高抗蚀性烧结钕铁硼制备与性能研究
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摘要
烧结钕铁硼是应用最广泛的稀土永磁材料,具有磁性能高、膨胀系数低和价格低等优点,成为现代社会和高新技术的重要基础材料。但由于晶界相和主相之间的电极电位差大,易发生晶间腐蚀,磁体耐蚀性差,严重限制其在重要领域的应用。本文基于双合金工艺,设计、制备了(Pr,Nd)-Fe-Cu和A1-Cu高腐蚀电位辅合金,通过优化辅合金含量,改善了晶界相组织和理化特性,抑制和消弱了晶界相与主相间的电化学反应,成功研制出兼具高抗蚀性和高磁性能的钕铁硼磁体。主要结果如下：
基于热力学分析、合金腐蚀理论和Nd-Fe-Cu相图,设计制备了(Pr,Nd)32.5Fe62.0-Cu5.5、(Pr,Nd)22.0Fe71.6Cu6.4、(Pr,Nd)12.0Fe80.8Cu7.2高电位辅合金。辅合金的组成元素不向(Pr,Nd)2Fe14B主相中扩散,有利于制备高磁性的磁体；辅合金的腐蚀电位高(--0.8 V),有利于降低晶界相与主相之间的电位差,降低晶界腐蚀动力；辅合金熔点低(～506℃),有利于磁体液相烧结。
利用高电位(Pr,Nd)-Fe-Cu辅合金粉,成功制备出兼具高抗蚀性和高磁性能的烧结钕铁硼磁体,研究揭示了磁体在不同环境中的抗蚀机理。磁体的最大磁能积为356.0-384.0 kJ/m3(45-48 MGOe),在120℃、2 atm、100%相对湿度环境中腐蚀96 h的质量损失为0.3-1.0 mg/cm2,在0.005 M H2SO4溶液中腐蚀电流密度可降至148.9μA/cm2。添加12 wt%(Pr,Nd)32.5Fe62.oCu5.5的替代磁体在0.005 MH2SO4、0.6 M NaCl、0.75 M NaOH溶液和湿热环境中,比非替代磁体((Pr,Nd)14.5-Fe79.5B6.o)的抗蚀性好,前者腐蚀96h的质量损失约为后者的1/16,其原因在于前者中的(Pr,Nd)6Fe13Cu晶界相与(Pr,Nd)2Fe14B主相的腐蚀电位(～0.7 V)接近,这降低了晶界相与主相之间的电位差,降低了晶界相发生电化学腐蚀的动力,也降低了晶界相与水发生氧化腐蚀的动力。磁体的最大磁能积随辅合金添加量的增加先增大后减小,(Pr,Nd)32.5(Pr,Nd)22.oFe71.6Cu6.4、(Pr,Nd)12.oFe80.8Cu7.2添加量分别为3 wt%、3 wt%和2 wt%时,磁能积达到最大值,分别为384.0、368.5、365.4 kJ/m3。
研究揭示了A1-Cu辅合金粉对烧结钕铁硼磁体显微组织、抗蚀性和磁性的作用机理。掺Al100-xCux(X=15,25,35,45 at.%)改善了(Pr,Nd)14.8Fe78.7B6.5的晶界相分布状况和化学稳定性,提高了磁体抗蚀性,磁体在120℃、2 atm、100%相对湿度环境中腐蚀96 h的质量损失从114.9 mg/cm2降为4.2 mg/cm2;同时也提高了磁性能,磁体的矫顽力从920 kA/m增加为1201 kA/m。磁体晶界显微组织与Cu/Al分布及合金化行为密切相关,增加Al-Cu添加量或其Cu含量,促进(Pr,Nd)Cu(除CuAl2之外)低熔点相析出,影响了晶界组织的演化特点,使磁体的最佳回火温度从550℃降至480℃。回火时(Pr,Nd)-Cu或Al-Cu液相能够改善富(Pr,Nd)晶界相的形态和分布状况,增强其去磁耦合作用,提高了矫顽力,改善了退磁曲线方形度,提高了磁体的磁能积。
Nd-Fe-B sintered magnets are the most widely used magnetic materials due to excellent magnetic properties, low expansion coefficient and low price. They have become the important basica materials for high technology in modern society. However, Nd-Fe-B magnets are sensitive to the grain boundary corrosion because of the large difference of electrode potential between the matrix and intergranular phases, which limits the applications in many important fields. The purpose of this work is to develop corrosion resistant mangets using two-alloy method through designing (Pr.Nd)-Fe-Cu and Al-Cu aid alloys with high corrosion potential. The morphologies as well as physical and chemical characteristics of grain boundaries were optimized to weaken the electrochemical reactions between the matrix and intergranular phases. Finally, corrosion-resistant Nd-Fe-B magnets with outstanding magnetic properties were produced through adopting the content of aid alloys. Main results of the thesis are as follows:
Acorrding to thermodynamics analysis, corrosion theory of alloys and phase diagram of Nd-Fe-Cu, aid alloys of (Pr,Nd)32.5Fe62.oCu5.5/(Pr,Nd)22.0Fe7i.6Cu6.4/ (Pr.Nd)12.oFe800.8Cu7.2 with high corrosion potential were designed and prepared. Their components did not diffuse into the (Pr,Nd)2Fe14B matrix phase, which benefits the fabrication of highly performant magnets. These alloys had higher corrosion potential (～-0.8 V), which benefits the decrease of the potential difference between the matrix and intergranular phases, thus decreaseing the driving force for the grain boundary corrosion. Moreover, these alloys possessed a low melting piont (～506℃), which benefits the liquid sintering of magnets.
