粒径可控球形TiO2的制备

在正丙醇与水的混合溶剂体系中以Ti(SO4)2为前驱物制备得到了粒径分布窄,分散性好的球形TiO2.对表面活性剂种类及用量,反应物浓度及焙烧温度和时间等影响因素进行了研究,结果表明,在正丙醇与水的体积比为1∶1的条件下,以聚乙烯吡咯烷酮(PVP)为表面活性剂,温度为70-90℃时可制得粒径分布窄、分散性好的高质量的球形TiO2颗粒.通过TG-DSC、SEM、XRD等分析表明,颗粒粒度大小及粒径分布受表面活性剂浓度和反应前驱物浓度影响大;物相间的转化主要由焙烧温度和时间来决定.并引入LaMer模型对颗粒形核、长大的过程进行理论说明.     

水解制备球形TiO2及其水解过程动力学

以硫酸钛(Ti(SO4)2)为前驱物水解得到超细球形TiO2. 研究了水解过程中前驱物浓度和体系温度对水解速率的影响, 并对实验值进行了拟合, 得到水解TiO2的质量分数与水解时间呈良好的指数关系, 根据Avrami方程进一步验证了拟合的可靠性. 分析了水解介质的影响作用, 确定介电常数和zeta电位也是影响水解速率的重要因素, 因此可通过改变溶剂成分来调节介电常数和zeta电位, 从而达到控制Ti(SO4)2水解速率的目的. 实验结果表明, Ti(SO4)2水解制备TiO2的过程中, 较低的前驱物浓度, 较高的水解温度和合适的溶剂体系有利于得到粒径分布窄、分散性好的TiO2.     

炭黑吸附法制备掺杂镨TiO2纳米粉体及其光催化性能

以硝酸镨为掺杂的前驱物,钛酸异丙酯为TiO2的前驱物,通过炭黑吸附高温水热法制得掺杂镨的量为0.07%的纳米Pr3+/TiO2粉体。分别采用热重/差热分析(TG-DTA)、X射线衍射(XRD)、扫描电镜(SEM)、紫外可见分析(UV-VIS)和比表面积吸附(BET)对不同焙烧温度下所得粉体的物相、颗粒度、分散性及光吸收性能进行表征和分析。实验结果表明:炭黑的吸附阻止了粉体在干燥和煅烧阶段的团聚和烧结,制得的Pr3+/TiO2纳米粉体团聚较少,呈现良好的分散性,颗粒均匀,经500℃焙烧,得到纳米粉体平均颗粒直径为18 nm,比表面积为78.08 g.m-2。光催化降解实验表明,炭黑吸附后TiO2的光催化活性在一定时间内比没有炭黑的提高了将近2倍,在紫外灯照射下Pr3+/TiO2能在60 min内对亚甲基蓝的降解率达到93%。     

微乳液和均匀沉淀耦合法制备CeO2纳米粒子

用W/O微乳液和草酸二甲酯均匀沉淀耦合法制备出单分散性好并具有较窄粒度分布的CeO2纳米粒子,测试了其形貌、粒径及粒径分布和晶体结构等特征.实验结果表明,表面活性剂的种类和反应物的相对初始浓度对产物平均粒径具有规律性的影响;随着焙烧温度升高,产物的平均粒径明显增大.     

共沉淀-喷雾干燥法制备Sm2O3掺杂CeO2纳米粉体

以Sm（NO3）3.6H2O和Ce（NO3）3.6H2O为原料,用共沉淀-喷雾干燥法制备了Sm2O3掺杂CeO2（SDC）粉体。通过沉降实验、TG-DSC、XRD、BET、SEM和粒度分布对前驱体的分散性、稳定性及制得的SDC粉体性能进行表征,研究了洗涤方法、分散剂对前驱体及SDC粉体的影响。结果表明：无机陶瓷膜洗涤后前驱体分散性好,经500℃以上温度焙烧后的粉体为立方萤石型结构。加入分散剂后前驱体的分散性明显提高,制得的SDC粉体比表面积显著增加,最终获得了晶粒平均粒径为12.51 nm、团聚态颗粒为球形的SDC纳米粉体。     

反相微乳液法制备纳米氧化铝

采用由环己烷、聚乙二醇辛基苯基醚(TritonX-100)、正丁醇与水溶液构成的反相微乳液体系, 合成了纳米Al2O3粉体. 采用X射线衍射、扫描电子显微镜、透射电子显微镜、比表面积分析仪等表征手段, 分别对产物的结构、形貌、比表面积和孔容进行了表征, 该纳米Al2O3比表面积约450 m2·g-1(随反应参数不同发生变化), 均属γ-Al2O3, 粒径均匀, 颗粒直径小于10 nm. 考察了微乳液体系中水与表面活性剂的物质的量之比r0、表面活性剂与助表面活性剂的体积比φ、焙烧温度等关键因素对产物比表面积等物理性质的影响. 结果表明, 当r0=20, φ=0.5, 焙烧温度为500 ℃时, 可以得到大比表面积、高孔容、分散性好及粒径分布均匀的γ-Al2O3粉体.     

