电子陶瓷材料元素分析的前处理方法研究

陶瓷材料,由于其耐高温、耐腐蚀、耐磨等性能优异,在各行各业应用相当广泛。但也正是因为它的这些特性,在使用化学方法进行元素分析时,会遇到样品难以消解的问题,导致测试无法进行。文章重点研究电子元件中常用的三氧化二铝、氧化锆类陶瓷材料的消解方法,并介绍使用ICP-OES对消解完全的样品溶液进行元素分析的注意事项。     

Compositional tailoring effect on crystal structure,mechanical and thermal properties of γ-AlON transparent ceramics

In view of the practical application of γ-AlON as a promising transparent structural ceramic, in-depth insight into its mechanical and thermal properties is essential. The solid-state MAS NMR technique was combined with XRD Rietveld refinement to confirm the crystal structure of Al_(8+x)/3O_4-xN_x (x = 0.299–0.575). These structural parameters were further applied to predict hardness and elastic properties based on theoretical exploration, which are in good agreement with the experimental values. A slight enhancement of mechanical properties with increasing nitrogen concentration is attributed to the stronger chemical bond in octahedra. The experimental thermal conductivity of γ-AlON transparent ceramics was improved slightly with the rise of x in the temperature range from 298 K to 1074 K. The intrinsic lattice thermal conductivity was determined by eliminating the extrinsic phonon scattering as well as the thermal radiation. The reason for the discrepancy between experimental and intrinsic thermal conductivity was revealed. The present methods provided powerful and accessible guidelines in optimizing the mechanical and thermal properties of oxynitride materials.     

Exploring Hf-Ta-O precipitation upon ablation of Hf-Ta-Si-C coating on C/C composites

To improve the ablation resistance of C/C composites, a Hf-Ta-Si-C coating was fabricated by chemical vapor co-deposition. The ablation resistances of Hf-Si-C and Hf-Ta-Si-C coatings were characterized comparatively. After introducing Ta, the ablation resistance, smoothness and integrity of the ablated coating improved. Hf-Si-O and Hf-Ta-Si-O glass wires were observed. To investigate the reaction processes of the two types of glass wires, TEM observation was carried out and coupled to molecular dynamics simulations. These illustrated that Hf and Ta atoms tend gather together at high temperature. To investigate the effect of Hf-Ta-O precipitation on the ablation behavior, supplementary experiments were carried out on bulk ceramics with the same target composition, confirming that precipitation reaction could accelerated the formation of a smooth and intact oxide layer, playing a positive role in protecting C/C composites.     

Silicon in intericosahedra chains of boron carbide

Interaction between boron carbide and silicon was studied at 1400–1700 ℃ in a vacuum. The results at 1400 ℃ suggest that silicon substitutes a single atom of carbon per formula unit B₁₂C₃, producing a phase with increased lattice parameters. Temperature increase improves the degree of transformation, but at 1700 ℃, the product starts to lose silicon. Analysis of DFT formation energies of configurations with B₁₂C₃ and B₁₂C₂Si stoichiometries shows that B₁₂C₂Si may have two ground states with practically equal stability. The first is B₁₁Si(C-B-C) with silicon in icosahedral polar position, and the second is B₁₂(C^Si^C), where the silicon is in the middle of an angular chain. The latter is suggested to be more favorable during the synthesis, while the former is very close to equilibrium with its precursor B₁₁C(C-B-C), and its formation may be inhibited. Comparison of XRD patterns for the synthesis products and modeled structures seems to confirm this suggestion.     

Sensitivity analysis on globularized fraction of α lamellae in titanium alloys

The sensitivity analysis functions on globularized fraction of α lamellae were established using a physically-based microstructure model and gradient method. These functions were applied to the sensitivity analysis on globularized fraction of α lamellae in TC17 alloy. The material constants in these functions are determined using the genetic algorithm-based objective optimization technique. The globularized fraction of α lamellae during isothermal compression of TC17 alloy was quantitatively analyzed based on scanning electron microscopy (SEM) observation. The results show that α lamellae mostly change to equiaxed α grains at a deformation temperature of 1083 K, a strain rate of 0.01 s^?1 and a strain of 1.2. The globularized fraction decreases with increasing strain rate because lower strain rate provides enough time for the spheroidization. The effect of deformation temperature on the globularized fraction is controlled by the strain rate. And, the predicted derivations of globularized fraction with respect to processing parameters show good agreement with the experimental values.     