Corrosion-resistant Nd-Fe-B sintered magnets with excellent magnetic properties were successfuly fabricated using the (Pr.Nd)-Fe-Cu aid alloy powders with high corrosion potential. Meanwhile, their corrosion-resistant mechanism in different enviorments was investigated. These magnets had the maximum energy products of 356.0-384.0 kJ/m3 (45-48 MGOe) and possessed a low mass loss of 0.3-1.0 mg/cm2 in 120℃,2 atm and 100% relative humid atmosphere for 96 h. Moreover, their corrosion current density reached 148.9μA/cm2 in 0.005 M H2SO4 solution. The magnet with 12 wt%(Pr,Nd)32.5Fe62.0Cu5.5 had a better corrosion resistance than (Pr.Nd)14.5Fe79.5-B6.0 in 0.005 M H2SO4,0.6 M NaCl,0.75 M NaOH solutions or humid/hot environments. The mass loss of the former magnet corrded for 96 h was about 1/16 times in comparison to the latter one. The reason for a better corrosion resistance of former magnet can be ascribed to the closer equal corrosion potential of (Pr,Nd)6Fe13Cu to the (Pr,Nd)2Fe14B phase. It reduces the potential difference between the cathodic matrix phase and the anodic grain boundary phases, leading to the decrease in the driving force for the electrochemical corrosion of grain boundary phases. Additionally it decreases driving force in the oxidation or hydrogen reactions of grain boundary phase with H2O. Moreover, the maxium energy product of magnets first increased with addition of (Pr,Nd)-Fe-Cu and then decreased after the maxiumu values at the optimum amount of 3 wt%,3 wt% and 2 wt% for (Pr,Nd)32.5Fe62.oCu5.5/ (Pr,Nd)22.oFe71.6Cu6.4/(Pr,Nd)12.oFe80.8Cu7.2. Their maximum values were 384.0,368.5 and 365.4 kJ/m3, respectively.
The mechanism of the effect of Al-Cu aid alloy powders on the microstructure, the corrosion resistance and the magnetic properties was investigated. It was found that addition of Al100-xCux (x=15,25,35,45 at.%) to (Pr,Nd)14.8Fe78.7B6.5 could improve the distribution and chemical stability of intergranular phases, which increase the corrosion resistance of magnets. Their mass loss was decreased from 114.9 to 4.2 mg/cm2 in 120℃,2 atm and 100% relative humid atmosphere for 96 h. Also the improvement of grain boundary microstructure increased the magnetic properties, especially the coercivity from 920 to 1201 kA/m. The grain boundary morphologies closely relate the distribution and alloying behavior of Cu/Al in magnets. Increasing Al-Cu amount or its Cu content promotes the precipation of the low-melting phases of (Pr,Nd)Cu besides CuAl2, which affects the morphology evolution of grain boundaries and thus reduces the optimum annealing temperature of magnets from 550 to 480℃. During annealing the (Pr,Nd)-Cu or Al-Cu liquid phase can improve the morphology/ distribution of the Nd-rich phase and increase the decouple effects, leading to the increase of coercivity. Meanwhile, it improves the squareness of demagnetizing loops and increases the maxium energy products of magnets.
