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.     

Ionic liquid-assisted hydrothermal synthesis of TiO2 nanoparticles and its applications towards the photocatalytic activity and electrochemical sensor

This work reports the synthesis of TiO₂ nanoparticles via ionic liquid-assisted hydrothermal method at 130?°C for two days. The obtained product was characterised by various techniques. The X-ray diffraction data reveal the anatase phase TiO₂ nanoparticles with crystallite size 37 nm. The Fourier transform infrared spectrum shows a band at 400 cm^?1 due to Ti–O–Ti stretching vibration, in addition to the presence of ionic liquid. The UV–Vis spectrum of TiO₂ nanoparticles shows an absorption band at 314 nm which indicates a blueshift compared with that of bulk TiO_2. The transmission electron microscopy images show almost spherical-shaped nanoparticles with an average diameter of 40–80 nm. TiO₂ nanoparticles exhibit excellent photocatalytic activity for the degradation of trypan blue, and also help in the reduction of Cr⁺⁶ to Cr⁺³. TiO₂ nanoparticles modified glassy carbon electrode exhibits better electrocatalytic oxidation towards dopamine compared with bare glassy carbon electrode.     

Microwave-assisted hydrothermal synthesis of nanocrystalline SnO powders

Tin oxide (SnO) powders were obtained by the microwave-assisted hydrothermal synthesis technique using SnCl₂·2H₂O as a precursor. By changing the hydrothermal processing time, temperature, the type of mineralizing agent (NaOH, KOH or NH₄OH) and its concentration, SnO crystals having different sizes and morphologies could be achieved. The powders were characterized by X-ray diffraction (X-ray), Field Emission Scanning Electron Microscopy (FE-SEM), High Resolution Transmission Electron Microscopy (HR-TEM) and Selected Area Electron Diffraction (SAED). The results showed that plate-like form is the characteristic morphology of growth and the TEM analyses indicate the growth direction as (200).     

纳米二氧化钛的晶型转变及光催化性能研究

采用溶胶-凝胶法制得稳定的TiO2透明溶胶．凝胶经焙烧制备了纳米TiO2粉体,利用FT-IR、XRD和原子力显微镜(AFM)技术对其进行了结构和形貌表征,考察了其对水杨酸的光催化活性。研究结果表明,醇胺不同的加入量,对TiO2从锐钛矿转变为金红石型的晶相转变温度(600～800℃)有很大影响．FT-IR谱的423cm^-1处吸收峰为金红石型TiO2的特征Ti-O键振动峰,采用310nm的紫外光波长照射时锐钛矿型TiO2粉体具有较高的光催化活性。     

纳米羟基磷灰石粉体的水热合成

采用Ca(NO3)2·4H2O和(NH4)3PO4·3H2O作为反应前驱物,通过水热合成颗粒尺寸在100nm以下的短棒状或针状HA晶体.X射线衍射(XRD)、透射电镜(TEM)和红外光谱(FTIR)分析讨论水热温度、反应时间、表面活性剂和烧结与物相组成、晶粒尺寸和晶体形貌的关系.实验结果表明升高反应温度和延长反应时间有利于HA的生成;表面活性剂有助于改善粉体的分散性能;烧结能提高晶体的结晶程度,但粉体易团聚,当温度高于800℃时HA发生分解.     

Hydrothermal synthesis and photocatalytic activity of anatase TiO2 nanofiber

TiO2 nanofiber consisting of 15 +/- 5 nm anatase grains was synthesized by hydrothermal treatment of fibrous hydrogen titanate precursor at 180 degrees C for 20 h. The hydrogen titanate precursor was synthesized by hydrothermal treatment of commercial P25 TiO2 powder in 10 M NaOH at 200 degrees C for 20 h followed by soaking in 0.1 M HNO3 to perform ion exchange between the as-synthesized Na titanate and H. By controlling pH of the solution during hydrothermal treatment of the hydrogen titanate precursor, pure anatase TiO2 nanofiber was obtained. Its band-gap energy determined from the onset of diffused reflectance spectrum was 3.19 eV which is equal to that of anatase TiO2 powder. The TiO2 nanofiber showed higher photodecomposition efficiency than the Cotiox KA-100 TiO2 but lower than the P25 TiO2. Photodegradation is the predominant process for 'Reactive blue 171' removal.     

Bi2O2CO3/TiO2复合粉体的制备及其光催化性能研究

采用水热法制备了Bi2O2CO3,并将其与TiO2进行了复合。XRD数据表明此复合光催化剂中Bi2O2CO3结晶性良好,紫外-可见漫反射光谱说明Bi2O2CO3的加入使其吸收带边有一定的红移。研究了紫外-可见光照射下Bi2O2CO3/TiO2复合光催化剂对亚甲基蓝溶液的降解性能,结果表明当Bi2O2CO3与TiO2的质量比为0.032时,得到性能最优的复合光催化剂,其光催化活性优于TiO2。     

红外上转换纳米发光材料的水热合成

利用稀土离子Y~(3+)、Yb~(3+)、Er~(3+)与乙二胺四乙酸形成的配合物,加入可溶性氟化物.控制溶液的pH值,利用配位-沉淀平衡体系制备了复合氟化物纳米粒子前驱物,在240℃下水热晶化前驱物,合成了红外上转换纳米发光材料.     

