The preparation and structural characterization of ambient-dried porous methylsilicone matrix doped with SiO2 powder

Porous methylsilicone monoliths doped with SiO₂ powder were prepared by dispersion of SiO₂ nanoparticles in methylsilicone oligomer solution followed by ammonia-catalyzed gelation and ambient drying. The microstructure of the porous composite monoliths was investigated by FTIR, SEM, and N₂ adsorption. The results indicated that SiO₂ evenly dispersed in methylsilicone matrix. The thermal stability of SiO₂-doped methylsilicone monoliths had been enhanced. The structure stability and hydrophobic property of the composite monoliths were maintained until 400 °C.     

Silica xerogels and aerogels synthesized with ionic liquids

The synthesis of silica gels with ionic liquids (IL) as either additives or co-solvents is described. The wet gels were either dried by supercritical CO₂ or by evaporation to obtain aerogels or xerogels, respectively. The effects of two ionic liquids: 1-butyl-3-methyl imidazolium tetrafluororate (IL1) and 1-butyl-4-methyl pyridinium tetrafluoroborate (IL2), on the structural and textural characteristics of gels were investigated. IL2 showed a more important influence than IL1, on the gelation time and gel structure, according to solid state NMR investigations. With both types of ionic liquids, the average pore radius of xerogels increased from ≈2 nm at an IL to Si molar ratio n_IL/n_Si = 0.07, to ≈4 nm at n_IL/n_Si ≈ 1.5 and the size distributions were rather well centered about each mean radius. Hence, ionic liquids appeared as interesting additives to target gels with a given pore size.     

Preparation and characterization of monolithic alumina aerogels

Alumina aerogels were prepared by a sol-gel method combined with the ethanol supercritical drying technique using aluminum tri-sec butoxide and nitric acid as the precursor and catalyzer respectively. This method affords high-surface-area alumina aerogel monoliths without the use of complexing agents. The structure and morphology of the aerogels were investigated by TEM, XRD, FTIR and BET techniques. The results confirmed that the as-prepared alumina aerogel possessed a network microstructure made up of pseudoboehmite fibers and a surface area of 690 m²/g. It was transformed to γ-Al₂O₃ after heat treatment at 800 °C without a significant loss in surface area. DMA analysis and hotdisk thermal analysis were performed to characterize the mechanical and thermal properties of the samples. The results indicated that the alumina aerogel was robust and exhibited excellent thermal insulating properties. The elastic modulus was up to 11.4 MPa after drying, which is the one of the highest modulus of alumina aerogels ever reported. The thermal conductivities at 30 °C and 400 °C were 0.028 W/mK and 0.065 W/mK respectively.     

Uniform TiO2 thin films with anatase nanocrystallites synthesized through evaporation-induced assembly

Uniform nanocrystalline anatase (nc-TiO₂) thin films have been synthesized in a ternary copolymer-ethanol–water system through evaporation-induced assembly (EIA) method. The EIA method combines sol–gel and organic–inorganic cooperative assembly technique. The resulting materials were characterized by X-ray diffraction, Fourier transform (FT) Raman spectroscopy, atomic force microscopy, scanning electron microscope, and ellipsometer measurements. The results showed uniform, spherical, and pure anatase crystallites were present in the calcined sample. Moreover, the prepared nc-TiO₂ thin films are smooth and exhibit crack-free nature. A reasonable formation mechanism of uniform nc-TiO₂ thin films is also presented in this work.     

Preparation of TiO2–Na2O glass by sol–gel method and structural characterization

The applicability of sol–gel process in glass formation of binary system, (100 − x)TiO₂–xNa₂O (x = 10, 20, 30), was investigated and the glasses were prepared successfully by the sol–gel process for the first time. The process of glass formation was checked by using X-ray diffraction measurement and DTA–TG analysis. In the baking step, a DTA peak related to the crystallization of gel was found. The short-range structure of glassified samples was studied by neutron scattering measurement. It is found from the results of neutron scattering measurement that the coordination number of O atom around Ti atom is about 4, and the O atoms around Ti atom form a planer square rather than a regular tetrahedron.     

