聚(N-异丙基丙烯酰胺)模板法制备二氧化硅中空微球

以在50 oC水溶液中析出的聚(N-异丙基丙烯酰胺) (PNI-PAM)聚集体作为软模板,使正硅酸乙酯吸附在PNIPAM聚集体表面进行水解缩合,原位生成二氧化硅包裹PNIPAM的核壳结构微球;进一步冷却至室温使PNIPAM溶解在水中除去内核,从而成功合成出SiO₂中空微球．实验表明,只有在足够的PNIPAM和正硅酸乙酯含量以及正硅酸乙酯水解时间下,才能形成稳定的SiO₂中空微球．用TEM、SEM和FTIR对合成的SiO₂中空微球进行了表征,结果表明,微球尺寸为150 nm左右,并且由于PNIPAM上酰胺基团和正硅酸乙酯水解出来的硅醇间具有静电相互作用,使得SiO₂壳层上依然有PNIPAM残留.     

热处理温度对蛋白石晶体的影响

 采用等体积快速混合法制备了不同粒径的单分散SiO₂微球,通过重力垂直沉降自组装形成了蛋白石模板,研究了热处理温度对蛋白石晶体模板形貌、结构与光学性能的影响。SEM,TG-DSC,UV-Vis等分析表明：热处理可提高组装微球的粘合性与模板的机械强度;SiO₂胶体模板煅烧温度在700～800 ℃较为合适;热处理能够改变蛋白石晶体光子带隙的位置,随着煅烧温度的升高,带隙发生蓝移并且带隙逐渐变窄。     

利用聚乙烯亚胺修饰的CaCO3仿生模板合成3D花朵型二氧化硅微球

利用聚乙烯亚胺(PEI)修饰的碳酸钙仿生模板合成了具有3D花朵型形貌的SiO₂微球.通过调整碳酸钙微粒表面不同浓度PEI的吸附量实现SiO₂微球的形貌控制呈现花朵或刀锋的形状. 用XPS和SEM对制备的SiO₂微粒进行表征. 结果表明,不用浓度的PEI修饰可以较好地控制3花朵型DSiO₂微球的形貌.     

沉降介质对单分散SiO2微球重力组装欧泊模板的影响

 以氨水作催化剂、正硅酸乙酯为硅源、乙醇为溶剂,采用改进溶胶-凝胶法制备了系列单分散SiO₂微球,研究了平均粒径为250,280,320 nm单分散SiO₂微球在水、无水乙醇、丙酮等介质中的沉降与自组装过程。还对单分散体系重力沉降组装欧泊模板的形成机理进行了讨论。SEM表明,微球在无水乙醇和丙酮沉降介质中均能组装形成3维有序密堆积结构的欧泊,但在无水乙醇中要优于在丙酮中。沉降速度实验表明,相同粒径的单分散SiO₂微球在水、乙醇、丙酮作为沉降介质中的沉降速度相差并不大,沉降介质对重力水平沉降组装模板的影响主要是由于其表面张力与粘度不同造成的。     

Eu(TTFA)3掺杂SiO2杂化胶体球的合成及特性

采用改进的碱催化法和种子法分别制得了稀土配合物Eu(TTFA)₃掺杂的SiO₂杂化胶体球,并用透射电子显微镜和荧光分光光度计对其显微形貌和荧光光谱特性进行了详细地研究.结果表明,两种方法都可以获得单分散性的、稀土配合物掺杂SiO₂杂化胶体球,且都具有Eu³⁺离子典型的荧光光谱特性.Eu(TTFA)₃掺杂入SiO₂胶体球中后,有机配体TTFA在短波长处的吸收明显增强了,最大的吸收峰位也向短波长方向移动大约20～30 nm,Eu³⁺离子5D0→7F2发射跃迁仍然具有良好的窄线发光特征,同时荧光峰值的形态和位置受SiO₂基体的影响发生轻微的变化.     

