金红石型TiO2纳米棒的制备及其在染料敏化太阳电池中的应用

采用十二烷基苯磺酸钠表面活性剂(DBS)辅助水热法合成TiO2纳米材料,XRD和TEM测试表明,不含DBS的TiO2溶胶水热处理后得到10~20nm锐钛矿型TiO2纳米颗粒;添加DBS后,生成了金红石型TiO2纳米棒.虽然金红石型TiO2纳米棒光电极的染料吸附性能和光电性能均不如锐钛矿型TiO2纳米颗粒光电极,但金红石型TiO2纳米棒漫反射性能较高.可用其制备具有光电转换性能的反射层,这种新型反射层使染料敏化太阳能电池光电转换效率提高了26.14%,而含Ti-nanoxide 300大颗粒TiO2构成的反射层仅能使电池光电转换效率提高11.04%.这种差异的根源在于金红石型TiO2纳米棒不仅具有散射光能力,其本身还可吸附染料进行光电转换.随着反射层厚度的增加,电池短路电流逐步提高.而不吸附染料且无光电转换能力的Ti-nanoxide 300传统反射层则没有这种功能.     

丙烯酸表面修饰法制备纳晶TiO2薄膜的研究

采用sol—gel法制备纳晶TiO2薄膜，在溶胶的制备过程中加入丙烯酸对纳米TiO2胶体颗粒进行表面修饰。溶胶的透射电镜(TEM)分析表明，丙烯酸的表面修饰作用可以抑制在制备和陈放过程中胶体颗粒的团聚。采用原位程序升温，使用X射线衍射仪(XRD)对TiO2粉体由锐钛矿向金红石的转变过程(A→R)进行了考察，结果显示，晶粒的迅速生长和晶型的转变有着密切的联系；此外，丙烯酸的修饰作用能显著提高A→R的温度，且有助于抑制热处理过程中纳晶TiO2颗粒的团聚。TiO2薄膜的原子力显微照片(AFM)表明，丙烯酸修饰法制备的TiO2薄膜，膜层均匀连续，颗粒为纳米尺度。     

硬脂酸对纳米TiO2有机表面修饰方法的研究

报道了一种利用硬脂酸对纳米TiO2进行有机表面修饰的新方法,主要包括纳米TiO2水分散液的制备和把纳米TiO2粒子由水分散液中转移到溶有硬脂酸的甲苯溶液中两个过程.采用红外光谱(FT-IR)、X射线光电子能谱(XPS)、热分析(TG-DTA)、透射电镜(TEM)、粒度分布、紫外-可见光谱和分散性实验等对所得的样品进行了...     

紫外诱导水相条件下Ag修饰TiO2纳米棒的制备及光催化性能

利用贵金属修饰氧化钛被认为是提高氧化钛光催化效率的重要途径。本文提出了一种新的制备方法,利用紫外光诱导还原作用,在水相体系中不使用表面活性剂合成Ag修饰TiO2纳米结构。首先,Ti(SO4)2水解能得到分散良好的锐钛矿相TiO2纳米棒。在TiO2纳米棒合成过程中,利用紫外光的诱导还原作用即可得到Ag/TiO2纳米结构。透射电镜显示Ag修饰TiO2纳米结构是由20～30nm的TiO2纳米棒和10nm左右的Ag"纳米头"组成。对亚甲基蓝的光降解实验证明,Ag/TiO2纳米结构相比纯TiO2在可见光和模拟太阳光下光催化性能分别提高了31倍和3倍。因此,此法合成的Ag/TiO2可被开发用作降解污染物的有效催化剂。     

PyDDP修饰纳米硼酸镧极压剂制备及性能研究

采用三步工艺合成了表面修饰剂二烷基二硫代磷酸吡啶(PyDDP),优化确定了PyDDP制备工艺条件,并利用红外光谱确认了其结构.将合成的PyDDP应用于硼酸镧表面修饰,并优化了合成的工艺参数.采用IR、TG-DTA、XRD等分析方法,对这3种表面修饰剂修饰的纳米微粒进行了表征.通过四球实验研究了所制备微粒的极压性能,并通过SEM、EDXA等方法对钢球表面的形貌、钢球表面存在的元素进行了分析.结果表明,以PyDDP为表面修饰剂获得了粒径约10 nm的PyDDP修饰的硼酸镧纳米微粒,其最大无卡咬负荷为745 N,并在蚀球表面发现了稀土元素.对PyDDP修饰硼酸镧结构与材料极压性能之间的关系进行了分析,指出稀土渗透层和稀土摩擦催渗硼的作用是该材料具有良好极压性能的主要原因.     

