Synthesis and characterization of TiO2 powders by electrospray pyrolysis method

Electrospray pyrolysis, i.e. combination of electrospray and in-flight thermal treatment, has attracted much attention as a preparation method of functional ceramic particles. In this paper, we report the processing detail of spherical TiO₂ nano- and microparticles by the electrospray pyrolysis method as well as their photocatalytic activity for hydrogen evolution. Titanium(IV) bis(ammonium lactato)dihydroxide aqueous solutions (TALH aq., 0.2–20 wt%) were injected into a capillary nozzle by a syringe pump (0.15–0.59 mL/min), and were electrosprayed by using DC 4 kV voltage, followed by the pyrolysis at 300–500 °C. Spherical TiO₂ nano- and microparticles were successfully obtained. Effects of precursor-liquid concentration, liquid flow-rate, and pyrolysis temperature on the particle size, microstructure and functions were discussed.     

均匀沉淀法工业生产纳米二氧化钛

介绍了以硫酸法钛白生产过程中的中间产物硫酸氧钛为原料,采用直接沉淀法和均匀沉淀法制备纳米TiO2的工艺路线,通过对2种制备工艺及几种中试方案的比较,提出了纳米TiO2工业化生产的原料与技术路线,并指出在的问题及解决方法。     

用反萃界面沉淀法制备二氧化钛超细粉体

用反萃界面沉淀法,以氨水为反萃剂,通过优化煅烧温度和反萃条件制备出超细TiO2光催化剂.结果表明,采用反萃沉淀法制备超细TiO2光催化剂,改变煅烧温度和水油相加入的方式、降低氨水的浓度、制备温度和陈化时间等因素均有显著的影响.用氨水反萃制备纳米TiO2其最佳煅烧温度为350℃,氨水的浓度和陈化温度存在最佳值.氨水浓度(体积比)为1:5,陈化温度为17.5℃有利于生成小颗粒;陈化时间较短和将水相加入油相有利于生成小颗粒.     

Preparation of Fe2O3/Al composite powders by homogeneous precipitation method

The Fe₂O₃/Al composite powders were prepared by homogeneous precipitation method. The influence of the concentration of Fe²⁺ and the molar ratio of raw materials on the preparation of Fe₂O₃/Al composite powders were investigated. X-ray diffractometer, scanning electron microscope, Fourier transform infrared spectroscopy and differential thermal analysis were used to analyze the morphology and structure of the Fe₂O₃/Al composite powders. The results show that the content of iron oxide in the composite powders could be effectively controlled by adjusting the concentration of Fe²⁺ and the molar ratio of raw materials in the plating solution. The surface of Al particle was coated with a layer of thick and dense iron oxide. The core-shell Fe₂O₃/Al composite powders with Fe₂O₃ content of 14.1% were produced, the coating efficiency of Fe₂O₃ reaches more than 77%. The iron oxide, which coated on the surface of the aluminium particle is flower-like cluster structure, each flower-like cluster is constituted by nano-flaky iron oxide.     

均匀水解低温晶化法氮掺杂TiO_2可见光催化剂的制备与表征

以硫尿为氮源,采用均匀水解低温晶化法制备了具有可见光活性氮掺杂的纳米TiO2。采用XRD、SEM、BET和UV-vis漫反射光谱等技术对其进行了表征。结果表明,所制备氮掺杂TiO2均为锐钛矿相,并且在可见光区域有明显的光吸收。以甲基橙溶液为模拟废水,研究氮掺杂TiO2在可见光下的光催化活性。实验表明,所制备的氮掺杂TiO2样品在可见光下具有高的光催化活性,可见光催化活性明显高于商业P25 TiO2光催化剂。     

Precipitation method to prepare conductive F-doped SnO2-coated rutile TiO2 whisker and its application in coating

Journal of Materials Science: Materials in Electronics - In this work, K2Ti4O9 whiskers are prepared by adding a certain amount of NaCl as the whisker reaction slow-release agent. Rutile TiO2...     

