SnO2纳米微晶的合成及气敏性分析

采用溶剂热技术分别在油酸体系及无水乙醇体系中成功地合成了球形和菱形的 Sn O2 纳米微晶。通过X-射线粉末衍射、选区电子衍射、透射电镜和比表面积测定等手段对合成产物的结构进行了表征 ,并对合成产物的气敏性进行了分析。结果表明 :含有精细结构的球形 Sn O2 纳米微晶的比表面积为 1 4 6 m2· g-1,灵敏温度为 1 6 0℃左右 ,适合于作气敏元件材料     

天然模板辅助水/醇溶胶浸渍-煅烧法合成纳米SnO2

选择孔道丰富的竹炭、锯末、脱脂棉和滤纸等作为天然模板,结合水/醇溶胶浸渍-煅烧法成功地制备了纳米SnO2;采用X射线衍射仪(XRD)和透射电镜(TEM)分析了所制备的纳米材料的晶型、形貌、粒径.结果表明,纳米SnO2产物呈球形,具有四方相金红石型结构,平均粒径在10～25 nm范围内;其粒径大小与模板类型和溶胶体系有关...     

表面修饰中空LaF3纳米微粒的制备及其摩擦学性能

在油酸钠/十六烷基溴化铵乳液体系中合成了表面修饰中空LaF3纳米微粒. 通过透射电子显微镜(TEM)、X射线衍射(XRD)、傅立叶变换红外光谱(FTIR)、热重分析(TG-DTG)、能谱分析(EDS)等测试手段对其结构和形貌进行了表征. 同时在四球摩擦磨损试验机上考察了LaF3纳米微粒作为润滑油添加剂时, 添加浓度和施加载荷对其抗磨减摩性能的影响. 结果表明, 此纳米微粒的表面为油酸修饰, 具有中空结构, 平均粒径约17.5 nm; 表面修饰中空油酸/三氟化镧纳米微粒作为成品润滑油的添加剂, 具有良好的抗磨性能. 另外, 对中空纳米微粒的形成机理进行了分析.     

表面修饰中空LaF3纳米微粒的制备及其摩擦学性能

在油酸钠,十六烷基溴化铵乳液体系中合成了表面修饰中空LaF3纳米微粒.通过透射电子显微镜(TEM)、X射线衍射(XRD)、傅立叶变换红外光谱(FTIR)、热重分析(TG-DTG)、能谱分析(EDS)等测试手段对其结构和形貌进行了表征.同时在四球摩擦磨损试验机上考察了LaF3纳米微粒作为润滑油添加剂时,添加浓度和施加载荷对其执磨减摩性能的影响.结果表明,此纳米微粒的表面为油酸修饰,具有中空结构,平均粒径约17.5nm;表面修饰中空油酸/三氟化镧纳米微粒作为成品润滑油的添加剂,具有良好的抗磨性能.另外,对中空纳米微粒的形机理进行了分析.     

反相微乳液介质中纳米Sm2O3的制备

用十六烷基三甲基溴化铵(CTAB)/正丁醇/正辛烷/钐盐水溶液(氨水)所形成的反相微乳液体系, 控制合成Sm2O3球形纳米粒子. 绘制出25 ℃下CTAB/正丁醇/正辛烷/钐盐水溶液(氨水)体系的拟三元相图, 得到了反相微乳液区.在此反相微乳区内合成了Sm2O3的前驱体, 对前驱体进行热分析(TG-DSC), 确定了得到纳米Sm2O3产物的适宜焙烧温度为900 ℃, 并考察了微乳液中反应物浓度、反应时间等因素对合成产物的影响. 采用X射线衍射(XRD)、透射电镜(TEM)、激光粒度仪(NSA)、荧光光谱(FS)仪等分析方法对Sm2O3产物的形貌、晶形、粒径及荧光性质进行了表征. 结果表明, 25 益下利用反相微乳液法, 成功地制备了粒径分布较窄、分散性良好的球形纳米Sm2O3粒子, 粒径约20 nm左右, 且表现出较强的荧光性质.     