低温苯甲醇醇解法制备高活性锐钛矿型纳米晶TiO2光催化剂

 以TiCl4 为钛源,采用低温苯甲醇醇解法制备了不同粒径及晶相组成的大表面TiO2纳米晶,利用X射线衍射、热重-差热分析、透射电子显微镜、拉曼光谱、紫外-可见漫反射光谱和N2物理吸附等方法考察了焙烧温度和焙烧时间对其晶相组成、晶粒尺寸、比表面积及孔体积等微结构性质的影响,并以苯酚的光催化降解为模型反应评价了样品的光催化活性. 结果表明,未经任何热处理的TiO2样品即为锐钛矿晶相,控制焙烧温度及焙烧时间可进一步调控样品的粒径、比表面积、晶相结构及表面氧缺位浓度. 经400 ℃焙烧3 h制备的纳米晶TiO2具有最佳的光催化活性,其活性比商用Degussa P-25 TiO2更高.     

水基溶胶-凝胶法制备稀土/碱土金属硅酸盐纳米粉

采用水基溶胶凝胶法,以廉价的无机盐Y2O3,MgO为前驱物,Si(OC2H5)4为络合剂,PEG4000为复合表面活性剂,氨水调节pH值,并利用无水乙醇超声分散技术,成功制备了分散性良好的稀土碱土金属复合硅酸盐纳米粉xY2O3·yMgO·zSiO2(YMS),考察了初始溶液的pH值、温度及浓度对溶液—溶胶—凝胶转变的影响,并利用TG DTA,XRD,TEM分析手段对复合硅酸盐纳米粉YMS的性质进行了研究。实验表明,在60℃相似文献   

熔盐法可控合成球形CeO_2的研究

以NaCl-KCl为熔盐,采用熔盐法制备了球形CeO_2纳米粉。在实验过程中,通过改变NaCl-KCl与Ce之间的比例、煅烧温度、煅烧时间等工艺参数,考察了熔盐法制备工艺参数对CeO_2粉末的形貌、颗粒尺寸和分散性的影响,以此实现了球形CeO_2的可控合成。通过SEM,XRD和激光粒度分析仪等测试方法对其颗粒形貌、分散性、物相、粒径等性能进行了表征。结果表明:通过控制制备条件,可以获得分散性良好、结晶完整的不同粒径的球形CeO_2纳米粉。当NaCl-KCl与Ce比为3∶1,煅烧温度为800℃,保温2 h时,获得的CeO_2纳米粉粒径约为85 nm。     

介孔二氧化钛微球的合成与表征

以非离子型表面活性剂TO8为模板剂,采用溶胶凝胶-表面活性剂法合成了介孔TiO2微球．运用SEM,TG—DTA,XRD,BET,UV等测试手段对其进行表征并探讨了TO8的加入量和不同热处理方式对样品形貌、结构的影响．实验表明TiO2微球呈单分散性,球径约800nm;介孔结构,孔径约3．5nm且分布较窄．TiO2微球为单一锐钛矿相,在190～380nm范围内有强紫外吸收．热处理时采取分步焙烧、控制升温速率和高温焙烧时间,可获得比表面较大的介孔TiO2微球．     

Synthesis of TiO2 nanoparticles utilizing hydrated reverse micelles in CO2

Titanium dioxide nanoparticles were produced by the controlled hydrolysis of titanium tetraisopropoxide (TTIP) in the presence of reverse micelles formed in CO2 with the surfactants ammonium carboxylate perfluoropolyether (PFPECOO-+NH4) (Mw = 587) and poly(dimethyl amino ethyl methacrylate-block-1H,1H,2H,2H-perfluorooctyl methacrylate) (PDMAEMA-b-PFOMA). Based on dynamic light scattering measurements, the amorphous TiO2 particles formed by injection of TTIP are larger than the reverse micelles, indicating surfactant reorganization. The size of the particles and the stability of dispersions in CO2 were affected by the molar ratio of water to surfactant headgroup (w(o)), precursor concentration, and injection rate. The amorphous particle size did not change upon depressurization and redispersion in CO2. PDMAEMA-b-PFOMA provided greater stability against particle aggregation at higher reactant concentration compared with PFPECOO-+NH4. The crystallite size after calcination, which was examined by X-ray diffraction and transmission electron microscopy, increased with w(o).     

