热处理温度对核-壳型SiO2@TiO2复合纳米材料光催化性能的影响

采用溶胶-凝胶法在二氧化硅(SiO2)纳米微球表面负载纳米二氧化钛(TiO2),制备核-壳SiO2@TiO2复合纳米颗粒.采用X射线衍射仪(XRD)、环境扫描电子显微镜(SEM-EDS)、比表面积测定(BET)等研究手段对样品的矿物组成、结构形貌进行了表征,并考察了其光催化活性.结果 表明:溶胶-凝胶法后期的热处理明显提高了核-壳SiO2@TiO2复合纳米颗粒光催化降解亚甲基蓝溶液的能力,其中,经过400℃热处理的样品催化效果最好,对质量浓度为20 mg/L的亚甲基蓝溶液90 min的降解率达到96.27％.     

微乳液法制备纳米二氧化硅粉末工艺的研究

采用微乳液法制备了高比表面积纳米SiO2粉末,考察了微乳液体系的配制、反应物浓度、反应温度、焙烧温度、共沸蒸馏脱水工艺制备的纳米SiO2性能的影响,并通过比表面积(BET)、透射电镜(TEM)、红外光谱分析(IR)、X射线衍射(XRD)对样品进行了表征.结果表明,粉末制备的工艺参数对样品性能影响较大,在较佳工艺条件下制备的纳米SiO2粉末近似呈球形,粒径为15～30nm,比表面积高达580～630m2/g .共沸蒸馏工艺能充分地脱去凝胶中残余的水分,防止因含水胶体干燥过程引起的粉末硬团聚,从而显著地提高了粉末的性能.     

纳米SiO2/TiO2复合粉体的制备及表征

以Na2SiO3为原料,采用非均匀成核法在纳米TiO2基体上制备了SiO2表面保护膜层,通过红外光谱、X射线光电子能谱、扫描电镜、粒径测量、BET比表面积测量分析,证实纳米TiO2颗粒表面包覆了一层均匀致密的SiO2纳米膜,而且两者是以化学键合方式结合在一起。分散性能测试表明:纳米SiO2/TiO2复合粉体的分散性能明显提高。     

多层陶瓷电容器用纳米复合粉添加剂的制备研究

采用溶胶-凝胶法及超临界干燥技术按多层陶瓷电容器磁粉添加剂配方比例制备Bi、Sr、Ce、Mn和Si的化合物纳米复合粉.以DTA、SEM、XRD等检测方法对纳米复合粉的表面形貌、粒度、晶相组成等进行表征.研究结果表明:温度为50℃,pH值为-0.25,H2O/TEOS=9/1(V/V),并加入占TEOS体积5%的硅烷偶联剂KH570,可以制备得到复合物体系的稳定凝胶.以无水乙醇为超临界萃取剂,进行超临界干燥,煅烧温度约高于700℃,得到分散性较好的纳米复合粉体,粉体一次颗粒径约为40～60hm,粉体形貌近似球型.复合粉的主要晶相为Bi2SiO5、CeO2和sr2Mn205.     

多层陶瓷电容器用的SrTiO3纳米粉体制备

采用溶液-溶胶-凝胶法,从Sr(NO3)2-Ti(OC4H9)4-H2O-C2H5OH体系制备多层陶瓷电容器用的纳米SrTiO3粉体.用热重-差示扫描分析研究了由前驱体干凝胶形成纳米SrTiO3粉体的加热过程.用X射线衍射等方法研究了醋酸、水、温度对凝胶化、纳米SrTiO3粉体的粒径和比表面积的影响.用扫描电镜和透射电镜观察了纳米SrTiO3粉体的形貌和颗粒大小.所制备的SrTiO3粉体分散性好,粒径为40～50 nm,比表面积为9～10 m2/g.     