非均匀沉淀法制备Cu包覆ZrW2O8复合粉体的研究

通过分部固相法制备ZrW2O8粉体。以ZrW2O8、CuSO4·5H2O（分析纯）和无水Na2CO3（分析纯）为原料，采用非均匀沉淀法制备了Cu包覆ZrW2O8复合粉体，并利用XRD、SEM、EDS测试手段，分析包覆粉的物相和形貌，研究了反应液浓度、表面活性剂、反应液滴加速度等反应条件对包覆效果的影响。研究表明：通过非均匀沉淀法可以制备Cu包覆ZrW2O8复合粉体，其关键是控制反应液的浓度和滴加速度，同时，不同分子量的表面活性剂对包覆前驱体的分散性影响很大．     

纳米氢氧化铜的均匀沉淀法制备及低温热容

使用氨水溶解硫酸铜，加入氢氧化钡沉淀分离硫酸根，所得铜氨清液加热蒸氨得氢氧化铜超细沉淀，沉淀分虽用氨水和无水乙醇洗涤，60℃干燥，放置干燥器中至恒重，XRD，TEM，ICP测定表明，其平均粒径尺寸为45nm，粒度分布范围窄，纯度高，用高粗密全自动量热仪的78－370K温区测定的热容，拟全出热容随温度变化的多项式方程，并对此氨浸新工艺－均匀沉淀法有关的热力学性质进行了讨论。     

TiO2/活性炭复合体的制备及其表征

以活性炭(AC)为载体,采用溶胶-凝胶法制备纳米TiO2/AC复合型催化剂.利用SEM,TG-DTA,XRD,等手段对其组成、结构、尺寸等进行分析和表征,结果表明,该复合材料由碳、钛、氧等3种元素组成,其中TiO2纳米粒子尺寸在2O-50nm之间,比本体TiO2纳米粒子尺寸小;在该纳米复合材料中,活性炭作为载体与TiO2结合牢固,存在着某种化学键,TiO2纳米颗粒间不发生团聚,并且活性炭载体的比表面积变化不大.     

纳米SnO2/TiO2复合颗粒形态结构表征

采用均匀沉淀法在纳米TiO2表面淀积SnO2,利用DTA,XPS,XRD,TEM,HREM等手段分析复合颗粒的形态结构。结果表明该复合颗粒由锐钛矿相TiO2和四方晶系SnO2所组成,TiO2表面SnO2淀积层尺寸为0.5-10nm.     

溶胶-凝胶法制备单相Ca2Co2O5粉体

以Co（N03）2.6H2O，Ca（NO3）2.4H2O为原料，柠檬酸为络合剂，利用溶胶-凝胶法（Sol-gel）制备出Ca2CO2O5粉体。采用TG-DSC、XRD和ESEM等测试方法对干凝胶体的热分解过程、样品的物相以及形貌进行了表征。实验结果表明：干凝胶体在700-900℃煅烧，煅烧2h后均能得到单相的Ca2CO2O5粉体，颗粒尺寸分布均匀，范围在1-2μm。在同一配比浓度、同一煅烧时间下，适当提高煅烧温度有利于Ca2CO2O5晶体的生长。     

Synthesis of ZrO2 and TiO2 nanocrystalline powders by hydrothermal process

In present work, nanocrystalline zirconia and titania were synthesized by hydrothermal treatment of zirconyl ZrO(NO₃)₂ and titanyl TiO(NO₃)₂ nitrates aqueous solutions and amorphous gels of the corresponding hydroxides. The hydrothermal synthesis was performed in a wide range of temperatures (150–250 °C), concentration of starting solutions (0.25–0.5 M) and duration of the process (from 10 min to up to 24 h). The hydrothermal treatment at high pressure about 2.0–4.0 GPa was also carried out. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and BET. Particle sizes, morphology and properties of the products were investigated. The influence of hydrothermal synthesis conditions on ZrO₂ and TiO₂ phase compositions were established.     

Synthesis and characterization of anatase and rutile TiO2 nanorods by template-assisted method

Well-aligned anatase and rutile TiO₂ nanorods and nanotubes with a diameter of about 80–130 nm have successfully been fabricated via sol-gel template method. The prepared samples were characterized by using thermogravimetric (TG) and differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectroscopy (EDS). The XRD results indicated that the TiO₂ nanorods were crystallized in the anatase and rutile phases, after annealing at 400–800 °C for different periods of time from 0.2 to 10 h.     

Preparation of spherical TiO2/SnO2 powders by ultrasonic spray pyrolysis and its spinodal decomposition

Spherical TiO₂/SnO₂ powders were prepared from the TiCl₄-SnCl₄ aqueous solution by ultrasonic spray pyrolysis. The particle size, particle-size distribution and morphology of the powders were studied in relation to concentration of source solutions and reaction temperatures. The width of the compositional undulation induced by spinodal decomposition in the sintered bodies increased with increasing starting particle sizes, which resulted from micro-compositional heterogeneity in the form of a solid solution within a TiO₂/SnO₂ secondary sphere.     