不同晶型TiO2的制备与光催化性能研究

采用溶胶凝胶法,利用不同温度热处理制备了不同晶体结构的TiO2纳米晶.利用XRD、SEM、EDS、XPS等分析方法对样品的晶体结构、形貌、化学元素组成以及价态进行了表征.结果表明400 ℃、500 ℃热处理TiO2为锐钛矿晶型,600 ℃ 热处理为锐钛矿金红石混合晶型,700 ℃热处理为金红石晶型,单颗粒子呈现类似球形形貌.以罗丹明B为目标污染物,测试了样品的光催化性能,结果表明400 ℃热处理TiO2具有最高的光催化活性,3 h后对罗丹明B的降解率达到94.6;,其反应速率常数达到0.969 h-1.     

Preparation and characterization of Nd doped gadolinium gallium garnet nanopowders and crystals

The structural and optical features of gallium gadolinium garnet (GGG) nanopowders doped with neodymium were investigated. Nanopowders of GGG:Nd were prepared by modified sol‐gel method using acetic acid as complexing agent. This way permitted to incorporate large amounts of dopant (up to 10 %) without destroying garnet structure. Small single crystals of Nd:GGG were grown by a μ‐pulling down method and spectroscopic features of nanopowders and their single crystal counterparts were compared. It has concluded that the Nd³⁺ ions are located preferentially in the same type of sites in crystal lattices of GGG:Nd nanopowders and their single crystal counterparts. In addition, it follows from the perfect agreement of emission wavelengths and line width recorded for nanopowders and single crystal samples that the crystal lattice of GGG in nanopowders is not distorted. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Multigram scale synthesis and characterization of low-density silica xerogels

The synthesis of silica with preserved porosity and tailored morphology by sol–gel process can be achieved by hybrid organic–inorganic synthesis: a modified alkoxide, viz. 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS), is introduced during the base catalysed synthesis with TEOS as main silica precursor. Additives with methoxy groups induce a nucleation mechanism because of their higher reactivity compared to main reagents with ethoxy groups. The nucleation model presented in previous papers was refined by taking into account the porosity of the particles and calculating the number of additive molecules by nucleus for each value of the ratio of additive/main reagent. The extrapolation of the synthesis process to semi-industrial scale goes through the replacement of laboratory grade reagents by industrial grade reagents and the scaling up to the production of higher quantities. At each of these two steps, the morphology and porosity of the samples has been compared to those of laboratory grade samples. It was shown that the texture and particle size has quasi totally been preserved.     

TiO2介孔材料的制备及其结构表征

以三嵌段高分子表面活性剂EO20PO70EO20(P123)为模板剂,异丙醇钛(TTIP)为无机母体源,采用溶胶-凝胶法制得稳定透明的TiO2凝胶,经煅烧后得到了TiO2介孔材料.分别用X射线衍射(XRD)、高分辨率透射电子显微镜(HRTEM)、N2吸附-脱附和紫外-可见分光光度计对TiO2介孔材料的结构、形貌、比表面积、孔径以及光催化活性进行了表征.所得结果表明:通过调整P123与TTIP的配比,在400℃下煅烧可得到局部结晶有序、比表面积大、催化活性高的TiO2介孔材料.     

氟改性TiO2的制备及光催化性能研究

以钛酸丁酯为钛源,氟化铵为氟源,采用溶胶凝胶法制备氟改性二氧化钛光催化剂,并用扫描电镜(SEM)、X射线衍射(XRD)、紫外可见光分度计(UV-Vis)、X射线光电子能谱(XPS)、光致发光荧光光谱仪(PL)、氮气吸附-脱附等方法对样品进行表征.以甲基橙(MO)为模拟污水,研究其光催化活性.结果 表明:F改性TiO2为纳米锐钛矿相,比表面积为141 m2/g.F以化学吸附态存在于TiO2的表面,形成(=)Ti-F基团,F的加入使得TiO2的吸收带边发生了红移,在甲基橙浓度为20 mg/L,紫外光照射时间为80 min时,F改性TiO2的脱色率最大达到了97;,具有较高的光催化活性.     

