DIFFERENTIAL SCANNING CALORIMETRY AND X-RAY DIFFRACTION STUDIES ON AGING BEHAVIOR OF Zn-Al ALLOYS

Decomposition processes of the quenched Zn-Al alloys were studied by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results show that the stabilities of supersaturated solid solution (SSS) of Zn-Al alloy and α' phase formed by quenching would reduce with the increase of Zn content and the precipitation of η-Zn phases even when aging at ambient temperature, so that the exothermic precipitation peak in DSC curve would disappear. The activation energy of the η-Zn precipitation and the reaction enthalpy were calculated and measured. The kinetics of α' decomposition or η-Zn formation was determined by XRD. The microstructure change during aging was observed by TEM.

Determination the content of gypsum fibrosum in Xiaokening tablets by powder X ray diffraction method

The research on the application of X-ray diffraction in the quantitative analysis of Chinese medicines is rare. The main reason is that the technical problems related to the internal standard and the selection of quantitative peaks are not well solved, and the accuracy and precision of the results are not satisfactory. This study employed the concept of mass absorption coefficient based on the internal standard method, and the full spectrum fitting and quantitative methods were used to solve the above technical problems. The sample was blended. the internal standard substance of zinc oxide was fully ground, and tablets were prepared by positive pressure method. Under certain instrumental conditions, the PXRD pattern was obtained by scanning. The percentage of gypsum fibrosum in Xiaokening tablet was obtained by quantitative analysis of full spectrum fitting internal standard by TOPAS software. The method was investigated by methodology. At the same time, the method was compared by ion chromatography, and SPSS software was used to make a significant t test on the results of the two methods. After the investigation, the average standard recovery rate of CaSO4-2H2O was 99.06%(RSD = 3.02%);and the recovery rate for simulated samples was 96.7%. The method had good specificity. After statistical analysis, there was no significant difference between the new PXRD method and the traditional method of ion chromatography.

Xray Diffraction Data and Rietveld Structure Refinement for CeNi_5Sn

The compound CeNi 5Sn was studied by means of X ray powder diffraction technique and refined by Rietveld method. It has a hexagonal structure with space group P 6 3/ mmc (No.194), Z =4, the lattice constants a =0 48912(3) nm, c =1 973(2) nm and D x=8 974 g·cm -3 . The Rietveld structural refinement was performed, leading to R p=0 138 and R wp =0 185. The figure of merit F N for the XRD data is F 30 =82 1(0 0068, 54). The X ray powder diffraction data are presented.

Crystal Structure and X-ray Powder Diffraction Data for Rare Earth Compound PrNiSn

The compound PrNiSn was studied by X ray powder diffraction technique. The crystal structure and the X ray diffraction data for this compound at room temperature were reported. The compound PrNiSn is orthorhombic with lattice parameters a =0.74569(3) nm, b =0.76851(5) nm, c =0.45676(8) nm, V =0.26176 nm 3, Z =4 and D x=8.076 g·cm -3 , space group Pna2 1(33). The figure of merit F N for the compound is F 30 =54 (0.0093, 60).

X-ray elastic constant determination and residual stress of two phase TiAl-based intermetallic alloy

To evaluate the residual stress in TiAl based alloys by X ray diffraction, X ray elastic constants (REC) of a γ TiAl alloy were determined. From these results, the stress state of a given phase in a duplex TiAl based alloy under a uniaxial tensile loading has been characterized by X ray diffraction. The results show that the X ray elastic constants and the microscopic stresses of the given phase are different from the apparent elastic constants and the macroscopic stresses of the alloy. The reason of the different distribution of the alloy was also discussed. [

Synthesis and characterization of copolyimides from bis(3,4-dicarboxyphenyl)dimethylsilane dianhydride

The silicon-containing poly (amic acid)s were synthesized from bis (3, 4-dicarboxyphenyl) dimethylsilane dianhydride (SIDA), pyromellitic dianhydride (PMDA) and 4,4′-oxydianiline (4,4'-ODA) in N, N-dimethylacetamide (DMAc). The poly (amic acid) films were obtained by solution-cast method from DMAc solutions and thermally converted into transparent, flexible and tough polyimide films. The wide-angle X-ray diffraction diagrams revealed that all the polyimides possessed amorphous character, and the regulation of those polyimides were decreased with the increase of the molar ratio of SIDA to PMDA. Differential scanning calorimeter measurements showed that the introduction of SIDA to polyimide backbone would make glass transition temperature shift to lower temperature. Thermogravimetric analyses indicated that the silicon-containing polyimides lowered decomposition temperature as compared with PMDA/4, 4′-ODA polyimides. However, UV-visible transmission and reflection spectra showed that the optical transparency of silicon-containing polyimide thin films was superior to that of PMDA/4, 4'-ODA polyimide thin films.

