溶胶-凝胶法有机-无机精细复合材料P(VDF/TeFE)-SiO_2的制备与显微结构

用溶胶－凝胶法制备了有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。利用水解－聚合反应由正硅酸乙脂（ＴＥＯＳ）合成ＳｉＯ２溶胶，乙醇作溶剂，盐酸作催化剂。将Ｐ（ＶＤＦ／ＴｅＦＥ）溶于丙酮，并与ＳｉＯ２溶胶均匀混合。凝胶后经干燥和热处理得到有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。用红外光谱分析、扫描电镜分析、差示扫描热分析和热失重分析对有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２进行了显微结构表征。     

TiO_2在MCM-41内表面单层及双层分散的结构表征

首次以有机物钛酸丁酯为前驱体,合成了ＴｉＯ２呈单层分散状态（Ｔｉ／Ｓｉ＝０.２０）或双层分散状态（Ｔｉ／Ｓｉ＝０．３９）的介孔分子筛ＭＣＭ－４１（Ｓｉ／Ａｌ＝３５）,并以 ＸＲＤ,ＦＴＩＲ,Ｎ２吸附－脱附,固体ＵＶ－ｖｉｓ 漫反射等表征手段对其结构特征和氧化钛分散状态进行了研究．结果表明： ＴｉＯ２在介孔分子筛ＭＣＭ－４１孔道中分散, ＭＣＭ－４１骨架结构结晶度降低,但是附着二层ＴｉＯ２后,仍能保持长程有序结构; ＴｉＯ２与ＭＣＭ－４１孔道表面的ＳｉＯ２以化学键连接,生成Ｓｉ－Ｏ—Ｔｉ键;无论是单层还是双层分散的 ＴｉＯ２在 ＭＣＭ－４１内孔壁均匀分散;且由于ＴｉＯ２粒子的减小使其对紫外光的吸收发生明显的蓝移现象．     

医用NiTi合金表面溶胶-凝胶法制备TiO2-SiO2薄膜

采用溶胶－凝胶法在ＮｉＴｉ形状记忆合金表面制备了ＴｉＯ_２－ＳｉＯ_２复合薄膜,在提高医用ＮｉＴｉ合金的抗腐蚀性方面,收到了显著的效果．运用电化学方法对不同组成的ＴｉＯ_２－ＳｉＯ_２薄膜在模拟体液中的腐蚀行为进行了研究,结果表明,随薄膜中 Ｔｉ／Ｓｉ比的增加,ＴｉＯ_２－ＳｉＯ_２薄膜的抗腐蚀性增强．划痕试验表明 ＴｉＯ_２－ＳｉＯ_２（Ｔｉ／Ｓｉ＝４：１）膜与ＮｉＴｉ合金基体具有较高的界面结合强度．用原子力显微镜（ＡＦＭ）对ＴｉＯ_２－ＳｉＯ_２薄膜的表面形貌及表面粗糙度进行观察和分析,解释并讨论了ＴｉＯ_２－ＳｉＯ_２薄膜的配方组成与其抗腐蚀性的关系,ＳｉＯ_２含量较少时,薄膜结构致密,膜层均匀平滑,且膜基结合力好,作为医用ＮｉＴｉ合金的表面保护层,可以使其耐腐蚀性有显著提高．     

溶胶—凝胶制备TiO2／SiO2复合薄膜的FT—IR表征

ＦＴ－ＩＲ吸收谱用来研究具有多孔结构的ＴｉＯ２／ＳｉＯ２复合薄膜；薄膜在１２００ｃｍ＾－１有一较强的肩峰，其强度与峰位随热处理温度度而生变化。在９５５ｃｍ＾－１的吸收峰是由于Ｓｉ－Ｏ－Ｔｉ和Ｓｉ－ＯＨ的结果，并随着热处理 度的提高其吸收峰完全是Ｓｉ－Ｏ－Ｔｉ振动所引起的，其峰位随着ＴｉＯ２的增加，向低频区域移动。     

Al2O3—SiO2—TiO2复合陶瓷薄膜的制备与结构

本文利用Ｓｏｌ－Ｇｅｌ法制备了Ａｌ２Ｏ－ＳｉＯ２－ＴｉＯ２复合陶瓷薄膜，讨论了主要内容是体系成分（Ａｌ：Ｓｉ：Ｔｉ摩尔比）对落膜制备过程及结构的影响。通过分步水解法可以得到稳定的Ａｌ２Ｏ３－ＳｉＯ２－ＴｉＯ２复合溶胶，进而制备复合陶瓷薄膜。组分间的静电作用是溶胶凝结的原因。三组分中，Ｓｉ／Ｔｉ摩尔比是决定溶胶稳定性的主要因素。通过ＸＲＤ对薄膜的相组成进行了分析，表明复合薄膜由Ａｌ４Ｔｉ２ＳｉＯ１２     

