SnO_2-based solid solutions for CH_4 deep oxidation: Quantifying the lattice capacity of SnO_2 using an X-ray diffraction extrapolation method

A series of SnO2‐based catalysts modified by Mn, Zr, Ti and Pb oxides with a Sn/M （M=Mn, Zr, Ti and Pb） molar ratio of 9/1 were prepared by a co‐precipitation method and used for CH4 and CO oxidation. The Mn3＋, Zr4＋, Ti4＋and Pb4＋cations are incorporated into the lattice of tetragonal rutile SnO2 to form a solid solution structure. As a consequence, the surface area and thermal stability of the catalysts are improved. Moreover, the oxygen species of the modified catalysts become easier to be reduced. Therefore, the oxidation activity over the catalysts was improved, except for the one modified by Pb oxide. Manganese oxide demonstrates the best promotional effects for SnO2. Using an X‐ray diffraction extrapolation method, the lattice capacity of SnO2 for Mn2O3 was 0.135 g Mn2O3/g SnO2, which indicates that to form stable solid solution, only 21%Sn4＋cations in the lattice can be maximally replaced by Mn3＋. If the amount of Mn3＋cations is over the capacity, Mn2O3 will be formed, which is not favorable for the activity of the catalysts. The Sn rich samples with only Sn‐Mn solid solution phase show higher activity than the ones with excess Mn2O3 species.

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.

Effect of rolling temperature on microstructure and texture of twin roll cast ZK60 magnesium alloy

Twin roll cast ZK60 alloy strip/sheet with final thickness of 0.5 mm was prepared, and effect of rolling temperature on microstructure and texture development was investigated using OM and XRD technique, microstructure and texture were measured on specimens subjected to rolling experiment at different rolling temperature, and macrotexture was also evaluated by X-ray diffraction method. In addition, the （1010）and （0002） pole figures were measured, and the tensile test was performed to reveal the influence of rolling temperature on mechanical properties. The results show that the microstrucmre of ZK60 alloy sheet consisted of fibrous structure with elongated grains, and shear bands along the rolling direction after warm rolling. Dynamic recrystallization could be found during the warm rolling process at rolling temperature 350℃ and above. And many fine recrystallized grain could be observed in the shear bands area. It is a little difficult to see the recrystallized grain in the sheet warm rolled at 300℃ because of higher density of shear bands. The warm rolled ZK60 alloy sheet exhibited strong （0002） pole texture, the intensity of （0002） pole figure decreases with the increasing of rolling temperature and the basal pole tilted slightly to the transverse direction after warm rolling.

Preparation and Characterization of High Purity Enriched 10B Boric Acid via Anti-Solvent Recrystallization

Self-made enriched IUB boric acid as raw material was purified by recrystallization. The effects of final crystallization temperature, crystallization time, stirring speed, crystallization frequency and other factors on the purity were investigated. The appropriate operating condition was that the final crystallization temperature and time were 5 ℃ and 10 h respectively under a low-speed stirring for crystallizing twice, which would make the purity and yield of boric acid reach 99.94% and 95.36%, respectively. Taking this as foundation, recrystallization process was optimized with acetone as anti-solvent, whose amount was the most important index. The boric acid solution was added into acetone and recrystallized under the same condition, and the purity and yield of boric acid would reach 99.98% and 99.61%, respectively. The product detected by XRD was confirmed as boric acid crystal. Main ion concentration in the product was detected by ICP, which basically met the national standard of high purity. Crystal morphology of boric acid was observed by SEM.

Study on the Influence of Ni Modifying on Phase Transformation and Photocatalytic Activity of TiO_2

The Ni-modified TiO2 was synthesized using two methods including co-precipitation(Ni doped TiO2, Ni-TiO2) and wet impregnation(Ni loaded TiO2, Ni/TiO2). The surface and bulk crystalline phases of Ni-modified TiO2 were investigated by using X-ray diffractometry(XRD), UV Raman spectroscopy, TEM, and SEM. It is observed that Ni doping can promote the phase transition and grain size growth of TiO2. Moreover, the propagation of the rutile phase from the bulk into the surface region of TiO2 is increased when the Ni doping amount reaches up to 3%. However, in Ni/TiO2, it is found out that the surface and bulk phase transformation of TiO2 can be inhibited after impregnation of 1% of Ni on the TiO2. Compared with the co-precipitation method, Ni species may be more enriched in the surface of the Ni/TiO2 sample upon adoption of the impregnation method, and the direct contact of anatase particles of TiO2 is avoided. As a consequence, the phase transition in the surface and bulk region of TiO2 can be effectively inhibited by Ni loading. Additionally, the activity of the photocatalytic degradation of RhB on the 3Ni-TiO2-600 ℃ sample is higher than that on the 3 Ni/TiO2-600 ℃ sample. The phase junction formed between anatase and rutile in the surface region of 3Ni-TiO2-600 ℃ may the main reason for its high photocatalytic activity.