国内期刊荟萃

水性聚氨酯-SiO2/TiO2复合涂料的制备与研究魏阳等.聚氨酯工业,2004,19(6):17采用溶胶-凝胶法制备了SiO2/TiO2纳米复合微粒,将其分散在聚醚型水性聚氨酯中,制备了新型水性聚氨酯-SiO2/TiO2复合涂料。经FTIR和TEM测试表明,纳米TiO2颗粒表面成功地包覆上SiO2。在聚氨酯乳液中复合微粒粒径为60nm左右;分光光度法测试表明TiO2质量分数为20%的复合微粒在聚氨酯水乳液中具有良好的分散性能;而加入质量分数为1%的十二烷基磺酸钠后,对SiO2/TiO2纳米粉末的分散性能改善最大;力学性能测试表明加入SiO2/TiO2纳米复合微粒质量分数为0.6%时…     

用于甲烷干法重整的Ni/SiO_2纳米复合空心结构催化剂

采用水热法制备了具有片层结构的Ni/SiO2纳米复合空心结构催化剂,研究了其对甲烷干法重整(DRM)反应的催化活性和稳定性,并以传统浸渍法制备的Ni/SiO2催化剂作为参照样。结果表明,Ni/SiO2纳米复合空心结构催化剂有很高的比表面积(405.6 m2/g)和显著提高的高温抗烧结与抗积碳能力。这归因于该复合空心结构以片层状镍硅酸盐为前驱体,金属镍纳米颗粒由前驱体在氢气气氛中高温还原分解得到,使得该结构具有很强的金属纳米颗粒与载体之间的相互作用,因而具有优异的催化性能。     

纳米SiO2／胶清橡胶复合材料力学性能的研究

采用乳液共混法,研究了纳米SiO2/胶清橡胶复合材料的力学性能.结果表明,采用乳液共混法制备纳米SiO2/胶清橡胶复合材料的力学性能优于机械共混法.纳米SiO2改性剂(硅烷偶联剂 TESPT)用量为7.5%～10%,搅拌时间为30min,纳米SiO2用量为20～30份,可制备出力学性能较好的纳米SiO2/NR复合材料.     

水/油微乳液技术制备单分散纳米CeO2

在十六烷基三甲基溴化铵 正丁醇/环己烷/水溶液组成的水/油型微乳液体系中,运用微乳液制备纳米粒子的原理,利用改进的两相液液法,测定了水/油微乳液的区域,并制备了纳米CeO2粉体.对制备得到的CeO2粉末的形貌特征、物相结构、成分等用透射电子显微镜、X射线衍射分析、热重-差示扫描量热法和红外光谱测试进行了表征.结果表明:在测定的微乳液区内能制备出颗粒分散性好,粒度分布均匀的纳米CeO2粒子,所得颗粒尺寸为3 nm左右.     

两步反相微乳液法原位制备纳米SiO2/聚甲基丙烯酸甲酯复合微粒

采用两步反相微乳液法原位聚合制备纳米SiO2／聚甲基丙烯酸甲酯(polymethylmethacrylate,PMMA)复合微粒。首先,通过混合2个分别增溶有2种反应物的微乳液,制备纳米SiO2粒子;然后,向混合后的微乳液中滴加单体及引发剂,通过单体的原位聚合反应得到SiO2,PMMA复合微粒。通过相图研究：确定了微乳液法制备复合微粒时初始组分的用量。通过透射电子显微镜、红外光谱、热重分析、X射线光电子能谱等手段对复合微粒进行了表征。结果表明：聚合后的PMMA包覆在SiO2表面．复合微粒的平均粒径为30nm．分散性良好。复合微粒中不能被抽提出来的聚合物占10．08％,这部分聚合物以Si-O-C键形式接枝在SiO2表面。     

SO_4~(2-)/SiO_2-ZrO_2复合固体超强酸催化α-蒎烯水合反应

以硫酸锆和硅胶为主要原料在水热条件下合成了SiO2 ZrO2复合体,晶化温度150℃,晶化时间24h。用c(H2SO4)=0 25mol/L水溶液处理焙烧过的SiO2 ZrO2复合体,经焙烧后制得SO2-4/SiO2 ZrO2复合固体超强酸。用FTIR、XRD、BET及NH3-TPD等技术表征了其结构。结果表明,该催化剂存在超强酸中心,比表面积高达203 7m2/g,孔径为16 6nm,孔容为0 8cm3/g,但不具有中孔分子筛的特征结构。将SO2-4/SiO2 ZrO2复合固体超强酸用于催化α 蒎烯水合反应,α 蒎烯的转化率接近100%,对α 松油醇的选择性达50%;该催化剂重复使用5次后,α 蒎烯的转化率由开始的100%变为83 5%,对α 松油醇的选择性仍为50%,表明该催化剂具有良好的重复使用性能。     