锡掺杂二氧化钛相变过程和微结构分析

本文采用溶胶凝胶法制备了锡掺杂纳米二氧化钛,通过高分辨透射电镜法(HRTEM),X-射线衍射法(XRD)等分析手段对样品的相变过程进行了表征.XRD和HRTEM测试表明纯二氧化钛在烧结温度高于500℃时出现金红石相,而25mol; Sn2+掺杂二氧化钛凝胶在300℃烧结2h后少量锐钛矿相析出的同时结晶出金红石相.实验结果表明Sn2掺杂抑制了锐钛矿和金红石相的晶粒长大;Sn2+掺杂明显地促进了锐钛矿向金红石的转变.Sn2氧化后形成Sn4+,Sn4+置换Ti4+而引起二氧化钛晶格膨胀的同时晶格畸变应力增加.     

Transparent oxide semiconductors based on TiO2 doped with V,Co and Pd elements

In this work, investigations of electrical and optical properties of as-deposited thin films of TiO₂ doped with Pd, Co and V elements prepared by the low-pressure hot-target reactive magnetron sputtering have been outlined. Results allowed to find out how selected properties of TiO₂ had changed from oxide non-conductor to oxide-semiconductor with desired p- or n-type electrical conduction due to the incorporation of the metal components, mentioned above.     

高热稳定性锐钛矿型Nd掺杂纳米TiO2的制备与表征

以钛酸丁酯为原料,采用溶胶凝胶法合成了纯TiO2与Nd掺杂TiO2纳米粉体,对其进行了350℃至850℃的热处理.利用XRD、SEM、和EDS对粉体的晶型结构,微观形貌和元素成分进行表征,研究了Nd掺杂对TiO2晶粒尺寸以及晶型转变的影响.结果表明:样品晶粒尺寸达到纳米级别,Nd掺杂后TiO2晶粒尺寸减小.纯TiO2在550℃时已经有金红石生成,750℃完成锐钛矿向金红石的转变;Nd掺杂TiO2在750℃时仍然是锐钛矿,850℃时有少许金红石生成,Nd掺杂提高了TiO2锐钛矿结构的热稳定性.     

高纯TiO2超微粉体的制备

以廉价的TiCl4为原料,液体石蜡为纯化剂,氨水作形核剂,制备出高纯TiO2超微粉体。用XRF分析了样品的物相组成;XRD和SEM等手段表征了粉体合成过程的物相变化和形貌特征。结果表明,TiCl4经过矿物油(液体石蜡)除钒和精馏除铁等杂质后进行水解,当TiCl4溶液浓度0.65 mol/L,水解温度60℃、反应时间2 h、pH值=7、在800℃煅烧2 h条件下,制备出TiO2的纯度达到99.9952%,晶型为金红石相,晶粒尺寸约0.65μm,形貌近球形。     

PAN/TiO2复合微粒的制备与表征

采用沉淀法合成聚丙烯腈(PAN),并通过化学吸附法制备得到PAN/TiO2纳米复合微粒.采用透射电镜(TEM)、X射线衍射(XRD)、红外光谱(IR)、X射线光电子能谱(XPS)、紫外可见漫反射吸收光谱(DRS)等方法对复合微粒的结构和性能进行了分析表征.结果表明,复合微粒的形貌、晶型和粒径和纯二氧化钛比较基本没有发生改变;PAN/TiO2纳米复合微粒在可见光区的光吸收能力增强.对甲基橙降解实验研究结果表明,所制备的PAN/TiO2纳米复合微粒具有良好的光催化降解性能,其14 h对甲基橙的降解去除率可以达到86.5;.     

