乙二醇溶剂热法制备纳米TiO2

用乙二醇溶剂热法制备了锐钛矿相纳米TiO2,用X射线粉末衍射(XRO)、红外光谱仪(FTIR)、热重分析(TG-DTA)和透射电子显微镜(TEM)对制备的样品进行了表征,研究了乙二醇浓度、含水量、反应温度和反应时间对纳米TiO2晶型和晶粒尺寸的影响.结果表明:所得的纳米TiO2粒径分布窄,单分散性好.随着溶剂热反应温度的升高,纳米TiO2的晶粒尺寸逐渐变大,但随着溶剂热反应时间的延长,纳米TiO2的晶粒尺寸却几乎不变.     

共沸蒸馏法制备TiO2、SnO2纳米粉体

采用共沸蒸馏法分别制备了TiO2、SnO2纳米粉体,并应用XRD和TEM等分析方法对所得粉体进行了表征.结果表明:采用共沸蒸馏法制备出了分散性较好、粒径约为7nm的TiO2纳米粉体和粒径约为10nm的SnO2纳米粉体.     

超重力法-醇水体系合成纳米钇铝石榴石

以NH4HCO3和NH3·H20为沉淀剂,醇水体系为溶剂,合成了钇铝石榴石（YAG）粉体,考察了超重力场和不同醇体积分数（R）对合成YAG粉体的影响,利用X射线衍射fXRD）、热重一差示扫描同步热分析（TG—DSC）和扫描电镜（SEM）等手段对粉体进行了研究,结果表明,超重力场中制备的YAG粉末颗粒更细小,分布范围更窄,分散性更好;醇水体系作为溶剂更有利于制备分散性好,粒径小的纯相YAG粉体;最适的醇体积分数为30％-50％。当以NH4HCO3和NH3·H3O为沉淀剂,R=30％的醇水体系为溶剂,在超重力场中合成的YAG前躯体在1000℃下煅烧2h,获得了分散性好、分布范围窄、晶型完整、平均粒径约为50nm的球形YAG粉体。     

溶胶-凝胶-冷冻法制备纳米TiO2及其表征

为解决纳米TiO2粉体易产生团聚的问题,采用溶胶-凝胶与冷冻干燥法制备纳米TiO2粉体.通过X射线衍射、扫描电子显微镜和紫外分光光度计对纳米TiO2粉体的物相组成、形貌和光催化活性进行了表征.实验结果表明:在400℃下所制得的TiO2纳米粉体的粒径约为6 nm,且粒度分布均匀,呈球形;所制得的TiO2纳米粉体在投加量为2 g/L时可使质量浓度为20 mg/L的甲基橙溶液在2.5 h内几乎全部降解.溶胶-凝胶与冷冻干燥法再结合阶段升温焙烧法可得到分散性好、粒径小和光催化活性好的粉体.     

锐钛矿型纳米TiO_2粉体的纯净制备

以钛酸丁酯为原料,采用可控醇盐水解沉淀法制得TiO2前驱体,450℃恒温煅烧2h后制备出粒径约10nm的纳米TiO2粉体,并与传统溶胶-凝胶法制备的TiO2纳米粉体的形貌、结构、工艺过程进行了对比.结果表明,可控醇盐水解沉淀法可制得纯度高、粒径小且分布范围窄的纳米TiO2粉体,工艺简单,流程最短.该方法的关键是实现了醇盐的可控水解.     

单分散纳米二氧化钛的研制

以钛酸四丁酯为原料,采用控制金属醇盐水解和表面修饰保护方法研制单分散、粒径可控的纳米级二氧化钛（TiO2)粒子。研究了反应物浓度、pH、反应时间、溶剂等反应条件对粒子粒径及分布的影响。采用透射电镜,红外光谱等技术对粒子的性能进行分析,结果表明,TiO2水合粒子呈非晶态,分散性好,粒径在50-300nm之间随反应条件的不同而变化,经700℃热处理后主要为金红石型TiO2。     

纳米TiO2的制备及其光催化活性

用高分子凝胶法制备纳米TiO2,研究了烧结温度对晶粒大小的影响以及粉体的平均粒径和光催化活性的关系.结果表明:高分子凝胶形成的小且均匀的网格限制了TiO2晶粒之间的接触和团聚,因此在较低温度下即可合成分散性好、平均粒径细小、粒径均匀且无团聚具有锐钛矿结构的纳米TiO2.随着煅烧温度的升高,纳米TiO2的平均粒径逐渐增大.纳米TiO2平均粒径的减小可提高其光催化活性以及对次甲基蓝的降解速率.适量的TiO2可以使次甲基蓝的降解率达到70%.     