基于热力学分析、合金腐蚀理论和Nd-Fe-Cu相图,设计制备了(Pr,Nd)32.5Fe62.0-Cu5.5、(Pr,Nd)22.0Fe71.6Cu6.4、(Pr,Nd)12.0Fe80.8Cu7.2高电位辅合金。辅合金的组成元素不向(Pr,Nd)2Fe14B主相中扩散,有利于制备高磁性的磁体；辅合金的腐蚀电位高(--0.8 V),有利于降低晶界相与主相之间的电位差,降低晶界腐蚀动力；辅合金熔点低(～506℃),有利于磁体液相烧结。
利用高电位(Pr,Nd)-Fe-Cu辅合金粉,成功制备出兼具高抗蚀性和高磁性能的烧结钕铁硼磁体,研究揭示了磁体在不同环境中的抗蚀机理。磁体的最大磁能积为356.0-384.0 kJ/m3(45-48 MGOe),在120℃、2 atm、100%相对湿度环境中腐蚀96 h的质量损失为0.3-1.0 mg/cm2,在0.005 M H2SO4溶液中腐蚀电流密度可降至148.9μA/cm2。添加12 wt%(Pr,Nd)32.5Fe62.oCu5.5的替代磁体在0.005 MH2SO4、0.6 M NaCl、0.75 M NaOH溶液和湿热环境中,比非替代磁体((Pr,Nd)14.5-Fe79.5B6.o)的抗蚀性好,前者腐蚀96h的质量损失约为后者的1/16,其原因在于前者中的(Pr,Nd)6Fe13Cu晶界相与(Pr,Nd)2Fe14B主相的腐蚀电位(～0.7 V)接近,这降低了晶界相与主相之间的电位差,降低了晶界相发生电化学腐蚀的动力,也降低了晶界相与水发生氧化腐蚀的动力。磁体的最大磁能积随辅合金添加量的增加先增大后减小,(Pr,Nd)32.5(Pr,Nd)22.oFe71.6Cu6.4、(Pr,Nd)12.oFe80.8Cu7.2添加量分别为3 wt%、3 wt%和2 wt%时,磁能积达到最大值,分别为384.0、368.5、365.4 kJ/m3。
研究揭示了A1-Cu辅合金粉对烧结钕铁硼磁体显微组织、抗蚀性和磁性的作用机理。掺Al100-xCux(X=15,25,35,45 at.%)改善了(Pr,Nd)14.8Fe78.7B6.5的晶界相分布状况和化学稳定性,提高了磁体抗蚀性,磁体在120℃、2 atm、100%相对湿度环境中腐蚀96 h的质量损失从114.9 mg/cm2降为4.2 mg/cm2;同时也提高了磁性能,磁体的矫顽力从920 kA/m增加为1201 kA/m。磁体晶界显微组织与Cu/Al分布及合金化行为密切相关,增加Al-Cu添加量或其Cu含量,促进(Pr,Nd)Cu(除CuAl2之外)低熔点相析出,影响了晶界组织的演化特点,使磁体的最佳回火温度从550℃降至480℃。回火时(Pr,Nd)-Cu或Al-Cu液相能够改善富(Pr,Nd)晶界相的形态和分布状况,增强其去磁耦合作用,提高了矫顽力,改善了退磁曲线方形度,提高了磁体的磁能积。
Nd-Fe-B sintered magnets are the most widely used magnetic materials due to excellent magnetic properties, low expansion coefficient and low price. They have become the important basica materials for high technology in modern society. However, Nd-Fe-B magnets are sensitive to the grain boundary corrosion because of the large difference of electrode potential between the matrix and intergranular phases, which limits the applications in many important fields. The purpose of this work is to develop corrosion resistant mangets using two-alloy method through designing (Pr.Nd)-Fe-Cu and Al-Cu aid alloys with high corrosion potential. The morphologies as well as physical and chemical characteristics of grain boundaries were optimized to weaken the electrochemical reactions between the matrix and intergranular phases. Finally, corrosion-resistant Nd-Fe-B magnets with outstanding magnetic properties were produced through adopting the content of aid alloys. Main results of the thesis are as follows:
Acorrding to thermodynamics analysis, corrosion theory of alloys and phase diagram of Nd-Fe-Cu, aid alloys of (Pr,Nd)32.5Fe62.oCu5.5/(Pr,Nd)22.0Fe7i.6Cu6.4/ (Pr.Nd)12.oFe800.8Cu7.2 with high corrosion potential were designed and prepared. Their components did not diffuse into the (Pr,Nd)2Fe14B matrix phase, which benefits the fabrication of highly performant magnets. These alloys had higher corrosion potential (～-0.8 V), which benefits the decrease of the potential difference between the matrix and intergranular phases, thus decreaseing the driving force for the grain boundary corrosion. Moreover, these alloys possessed a low melting piont (～506℃), which benefits the liquid sintering of magnets.