Sol-gel low-temperature synthesis of stable anatase-type TiO2 nanoparticles under different conditions and its photocatalytic activity

In this work, TiO(2) nanoparticles in anatase phase was prepared by sol-gel low temperature method from titanium tetra-isopropoxide (TTIP) as titanium precursor in the presence of acetic acid (AcOH). The effects of synthesis parameters such as AcOH and water ratios, sol formation time, synthesis and calcination temperature on the photocatalytic activity of TiO(2) nanoparticles were evaluated. The resulting nanoparticles were characterized by X-ray diffraction, UV-Vis reflectance spectroscopy, transmission electron microscopy and Brunauer-Emmett-Teller techniques. Photocatalytic activity of anatase TiO(2) nanoparticles determined in the removal of C. I. Acid Red 27 (AR27) under UV light irradiation. Results indicate that with increasing AcOH/TTIP molar ratio from 1 to 10, sol formation time from 1 to 3 h and synthesis temperature from 0 to 25°C, increases crystallite size of synthesized nanoparticles. It was found that optimal conditions for low temperature preparation of anatase-type TiO(2) nanoparticles with high photocatalytic activity were as follows: TTIP:AcOH:water molar ratio 1:1:200, sol formation time 1 h, synthesis temperature 0°C and calcination temperature 450°C.     

Effects of template and precursor chemistry on structure and properties of mesoporous TiO2 thin films

Mesoporous TiO2 thin films were synthesized by sol-gel processing using an aqueous-based, inexpensive, and environmentally friendly precursor and cationic surfactants as templates under mild reaction conditions. The films were prepared by spin-coating on glass substrates followed by calcination to remove the surfactant. N2 sorption, X-ray diffraction, and transmission electron microscopy were used to characterize the porosity, pore size, and pore structure before and after calcination. Films were found to have wormlike pore structures after calcination and surface areas on the order of 200 m2/g. These results show that the mesostructure and porosity of the thin films can be controlled by the surfactant template chemistry such as surfactant/Ti ratio, pH, and rate of solvent evaporation.     

低温下溶胶凝胶法制备TiO2纳米晶

从含过量水的溶胶出发,在室温下得到了TiO₂纳米晶。通过红外光谱,透射电子显微镜法和X射线粉末衍射法对含有过量水的溶胶体系中TiO₂纳米晶的室温形成机理进行了研究。与传统的溶胶凝胶法相比,在改良的溶胶凝胶体系中,在缩聚反应之前由于水过量使得钛的先驱体快速且充分的水解,从而生成[TiO₆]基团,随之形成TiO₂纳米晶。晶粒的尺寸为约3.5 nm,该法得到的TiO₂纳米晶比传统溶胶凝胶法得到的TiO₂纳米晶和商用光催化剂德固赛P25具有更好的光催化活性。     

溴化银/二氧化钛复合材料的可见光催化性能

将硝酸银的乙醇溶液与溶胶凝胶TiO2混合得到前驱体,随后经共沉淀-煅烧制备得到AgBr/TiO2复合材料;采用扫描电镜、X射线衍射仪、X射线光电子能谱仪分析了复合材料的形貌、晶体结构、Ag元素的价态,采用紫外-可见漫反射光谱仪测定了其光吸收性能;进而以甲基橙(MO)的可见光降解为探针反应测定了AgBr/TiO2复合材料的可见光催化性能.结果表明,当前驱体在不同温度下煅烧后,无定形TiO2颗粒逐渐增大,并逐渐转变为锐钛矿结构;担载的AgBr可明显拓展TiO2的可见光吸收范围;Ag物种主要以Ag+形式存在.当煅烧温度为300℃时,复合材料的光催化活性最高,MO的降解率在60min内达到90%以上;随着煅烧温度的增加,催化活性逐渐降低.     