Extraction of metals from complex sulfide nickel concentrates by low-temperature chlorination roasting and water leaching

The recovery of valuable metals from complex sulfide concentrates was investigated via chlorination roasting followed by water leaching. A reaction process is proposed on the basis of previous studies and the results of our preliminary experiments. During the process, various process parameters were studied, including the roasting temperature, the addition of NH4Cl, the roasting time, the leaching time, and the liquid-to-solid ratio. The roasted products and leach residues were characterized by X-ray diffraction and vibrational spectroscopy. Under the optimum condition, 95% of Ni, 98% of Cu, and 88% of Co were recovered. In addition, the removal of iron was studied in the water leaching stage. The results demonstrate that this process provides an effective approach for extracting multiple metals from complex concentrates or ores. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

Preparation and catalytic activity of CO-resistant catalyst core-shell Au@Pt/C for methanol oxidation

Au@Pt core-shell nanoparticles were successfully synthesized by a successive reduction method and then assembled on Vulcan XC-72 carbon surface. Furthermore, its composition, morphology, structure, and activity towards methanol oxidation were characterized by UV-vis spectrometry, transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and cyclic voltammetry (CV). Results reveal that Au@Pt/C catalyst has better activity towards methanol oxidation than the pure platinum prepared under the same conditions. When the atomic ratio of Au to Pt in the prepared Au@Pt/C catalyst is 1:2, this catalyst exhibits best electrocatalytic activity towards methanol oxidation in acidic media, and the peak current density on this catalyst is ~2.0 times higher than that on Pt/C catalyst. The better catalytic activity of Au@Pt/C results from its better resistance to toxic CO than Pt/C because the CO oxidation on Au@Pt/C is 60 mV more negative than the case on Pt/C. © The Nonferrous Metals Society of China and Springer-Verlag Berlin Heidelberg 2012.

Amine-functionalized low-cost industrial grade multi-walled carbon nanotubes for the capture of carbon dioxide

Industrial grade multi-walled carbon nanotubes(IG-MWCNTs) are a low-cost substitute for commercially purified multi-walled carbon nanotubes(P-MWCNTs). In this work, IG-MWCNTs were functionalized with tetraethylenepentamine(TEPA) for CO2capture. The TEPA impregnated IG-MWCNTs were characterized with various experimental methods including N2adsorption/desorption isotherms, elemental analysis, X-ray diffraction, Fourier transform infrared spectroscopy and thermogravimetric analysis. Both the adsorption isotherms of IGMWCNTs-n and the isosteric heats of different adsorption capacities were obtained from experiments. TEPA impregnated IG-MWCNTs were also shown to have high CO2adsorption capacity comparable to that of TEPA impregnated P-MWCNTs. The adsorption capacity of IG-MWCNTs based adsorbents was in the range of 2.145 to 3.088 mmol/g, depending on adsorption temperatures. Having the advantages of low-cost and high adsorption capacity, TEPA impregnated IG-MWCNTs seem to be a promising adsorbent for CO2capture from flue gas.

Relaxation of residual stresses in 20%SiC_w/6061Al composite as-extruded at high temperature

The residual stress in a 20%SiC w/6061Al composite as extruded was investigated by using X ray stress measurement method. It was found that, high residual stress existed in the composite and residual stress distribution in each direction are not uniform. Relaxation process of residual stress in the composite was dynamically measured during annealing at high temperature. It is verified that the relaxation of residual stress obeys the power law at high temperature. With the creep mechanism, the relaxation behavior of residual stresses at high temperature was analyzed. The results show that, the stress exponent and activation energy for stress relaxation of the composite are obviously higher than those of the matrix alloy.