反相胶束法制备ZrO2纳米粉体的研究

采用反相胶束法制备ZrO2纳米粉体,以可溶性锆盐溶液/庚烷的反相胶束体系为基础,以氨水为沉淀剂,司盘为分散剂,通过化学反应产生凝胶状沉淀,经蒸馏、洗涤、冷冻干燥、焙烧得到单分散、粒径分布窄的ZrO2纳米粉体.实验研究了庚烷与水体积比、氨水用量以及乳化剂的影响.采用X射线衍射仪、透射电镜及粒度仪等对样品进行物相分析和形态表征,结果表明通过此方法制备的ZrO2纳米粉体粒径可控制在40nm的范围内,且具有良好的分散性.     

正交设计在溶胶-凝胶法制备单分散球形SiO_2中的研究

通过正交试验设计,用L9(43)正交表安排实验,在醇氨反应体系中采用溶胶-凝胶(sol-gel)法制备单分散球形SiO2,运用直观图和极差分析确定各主要原料对制备不同粒径SiO2的影响,优化配比。研究表明:对单分散球形SiO2的平均粒径的影响次序为:用水量、醇用量、氨水和正硅酸乙酯(TEOS)用量。通过控制反应条件,可实现在一定范围内获得尺寸均一、不同粒径、分散性好的球形SiO2。制备出的单分散球形SiO2颗粒形态完整,粒径140～500nm,分布窄、单分散性好。     

表面活性剂对二氧化钛纳米流体分散性的影响

通过二步法将纳米二氧化钛分散到去离子水中,制备TiO2-水纳米流体。通过加入3种不同的表面活性剂作为分散剂,即阴离子表面活性剂十二烷基苯磺酸钠(SDBS)、非离子表面活性剂聚乙烯吡咯烷酮(PVP)和阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)制备出3种不同的纳米流体。用纳米粒度分析仪测定纳米流体中的纳米粒子的粒径和粒径分布,用Zeta电位分析仪测量纳米流体的电位,分析了不同浓度、不同种类的表面活性剂对水基TiO2纳米流体分散性的影响。     

The direct synthesis of mesoporous structured MnO(2)/TiO(2) nanocomposite: a novel visible-light active photocatalyst with large pore size

A series of visible-light-driven mesoporous structured MnO(2)/TiO(2) nanocrystal photocatalysts have been synthesized through a modified sol-gel method, and the N(2) adsorption-desorption isotherm confirms that the mesoporous materials possess large pore size (up to 9.2?nm) and a narrow pore size distribution. X-ray powder diffraction (XRD) analyses and complementary x-ray photoelectron spectroscopy (XPS) measurements reveal that the doping of the transition metal Mn inhibits the growth of TiO(2) anatase nanocrystals and the Mn species are highly dispersed on the surface of TiO(2). The ultraviolet (UV)-vis spectrum demonstrates the excellent adsorption properties of MnO(2)/TiO(2) over the whole region of visible light, which enables this novel photocatalysis material to possess remarkable activity in the photocatalytic degradation of methylene blue under visible light radiation. Moreover, a 'coating mechanism' based on the nucleation of titania nanocrystals along with the interaction between the dopant precursors and titania clusters has been suggested.     

