掺铝ZnO纳米粉的制备与气敏特性研究

用可溶性无机盐法(ISG法)制备掺杂Al^3 的ZnO纳米气敏材料，用D／Max0-rB型X-射线粉末衍射仪研究纳米晶的结构。结果表明制备的掺铝ZnO纳米材料属于六方晶系，纤锌矿结构。用Seherrer公式计算得ZnO和掺铝ZnO的平均晶粒分别为40nm和35nm。用掺铝的ZnO纳米粉做成气敏元件，测试了不同铝含量的纳米材料在不同浓度的乙醇气体和氢气下的敏感特性。结果表明随着气体浓度的增加，灵敏度逐渐上升；随着Al含量的减少，材料气敏灵敏性逐渐增强。当铝含量为Al／ZnO=O．5％(mol)时，对O．2％的乙醇气体的灵敏度最大可达到127。并讨论了纳米材料对敏感气体的物理吸附和化学吸附以及纳米氧化物的气敏机理。     

碳纳米管修饰的空心多孔NiO/SnO2纳米复合材料对丙酮传感性能的优化

通过静电纺丝法制备中空多孔的NiO/SnO2复合纳米纤维,在复合纤维表面装饰碳纳米管,在此基础上制备气敏传感器器件。利用TGA确定了复合材料热分解温度,得到热处理工艺;利用SEM、XRD、TEM、XPS分别对复合材料的形貌、结构、尺寸、表面成分进行了表征。使用WS-30A气敏元件测试仪对气敏元件响应进行测试,结果表明CNTs装饰的NiO/SnO2复合纳米材料制备的气敏传感器降低了丙酮检测最佳工作温度,为160℃,提高了检测灵敏度,对50 ppm丙酮的响应达到25.25,对检测丙酮有快速的响应(~8.2 s)以及恢复性能(~10.5 s),同时在30天的长期稳定性测试中也体现了良好的稳定性。证明了装饰CNTs 的 NiO/SnO₂复合材料在检测丙酮方面的潜在价值,同时本文也进一步讨论了CNTs, 中空多孔结构的NiO/SnO₂提高检测性能的作用机理。     

（Al，Sb）／ZnO复合氧化物对乙醇气体气敏功能特性的影响

用可溶性无机盐法制备了较宽工作温度范围的纳米(Al，Sb)/ZnO气敏材料。该材料主相属于ZnO纤锌矿结构，并同时存在Sb2O5、Sb6O132种微量杂相。该复合氧化物的平均晶粒为86nm。用制备的氧化物纳米粉做成气敏元件，测试了不同铝含量的纳米材料在2000μg/g浓度乙醇气体下的敏感特性。当铝含量为Al/ZnO=1．5％(mol比，下同)时，对2000μg的乙醇气体的灵敏度最大可达到26。固定Al/ZnO=3％时，掺入不同量锑得到对乙醇气体有更大工作温度范围的纳米复合氧化物材料。同时讨论了掺铝掺锑复合氧化物对敏感气体的物理吸附和化学吸附及其气敏机理。     

水热法制备MoS_2纳米花电极及其电化学性能

以三氧化钼和硫氰酸铵为起始原料,采用温和的水热法制备了MoS2纳米花。考察了反应温度(160~200℃)和反应时间(12~48h)对MoS2纳米花电极化学性能的影响。利用X射线衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)和N2吸附-脱附曲线(BET)对样品的晶型、形貌、组分和比表面积进行了表征。结果表明,所制备的样品呈现出了花瓣状的片层结构,并有序堆垛成花状纳米球,且具有较大的比表面积(23.13m2·g-1)。循环伏安测试表明,MoS2电极的催化活性优于铂电极。光电化学性能测试表明,基于MoS2对电极的染料敏化太阳能电池(DSSCs)的光电转换效率(2.44%)高于铂电极(2.33%),有望在染料敏化太阳能电池(DSSCs)电极材料方面得到应用。     

花瓣状钌掺杂氧化锌纳米片的水热/煅烧法制备及气敏性能

以硝酸锌、氢氧化钠为原料,通过水热/煅烧法制备结构新颖的厚度在20 nm至40 nm之间的钌掺杂花瓣状氧化锌纳米片。采用粉末X射线衍射仪、场发射扫描电镜、氮气吸附法、气敏测试系统对产物进行物相、结构形貌、比表面积、气敏性能等的表征。结果表明,钌掺杂氧化锌纳米片对乙醇和丙酮气体的灵敏度高,探测浓度低,响应和恢复迅速。在360°C和100×10^-6的条件下,对乙醇和丙酮的灵敏度分别达到33和67。在10×10^-6的乙醇和丙酮气体中,其响应和恢复速度分别为4 s和9 s,3 s和10 s.     