Synthesis of polyhedral particles by dispersion polymerization in supercritical carbon dioxide

The novel synthesis of polyhedral particles was attained by the dispersion polymerization of styrene in supercritical carbon dioxide using a polydimethylsiloxane-based macroazoinitiator as a precursor of the surfactant. The macroazoinitiator, VPS-1001, composed of poly(dimethylsiloxane) and 6-8 molecules of the azo groups served as a precursor of the surfactant for the dispersion polymerization by azobisisobutylonitrile as an initiator to produce 0.8-4 μm polyhedral particles. The size of the particles decreased as a result of increasing the VPS-1001 concentration. Too high a concentration of VPS-1001 caused coagulation of the particles. A decrease in the temperature increased the particle size and size distribution, while a decrease in the pressure produced particles with nonspecific shapes. An increase in the stirring rotation speed tended to increase the size and size distribution. However, too high a speed of rotation also caused coagulation of the particles.     

Polyacrylamide gel method: synthesis and property of BeO nanopowders

Effects of monomer (AM) concentration, monomer/crosslinker (AM/MBAM) ratio and salt concentration on the thermal behavior of precursor gel and the properties of BeO nanopowder synthesized by polyacrylamide gel method were investigated. The decomposition process of precursor gel was also studied. The decomposition process of precursor gel is that, first, the extraction of free and crystallized water, and then the thermal degradation of polymeric network under temperature higher than 600 °C, final, the decomposition of nanoscale beryllium sulfate to BeO nanopowder. As the monomer concentration increases, the calcination temperature of precursor gel decreases due to more compact network structure of gel and thus smaller size of salt in nanocaves in gel. The average particle size of nanopowder reduces correspondingly. The AM/MBAM ratio also has significant effect on the thermal behavior of precursor gel and the average particle size of product. When the ratio of AM to MBAM is 6, the calcination temperature of precursor gel is the lowest, the average particle size of powders is the smallest, because the network structures of gel is the tightest and thus the sizes of salts in precursor gels are the smallest. As the AM/MBAM ratio deviates from this value, the network structures of gel becomes looser and thus the size of salt in precursor gel becomes larger, so the calcination temperature increases and the average particle size of powders becomes larger certainly. For the same reason, both the calcination temperature and the average particle size of powders increases with increasing the salt concentration. The synthesis conditions have no effect on the particle size distribution of the final product due to the natural random distribution of porosity in gel.     

Preparation of nanometer-sized In2O3 particles by a reverse microemulsion method

Nanometer-sized indium oxide (In(2)O(3)) particles have been prepared by chemical reaction of inorganic indium compounds and ammonia gas in a reverse microemulsion system consisting of water, Triton X-100 (surfactant), n-heptanol (co-surfactant), and n-octane (oil). Precursor hydroxides precipitated in the droplets of water-in-oil (W/O) microemulsion were calcined at different temperatures to form indium oxide powder. The factors affecting the particle size have been discussed; the calcination temperature is considered to be the important factor for controlling the size. In(2)O(3) calcined at 400 degrees C had a spherical form and a narrow size distribution. Calcination at 800 degrees C led to the formation of particles not only of irregular shape, but also of a wide size distribution. With the increase in calcination temperature from 400 to 800 degrees C, the average size of the particles grew from 7 to about 40 nm. The species of reactants used in the aqueous phase had a significant effect on the size of the particles. The average diameter of In(2)O(3) particles derived from reactant InCl(3) was 7 nm; that of particles derived from In(NO(3))(3) was 15 nm. The In(2)O(3) nanoparticles were characterized by transmission electron microscopy and X-ray diffraction. The phase behavior of the microemulsions is discussed.     

Synthesis of ZnO nanoparticles in 2-propanol by reaction with water

We report on the synthesis of ZnO particles from Zn(CH(3)CO(2))(2) in 2-propanol as a function of the concentration of water, in the absence of a base such as NaOH. Particles with diameters of 3-5 nm are formed depending on time, temperature, and water concentration. The nucleation and growth are slower than in the presence of NaOH, and at longer times the increase in particle size is dominated by diffusion-limited coarsening. The rate constant for coarsening increases with increasing water concentration up to 150 mM, above which the rate constant is 1.1 x 10(-4) cm(3) s(-1), independent of the water concentration. The width of the particle size distribution decreases with increasing water concentration, and at 250 mM water, the full width at half-maximum of the distribution function is essentially the same as for the synthesis of ZnO using NaOH as a reactant. The temperature dependence of coarsening is determined by the bulk solubility of the ZnO nanoparticles and yields an apparent activation energy of 1.12 eV. This is significantly larger than the activation energy of 0.35 eV for coarsening of ZnO from 1 mM Zn(CH(3)CO(2))(2) in 2-propanol with 1.6 mM NaOH.