铜—银、镍—银核—壳型双金属粉及锆酸钙包覆镍粉的研制
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摘要
近年来,多层陶瓷电容器(MLCC)内电极贱金属化的飞速发展拓展了铜、镍粉的应用领域;在电子、电器、通信、现代电子战争、军舰、核潜艇等领域,为了防止外来的电磁干扰和防止本身的电磁波向外辐射,镍粉由于具有良好的电磁屏蔽性能成为电磁屏蔽导电涂料的主要原料。镍、铜在高温下易氧化,形成绝缘性氧化膜,故在使用过程中必须解决铜、镍粉的氧化问题。
本论文旨在探索和研究贱金属铜、镍粉高温抗氧化问题。在调研有关金属粉体表面改性文献及理论分析的基础上,采用银盐滴加镀银新工艺,开展了化学镀法制备银包铜粉与银包镍粉的研究;开展了化学沉淀法在镍粉表面包覆一层锆酸钙进行表面改性的研究,具体内容如下:
铜、镍活性比金属银强,与Ag的置换反应不利于光洁的Ag镀层的形成。通过热力学分析,选择了水合肼作为还原剂,分析了其抑制体系中银铜置换反应的可行性。
通过Zeta电位及浊度的测量,表征了铜粉与镍粉在不同分散体系的稳定性。首先研究了铜粉在PVP和酒石酸钠溶液体系中的分散,结果表明两者皆具有良好的分散效果;静电斥力是酒石酸钠改善分散体系稳定状态的基础,而静电斥力稳定作用和空间位阻效应是PVP改善分散体系稳定状态的基础。其次研究了镍粉在PVP-水-乙醇及酒石酸钠-水体系中的分散,结果表明两者皆具有良好的分散效果。
化学镀法制备铜-银双金属粉过程中,采用了低成本的AgNO_3取代传统的PdCl_2,研究了惰性基体铜粉表面的敏化、活化工艺及活化机理。研究了镀液pH、反应温度、PVP添加量、水合肼浓度等因素对双金属粉高温抗氧化性能及残留银离子浓度的影响。实验结果显示最佳工艺条件为:铜粉分散液组成:乙醇浓度333mL/L,活化铜粉33.3g/L、PVP用量为10.0g/L、起始pH为10.0、水合肼浓度2.5mol/L;铜粉分散液用量150mL;反应温度50～55℃;银氨溶液浓度0.5mol/L,用量78.1mL。银盐滴加镀银新工艺,有效解决了镀银过程中银粉单独沉积的问题,制备的银包铜粉仍具有良好的分散性、常温和高温抗氧化性能;二次包覆双金属粉表面形成了连续的银膜,其氧化增重从原样铜粉的23.78%降低到了1.20%;双金属粉在氧化气氛下仍保持良好的导电性能。
化学镀法制备镍-银双金属粉过程中,探讨了镀液pH、反应温度、PVP添加量及加入方式、水合肼浓度、分散体系等因素对双金属粉高温抗氧化性及残留银离子浓度的影响。结果显示最佳工艺条件为:镍粉分散体系组成:乙醇浓度417mL/L,镍粉25.0g/L、PVP添加量为8.33g/L、起始pH为11.0、水合肼浓度2.5mol/L;镍粉分散液用量120mL;反应温度60℃;银氨溶液浓度0.5mol/L,用量51mL,加入方式为缓慢滴加。通过化学镀获得的镍-银双金属粉体具有良好的分散性能;二次包覆镍-银双金属粉高温抗氧化性与原样镍粉相比,起始氧化温度由最初的290.45℃上升到389.36℃。
采用化学沉淀法在甲醇-水体系中成功制备了锆酸钙包覆复合镍粉,考察了包覆试剂用量、搅拌速度、包覆试剂加入方式、复合镍粉前驱体热处理温度、搅拌时间、反应温度、分散剂用量、包覆试剂加入速度以及镍粉表面处理对复合镍粉性能、形貌的影响。根据实验结果,获得最佳工艺条件为:包覆试剂以锆酸钙计与镍粉的重量比5.9:100;采用将锆-钙溶液与沉淀剂溶液同时滴加到镍粉的醇水包覆体系中的试剂加入方式;加入流量0.65 mL·min~(-1);镍粉分散体系总量186 mL,其中H_2O 60mL,甲醇126mL;反应温度55℃;反应时间90min;搅拌速度350r/min;前驱体热处理温度690℃。此条件下制得的复合镍粉,通过TG-DTA、SEM、导电性等来表征其性质,结果表明所得复合镍粉具有良好的导电性及高温抗氧化,粉体分散性好,适于用作MLCC内电极材料。
Recent years,the application scopes of copper and nickel powders were broadened with the rapid development of inner electrode utilizing base metal for MLCC(multilayer ceramic capacitors).In order to avoid electromagnetism interference and electromagnetism wave radiating, nickel powders become a main material of electric paint because of its excellent electromagnetism wave shielding properties in the scopes of electron,electrical facility,communications,modern electron war, warship,nuke and so on.Copper and nickel powders are apt to be oxidated in high temperature,to form an insulated oxide film,so the oxidation problem of them must be solved.
