SnO_2形貌调控与改性及其在Ag基电接触材料中的应用
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摘要
Ag/SnO2是当前替代有毒Ag/CdO电接触材料的一种极具发展前景的环保型电接触材料,在低压电器方面已经获得一定程度的研究与应用。现有Ag/SnO2电接触材料主要采用粉末冶金法和Ag-Sn合金内氧化法制备。然而,SnO2颗粒在Ag基体中分散性差、易偏析等问题导致电接触材料接触电阻大、温升高、抗电弧侵蚀性差、电寿命短。因此,开展SnO2增强相的研究,改善SnO2与Ag的润湿性及其在Ag基体中的分布,对于制备高性能Ag/SnO2电接触材料具有重要的理论意义与实用价值。
本文采用湿化学方法,控制纳米Sn02的制备与组装,获得不同形貌的SnO2颗粒,在此基础上通过表面载银、制备Ag-SnO2中间体等手段改善SnO2与Ag的润湿性及其在Ag基体中的分布,研究了SnO2形貌及改性方法对Ag/SnO2电接触材料性能的影响,探索具有优异电学性能和力学性能的Ag/SnO2电接触材料的制备方法。主要研究内容及结论如下：
(一)采用湿化学方法制备不同形貌的SnO2颗粒,系统研究原料配方与工艺条件对Sn02颗粒形貌的影响,实现对SnO2纳米颗粒、实心微球、空心微球、亚微米棒的可控制备。(1)采用液相沉淀法,以SnCl4为原料,PEG2000作为分散剂,在pH=8条件下制备出分散性好、晶粒尺寸为13nm的金红石相SnO2内米颗粒；(2)采用溶剂热法,以PEG6000为模板导向剂,在180℃下反应12h制备出由SnO2纳米晶组装而成、尺寸为1μm左右的单分散SnO2微球；(3)采用水热法,以Na2SnO3和尿素为原料,尿素分解形成气泡为模板,在150℃下反应24h制备出具有开口结构的SnO2空心微球,并对开口形成机制进行研究；(4)采用液相沉淀法,以PEG400与乙醇为混合溶剂,制备出由SnO2纳米晶组装而成,直径为200nm、长径比为15：1的Sn02亚微米棒。
(二)开展Sn02微球表面载银改性研究,制备出表面包覆效果好、Ag-SnO2键合力强的载银SnO2复合微球。(1)利用Sn2+表面修饰Sn02实心微球,以PVP为还原剂,可有效调控纳米Ag颗粒在Sn02实心微球表面形核、生长,实现Ag纳米颗粒对Sn02实心微球的包覆；(2)以Na2SnO3、AgNO3为原料,尿素分解形成气泡为模板,在150℃水热反应24h,实现SnO2空心微球制备与表面载银的同步进行,制备出表面包覆Ag纳米颗粒的SnO2空心微球,Sn02核与Ag壳之间存在较强的键合作用。
(三)开展Ag-SnO2中间体复合粉体制备研究,实现SnO2纳米颗粒在Ag粉中的弥散分布。(1)以SnO2内米颗粒及化学银粉为原料,采用高能球磨工艺在添加质量百分数为5%的PEG6000为工艺控制剂、球料比为10：1、转速为260r/min、球磨时间4h的条件下,利用高能球磨机械碰撞及挤压作用实现SnO2纳米颗粒均匀弥散镶嵌于Ag粉中,制备出Sn02质量百分数为60%的Ag-SnO2(60)中间体复合粉体；(2)采用阴阳离子共沉淀法,以Na2SnO3、AgNO3为原料,通过调节体系pH值,利用SnO32-与Ag+的共同沉积实现Sn02纳米颗粒与Ag纳米颗粒的均匀复合,制备出Sn02质量百分数为42%的Ag-SnO2(42)中间体复合粉体;(3)采用氧化还原沉淀法,以SnCl2·2H2O、AgNO3为原料,在弱碱性条件下,利用Sn2+与Ag+的氧化还原反应,实现SnO2内米颗粒与Ag纳米颗粒的均匀复合,制备出Sn02质量百分数为63%的Ag-SnO2(63)中间体复合粉体。
(四)采用复压复烧工艺制备Ag/SnO2电接触材料,考察了SnO2形貌及表面载银、制备Ag-SnO2中间体等改性方法对Ag/SnO2电接触材料性能的影响。(1)在Sn02纳米颗粒、实心微球、空心微球、亚微米棒等形貌中,以Sn02亚微米棒为增强相的电接触材料具有较好的综合性能,其闭合燃弧时间和能量比Sn1-xSbxO2增强的材料减小了1/3,接触电阻稳定,熔焊力小,质量损失减少约80%,材料的抗电弧侵蚀性能好；(2)Sn02微球表面载银可以改善与Ag基体的润湿性,提高电接触材料的性能,与载银前相比,电接触材料的密度、硬度及电导率都得到一定程度的提高,组织结构均匀;(3)采用Ag-SnO2中间体向Ag/SnO2电接触材料中引入纳米Sn02颗粒,可以减轻Sn02纳米颗粒在Ag/SnO2电接触材料制备、烧结过程中的团聚,明显改善电接触材料的结构与性能,尤其是高能球磨制备的中间体。与传统制备方法相比,Sn02纳米颗粒在Ag/SnO2电接触材料中弥散分布,可使电接触材料的闭合燃弧时间由10ms变为6ms,燃弧能量由1000mJ变为500mJ,材料的接触电阻低且稳定,熔焊力小,抗电弧侵蚀能力好。
Ag/SnO2, an environmentally friendly electrical contact material for the re-placement of toxic Ag/CdO, has been studied and found application in different low voltage switchgear devices to some extent. The most common commercial routes to manufacture Ag/SnO2electrical contact materials are powder metallurgy and internl oxidation of Ag-Sn alloy. However, the bad distribution and aggregatation of SnO2in Ag matrix will increase the contact resistance and over-temperature, degrade the an-ti-arc erosion ability and shorten the electrical endurance. So, it is hence of great the-oretical and practical significance to research the surface modification of SnO2phase, improvement of the wettability between SnO2and Ag and the dispersion of SnO2in Ag martix for the preparation of Ag/SnO2electricial contact materials with superior performance.