Synthesis of SnO2 nanoparticles through the controlled precipitation route

The controlled precipitation method allowed to the synthesis of SnO₂ with advantageous specific properties, such as size and shape employing an aqueous SnCl₂·2H₂O solution as precursor. Through XRD analyses, the optimum pH value of the solution that yielded the desired product was found to be 6.25. After a thermal treatment at 600 °C, the final powder presented an average particle size below 50 nm with a surface area of 19 m² g⁻¹ and a large reactivity. The evolution of the most important functional groups during the steps involved in this synthesis route is explained in view of the results obtained with FTIR and XRD. A thorough discussion on the different intermediates involved in the whole process is presented on the basis of hydrolysis and condensation reactions. The conclusions are supported with a complete characterization through differential and gravimetric thermal analysis (DTA/TGA), electron microscopies (SEM/TEM) and surface area determinations (BET).     

TiO2-SnO2纳米粉末的制备及表征

以廉价的无机盐为原料,采用溶胶-凝胶(Sol-Ge l)法制备了TiO2-SnO2纳米粉,并采用DTA、XRD、TEM技术对粉体进行了表征.实验结果表明:用该法制得的TiO2-SnO2超细粉体粒径在5～7 nm左右.     

Synthesis and characterization of highly dispersed TiO2 nanocrystal colloids by microwave-assisted hydrothermal method

Anatase TiO₂ nanocrystal colloids with high dispersion and photocatalytic activity were rapidly synthesized from peroxo-titanium-acid precursor by microwave-assisted hydrothermal method within 30?min at low temperature (120–180?°C). The transmission electron microscopy results indicate that the as-prepared TiO₂ have a narrow particle size distribution (25–29?nm) and high dispersion. The crystal structure of all these products are pure anatase phase (XRD, Raman), and they show good crystallinity and large surface area (N₂ adsorption–desorption measurements BET). The results of the UV–Visible absorbance and Fourier transform infrared spectra indicate that the surface peroxo group Ti(O₂) still remains in TiO₂ nanoparticles prepared by microwave-assisted hydrothermal method at 120?°C, and this surface peroxo group can be decomposed effectively by drying at 140?°C. The photocatalytic activity of the as-prepared TiO₂ were evaluated by the degradation of reactive brilliant red X-3B, it is found that the as-prepared TiO₂ exhibited good photocatalytic performance. Moreover, the existence of surface peroxo group greatly suppressed the photocatalytic activity of the TiO₂ nanoparticles.     

TEM microstructure characterization of nano TiO2 coated on nano ZrO2 powders and their photocatalytic activity

Nano TiO₂ coated commercial nano ZrO₂ powders (20 and 80 wt.%) were synthesized by a sol–gel process. Their microstructure and crystal structure depending on the calcination temperatures were investigated using XRD and HRTEM techniques. In the as-received powders, the nano TiO₂ particles attached to the ZrO₂ particles existed in an amorphous phase. After calcination at 450 and 600 °C, most of the TiO₂ powders were crystallized to an anatase type, whereas at 750 °C, they were changed to a rutile phase.From the comparison of photocatalytic activity, the nano TiO₂ coated ZrO₂ powders calcined at 450 and 600 °C showed excellent efficiency for the removal of methyl orange (MO). However, in the powders calcined at 750 °C, the photocatalytic activity was decreased due to the appearance of a rutile phase.     

二氧化锡薄膜的MOD法制备和表征

采用新颖的金属有机物热分解方法（MOD）制备了二氧化锡薄膜,红外分析和热分析表明,先体制备过程中生成了锡的有机物,这对制备质量良好的光学薄膜起了决定作用。对薄膜的红外光谱和紫外－可见光谱的分表明,薄的热处理过程中经历了溶剂挥发、有机物燃烧和析晶等过程,随热处理温度的升高,薄膜的孔率显著减小,薄的结构致密,这是由制备过程的特点决定的。     

Synthesis and photocatalytic property of SnO2/TiO2 nanotubes composites

SnO2/TiO2 nanotubes composite photocatalysts with different SnO2 contents were successfully synthesized by means of a simple solvothermal process. The synthesized products were characterized physically by X-ray diffraction (XRD) and high-resolution transmission electron microscope (HRTEM). The composite photocatalysts can not only make the target pollutant, methylene blue (MB), adsorbed at a high concentration level around the surface of the composites but also decrease the recombination rate of electron-hole pairs so as to achieve good photocatalytic performance. The effect of SnO2 contents on the photocatalytic activities of the composites was also investigated. The results showed that the SnO2/TiO2 nanotubes composite photocatalyst with 5 wt.% SnO2 loading had the highest photocatalytic efficiency.