PyDDP表面修饰纳米硼钼剂的制备及极压性能研究

以二烷基二硫代磷酸吡啶（PyDDP）为表面修饰剂, 分别制备了PyDDP表面修饰纳米硼酸镧和PyDDP表面修饰纳米二硫化钼, 并将两者复配制备了PyDDP表面修饰纳米硼钼剂. 采用IR、XRD、TEM等分析方法对表面修饰纳米微粒进行了表征. 结果表明, 纳米硼钼剂由硼酸镧和二硫化钼微粒组成, 粒径在30～50nm之间. 通过四球试验研究了PyDDP表面修饰纳米硼钼剂的摩擦学性能, 并利用SEM、EDXA、XPS等方法对蚀球表面形貌和表面元素进行了分析. 结果表明, PyDDP表面修饰纳米硼钼剂具有较好的极压抗磨性能, 表面元素在摩擦副表面形成无机化学反应膜是具有良好的极压性能的主要原因.     

TiO2微球级次结构的制备及其光催化降解甲基橙活性

在正辛醇体系中,通过溶剂热反应制备出表面具有超细纳米棒的TiO2微米球,通过X射线衍射确定了产品的物相和组成为金红石结构的TiO2,通过扫描电镜和透射电镜对样品的外观形貌、大小以及表面结构进行了观察,利用差热-热重分析仪对样品的固含量进行了测量,最后利用所制备的TiO2微米球催化剂降解水溶液中的甲基橙,结果显示其具有较快的光催化速度     

硬脂酸对CeO2纳米粒子的表面修饰研究

利用表面修饰法合成了硬脂酸修饰的 CeO2 纳米粒子,采用透射电子显微镜(TEM)观察了经表面修饰的CeO2 纳米粒子的形貌及分散性,并采用红外光谱(IR)、紫外可见分光光度计等对修饰的CeO2 纳米粒子进行了表征。结果表明:表面修饰剂硬脂酸与 CeO2 纳米粒子表面之间发生了化学键合作用;修饰后的CeO2 纳米粒子表面存在疏水有机基团,阻隔了 CeO2 纳米粒子的团聚,起到了分散作用;同时,修饰后的CeO2 纳米粒子在苯乙烯中的稳定性得到了提高。并且获得了硬脂酸的修饰量与CeO2 纳米粒子的最佳配比。     

水杨酸原位表面改性纳米TiO2的制备及性能研究

通过控制四氯化钛(TiCl4)的水解速度,制备出水杨酸(SA)原位表面修饰的TiO2纳米颗粒(TiO2/SA).通过X射线衍射仪(XRD),高分辨透射电子显微镜(HRTEM),红外光谱仪(FT-IR),热分析(TG-DTA)和X射线光电子能谱(XPS)等实验分析手段对表面改性前后的TiO2纳米颗粒进行了表征,结果表明表面修饰水杨酸的TiO2纳米颗粒在乙醇中有良好的分散性,将TiO2/SA加入到光信息存储薄膜材料(PVA/AM)中,能大大提高材料的衍射效率,降低布拉格偏移.     

溶剂和修饰剂对化学法合成Bi-Sb-Te纳米晶尺寸和形貌的影响

采用简单的水热/溶荆热法合成了纳米结构的Bi0.5Sb1.5Te3晶粒,通过改变溶剂种类和表面修饰剂的添加量可以实现对Bi0.5Sb1.5Te3纳米晶体的尺寸和形貌的控制.当表面修饰剂的浓度较小时,合成的Bi0.5-Sb1.5Te3晶粒只有数十纳米,有望为高性能的纳米结构块体热电材料提供原始粉末.产物的颗粒尺寸减小和片状形貌的获得,可能是生成物的合成速率减缓和表面修饰剂选择性吸附所致.     

Controlled fabrication of TiO2 rutile nanorod/anatase nanoparticle composite photoanodes for dye-sensitized solar cell application

We present a straightforward procedure to prepare composite photoanodes which consisted of TiO2 rutile nanorods/anatase nanoparticles synthesized under hydrothermal conditions, with the ratio of rutile to anatase controlled simply by adjusting the volume of nitric acid. The as-prepared TiO2 composites exhibited high specific surface area, light-scattering effect, and good crystallinity. The dye-sensitized solar cells (DSCs) using the TiO2 composites showed higher short-circuit photocurrent and overall conversion efficiency than the DSC from pure-anatase nanoparticles. The highest conversion efficiency was achieved from the DSC based on TiO2 nanocomposites with 24 wt% rutile nanorods, which was attributed to improved light harvesting caused by the enhancement of specific surface area and scattering effect from rutile nanorods.     

