超细矿粉对混凝土界面区硫酸盐腐蚀的影响

为了研究骨料与水泥石界面区(ITZ)的组成及结构对混凝土抗硫酸盐腐蚀性能的影响,利用紫外分光光度计绘制了硫酸钠溶液浸泡混凝土试样的SO2-4浸入浓度/深度曲线,并辅以扫描电镜(SEM)和电子探针能谱(EDS)等对ITZ进行观测;同时利用XRD定量分析研究了混凝土本体相和界面相的水化产物富集的差异.结果表明:Ca(OH)2、钙矾石(AFt)等晶体富集于硫酸钠溶液浸泡后试样的ITZ,引起AFt二次结晶型的硫酸盐腐蚀破坏.在适量石膏的激发下,掺入超细矿粉(GGBS)可阻止AFt转变成单硫型水化硫铝酸钙(AFm),减少AFt二次结晶的生成,明显提高抗硫酸盐侵蚀能力,试样的同深度硫酸根浓度最低,抗硫酸盐侵蚀性能最好.     

Preparation and characterization of PEGDE crosslinked silk fibroin film

To obtain water-insoluble silk fibroin(SF) materials, polyethylene glycol diglycidyl ether(PEG-DE) was selected as a crosslinking agent to prepare SF films(blends). The reaction conditions were optimized for the crosslinking of the SF molecules. The hot water stability of the blends was measured using BCA protein assay and gravimetric analysis. The molecular conformation and crystalline structure of the blends were analyzed by FTIR and XRD, respectively. When the mass ratio of SF:PEG-DE was 1.0:0.8, the hot water loss rate of the SF blends was minimized. PEG-DE could induce SF molecules to form β-sheets during the gel reaction process, resulting in improved crystallinity and hot water dissolved resistance of the blend films. In order to demonstrate the cytotoxicity of the chemical reagents used to crosslink SF, L929 cells were seeded on the blend film(SF:PEG-DE = 1:1) and cultured for 3 days. Cells of L929 readily adhered and spread in the fusiform on the blend film resulting in high cell viability. The extracted liquid from the SF porous film did not inhibit cell proliferation, as estimated by the MTT assay.     

负载型钼基催化剂的制备及其合成甲硫醇的性能研究

本文采用等体积浸渍法制备了一系列负载型钼基催化剂,系统研究了不同K/Mo摩尔比、第二助剂和不同载体的钼基催化剂对混合气(CO/H2S/H2)制备甲硫醇性能的影响.由催化剂的活性评价可知,当K/Mo摩尔比为2.0时,催化剂具有最大的反应活性;分别添加铁、钴和镍3种过渡金属制备的催化剂对甲硫醇的选择性大小顺序为:CoNiFe;比较SBA-15和Si O2两种载体,发现K-Mo-Co/SBA-15的催化活性明显高于K-Mo-Co/Si O2,甲硫醇的选择性达到46.77%.实验分别采用N2-吸脱附、XRD和H2-TPR等手段对不同K/Mo摩尔比和负载2种不同载体的钼基催化剂进行了表征,并对催化剂的结构和性能进行了探讨.     

纳米TiO2碳热氮化制备纳米晶Ti(C0.7,N0.3)固溶体

在封闭系统中,对纳米TiO2碳热还原氮化反应合成纳米晶Ti(C,N)固溶体粉末进行研究。结果表明,当以C/Ti值为2.7配料,氮气压力为0.005 MPa时,一定量纳米TiO2/纳米碳黑混合料在1600℃下保温4 h,可以合成晶粒尺寸为32 nm的球形Ti(C0.7,N0.3)固溶体粉末。     

电铸金刚石-镍复合膜微观应力分析

用电铸方法，采用低应力电镀液，研制出了金刚石-金属复合膜。该复合膜的厚度为20-45μm，可用于制作超薄切割刀具。介绍了用X射线衍射法（xRD）测量多晶体微观应力的基本原理和用X射线衍射法测量镍多晶体显微应变的程序。用单波法计算了电铸金刚石-镍复合膜的显微应变，并用扫描电镜（SEM）观察了该复合膜的表面形貌。结果发现：阴极电流密度严重影响复合膜的显微应变，在实验所用电流密度范围内（0．6-3．5A／dm^2），随着电流密度的增加，显微应变减小。     