Au/(Si/SiO2)/p型Si结构的可见电致发光研究

Ｓｉ／ＳｉＯ２薄膜采用射频磁控溅射技术制备,当正向偏压大于５Ｖ时即可观测到来自不同Ｓｉ层厚度的Ａｕ／（Ｓｉ／ＳｉＯ２）／ｐ－Ｓｉ结构在室温下的可见电致发光,其发光谱峰位均位于６６０ｎｍ处,测得的各种储藏坟下的发光峰位不随正向偏压的升高而移动。突验结果表明光发射主要来自于ＳｉＯ２层中的发光中心上的复合发光。     

TiO2—聚乙烯复合膜的制备有红外光谱对其膜层结构的表征

开发了以Ｔｉ＾４＋为桥联剂制备无机－有机复合膜的新方法，以自制的硅薄土多孔陶 为基膜（支撑体），使用浸涂法－热致相转相结合制备了ＴｉＯ２－聚乙烯复合膜，并用红外光谱表征了复合膜层与层之间的结合方式和强度，支撑体中的ＳｉＯ２通过Ｔｉ＾４＋与聚乙烯的分子之间形成了新的化合物型膜层。     

SiC_w／Al_2O_3－（Ti，W）C复相陶瓷的微观结构及其力学性能

本文对Ａｌ_２Ｏ_３（Ｔｉ，Ｗ）Ｃ和ＳｉＣｗ－Ａｌ_２Ｏ_３（Ｔｉ，Ｗ）Ｃ的力学性能进行了分析对比，研究了热压工艺、ＳｉＣ晶须含量、晶须分散效果和晶须／基体的复合情况等对Ａｌ_２Ｏ_３（Ｔｉ，Ｗ）Ｃ复相陶瓷力学性能的影响。从热膨胀系数失配角度分析和微观结构的观察证实，ＳｉＣ晶须及（Ｔｉ，Ｗ）Ｃ固溶体对改善Ａｌ_２Ｏ_３陶瓷力学性能的效果是显著的，ＳｉＣ_ｗ－Ａｌ_２Ｏ_３．（Ｔｉ，Ｗ）Ｃ陶瓷材料的增韧机制主要是裂纹偏转和裂纹桥接。     

PZT／Si薄膜的扩散反应研究

运用ＸＰＳ和ＡＥＳ研究了ＰＺＴ膜／Ｓｉ在热处理过程中的薄膜及界面化学反应；在热处理过程中，气氛中的气通过ＰＺＴ的缺陷通道扩散到ＰＺＴ／Ｓｉ同旧，并与界面上的硅发生氧化反应形成ＳｉＯ２界面层。同时基底上的硅通过ＰＺＴ的缺陷扩散么样品表面形成ＳｉＯ２表面层。此外，在ＰＺＴ／Ｓｉ界面上，Ｔｉ的氧化物和Ｓｉ发生还原反应，形成了ＴｉＳｉｘ金属硅化物，并残留在ＰＺＴ膜层和和ＳｉＯ２界面层中。在ＰＺＴ膜层内，有     

溶胶—凝胶法有机—无机精细复合材料P（VDF／TeFE）—SiO2的制备与显微 …

用溶胶－凝胶法制备了有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。利用水解－聚合反应由正硅酸乙酯（ＴＥＯＳ）合成ＳｉＯ２溶胶，乙醇作溶剂，盐酸作催化剂。将Ｐ（ＶＤＦ／ＴｅＦＥ）溶于丙酮，并与ＳｉＯ２溶胶均匀混合。凝胶后经干燥和热处理得到有机－无机精细复合材料Ｐ（ＶＤＦ／ＴｅＦＥ）－ＳｉＯ２。用红外光谱分析、扫描电镜分析、差示扫描热分析和热失重分析对有机－无机精细复事材料Ｐ（ＶＤＦ／ＴｅＦ     

A study of the dynamic properties of photo-induced charge carriers at nanoporous TiO(2)/conductive substrate interfaces by the transient photovoltage technique

