镱掺杂二氧化锡纳米粉体的制备工艺影响因素研究

以SnCl4•5H2O和Yb(NO3)3•6H2O为原料,氨水为沉淀剂,采用化学共沉淀法制备了镱掺杂二氧化锡纳米粉体,考察了反应温度、煅烧温度、分散剂的种类对所得纳米镱掺杂二氧化锡粉体的物相、晶粒度和形貌的影响。对粉体的前驱体进行综合热分析(TG-DTA),用X射线衍射仪(XRD)、扫描电子显微镜(SEM)对产物的结构和形貌进行表征,得到共沉淀法制备纳米镱掺杂二氧化锡粉体的最佳条件：反应温度60 ℃,煅烧温度600 ℃,用非离子型PEG-600为分散剂。     

一种制备锑掺杂二氧化锡纳米粉体的方法

一种制备锑掺杂二氧化锡纳米粉体的方法，先将锑白溶解于酒石酸氢钠饱和溶液中，得到酒石酸锑钠溶液，同时配制一定浓度的锡酸钠溶液；根据ATO纳米粉末的锑掺杂量，将酒石酸锑钠溶液和锡酸钠溶液混合并加入酒石酸氢钠作为配合剂，同时加入双氧水作为氧化剂，用硫酸调节混合溶液的酸度；上述混合溶液在高压釜中反应一定时间，     

湿化学法制备铋掺杂二氧化锡纳米粉体的硬团聚控制

Bismuth-doped tin dioxide （BTO） nanometer powders were prepared by the wet chemical method using tin tetrachloride （SnCl4）, bismuth nitrate EBi（NO3）3] and ammonia as raw materials. Nonbridge hydroxides and capillary force between particles were found to be key factors causing hard aggregation of BTO through analyzing the formation mechanism of hard aggregation. The hard aggregation of BTO was eliminated effectively when the Bi-Sn precursor （BSP） was treated with post processing including dispersing with ultrasonic wave, refluxing and distilling with addition of n-butanol and benzene （DRD） and drying by microwave. Characterized with X-ray diffraction （XRD） and transmission electron microscopy （TEM）, BTO spherical particles with tetragonal phase structure are well crystallized, dispersed easily and the average size was less than 10 nm.     

化学共沉淀法制备纳米铋掺杂氧化锡

以SnCl4.5H2O和Bi(NO3)3.5H2O为原料,氨水为沉淀剂,采用化学共沉淀法制备了铋掺杂氧化锡(BTO)纳米粉体,考察了反应温度、滴定终点pH、铋掺杂量、煅烧温度和分散剂PEG-600对所得的纳米BTO粉体物相、晶粒度和形貌的影响,对粉末的前驱体进行综合热分析(TG-DTA),用X射线衍射(XRD)、扫描电镜(SEM)对产物的结构和形貌进行表征,得到共沉淀法制备纳米BTO粉体的最佳条件:反应温度60℃,滴定终点pH=3,煅烧温度600℃;该条件下制得BTO粉体的电阻率最小为3.48Ω.cm。     

叶腊石基锑掺杂二氧化锡复合导电粉体的制备及电性能

通过化学共沉淀法制备了以叶腊石微粉为基体、表面包覆锑掺杂二氧化锡的复合导电粉体,采用X射线衍射(XRD)和场发射扫描电子显微镜(FE-SEM)分别对该复合导电粉体晶体结构和微观形貌进行表征,并进一步研究了各反应条件对复合粉体体积电阻率的影响。实验结果表明,当水解温度60℃、水解pH值为1、SnCl4加入量100%、Sb掺杂量16%、600℃煅烧1 h时,可得到体积电阻率为26.cm的复合导电粉体。该复合导电粉体可作为填料广泛应用于导电塑料、橡胶等复合导电产品,同时为矿物基功能材料的低成本制备提供了新的思路。     

锑掺杂二氧化锡纳米粉体的制备及性能

以SnCl4·5H2O和SbCl3为主要原料,采用化学共沉淀法制得了纳米级的高导电性能的锑掺杂二氧化锡(ATO)超细粉体.研究了制备工艺对ATO粉体粒径和导电性能的影响,并探讨其影响机理,得到最佳工艺参数.运用热重-差热(TG-DTA)、X-射线衍射(XRD)、透射电镜(TEM)等测试方法对ATO粉体进行表征,并将试验产品与国内市场的同类产品性能进行了对比.     