Molecular Fundaments of Mechanical Properties of Spider Silk

Dragline,framework and cocoon silk fibers of Araneus Ventricosus were used for this study.To investigate the microstructure mechanisms of stress-strain behavior of spider silk,firstly,amino acid compositions were analyzed and molecular conformations and crystallinity were measured with Raman spectra and X-ray diffraction respectively.The results showed that there were more amino acids with large side groups and polar ones in spider silk than those of Bombyx silk,and the amino acid distribution varied with different spider silk.The molecular structures were mainly α-helix and β-sheet,and random coil and β-turn existed as well.The proportions and arrangement of these conformations of dragline silk were different from framework and cocoon silk fibers.Microstructure was one of important factors of excellent mechanical properties of spider silk.Crystallinity of spider silk was very low,which implied that the roles of crystal on spider silk were not as great as other protein fibers.

Synthesis and Study of Heteronuclear Citrates

Terms of synthesis were determined for creation of new generation premixes and for their testing in experiments. Heteronuclear chelate citrates of general formula： M12MnL2.nH2O （where, M^I = Zn, Co, Fe, Mn, Cu; MH = Mn, Zn, Co, Cu; n = 0/4） were synthesized. Identity and composition of synthesized compounds were defined by microelemental analysis, determination of melting temperature and X-ray diffraction analysis. X-ray diffraction method was used also to define crystallinity of the compounds and their citric acid （H4L） component. X-ray amorphous and iso-structural orders were also revealed.

Preparation of BaAl_2O_4 by microwave sintering

The desulfurater(BaAl2O4) was successfully synthesized with BaCO3 and Al(OH)3 powders as raw materials by microwave sintering method.The mass loss of raw materials and the characterization of the outcome were investigated by means of TG-DSC,XRD and optical microscopy.The reaction mechanism was discussed.The experimental results show that synthesized BaAl2O4 by microwave sintering method is feasible.Compared with conventional sintering method,microwave sintering is a better way to synthesize BaAl2O4 with advantages of low temperature sintering,short time sintering and high synthesis rate.

Combinatorial Optimization of Ba/Fe-cordierite Solid Solution （Ba0.05Fe0.1Mg）2Al4Si5O18 for High Infrared Radiance Materials

A combinatorial chemistry method was employed to screen the Ba2＋ and Fe3＋ incorporated into cordierite structure （Ba0.05Fe0.1Mg）2A14Si5018 for exploring of high infrared radiance materials. A series of square-type sample array that consists of 7×7 compositions was syn- thesized by ink-jetting nitrate solutions into micro-reactor wells in a ceramic plate and then heat-treated at high temperatures. X-ray diffraction and infrared thermograph were used to analyze the effects of Ba2＋/Fe3＋ incorporating on the lattice distortion of cordierite and resultant changes in infrared radiance properties. Based on the results of X-ray phase analy- sis and radiance measurement of the scale-up prepared samples, the optimal Ba2＋ and Fe3＋ co-adding amount was determined to be 5%Ba2＋ plus 10%Fe3＋. Moreover, the infrared emissivity of the optimal composition at 100 ℃ was found to be higher than 0.8 in a wide wavelength range of 5-24μm. The research work demonstrates a promising application of Ba2＋/Fe3＋ cordierite solid solution as a kind of infrared heating materials for energy saving.

Anodic passivation of Pb-Ag-Nd anode in fluoride-containing H_2SO_4 solution

An attempt was made to build up a thick and compact oxide layer rapidly by pre-treating the Pb-Ag-Nd anode in fluoride-containing H2SO4 solution. The passivation reaction of Pb-Ag-Nd anode during pre-treatment process was investigated using cyclic voltammetry, linear scanning voltammetry, environmental scanning electron microscopy and X-ray diffraction analysis. The results show that Pb F2 and PbSO4 are formed near the potential of Pb/PbSO4 couple. The pre-treatment in fluoride-containing H2SO4 solution contributes to the formation of a thick, compact and adherent passive film. Furthermore, pre-treatment in fluoride-containing H2SO4 solution also facilitates the formation of PbO2 on the anodic layer, and the reason could be attributed to the formation of more PbF2 and PbSO4 during the pre-treatment which tend to transform to PbO2 during the following electrowinning process. In addition, the anodic layer on anode with pre-treatment in fluoride-containing H2SO4 solution is thick and compact, and its predominant composition is β-PbO2. In summary, the pre-treatment in fluoride-containing H2SO4 solution benefits the formation of a desirable protective layer in a short time.