Two interfaces with opposite orientations of the built-in electric field, nanoporous TiO(2)?film/ FTO electrode and nanoporous TiO(2) film/semitransparent Pt substrate, were constructed. The separation and transport of photo-induced charge carriers in the two systems of nanoporous TiO(2)/conductive substrate were studied by the transient photovoltage technique. Various transient photovoltage responses were obtained when the laser beam was incident from the surface of the nanoporous TiO(2) film (top illumination) or the TiO(2)/substrate interface (bottom illumination). A linear and a logarithmic dependence of the photovoltage amplitude on the excitation level were observed for top illumination and bottom illumination, respectively. The results indicate that diffusion is the major way for the separation of charge carriers in the nanoporous TiO(2) film and that the excess carriers were separated by drift under the built-in electric field at the TiO(2)/substrate interfaces.     

SiO2/TiO2复合气凝胶的孔道结构研究

为了在常压干燥下制备高比表面积且具有多级孔道结构的SiO2/TiO2复合气凝胶,以正硅酸乙酯、钛酸丁酯为原料,利用低聚体聚合将分相平行引入到溶胶凝胶过程中,获得SiO2/TiO2醇凝胶,并通过溶剂替换技术实现气凝胶的常压干燥制备.不同硅钛比气凝胶的内部结构研究表明:合成的气凝胶是由纳米SiO2和TiO2颗粒分散复合而成的介孔块体,其中Ti—O—Ti、Si—O—Si和Ti—O—Si键相互交织.气凝胶的结构变化是分相与溶胶凝胶过程相互竞争的结果.Si含量能显著改善气凝胶的结构,当n(Ti)∶n(Si)为3∶1时,比表面积高达712.2 m2/g,平均孔径为3.36 nm;当n(Ti)∶n(Si)为1.5∶1时,复合气凝胶具有明显双连续孔道,比表面积高,同时孔状结构清晰.     

NH3 sensing characteristics of nano-WO3 thin films deposited on porous silicon

The NH3 sensing characteristics of nano-tungsten trioxide (WO3) thin films deposited on porous silicon (PS) were investigated in the present study. Porous silicon layer was first prepared by electrochemical etching in an HF-based solution on a p(+)-type silicon substrate. Then, WO3 nano-films were deposited on the porous silicon layer by DC magnetron sputtering. Pt electrodes were deposited on the top surface of the WO3 films to obtain the WO3/PS gas sensor. The WO3 films deposited on PS were characterized by SEM, XRD and XPS. The NH3 sensing characteristics for WO3/PS gas sensor were tested at room temperature and 50 degrees C. The results showed that the NH3 sensing characteristics of WO3/PS were superior to WO3/Al2O3 at room temperature. The sensing mechanism of the nano-WO3 thin films based on PS was also discussed.     

Low-concentration NO/sub 2/ detection with an adsorption porous silicon FET

Adsorption porous silicon FET (APSFET) is a porous silicon (PS)-based device constituted of a FET structure with a porous adsorbing layer between drain and source. Adsorbed gas molecules in the porous layer induce an inverted channel in the crystalline silicon under the PS itself. The mobile charge per unit area in the channel depends on the molecular gas concentrations in the sensing layer so that adsorbed gas molecules play a role similar to the charge on the gate of a FET. In this work, NO/sub 2/ detection by using the APSFET is demonstrated for the first time. NO/sub 2/ concentration as low as 100 ppb was detected. Devices with both as-grown and oxidized PS layers were fabricated and compared in order to investigate the effect of a low-temperature thermal oxidation on the electrical performances of the sensor. Nonoxidized sensors show a high sensitivity only for fresh devices, which reduces with the aging of the sample. Oxidation of the PS layer improves the electrical performance of sensors, in terms of stability, recovery time, and interference with the relative humidity level, keeping the high sensitivity to nitrogen dioxide.     

多孔硅对单晶硅少子寿命影响状况的研究

以p型单晶硅片为研究对象,在单晶硅片表面采用化学腐蚀方法制备多孔硅层,通过实验选取制备多孔硅的最佳工艺条件,采用SEM观察多孔硅表面形貌,以及用微波光电导法测试少子寿命的变化情况。结果表明,在相同的腐蚀溶液配比条件下腐蚀11min得到的多孔硅层的表面形貌最好,孔隙率最大。在850℃下热处理150min时样品少子寿命的提高达到最大,不同腐蚀时间的样品少子寿命提高程度不同,腐蚀11min的样品少子寿命提高最大,约有10%左右。多孔层的形成伴随着弹性机械应力的出现,引起多孔层-硅基底界面处产生弹性变形,这有利于缺陷和金属杂质在界面处富集。另外,多孔硅仍具有晶体结构,但其表面方向上的晶格参数要比初始硅的晶格参数大,也有利于金属杂质向多孔层迁移。     