In this paper, SnO2particles with different morphology were obtained by domi-nating the preparation and assembly of SnO2nanoparticles via wet chemical methods. The wettability between SnO2and Ag was enhanced by coating SnO2with Ag nano-particles and the dispersivity of SnO2in Ag matrix was improved by introducing Ag-SnO2intermediates. Effects of morphology and surface modification of SnO2on the properties of Ag/SnO2electrical contact materials were investigated. Methods for preparing Ag/SnO2electrical contact materials with excellent electrical and mechani-cal performance were explored. The main results are as follows:
SnO2particles with different morphology were prepared by wet chemical methods and effects of raw materials and technological paramters on the morphology of SnO2were investigated. Realized the controllable preparation of SnO2nanoparticles, SnO2microspheres and SnO2submicron rods:(1) Well-dispersed rutile SnO2nanoparticles with an average grain size of ca.13nm were prepared by chemical precipitation method, using SnCl4as raw materials and PEG2000as dispersing agent.(2) Mono-dispersed SnO2microspheres with a diameter of ca.1μm, self-assembled by nano-crystalline, were obtained using PEG6000as inducing template reagents via sol-vothermal method at180℃for12hours.(3) SnO2hollow microspheres with an open structure were prepared using Na2SnO3and urea as raw materials, bubles as the tem-plate via hydrothermal method, and the formation mechanism were analyzed.(4) SnO2submicron rods with a diameter of ca.200nm assembled by nanocrystals were prepared by precipitation method using PEG400and ethanol as solvent. The ratio of length to diameter is approximately20:1.
SnO2microspheres coated with Ag were prepared and realized the strong inter-action between Ag layer and SnO2core:(1) Utilizing PVP as mild and green reductant to regulate the nucleation and growth of Ag nanoparticles on Sn2+-decorated SnO2microspheres and realized the well coating of SnO2microspheres with Ag nanoparti-cles.(2) Utilizing AgNO3and Na2SnO3as the raw materials, bubbles released by the decomposition of urea as the template, realized the simultaneous process of prepara-tion of SnO2and coating Ag on SnO2hollow microspheres. The hollow SnO2micro-spheres coated with Ag nanoparticles showed strong interaction between SnO2core and Ag shell.
