EDTA辅助水热合成FeS2/NiSe2复合纳米晶及其薄膜光电性质

以EDTA为螯合剂，加入MX2结构化合物NiSe₂作为晶种，水热合成了FeS₂纳米晶. x射线衍射分析结果表明产物为单一相黄铁矿型FeS₂（pyrite）,平均粒径约40—50nm.丝网印刷成膜且高温退火后FeS₂薄膜光学直接带隙变宽.随晶种量的增加，吸收边在紫外—可见光谱区红移、方块电阻升高、霍尔迁移率上升和载流子浓度下降，实现了n型掺杂.并且对FeS₂的形成机理进行了讨论. 关键词： 2纳米晶')" href="#">FeS₂纳米晶 水热 诱导结晶 直接禁带宽度      

利用紫外、可见光谱探索固氮酶活性中心模拟元件物的组合反应——Ⅰ.溶剂对(Et_4N)_2[Cl_2FeS_2MoS_2]、(Mg·6DMF)[Cl_3FeOFeCl_3]及其组合反应的影响

用紫外、可见光谱考察了四种溶剂(DMF、NMF、CH_3CN、DMSO)对(Et_4N)_2(Cl_2FeS_2MoS_2](简称K_A)、(Mg·6DMF)[Cl_3FeOFeCl_3](简称K_D)及其组合反应的影响。结果表明,在DMF中,K_A与K_D基本上不反应;在NMF中,K_A分解后与K_D不反应;在CH_3CN中,K_A与K_D反应生成[Cl_2FeS_2MoS_2FeCl_2]~(2-)+FeCl_3;在DMSO中,K_A与K_D反应可能生成类立方烷铁-钼-硫原子簇化合物,为“元件设想”提供了依据。同时讨论了K_A+K_D—DMSO体系的反应机理及DMSO在反应中的作用。     

少量Mn替代对Gd2Co17化合物结构与磁性的影响

通过X射线衍射和磁性测量研究了Gd2Co17-xMnx(x=0—1)化合物的结构和磁性.X射线衍射表明样品均为Th2Zn17型菱方结构.晶胞体积随Mn含量x线性增大,居里温度TC单调下降,饱和磁化强度Ms单调增加,化合物的磁晶各向异性场μ0Ha先随Mn含量减少,当x=0.6时达到最小,然后再增大 关键词： 2∶17型化合物 晶体结构 磁性     

Cu/Co掺杂FeS_2电子结构及光学性质的第一性原理研究

采用第一性原理,对Cu/Co掺杂前后FeS_2的几何结构、电子结构和光学性质分别进行了计算与分析。分析结果表明,掺杂FeS_2晶格常数变大,禁带宽度减小,电导率增大。掺杂后介电函数虚部、吸收系数和能量损失谱的主峰均出现红移、峰值减小。共掺杂后FeS_2的光跃迁强度明显增强,可见光区的光吸收系数和光电导率均增大,说明Cu-Co共掺杂显著增强了FeS_2对光的吸收且提高了光电转换效率。     

电子束蒸发制备HfO_2高k薄膜的结构特性

使用高真空电子束蒸发在p型Si(1 0 0 )衬底上制备了高kHfO2 薄膜 .俄歇电子能谱证实薄膜组分符合化学配比 ;x射线衍射测量表明刚沉积的薄膜是近非晶的 ,高温退火后发生部分晶化 ;原子力显微镜和扫描电子显微镜检测显示在高温退火前后薄膜均具有相当平整的表面 ,表明薄膜具有优良的热稳定性 ;椭偏测得在 6 0 0nm处薄膜折射率为 2 0 9;电容 电压测试得到的薄膜介电常数为 1 9.这些特性表明高真空电子束蒸发是一种很有希望的制备作为栅介质的HfO2 薄膜的方法     

一种新型渔群探测仪问世

最近,中船总公司七院第七二六厂研制成一种YT500 型屏幕显示垂直渔群探测仪,配用了引进美国海龙公司的显示单元。该仪器主要由显示器、换能器和稳压电源构成。YT500型分YT500-1和YT500-2两种。YT500-1型的主要技术性能为 1.测量范围0—25m,0—50m,0—100m 0—150m,0—250m,0—500m(六个量程); 2.发射功率 浅水85W(电功率有效值);深水150W(电功率有效值);     

基于Al2O3/Pt纳米晶/HfO2叠层的MOS电容存储效应研究

采用电子束蒸发Pt和后快速热退火的方法,研究了退火条件对Pt纳米晶的生长特性的影响,结果显示Pt纳米晶的密度随退火温度的升高和退火时间的延长均表现出先增大后减小的趋势.在800℃下退火20 s能得到分布均匀的、密度为30×10¹¹ cm^-2的Pt纳米晶.进一步研究了基于Al₂O₃/Pt纳米晶/HfO₂叠层的MOS电容结构的存储效应,表明其在-3—+8 V扫描电压范围下C-V< 关键词： Pt纳米晶 快速热退火 原子层淀积 存储效应     

