Preparation and characterization of conductive antimony-doped tin oxide (ATO) nanoparticles

In this paper, conductive antimony-doped tin oxide (ATO) composite particles is prepared by hydroxylation method of metal alcoxides. This method has many advantages such as little pollution, low-cost, simple sheet and equipment. The synthesis processing and the ATO nanoparticles are characterized by means of transmission electron microscope (TEM), X-ray diffraction (XRD), thermal gravimetric and differential thermal analysis, and BET. The results show that the ATO nanoparticles is tetragonal rutile crystal structure. TEM show that the particles are monodispersed with weak aggromation. The size of the particles calcinated at 700 is about 8nm. The specific areas are 153 m^2·g~ -1 . In addition to, ATO nanoparticles have good electric

Preparation of Arsenic Oxide and High Purity Ultrafine Antimony Compounds from Flue Dust Containing Arsenic and Antimony

1 INTRODUCTIONIt is estimated that there are about 6000 tons of arsenic loaded into smelters along with theirvarious concentrates each year in China(reference data from 1986).As result,a lot of flue dustcontaning arsenic and antimony is produced.Utilization and treatment of this flue dust are ofsignificance for the econony of recovery of arsenic and antimony and the environmental protection.But conventional treatment processes of Pyrometallurgical volatilization and hydrometallurgicalleaching are unsatisfactory because of the difficulty in seperating As and Sb as well as inpreventing secondary pollution.This research is intended to develop a new low temperaturechlorination-distillation process with high recovery of val uables and low pollution.

Preparation of Highly Dispersed Antimony-doped Tin Oxide Nano-powder via Ion-exchange Hydrolysis of SnCl_4 and SbCl_3 and Azeotropic Drying

Antimony-doped tin hydroxide colloid precipitates have been synthesized by hydrolysis of SnCl4 and SbCl3 using： （1） an ion-exchange hydrolysis to remove chlorine ions, and （2） isoamyl acetate as an azeotropic solvent to obviate water. The obtained dried powder is of high dispersivity without any need for further grinding. The size and dispersivity of the final particles are investigated with the aid of TG-DTA, BET, XRD and TEM. After having calcined, the antimony-doped tin oxide nanopowder possesses a tetragonal rutile structure with high dispersivity, uniform particles and low hard agglomeration.

Preparation of highly dispersed antimony-doped tin oxide nanopowders by azeotropic drying with isoamyl acetate

Antimony-doped tin hydroxide colloid precipitates were prepared by hydrolysis of SnCl4·5H2O and SbCl3 ethanol solutions. Isoamyl acetate was selected as azeotropic drying solvent and was compared with the most commonly used n-butanol solvent on treating precipitate for low hard agglomeration precursor powders. The FT-IR, BET, XRD, and TEM results of the precursor powders and calcinated antimony-doped tin oxide powders were recorded. The results demonstrate that isoamyl acetate is an excellent azeotropic drying solvent that can effectively prevent the agglomeration of particles and greatly improve the fluffiness of the obtained dried powders. After these precursor powders are calcined, antimony-doped tin oxide nanopowders with tetragonal rutile structure and high dispersivity can be obtained.

An Antimony Oxide pH Electrode for Tissue Culture Medium

A new approach named“caterpillar melt method”was developed to prepare wire type antimony oxide electrode for pH measurement in agar medium for tissue culture.A micro antimony wire was prepared from melt of the metal with the help of a glass capillary and the surface of the wire was oxidized in nitrate melt to obtain an antimony oxide electrode. Characterization results showed that the oxide layer is dense and uniform,with high physical and chemical stability.The electrode has a fast and stable response toward pH change for aqueous solutions.The potential of the antimony electrode has a linear relationship with the pH of the solution (R^2=1.00) with a sensitivity of 54.1mV/pH.The electrode works well and is more stable in agar medium during tissue culture for pH monitoring.

Fabrication and performance of atmospheric plasma sprayed solid oxide fuel cells with liquid antimony anodes

A solid oxide fuel cell(SOFC)with a liquid antimony anode(LAA)is a potential energy conversion technology for the use of impurity-containing fuels.Atmospheric plasma spraying(APS)technology has become a promising LAASOFC preparation method because of its economy and convenience.In this paper,button SOFCs with different cathode materials and ratios of pore former were prepared by the APS method and were operated at 750C.The effect of the cathode structure on the electrochemical performance of the LAA-SOFCs was analyzed,and an optimized spraying method for LAA-SOFCs was developed.A tubular LAA-SOFC was prepared using the APS method based on the optimized spraying method,and a peak power of 2.5 W was reached.The tubular cell was also measured at a constant current of 2 A for 20 h and was fed with a sulfur-containing fuel to demonstrate its impurity resistance and electrode stability.