Carbothermic reduction of alumina with carbon in vacuum

Carbothermic reduction alumina in vacuum was conducted, and the products were analysed by means of XRD and gas chromatography. Thermodynamic analysis shows that in vacuum the initial carbothermic reduction reaction temperature reduces compared with that under normal pressure, and the preferential order of products is Al404C, Al4C3, Al2OC, Al20 and A1. Experiment results show that the carbothermic reduction products of alumina are A1404C and A14C3, and neither A12OC, Al20 or Al was found. During the carbothermic reduction process, the reaction rate of Al203 and carbon decreases gradually with increasing time. Meanwhile, lower system pressure or higher temperature is beneficial to the carbothermic reduction of alumina process. A1404C is firstly formed in the carbothermic reaction, and then A14C3 is formed in lower system pressure or at higher temperature.

A free-cutting and ductile CuAlMnZnTiB shape memory alloy

The mechanical properties and cutting performance of the designed Cu Al Mn Zn Ti B shape memory alloy were studied by tensile test and microstructure observation. Using X-ray diffractometry, differential scanning calorimetry(DSC) and semi-quantitative shape memory effect test, the microstructure and shape memory effect were analyzed. It is found that lots of βphase and few α phase are formed in the quenching of Cu-7.5Al-9.7Mn-3.4Zn-0.3Ti-0.14B(mass fraction, %) alloy, a great deal of martensite and few α phase are formed in the aging alloy, while the annealing alloy is composed of a great deal of α phase and few βphase. The tensile strength and elongation of the annealed alloy are 649 MPa and 17.1%, respectively. Some tiny and dispersion distributed second phase particles are generated in Ti and B precipitates, greatly improving the alloy machinability.

Enhanced Photocatalytic Properties of Silver Oxide Loaded Bismuth Vanadate

In this work, BiV04 powders were synthesized by a sol-gel method, and the BiV04 gels with different calcination temperature were investigated by X-ray diffraction （XRD）. Absorption range and band gap energy, which are respon- sible for the observed photocatalyst behavior, were investigated by UV/vis diffuse reflectance spectroscopy （DRS） for pure and silver oxide loaded BiV04. Pbotocatalytic properties of the prepared samples were examined by studying the degradation of the methyl orange. When using NaCI02 as an electron acceptor, the possible photocatalytic mech- anism has been discussed by photocatalytic reactions. With the help of electron acceptor, the results show clearly that the BiV04 loaded silver oxide exhibited superior photocatalytic activity in simulated dye wastewater treatment.

Preparation of microsized single-crystalline Co_3O_4 by high-temperature hydrolysis

Microsized single-crystalline Co3O4 has been synthesized by high-temperature hydrolysis of CoCD2H20 at 600℃. The samples were characterized by powder X-ray diffraction （XRD）, scanning electron microscopy （SEM） and transmission electron microscopy （TEM）. The results reveal that the as-prepared powders are microsized single-crystalline CO3O4 with cubic spinel structure. An increase in the high-temperature hydrolysis time results in the evolution of particle shapes from cube to quasi-sphere, and then to octahedron. The effect of NaCl additive on the surface morphologies of Co3O4 particles was experimentally investigated. The results indicate that the NaCl additive acts as an inert disperse phase in the high-temperature hydrolysis, and prevents the aggregation of Co3O4 particles effectively.

Preparation and characterization of Cu-doped mesoporous CeO_2 for CO oxidation

Mesoporous CeO2 was first synthesized by hydrothermal method,and then used to synthesize different contents of CuO)x/CeO2(x:molar ratio of Cu to Ce) by deposition-precipitation method.These materials were characterized by X-ray diffraction(XRD),N2 adsorption and desorption,H2 temperature programmed reduction(H2-TPR) and O2 temperature programmed desorption(O2-TPD) to study the crystal structure,surface area,and the mechanism of CO oxidation.The results show that,on XRD patterns,no evidence of CuO diffraction peaks is present until Cu loading is increased to 20%.The BET surface area decreases noticeably with the increase of Cu content.Compared with other samples,the better reducibility and activity oxygen species of(CuO)10%/CeO2coincide with its better catalytic activity.