Ag/TiO2的制备及光催化性能研究

以钛酸丁酯为钛源,采用溶胶-凝胶法制备了Ag掺杂纳米TiO2,结合XRD、TEM、Uv-vis等测试手段,对样品的结构和性能进行了表征.以甲基橙溶液为目标降解物,探讨了Ag掺杂纳米TiO2的光催化活性,分析了Ag掺杂纳米TiO2提高光催化性能的机理.结果表明,Ag掺杂使TiO2晶粒减小,拓展了TiO2的光谱响应范围,降低了光生电子和空穴的复合几率;Ag掺杂后,TiO2光催化剂的吸收光谱向可见光区发生红移.Ag掺杂量为n(Ag)∶n(TiO2)=0.08;,紫外光下240 min,Ag掺杂纳米TiO2前后材料对甲基橙溶液去除率由60.3;提高到83.1;.     

Ce掺杂TiO2纳米粉体的制备及其光催化性能研究

以钛酸丁酯为前驱体,冰醋酸为螫合剂,以硝酸铈为掺杂剂,采用溶胶.凝胶法制备了铈掺杂TiO2纳米粉体.研究了铈掺杂对TiO2相组成和晶粒尺寸的影响及不同掺杂量对TiO2光催化活性的影响,确定了Ce的最佳掺杂量.结果表明:Ce掺杂缩小了TiO2的锐钛矿相→金红石相(A→R)的相变温区范围,抑制了TiO2的晶粒增长.热处理温度升高,二氧化钛的比表面积下降.掺杂适量的铈提高了TiO2的光催化活性,Ce掺杂为0.05;摩尔分数时Ce-TiO2的光催化活性达到最佳,甲基橙降解率可达90;左右.     

SnO2负载TiO2纳米管的制备与光催化活性

结合阳极氧化法和脉冲沉积法合成SnO2/TiO2纳米管光催化剂,实现了SnO2纳米颗粒在TiO2纳米管表面的均匀负载.利用场发射扫描电子显微镜(FE-SEM)、能谱仪(EDS)、X射线衍射仪(XRD)以及紫外-可见漫反射光谱(UV-Vis DRS)对样品进行表征,以甲基橙为模拟污染物,评价了纳米管的光催化活性.结果表明,SnO2/TiO2纳米管经750℃煅烧后主晶相为锐钛矿相TiO2,含少量金红石相TiO2和SnO2,三者两两之间形成三元异质结,促进光生电子-空穴对的分离,此时SnO2/TiO2纳米管表现出最佳的光催化活性,紫外光下对甲基橙1 h分解比例由32.4;提升至96.5;.     

CeO2/TiO2异质结纳米花的制备及光催化性能研究

异质结催化剂以其优异的光电性能、光催化性能及在降解有机污染物上的实用性,吸引了广大研究者的注意.采用水热法,制备了CeO2/TiO2异质结纳米花,利用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)、和紫外-可见光吸收(UV-vis)等分析手段对制备的样品形貌和结构进行表征,并以甲基橙为目标污染物,考察了样品的光催化性能,并且对光催化降解的机理进行了分析.我们发现,这种异质结构将其紫外-可见光吸收边由紫外光区域拓宽到可见光区域,从而提高光响应范围.研究表明CeO2/TiO2异质结纳米花表现了优异的催化活性,在60 min内降解了98;的甲基橙,这主要是源于其特殊的异质结构,能增强光催化活性.     

超声辅助介孔纳米TiO2光催化剂制备与光催化性能

以钛酸丁酯为钛源,在高能超声的辅助作用下,通过溶胶-凝胶法合成了纳米TiO2光催化剂,利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和紫外-可见光光度计(UV-Vis)等对光催剂进行检测与表征.结果表明:高能超声的空化作用细化了纳米TiO2的显微结构,形成了分散有序的介孔结构.当超声频率为45 kHz时,纳米TiO2的晶粒尺寸约为12 nm,介孔孔道尺寸为10 nm,对有机污染物的有效降解率为92;.