This dissertation aimed to solve anti-oxidation of copper and nickel powders in high temperature.On the basis of thorough review of large amount of references on surface modification and theory analysis,a novel electroless plating method—silver salt dripping method has been proposed and used for the preparation of Cu-Ag and Ni-Ag bimetals.The surface modification of nickel powders has been carried out by using chemical precipitation to coat Ni powders with CaZrO_3.The details are summarized as the followings.
Copper and nickel powders have stronger activity than silver,their displacement reaction with silver makes against forming a smooth silver layer.Through thermodynamic analysis,N_2H_4 was selected as the reducing agent and possibility of restraining the displacement reaction was studied.
The dispersibility of Cu powder and Ni powder suspended solutions was investigated by measuring Zeta potential and turbidity of the suspended solutions.First,dispersion stability of Cu powder respectively using PVP and sodium Tartrate as a dispersant,Cu powder possesses good dispersion property both in PVP-water-ethanol system and sodium Tartrate-water system.The system stabilization is based on electrostatic repulsion with sodium Tartrate acting as dispersant,and based both on electrostatic repulsion and spatial position resistance with PVP as dispersant.Secondly,dispersion stability of nickel powder was discussed in the system of PVP-water-ethanol and sodium Tartrate-water, experiments show that both of them possessed good dispersion effect.
During the preparation of Cu-Ag bimetal via electroless plating,first of all,the sensitization and activation process on copper powder surface were studied using AgNO_3 as an activating agent instead of conventional PdCl_2,and the activation mechanism was determinate.The effects of pH, reaction temperature,dosage of PVP,concentration of N_2H_4 on anti-oxidation property of bimetal and residual Ag~+ concentration were studied.Experiments show that the optimal conditions are as the followings:the copper-suspended solution compositions are ethanol 333mL/L,the activated copper powers 33.3g/L,pH 10.0,dosage of PVP 10g/L,N_2H_4 2.5mol/L;the copper-suspended solution volume is 150mL; reaction temperature is 50～55℃;the N_2H_4 concentration and volume of silver ammine solution are 0.5mol/L and 78.1mL respectively.The results show that the dipping mode of silver ammine solution can prevent silver from precipitating as separate particles.Prepared bimetal powders possess good dispersion property and good anti-oxidation at room and high temperature.A continuous film is formed on the surface of copper particles applied Ag coating two times,and the oxidation mass increase reduced from 23.78%of uncoated copper powders to 1.20%.Bimetal powders possess better electric performance in air atmosphere.
During the preparation of Ni-Ag bimetal via electroless plating,the effects of pH,reaction temperature,dosage and feed mode of PVP, concentration of N_2H_4 and dispersion system on bimetal anti-oxidation properties and residual Ag~+ concentration were studied.Experiments show that the optimal conditions were as the followings:the nickel-suspended solution compositions are ethanol 417mL/L,the nickel powers 25g/L,pH 11.0,dosage of PVP 8.33 g/L,N_2H_4 2.5mol/L;the copper-suspended solution volume is 120mL;reaction temperature is 60℃;the N_2H_4 concentration and volume of silver ammine solution are 0.5mol/L and 51mL respectively.Ni-Ag bimetal powders possess good dispersion property.The initial oxidation temperature notably rises from 290.45℃to 389.36℃.
CaZrO_3-coated nickel powders have been synthesized in methanol-water solvent.The effects of the amount of modification agent and dispersant,mixing speed,feed mode and flow rate of modification agent,heat treatment temperature of the composite nickel powder precursor,mixing time,reaction temperature and surface treatment of the origin Ni on composite nickel powders' properties were investigated. Through analysis of the experiment data,the optimum conditions were as the followings:the mass ratio of modification agent counted by CaZrO_3 to original nickel powder is 5.9 to 100;both precipitation agents solution and zirconium-calcium solution are dripped at the meantime into the Ni-particle-dispersed methanol solution,with the flow rate of 0.65mL·min~(-1) respectively,H_2O is 60mL and CH_3OH is 126mL in methanol-water solvent,reaction temperature is 55℃,reaction time is 90 min,mixing speed is 350r/min,heat treatment temperature of the composite nickel powder precursor is 690℃.Composite nickel powders obtained under the optimum conditions were characterized by TG-DTA、SEM and the electric conductivity.It was approved that those composite nickel powders not only afforded the strong resistance to oxidation,but also had high electric conductivity.In addition,these powders have displayed good dispersion property.These features of CaZrO_3-coated Ni powders have a good agreement with the demand of internal electrode material of MLCC.
