三维有序大孔聚苯乙烯的制备及表征

采用播种生长法制备了粒径为330 nm的单分散胶体二氧化硅（SiO2），并对单分散的SiO2颗粒表面进行改性，以提高颗粒对苯乙烯单体的亲和力.然后通过垂直沉积法组装出SiO2胶粒晶体模板.依靠毛细管力将苯乙烯前驱物快速填充进模板颗粒的间隙，加热原位聚合 ，用氢氟酸去除模板后制得三维有序大孔聚苯乙烯.扫描电子显微镜结果显示，所合成的孔材料高度有序，孔腔尺寸约为210 nm，孔腔之间由较小孔窗连接，形成非常开放的通道网络 . 关键词： 三维有序大孔材料(3DOM) 聚苯乙烯 模板 二氧化硅     

三维有序大孔ZrO2的制备及其光学性质

以聚苯乙烯(PS)微球作为模板剂,采用溶胶-凝胶及煅烧处理等方法制备了三维有序大孔ZrO2材料。通过X射线衍射(XRD)以及扫描电镜(SEM)对其结构和形貌进行了表征。结果表明所制备的ZrO2材料为孔径约为180 nm的高度有序、堆叠紧密的三维有序大孔结构(3DOM)。对3DOM ZrO2的光谱分析表明:在宽禁带的ZrO2材料中存在着本征缺陷发光(氧空位缺陷)和杂质缺陷(主要杂质为TiO2)发光,掺杂浓度与基质的晶相结构对两种发光起到了至关重要的作用。对发光过程提出了简单的机理模型。     

低压化学气相沉积技术制备锗反蛋白石三维光子晶体

采用溶剂蒸发对流自组装法将单分散SiO2微球组装形成三维有序胶体晶体模板,用低压化学气相沉积法填充高折射率材料锗,酸洗去除SiO2模板,获得了锗反蛋白石三维光子晶体.通过扫描电镜、X射线衍射仪和紫外-可见-近红外光谱仪对锗反蛋白石的形貌、成分、结构和光学性能进行了表征.结果表明：锗在SiO2微球空隙内具有较高的结晶质量,填充致密均匀.通过改变沉积工艺,可控制锗的填充率;制备的锗反蛋白三维光子晶体具有明显的光学反射峰,表现出光学带隙效应.测试的光学性能与理论计算基本吻合.     

低压化学气相沉积技术制备锗反蛋白石三维光子晶体

采用溶剂蒸发对流自组装法将单分散SiO2微球组装形成三维有序胶体晶体模板,用低压化学气相沉积法填充高折射率材料锗,酸洗去除SiO2模板,获得了锗反蛋白石三维光子晶体.通过扫描电镜、X射线衍射仪和紫外-可见-近红外光谱仪对锗反蛋白石的形貌、成分、结构和光学性能进行了表征.结果表明:锗在SiO2微球空隙内具有较高的结晶质量,填充致密均匀.通过改变沉积工艺,可控制锗的填充率;制备的锗反蛋白三维光子晶体具有明显的光学反射峰,表现出光学带隙效应.测试的光学性能与理论计算基本吻合.     

多孔PMP聚合物薄膜微结构控制

将二氧化硅(SiO2)微球为模板材料分散在聚-4-甲基-1-戊烯(PMP)溶液中,通过对流自组装方法将其涂覆于基片上,经过热致相分离(TIPS)过程形成含SiO2微球模板的PMP薄膜,然后通过氢氟酸(HF)溶液腐蚀除去SiO2微球,获得了具有规则多孔结构的PMP聚合物薄膜。采用扫描电子显微镜(SEM)对含SiO2微球的PMP薄膜以及除去SiO2微球后的PMP多孔薄膜的微结构进行了表征。研究结果表明:SiO2微球在聚合物中呈有序排列,腐蚀除去SiO2微球后PMP薄膜有效复制了SiO2微球形成的有序结构,形成了有序多孔PMP薄膜。     

聚苯乙烯多孔薄膜的密度梯度控制

利用单分散的SiO2微球自组装制备了含一种尺寸微球的SiO2胶体晶体和含多种尺寸微球的多层异质结构。对含一种尺寸微球的SiO2胶体晶体进行煅烧和刻蚀处理后,胶体晶体中空隙所占比例大于立方密堆结构的26%,形成了非密堆结构,而且刻蚀时间越长,空隙比例越大。在同样的热处理和刻蚀条件下,微球尺寸越小的胶体晶体被刻蚀的程度越高,结构中空气空隙所占的比例越大。对SiO2多层异质结构经过煅烧和刻蚀处理后,得到了空隙梯度变化的多层结构,以此为模板制备了密度梯度变化的聚苯乙烯多孔薄膜。薄膜各层之间形成了平滑的过渡,没有显示出明显的层间缺陷,且孔与孔之间没有出现3维有序多孔结构中常见的大的连通孔道。     

