化学镀法制备银氧化镱触点材料的研究
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摘要
论文针对共沉淀法制备AgYb203触点材料时,第二相粒子的粒径与形貌无法控制,且Ag与Yb_2O_3界面结合性能差等问题,开展化学镀法制备AgYb_2O_3复合粉体的研究,以期进一步提高AgYb_2O_3触点材料性能。
论文采用SEM、DSC等分析测试方法研究了前驱体粉体的粒径与形貌和焙烧制度对Yb_2O_3粉体粒径与形貌的影响。用液相沉淀法可以制得不同粒径及形貌的Yb_2O_3前驱体:用草酸为沉淀剂得到分散性良好的微米级条状前驱体Yb_2(C_2O_4)_3·4H_2O;用氨水和碳酸氢铵为沉淀剂,分别得到无定形的纳米级前驱体Yb(OH)_3·2H_2O和Yb_2(CO_3)_3·2.5H_2O;用尿素为沉淀剂得到球形的无定形的单分散前驱体Yb(OH)CO_3·H_2O。通过控制反应物浓度、反应温度、陈化温度与时间可以得到粒径在1-3μm间大小均一的草酸镱颗粒。依据前驱体的TG与DSC曲线确定非线性焙烧制度,改善了一般焙烧制度中颗粒团聚现象。相同升温制度下,焙烧温度越高,焙烧产物粒径越大。
利用化学镀法在不同粒径的氧化镱粉体表面包覆银,得到核壳结构的AgYb_2O_3复合粉体。本文研究了粉体预处理工艺、还原剂种类、PH值、甲醛浓度和反应温度对Yb_2O_3表面镀银效果和银还原率的影响。研究表明:敏化、活化处理促进银在Yb_2O_3表面还原析出,避免生成大量银镜。选择合适的还原剂可控制银还原速率,得到致密均匀的包覆层。PH值和反应温度的提高都可以增强甲醛的还原能力,但PH值和反应温度太高时,主盐溶液在反应过程中发生自分解。随着甲醛浓度的提高到60ml/L,甲醛与氨水反应生成六亚甲基四胺,所以银还原率先增大后减小。
复合粉体经压制、烧结、挤压和拉丝工艺制备成AgYb_2O_3线材,制得的线材具有良好的机械加工性能及物理性能。结果显示化学镀法制备的线材延伸率为17-19%,电阻率2.05-2.11/μΩ·cm,抗拉强度217-230MPa,硬度804-844N·mm~2。其机械加工性能优于共沉淀法制备的线材。
In order to improve the performance of AgYb_2O_3 electrical contact materials, it needs to control the morphology and size of Yb_2O_3 particle in electrical contact materials and improve the wettability and interface behavior of Ag-Yb_2O_3. AgYb_2O_3 composite powder was prepared by electroless plating instead of coprecipitation, accordingly.
Effects of the morphology and size of the precursors and calcination methods on the morphology and size of Yb_2O_3 powder were studied. The Yb_2O_3 precursors with different morphology and size can be made by precipitation in solution. Strip precursor Yb_2(C_2O_4)_3·4H_2O which is well dispersed in micron dimension was got using oxalic acid as precipitating agent. And amorphous precursor Yb(OH)_3·2H_2O and Yb_2(CO_3)_3·2.5H_2O in nano dimension when using ammonia and ammonium bicarbonate as precipitating agent. Single-dispersed spherical amorphous precursor Yb(OH)CO_3·H_2O can be got using urea as precipitation. Uniform ytterbium oxalate particle with the average diameter between 1-3μm can be prepared by controlling reactant concentration, react temperature, aging temperature and aging time. According to thermogravimetry and differential scanning calorimetry curves of precursor, a non-linear calcination method was established which can alleviate reunite phenomenon in calcination. The higer the calcination temperature is,the larger size Yb_2O_3 particle got.