不锈钢丝网上薄膜TiO2光催化剂的Raman光谱研究

用Raman光谱方法来研究用Sol Gel法负载于金属丝网的薄膜TiO2 光催化剂的物相结构、厚度以及粒径大小。研究结果显示 ,薄膜达到一定厚度能够阻止基底Fe元素向薄膜表层的扩散 ;在 4 0 0℃下灼烧制得的薄膜TiO2 光催化剂具有锐钛矿晶型 ,而高于 4 0 0℃时 ,将出现金红石相TiO2 ;锐钛矿晶型TiO2 的Raman特征峰产生偏移 ,表明薄膜粒径的变化 ,通过计算表明 ,薄膜TiO2 的粒径为 10nm左右 ,TEM的分析结果也与之一致。     

SiO2-Al2O3-ZnO-Na2O(F,Br)体系光热折变玻璃的析晶机理研究

使用"五步法"热定影工艺制备体布拉格光栅,阐述了光热折变玻璃内部的析晶机理,借助拉曼光谱与扫描电镜直观探测到了离子迁移过程与NaF析晶过程,通过掺杂与未掺杂KBr两种组分玻璃的衍射效果以及透过率光谱对比,发现了位于350～600 nm处的吸收带,确定成核过程内部形成的胶体为溴化银与纳米银复合物.该胶体聚合生长为胶团,诱导NaF晶体在其表面析出生长,实现折射率调制.并且从胶体成核阶段、NaF析晶阶段、曝光剂量三个方面探究影响光热折变玻璃内部析晶颗粒的关键因素,研究结果表明:成核过程中[Ag0n·(AgBr)m]胶团大小是决定NaF析晶大小的关键;NaF析晶阶段主要影响析晶颗粒数量而对改变NaF析晶大小作用不大;NaF析晶大小随着曝光剂量出现先减小后增大的现象,在1.8 J/cm~2附近出现拐点、析晶颗粒最小.     

Na_2TiO_3晶型及其相变的高温原位拉曼光谱与X射线衍射联合研究

本文设计了α、β和γ三种晶型的Na_2TiO_3晶体的制备方法,采用固相烧结技术成功制备了该晶体的上述三种晶型,并对其常温拉曼光谱进行了比较研究。对其中已知晶型结构的γ-Na_2TiO_3的拉曼光谱进行密度泛函理论的模拟计算,基于计算对其拉曼光谱高频区主要振动模式进行归属。运用高温原位拉曼光谱技术和X射线衍射技术对无序型亚稳态α-Na_2TiO_3晶体升温过程的相变及其结构变化进行了原位追踪与研究,为不同晶型的Na_2TiO_3晶体的温致结构演变及晶型的鉴定提供重要的实验依据。     

基于XPS对硫铁矿去除SeO2-3的机理研究

硒是动植物及人体生长必需的十五种微量元素之一，具有清除体内自由基、抗氧化、增强免疫力等功能，但其安全剂量的范围却很窄。利用扫描电子显微镜（SEM）和X射线衍射仪（XRD）对湿法球磨制备的硫铁矿形貌进行了表征。SEM观测发现加乙醇助磨后的硫铁矿为粒径大小较均匀的球形颗粒团聚体，粒径范围在17～200 nm之间，平均粒径138 nm。XRD衍射图谱中的特征峰与FeS₂衍射图谱中各峰位置基本一致，因此判定硫铁矿中主要化学组分为FeS₂，且图谱中基本没有杂峰，表明制备过程中并未混入杂质，样品纯度较高。实验结果表明，该法制备的硫铁矿具有颗粒粒径小、比表面积大、反应活性高等优点。研究中利用X射线光电子能谱仪（XPS）对硫铁矿去除水体中SeO2-₃的机理进行了研究。研究结果表明, （1）在较为广泛的实验pH范围（pH 2.2～11.5），硫铁矿均能有效去除水体中SeO2-₃，去除效率（除pH值7.8以外）均达到90%以上；（2）硫铁矿与SeO2-₃发生反应后，其主要组成元素的XPS特征峰结合能有所减小，表明硫铁矿表面发生了一定化学变化；（3）酸碱环境下硫铁矿去除SeO2-₃的机理不完全相同，酸性环境下，硫铁矿对SeO2-₃的去除是单纯的氧化还原过程，即硫铁矿中被酸活化的S2-₂将SeO2-₃还原为单质Se(0)，并且酸性越强，SeO2-₃去除效果越好；碱性环境下，SeO2-₃的去除过程中氧化还原与络合反应并存，硫铁矿表面有络合态Fe(OH)SeO₃和单质Se(0)两种存在形态，且碱性越强，络合态Fe(OH)SeO₃含量越高。以上研究结果为硫铁矿去除固定水体和土壤中以SeO2-₃为代表的可变价金属阴离子提供重要理论依据和应用基础。     