Growth of TiO2 Nanorods by Sol-gel Template Process

In this work, TiO2 nanorods with uniform diameter of about 100 nm and a length of several micrometers were successfully prepared by the sol-gel template method. Also the influence of molar ratios of precursor on the morphology and structure of TiO2 nanorods has been investigated. The prepared samples were characterized by Fourier transform infrared spectroscopy （FTIR）, X-ray diffraction （XRD） and scanning electron microscopy （SEM）. The XRD results indicated that the TiO2 nanorods were crystallized in the anatase and rutile phases, after annealing to 400-700℃ up to 2 h.     

酸在制备金红石型纳米TiO2中的作用

以成本低廉的偏钛酸和浓硫酸为起始反应物,采用水热合成法进行了纳米金红石型TiO2的合成研究.研究了制备过程中浓硫酸对偏钛酸的溶解情况,以及水热反应的pH值对TiO2晶型转变的影响.结果表明:只有当偏钛酸完全溶解,并且水热反应时的pH小于等于0.4时,才能制得纯相的金红石型TiO2.     

Phase-pure TiO(2) nanoparticles: anatase, brookite and rutile

We report on the synthesis of phase-pure TiO(2) nanoparticles in anatase, rutile and brookite structures, using amorphous titania as a common starting material. Phase formation was achieved by hydrothermal treatment at elevated temperatures with the appropriate reactants. Anatase nanoparticles were obtained using acetic acid, while phase-pure rutile and brookite nanoparticles were obtained with hydrochloric acid at a different concentration. The nanomaterials were characterized using x-ray diffraction, UV-visible reflectance spectroscopy, dynamic light scattering, and transmission electron microscopy. We propose that anatase formation is dominated by surface energy effects, and that rutile and brookite formation follows a dissolution-precipitation mechanism, where chains of sixfold-coordinated titanium complexes arrange into different crystal structures depending on the reactant chemistry. The particle growth kinetics under hydrothermal conditions are determined by coarsening and aggregation-recrystallization processes, allowing control over the average nanoparticle size.     

Effects of TiO2 nanorod length and post-annealing on the electrical properties of TiO2 nanobarbed fiber structures

TiO2 nanobarbed fiber (NBF) structures consisting of TiO2 nanorods (NRs) on TiO2 nanofibers (NFs) were fabricated. The mean length and diameter of the TiO2 NRs grown for 6 h was 1.38 microm and 71 nm, respectively. One NR was connected to other NRs and the junction points between the TiO2 NRs increased with increasing TiO2 NR length. The crystal structure of the TiO2 NFs and NRs was rutile and anatase, respectively. After post-annealing, only the intensity of the TiO2 NBF peaks increased without any significant structural changes. Raman spectroscopy showed that the TiO2 NBF structure consisted of anatase (TiO2 NFs) and rutile (TiO2 NRs). The bandgap of the TiO2 NBF structure prepared during a TiO2 NR growth time from 0 to 6 h decreased from 3.23 eV to 3.10 eV. The conductivity of the TiO2 NBFs with longer NRs was enhanced by post-annealing.     

Template-free formation of vertically oriented TiO2 nanorods with uniform distribution for organics-sensing application

High-density arrays of vertically oriented TiO(2) nanorods with uniform distribution on Ti foil have been formed through template-free oxidation of Ti in hydrogen peroxide solutions. Subsequent thermal treatment was applied for growing mixed crystal structures to pursue higher performance. Morphology characterization using field emission scanning electron microscopy (FESEM) shows a nanorod diameter in the range of 20-50 nm with a length of 1.5 μm. X-ray diffraction (XRD) measurement demonstrates the crystallization of the TiO(2) nanorods prior to thermal treatment and the formation of anatase and rutile mixed phase after thermal treatment. The mixed crystal TiO(2) nanorods show a much higher performance than pure anatase in photoelectrochemical experiments. Steady-state photocurrent resulted from photocatalytic oxidation of organic compounds by TiO(2) nanorods is employed as response signal in determination of the organics to yield a linear range of 0-1.1mM for glucose. For other organics, an excellent linear relationship between the net steady-state photocurrent and the concentration of electrons transferred in exhaustive oxidation for these organics is obtained, which empowers the mixed crystal TiO(2) nanorods to serve as versatile material in organics-sensing application.     

钛酸盐一维纳米材料向TiO2纳米材料的水热转化研究

采用强碱性水热处理法分别控制第一次水热反应为160℃和200℃,制备出一维纳米管和纳米棒2种形貌的产物,将其作为第二次水热反应的前驱体,考察了第二次水热体系中pH值和温度对TiO2纳米材料的晶相组成及其微观形貌的影响;采用XRD、TEM以及HRTEM对样品进行了分析.结果表明,当以纳米管为前驱体时,除在pH=0的体系中得到了以金红石相为主的单晶纳米棒外,在pH值为2、4和7的条件下均得到了单晶纯锐钛矿相TiO2纳米颗粒.当以纳米棒为前驱体时,在pH=0的体系中得到了金红石相与板钛矿相共存的纳米棒和纳米颗粒混合产物;在pH值为2、4和7的条件下均得到了纯锐钛矿相TiO2纳米棒;当二次水热温度低于180℃时,前驱体没有转化完全,所得产物为前驱体与锐钛矿相TiO2共存的纳米棒;当水热温度为180℃和210℃时,产物为纯锐钛矿相纳米棒.     