本论文旨在探索和研究贱金属铜、镍粉高温抗氧化问题。在调研有关金属粉体表面改性文献及理论分析的基础上,采用银盐滴加镀银新工艺,开展了化学镀法制备银包铜粉与银包镍粉的研究;开展了化学沉淀法在镍粉表面包覆一层锆酸钙进行表面改性的研究,具体内容如下:
铜、镍活性比金属银强,与Ag的置换反应不利于光洁的Ag镀层的形成。通过热力学分析,选择了水合肼作为还原剂,分析了其抑制体系中银铜置换反应的可行性。
通过Zeta电位及浊度的测量,表征了铜粉与镍粉在不同分散体系的稳定性。首先研究了铜粉在PVP和酒石酸钠溶液体系中的分散,结果表明两者皆具有良好的分散效果;静电斥力是酒石酸钠改善分散体系稳定状态的基础,而静电斥力稳定作用和空间位阻效应是PVP改善分散体系稳定状态的基础。其次研究了镍粉在PVP-水-乙醇及酒石酸钠-水体系中的分散,结果表明两者皆具有良好的分散效果。
化学镀法制备铜-银双金属粉过程中,采用了低成本的AgNO_3取代传统的PdCl_2,研究了惰性基体铜粉表面的敏化、活化工艺及活化机理。研究了镀液pH、反应温度、PVP添加量、水合肼浓度等因素对双金属粉高温抗氧化性能及残留银离子浓度的影响。实验结果显示最佳工艺条件为:铜粉分散液组成:乙醇浓度333mL/L,活化铜粉33.3g/L、PVP用量为10.0g/L、起始pH为10.0、水合肼浓度2.5mol/L;铜粉分散液用量150mL;反应温度50～55℃;银氨溶液浓度0.5mol/L,用量78.1mL。银盐滴加镀银新工艺,有效解决了镀银过程中银粉单独沉积的问题,制备的银包铜粉仍具有良好的分散性、常温和高温抗氧化性能;二次包覆双金属粉表面形成了连续的银膜,其氧化增重从原样铜粉的23.78%降低到了1.20%;双金属粉在氧化气氛下仍保持良好的导电性能。
化学镀法制备镍-银双金属粉过程中,探讨了镀液pH、反应温度、PVP添加量及加入方式、水合肼浓度、分散体系等因素对双金属粉高温抗氧化性及残留银离子浓度的影响。结果显示最佳工艺条件为:镍粉分散体系组成:乙醇浓度417mL/L,镍粉25.0g/L、PVP添加量为8.33g/L、起始pH为11.0、水合肼浓度2.5mol/L;镍粉分散液用量120mL;反应温度60℃;银氨溶液浓度0.5mol/L,用量51mL,加入方式为缓慢滴加。通过化学镀获得的镍-银双金属粉体具有良好的分散性能;二次包覆镍-银双金属粉高温抗氧化性与原样镍粉相比,起始氧化温度由最初的290.45℃上升到389.36℃。
采用化学沉淀法在甲醇-水体系中成功制备了锆酸钙包覆复合镍粉,考察了包覆试剂用量、搅拌速度、包覆试剂加入方式、复合镍粉前驱体热处理温度、搅拌时间、反应温度、分散剂用量、包覆试剂加入速度以及镍粉表面处理对复合镍粉性能、形貌的影响。根据实验结果,获得最佳工艺条件为:包覆试剂以锆酸钙计与镍粉的重量比5.9:100;采用将锆-钙溶液与沉淀剂溶液同时滴加到镍粉的醇水包覆体系中的试剂加入方式;加入流量0.65 mL·min~(-1);镍粉分散体系总量186 mL,其中H_2O 60mL,甲醇126mL;反应温度55℃;反应时间90min;搅拌速度350r/min;前驱体热处理温度690℃。此条件下制得的复合镍粉,通过TG-DTA、SEM、导电性等来表征其性质,结果表明所得复合镍粉具有良好的导电性及高温抗氧化,粉体分散性好,适于用作MLCC内电极材料。
Recent years,the application scopes of copper and nickel powders were broadened with the rapid development of inner electrode utilizing base metal for MLCC(multilayer ceramic capacitors).In order to avoid electromagnetism interference and electromagnetism wave radiating, nickel powders become a main material of electric paint because of its excellent electromagnetism wave shielding properties in the scopes of electron,electrical facility,communications,modern electron war, warship,nuke and so on.Copper and nickel powders are apt to be oxidated in high temperature,to form an insulated oxide film,so the oxidation problem of them must be solved.