Studies on Photocatalytic Degradation of Acridine Orange and Chloroform Sensing Using As-Grown Antimony oxide Microstructures

Flower shaped antimony oxide (Sb2O3) microstructures were synthesized in a large quantity via simple solution method using aqueous mixtures of antimony chloride and hexamethylene diamine (HMDA). The morphological characterizations were done by field emission scanning electron microscopy (FESEM), which revealed that the synthesized products possess flower-shaped microstructures. The detailed structural characterizations performed by X-ray diffraction (XRD), Fourier transform infrared spectrophotometer (FT-IR) and Raman spectrophotometer confirmed that the synthesized microstructures are well-crystalline antimony oxide. The Energy dispersive spectroscopy (EDS) shows that the grown products are composed of Sb and O. Optical properties of the synthesized products were characterized by UV-Visible spectrophotometer which exhibits a well defined peak at ~ 291.0 nm. The photo-catalytic activity of the Sb2O3 microstructures was evaluated by degradation of acridine orange (AO), which mineralized almost 63.0% in 150 min. The chemical sensing properties of Sb2O3 microstructures was also studied by I-V technique using chloroform as a detecting solvent. The fabricated chloroform sensor demonstrates good sensitivity of 0.1154 μA cm–2 mM–1, lower-detection limit (~0.1 mM), large-linear dynamic range (LDR, 0.122 mM to 1.22 M) with linearity (R = 0.7898) in short response time (10.0 sec).

Antimony oxides-protected ultrathin Ir-Sb nanowires as bifunctional hydrogen electrocatalysts

Developing electrocatalysts with fast kinetics and long-term stability for alkaline hydrogen oxidation reaction(HOR)and hydrogen evolution reaction(HER)is of considerable importance for the industrial production of green and sustainable energy.Here,an ultrathin Ir-Sb nanowires(Ir-Sb NWs)protected by antimony oxides(SbO_(x))was synthesized as an efficient bifunctional catalyst for both HOR and HER under alkaline media.Except from the much higher mass activities of Ir-Sb nanowires than those of Ir nanowires(Ir NWs)and commercial Pt/C,the SbO_(x) protective layer also contributes to the maintenance of morphology and anti-CO poisoning ability,leading to the long-term cycling performance in the presence of CO.Specifically,the Ir-Sb NW/SbO_(x) exhibits the highest catalytic activities,which are about 3.5 and 4.8 times to those of Ir NW/C and commercial Pt/C toward HOR,respectively.This work provides that the ultrathin morphology and H_(2)O-occupied Sb sites can exert the intrinsic high activity of Ir and effectively optimize the absorption of OH*both in alkaline HER/HOR electrolysis.

Mixed iridium-nickel oxides supported on antimony-doped tin oxide as highly efficient and stable acidic oxygen evolution catalysts

Proton exchange membrane(PEM)water electrolysis represents a promising technology for green hydrogen production,but its widespread deployment is greatly hindered by the indispensable usage of platinum group metal catalysts,especially iridium(Ir)based materials for the energy-demanding oxygen evolution reaction(OER).Herein,we report a new sequential precipitation approach to the synthesis of mixed Ir-nickel(Ni)oxy-hydroxide supported on antimony-doped tin oxide(ATO)nanoparticles(IrNiyO_(x)/ATO,20 wt.%(Ir+Ni),y=0,1,2,and 3),aiming to reduce the utilisation of scarce and precious Ir while maintaining its good acidic OER performance.When tested in strongly acidic electrolyte(0.1 M HClO_(4)),the optimised IrNi1Ox/ATO shows a mass activity of 1.0 mAµgIr^(−1) and a large turnover frequency of 123 s^(−1) at an overpotential of 350 mV,as well as a comparatively small Tafel slope of 50 mV dec^(−1),better than the IrOx/ATO control,particularly with a markedly reduced Ir loading of only 19.7µgIr cm^(−2).Importantly,IrNi1O_(x)/ATO also exhibits substantially better catalytic stability than other reference catalysts,able to continuously catalyse acidic OER at 10 mA cm^(−2) for 15 h without obvious degradation.Our in-situ synchrotron-based x-ray absorption spectroscopy confirmed that the Ir^(3+)/Ir^(4+)species are the active sites for the acidic OER.Furthermore,the performance of IrNi1Ox/ATO was also preliminarily evaluated in a membrane electrode assembly,which shows better activity and stability than other reference catalysts.The IrNi1Ox/ATO reported in this work is a promising alternative to commercial IrO_(2) based catalysts for PEM electrolysis.

