纳米TiO_2/SiO_2的制备与表征及其光催化活性的研究

针对二氧化钛(TiO2)纳米颗粒极易团聚、分散性差的问题,以提高TiO2分散稳定性与光催化活性为目的,采用并流中和法,以锐钛矿型纳米TiO2粉体为载体,硅酸钠(Na2SiO3)为包覆剂,使用硫酸(H2SO4)调节pH值,在纳米TiO2表面包覆致密的氧化硅(SiO2)膜。借助Fourier变换红外光谱(FTIR),X射线能量散射谱(EDS)和场发射扫描电子显微镜(FESEM)表征样品的键合情况、表面化学成分、分散性,同时借助紫外-可见分光光度计(UV-Vis Spectrophotometer)以亚甲基蓝的光催化降解反应对其光催化活性进行评价。FTIR和EDS结果表明:采用该包覆法后,SiO2以化学键合的方式沉积在纳米TiO2表面,在包覆层和纳米TiO2颗粒之间的界面上形成了Ti—O—Si键。SEM结果表明:TiO2/SiO2纳米复合粒子分散均匀,无严重团聚和大块堆积现象。光催化实验结果表明:以SiO2表面包覆后的TiO2颗粒光催化活性明显高于纯TiO2。     

环境净化功能TiO2/SiO2复合纳米粉体的制备与表征

以锐钛矿型TiO2纳米粉体为载体,Na2SiO3为包覆剂,H2SO4为中和剂,采用溶胶-凝胶法制备了系列环境净化功能TiO2/SiO2复合纳米粉体.用XRD、XRF、TEM、BET比表面分析对其进行了表征,并以亚甲基蓝溶液的光催化降解率和COD去除率为指标评价了其光催化活性.结果表明,在TiO2纳米颗粒表面包覆一层多孔非晶态水合二氧化硅纳米膜,可以显著提高其水分散性,有效控制其光催化活性,进而提高了涂料的抗老化性和耐候性.中和时间对包硅效率影响较大,适当增加中和时间有利于提高包硅效率;包覆温度对包硅效率影响较小,升高温度使包硅效率略有降低.低温包覆,成膜相对疏松,改性粉体的光催化活性相对较高;高温包覆,成膜相对致密,改性粉体的光催化活性相对较低.     

ZnO/Al_2O_3复合纳米颗粒的制备与表征

为研究ZnO/Al2O3复合纳米颗粒在涂料、化妆品等领域的应用,采用直接沉淀法制备了纳米ZnO,用硫酸铝水解生成的Al2O3对纳米ZnO进行了表面改性。采用IR、TEM、SEM、XRD等手段对改性前后的粉体进行表征。分析结果表明,改性后粉体颗粒的团聚现象减轻。粉体的光催化降解甲基橙的实验研究表明,改性后ZnO粉体的光催化活性明显下降,进一步证明纳米ZnO颗粒表面存在Al2O3的包覆层。     

ZnO/Al2O3复合纳米颗粒的制备与表征

以硫酸锌和氢氧化钠为原料,采用直接沉淀法制备了纳米氧化锌,并用硫酸铝水解生成的三氧化铝对钠米氧化锌进行了表面改性,并采用IR、TEM、SEM、XRD等手段对改性前后的粉体进行表征研究.TEM和SEM分析结果表明,改性后粉体颗粒的粒径小、团聚现象减轻.此外,进行了粉体的光催化降解甲基橙的实验研究.实验结果表明,改性后ZnO粉体的光催化活性明显下降,这进一步证明了纳米氧化锌颗粒表面存在三氧化二铝的包覆层.     