SiO_2钛酸钾晶须复合微粒的制备及性质研究

通过溶胶凝胶法制备了SiO2均匀包覆钛酸钾晶须(PTW)的核壳式复合微粒,并通过SEM、EDS、XRD、FTIR对这种复合微粒进行了表征。未处理的PTW在pH=2.0的酸性溶液中开始被腐蚀,并能被煮沸的浓硫酸所溶解;而SiO2PTW复合微粒耐酸性增强,在浓硫酸中煮沸40min后,仍能保持纤维形貌。PTW表面的SiO2壳层可以阻碍PTW中水溶性钾离子的析出。     

超重力反应沉淀法制备超细二氧化硅

以水玻璃和硫酸为原料，采用超重力反应沉淀法合成了超细二氧化硅粉体。研究表明：与传统搅拌槽反应器相比，在超重力反应器内，二氧化硅沉淀反应的时间可大大缩短（缩短至10min以内）；通过产品分析测试发现，所得到的二氧化硅产品具有粒径小（〈20nm）、粒度均匀、比表面积大、孔径分布较窄等特点，并具备能提高与高分子材料的相互作用的中大孔结构。     

Preparation and characterization of platinum-ruthenium bimetallic nanoparticles using reverse microemulsions for fuel cell catalyst

Platinum-ruthenium bimetallic nanoparticles are prepared by chemical reduction using sodium borohydride in reverse microemulsions of water/isooctane/Igepal CA-630/2-propanol for fuel cell catalysts. The prepared nanoparticles are characterized by transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and energy-dispersive X-ray analysis. The average size and morphology of nanoparticles are dependent on the water volume fraction in reverse microemulsion system in the range of ca. 2-4 nm. The morphology of particles is related with the percolation behavior of water droplets in reverse microemulsions. By the pretreatment of water phase using a hydrochloric acid, the particles of a homogeneous solid solution state can be obtained. The CO stripping cyclovoltammetry and the electrochemical measurements compared with commercial catalyst show that the prepared particles have a high electrochemically active surface area and a stable and high catalytic activity for reformate gas oxidation.     

机械化学法改性纳米SiO_2粒子(英文)

利用机械化学法对纳米SiO2进行了表面修饰改性。首先通过高速机械冲击将纳米SiO2粒子镶嵌在微米级的CaCO3粒子表面形成草莓结构的CaCO3/SiO2复合粒子,从而阻止纳米SiO2的团聚。而后又以六甲基二硅氮烷(hexmethyldisilazane,HMDS)和γ-氨丙基三乙氧基硅烷KH550为改性剂对CaCO3/SiO2复合粒子进行了表面改性。用红外光谱和热重分析对复合粒子进行了表征与分析。考察了搅拌速度、CaCO3/SiO2配比、改性温度、改性时间和改性剂用量对CaCO3/SiO2复合粒子形貌和表面改性效果的影响。结果表明:在搅拌速度为6500r/minCaCO3与SiO2的质量比为5:1,以HMDS为改性剂在200℃反应90min时,对纳米SiO2的改性效果最好。CaCO3/SiO2复合粒子既保持了纳米SiO2的纳米效应,同时又具有多重表面结构,在橡胶补强填料和超疏水涂层制备方面有着广阔的应用空间。     

Preparation and properties of composite mineral powders

Mineral powders such as ground calcium carbonate (GCC) and wollastonite are widely used as fillers in plastics, rubber, paper, paints and other fields. The interface compatibility between the polymer matrix and the mineral particles is relatively weak, both because of the smooth cleavage surface and the sharp particle edges formed during pulverizing. It is beneficial therefore to modify the surface properties of mineral powders before they are used in a polymer composite. In this paper, we report the successful preparation of composite mineral particles, coated by nanoparticles of calcium carbonate of 20-100 nm particle size, by chemical reaction using the Ca(OH)₂-H₂O-CO₂ system. The degree of nanoparticle coverage can reach 100% if the operating parameters are effectively controlled, and the specific surface area can be increased to three times the value before modification. Mechanical testing of polypropylene containing composite wollastonite powder as a filler shows an increase in the impact strength of 65% compared to similar samples prepared using conventional filler powder.     