Ag-SnO2intermediates composite powders were prepared and realized the great-er SnO2dispersion in Ag matrix:(1) Ag-SnO2(60) intermediates with a mass percent-age of SnO2is60%were prepared by high-energy ball milling process for4hours at a speed of260r/min, using Ag and SnO2nanoparticles as the raw materials,5%PEG6000as the additives. The dispersion of SnO2nanoparticles was realized with the help of drastic mechanical collision and squeeze during high energy milling.(2) By varying pH values, Ag-SnO2(42) intermediates with a mass percentage of SnO2is42%were prepared by coprecipitation reaction of SnO32-and Ag+,using AgNO3and Na2SnO3as raw materials.(3) Ag-SnO2(63) intermediates with a mass percentage of SnO2is63%were prepared by oxidation reduction reaction of Sn2+and Ag+in weak alkaline condition, using AgNO3and SnCl2as raw materials.
Ag/SnO2electrical contact materials were prepared by re-pressing and re-sintering technology and effects of the morphology of SnO2, surface modification of SnO2and the intermediates on the properties of Ag/SnO2electrical contact materi-als were investigated:(1) Ag/SnO2electrical contact material prepared from SnO2submicron rods exhibits best overall properties.Compared with Sn1-xSbxO2reinforced electrical contact materials, the making arcing duration and arcing energy of electrical contact materials form SnO2submicron rods are reduced by1/3while the weight loss decreased by80%. It's stable contact resistance and smaller welding force result in the better anti-arc erosion and anti welding.(3) SnO2microspheres coated with Ag nano-particles enhanced the wettability between SnO2particles and Ag matrix, improved the homogeneity of organization structure and the properties of Ag/SnO2electrical contact materials.(4) Ag-SnO2intermediates can alleviate the aggregation of SnO2nanoparticles in the following molding and sintering of Ag/SnO2electrical contact material and improved the properties of Ag/SnO2electrical contact materials,espe-cially for intermediates by high-energy ball milling. Compared with the electrical contact material prepared by traditional method, the better dispersion of SnO2nano-particles from intermediates significantly improved the properties of Ag/SnO2electri-cal contact material.The making arcing time and arcing energy are reduced from10ms to5ms,1000mJ to500mJ, respectively. The lower contact resistance and smaller welding force improve the anti-arc erosion ability and anti welding ability of Ag/SnO2electrical contact materials.