Electronic and thermodynamic and elastic properties of pyrite RuO2

This paper calculates the elastic,thermodynamic and electronic properties of pyrite (P a3ˉ) RuO2 by the plane-wave pseudopotential density functional theory (DFT) method.The lattice parameters,normalized elastic constants,Cauchy pressure,brittle–ductile relations,heat capacity and Debye temperature are successfully obtained.The Murnaghan equation of state shows that pyrite RuO2 is a potential superhard material.Internal coordinate parameter increases with pressure,which disagrees with experimental data.An analysis based on electronic structure and the pseudogap reveals that the bonding nature in RuO2 is a combination of covalent,ionic and metallic bonding.A study of the elastic properties indicates that the pyrite phase is isotropic under usual conditions.The relationship between brittleness and ductility shows that pyrite RuO2 behaves in a ductile matter at zero pressure and the degree of ductility increases with pressure.     

水热法合成FeS2粉晶及其生长热动力学的研究

采用溶胶_凝胶水热法合成了单相黄铁矿结构的FeS2₂粉晶. 用x射线衍射、傅 氏变换红外光谱等分析手段对FeS2₂粉晶进行了表征，以简化的数学模型及相 变理论讨论了晶体 生长过程. 结果表明：FeS2₂晶粒的生长过程属于相变与扩散的混合机制，符 合经时间 指数修正的二次方动力学方程，是一个生长速率随时间变化的过程；水热晶化温度高于453 K、反应时间超过18 h且有适量的硫参与反应时，可得到单相的黄铁矿型的FeS2₂关键词： 溶胶_凝胶水热法 2粉晶')" href="#">FeS2₂粉晶 晶粒生长 热动力学     

Low temperature uniaxial growth of conducting LaNiO3 thin films on glass substrates with RbLaNb2O7 seed layer

Conducting LaNiO₃ thin films have been fabricated on the borosilicate glass substrates with and without the uniaxial oriented RbLaNb₂O₇ seed layer by an excimer laser assisted metal organic deposition process with a KrF laser irradiation at 400°C in air. The LaNiO₃ thin film prepared on the seed layer had a very high Lotgering factor at F(100)=0.971, indicating highly (100)-oriented growth. The obtained LaNiO₃ thin films with and without the seed layer showed low resistivity values, 4.42 and 1.02 mΩ cm at room temperature, respectively. The ρ value of the (100)-oriented LaNiO₃ film on the seed layer was comparably lowered to that of the films prepared at high process temperatures reported in the previous reports.     

Growth of hierarchical based ZnO micro/nanostructured films and their tunable wettability behavior

Hierarchical zinc oxide (ZnO) micro/nanostructured thin films were grown onto as-prepared and different annealed ZnO seed layer films by a simple two step chemical process. A cost effective successive ionic layer adsorption and reaction (SILAR) method was employed to grow the seed layer films at optimal temperature (80 °C) and secondly, different hierarchical based ZnO structured thin films were deposited over the seed layered films by chemical bath deposition (CBD). The influence of seed layer on the structural, surface morphological, optical and wettability behavior of the ZnO thin films were systematically investigated. The XRD analysis confirms the high crystalline nature of both the seed layer and corresponding ZnO micro/nanostructured films with a perfect hexagonal structure oriented along (0 0 2) direction. The surface morphology revels a complex and orientated hierarchical based ZnO structured films with diverse shapes from plates to hexagonal rod-like crystal to tube-like structure and even much more complex needle-like shapes during secondary nucleation, by changing the seed layer conditions. The water contact angle (WCA) measurements on hierarchical ZnO structured films are completely examined to study its surface wettability behavior for its suitability in future self-cleaning application. Photoluminescence (PL) spectra of the ZnO structured film exhibit UV and visible emissions in the range of 420-500 nm. The present approach demonstrates its potential for low-temperature, large-scale, controlled synthesis of crystalline hierarchical ZnO nanostructures films.     