ZnO/Al2O3复合纳米颗粒的制备与表征

以硫酸锌和氢氧化钠为原料,采用直接沉淀法制备了纳米氧化锌,并用硫酸铝水解生成的三氧化铝对钠米氧化锌进行了表面改性,并采用IR、TEM、SEM、XRD等手段对改性前后的粉体进行表征研究.TEM和SEM分析结果表明,改性后粉体颗粒的粒径小、团聚现象减轻.此外,进行了粉体的光催化降解甲基橙的实验研究.实验结果表明,改性后ZnO粉体的光催化活性明显下降,这进一步证明了纳米氧化锌颗粒表面存在三氧化二铝的包覆层.     

用于合成纳米苯丙乳液的纳米TiO2表面改性及表征

研究了利用硅烷偶联剂改性纳米TiO2的方法,并通过FTIR、TEM等手段表征化学改性产物的结构和改性后纳米二氧化钛的分散性,结果表明偶联剂与二氧化钛表面发生化学偶联反应,使二氧化钛表面被偶联剂包覆,从而使二氧化钛改性产物在有机物中具有良好的分散性能.通过TEM分析用改性后的纳米TiO2原位合成的纳米TiO2/苯丙乳液复合体系具有以纳米TiO2粒子为核,以聚合物为壳的核壳结构,该乳液涂膜的耐水性达120h不泛白,硬度为H级,明显优于非纳米苯丙乳液,且具有很好的抑菌作用,可用于制备纳米水性涂料.     

硅烷偶联剂对纳米二氧化钛表面改性的研究

利用硅烷偶联剂（KH-570）对表面包覆氧化硅的金红石相纳米TiO2进行了有机表面改性．采用红外光谱（IR）、X射线光电子能谱（XPS）、热分析（TG-DTA）、透射电镜（TEM）和润湿性实验等分析手段对表面改性前后的纳米TiO2进行了表征．红外光谱和X射线光电子能谱表明，KH-570以化学键合的方式结合在纳米TiO2的表面，并形成了有机包覆层．经测量，纳米TiO2表面包覆的KH-570的质量分数约为7．42％-8．59％．润湿性实验显示，经KH-570表面改性的纳米TiO2具有疏水性．力学性能实验表明，经KH-570表面改性的纳米TiO2能同时提高复合材料的强度和韧性．     

纳米TiO2表面无机/有机复合改性研究

用液相沉积法对纳米TiO2进行了表面无机/有机复合改性.用XRD、FT-IR进行了包覆膜结构表征,用TEM观察改性后颗粒的形态.测量了有机包覆量对改性样品亲油性的影响.结果表明,液相沉积并经105℃烘干得到的Al2O3膜为非晶态结构,煅烧后才能晶化;有机膜可以在无机膜上生成,其最大包覆量约为7%,且与包覆温度无关;复合包覆后纳米颗粒外形不变,分散性提高;有机包覆量对纳米TiO2的亲油性有非线性影响,包覆量为1.2%时其亲油性最好.     

氧化钛基光催化材料的离子掺杂和酸化改性

本文基于光催化反应的机理分析,采用了金属离子掺杂和表面酸化相结合的改性方法对TiO2颗粒做了优化处理.对改性后的样品利用XRD、FTIR和PL等测试技术对样品进行了表征并以亚甲基兰为模拟污染物进行了光催化降解实验.结果表明包覆在粉体表面的新相以金红石为主;Fe离子掺杂降低了光生电子和空穴的复合几率;表面酸化增加了TiO2表面以双齿桥方式配位的羟基,此种羟基对TiO2光催化活性有重要影响;铁离子掺杂和表面酸化协同的改性方法可以明显提高TiO2粉体的光催化活性.     

高活性纳米二氧化钛的制备、表征及光催化性能

采用改进的钛醇盐水解法制备了高活性的纳米TiO2,并通过光催化降解甲胺磷来表征其光催化活性.IR、DTA、TG、XRD、TEM、BET、XPS等分析表明TiO2的光催化活性必须用其晶型、结晶度、粒径大小、比表面积、表面羟基等综合起来评价.本研究认为影响光催化活性的最主要因素是结晶度.     