Microwave-assisted hydrothermal synthesis and photocatalytic activity of ZnO

The effect of synthesis temperature on the morphology of fine zinc oxide powders prepared by microwave-assisted hydrothermal processing of Zn(OH)₂ suspensions has been studied using x-ray diffraction and low-temperature nitrogen BET measurements. The photocatalytic activity of the powders for Methyl Orange photodegradation has been assessed as a function of synthesis temperature. The results indicate that the specific surface of ZnO powders plays a key role in determining their photocatalytic activity.     

Controlled synthesis of anatase TiO2 octahedra with enhanced photocatalytic activity

Titanium dioxide (TiO₂) nanocrystals with specific exposed crystal facet have attracted considerable interest due to their promising applications in the fields of energy and environment. In this paper, we report on a simple solvothermal approach for the synthesis of anatase TiO₂ octahedra with high yield, using titanium(IV) sulfate and hydrazine hydrate as the starting materials. The formation mechanism of anatase TiO₂ octahedra is suggested. The samples were characterized with XRD, Raman, SEM, TEM, FTIR, XPS, and UV/vis techniques, and further tested as a candidate in photocatalysis to decompose methyl orange in aqueous solution at room temperature. The results show that SO₄²⁻ ions not only benefit the formation of octahedral nanocrystals, but also inhibit nitrogen doping into TiO₂ matrix. More importantly, it is found that the octahedral TiO₂ nanocrystals show enhanced photocatalytic activity compared to TiO₂ P25 and anatase TiO₂ counterparts.     

Preparation of Ti3+/N-co-doped TiO2 by one-step hydrothermal synthesis method with high photocatalytic degradation performance under visible light

Journal of Materials Science: Materials in Electronics - Ti3+/N-co-doped TiO2 was successfully synthesized in situ by one-step hydrothermal method using tetrabutyl titanate (TBOT) as the titanium...     

Template-free hydrothermal synthesis of macroporous TiO2 microspheres on a large scale

Macroporous TiO₂ microspheres have been synthesized on a large scale by a facile hydrothermal process using titanium tetrachloride (TiCl₄) as the titanium source, ammonium fluoride (NH₄F) and hydrogen peroxide (H₂O₂) as the etchant. X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM) studies show that the anatase TiO₂ microspheres are well-crystalline with an average diameter of 5.43 μm. N₂ adsorption–desorption and mercury intrusion porosimetry analysis reveal that the as-prepared TiO₂ microspheres are composed of numerous pore networks with an average pore diameter of 274 nm and porosity of 39.8%. In addition, the formation mechanisms of macroporous TiO₂ microspheres were also investigated.     

Microemulsion-mediated solvothermal synthesis and photocatalytic properties of crystalline titania with controllable phases of anatase and rutile

Titanium oxide with different ratios of anatase to rutile has been prepared by the microemulsion-mediated solvothermal method. The resulting samples were investigated by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, UV-vis diffuse reflectance spectra, transmission electron microscopy and Brunauer-Emmett-Teller analysis. The contents of anatase and rutile in the TiO₂ particles have been successfully controlled by simply adjusting the amount of urea in the aqueous phase of the microemulsion. Both the degradation of Rhodamine B in aqueous solutions and mineralization of TOC revealed that the catalyst containing 47.6% anatase have presented the highest photocatalytic activity. A proposed mechanism is discussed to interpret the evolution of the phases based on the effect of different amount of urea.     

不同晶型纳米TiO2的水热合成及光催化性能

采用水热法制备了TiO2 纳米粉 ,并通过XRD、TEM、激光粒度分析对产物进行表征。结果发现 ,采用不同的钛源 ,不同的加料方式 ,可得到不同晶型的TiO2 纳米粒子。通过系列样品对甲基橙溶液的光催化性能的研究 ,发现混晶相纳米TiO2 的光催化性能最好 ,其次是锐钛矿相 ,金红石相的光催化性能最差。     

Ionic liquid-assisted one-step hydrothermal synthesis of TiO2-reduced graphene oxide composites

We have demonstrated a facile and efficient strategy for the fabrication of soluble reduced graphene oxide sheets (RGO) and the preparation of titanium oxide (TiO₂) nanoparticle-RGO composites using a modified one-step hydrothermal method. It was found that graphene oxide could be easily reduced under solvothermal conditions with ascorbic acid as reductant, with concomitant growth of TiO₂ particles on the RGO surface. The TiO₂-RGO composite has been thoroughly characterized by Fourier transform infrared spectroscopy, Raman spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and thermogravimetric analysis. Microscopy techniques (scanning electron microscopy, atomic force microscopy, and transmission electron microscopy) have been employed to probe the morphological characteristics as well as to investigate the exfoliation of RGO sheets. The TiO₂-RGO composite exhibited excellent photocatalysis of hydrogen evolution.      

Microemulsion-mediated solvothermal synthesis of ZnS nanowires

Uniform and high-aspect-ratio ZnS nanowires with length up to several micrometers and diameter of 30–50 nm are synthesized by a facile and low-cost microemulsion-mediated solvothermal method. Moreover, ZnS nanorods and bamboo-leaf-like ZnS nanostructures were also obtained by modulating the reaction parameters. Especially, hollow bamboo-leaf-like ZnS nanostructures formed by radiating those bamboo leaves with electron beam. A reasonable mechanism to the formation of the as-prepared one-dimension zinc blend ZnS nanocrystals is also discussed.