Nitridation of chromium powder in ammonia atmosphere

CrN powder was synthesized by nitriding Cr metal in ammonia gas flow, and its chemical reaction mechanism and nitridation process were studied. Through thermodynamic calculations, the Cr-N-O predominance diagrams were constructed for different temperatures. Chromium nitride formed at 7002-1200℃ under relatively higher nitrogen and lower oxygen partial pressures. Phases in the products were then investigated using X-ray diffraction (XRD), and the Cr₂N content varied with reaction temperature and holding time. The results indicate that the Cr metal powder nitridation process can be explained by a diffusion model. Further, Cr₂N formed as an intermediate product because of an incomplete reaction, which was observed by high-resolution transmission electron microscopy (HRTEM). After nitriding at 1000℃ for 20 h, CrN powder with an average grain size of 63 nm was obtained, and the obtained sample was analyzed by using a scanning electron microscope (SEM).     

自组装γ-MnO2空心球的水热制备及光催化性质

在160°C的水热条件下经过6h合成了γ-MnO2的空心微米球结构,利用X射线粉末衍射(XRD),扫描电子显微镜(SEM),透射电子显微镜(TEM)等方法对其进行了表征,结果表明空心球由单相γ-MnO2构成,其直径大约在1μm左右。进一步的紫外吸附实验说明γ-MnO2对有机染料,如甲基橙具有催化作用,这在光催化方面有潜在应用价值。     

Effect of decarburization annealing temperature and time on the carbon content,microstructure, and texture of grain-oriented pure iron

In this study, the effect of decarburization annealing temperature and time on the carbon content, microstructure, and texture of grain-oriented pure iron was investigated by optical microscopy and scanning electron microscopy with electron-backscatter diffraction. The results showed that the efficiency of decarburization dramatically increased with increasing decarburization temperature. However, when the annealing temperature was increased to 825℃ and 850℃, the steel's carbon content remained essentially unchanged at 0.002%. With increasing decarburization time, the steel's carbon content generally decreased. When both the decarburization temperature and time were increased further, the average grain size dramatically increased and the number of fine grains decreased; meanwhile, some relatively larger grains developed. The main texture types of the decarburized sheets were approximately the same:{001}<110> and {112~115}<110>, with a γ-fiber texture. Furthermore, little change was observed in the texture. Compared with the experimental sheets, the texture of the cold-rolled sheet was very scattered. The best average magnetic induction (B₈₀₀) among the final products was 1.946 T.     

Fabrication of tungsten films by metallorganic chemical vapor deposition

Tungsten films growing on copper substrates were fabricated by metallorganic chemical vapor deposition (MOCVD). The chemical purity, crystallographic phase, cross-sectional texture, and resistivity of the deposited films both before and after annealing treatment were investigated by X-ray energy-dispersive spectroscopy (EDS), X-ray diffraction (XRD), scanning electron microscopy (SEM), and four-point probe method. It is found that the films deposited at 460℃ are metastable β-W with (211) orientation and can change into α-W when annealed in high-purity hydrogen atmosphere at high temperature. There are small amounts of C and O in the films, and the W content of the films increases with increasing deposition temperature and also goes up after annealing in high-purity hydrogen atmosphere. The films have columnar microstructures and the texture evolution during their growth on copper substrates can be divided into three stages. The resistivity of the as-deposited films is in the range of 87-104 μΩ·cm, and low resistivity is obtained after annealing in high-purity hydrogen atmosphere.     

Synthesis of Li_4Ti_5O_(12) nanostructural anode materials with high charge–discharge capability

This study demonstrates a facile and efficient hydrothermal method to prepare spindle titanate(Li4Ti5O12 denoted as LTO)and/or carbon-LTO nanocomposites(CLTO),in which the LTO or C-LTO microspheres have diameters of a few micrometers,composed of numerous nanosheets with thickness of*30 nm and edge length of hundreds of nanometers.The morphology and size control of these nanoparticles could be achieved by varying experimental parameters including concentration of titanium butoxide,lithium hydroxide,and cetyltrimethylammonium bromide,as well as reaction temperature and time.These micro-nanostructures were characterized by several advanced techniques,such as transmission electron microscopy,scanning electron microscopy,X-ray diffraction,energy dispersive spectroscopic analysis,surface area,and electrochemical measurements.The LTO and C-LTO microstructures were examined in the charge–discharge capacity at a rate of 50 C,as well as the stability after 100 cycles at a rate of 10 C.The excellent capability may be attributed to good conductivity,large surface area,and stable assembly structure of such micro-nanostructures,which could be explored as a promising anode material for lithium-ion batteries.     