Hydrothermal Synthesis of Molybdenum Disulfide for Lithium Ion Battery Applications

Molybdenum disulfide nanoflakes were synthesized by a simple hydrothermal process using sodium molybdate and thiourea as reactants at a relatively low temperature. X-ray diffraction(XRD) and transmission elec-tron microscopy(TEM) indicate that the samples have the structure of 2H-MoS2 and the morphology of nanoflakes with the average thickness around 5-10 nm. The results of electrochemical properties indicate that the morphology and size of MoS2 particles have effects on their capacity when they are used as the anode for lithium ion battery. The as-prepared MoS2 samples have high reversible discharge capacity up to 994.6 mA·h·g-1 for the MoS2-1 elec-trode and 930.1 mA·h·g-1 for the MoS2-2 electrode and show excellent cycling performances. The MoS2-1 electrode has a better cycling stability than the MoS2-2 electrode due to their difference in the uniformity of the samples.

Fabrication of LaNiO3 nanofibers by electrospinning

In order to acquire LaNiO3 nanofibers with particular morphology and structure, electrospinning technique, for the first time, was successfully applied to fabricate LaNiO3 nanofibers in the paper. Polyvinyl alcohol（PVA）/ [La（NO3）3＋Ni（CH3COO）2] composite nanofibers were fabricated by electrospinning, and polycrystalline LaNiO3 nanofibers were prepared by calcination of the PVA/[La（NO3）3＋Ni（CH3COO）2] composite nanofibers at 6000C for 10 h. The samples were characterized by using thermogravimetric-differential thermal analysis （TG-DTA）, X-ray diffraction spectrometry（XRD）, scanning electron microscopy （SEM） and Fourier transform infrared spectrometry （FTIR）. The results showed that PVA/[La（NO3）3＋ Ni（CH3COO）2] composite nanofibers were amorphous in structure, and pure phase LaNiO3 nanofibers were trigonal with space group R3m. The surface of as-prepared composite nanofibers was smooth, and the diameter was about 200 nm. The diameter of LaNiO3 nanofibers was smaller than that of the relevant composite fibers. The surface of the LaNiO3 nanofibers becomes coarse with the increase of calcination temperatures. The diameter of LaNiO3 nanofibers was ca. 80 nm, and the length was greater than 100μm. The mass of the sample remained constant when the temperature was above 463℃, and the total mass loss percentage was 90.9%. Possible formation mechanism of LaNiO3 nanofibers was preliminarily proposed.

The Process of Immobilization of ZnO Nanorods Surface with Galactose Oxidase

ZnO nanorods, with the c-axis orientation used for transparent conductors, solar cells, sensors especially the functionalized ZnO nanorods with some kinds of enzymes have been used for biosensor. In this work, we describe the process immobilization of galactose oxidase on ZnO nanorods surface with glutaraldehyde as a cross-linker molecule to make the working electrode in electrochemical biosensor. ZnO nanorods were grown on FTO （Fluorine-doped tin oxide） substrate by solution method at low temperature. The crystalline phase and orientation of ZnO nanorods were identified using X-ray diffraction. The efficiency of the immobilization was calculated by Braford method showed that about 36% enzyme content was immobilized on ZnO nanorods surface. The working electrode based on the immobilized ZnO nanorods was tested in galactose solution by CV （cyclic voltammetry） method indicated the value of current intensity is about 0.14 μA. These results clearly demonstrate the potential of galactose sensor based on ZnO nanorod.

Electrochemical Performance and Capacity Fading Mechanism of LiFePO4 at Different pH Aqueous Electrolyte Solutions

The electrochemical stability of LiFePO4 in a Li＋-containing aqueous electrolyte solution is critically dependent on the pH value of the aqueous solution. It shows a considerable decay in capacity of LiFePO4 upon cycling when the pH value is increased to 11. The mechanism responsible for the capacity fading is extensively investigated by means of cyclic voltammogram, ac impedance, charge/discharge, ex situ X-ray diffraction, and chemical analysis. LiFePO4 is relatively electrochemically stable in LiNO3 aqueous solution with pH=7. But the electrochemical performance of LiFePO4 in aqueous electrolyte is inferior to that in organic electrolyte. It is attributed to the loss of Li and the Fe, P dissolution during prolonged charge-discharge in aqueous medium. A precipitate is formed on the surface of LiFePO4 electrodes. It results in the change of crystalline structure, a large electrode polarization, and capacity fading.