本文采用湿化学方法,控制纳米Sn02的制备与组装,获得不同形貌的SnO2颗粒,在此基础上通过表面载银、制备Ag-SnO2中间体等手段改善SnO2与Ag的润湿性及其在Ag基体中的分布,研究了SnO2形貌及改性方法对Ag/SnO2电接触材料性能的影响,探索具有优异电学性能和力学性能的Ag/SnO2电接触材料的制备方法。主要研究内容及结论如下：
(一)采用湿化学方法制备不同形貌的SnO2颗粒,系统研究原料配方与工艺条件对Sn02颗粒形貌的影响,实现对SnO2纳米颗粒、实心微球、空心微球、亚微米棒的可控制备。(1)采用液相沉淀法,以SnCl4为原料,PEG2000作为分散剂,在pH=8条件下制备出分散性好、晶粒尺寸为13nm的金红石相SnO2内米颗粒；(2)采用溶剂热法,以PEG6000为模板导向剂,在180℃下反应12h制备出由SnO2纳米晶组装而成、尺寸为1μm左右的单分散SnO2微球；(3)采用水热法,以Na2SnO3和尿素为原料,尿素分解形成气泡为模板,在150℃下反应24h制备出具有开口结构的SnO2空心微球,并对开口形成机制进行研究；(4)采用液相沉淀法,以PEG400与乙醇为混合溶剂,制备出由SnO2纳米晶组装而成,直径为200nm、长径比为15：1的Sn02亚微米棒。
(二)开展Sn02微球表面载银改性研究,制备出表面包覆效果好、Ag-SnO2键合力强的载银SnO2复合微球。(1)利用Sn2+表面修饰Sn02实心微球,以PVP为还原剂,可有效调控纳米Ag颗粒在Sn02实心微球表面形核、生长,实现Ag纳米颗粒对Sn02实心微球的包覆；(2)以Na2SnO3、AgNO3为原料,尿素分解形成气泡为模板,在150℃水热反应24h,实现SnO2空心微球制备与表面载银的同步进行,制备出表面包覆Ag纳米颗粒的SnO2空心微球,Sn02核与Ag壳之间存在较强的键合作用。
(三)开展Ag-SnO2中间体复合粉体制备研究,实现SnO2纳米颗粒在Ag粉中的弥散分布。(1)以SnO2内米颗粒及化学银粉为原料,采用高能球磨工艺在添加质量百分数为5%的PEG6000为工艺控制剂、球料比为10：1、转速为260r/min、球磨时间4h的条件下,利用高能球磨机械碰撞及挤压作用实现SnO2纳米颗粒均匀弥散镶嵌于Ag粉中,制备出Sn02质量百分数为60%的Ag-SnO2(60)中间体复合粉体；(2)采用阴阳离子共沉淀法,以Na2SnO3、AgNO3为原料,通过调节体系pH值,利用SnO32-与Ag+的共同沉积实现Sn02纳米颗粒与Ag纳米颗粒的均匀复合,制备出Sn02质量百分数为42%的Ag-SnO2(42)中间体复合粉体;(3)采用氧化还原沉淀法,以SnCl2·2H2O、AgNO3为原料,在弱碱性条件下,利用Sn2+与Ag+的氧化还原反应,实现SnO2内米颗粒与Ag纳米颗粒的均匀复合,制备出Sn02质量百分数为63%的Ag-SnO2(63)中间体复合粉体。
(四)采用复压复烧工艺制备Ag/SnO2电接触材料,考察了SnO2形貌及表面载银、制备Ag-SnO2中间体等改性方法对Ag/SnO2电接触材料性能的影响。(1)在Sn02纳米颗粒、实心微球、空心微球、亚微米棒等形貌中,以Sn02亚微米棒为增强相的电接触材料具有较好的综合性能,其闭合燃弧时间和能量比Sn1-xSbxO2增强的材料减小了1/3,接触电阻稳定,熔焊力小,质量损失减少约80%,材料的抗电弧侵蚀性能好；(2)Sn02微球表面载银可以改善与Ag基体的润湿性,提高电接触材料的性能,与载银前相比,电接触材料的密度、硬度及电导率都得到一定程度的提高,组织结构均匀;(3)采用Ag-SnO2中间体向Ag/SnO2电接触材料中引入纳米Sn02颗粒,可以减轻Sn02纳米颗粒在Ag/SnO2电接触材料制备、烧结过程中的团聚,明显改善电接触材料的结构与性能,尤其是高能球磨制备的中间体。与传统制备方法相比,Sn02纳米颗粒在Ag/SnO2电接触材料中弥散分布,可使电接触材料的闭合燃弧时间由10ms变为6ms,燃弧能量由1000mJ变为500mJ,材料的接触电阻低且稳定,熔焊力小,抗电弧侵蚀能力好。
Ag/SnO2, an environmentally friendly electrical contact material for the re-placement of toxic Ag/CdO, has been studied and found application in different low voltage switchgear devices to some extent. The most common commercial routes to manufacture Ag/SnO2electrical contact materials are powder metallurgy and internl oxidation of Ag-Sn alloy. However, the bad distribution and aggregatation of SnO2in Ag matrix will increase the contact resistance and over-temperature, degrade the an-ti-arc erosion ability and shorten the electrical endurance. So, it is hence of great the-oretical and practical significance to research the surface modification of SnO2phase, improvement of the wettability between SnO2and Ag and the dispersion of SnO2in Ag martix for the preparation of Ag/SnO2electricial contact materials with superior performance.