乙二醇甲醚中电解锡电解液直接水解制备纳米SnO2

采用锡金属为阳极，在无隔膜电解槽中，电化学溶解锡于乙二醇甲醚中制备得到纳米SnO2前驱体Sn(OCH2CH2OCH3)4，将电解液直接水解经溶胶-凝胶法制备纳米SnO2，前驱体通过拉曼和红外光谱进行表征.纳米SnO2采用X射线粉末衍射(XRD)和透射电子显微镜(TEM)进行表征.实验表明,电解合成的Sn(OCH2CH2OCH3)4能够溶解于乙醇中, 适宜作为溶胶-凝胶(sol-gel)法制备纳米SnO2的原料，制得的纳米SnO2经600 ℃煅烧后呈球形单分散结构，晶型为四方锡石型, 比表面为62.58 m2·g－1，平均粒径在(10.0±0.4) nm左右.产率为89.3％，电流效率为86.9％.     

反相微乳液介质中纳米Sm2O3的制备

用十六烷基三甲基溴化铵(CTAB)/正丁醇/正辛烷/钐盐水溶液(氨水)所形成的反相微乳液体系,控制合成Sm2O3球形纳米粒子.绘制出25℃下CTAB/正丁醇/正辛烷/钐盐水溶液(氨水)体系的拟三元相图,得到了反相微乳液区.在此反相微乳区内合成了Sm2O3的前驱体,对前驱体进行热分析(TG-DSC),确定了得到纳米Sm2O3产物的适宜焙烧温度为900℃,并考察了微乳液中反应物浓度、反应时间等因素对合成产物的影响.采用X射线衍射(XRD)、透射电镜(TEM)、激光粒度仪(NSA)、荧光光谱(FS)仪等分析方法对Sm2O3产物的形貌、晶形、粒径及荧光性质进行了表征.结果表明,25℃下利用反相微乳液法,成功地制备了粒径分布较窄、分散性良好的球形纳米Sm2O3粒子,粒径约20 nm左右,且表现出较强的荧光性质.     

形貌可控γ-硫化锰纳米晶的制备及表征

在表面修饰剂聚乙烯吡咯烷酮(PVP)存在的条件下,使氯化锰和硫化钠发生反应,在76℃无水乙醇溶液中,制备出了亚稳态的-γMnS纳米晶.当反应的搅拌速度不同时,得到的产物分别呈球形和椭球形.采用X射线衍射(XRD)、透射电镜(TEM)、紫外吸收光谱分析(UV)、X射线光电子能谱(XPS)等手段对产物的形貌、结构和光学性质进行了表征,并据此推导了不同形貌纳米微粒的生长机理.     

从Mn3O4前驱体到MnO2纳米结构的形貌和结构变化

锰氧化物是一类重要的且具有广泛应用背景的材料, 控制合成不同形貌和组成的锰氧化物纳米结构将有助于拓宽其应用领域. 本文报道了以Mn3O4为前驱体, 通过水热法控制合成MnO2纳米结构的方法. 用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)等手段对产物进行表征. 在硫酸体系中,当反应温度为80 和180 ℃时, 所得产物分别为γ-MnO2海胆结构和β-MnO2单晶纳米棒. 此外, MnOOH纳米线可以在稀酸溶液中合成. 考察了反应温度、溶液酸度、反应时间对产物结构的影响, 并提出了基于γ-MnO2为中间产物的反应机理. 实验结果表明, 水热体系促进了产物的各向异性生长并最终形成不同形貌和结构的锰氧化物.     

从Mn_3O_4前驱体到MnO_2纳米结构的形貌和结构变化(英文)

锰氧化物是一类重要的且具有广泛应用背景的材料,控制合成不同形貌和组成的锰氧化物纳米结构将有助于拓宽其应用领域.本文报道了以Mn3O4为前驱体,通过水热法控制合成MnO2纳米结构的方法.用X射线衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)等手段对产物进行表征.在硫酸体系中,当反应温度为80和180℃时,所得产物分别为γ-MnO2海胆结构和β-MnO2单晶纳米棒.此外,MnOOH纳米线可以在稀酸溶液中合成.考察了反应温度、溶液酸度、反应时间对产物结构的影响,并提出了基于γ-MnO2为中间产物的反应机理.实验结果表明,水热体系促进了产物的各向异性生长并最终形成不同形貌和结构的锰氧化物.     