g-C3N4-Cd2SnO4复合材料的制备及其气敏性能

摘 要：采用水热-煅烧法制备了Cd2SnO4,并使用超声混合法制备一系列不同质量比例的g-C3N4-Cd2SnO4复合材料。通过X射线衍射（XRD）、扫描电镜（SEM）、X射线光电子能谱（XPS）等方法对g-C3N4-Cd2SnO4复合材料进行了表征,研究了不同比例的g-C3N4-Cd2SnO4复合材料的气敏性能。气敏性能研究结果表明：当g-C3N4的加入量为2.5 wt%（质量分数）时,g-C3N4-Cd2SnO4复合材料对于异丙醇气体的灵敏度最高,在170℃的最佳工作温度下,对100 μL/L的异丙醇气体的灵敏度可达117,与纯Cd2SnO4的灵敏度1.4相比提高了78倍,最低检测限为0.1 μL/L。     

Ni掺杂SnO_2的光谱特性及气敏性能研究

采用溶剂热法将Ni掺杂到纳米SnO2中,分别利用TEM、EDAX、XRD、Raman和XPS表征了Ni掺杂后SnO2的微观形貌、结构和元素组成特征,分析了Ni掺杂对增强SnO2气敏性能的作用机理。实验结果表明,Ni的掺杂可抑制SnO2晶粒增长,减小SnO2晶粒尺寸,进而提升传感器的气敏性能。少量的Ni掺杂能够使Ni2+进入SnO2晶格中取代Sn4+产生氧空位,促进SnO2气敏性能的提高;而当Ni掺杂量达到30%时,会导致部分Ni以其他的形式存在于SnO2晶体表面上,降低SnO2气敏性能。     

基片温度对WO_3薄膜的微观结构和NO_2气敏特性的影响

采用直流反应磁控溅射法,在不同的基片温度条件下制备出具有不同微观结构的WO3薄膜,探讨这些薄膜作为气敏材料对NO2气体的气敏特性。WO3薄膜的晶体结构、表面及断面形貌分别采用X射线衍射和扫描电子显微镜进行表征。结果表明:随着基片温度的升高,具有单斜晶WO3结构薄膜的(200)衍射峰强度逐渐增强,薄膜由低基片温度(-75℃)的纳米粉体、过渡到中间基片温度(-50~300℃)的纳米薄膜、直至高基片温度(500℃)的纳米棒组成。所有WO3薄膜均在200℃的工作温度下获得对NO2气体的最大灵敏度。在相同的检测条件下,气体灵敏度随着基片温度的减小和NO2气体浓度(体积分数)的增加而增大。     

Detonation Synthesis of SnO2 Nanoparticles in Gas Phase

以 SnCl4为前驱体、以氧气和氢气的混合气体为爆源,通过气相爆轰制备纳米二氧化锡粉末。并通过 XRD 和 TEM 等测量手段对纳米 SnO2进行表征及分析,发现所制备的纳米 SnO2颗粒形状呈球形,粒径在 1~10 nm 之间。由此可以得出结论:气相爆轰可以设计合成独特的纳米 SnO2。     

SnO2纳米颗粒的水热法和溶胶-凝胶法制备及其气敏特性

通过不同条件的水热法和溶胶-凝胶技术分别制备了单分散SnO2纳米粉体。利用X射线衍射、透射电子显微镜和比表面积分析仪对产物进行了检测,采用静态配气法测试了样品的气敏性能。结果表明,水热时间越长,颗粒尺寸越大,以反应时间为6 h制备的粉体比表面积最大;溶胶-凝胶产物中,以SnCl2的乙醇溶液为原料制得的颗粒克服了热处理过程中产物易团聚的问题,颗粒尺寸均匀,具有良好的分散性和较高的比表面积。两种方法制备的粉体均对酒精具有良好的灵敏度,SnCl2的乙醇溶液为原料、溶胶-凝胶技术获得的材料对酒精的灵敏度更高,并认为热处理过程中Cl-的去除是导致材料气敏性能不同的主要因素。     

Synthesis of TiO_2@ZnIn_2S_4 hollow nanospheres with enhanced photocatalytic hydrogen evolution

In this work, we designed and prepared the novel TiO_2@ZnIn_2 S_4 nano-sized hollow structure via templating method assisted by hydrothermal synthesis process. Its unique hollow structure and type-II heterojunction between TiO_2 hollow nanospheres and ZnIn_2 S_4 nanosheet can provide enough interior cavities and transfer paths for the light absorption and charge quick migration. The crystal structure, morphology and charges separation property were measured. The characterization results show that the hollow-structured Ti O_2@ZnIn_2 S_4 was successfully prepared,and the optimal sample exhibited excellent photocatalytic hydrogen generation compared with TiO_2/ZnIn_2 S_4 cluster exceeding by a factor of 1.1 under overall light irradiation.Specially, the detailed mechanism of the photocatalytic H_2 evolution and charge carrier migration for the as-prepared TiO_2@ZnIn_2 S_4 hollow nanosphere was also studied.     