BiVO4空心微球的合成及其光催化降解亚甲基蓝的性能研究

以BiNO₃·5H₂O和NH₄VO₃为原料,柠檬酸为络合剂,成功合成了BiVO₄空心纳米球．采用TEM、XRD、UV-Vis等测试技术对样品的形貌、相结构以及光吸收性能等进行了表征．结果表明,所制备的BiVO₄空心微球在紫外区和可见区均有较强的光吸收,空心球平均粒径为160 nm,空腔直径为10～80 nm．以亚甲基蓝染料溶液的脱色降解实验为模型反应研究了样品的光催化性能．光催化实验结果表明,在可见光照射下,反应150 min后,样品对亚甲基蓝溶液的脱色率可达到95%以上．此外,考察了柠檬酸添加量对空心球形貌的影响,并提出了BiVO₄空心纳米球的可能形成机理．     

介孔SiO2纳米棒的制备及其表面锚接金纳米粒子

 以正硅酸乙酯为硅源,十六烷基三甲基溴化铵为模板剂,聚乙二醇为分散剂,采用溶胶-凝胶法制备出SiO₂纳米粒子,应用透射电镜、扫描电镜、X射线衍射仪、红外光谱仪和X射线能谱仪研究了粒子的性能。结果表明：所得产物是具有周期性规则介孔的棒状粒子,长径比随着硅源、模板剂和分散剂浓度的降低而减小;向反应体系中引入乙醇,随着乙醇与水的体积比例的增加,粒子由棒状向球状转变,进而形成不规则絮状凝聚体。用硅烷化技术对SiO₂纳米棒表面进行修饰后吸附平均粒径3.7 nm的金种子,再用多轮生长法使种子长大,经过30轮生长,种子平均粒径增大至59 nm,得到了SiO₂-Au复合纳米体系。透射电镜和紫外-可见分光光度计分析结果表明：金纳米粒子锚接在SiO₂纳米棒表面的某些点位,呈分散分布;复合体系表现出强烈的金的表面等离子体共振吸收峰,该峰随着金粒子的粒径增大,在500~700 nm波段内红移。     

采用溶胶凝胶协同自组装方法制备SiO2反蛋白石结构薄膜及其光学性质研究

研究了溶胶凝胶协同自组装制备大面积高质量SiO₂反蛋白石结构薄膜的方法. 向单分散的聚苯乙烯(PS)胶体溶液中添加SiO₂前驱物溶液,用垂直自组装法一步得到微球空隙中均匀填充有凝胶的 复合PS胶体晶体薄膜,在空气中烧结去除PS后得到SiO₂反蛋白石结构薄膜.通过对添加前驱物溶液比例、 自组装温度以及烧结温度等参数的研究,用不同粒径的PS微球制备了不同孔径的高质量SiO₂反蛋白石结构薄膜. 用扫描电子显微镜和X射线能量色散谱仪对制备得到的薄膜样品进行显微形貌和成分表征,并测试了其透射光谱. 结果表明:溶胶凝胶协同自组装法制备的SiO₂反蛋白石结构薄膜大面积高度有序,孔径可以控制且选择范围宽; 薄膜的透射光谱带隙明显,带隙中心波长与理论计算结果相符.     

层间热处理对SiO2/ZrO2双层膜的影响

 以正硅酸乙酯和丙醇锆为前驱体,用溶胶-凝胶法在K9基片上提拉镀制SiO₂/ZrO₂双层膜。采用不同实验步骤制备了2个样品,样品1镀完SiO₂后直接镀ZrO₂ ,样品2镀完SiO₂经热处理后再镀ZrO₂。采用原子力显微镜、椭偏仪、紫外-可见分光光度计对薄膜进行表征。针对SiO₂/ZrO₂双层膜,考虑到膜间渗透的影响,采用３层Cauchy模型进行椭偏模拟,椭偏参数的模拟值曲线与椭偏仪的测量值曲线十分吻合,进而发现热处理可以使SiO₂/ZrO₂双层膜之间的渗透减少近23 nm,从而提高其峰值透射率。利用输出波长1.064 mm,脉宽8.1 ns的激光束对样品进行了损伤阈值的测试,用光学显微镜观察损伤形貌,结果发现两者损伤阈值分别为13.6 J/c2和14.18 J/cm²,均为膜的本征损伤。     

三维海胆状Co3O4的微纳结构制备及锂电池性能

水热法制备的合成海胆状Co₃O₄前驱物在空气中退火得到三维海胆状Co₃O₄的微纳结构. 采用FESEM、TEM、HRTEM以及XRD对产物进行形貌和结构的表征. 结果表明,合成的海胆状结构Co₃O₄由许多粒径约为15 nm的颗粒串接形成. 锂电池测试性能表明,制备的海胆状Co₃O₄首次放电容量达到1.369 Ah/g,经过20次循环     