Direct oxidation of methane at low temperature using Pt/C,Pd/C,Pt/C-ATO and Pd/C-ATO electrocatalysts prepared by sodium borohydride reduction process

The main objective of this paper was to characterize the voltammetric profiles of the Pt/C,Pt/C-ATO,Pd/C and Pd/CATO electrocatalysts and study their catalytic activities for methane oxidation in an acidic electrolyte at 25 ℃ and in a direct methane proton exchange membrane fuel cell at 80 ℃. The electrocatalysts prepared also were characterized by X-ray diffraction( XRD) and transmission electron microscopy( TEM). The diffractograms of the Pt/C and Pt/C-ATO electrocatalysts show four peaks associated with Pt face-centered cubic( fcc) structure,and the diffractograms of Pd/C and Pd/C-ATO show four peaks associated with Pd face-centered cubic( fcc) structure. For Pt/C-ATO and Pd/C-ATO,characteristic peaks of cassiterite( SnO_2) phase are observed,which are associated with Sb-doped SnO_2( ATO) used as supports for electrocatalysts. Cyclic voltammograms( CV) of all electrocatalysts after adsorption of methane show that there is a current increase during the anodic scan. However,this effect is more pronounced for Pt/C-ATO and Pd/C-ATO. This process is related to the oxidation of the adsorbed species through the bifunctional mechanism,where ATO provides oxygenated species for the oxidation of CO or HCO intermediates adsorbed in Pt or Pd sites. From in situ ATR-FTIR( Attenuated Total Reflectance-Fourier Transform Infrared) experiments for all electrocatalysts prepared the formation of HCO or CO intermediates are observed,which indicates the production of carbon dioxide. Polarization curves at 80 ℃in a direct methane fuel cell( DMEFC) show that Pd/C and Pt/C electroacatalysts have superior performance to Pd/C-ATO and Pt/C-ATO in methane oxidation.

DOP对纳米ATO水性浆料稳定性和涂层性能的影响

以含邻苯二甲酸二辛酯(DOP)的去离子水为分散介质,使用机械与超声相结合的方法,制备了纳米掺锑二氧化锡(ATO)水性浆料。使用静置沉降法、激光粒度仪和紫外-可见分光光度计对该水性浆料的分散稳定性进行了表征,并研究了DOP用量对含纳米ATO的水性聚氨酯(WPU)涂层性能的影响。结果表明:DOP与异丙醇、无水乙醇相比,更能促进纳米ATO粒子的分散。当ATO、DOP与水的质量比为5∶6∶89;匀浆机转速为30000 r/min,研磨时间为25 min,探头超声功率为600 W,离心机转速为6000 r/min时,可得到粒径分布较窄且颗粒尺寸较小的纳米ATO水性浆料。在适宜的条件下,厚度为150μm的ATO隔热WPU涂层的可见光透过率、紫外阻隔率及隔热率分别为81.2%、21.2%和11.5%。

基于长时间测试的ATO/PU涂层隔热机理的研究

对掺锑二氧化锡(ATO)基透明隔热涂层的隔热效果进行了长时间测试,发现无论对被隔热空间还是对涂层本身,一定时间后能量均达到动态平衡,涂层具有持久隔热效果。用紫外-可见光-红外分光光度计表征了涂层光谱性能,发现其对红外光主要以吸收为主而非反射。根据光源能量流程去向和半导体物理学的相关理论对宏微观隔热机理进行了深入研究,认为ATO/PU(聚氨酯)涂层对入射光能量的阻隔,在紫外区域以本征吸收为主,反射为辅,在红外区域以自由载流子吸收为主,反射为辅,从而产生良好的隔热效果。

纳米ATO粉体制备及其悬浮液的分散稳定性

采用化学共沉淀法制备锑掺杂二氧化锡(ATO)纳米微粉,研究了反应温度、滴定终点pH值、掺锑量及煅烧温度对粉体平均粒径的影响。并用透射电镜(TEM)、X-射线衍射分析(XRD)对粉体形貌及晶形进行了表征。讨论了pH值、分散剂种类、添加量等对ATO水浆分散稳定性的影响,通过粒径分析及Zeta电位的测定,对各种影响因素进行优化筛选,最终制得分散性、稳定性均较好的纳米ATO水浆。

制备工艺对ATO超细粉体导电性能的影响

采用化学共沉淀法制备锑掺杂二氧化锡 ( ATO)超细导电粉体 ,研究了反应温度、滴定终点 p H值、掺锑量及锻烧温度对粉体导电性的影响 。

锑掺杂二氧化锡(ATO)导电机理及制备方法研究现状

介绍了锑掺杂二氧化锡(ATO)的导电机理和该材料湿相制备方法的研究现状。晶格的氧缺位、5价Sb杂质在SnO_2禁带形成施主能级并向导带提供n-型载流子是ATO导电的2种主要机理,湿相制备超细ATO可分为均相沉淀和非均相沉淀方案,其中均相沉淀法的产品质量最佳。最后列举了ATO超细粉制备存在的问题。