SnO2纳米晶的水热合成及其气敏特性

SnO2 nanocrystal with different crystalline sizes were prepared with SnCl2 2H2O and H2O2 raw materials by a hydrothermal process. The synthesized powders at different reaction temperatures were characterized by means of powder X-ray diffraction, transmission electron microscope, specific surface area and gas sensitivity measurements. The results revealed that the pure SnO2 nanocrystallites synthesized at 120 ℃ have high specific surface area （210.3 m2/g）, and show a high sensitivity to C2H5OH gas. Both traits are beneficial in gas-sensitive detection application.     

高度取向ZnO单晶亚微米棒阵列的制备与表征

通过低温压热的方法,在经过预先处理长满晶核的SnO2导电玻璃基底上制备出具有高度取向的ZnO亚微米棒阵列.用扫描电子显微镜(SEM)、选区电子衍射(SAED)及X射线粉末衍射(XRD),对制备出的ZnO亚微米棒的结构和形貌进行了表征.SEM测试结果表明,ZnO亚微米棒是六方型的,近乎垂直地长在基底上,棒的直径为400～500 nm,长度约为2 μm. SAED和XRD结果表明,ZnO亚微米棒为单晶,属于六方晶系,并且沿[001]方向择优取向生长.     

SnO纳米晶须的制备及其性能表征

SnO nanowhiskers were successfully prepared by the pressure thermalcrystallization method using SnCl2·2H2O as raw material, Na2CO3 as mineralizing reagent and cetyltrimethylammoniumbromide as surfactant. Microstructure and morphology of the prepared products has been characterized by means of transmission electron microscopy,selected area electron diffraction and X-ray diffraction. The results showed the particle has rod like apparent structure. The diameter and the length of the particle were 10~40 nm and 100~400 nm, respectively. The influence of some reaction parameters, including the pressure, the surfactant and the reaction duration, on the formation, morphology and particle size of SnO crystallite was discussed. It revealed that increasing the pressure and prolonging the reaction time duration are favorable for the formation of tetragonal stannous oxide whiskers. The mechanism of the formation of SnO nanowhiskers was also simply investigated.     

水热法制备Fe3+改性的SnO2纳米颗粒

采用水热法制备了Fe3+改性的SnO2纳米颗粒, 通过XRD、BET、TEM、FT-IR和紫外-可见漫反射光谱(DRS)对其结构和光学性质进行研究. 结果表明, 水热过程实现了氧化锡的直接晶化, 产物为金红石结构, Fe3+进入SnO2的晶格之中形成固溶体. 这种方法制备的Fe3+改性的SnO2纳米颗粒为单分散状态, 粒径分布均匀, 纯的SnO2未焙烧前平均粒径为6.0 nm, 随着Fe3+添加量的增大, 样品的粒径减小. BET显示纯的SnO2样品比表面积为206.1 m2•g−1, 随着Fe3+添加量增大, 产物的比表面积增大, 同时样品的紫外-可见吸收发生红移.     

阳极电沉积条件对Ti/SnO2-Sb2O5/PbO2+Nano-Co3O4复合电极组成、形貌和结构的影响

本文在涂有中间层SnO2-Sb2O5的Ti基体上,采用阳极复合电沉积法制备了Ti/SnO2-Sb2O5/PbO2+Nano-Co3O4复合电极材料,借助于X射线衍射（XRD）、X射线光电子能谱（XPS）、扫描电镜（SEM）等分析方法研究了制备条件对该复合电极材料的组成、结构和形貌的影响。结果表明,纳米Co3O4的掺杂可提高PbO2电极表面的粗糙度和空隙率;沉积电位、镀液中Co3O4粒子浓度及有机溶剂的添加均对镀层中Co3O4的嵌入量有很大影响。     

Surfactant assisted hydrothermal synthesis of SnO nanoparticles with enhanced photocatalytic activity