Microstructure and texture evolution in commercial-purity Zr 702 during cold rolling and annealing

Microstructure and texture evolution in commercial-purity Zr 702 during cold rolling and annealing was investigated by optical microscopy, transmission electron microscopy, and X-ray diffraction. The results showed that crystallographic slip was the predominant deformation mechanism in the early stage of deformation. Deformation twins started to form when the rolling reduction was larger than 38.9%; both the dislocation density and the number of twins increased with increasing rolling reduction. The initial texture of the Zr 702 plate consisted of the basal fiber component. During cold rolling the strength of the basal fiber first decreased and then increased with increasing rolling reduction. The cold-rolled sheets were fully recrystallized after being annealed at 550°C. The recrystallization temperature and the size of recrystallized grains decreased with increasing rolling reduction. A larger rolling reduction resulted in a higher grain growth rate when the annealing temperature increased from 550°C to 700°C. The recrystallization texture was characterized by a major basal fiber and a minor {0113}<2110> component. The strength of the recrystallization texture increased with increasing rolling reduction.     

Grain boundary segregation of minor arsenic and nitrogen at elevated temperatures in a microalloyed steel

Auger electron spectroscopy (AES) was used to investigate the grain boundary segregation of arsenic and nitrogen in a kind of microalloyed steel produced by a compact strip production (CSP) technology at 950 to 1100℃, which are similar to the hot working temperature of the steel on a CSP production line. It was discovered that arsenic segregated on grain boundaries when the steel was annealed at 950℃ for 2 h. When the annealing temperature increased to 1100℃, arsenic was also found to have segregated on grain boundaries in the early annealing stage, for instance, within the first 5 min annealing time. However, if the holding time of the steel at this temperature increased to 2 h, arsenic diffused away from grain boundaries into the matrix again. Nitrogen was not found to have segregated on grain boundaries when the steel was annealed at a relatively low temperature, such as 950℃. But when the annealing temperature increased to 1100℃, nitrogen was detected to have segregated at grain boundaries in the steel.     

Grain size effect of IrO2 nanocatalysts for the oxygen evolution reaction

Combined with air annealing, rutile-structured IrO 2 nanoparticles with various sizes were prepared using colloidal method. The nanoparticles were used as the electrocatalysts for the oxygen evolution reaction (OER) in acidic media, and their grain size effect was studied. The results show that with the increase in annealing temperature, the grain size of the catalyst increases, and the voltammetric charges (the electroactive areas) and apparent activity for the OER decrease. The relationship between the intrinsic activity and the annealing temperature exhibits a volcano-type curve and the catalyst annealed at 550 ℃ achieved the best result.     

二硫化镍空心微球的制备和表征

以NiCl2.6H2O和Na2S2O3.5H2O为原料,在150℃较低温度的水热条件下制备了NiS2空心微球,用XRD和SEM对产物进行了表征,NiS2粉体的X射线衍射的衍射峰均与标准衍射图一致(JCPDS:653 325,立方晶系,a=0.567 8 nm),SEM图表明产物是分散较好的空心微球,微球直径为2μm,空心球壁厚为100 nm。并讨论了不同反应条件对产物的影响。     

Microstructures and impact toughness behavior of Al 5083 alloy processed by cryorolling and afterwards annealing

The influence of rolling at liquid nitrogen temperature and annealing on the microstructure and mechanical properties of Al 5083 alloy was studied in this paper. Cryorolled samples of Al 5083 show significant improvements in strength and hardness. The ultimate tensile strength increases up to 340 MPa and 390 MPa for the 30% and 50% cryorolled samples, respectively. The cryorolled samples, with 30% and 50% reduction, were subjected to Charpy impact testing at various temperatures from ?190℃ to 100℃. It is observed that increasing the percentage of reduction of samples during cryorolling has significant effect on decreasing impact toughness at all temperatures by increasing yield strength and decreasing ductility. Annealing of samples after cryorolling shows remarkable increment in impact toughness through recovery and recrystallization. The average grain size of the 50% cryorolled sample (14 μm) after annealing at 350℃ for 1 h is found to be finer than that of the 30% cryorolled sample (25 μm). The scanning electron microscopy (SEM) analysis of fractured surfaces shows a large-size dimpled morphology, resembling the ductile fracture mechanism in the starting material and fibrous structure with very fine dimples in cryorolled samples corresponding to the brittle fracture mechanism.     