低温等离子体增强化学气相沉积法制备Ge反opal三维光子晶体及其光学性能

通过溶剂蒸发对流自组装法制备SiO2三维有序胶体晶体模板,采用等离子体增强化学气相沉积法在200℃低温条件下填充高折射率材料Ge,获得了Ge反opal三维光子晶体.实现了低于GeH4热分解温度的低温填充.通过扫描电镜、X射线衍射仪和傅里叶变换显微红外光谱仪对Ge反opal的形貌、成分和光学性能进行了表征.结果表明:沉积得到无定型态Ge,退火后形成多晶Ge,Ge在SiO2微球空隙内填充致密均匀.Ge反opal的反射光谱有明显的光学反射峰,表现出光子带隙效应,其带隙中心波长为1650nm和2640nm,测试的光学性能与理论计算基本符合.采用SU-8光刻胶薄膜也进行了Ge沉积,证实了SU-8模板可以耐受这一沉积温度.低温沉积降低了Ge的填充温度,可以直接采用不耐高温的高分子材料作为初始模板,单次复型制备得到多种构型的完全带隙三维光子晶体.     

纳米Zn_2SiO_4∶Mn包覆SiO_2颗粒的制备及表征

采用水热合成方法添加KOH在SiO2颗粒表面包覆Mn2+掺杂纳米Zn2SiO4,通过X射线衍射(XRD)仪、扫描电子显微镜(SEM)、能谱、光致发光(PL)光谱仪对产物的晶体结构、形貌及光学性能进行表征,并对Zn2SiO4晶体在水热反应过程中的反应机制进行了讨论。XRD测试结果表明:220℃水热条件下,添加少量KOH,反应不同时间后,可在石英砂表面生成一层Zn2SiO4;SEM照片显示所生成的Zn2SiO4为六棱柱形,并且不同反应条件下Zn2SiO4的包覆程度不同。反应产物经光致发光性能研究表明:Mn2+掺杂纳米Zn2SiO4包覆SiO2样品中显示两套光致发光谱,一套为250nm左右激发产生的522nm绿色发光带,另一套为340～410nm宽带激发的440nm蓝色发光带,前者为典型的Mn2+离子发光,后者440nm发光带则有可能来源于基体SiO2的氧空位缺陷。     

介孔分子筛Al-MCM-41的合成与催化异构化性能

采用正硅酸乙酯(TEOS)为硅源,九水硝酸铝为铝源,十六烷基三甲基溴化胺(CTMABr)为模板剂,在室温条件下合成了介孔Al-MCM-41分子筛.通过XRD、N2等温吸附、SEM、FTIR等分析测试手段表征了分子筛的介孔结构和表面性质.结果表明所合成的分子筛有良好的介孔结构和较高的有序度,并且有较高的比表面积(达到816 m2·g-1)和窄的孔径分布.采用程序升温的焙烧方式、凝胶Al/Si比最大范围控制在0.06～0.13有利于合成高度有序的介孔Al-MCM-41分子筛.评价结果表明,所合成的Al-MCM-41分子筛对桥式四氢双环戊二烯(endo-TCD)异构化反应合成挂式异构体exo-TCD及金刚烷具有较高的催化活性和极高的选择性.     

Zn2SiO4∶Mn2+发光材料的低温合成及其发光性能

采用水热合成工艺低温制备了Mn2+掺杂的Zn2SiO4发光材料,采用X射线衍射(X-ray diffraetion,XRD)、扫描电子显微镜(Scanning electron microscope,SEM)对样品的结构和形貌进行观察,并以此分析了水热过程中Zn2SiO4的形成机制.采用吸收光谱、荧光光谱对其光吸收及光...     

Structural and cathodoluminiscent properties of Zr0.95Ce0.05O2 nanopowders prepared by sol-gel and template methods

Nanopowders of Zr_0.95Ce_0.05O₂ composition have been prepared by a standard Pechini-type sol-gel process and by means of a colloidal crystal template approach. In the latter method, inverse opal Zr_0.95Ce_0.05O₂ powders were fabricated employing poly(methyl methacrylate) (PMMA) colloidal crystals as a template. The effects of the two different synthesis routes on the structure and microstructural characteristics of the prepared nanopowders were evaluated by X-ray diffraction and scanning electron microscopy. For both preparation routes, the X-ray diffraction analysis has shown that a tetragonal fluorite structure is formed with a crystallite size of ∼35-40 nm. The scanning electron microscopy measurements indicate that the powder obtained by the sol-gel Pechini-type process is comprised of nanoparticles that are arranged in agglomerates with shape and size relatively uniform whereas the inverse opal Zr_0.95Ce_0.05O₂ nanopowders exhibit the formation of macropores with a mean size of ∼100 nm. The cathodoluminescence spectra of the prepared Zr_0.95Ce_0.05O₂ nanomaterials have been measured in the 300-800 nm wavelength range. The powder prepared by sol-gel method yields a broad emission band centered at 482 nm whereas the emission from the inverse opal preparation is considerably less intense.     