化学共沉淀法制备纳米铋掺杂氧化锡的影响因素研究

以SnCl4.5H2O和Bi(NO3)3.5H2O为原料,氨水为沉淀剂,采用化学共沉淀法制备了铋掺杂氧化锡（BTO）纳米粉体,研究了反应温度、滴定终点pH值、铋掺杂量,煅烧温度和分散剂PEG-600对所得的纳米BTO粉体物相、晶粒度和形貌的影响,对粉末的前驱体进行综合热分析（TG-DTA）,用X-射线衍射（XRD）,扫描电镜(SEM)对产物的结构和形貌进行表征,得到共沉淀法制备纳米BTO粉体的最佳条件：反应温度60℃,滴定终点pH值为3,煅烧温度600℃;该条件下制得BTO粉体的电阻率最小为3.48Ω•cm。     

化学共沉淀法制备镧掺杂纳米二氧化锡的研究

以SNCl4和La2O3为原料,采用化学共沉淀法制备掺杂La的纳米SnO2,并对其物相和粒度进行了分析.结果发现采用化学共沉淀法制备La掺杂SnO2粉末,焙烧温度在400～650℃时,其晶体结构保持SnO2的四方结构;750℃以上焙烧,得到La2Sn2O7和SnO2两相结构.La元素的掺杂明显抑制SnO2晶粒的长大,并且随含量的增加抑制SnO2长大的效果更明显.同时掺杂La元素使纳米SnO2晶粒的形成与长大对保温时间不敏感,在550℃焙烧1 h与8 h晶粒大小只相差1 nm左右.     

钇离子掺杂制备二氧化锡及其表征

本文以SnCl4.5 H2O、CO（NH2）2和YCl3为原料,利用微波水解法分别制备了纯的和掺杂2mol%、3mol%、5mol%Y3＋的SnO2粉体。并利用X-射线衍射（XRD）,扫描电镜（SEM）对其进行表征。结果表明：实验掺杂范围内,Y3＋的掺杂对SnO2晶格没有影响;掺杂的Y3＋可以抑制SnO2晶粒的生长,使得晶粒变小且变的均匀,孔隙率增大。     

二氧化锡纳米粉体的制备及表征

本文以廉价的SnCl4·5H2O为母盐,分别以NH3·H2O为沉淀剂,采用溶胶—凝胶法和以CO(NH2)2为沉淀剂,利用微波水热法制备SnO2纳米粉体。利用X-射线衍射(XRD),傅里叶变换红外光谱(FT-IR),透射电镜(TEM)技术对产物进行表征。结果表明：溶胶—凝胶法制备的SnO2粉体颗粒约为80nm但颗粒大小分...     

纳米氧化铟锡制备方法研究

介绍了近年来纳米氧化铟锡(ITO)粉末几种常用的制备方法,着重讨论了共沉淀法,溶胶-凝胶法,水热法等工艺,并比较了几种制备方法的优缺点。共沉淀法具有流程简单,操作容易控制,环境污染少,产品性能稳定等特点,是较有前途的方法。     

Study of the Gelling Process for the Preparation of Tin Oxide Materials Based on Tin Tetrabutoxide

The gelling process in the preparation of tin oxide materials based on tin tetrabutoxide is studied. Sn(OBun)4 modified by two moles of acetylacetone (AcAc) has a stable six-member ring structure and is less susceptive to water. In a system with a lower molar ratio of acetylacetone to Sn(OBun)4 ([AcAc]/[Sn(OBun)4]<2.0) or a larger portion of water ([H2O]/[Sn(OBun)4]>2.5), colloidal suspension or white precipitation will take place. A system with molar ratios of both acetylacetone to Sn(OBun)4 and water to Sn(OBun)4 at 2.0 is transparent and olivaceous sol. As catalysts, hydrofluoric, hydrochloric, hydrobromic and acetic acids, and ammonia all accelerate the hydrolysis and condensation of Sn(OBun)4 during the sol-gel process. Light scattering measurement indicates that cluster size distribution in the sol system undergoes gradual broadening during the sol-gel transition.     