Varied size ytterbia powder coated with Ag by electroless plating, AgYb_2O_3 composite powder with core/shell microstructure can be attained. The influence of powder pretreatment technics, reductant, PH values, formaldehyde concentration and react temperature was studied on plating Ag effect and the ratio of reduced Ag. It was found that Ag can be easily reduced on the surface of Yb_2O_3 powder after sensitization and activation treatment avoiding the appearnce of silver glass at the same time. Chosing right reductant can get compact and fine silver layer by controlling reducing speed. Increasing PH value and react temperature can enhance reducing ability of formaldehyde, but if they were too high, the solution will be self-reduced. When the formaldehyde concentration is more than 60ml/L, formaldehyde begins to react with ammonia. As the result, the ratio of reduced Ag rises at first ,then falls down.
AgYb_2O_3 wire was perared by AgYb_2O_3 composite powder via billet molding, sintering, extrusion and wire drawing. The result shows that the wire prepared by electroless plating behave better than the wire by coprecipitation on mechanical performance. The performance of former was that tensile strength was 217-230MPa, and hardness was 804-844 N·mm~2,and elongation was 17-19%; specific resistance was 2.05-2.11μΩ·cm.
论文采用SEM、DSC等分析测试方法研究了前驱体粉体的粒径与形貌和焙烧制度对Yb_2O_3粉体粒径与形貌的影响。用液相沉淀法可以制得不同粒径及形貌的Yb_2O_3前驱体:用草酸为沉淀剂得到分散性良好的微米级条状前驱体Yb_2(C_2O_4)_3·4H_2O;用氨水和碳酸氢铵为沉淀剂,分别得到无定形的纳米级前驱体Yb(OH)_3·2H_2O和Yb_2(CO_3)_3·2.5H_2O;用尿素为沉淀剂得到球形的无定形的单分散前驱体Yb(OH)CO_3·H_2O。通过控制反应物浓度、反应温度、陈化温度与时间可以得到粒径在1-3μm间大小均一的草酸镱颗粒。依据前驱体的TG与DSC曲线确定非线性焙烧制度,改善了一般焙烧制度中颗粒团聚现象。相同升温制度下,焙烧温度越高,焙烧产物粒径越大。
利用化学镀法在不同粒径的氧化镱粉体表面包覆银,得到核壳结构的AgYb_2O_3复合粉体。本文研究了粉体预处理工艺、还原剂种类、PH值、甲醛浓度和反应温度对Yb_2O_3表面镀银效果和银还原率的影响。研究表明:敏化、活化处理促进银在Yb_2O_3表面还原析出,避免生成大量银镜。选择合适的还原剂可控制银还原速率,得到致密均匀的包覆层。PH值和反应温度的提高都可以增强甲醛的还原能力,但PH值和反应温度太高时,主盐溶液在反应过程中发生自分解。随着甲醛浓度的提高到60ml/L,甲醛与氨水反应生成六亚甲基四胺,所以银还原率先增大后减小。
复合粉体经压制、烧结、挤压和拉丝工艺制备成AgYb_2O_3线材,制得的线材具有良好的机械加工性能及物理性能。结果显示化学镀法制备的线材延伸率为17-19%,电阻率2.05-2.11/μΩ·cm,抗拉强度217-230MPa,硬度804-844N·mm~2。其机械加工性能优于共沉淀法制备的线材。
In order to improve the performance of AgYb_2O_3 electrical contact materials, it needs to control the morphology and size of Yb_2O_3 particle in electrical contact materials and improve the wettability and interface behavior of Ag-Yb_2O_3. AgYb_2O_3 composite powder was prepared by electroless plating instead of coprecipitation, accordingly.