酸-水热法辅以水热温度对钛材生物活性的影响

为提高医用钛材的生物活性,通过酸-水热复合法在其表面设计并制备了TiO_2纳米棒,探讨水热温度对钛表面TiO_2纳米棒形成的影响,然后对试样进行模拟体液生物活性实验,采用扫描电子显微镜(SEM)、能谱仪(EDS)和X射线衍射仪(XRD)分析手段研究了钛表面生成产物的形貌、元素组成和物相组成.结果表明:随着水热温度的增加,二氧化钛层的表面形貌发生改变,从片状到棒状,之后纳米棒发生团聚;试样中金红石相和锐钛矿相的衍射峰强度随水热温度的增加而增强;水热温度为130℃时,钛表面可以形成尺寸均匀、长度基本一致的TiO_2纳米棒,其厚度、长度和直径分别为2.5μm、150 nm和10 nm,且纳米棒是由锐钛矿型和金红石型TiO_2的混合相组成.模拟体液生物活性实验后,水热处理后材料表面有富含Ca、P的羟基磷灰石生成,而羟基磷灰石的形成主要与纳米棒的形成和膜层的厚度有关.其中,水热温度为130℃时形成的纳米棒结构较好,膜层较厚,其表面诱导磷灰石沉积的含量最多,具有较好的生物活性.     

Optimized method for preparation of TiO2 nanoparticles dispersion for biological study

The objective of the present study was to develop a practical method to prepare a stable dispersion of TiO2 nanoparticles for biological studies. To address this matter a variety of different approaches for suspension of nanoparticles were conducted. TiO2 (rutile/anatase) dispersions were prepared in distilled water following by treated with different ultrasound energies and various dispersion stabilizers (1.0% carboxymethyl cellulose, 0.5% hydroxypropyl methyl cellulose K4M, 100% fetal bovine serum, and 2.5% bovine serum albumin). The average size of dispersed TiO2 (rutile/anatase) nanoparticles was measured by dynamic light scattering device. Agglomerate sizes of TiO2 in distilled water and 100% FBS were estimated using TEM analysis. Sedimentation rate of TiO2 (rutile/anatase) nanoparticles in dispersion was monitored by optical absorbance detection. In vitro cytotoxicity of various stabilizers in 16-HBE cells was measured using MTT assay. The optimized process for preparation of TiO2 (rutile/anatase) nanoparticles dispersion was first to vibrate the nanoparticles by vortex and disperse particles by ultrasonic vibration in distilled water, then to add dispersion stabilizers to the dispersion, and finally to sonicate the nanoparticles in dispersion. TiO2 (rutile/anatase) nanoparticles were disaggregated sufficiently with an ultrasound energy of 33 W for 10 min. The formation of TiO2 (rutile/anatase) agglomerates in distilled water was decreased obviously by addition of 1.0% CMC, 0.5% HPMC K4M, 100% FBS and 2.5% BSA. For the benefit of cell growth, FBS is the most suitable stabilizer for preparation of TiO2 (rutile/anatase) particle dispersions and subsequent investigation of the in vivo and in vitro behavior of TiO2 (rutile/anatase) nanoparticles. This method is practicable to prepare a stable dispersion of TiO2 (rutile/anatase) nanoparticles for at least 120 h.     

Surface modified TiO2 nanostructure with 3D urchin-like morphology for dye-sensitized solar cell application

Three-dimensional (3D) urchin-like rutile TiO2 powders were synthesized by a mild hydrothermal method without any templates. An individual urchin-like TiO2 powder consists of self-assembled nanorods with a length of about 150 nm and width of about 10 nm. Additionally, the urchin-like TiO2 nanopowders were coated with an ultra-thin ZnO layer in order to modify the surface properties of the nanopowders, and the ZnO layer was confirmed by high-resolution transmission electron microscopy (HRTEM) and X-ray photoelectron spectroscopy (XPS) analysis. The ZnO-modified TiO2 was used as a photoelectrode of a dye-sensitized solar cell (DSSC) and the solar cell performances were investigated. In comparison with bare TiO2, ZnO-modified TiO2 improved the photovoltaic performances, i.e., energy conversion efficiency, open circuit voltage, and short circuit current were increased. The higher DSSC performance of ZnO-modified TiO2 was attributed to its higher dye loading and lower charge recombination rate.