This dissertation aimed to solve anti-oxidation of copper and nickel powders in high temperature.On the basis of thorough review of large amount of references on surface modification and theory analysis,a novel electroless plating method—silver salt dripping method has been proposed and used for the preparation of Cu-Ag and Ni-Ag bimetals.The surface modification of nickel powders has been carried out by using chemical precipitation to coat Ni powders with CaZrO_3.The details are summarized as the followings.
Copper and nickel powders have stronger activity than silver,their displacement reaction with silver makes against forming a smooth silver layer.Through thermodynamic analysis,N_2H_4 was selected as the reducing agent and possibility of restraining the displacement reaction was studied.
The dispersibility of Cu powder and Ni powder suspended solutions was investigated by measuring Zeta potential and turbidity of the suspended solutions.First,dispersion stability of Cu powder respectively using PVP and sodium Tartrate as a dispersant,Cu powder possesses good dispersion property both in PVP-water-ethanol system and sodium Tartrate-water system.The system stabilization is based on electrostatic repulsion with sodium Tartrate acting as dispersant,and based both on electrostatic repulsion and spatial position resistance with PVP as dispersant.Secondly,dispersion stability of nickel powder was discussed in the system of PVP-water-ethanol and sodium Tartrate-water, experiments show that both of them possessed good dispersion effect.
During the preparation of Cu-Ag bimetal via electroless plating,first of all,the sensitization and activation process on copper powder surface were studied using AgNO_3 as an activating agent instead of conventional PdCl_2,and the activation mechanism was determinate.The effects of pH, reaction temperature,dosage of PVP,concentration of N_2H_4 on anti-oxidation property of bimetal and residual Ag~+ concentration were studied.Experiments show that the optimal conditions are as the followings:the copper-suspended solution compositions are ethanol 333mL/L,the activated copper powers 33.3g/L,pH 10.0,dosage of PVP 10g/L,N_2H_4 2.5mol/L;the copper-suspended solution volume is 150mL; reaction temperature is 50～55℃;the N_2H_4 concentration and volume of silver ammine solution are 0.5mol/L and 78.1mL respectively.The results show that the dipping mode of silver ammine solution can prevent silver from precipitating as separate particles.Prepared bimetal powders possess good dispersion property and good anti-oxidation at room and high temperature.A continuous film is formed on the surface of copper particles applied Ag coating two times,and the oxidation mass increase reduced from 23.78%of uncoated copper powders to 1.20%.Bimetal powders possess better electric performance in air atmosphere.
During the preparation of Ni-Ag bimetal via electroless plating,the effects of pH,reaction temperature,dosage and feed mode of PVP, concentration of N_2H_4 and dispersion system on bimetal anti-oxidation properties and residual Ag~+ concentration were studied.Experiments show that the optimal conditions were as the followings:the nickel-suspended solution compositions are ethanol 417mL/L,the nickel powers 25g/L,pH 11.0,dosage of PVP 8.33 g/L,N_2H_4 2.5mol/L;the copper-suspended solution volume is 120mL;reaction temperature is 60℃;the N_2H_4 concentration and volume of silver ammine solution are 0.5mol/L and 51mL respectively.Ni-Ag bimetal powders possess good dispersion property.The initial oxidation temperature notably rises from 290.45℃to 389.36℃.
CaZrO_3-coated nickel powders have been synthesized in methanol-water solvent.The effects of the amount of modification agent and dispersant,mixing speed,feed mode and flow rate of modification agent,heat treatment temperature of the composite nickel powder precursor,mixing time,reaction temperature and surface treatment of the origin Ni on composite nickel powders' properties were investigated. Through analysis of the experiment data,the optimum conditions were as the followings:the mass ratio of modification agent counted by CaZrO_3 to original nickel powder is 5.9 to 100;both precipitation agents solution and zirconium-calcium solution are dripped at the meantime into the Ni-particle-dispersed methanol solution,with the flow rate of 0.65mL·min~(-1) respectively,H_2O is 60mL and CH_3OH is 126mL in methanol-water solvent,reaction temperature is 55℃,reaction time is 90 min,mixing speed is 350r/min,heat treatment temperature of the composite nickel powder precursor is 690℃.Composite nickel powders obtained under the optimum conditions were characterized by TG-DTA、SEM and the electric conductivity.It was approved that those composite nickel powders not only afforded the strong resistance to oxidation,but also had high electric conductivity.In addition,these powders have displayed good dispersion property.These features of CaZrO_3-coated Ni powders have a good agreement with the demand of internal electrode material of MLCC.
引文
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