GaAs／AlAs DBR的GSMBE优化生长及表征

采用气态源分子束外延（GSMBE）技术优化生长了GaAs／AlAs分布布拉格反射镜（DBR）材料，并用X射线衍射（XRD）及反射光谱对其生长质量进行了表征。结果表明，采用5S间断生长的GaAs／AlAs DBR材料质量和界面质量优于无间断生长，并且10对GaAs／AlAs DBR的质量优于30对，说明DBR对数越多，周期厚度波动越大，材料质量越差。优化生长得到的30对GaAs／AlAsDBR的反射率大于99％，中心波长为1316nm，与理论设计结构的模拟结果基本一致，可用作1．3μm垂直腔面发射激光器（VVSEL）直接键合的反射腔镜。     

Influence of chromium on the local structure and morphology of ferric oxyhydroxides

The extended X-ray absorption fine structure (EXAFS) method and transmission electron microscopy (TEM) have been used for characterizing the local structure and morphology of ferric oxyhydroxides, α-FeOOH and γ-FeOOH, with and without chromium. These ferric oxyhydroxide powders were prepared from aqueous solutions containing iron and chromium ions. Radial structural functions for iron obtained by Fe K edge EXAFS spectra showed that the linkage of structural units formed by FeO₆ octahedra in γ-FeOOH is distorted by chromium addition, while such distortion in α-FeOOH is not clearly detected. On the other hand, Cr K edge EXAFS spectra showed that the local structure around chromium does not necessarily correspond to the local structure around of iron, which is observed by Fe K edge EXAFS spectra. This suggests that the structural units containing iron and chromium are heterogeneously distributed in these ferric oxyhydroxides. The local structural information was discussed coupled with morphological features of these ferric oxyhydroxides observed by TEM.     

Preparation of epitaxial and polycrystalline bismuth titanate thin films on single crystal (100) MgO by chemical solution deposition

Epitaxial and polycrystalline Bi₄Ti₃O₁₂ thin films were prepared on single crystal (100) MgO substrates by a chemical solution deposition process using metal naphthenates as starting materials. Pyrolyzed films (at 500°C) were annealed for 30 min in air at 650, 700, 750 and 800°C, respectively. The effects of annealing temperature on the crystallinity, epitaxy and surface morphology of the films were investigated by X-ray diffraction θ-2θ scans, pole-figure analysis, and atomic force microscopy (AFM). Epitaxially grown films annealed at 700 and 750°C, respectively, showed growth of three-dimensional needle-shaped grains. During annealing at 800°C, grain growth of Bi₄Ti₃O₁₂ may be suppressed by the formation of a titanium-rich phase such as Bi₂Ti₂O₇ owing to Bi volatilization, resulting in lower root mean square roughness than that of film annealed at 750°C.     

基于XRD的薄膜界面结合强度试验研究

利用X射线衍射技术（XRD）分析了薄膜结合界面应力及其变化规律，通过对薄膜界面结合状态的检测，建立了X衍射法测量薄膜界面结合强度的原理、方法与过程。其检测界面结合强度方法可对薄膜试样进行非接触检测，适用于晶体或多晶体薄膜的界面结合强度测量，是一种研究无损检测薄膜结合强度的试验新方法。     

Evolution of patinas on copper exposed in a suburban area

Copper plates were exposed under sheltered outdoor conditions for up to one year, starting in September 2001 in Musashino City, Tokyo, a suburban area. Following various periods of exposure, the patinas on the plates were characterized to investigate their evolution by using X-ray fluorescence analysis, X-ray diffraction, field emission scanning electron microscopy, and glow discharge optical emission spectroscopy. The difference in the roles of sulfur and chlorine in the early stages of copper patination were identified by analyzing the depth profiles of these two elements. Sulfur was found on top of the patina as cupric sulfates such as posnjakite (Cu₄SO₄(OH)₆ · H₂O) or brochantite (Cu₄SO₄(OH)₆). Brochantite appeared only after 12 months of exposure. In contrast, chlorine was found on the surface after only one month of exposure. It gradually penetrated the patina as the exposure period lengthened, forming copper chloride complexes. Chloride ions accumulated at the patina/copper interface, forming nantokite (CuCl), which promoted corrosion.