Preparation of RuO_2-SnO_2 nanomaterial by sol gel technique

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用闪锌矿制备ZnS-ZnO异质结及其NO2气敏特性

将闪锌矿纯矿物通过焙烧工艺制备成ZnO前驱体,随后添加Na2S·9H2O实现对ZnO前驱体的硫化,从而制备出ZnS-ZnO异质结材料,采用XRD、SEM、FTIR等检测手段对其进行结构表征。结果表明,制备出的ZnS-ZnO异质结材料呈颗粒状,尺寸在80 nm左右,且具有较大的比表面积。ZnS-ZnO异质结材料对NO2气体具有良好的响应和恢复特性,并在工作温度250℃时获得最大灵敏度,且灵敏度与NO2气体浓度符合指数函数关系。在相同检测条件下,与单一ZnO材料相比,ZnS-ZnO异质结材料呈现出工作温度低、灵敏度高、响应和恢复时间短等优异特性。在ZnS与ZnO晶界处所形成的n-n型异质结结构是改善气敏特性的关键因素。     

均相沉淀模板法制备纳米Y2O3空心球研究

以粒径约150 nm的碳球为模板,通过均相沉淀法制备出Y(OH)3/碳球复合微球,煅烧除去碳球模板,得到粒径约300 nm的纳米Y2O3空心球。通过傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射(XRD)和热失重分析(TG)以及X射线光电子能谱(XPS)等测试手段表征复合微球和纳米Y2O3空心球的形貌和结构。结果表明:空心球由立方晶系纳米Y2O3构成,粒径约为300 nm,壳厚度约为20 nm。     

Polymer-induced generation and characterization of electrophoretic properties of hollow TiOX nanospheres for electronic paper

Hollow TiO_X nanospheres have been successfully prepared using hollow core–double shell latex particles (poly(styrene-co-methyl methacrylate-co-butyl acrylate-co-methacrylic acid) (abbreviated in poly(St-co-MMA-co-BA-co-MAA)) as template, which involves the deposition of inorganic coating on the surface of hollow core–shell latex particles and subsequent removal of the latex by calcinations in air or ammonia gas. Ti(OBu)₄ was used as precursor for the preparation of hollow TiO_X nanospheres. TEM of white hollow core–double shell polymers particles with an aperture of approximately 225 nm displays the perfect characteristic hollow nanospheres structure of primary core–double shell particles. The formation of TiO_X was confirmed by XRD analysis and hollow structure of the particles was revealed by transmission electron microscopy (TEM). When the calcined temperature was at 800 °C, hollow TiO₂ nanospheres were arranged regularly with the diameter range of 130–170 nm. The electrophoretic properties were characterized by JS94J micro-electrophoresis apparatus. The electrophoretic mobility of white TiO₂ and black TiO hollow spheres in tetrachloroethylene were 1.09 × 10⁻⁵ and 3.12 × 10⁻⁵ cm²/V s, and the zeta potentials were 7.10 and 20.24 mV, respectively. The results show that white TiO₂ particles and black TiO hollow nanoparticles are suitable as electrophoretic particles and possess the application potential in the future electrophoretic display.     

3D自组装纳米功能材料制备的研究进展

自组装是在没有人工干预的情况下,由基本结构单元自发形成高度有序的空间结构。3D自组装结构具有较大的比表面,因而表现出优异的催化和光电化学等性能,已经成为纳米材料制备科学和技术的一个研究热点。因此,本文评述了3D自组装纳米功能材料的主要制备方法,具体包括：水热/溶剂热法、模板法、外场诱导法等。     

SnO2 coated Ni particles prepared by fluidized bed chemical vapor deposition

A Fluidized Bed Metal–Organic Chemical Vapor Deposition (FB-MOCVD) process was developed for the growth of tin oxide thin films on large hollow Ni particles. Tetraethyl tin was used as tin source and dry air both as fluidization gas and oxidant reagent. The SnO₂ films were grown in a FBCVD reactor under reduced pressure (13.3 kPa) in the temperature range of 633–663 K. A series of specific experiments was carried out to optimize the design of the reactor and to determine the range of experimental parameters (flow rate, pressure, temperature) leading to good fluidization of the large hollow Ni particles used as base material. The SnO₂ films deposited on particles exhibited a dense nodular surface morphology similar to that previously observed on flat substrates. The relative thickness of the films was determined by EDS analyses and the real values were measured by SEM on cross-sections of particles. The SnO₂ films exhibit satisfactory thickness uniformity from one particle to another in the same batch and from run to run. XRD studies revealed that the films exhibited good crystallinity with the cassiterite structure. Traces of NiO were found at the SnO₂/Ni interface. Finally, the SnO₂ CVD coated-Ni particles were used as anodes in an electrochemical cell. The potential limit of oxygen evolution measured was that of the SnO₂ layer despite the initial porosity of the hollow Ni particles inherent to their preparation. This work is the first step towards the preparation of high specific surface area electrodes.