有机模板剂对合成纳米TiO_2结构影响规律的研究

以钛酸四丁酯为前驱体,乙醇为溶剂,采用溶胶-凝胶法制备纳米二氧化钛。选择P123作为模板剂考察了不同n(P123)/n(Ti)对TiO2织构性能以及晶粒尺寸的影响。采用碳化的方法使有机物在氩气气氛中高温焙烧后形成的炭层对孔道起支撑作用,防止孔道的塌陷并得到高度晶化的二氧化钛,同时考察了碳化温度和不同模板剂对二氧化钛织构性能的影响规律。结合X射线衍射(XRD)、N2吸附脱附、热分析(TG/DSC)表征手段得到以下结论:物质的量比在0～0.030范围内,P123含量的增加有利于晶粒尺寸的减小和比表面积的增大;碳化过程提高了TiO2的热稳定性,随着碳化温度的升高TiO2比表面积变化不大;P123、PEG2000、CTAB 3种模板剂中P123得到的样品性能最好。     

Characterization of silver nanoparticles synthesized on titanium dioxide fine particles

Silver nanoparticles with a narrow size distribution were synthesized over the surface of two different commercial TiO(2) particles using a simple aqueous reduction method. The reducing agent used was NaBH(4); different molar ratios TiO(2):Ag were also used. The nanocomposites thus prepared were characterized using transmission electron microscopy (TEM), scanning transmission electron microscopy (STEM), scanning electron microscopy (SEM), energy-dispersive spectroscopy (EDS), x-ray photoelectron spectroscopy (XPS), x-ray diffraction (XRD), dynamic light scattering (DLS) and UV-visible (UV-vis) absorption spectroscopy; the antibacterial activity was assessed using the standard microdilution method, determining the minimum inhibitory concentration (MIC) according to the National Committee for Clinical Laboratory Standards. From the microscopy studies (TEM and STEM) we observed that the silver nanoparticles are homogeneously distributed over the surface of TiO(2) particles and that the TiO(2):Ag molar ratio plays an important role. We used three different TiO(2)Ag molar ratios and the size of the silver nanoparticles is 10, 20 and 80?nm, respectively. It was found that the antibacterial activity of the nanocomposites increases considerably comparing with separated silver nanoparticles and TiO(2) particles.     

Effects of Additive AlCl3 on Crystal Phase, Particle Size and Microstructural Parameters of Nanocrystalline TiO2 Prepared by HF-PCVD

Nanocrystalline TiO2 was prepared by high frequency plasma chemical vapor deposition (HF-PCVD). The effects of additive AlCl3 on crystal phase, particle size and microstructurai parameters of TiO2 nanocrystallites were investigated by X-ray diffraction(XRD) and transmission electron microscopy (TEM). The nanocrystallites obtained experimentally are mixture of anatase and rutile, the uniform diameters of particles are about 30 nm. The phase transformation from anatase to rutile was accelerated by AlCl3, and rutile content is increased from 26.7 wt pct to 53.6 wt pct with increasing of addition of AlCl3 from 0.0 wt pct to 5.0 wt pct. The particle size is reduced and the size distribution becomes very narrow. The crystal lattice constants have the trend to decrease, and celi volumes appear as shrinkable     

微混合沉淀技术制备纳米TiO2颗粒

以Ti(SO4)2为分散相，NH4HCO3为连续相，通过膜分散实现液液的微混合沉淀，从而制备纳米TiO2晶体颗粒、分别研究了两种反应物浓度和流量对制备的TiO2颗粒的影响，并利用XRD和TEM分别对所得颗粒的晶型和形态进行了表征．实验结果表明，制得的颗粒具有球形度高，粒径小，分布范围窄，且为锐钛矿结构的特点．TiO2的晶粒粒度和颗粒粒径随Ti(SO4)2和NH4HCO3浓度的上升，先有所上升再下降；随Ti(SO4)2流量的上升而下降；随NH4HCO3流量的上升而上升．微混合沉淀技术是一种很好的控制颗粒粒径、且连续化沉淀制备TiO2超细颗粒的新方法。     