High-temperature transformation of pyrite in CO2: Effects of residence time and the presence of O2

To understand the behavior of pyrite (a key slag-inducing coal mineral) in oxyfuel combustion (O₂/CO₂ combustion), our previous work firstly investigated the effects of pure CO₂ on fixed bed reactors and at low temperatures (<1273 K) and long residence time (order of minutes). As a consecutive contribution, this work explores pyrite transformation in CO₂ with the presence of O₂ on a drop tube furnace (DTF) and at a high temperature of 1573 K. These conditions are more relevant to practical oxyfuel combustion. Pulverized pyrite samples of sizes between 63 and 75 µm were tested in CO₂ with varying O₂ from 0 to 3%, mimicking the conditions near the boiler burners. The changes of pyrite transformation with residence time were investigated by examining the intermediate products, collected by a high-temperature sampling probe. For a clear clarification of the effects of CO₂, tests were also carried out in O₂/N₂ for comparison. The solid products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometry (EDS). The gas products were analyzed online by a gas analyzer. Results showed that, in the absence of O₂, CO₂ chemically accelerated pyrite decomposition and oxidation when compared with N₂. This finding was consistent with that in previous work performed on fixed-bed reactors. In the presence of the same O₂ concentration, the positive roles of CO₂ persisted, enhancing the formation of magnetite (Fe₃O₄) and SO₂. In either O₂/CO₂ or O₂/N₂, increasing O₂ concentration also favored the formation of magnetite and SO₂. Significant changes of SO₂ and S in pyrrhotite (FeS_x) were observed between 0.5–0.7 s, and longer residence time did not seem to have significant effects. However, the amount of magnetite formed increased with increasing residence time. The obtained knowledge is new and very useful to further understanding of pyrite behavior in real oxyfuel combustion systems.     

The preferential growth of pyrite films prepared by thermal sulfuration of Fe2O3 films

Pyrite thin films were prepared by the sol-gel dip coating process and sulfuration treatment. The evolution of crystal orientation for the pyrite films was investigated as a function of sulfuration temperature. And the effect of crystal orientation on the electrical and optical properties was studied. It was found that films show (1 1 1) preferred orientation after sulfurized at low temperature. However, the (2 0 0) and (3 1 1) mixed preferred orientations were observed when pyrite films were sulfurized at higher temperature. Experimental results also indicate that the carrier concentration is high when the films show (1 1 1) preferred orientation. And the optical absorption coefficient is also large when the films grow with (1 1 1) preferred orientation. It is speculated that surface free energy could play a more important role in determination of preferred orientation when films were sulfurized at low temperature. However, the strain energy plays a more important role in determination of preferred orientation when films were sulfurized at higher temperature.     

Complete filling of 41 nm trench pattern using Cu seed layer deposited by SAM-modified electroless plating and electron-beam evaporation

To overcome the limitation of the sputtered Cu seed layer in electroplating of Cu interconnects imposed by the shadow effect, a new method for depositing a Cu seed layer on a 41 nm trench pattern based on combination of electroless plating (ELP) and electron-beam (E-Beam) evaporation was developed. A Cu seed layer formed by ELP alone was too thin to be used for electroplating due to its high resistivity. To solve this problem, an additional Cu layer was deposited on top of the trench by E-Beam evaporator to enhance the electrical conductivity of the Cu seed layer. The electrical resistivity of the resulting Cu layer was reduced to 4.8 μΩ cm, which was sufficient for the conductive seed layer for electroplating the 41 nm trench pattern. The gap-filling capability also improved and there were no voids or seams in the 41 nm trench pattern. The proposed method can be an effective solution for fabrication of a conductive seed layer to fill a 41 nm trench pattern by electroplating.     

Ultra‐thin (002)‐oriented Al‐doped zinc oxide transparent electrode grown on oxygen‐controlled homo‐seed layer

Highly (002)‐oriented Al‐doped zinc oxide (AZO) thin films with the thickness of less than 200 nm have been deposited on an oxygen‐controlled homo‐seed layer at 200 °C by DC magnetron sputtering. With the homo‐seed layer being employed, the full‐width at half maximum (FWHM) of the (002) diffraction peak for the AZO ultra‐thin films decreased from 0.33° to 0.22°, and, the corresponding average grain size increased from 26.8 nm to 43.0 nm. The XRD rocking curves revealed that the AZO ultra‐thin film grown on the seed layer deposited in atmosphere of O₂/Ar of 0.09 exhibited the most excellent structural order. The AZO ultra‐thin film with homo‐seed layer reached a resistivity of 4.2 × 10^–4 Ω cm, carrier concentration of 5.2 × 10²⁰ cm^–3 and mobility of 28.8 cm² V^–1 s^–1. The average transmittance of the AZO ultra‐thin film with homo‐seed layer reached 85.4% in the range of 380–780 nm including the substrate. (© 2014 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)