聚苯乙烯和聚乙二醇对TiO2薄膜微观结构及DSSC性能的影响

用水热法制备了多孔TiO2光电薄膜;分析了聚苯乙烯和聚乙二醇对纳米TiO2晶体薄膜微观结构的影响;用紫外-可见-近红外分光光度计和场发射扫描电镜对纳米TiO2薄膜进行了表征;并对组装的染料敏化太阳能电池进行了光电性能测试,发现用聚苯乙烯处理后的TiO2薄膜提高了染料敏化太阳能电池(DSSC)的开路电压、短路电流密度、填充因子和光电转换效率.     

多孔硅与聚甲基丙烯酸甲酯复合光致发光特性研究

多孔硅与有机材料复合可以改善多孔硅的光致发光特性。用化学腐蚀的方法制备了多孔硅，通过不同方法实现了多孔硅与聚甲基丙烯酸甲酯(PMMA)的复合。实验结果表明，用旋涂法实现的PMMA固化后再与多孔硅复合而制得的样品的结果最好，它与原始的多孔硅样品相比，发光峰发生了蓝移而且发光强度下降很小。PMMA层有限的厚度和PMMA对多孔硅表面的保护使复合后发光强度下降很小。制备的多孔／PMMA复合体系的发光强度几乎不随时间而下降，这可能是由于PMMA有效地隔绝多孔硅与空气的接触，保护了多孔硅的表面，不会产生更多的悬挂键。     

Effects of porous silicon morphology on ballistic electron emission

Porous silicon ballistic electron emission source with a structure of metal/porous silicon/Si/metal is obtained by anodization, rapid thermal oxidation, and sputtering. The microstructures of porous silicon layers are characterized by means of scanning electron microscope. The results show that disordered pores are formed at anodization current densities of 15 mA/cm2, 30 mA/cm2, and 45 mA/cm2 for 5 min, respectively. However, straight pores are formed at anodization current densities of 60 mA/cm2, and 75 mA/cm2 for 5 min, respectively. The electron emission characteristic of porous silicon ballistic electron emission sources is measured in vacuum. The results show that electrons emitted into the vacuum from the porous silicon samples with disordered pores. Under a bias condition, injected electrons from the substrate are accelerated by the strong electric field on the surfaces of the Si nanocrystallites in disordered pores, and then emitted into the vacuum through Pt film. However, no electron emission is observed in porous silicon samples with straight pores. It attributes to the lack of Si nanocrystallites in straight pores. So there is not accelerating tunnels enough for electrons. According to disordered or straight pores, we can estimate whether PS samples emit electrons or not.     

CO2 and H2 detection with a CHx/porous silicon-based sensor

There has been great interest in the last years in gas sensors based on porous silicon (PS). Recently, a gas sensing device based on a hydrocarbon CH_x/porous silicon structure has been fabricated. The porous samples were coated with hydrocarbon groups deposited in a methane argon plasma. We have experimentally demonstrated that the structure can be used for detecting a low concentration of ethylene, ethane and propane gases [Gabouze N, Belhousse S, Cheraga H. Phy State Solidi (C), in press].In this paper, the CH_x/PS/Si structure has been used as a sensing material to detect CO₂ and H₂ gases. The sensitivity of the devices, response time and impedance response to different gas exposures (CO₂, H₂) have been investigated.The results show that current-voltage and impedance-voltage characteristics are modified by the gas reactivity on the PS/CH_x surface and the sensor shows a rapid and reversible response to low concentrations of the gases studied at room temperature.     

Microwave based nanogenerator using the ratchet effect in Si/SiGe heterostructures

Ratchet based microwave current generators and detectors were developed in Si/SiGe heterostructures for wireless communication with the possibility of extending the detection limit to the terahertz range. A microwave induced ratchet current was generated in the two-dimensional electron gas by patterning an array of semicircular antidots in hexagonal geometry. The spatial asymmetry created by the semicircular antidots forces the electrons under the influence of the microwave electric field to move preferentially towards the direction of the semidisc axis. A photovoltage of the order of few millivolts was observed. Such a photovoltage was completely absent in a symmetric system consisting of circular antidots. The induced photovoltage increased monotonically with microwave power and was found to be independent of the microwave polarization. This device opens the possibility of employing silicon based heterostructures for nanogenerators and other wireless communication devices using microwaves.