Effects of the morphology and size of the precursors and calcination methods on the morphology and size of Yb_2O_3 powder were studied. The Yb_2O_3 precursors with different morphology and size can be made by precipitation in solution. Strip precursor Yb_2(C_2O_4)_3·4H_2O which is well dispersed in micron dimension was got using oxalic acid as precipitating agent. And amorphous precursor Yb(OH)_3·2H_2O and Yb_2(CO_3)_3·2.5H_2O in nano dimension when using ammonia and ammonium bicarbonate as precipitating agent. Single-dispersed spherical amorphous precursor Yb(OH)CO_3·H_2O can be got using urea as precipitation. Uniform ytterbium oxalate particle with the average diameter between 1-3μm can be prepared by controlling reactant concentration, react temperature, aging temperature and aging time. According to thermogravimetry and differential scanning calorimetry curves of precursor, a non-linear calcination method was established which can alleviate reunite phenomenon in calcination. The higer the calcination temperature is,the larger size Yb_2O_3 particle got.
Varied size ytterbia powder coated with Ag by electroless plating, AgYb_2O_3 composite powder with core/shell microstructure can be attained. The influence of powder pretreatment technics, reductant, PH values, formaldehyde concentration and react temperature was studied on plating Ag effect and the ratio of reduced Ag. It was found that Ag can be easily reduced on the surface of Yb_2O_3 powder after sensitization and activation treatment avoiding the appearnce of silver glass at the same time. Chosing right reductant can get compact and fine silver layer by controlling reducing speed. Increasing PH value and react temperature can enhance reducing ability of formaldehyde, but if they were too high, the solution will be self-reduced. When the formaldehyde concentration is more than 60ml/L, formaldehyde begins to react with ammonia. As the result, the ratio of reduced Ag rises at first ,then falls down.
AgYb_2O_3 wire was perared by AgYb_2O_3 composite powder via billet molding, sintering, extrusion and wire drawing. The result shows that the wire prepared by electroless plating behave better than the wire by coprecipitation on mechanical performance. The performance of former was that tensile strength was 217-230MPa, and hardness was 804-844 N·mm~2,and elongation was 17-19%; specific resistance was 2.05-2.11μΩ·cm.
引文
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[4] 李英民，薛纪文，王俊勃．AgSnO_2电触头的研究进展[J]．电工材料，2003，(2)：20-27．
[5] 堵永国，白书欣，张家春．一种全新AgSnO_2触点材料的设计与制备[J]．电工合金，2000，(1)：15-22．
[6] 王家真，王亚平，杨志懋．CuO添加剂对Ag／SnO_2润湿性与界面特性的影响[J]．稀有金属材料与工程，2005，34(3)：405-408．
[7] Schoepf T.J., Behrens V., Honig T. Development of silver zinc oxide for general-purpose relays[J]. Transactions On Component and Packaging Technologies, 2002, 25(4):656-662.
[8] 范莉．添加镍元素对烧结Ag-ZnO电触头性能的影响[J]．新技术新工艺，2003，(2)：40-41．
[9]中村哲也，坂口理，草森裕之．Ag-ZnO系电触点材料的制造方法及该电触点材料[P]．CN Patent：1300440A．2000．
[10]王继周，徐永昌，石路．稀土贵金属电接触材料的进展[J]．有色矿冶，1995，(5)：35-39．
[11]闫杏丽，陈敬超，于杰．合金内氧化法在制备银氧化铜(AgCuO)电触头材料中的应用[J]．电工材料，2003，(2)：28-31．
[12]Hauner F. Ag-Fe and Ag-Fe_2O_3 contact materials for low votage switchgear[C].Proc 19th ICEC, 1998.
[13] Behrens V., Honig T.H. An advanced silver/tin Oxide contact material[C]. Proc 17th IEEE Trans, 1994.
[14]Joshi P.B., Murti N.S.S., Gadgeel V.L. Preparation and characterization of Ag-ZnO powders for applications in electrical contact materials[J]. Journal of Materials Science Letters, 1995, (14):1099-1011.
[15] Ernest M.J., Kirk M. Electrically conductive material and method for making[P]. US Patent: 5846288. 1998.
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