Influence of post-annealing on the properties of Ta-doped In<Subscript>2</Subscript>O<Subscript>3</Subscript> transparent conductive films

Ta-doped In₂O₃ transparent conductive oxide films were deposited on glass substrates using radio-frequency (RF) sputtering at 300°C. The influence of post-annealing on the structural, morphologic, electrical and optical properties of the films was investigated using X-ray diffraction, field emission scanning electron microscopy, Hall measurements and optical transmission spectroscopy. The obtained films were polycrystalline with a cubic structure and were preferentially oriented in the (222) crystallographic direction. The lowest resistivity, 5.1×10⁻⁴ Ω cm, was obtained in the film annealed at 500°C, which is half of that of the un-annealed film (9.9×10⁻⁴ Ω cm). The average optical transmittance of the films was over 90%. The optical bandgap was found to decrease with increasing annealing temperature.     

Photocatalytic property of TiO2 sensitized by different crystal phase CdS

TiO2 samples sensitized by different crystal phase CdS(CT) are synthesized by hydrothermal process at different reaction temperature. The samples are characterized by X-ray diffraction(XRD), transmission electron microscopy(TEM), and UV-Vis diffuse reflectance(UV-Vis). The XRD result reveals that the crystal phase of CdS is transformed from cubic phase to hexagonal phase with the increase of hydrothermal reaction temperature(120-160 ℃). The absorption edge of CT is extended from 498 nm to 546 nm. The photocatalytic degradation of rhodamin B(RhB) in aqueous solution is used to evaluate the photocatalytic activity of CT. With the increase of the preparation temperature, the photocatalytic activity of CT becomes stronger. The degradation rate of RhB by CdS/TiO2 at 160 ℃(CT-160 ℃)reaches 78%.     

Preparation and characterization of CoFe2O4/SiO2 nanocomposites

Recent years see an increasing interest in nanocomposites synthesized by a sol-gel procedure consisting of magnetic nanosized particles embedded in a silica matrix. due to their specific physical and chemical properties[1―4]. Sol-gel derived amorphous si…     

Preparation of high-strength Al-Mg-Si-Cu-Fe alloy via heat treatment and rolling

An Al-Mg-Si-Cu-Fe alloy was solid-solution treated at 560°C for 3 h and then cooled by water quenching or furnace cooling. The alloy samples which underwent cooling by these two methods were rolled at different temperatures. The microstructure and mechanical properties of the rolled alloys were investigated by optical microscopy, scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and tensile testing. For the water-quenched alloys, the peak tensile strength and elongation occurred at a rolling temperature of 180°C. For the furnace-cooled alloys, the tensile strength decreased initially, until the rolling temperature of 420°C, and then increased; the elongation increased consistently with increasing rolling temperature. The effects of grain boundary hardening and dislocation hardening on the mechanical properties of these rolled alloys decreased with increases in rolling temperature. The mechanical properties of the 180°C rolling water-quenched alloy were also improved by the presence of β″ phase. Above 420°C, the effect of solid-solution hardening on the mechanical properties of the rolled alloys increased with increases in rolling temperature.     

Highly active brookite TiO2-assisted photocatalytic degradation of dyes under the simulated solar−UVA radiation

Brookite TiO_2 nanoparticles were synthesized by hydrothermal method and characterized by X-ray powder diffraction(XRD), diffuse reflectance UV–Visible spectroscopy(DRUV), and scanning electron microscopy(SEM). The obtained particles were spherical in shape with the diameter of about ～10 nm under the hydrothermal temperature of 175 °C. The photocatalytic performance of brookite was investigated in the photodegradation of dyes(rhodamine B and rose bengal) under UV-A radiation by low-power lamp. The activity of brookite and the photodegradation efficiency of dyes were estimated using a UV–Visible spectrophotometer and a total organic carbon(TOC) analyzer. Compared to anatase and rutile prepared by the similar synthesis procedure, brookite is highly active in terms of decolourization, aromatic ring opening, and mineralization.     