仿生微模塑制备超疏水半透明隔热ATO/PU复合薄膜

掺锑二氧化锡(ATO)基透明隔热涂层或贴膜是一种节能新材料,但其表面不耐脏,超疏水化可解决此问题。今在聚二甲基硅氧烷(PDMS)软模板上,采用溶液浇注微模塑法制得了不同ATO含量的ATO/水性聚氨酯(WPU)复合功能膜,其水静态接触角达(151.3±2.1)°,水滴在膜表面极易滚落,同时具有优良的隔热性能和半透明性。扫描电子显微镜(SEM)表征了薄膜表面微结构,发现ATO纳米粒子的加入,使得微米级乳突表面及乳突之间布满纳米级小凸起,这种微米结构和纳米结构相结合的二阶结构,与天然荷叶表面极其相似,是引起隔热薄膜表面超疏水的主要原因。研究结果为规模制备半透明隔热自清洁聚氨酯薄膜提供了理论和实验依据。

配合-共沉淀法制备锑掺杂二氧化锡(ATO)粉

在充分回收含锡阳极泥有价金属的基础上,采用从锡锑二次资源中直接提取的高纯氯锡酸铵和氯氧锑为原料,合成了性能优良的纳米级锑掺杂二氧化锡(ATO)粉。针对液相共沉淀法制备ATO的过程中,锡和锑的水解不同步从而未能实现真正共沉淀掺杂的问题,以(NH4)2SnCl6和Sb4O5Cl2为原料,采用配合共沉淀法,考察了反应过程中的pH、反应温度、掺锑浓度、煅烧温度、前驱体洗涤次数和分散剂种类等对ATO粒度和形貌的影响,确定了最优化条件,即:滴定终点pH=3,反应温度60℃,锑掺杂浓度10%(质量分数),热处理温度600℃,前驱体洗涤次数为6次,采用分散剂c,并进行了实验验证。

溶胶–凝胶法制备ATO-SiO_2抗静电复合薄膜的特性研究

采用两步溶胶–凝胶法制备出 ATO(掺锑氧化锡)-SiO_2复合抗静电薄膜。通过 DTA-TG、XRD、SEM 对 薄膜的结构和形貌进行了表征,结果表明:抗静电复合薄膜表面均匀致密。薄膜中 SiO_2为无定形结构,ATO 的衍射峰 与 SnO_2一致。研究了 SnO_2的含量对薄膜导电性能、结合强度和透过率的影响,发现随 SnO_2含量增加 ?(SnO_2/ SiO_2)从 5 至 12.5,薄膜的表面电阻降低(从 1010ù/□降低到 108ù/□),薄膜的结合强度下降,薄膜的透过率降低(从 89.0%降至 84.2%),结合三方面性能,得出最佳 SnO_2的配比为:?(SnO_2/ SiO_2)=10。

ATO/GO纳米复合材料的制备及性能

以氧化石墨烯（GO）为前体,通过氨丙基三乙氧基硅烷（KH550）将氧化锡锑（ATO）锚定到氧化石墨烯片层上,制备得到氧化锡锑-氧化石墨烯纳米复合材料（ATO/GO）。通过高速分散法与水性环氧树脂乳液（AE）共混,制备得到氧化锡锑-氧化石墨烯/水性环氧树脂复合乳液（ATO/GO-AE）。通过XRD,XPS和SEM对其结构进行了表征。考察了ATO/GO含量对水性环氧涂料防腐及抗静电性能的影响。结果表明：随ATO/GO含量的增加,复合涂料表面电阻降低,ATO/GO质量分数等于3.0%时,表面电阻降低至1.0×10^9Ω以下,达到了抗静电的使用要求,漆膜水蒸汽透过率降低至62.13 g/（m^2·h）,具有最低的腐蚀电流（Icorr=3.73×10^（-9） A/cm^2）和最高的腐蚀电压（Ecorr=–0.1993 V）,ATO/GO的防腐效率与AE相比提高了99.95%。

纳米ATO水性分散液的制备及其分散稳定性研究

采用球磨法制备了3种纳米锑掺杂二氧化锡(简称ATO)水性分散液,包括未加分散剂,以非离子型高分子分散剂改性和以阴离子分散剂与非离子高分子分散剂复合改性3种情况,并通过Zeta电位仪、激光粒度仪、透射电镜、静止沉降实验等测试方法对纳米ATO水性分散液的稳定性进行了表征。结果发现,ATO纳米颗粒通过分散剂复合改性后,其水性分散液的稳定性最佳,当阴离子分散剂与非离子高分子分散剂的质量比为1∶2,复合分散剂用量为ATO粉体质量的6%时,所得ATO水性分散液的稳定性最好。