.15Al0.05O2 （NCA） material is successfully synthesized with a modified co-precipitation method,in which NH3,H2O and EDTA are used as two chelating agents. The obtained LiNi0.9Co0.15Al0.05O2 materialhas well-defined layered structure and uniform element distribution, which reveals an enhanced electro-chemical performance with a capacity retention of 97.9% after 100 cycles at 0.2 C, and reduced thermalrunaway from the isothermal calorimetry test. In situ X-ray diffraction （XRD） was employed to capturethe structural changes during the charge-discharge process. The reversible evolutions of lattice parame-ters （a, b, c, and V） further verify the structural stability.

Microstructure and strain analysis of GaN epitaxial films using in-plane grazing incidence x-ray diffraction

This paper investigates the major structural parameters, such as crystal quality and strain state of （001）-oriented GaN thin films grown on sapphire substrates by metalorganic chemical vapour deposition, using an in-plane grazing incidence x-ray diffraction technique. The results are analysed and compared with a complementary out-of-plane x- ray diffraction technique. The twist of the GaN mosaic structure is determined through the direct grazing incidence t of （100） reflection which agrees well with the result obtained by extrapolation method. The method for directly determining the in-plane lattice parameters of the GaN layers is also presented. Combined with the biaxial strain model, it derives the lattice parameters corresponding to fully relaxed GaN films. The GaN epilayers show an increasing residual compressive stress with increasing layer thickness when the two dimensional growth stage is established, reaching to a maximum level of-0.89 GPa.

Fitting Full X-Ray Diffraction Patterns for Quantitative Analysis: A Method for Readily Quantifying Crystalline and Disordered Phases

Fitting of full X-ray diffraction patterns is an effective method for quantifying abundances during X-ray diffraction (XRD) analyses. The method is based on the principal that the observed diffraction pattern is the sum of the individual phases that compose the sample. By adding an internal standard (usually corundum) to both the observed patterns and to those for individual pure phases (standards), all patterns can all be normalized to an equivalent intensity based on the internal standard intensity. Using least-squares refinement, the individual phase proportions are varied until an optimal match is reached. As the fitting of full patterns uses the entire pattern, including background, disordered and amorphous phases are explicitly considered as individual phases, with their individual intensity profiles or “amorphous humps” included in the refinement. The method can be applied not only to samples that contain well-ordered materials, but it is particularly well suited for samples containing amorphous and/or disordered materials. In cases with extremely disordered materials where no crystal structure is available for Rietveld refinement or there is no unique intensity area that can be measured for a traditional RIR analysis, full-pattern fitting may be the best or only way to readily obtain quantitative results. This approach is also applicable in cases where there are several coexisting highly disordered phases. As all phases are considered as discrete individual components, abundances are not constrained to sum to 100%.

Powder x-ray diffraction and Rietveld analysis of (C_(2)H_(5)NH_(3))_(2)CuCl_(4)

Structural properties of the organic-inorganic hybrid(C_(2)H_(5)NH_(3))_(2)CuCl_(4) have been investigated by means of x-ray powder diffraction and Rietveld analysis. A structural phase transition from Pbca to Aba2 occurs at T_(4)= 240 K, which results in a paraelectric–ferroelectric phase transition. The release of the Jahn–Teller distortion with increasing temperature toward T_(4) is revealed by the structural analysis.

SEPARATION OF DIASTEREOISOMERSNEOCLAUSENAMIDE AND ISONEOCLAUSEAMIDE AND X-RAY DIFFRACTION ANALYSIS

Neoclausenamide with lowering effect on the elevated SGPT levels was isolated from leaves of Clausena Lansium (lour) Skeels. Its content in the plant is less than 0.01%. For more intense pharmacological studies, larger amount of

AN INCREMENTAL METHOD OF X-RAY DIFFRACTION QUANTITATIVE PHASE ANALYSIS OF SAMPLESCONTAINING AMORPHOUS MATERIAL

A new method for quantitative X-ray diffraction phase analysis of a powder misture has been developed according to Popovic's doping method. The weight fraction of amorphous material in the analysed sample is obtained. For a multicomponent system in which (n-2) pure phases are added into an n-phase compnent sample and theweight fractions of all n phases can be determined by the method. The test results of confirmation agree well with the theory.