甘氨酸燃烧法制备纳米晶CoFe2O4铁氧体及烧结温度对其磁性能的影响

利用甘氨酸作为燃料和配合剂, 采用自蔓延燃烧法制备纳米晶钴铁氧体, 并通过X射线衍射、 扫描电子显微镜和振动样品磁强计表征样品的结构和磁性能. 结果表明, 平均晶粒尺寸对样品的磁性能影响较大, 晶粒尺寸随烧结温度的变化而变化, 并得到了矫顽力H_c和比饱和磁化强度σ_s随烧结温度的变化曲线.      

Topography,structure, and formation kinetic mechanism of carbon deposited onto nickel in the temperature range from 400 to 850℃

The carbon deposition behavior on nickel particles was observed within the temperature range from 400 to 800℃ in a pure methane atmosphere. The topography, properties, and molecular structure of the deposited carbon were investigated using field-emission scanning electron microscopy (FESEM), temperature-programmed oxidation (TPO) technology, X-ray diffraction (XRD), and Raman spectroscopy. The deposited carbon is present in the form of a film at 400-450℃, as fibers at 500-600℃, and as particles at 650-800℃. In addition, the structure of the deposited carbon becomes more ordered at higher temperatures because both the TPO peak temperature of deposited carbon and the Raman shift of the G band increase with the increase in experimental temperature, whereas the intensity ratio between the D bands and the G band decreases. An interesting observation is that the carbon deposition rate is suppressed in the medium-temperature range (M-T range) and the corresponding kinetic mechanism changes. Correspondingly, the FWHM of the G and D1 bands in the Raman spectrum reaches a maximum and the intensities of the D2, D3, and D4 bands decrease to low limits in the M-T range. These results indicate that carbon structure parameters exhibit two different tendencies with respect to varying temperature. Both of the two group parameters change dramatically as a peak function with increasing reaction temperature within the M-T range.     

静态再结晶处理对Co36Fe36Cr18Ni8Ti2合金力学性能与耐腐蚀性的影响

对冷变形后的Co₃₆Fe₃₆Cr₁₈Ni₈Ti₂合金在700 ℃和800 ℃下再结晶退火,制备成具有高强度及良好耐蚀性的多主元合金。采用电子背散射衍射（electron back-scattered diffraction, EBSD）表征了合金的相分布、再结晶组织以及晶界分布等微观结构特征,采用静态拉伸试验测试了合金的力学性能。结果表明,700 ℃退火的合金断后伸长率较低,但其抗拉强度与屈服强度分别达到了1 038和956 MPa。采用电化学工作站与扫描电子显微镜（scanning electron microscope, SEM）表征了合金在模拟体液中的耐蚀性。结果表明,700 ℃退火的样品具有较好的耐蚀性,腐蚀后的样品表面较为均匀。结合力学性能可知,700 ℃退火的样品具有作为新型医用金属材料的潜力。     

Effects of annealing temperature on the microstructure and properties of the 25Mn-3Si-3Al TWIP steel

Microstructures and mechanical properties of the 25Mn twinning induced plasticity (TWIP) steel at different annealing temperatures were investigated. The results indicated that when the annealing temperature was 1000℃, the 25Mn steel showed excellent comprehensive mechanical properties, the tensile strength was about 640 MPa, the yield strength was higher than 255 MPa, and the elongation was above 82%. The microstructure was analyzed by optical microscopy (OM), X-ray diffraction (XRD), and transmission electron microscopy (TEM). Before deformation the microstructure was composed of austenitic matrix and annealing twins at room temperature; at the same time, a significant amount of annealing twins and stacking faults were observed by TEM. Mechanical twins played a dominant role in deformation and as a result the mechanical properties were found to be excellent.     

二氧化硅@裸银纳米颗粒微球制备及其对大肠杆菌活性的影响

以SiO₂微球为载体, 利用其表面可自动吸附与还原银离子的能力, 制备新型二氧化硅@银纳米颗粒微球复合材料（SiO₂@Ag NPs）, 并用透射电镜、 Raman光谱、 X射线光电子能谱等对其进行表征, 测试其对大肠杆菌的抑菌性能. 结果表明: 当SiO₂@Ag NPs质量浓度为2.0 mg/mL时, 复合材料的抑菌率为99.8%; 当银纳米颗粒表面含有稳定剂聚乙烯吡咯烷酮时, 其抑菌率降低. 表明稳定剂可保护银纳米颗粒的单分散性, 但不利于其抑菌性的发挥.