In this paper, SnO2particles with different morphology were obtained by domi-nating the preparation and assembly of SnO2nanoparticles via wet chemical methods. The wettability between SnO2and Ag was enhanced by coating SnO2with Ag nano-particles and the dispersivity of SnO2in Ag matrix was improved by introducing Ag-SnO2intermediates. Effects of morphology and surface modification of SnO2on the properties of Ag/SnO2electrical contact materials were investigated. Methods for preparing Ag/SnO2electrical contact materials with excellent electrical and mechani-cal performance were explored. The main results are as follows:
SnO2particles with different morphology were prepared by wet chemical methods and effects of raw materials and technological paramters on the morphology of SnO2were investigated. Realized the controllable preparation of SnO2nanoparticles, SnO2microspheres and SnO2submicron rods:(1) Well-dispersed rutile SnO2nanoparticles with an average grain size of ca.13nm were prepared by chemical precipitation method, using SnCl4as raw materials and PEG2000as dispersing agent.(2) Mono-dispersed SnO2microspheres with a diameter of ca.1μm, self-assembled by nano-crystalline, were obtained using PEG6000as inducing template reagents via sol-vothermal method at180℃for12hours.(3) SnO2hollow microspheres with an open structure were prepared using Na2SnO3and urea as raw materials, bubles as the tem-plate via hydrothermal method, and the formation mechanism were analyzed.(4) SnO2submicron rods with a diameter of ca.200nm assembled by nanocrystals were prepared by precipitation method using PEG400and ethanol as solvent. The ratio of length to diameter is approximately20:1.
SnO2microspheres coated with Ag were prepared and realized the strong inter-action between Ag layer and SnO2core:(1) Utilizing PVP as mild and green reductant to regulate the nucleation and growth of Ag nanoparticles on Sn2+-decorated SnO2microspheres and realized the well coating of SnO2microspheres with Ag nanoparti-cles.(2) Utilizing AgNO3and Na2SnO3as the raw materials, bubbles released by the decomposition of urea as the template, realized the simultaneous process of prepara-tion of SnO2and coating Ag on SnO2hollow microspheres. The hollow SnO2micro-spheres coated with Ag nanoparticles showed strong interaction between SnO2core and Ag shell.
Ag-SnO2intermediates composite powders were prepared and realized the great-er SnO2dispersion in Ag matrix:(1) Ag-SnO2(60) intermediates with a mass percent-age of SnO2is60%were prepared by high-energy ball milling process for4hours at a speed of260r/min, using Ag and SnO2nanoparticles as the raw materials,5%PEG6000as the additives. The dispersion of SnO2nanoparticles was realized with the help of drastic mechanical collision and squeeze during high energy milling.(2) By varying pH values, Ag-SnO2(42) intermediates with a mass percentage of SnO2is42%were prepared by coprecipitation reaction of SnO32-and Ag+,using AgNO3and Na2SnO3as raw materials.(3) Ag-SnO2(63) intermediates with a mass percentage of SnO2is63%were prepared by oxidation reduction reaction of Sn2+and Ag+in weak alkaline condition, using AgNO3and SnCl2as raw materials.
Ag/SnO2electrical contact materials were prepared by re-pressing and re-sintering technology and effects of the morphology of SnO2, surface modification of SnO2and the intermediates on the properties of Ag/SnO2electrical contact materi-als were investigated:(1) Ag/SnO2electrical contact material prepared from SnO2submicron rods exhibits best overall properties.Compared with Sn1-xSbxO2reinforced electrical contact materials, the making arcing duration and arcing energy of electrical contact materials form SnO2submicron rods are reduced by1/3while the weight loss decreased by80%. It's stable contact resistance and smaller welding force result in the better anti-arc erosion and anti welding.(3) SnO2microspheres coated with Ag nano-particles enhanced the wettability between SnO2particles and Ag matrix, improved the homogeneity of organization structure and the properties of Ag/SnO2electrical contact materials.(4) Ag-SnO2intermediates can alleviate the aggregation of SnO2nanoparticles in the following molding and sintering of Ag/SnO2electrical contact material and improved the properties of Ag/SnO2electrical contact materials,espe-cially for intermediates by high-energy ball milling. Compared with the electrical contact material prepared by traditional method, the better dispersion of SnO2nano-particles from intermediates significantly improved the properties of Ag/SnO2electri-cal contact material.The making arcing time and arcing energy are reduced from10ms to5ms,1000mJ to500mJ, respectively. The lower contact resistance and smaller welding force improve the anti-arc erosion ability and anti welding ability of Ag/SnO2electrical contact materials.
引文
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