Enthalpy and heat capacity of the actinide oxides

The available enthalpy data on UO₂, ThO₂, PuO₂, (Th, U)O₂, and (Pu, U)O₂ have been analyzed and equations have been derived to fit the data. Phase transitions were found in UO₂, ThO₂, (Th, U)O₂, and (Pu, U)O₂. The high temperature PuO₂ data were too scattered to determine whether a phase transition exists. Above the phase transition temperature, the enthalpy data were fit with a linear equation. Enthalpy data for PuO₂ and ThO₂ below the phase transition temperature were fit with two-term equations whose contributions are due to phonons and thermal expansion. For UO₂ below its phase transition, a term for an electronic contribution was added to this basic equation. Below the phase transitions for (Th, U)O₂, enthalpy data were fit by a mole average of the equations used to fit the ThO₂ and UO₂ data below their phase transitions; however, the mole average equation was not valid for 90 and 92% ThO₂ in the mixed oxide. Since it was found that mole averages of the PuO₂ and UO₂ data do not fit the (Pu, U)O₂ data, these data were fit with an equation of the same form as that that used for UO₂.     

Nitrogen dioxide gas sensors based on titanium dioxide thin films deposited on langasite

Conductometric sensors, based on pure and Au-doped TiO₂ thin films on langasite (LGS) substrates have been investigated for detecting low concentrations (510 ppb and 1060 ppb) of NO₂ in synthetic air at a temperature range between 220 °C and 320 °C. Thin films of TiO₂ were deposited using the radio frequency (RF) magnetron sputtering method. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques were employed for the characterization of thin films. It was observed that the Au-doped TiO₂ sensor has fast response and recovery time of 10 and 29 s respectively towards 510 ppb of NO₂ at 273 °C.     

SiO2-WO3-TiO2三元表面协同型光催化剂的性能研究

以溶胶-凝胶法制得的TiO2为主体,利用H4SiW12O40浸渍烧结法成功地制备了三元表面协同型SiO2-WO3-TiO2光催化剂。采用TGA-DTA、TEM、BET、XRD、FT-IR对该催化剂进行了结构表征。以酸性品红AF水溶液为降解处理对象,考察了SiO2-WO3-TiO2光催化剂的催化活性。结果表明:SiO2-WO3-TiO2光催化剂与TiO2相比,光催化活性有明显的提高。     

Film morphology modification in ion-assisted glancing angle deposition

Porous structured films grown with the glancing angle deposition technique have been widely studied for thin film optical device applications. We report the use of ion assistance to modify the structural and optical properties of porous silicon dioxide and titanium dioxide columnar thin films grown at deposition angles of 70° and 85°. Optical characterization studies show that tilted columnar structures will undergo an increase in tilt angle and film density with increasing ion dose. These two trends contrast with unassisted films where film density and column tilt angle are primarily controlled by the deposition angle. Thus, a regime of film structures simultaneously exhibiting high film density and large column tilt angle is enabled by incorporating an ion-assisted process. The phisweep substrate motion algorithm for minimizing columnar anisotropy used in conjunction with ion-assisted deposition provides additional control over film morphology and expands the utility of this modified fabrication process.     

Role of surface properties of MoO3-doped SnO2 thin films on NO2 gas sensing

The role of surface morphology of MoO₃-doped SnO₂ thin film on the gas sensing properties is analyzed. SnO₂ thin films doped with 1, 3, 5 and 10 wt% MoO₃ are prepared by sol-gel spin coating process. Structural and morphological properties are studied using glancing angle X-ray diffractometer, atomic force microscopy, transmission electron microscopy and high resolution transmission electron microscopy. Energy dispersive X-ray analysis and X-ray photoelectron spectroscopy studies are used for chemical analysis. A good correlation is found between the characteristics of the surface and gas sensing properties of these films. MoO₃ addition is found responsible for increase in acidic nature of films which in turn increases their sensitivity and selectivity towards NO₂ gas.     