Corrosion-resistant Nd-Fe-B sintered magnets with excellent magnetic properties were successfuly fabricated using the (Pr.Nd)-Fe-Cu aid alloy powders with high corrosion potential. Meanwhile, their corrosion-resistant mechanism in different enviorments was investigated. These magnets had the maximum energy products of 356.0-384.0 kJ/m3 (45-48 MGOe) and possessed a low mass loss of 0.3-1.0 mg/cm2 in 120℃,2 atm and 100% relative humid atmosphere for 96 h. Moreover, their corrosion current density reached 148.9μA/cm2 in 0.005 M H2SO4 solution. The magnet with 12 wt%(Pr,Nd)32.5Fe62.0Cu5.5 had a better corrosion resistance than (Pr.Nd)14.5Fe79.5-B6.0 in 0.005 M H2SO4,0.6 M NaCl,0.75 M NaOH solutions or humid/hot environments. The mass loss of the former magnet corrded for 96 h was about 1/16 times in comparison to the latter one. The reason for a better corrosion resistance of former magnet can be ascribed to the closer equal corrosion potential of (Pr,Nd)6Fe13Cu to the (Pr,Nd)2Fe14B phase. It reduces the potential difference between the cathodic matrix phase and the anodic grain boundary phases, leading to the decrease in the driving force for the electrochemical corrosion of grain boundary phases. Additionally it decreases driving force in the oxidation or hydrogen reactions of grain boundary phase with H2O. Moreover, the maxium energy product of magnets first increased with addition of (Pr,Nd)-Fe-Cu and then decreased after the maxiumu values at the optimum amount of 3 wt%,3 wt% and 2 wt% for (Pr,Nd)32.5Fe62.oCu5.5/ (Pr,Nd)22.oFe71.6Cu6.4/(Pr,Nd)12.oFe80.8Cu7.2. Their maximum values were 384.0,368.5 and 365.4 kJ/m3, respectively.
The mechanism of the effect of Al-Cu aid alloy powders on the microstructure, the corrosion resistance and the magnetic properties was investigated. It was found that addition of Al100-xCux (x=15,25,35,45 at.%) to (Pr,Nd)14.8Fe78.7B6.5 could improve the distribution and chemical stability of intergranular phases, which increase the corrosion resistance of magnets. Their mass loss was decreased from 114.9 to 4.2 mg/cm2 in 120℃,2 atm and 100% relative humid atmosphere for 96 h. Also the improvement of grain boundary microstructure increased the magnetic properties, especially the coercivity from 920 to 1201 kA/m. The grain boundary morphologies closely relate the distribution and alloying behavior of Cu/Al in magnets. Increasing Al-Cu amount or its Cu content promotes the precipation of the low-melting phases of (Pr,Nd)Cu besides CuAl2, which affects the morphology evolution of grain boundaries and thus reduces the optimum annealing temperature of magnets from 550 to 480℃. During annealing the (Pr,Nd)-Cu or Al-Cu liquid phase can improve the morphology/ distribution of the Nd-rich phase and increase the decouple effects, leading to the increase of coercivity. Meanwhile, it improves the squareness of demagnetizing loops and increases the maxium energy products of magnets.
引文
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