Consolidation mechanism of gold concentrates containing sulfur and carbon during oxygen-enriched air roasting

Consolidation in calcines is a common problem in the oxygen-enriched air roasting of refractory gold concentrates containing sulfur and carbon when the initial temperature is greater than 600°C. To determine the phases that caused consolidation, gold concentrates were roasted under different conditions and the calcines were mainly detected by X-ray diffraction (XRD). The possible underlying mechanism was then studied through comparisons of the XRD patterns of different calcines. The results indicated that the generation of calcium magnesium silicate, iron-doped calcium aluminosilicate, and calcium aluminate caused the consolidation. Furthermore, an enriched oxygen atmosphere accelerated the oxidation reaction and the emitted heat increased the local temperature in calcines. The local temperature was inferred to have increased to the generation temperature zone of the corresponding liquid phases. Oxidation of the pyrite and decomposition of the dolomite and muscovite mainly occurred at the initial stage of oxygen-enriched air roasting. Calcium was confirmed to be essential to the consolidation process. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.

Effects of the crystallization time on the mesoporous structure,texture, morphology and styrene oxidation performances of V-MCM-41

The new V-MCM-41 molecular sieves with good ordered hexagonal mesoporous structure and crystallinity were synthesized through in-situ hydrothermal preparation method. The effects of the crystallization time were discussed. The synthesized samples were characterized by X-ray diffraction, N2adsorption/desorption, Fourier transformed infrared and scanning electron microscopy. The different structures, textures, morphologies of V-MCM-41 obtained with different crystallization times were observed and analyzed on the basis of the characterized results. The results showed that the V-MCM-41 molecular sieve obtained at 110 °C for 48 h crystallization times was of good spherical morphology, ordered hexagonal structure, most uniform pore size distribution and high surface area compared with other samples. Meanwhile, the V-MCM-41 molecular sieve with the high skeleton Si condensation and the good crystallinity was obtained. The heteroatom could be incorporated into MCM-41 framework with increasing crystallization times, which was beneficial to improve the catalytic activity and selectivity of pure siliceous MCM-41. The V-MCM-41 showed the good catalytic selectivity in catalytic oxidation of styrene using hydrogen peroxide, and the selectivity of the benzaldehyde and phenylacetic acid reached 30.68% and 49.44%, respectively. © 2016

Effects of Yttrium on the Microstructures and Interfaces in a Low Expansion Superalloy

The forms and structures of the phases in Fe-Ni-Co-Nb-Ti-Si low expansion superal-loys have been studied using analytical electron microscopy, high resolution electron microscopy, chemical phase analysis, X-ray diffraction, etc. The effects of yttrium on the microstructures and properties in the superalloys have also been investigated. The results reveal that trace yttrium mainly located in the platelet precipitates makes the crystal structure changed. The platelet precipitates become smaller, denser and rather homogeneous with appropriate yttrium addition. Compared with the conventional low expansion superalloy, the misfit of the platelet phase with the matrix in the yttrium-containing low expansion superalloy decreases from 0.7% to 0.07%, which indicates very low stress at the interface.

EXAFS STUDY OF THE SHORT RANGE STRUCTURE OF NANOCRYSTALLINE BCC-Fe_(80)Cu_(20) SOLID SOLUTION

The structure of bcc-Fe80Cu20 solid solution produced by mechanical alloying of the elemental bcc-Fe and fcc-Cu powders has been studied using X-ray diffraction and the extended X-ray absorption fine structure (EXAFS) techniques. The disappearance of elemental Fe and Cu X-ray diffraction (XRD) peaks and the presence of bcc structural XRD peaks illustrate the formation of a nanocrystalline single-phase bcc-Fe80Cu20 solid solution. From the EXAFS result, the clear observation of Cu atoms taking on bcc coordination in the solid solution and Fe atoms remaining bcc structure further verifies the reality of atomic alloying between Fe and Cu atoms and the lattice change of Cu from fcc to bcc. However, the supersaturated bcc solid solution is not chemically uniform, i.e., some regions are rich in Fe atoms and other regions rich in Cu atoms.

Investigation on Oxidation Behavior of Al-Cu-Fe Quasi-crystal

An Al62.5Cu25Fe12.5 quasi-crystalline alloy was prepared by are melting. X-ray diffraction and scanning electron microscopy were used to study the microstructure of the quasi-crystalline alloy. Isothermal weight gain of the Al-Cu-Fe quasi-crystal at elevated temperature in dry air was measured by means of a thermal balance and the oxidation behavior was evaluated by oxidation kinetic curves, from which it was deduced that the quasi-crystal exhibits good oxidation resistance. The surface morphologies of the Al-Cu-Fe quasi-crystal after isothermal oxidation at 700°C and 800°C for different times were observed. The oxidation resistance of quasi-crystalline powder and normal crystalline powder in the Al-Cu-Fe system was also quantitatively compared in quantity.