ACF/TiO2复合材料的制备及光催化降解偏二甲肼废水

用溶胶-凝胶法制备ACF/TiO2复合材料,并用于光催化降解偏二甲肼废水。同时,还讨论了材料的活化温度、偏二甲肼废水的初始浓度、H2O2及催化剂重复利用等因素对光催化效率的影响。实验结果表明,当材料的活化温度为300℃,体系中H2O2的浓度为0.12mol/L时,偏二甲肼的降解效果良好,偏二甲肼40min后的降解率达到99%以上。     

PS模板法制备铜纳米颗粒

采用双槽电化学腐蚀法制备多孔硅(porous silicon, PS), 对其进行超声后处理.以PS为模板采用一步浸渍沉积法制备大小均匀、形状规则的铜纳米颗粒, 并研究沉积时间对纳米颗粒形状、尺寸的影响.结果表明:PS超声后处理并未造成其物理和化学结构的破坏, 大量的硅氢键(SiH_x)和蜂窝状多孔结构(直径150 nm左右)分别为纳米铜的形成和生长提供了还原剂和场所;沉积时间对铜纳米颗粒形貌具有重要影响, 当沉积时间为40s时得到形状和尺寸较为均匀的铜纳米颗粒.     

Investigation on Purification of Saturated LiNO3 Solution Using Titanium Phosphate Ion Exchanger: Kinetics Study

Lithium compounds are of high interest to many industries. The presence of undesirable impurities in Li precursors leads to uncontrolled change in the functional properties of final compounds. Therefore, the development of reliable methods for lithium salt purification is considered a key factor for their application in various industries. This work focuses on the application of a titanium phosphate ion exchanger (Li-TiOP) toward Cu²⁺, Co²⁺, Mn²⁺, Ni²⁺, and Cr³⁺ ions in the purification of a saturated LiNO₃ solution. The sorption kinetics of the selected ions, considering external and internal mass transfer, as well as chemical interaction, were deeply studied. The kinetic study showed that the values of intraparticle diffusion rate and effective diffusion coefficients for the studied ions decreased in the following order: Cr(III) ˃ Cu(II) Mn(II) ˃ Co(II) ˃ Ni(II). For all the selected ions, chemical interaction was described with a pseudo-second-order reaction model. The sorption kinetics were controlled by the size of the solvated metal ion, its effective charge, the electronic structure of the adsorbed ion, and the interaction with the functional groups of the sorbent. Due to fast kinetics, the high degree of removal of trace quantities of the impurities this material gives it consideration as a promising sorbent for the deep purification of lithium salts.     

高纯度纳米硅粉的制备及其在水中的分散工艺研究

采用直流电弧等离子体蒸发法制备高纯度纳米级硅粉, 利用X射线衍射、X射线荧光分析、氮氧分析仪、透射电子显微镜和相应的选区电子衍射等测试手段对样品物理化学性质进行表征。采用紫外分光光度计法研究超声时间和不同的分散剂及其加入量对纳米硅粉在水介质中分散效果的影响。结果表明:制备出近球形、立方晶型结构的纳米硅粉, 粒径分布窄, 其纯度达到99.93% (质量比)。随着超声时间和分散剂浓度的增加, 分散效果呈现先增大后趋向平稳的趋势, 十六烷基三甲基溴化铵 (CTAB) 对纳米硅粉在水介质中的分散效果最好。纳米硅粉在水介质中较好的分散工艺为:在pH=6、超声功率为560 W的情况下, CTAB加入量为4%, 超声时间为80 min。分散后的硅粉比未分散的硅粉首次放电比容量提升14.93%, 达到了2640 m Ah/g, 首次库伦效率达到34.92%。