The instant-direct-templating synthesis of phenyl-functionalized HOM-type mesoporous silica materials

Two kinds of novel phenyl-functionalized mesoporous silica materials have fabricated for the first time by an instant-direct-templating method using poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) and tetraethyl orthosilicate as surfactant template and precursor, respectively. Samples were characterized by Fourier transform infrared spectroscopy, small-angle X-ray diffraction, thermogravimetric analysis, N₂ adsorption-desorption, scanning electron micrography and transmission electron micrography. The results show that phenyl groups are attached covalently to the pore wall of mesoporous materials after modification. The functionalized materials still preserve a desirable ordered hexagonal P6mm and cubic Ia3d mesophase structure, respectively, have high specific surface area, large pore volume and narrow pore size distribution.     

Preparation of Manganese Oxide Hollow Spheres Using pH-responsive Microgels as Templates

以pH响应型微凝胶为模板制备出了二氧化锰空心球材料,并利用XRD、TGA、SEM、FT-IR和TEM等手段对其进行了表征. 结果表明,通过调节KMnO₄的用量可以有效控制二氧化锰空心球的球壳厚度. 对洗脱后上层清夜中的pH响应型微凝胶进一步研究发现,部分微凝胶呈现出非可逆的膨胀-收缩转变,这一现象主要是由于其内部的交联程度不高造成的. 在对表征结果进行分析后提出了空心球结构的形成机理.     

Electric-field-assisted self-assembly of colloidal particles

A method for formation of photonic crystals has been proposed. The method is based on convective deposition of colloidal particles onto vertical substrates in the presence of a direct-current electric field directed perpendicular to the surface of the formed film and an alternating-current electric field applied parallel to the substrate plane. The structure and optical properties of the prepared colloidal crystals have been investigated using scanning electron microscopy, high resolution small-angle X-ray diffraction, and optical spectroscopy.     

石墨炉内石墨探针表面上的原子化机理研究 Ⅳ钒的原子化机理

本文通过X-射线衍射分析(XRD),扫描电子显微镜分析(SEM),化学分析光电子能谱分析(ESCA),并结合原子吸收测量,研究了钒在普通石墨管中石磨探针表面上发生的固相化学反应。结果表明,钒化合物在灰化阶段即可转化为热稳定性较高的碳化物,原子化的最后步骤为碳化物的热分解。     

Template synthesis of well-aligned titanium dioxide nanotubes

TiO₂ nanotubes of the anatase form have been synthesized by sol-gel chemical method using anodic aluminum oxide (AAO) as a template. Transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X-ray diffraction were used to investigate the structure and morphology of the TiO₂ nanotubes. The results showed that TiO₂ nanotubes obtained are highly ordered and uniform. The diameter and length of the obtained nanotubes were determined by the pore size and the thickness of AAO template. It was found that through control of immersion time of AAO membrane in sol, both tubules and fibrils can be prepared. PACS 61.46.+w     

Electrochemical template-assisted fabrication of CdS micro/nanostructures

One-dimensional (1D) cadmium sulphide (CdS) nanostructures, including micro/nanorods, and nanostructures resembling flowers and cactus have been synthesized by electrochemical template deposition technique, using polycarbonate membranes, by controlling various reaction parameters. These 1D CdS nanostructures were characterized structurally through the X-ray diffraction (XRD) studies and morphologically through scanning electron microscopy (SEM). It was found that apart from the dimensions of the pores of the templates, the geometrical morphologies of the CdS 1D nanostructures were significantly influenced by the synthesizing parameters also. The optical characterization has been done by UV–visible absorption and room-temperature photoluminescence (PL) studies.     

Electrochemical template-assisted fabrication of CdS micro/nanostructures

One-dimensional (1D) cadmium sulphide (CdS) nanostructures, including micro/nanorods, and nanostructures resembling flowers and cactus have been synthesized by electrochemical template deposition technique, using polycarbonate membranes, by controlling various reaction parameters. These 1D CdS nanostructures were characterized structurally through the X-ray diffraction (XRD) studies and morphologically through scanning electron microscopy (SEM). It was found that apart from the dimensions of the pores of the templates, the geometrical morphologies of the CdS 1D nanostructures were significantly influenced by the synthesizing parameters also. The optical characterization has been done by UV–visible absorption and room-temperature photoluminescence (PL) studies.