Highly efficient and stable electrooxidation of methanol and ethanol on 3D Pt catalyst by thermal decomposition of In2O3 nanoshells

In this paper In2O3nanoshells have been synthesized via a facile hydrothermal approach. The nanoshells can be completely cracked into pony-size nanocubes by annealing, which are then used as a support of Pt catalyst for methanol and ethanol electrocatalytic oxidation. The prepared In2O3and supported Pt catalysts (Pt/In2O3) were characterized by X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), field effect scanning electron microscopy (FESEM), and transmission electron microscopy (TEM). Cyclic voltammetry (CV), linear sweep voltammetry (LSV), chronoamperometry and electrochemical impedance spectroscopy (EIS) were carried out, indicating the excellent catalytic performance for alcohol electrooxidation can be achieved on Pt/In2O3nanocatalysts due to the multiple active sites, high conductivity and a mass of microchannels and micropores for reactant diffusions arising from 3D frame structures compared with that on the Pt/C catalysts. © 2016 Science Press

Oxygen diffusion in c-textured epitaxial YBa_2Cu_3O_(7-δ) thin films

Isothermal oxygen in diffusion in c textured epitaxial YBa 2Cu 3O 7- δ thin films was studied by in situ X ray diffraction. Thermal expansion coefficients of c axis length with different oxygen contents are α c (6.91, O 2)=19.1×10 -6 K -1 and α c (6.0, N 2)=19.3×10 -6 K -1 respectively. Chemical diffusion process of oxygen was described by relaxation time. From the Arrhenius plot of relaxation time, an activation energy of lattice diffusion was obtained as 1.1?eV, which is close to the results of SIMS (0.95?eV) and internal friction (1.02?eV).

Performance of grouts for post-tensioned prestressed structures

New high performance grouts with high volume stability and good fluidity were prepared with Portland cement and a multifunctional admixture (MFA). The theological characteristics and mechanical performance of the grouts were investigated. The addition of MFA effectively improves the pseudo-plasticity of the grout. The Ma cone flow time decreases obviously, and the bleeding rate tends to be zero. The deformation behaviors of fresh mixture and hardened grout are systematically studied. Mercury injection method (MIP), scanning electron microscopy (SEM) and X-ray diffractory analysis experiments are used to analyze the microstructure evolution of the grouts, which manifests that the co-action of the early bubble reaction and the latter ettringite crystallization ensure the volume stability throughout the whole hydration process and result in refined pore structure of the grout.

Preparation and Characterization of Solid Dispersions of Silymarin with Polyethylene Glycol 6000

Aim To prepare and characterize solid dispersions of silymarin with the intention of improving their dissolution properties. Methods The solid dispersions were prepared by the fusion method with polyethylene glycol 6000(PEG 6000) as the carrier. Evaluation of the properties of the dispersions was performed using dissolution studies, X ray powder diffraction and Fourier transform infrared (FT IR) spectroscopy. Results The rate of dissolution of silymarin was considerably improved as compared with pure silymarin when formulated in solid dispersions with PEG 6000. The data of the X ray diffraction showed some changes in the parameters of lattice spacing [ d ], peak position and relative intensities. FT IR together with those from X ray diffraction showed the absence of well defined drug polymer interactions. Conclusion The dissolution improvement of poorly soluble silymarin could be illuminated by the changes of the lattice parameters of PEG 6000 and the drug.

Microstructure and properties of mullite-based porous ceramics produced from coal fly ash with added Al_2O_3

Using coal fly ash slurry samples supplemented with different amounts of Al2O3, we fabricated mullite-based porous ceramics via a dipping-polymer-replica approach, which is a popular method suitable for industrial application. The microstructure, phase composition, and compressive strength of the sintered samples were investigated. Mullite was identified in all of the prepared materials by X-ray diffraction analysis. The microstructure and compressive strength were strongly influenced by the content of Al2O3. As the Al/Si mole ratio in the starting materials was increased from 0.84 to 2.40, the amount of amorphous phases in the sintered microstructure decreased and the compressive strength of the sintered samples increased. A further increase in the Al2O3content resulted in a decrease in the compressive strength of the sintered samples. The mullite-based porous ceramic with an Al/Si molar ratio of 2.40 exhibited the highest compressive strength and the greatest shrinkage among the investigated samples prepared using coal fly ash as the main starting material. © 2017, University of Science and Technology Beijing and Springer-Verlag Berlin Heidelberg.