Preparation of Porous Tin Oxide Nanobelts Using the Electrospinning Technique

The electrospinning method is adopted to prepare utralong PEO/stannic hydroxide composite nanofibers. Tin-oxide nanobelts can be obtained by calcination of the composite nanofibers in an open atmosphere. The nanobelts were characterized by a field emission scanning electron microscope, X-ray diffraction, a transmission electron microscope, a Raman spectromicroscope, and Fourier transform infrared spectroscopy. Microstructural analysis has shown that the nanobelts prepared consist of a continuous network of interconnected SnO₂ grains. As a result, the SnO₂ nanobelts possess a high surface area and continuous porosity, which may be applied for the fabrication of sensitive gas sensors.     

热处理对掺锑二氧化锡纳米棒结构和导电性能的影响

以SnCl4·5H2O和SbCl3为原料,采用化学共沉淀法制得纳米级掺锑二氧化锡(ATO)的前驱物,在一定条件下热处理,成功制备了直径为10～30nm,长为50～500nm的金红石结构的ATO纳米棒.运用热重分析(TGA)、X射线衍射(XRD)、透射电镜(TEM)及比表面仪(BET法)对纳米棒进行了表征,初步探讨了其形成机理,较系统地研究了热处理温度及热处理时间对粉体形貌结构和导电性能的影响规律.     

Preparation of Stabilized Nanosized Tin Oxide Particles by Hydrothermal Treatment

Stable colloidal suspensions of tin oxide (content 0.9–6.1 wt%) were synthesized by subjecting conventionally prepared tin oxide gels to hydrothermal treatment with an ammonia solution (pH 10.5) at 200°C for 3 h in an autoclave. Based on X-ray diffractometry analyses, the tin oxide crystallites after hydrothermal treatment were resistant to thermal growth at elevated temperatures, and this feature became more conspicuous as the tin oxide content of the colloidal suspension decreased. For the powder derived from a 1.8 wt% colloidal suspension, for example, the mean sizes of the tin oxide crystallites were 7.5 and 13 nm after calcination at 600° and 900°C, respectively, in comparison with corresponding values of 13.5 and 29 nm for the untreated gel-derived powder. Thin film spin-coated from the same suspension had good uniformity, packed with tin oxide grains (crystallites) of a mean size of 6 nm after calcination at 600°C. Optical determination of the tin oxide sol particle size, as well as gravimetric analysis of the dehydration from the powder samples, were conducted to determine effects of hydrothermal treatment.     

制备条件对羟基磷灰石纳米粒子形貌的影响

在以NH4HPO4和Ca(NO3)2为原料制备羟基磷灰石纳米粒子的反应体系中,比较了不同原料加入方式和陈化条件对粒子分散特性的影响.相对于倾倒加料方式,滴加加料方式能将反应中形成的羟基磷灰石晶核有效地分散,进而避免了HA粒子的团聚;在沸腾条件下陈化处理反应沉淀物会产生严重的团聚现象,水热条件下的陈化会出现明显的生长现象,室温下陈化处理可以确保羟基磷灰石粒子准确的化学计量并有效地抑制粒子的生长和团聚.     

纳米结构SnO2的制备及其气敏性研究进展

本文总结了纳米结构SnO2的制备及其作为气敏材料的研究现状.通过改进合成方法与控制合成条件均可以获得颗粒尺寸小,比表面积大,特殊形貌包括纳米球,纳米棒,纳米薄膜,多孔结构等SnO2,从而提高SnO2气敏元件灵敏度和选择性.并分析了微波加热法、水热法和溶剂热法制备纳米SnO2的特点.     

纳米WO_3的制备工艺探讨与结构表征

通过气液反应制备了纳米WO3光催化剂,并用紫外吸收光谱、粉末X射线衍射(XRD)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、能量散射谱(EDS)等手段对催化剂进行了表征.讨论了乙二醇加入量和表面活性剂十二烷基苯磺酸钠对催化剂粒度大小和形貌的影响.结果表明:当水和乙二醇的比例为25∶75时所得WO3粒径为30 nm左右.在此比例条件下加入0.1 g表面活性剂十二烷基苯磺酸钠,可制得片状WO3,粒径约为80 nm.对自制的两种纳米WO3光催化剂在紫外光照射时降解苯酚的活性进行了初步探讨,两者的催化性能均明显优于商品WO3.