TiO_2-SnO_2纳米粉体的制备与研究

采用水热法制备了TiO2-SnO2纳米粉体。利用X射线衍射(XRD)和透射电镜(TEM)对其微观结构进行了表征,并利用X射线能谱(EDS)研究了不同原料配比制备的TiO2-SnO2纳米粉体中的元素含量。结果表明:TiO2-SnO2纳米粉体结晶尺寸较小,有明显的团聚现象;TiO2-SnO2纳米粉体中Sn元素的含量高于原料中的含量。     

PbO2-MnO2共沉积电化学行为研究

采用旋转圆盘电极(Rotating disk electrode,RDE),通过循环伏安法(Cyclic voltammetry,CV)分析了硝酸锰浓度、硝酸浓度、硝酸铅浓度和溶液温度对PbO_2和MnO_2共沉积的影响规律,获得了PbO_2和MnO_2共沉积的最优条件。探究了旋转圆盘电极转速对PbO_2和MnO_2共沉积的影响,发现最优条件下其共沉积行为主要受电化学控制。使用扫描电镜(Scanning electron microscope,SEM)观察PbO_2-MnO_2沉积层表面形貌,发现PbO_2-MnO_2沉积层表面以圆球状结构为主。通过X射线衍射仪(X-ray diffraction,XRD)检测到PbO_2-MnO_2沉积层表面出现了一种α-MnO_2、α-PbO_2、β-PbO_2三相同时存在的混合结晶状态。     

Photoreduction of CO2 by TiO2 nanocomposites synthesized through reactive direct current magnetron sputter deposition

The photoreduction of CO₂ into methane provides a carbon-neutral energy alternative to fossil fuels, but its feasibility requires improvements in the photo-efficiency of materials tailored to this reaction. We hypothesize that mixed phase TiO₂ nano-materials with high interfacial densities are extremely active photocatalysts well suited to solar fuel production by reducing CO₂ to methane and shifting to visible light response. Mixed phase TiO₂ films were synthesized by direct current (DC) magnetron sputtering and characterized by X-ray diffraction (XRD), atomic force microscope (AFM), scanning electron microscope (SEM) and transmission electron microscope (TEM). Bundles of anatase-rutile nano-columns having high densities of two kinds of interfaces (those among the bundles and those between the columns) are fabricated. Films sputtered at a low deposition angle showed the highest methane yield, compared to TiO₂ fabricated under other sputtering conditions and commercial standard Degussa P25 under UV irradiation. The yield of methane could be significantly increased (~ 12% CO₂ conversion) by increasing the CO₂ to water ratio and temperature (< 100 °C) as a combined effect. These films also displayed a light response strongly shifted into the visible range. This is explained by the creation of non-stoichiometric titania films having unique features that we can potentially tailor to the solar energy applications.     

N掺杂TiO2/SiO2双层中空微球的制备及可见光光催化活性研究

以阳离子PS为模板,正硅酸乙酯和钛酸丁酯为前驱体,三乙胺为氮源,采用溶胶-凝胶法,通过层层静电自组装制备了N掺杂TiO2/SiO2 (N-TS)复合微球,并经高温焙烧得到具有介孔结构的N-TS双层中空微球.采用Zeta-plus激光粒度及电位仪、SEM、XRD、UV-Vis等对微球的结构进行表征,以亚甲基蓝为目标污染物,考察了N-TS双层中空微球的可见光光催化活性.结果表明,通过SiO2和TiO2的交替包覆形成了双壳层结构,保持了中空微球完整的球形形貌;N的掺入有效拓宽了TiO2光响应范围且在可见光区域吸收明显增强,在掺N量为n(N) /n(Ti)=10、500℃焙烧得到的双层中空微球可见光催化活性最优,2h内亚甲基蓝几乎完全降解,同时中空微球在重复使用过程中依然能保持较高的可见光光催化活性.     

二氧化碳中的磷烷分析

介绍了二氧化碳中的磷烷分析。