介孔TiO_2的合成及其对氟离子的吸附性能研究

以十六烷基三甲基溴化铵(CTAB)为模板剂,采用水热法制备了介孔TiO2,对制得的样品进行了XRD、TEM、N2吸附-解吸表征,并探究了不同吸附条件对样品吸附性能的影响。结果表明,所得样品为窄孔道分布,其比表面积为161.2m2/g,最可几孔径为5.2nm;与非介孔TiO2相比,介孔TiO2对氟离子的吸附性能明显优越,其对氟离子的吸附速率符合Bang-ham吸附速率方程,吸附量随氟离子浓度的增大而增大,而且吸附符合Langmuir等温吸附方程,属于放热吸附。     

TiO2纳米微晶的RF-PCVD法制备及表征

以TiCl4为原料,采用高频等离子化学气相沉积(RF-PCVD)法制备了TiO2纳米微晶,考察了控制粒径大小及晶相转化的关键操作条件.借助XPS、TEM、XRD、BET等技术对颗粒的化学组成、形貌、晶相结构等进行了表征.研究表明:所得TiO2纳米微晶大部分为球形体颗粒,粒径30～50 nm,单分散性良好;颗粒中锐钛相和金红石相两相共存,结晶完整;金红石相含量在26.7%～53.6%之间可调.     

基于光催化性能的Cu-Ce/TiO_2湿性能

以Cu(NO_3)_2·3H_2O和Ce(NO_3)_3·6H_2O为改性剂,采用溶胶-凝胶法制备Cu-Ce/TiO_2。探讨Cu-Ce负载量、Cu与Ce摩尔比和煅烧温度对Cu-Ce/TiO_2性能的影响。利用SEM,LPSA,BET和UV-Vis测试Cu-Ce/TiO_2的表面形貌、粒度分布、孔结构和光学性能。结果表明:Cu-Ce负载量3%、Cu与Ce摩尔比1∶1、煅烧温度500℃时,制备的Cu-Ce/TiO_2具有良好的光催化性能与湿性能。Cu-Ce/TiO_2呈近似球体,具有较好的均匀化和分散性,其粒径分布为1202.98~5364.48nm,其中d50为2437.57nm。Cu-Ce/TiO_2具有狭小瓶颈的"墨水瓶"型孔结构,其比表面积为105.55m2/g,孔体积为0.1200~0.1246mL/g,平均孔直径为3.44~4.02nm。Cu-Ce掺杂促使Cu-Ce/TiO_2内部形成新的能级,提高捕获e-和h+的能力,增强光子的利用效率,促使吸收边带发生红移。     

Synthesis of uniform TiO2 nanoparticles with egg albumen proteins as novel biotemplate

A novel bio-templated route was reported for the fabrication of uniform and well dispersed TiO, nanoparticles using denatured egg albumen (EA) proteins network as template. Anatase TiO2 nanoparticles of ca. 9 nm with narrow size distribution were obtained under employed reaction conditions, as proved by the XRD and TEM results. The as-prepared TiO2 nanoparticles were further characterized by means of XPS, FTIR, TG-DTA and UV-Vis. Based on the characterization results, a possible process of heat-induced denatured protein network as template matrix to fabricate TiO2 nanoparticles was carefully proposed. The method with egg albumen as bio-template provides us a cheap, green and repeatable route for the fabrication of nanoparticles under mild conditions.     

潜伏性热释放2PZ-PS-co-MAA微胶囊固化剂的制备与性能

以2-苯基咪唑(2PZ)为芯材,苯乙烯-甲基丙烯酸共聚物(PS-co-MAA)为壁材,采用溶剂挥发技术,成功地制备了一种新型潜伏性热释放2PZ-PS-co-MAA微胶囊固化剂。通过红外光谱仪(FT-IR)、热重分析仪(TGA)、扫描电子显微镜(SEM)、粒度分析仪和差示扫描量热仪(DSC)对微胶囊固化剂的化学结构、芯材含量、表面形貌、粒径分布及固化性能等进行了表征。所制备的微胶囊固化剂表面光滑,粒径分布较窄,平均粒径约为15.60μm,壁材厚度约为0.5μm,芯材2PZ含量约为39.19%。由微胶囊固化剂与环氧树脂E-51制备的单组分胶粘剂,具有优良的固化特性和潜伏性能,可在100℃,30 min内实现固化,室温储存期可达32 d以上。