二氧化硅增透膜微观结构与激光损伤阈值的调控

采用溶胶-凝胶技术制备了二氧化硅增透膜,通过向溶胶中添加高分子聚乙烯醇缩丁醛（PVB）,调控胶体的粒径,进而控制膜层微观结构,研究膜层微观结构与激光损伤阈值的关系。纳米粒度仪和扫描探针显微镜测试表明:PVB加入溶胶后,控制了二氧化硅胶粒的生长,使二氧化硅胶粒生长更均匀,因而膜层的微观结构更均匀。当PVB质量分数为1%时,胶体粒径为15 nm,分散系数小于0.1。用该胶体镀膜,膜层均匀,表面粗糙度小于3.25 nm。并且PVB加入后增加了膜层胶粒间的黏附性,使得膜层强度增大。PVB加入使膜层的激光损伤阈值有所增加。当PVB的添加量为1%时,膜层的激光损失阈值从30.0 J/cm2增加到40.1 J/cm2。膜层激光损伤阈值的增加与膜层微观均匀性和物理强度的增加有关。     

Synthesis and characterization of hydrophobic silica nanocomposites

Hydrophobically modified silica nanocomposites have been prepared using a low temperature sol-gel process. In this study, an alkyltriethoxysilane derivative, hexdecyltrimethoxysilane (HDTMS), was co-condensed with tetraethoxyorthosilicate (TEOS) with and without a cross-linking agent, 3-glycidoxypropyltrimethoxysilane (GPTMS), to produce the modified composites. The hydrophobic properties were determined using contact angle measurement. FESEM observations revealed a semispherical nanostructure of the composites with grain size of about 50-75 nm in diameter. The chemical modification was studied by FTIR and EDX, whereas the physicothermal properties were analyzed by DSC and TGA. These long-chain alkyl modified silica nanocomposites are promising materials for use in hydrophobic and water-resistant applications.     

SiO2干凝胶中CdS量子点的光致发光性质

以正硅酸乙酯(TEOS)为SiO2的前驱物,硝酸镉为镉源,硫脲为硫源,用溶胶-凝胶法制备了CdS量子点掺杂的SiO2干凝胶,利用XRD、紫外-可见吸收光谱、光致发光谱对其性质进行研究.样品的测试结果表明在SiO2干凝胶的网状结构中形成了CdS量子点,平均粒径为5.1 nm.SiO2凝胶中CdS吸收峰位置明显蓝移.在一定...     

Sonochemical coating of magnetite nanoparticles with silica

Magnetite nanoparticles were coated with silica through the hydrolysis and condensation of tetraethyl orthosilicate (TEOS) under ultrasonic irradiation. The ultrasonic irradiation was used to prevent the agglomeration of the magnetite particles and accelerate the hydrolysis and condensation of TEOS. TEM, DLS, XRF, VSM, TG and sedimentation test were used to characterize the silica-coated magnetite particles. The dispersibility of silica-coated magnetite particles in aqueous solution was improved significantly and the agglomerate particle size was decreased to 110 nm. It was found that the agglomerate particle size of silica-coated magnetite particles was mainly decided by the coating temperature and the pH value in the silica-coating process. The weight ratio of silica in silica-coated magnetite particles was mainly decided by the pH value in the silica-coating process. The dispersibility of silica-coated magnetite particles was mainly decided by the agglomerate particle size of the suspension. The oxidation of magnetite particles in air was limited through the coated silica. The magnetism of silica-coated magnetite particles decreased slightly after silica-coating.     

Synthesis of core–shell nanoparticles with a Pt nanoparticle core and a silica shell

A method to prepare a core–shell structure consisting of a Pt metal core coated with a silica shell (Pt(in)SiO₂) is described herein. A silica shell was grown on poly(vinylpyrrolidone) (PVP)-stabilized Pt nanoparticles 2–3 nm in size through hydrolysis and condensation reactions of tetraethyl orthosilicate (TEOS) in a water/ethanol mixture with ammonia as a catalyst. This process requires precise control of the reaction conditions to avoid the formation of silica particles containing multiple Pt cores and core-free silica. The length of PVP molecules, water content, concentration of ammonia and Pt nanoparticles in solution were found to significantly influence the core–shell structure. By optimizing these parameters, it was possible to prepare core–shell particles each containing a single Pt nanoparticle with a silica layer coating approximately 10 nm thick.     