SnO nanoparticles have been successfully synthesized in the presence of Triton-X 100 (TX-100) surfactant via hydrothermal method for the first time, and the photocatalytic activity under UV and visible light irradiation for the degradation of Methylene Blue (MB) and Rhodamine B (RdB) organic textile dyes was investigated. The structural, morphological and chemical characterizations were investigated by using X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), selected area electron diffraction (SAED), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS), Fourier Transform Infrared Spectroscopy (FTIR), UV–vis. diffuse reflectance spectroscopy (UV–vis DRS) and photoluminescence (PL) analysis. The results reveal that the addition of surfactant, TX-100, in the precursor solutions leads to reduction in crystallite size with significant changes in morphological structure of SnO nanoparticles. The synthesized SnO nanoparticles show excellent photocatalytic activity under UV or visible light irradiation. MB and RdB dyes degraded completely under UV irradiation after 90 and 150 min, respectively. Also, MB and RdB dyes degraded only 150 min later under visible light illumination with a little amount of photocatalyst (0.8 g/L). Hence, this work explores the facile route to synthesizing efficient SnO nanoparticles for degrading organic compound under both UV and visible light irradiations.     

A Mixed Solvothermal Route to Synthesis of Dice‐Like PbS

The authors developed a simple solvothermal route to synthesis of PbS nanocrystals in the mild binary mixed solvent made of diethylenetriamine (DETA) and water. Two kinds of PbS nanostructures (dice‐like and cubic) have been successfully synthesized in the binary mixed solvothermal system at 150 °C by changing the sulfur source. The products were characterized by X‐ray diffraction (XRD), field emission scanning electron microscope (FESEM) and transmission electron microscope (TEM). The results show that the as‐prepared dice‐like PbS crystals have a hole on each of their faces. To elucidate the relationship between reaction systems and the morphologies of the final products, the authors also investigated the crystal growth by using different sulfur source. Based on the experimental results, the possible growth mechanism of the dice‐like PbS crystals was proposed.     

SO_4~(2-)/SnO_2/SBA-15固体酸催化剂的制备及其在环酮缩合反应中的应用

采用等体积浸渍法制备了不同负载量的固体酸催化剂SO42-/SnO2/SBA-15,利用X射线粉末衍射、N2吸附-脱附和透射电镜等手段对样品进行了表征,并考察了催化剂对4-叔丁基环己酮与乙二醇缩合反应的催化性能.结果表明,SO42-/SnO2催化剂负载于SBA-15后其催化性能明显改善.研究了SO42-/20%SnO2/SBA-15催化剂上部分酮类化合物与乙二醇及1,2-丙二醇的缩合反应,并考察了反应时间和催化剂用量等因素对反应性能的影响.在适宜的温和条件下,一些环酮类底物如环己酮、4-甲基环己酮和4-叔丁基环己酮等均可反应得到相应的缩醛化产物,且催化剂至少可循环使用4次.     

Preparation of Ru-doped SnO2-supported Pt catalysts and their electrocatalytic properties for methanol oxidation

Ru-doped SnO2 nanoparticles were prepared by chemical precipitation and calcinations at 823 K. Due to high stability in diluted acidic solution, Ru-doped SnO2 nanoparticles were selected as the catalyst support and second catalyst for methanol electrooxidation. The micrograph, elemental composition, and structure of the Ru-doped SnO2 nanoparticles were characterized by scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction, respectively. The electrocatalytic properties of the Ru-doped SnO2-supported Pt catalyst (Pt/Ru-doped SnO2) for methanol oxidation have been investigated by cyclic voltammetry. Under the same loading mass of Pt, the Pt/Ru-doped SnO2 catalyst shows better electrocatalytic performance than the Pt/SnO2 catalyst and the best atomic ratio of Ru to Sn in Ru-doped SnO2 is 1/75. Additionally, the Pt/Ru-doped SnO2 catalyst possesses good long-term cycle stability.     

Electrochemical insertion of lithium in mechanochemically synthesized Zn2SnO4

We studied the electrochemical insertion of Li in mechanochemically prepared Zn(2)SnO(4). The mechanism of the electrochemical reaction was investigated by using X-ray diffraction, nuclear magnetic resonance spectroscopy, and M?ssbauer spectroscopy. Changes in the morphology of the Zn(2)SnO(4) particles were studied by in situ scanning electron microscopy. The results were compared with mixtures of SnO(2) + ZnO and with Zn(2)SnO(4) prepared by conventional solid-state synthesis and showed that the mechanochemically prepared Zn(2)SnO(4) exhibits the best cyclic stability of these samples.