包覆型CeO_2/SiO_2和CeO_2/聚苯乙烯复合磨料的制备及其化学机械抛光性能

以SiO2和聚苯乙烯(polystyrene,PS)微球为内核,采用液相沉淀工艺制备了具有包覆结构的CeO2/SiO2和CeO2/PS复合颗粒。利用X射线衍射仪、透射电子显微镜、场发射扫描电子显微镜、X射线光电子能谱仪、动态光散射仪和zata电位测定等手段对所制备样品进行了表征。将所制备的CeO2/SiO2和CeO2/PS复合颗粒用于硅晶片热氧化层的化学机械抛光,用原子力显微镜(atomic force microscope,AFM)观察抛光表面的微观形貌、测量表面粗糙度。结果表明:所制备的CeO2/SiO2和CeO2/PS复合颗粒呈球形,粒径在150～200nm,CeO2纳米颗粒在SiO2和PS微球内核表面包覆均匀。包覆的CeO2颗粒与SiO2内核之间形成了化学键结合。CeO2颗粒的包覆显著的改变了复合颗粒的表面电性。AFM测量结果表明:经CeO2/SiO2和CeO2/PS复合磨料抛光后的硅热氧化片表面在5μm×5μm范围内粗糙度值分别为0.292nm和0.180nm。     

ACR/纳米SiO2复合粒子的合成及其对PVC的增韧作用

研究了细乳液聚合制备ACR/纳米SiO2复合粒子及其对PVC的增韧作用。对丙烯酸酯单体中的纳米SiO2粒子进行偶联改性,提高了ACR对纳米粒子的包覆率和接枝率,复合粒子与PVC共混后纳米SiO2粒子在PVC基体中的分散性好。复合粒子对PVC的增韧效果明显优于纳米SiO2粒子和未改性ACR共聚物,复合粒子的用量较少时,就可明显提高PVC的冲击强度。     

稻壳制备高纯高表面积SiO2的研究

稻壳在稀盐酸中沸煮、干燥后,于540℃煅烧,制得了一种高纯高表面积SiO2。ICP-AES测定结果表明了该SiO2中杂质的质量含量为5.6×10-6,激光粒度仪测定其体积平均粒径为19.67μm,BET法研究表明了它的比表面积为280m2/g。并利用XRD研究了稻壳在制备过程中的结构变化。     

Chemical and Textural Characterization of Iron Oxide Nanoparticles and Their Effect on the Thermal Decomposition of Ammonium Perchlorate

Metal oxide nanoparticles have been used as burning rate catalysts for ammonium perchlorate (AP) decomposition in composite solid propellants. Though most papers point to the efficiency of different sizes, shapes and compositions, the texture of the agglomerated particles plays an important role in the catalytic efficiency, but this aspect is not always discussed. In this paper, iron oxide and composite iron oxide/silica powders were synthesized in microemulsion systems and their effect on the decomposition of AP was investigated. X‐ray diffraction (XRD) analysis and Fourier transformed infrared spectroscopy (FT‐IR) showed that the synthesized powders have an amorphous to nanocrystalline pattern, with Fe₂O₃ composition. The use of different FT‐IR spectroscopic techniques – transmission, diffuse reflectance (DRIFT) and universal attenuated total reflectance (UATR) – allied to electron microscopy analysis allowed the characterization of the samples’ surface, indicating that silicon oxide forms a thick matrix that covers the iron oxide nanoparticles. Adsorption of N₂, light scattering and electron microscopy pointed that all samples are formed by mesoporous agglomerated nanoparticles containing micropores indicating that silicon oxide forms a thick matrix that covers the iron oxide nanoparticles. Adsorption of N₂, pointed that all samples show different microstructures and light scattering indicated results refer to agglomerated particles. Finally, the catalytic effect of the samples on the decomposition of AP was evaluated by thermogravimetric analysis coupled to differential thermal analysis (TG/DTA), showing that only the high temperature decomposition step of AP was affected by the catalyst, shifting to lower temperatures the higher the surface area of the synthesized iron oxide sample, regardless of the presence of the silica matrix.