单甲基原位改性SiO2疏水减反膜的制备与性能研究

 在碱性条件下通过TEOS和MTES的共水解缩聚反应制备了单甲基原位改性的SiO₂溶胶，并使用提拉法在K9玻璃基片上镀制了疏水减反膜。通过透射电镜（TEM）考察了镀膜溶胶的微结构，分别使用红外光谱（FTIR）分析了薄膜的组分，用原子力显微镜（AFM）观察了薄膜的表面形貌和起伏状况，用紫外可见光谱（UV-vis）考察了薄膜的减反射性能，用接触角仪测量了薄膜对水的接触角。并使用“R-on-1”的方式测量了薄膜在Nd:YAG激光（1 064 nm，1 ns）作用下的损伤阈值。结果表明，通过共水解缩聚反应可以把甲基引入镀膜溶胶簇团中，改善了溶胶簇团的网络结构，使薄膜得到相当好的疏水性能和更好的抗激光损伤性能，同时薄膜能保持较好的减反射性能。     

丹酰氯SiO2纳米发光标记物的制备

通过合成丹酰氯的荧光单体硅酯前驱物,采用油包水的反相微乳液法,以丹酰氯的荧光单体硅酯前驱物为核材料,成功地制备了丹酰氯的荧光纳米颗粒,克服了传统方法制备核壳荧光纳米颗粒中存在的荧光染料泄漏问题.通过透射电子显微镜表征该纳米粒子呈球形,大小均匀,直径为40nm左右.所制得纳米颗粒荧光性质稳定,受外界环境的影响小,且潜在生物亲和性,是一种新型的荧光标记物.     

超声波酸性体系下MCM-41的合成及表征

以十六烷基三甲基溴化铵(CTAB)为模板剂,正硅酸乙酯(TEOS)为硅源,以超声波为辅助手段于酸性介质中制备出了MCM-41介孔分子筛,采用XRD、TEM、FTIR等手段对样品进行了分析表征.结果表明,所合成样品具备MCM-41所特有的六方排列的一维孔道结构和较高的有序度,所合成的MCM-41平均粒径为11nm,孔径约为2.7nm.     

Gravitational sedimentation effect of colloidal silica crystals in binary systems of titanium dioxide and silica particles

Colloidal crystals can be formed of silica particles while those of titania particles are not known under the normal gravitational field, because of their high specific gravity. We found by the Kikuchi--Kossel diffraction technique that, when silica particles (diameter: D?=?170?nm; density: ρ?=?2.2?g cm^?3) are mixed with titania particles (D?=?127?nm; ρ?=?3.9?g cm^?3), colloidal crystals are formed. Colloidal crystals started out with body-centred-cubic structure and changed to face-centred-cubic structures after about 60 days. Transitions began from the bottom of the container. Thus, the transitions are considered to be due to gravitational sedimentation. It is significant that the crystal growth process, which has not been observed in one-component dispersions of the silica particles, was found using titania particles with a wide range of the practical applicability.     

Particle Sampling and Real Time Size Distribution Measurement in H2/O2/TEOS Diffusion Flame

Growth characteristics of silica particles have been studied experimentally using in situ particle sampling technique from H₂/O₂/Tetraethylorthosilicate (TEOS) diffusion flame with carefully devised sampling probe. The particle morphology and the size comparisons are made between the particles sampled by the local thermophoretic method from the inside of the flame and by the electrostatic collector sampling method after the dilution sampling probe. The Transmission Electron Microscope (TEM) image processed data of these two sampling techniques are compared with Scanning Mobility Particle Sizer (SMPS) measurement. TEM image analysis of two sampling methods showed a good agreement with SMPS measurement. The effects of flame conditions and TEOS flow rates on silica particle size distributions are also investigated using the new particle dilution sampling probe. It is found that the particle size distribution characteristics and morphology are mostly governed by the coagulation process and sintering process in the flame. As the flame temperature increases, the effect of coalescence or sintering becomes an important particle growth mechanism which reduces the coagulation process. However, if the flame temperature is not high enough to sinter the aggregated particles then the coagulation process is a dominant particle growth mechanism. In a certain flame condition a secondary particle formation is observed which results in a bimodal particle size distribution.