CN111018519B - 一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法 - Google Patents

一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法 Download PDF

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CN111018519B
CN111018519B CN201911411367.1A CN201911411367A CN111018519B CN 111018519 B CN111018519 B CN 111018519B CN 201911411367 A CN201911411367 A CN 201911411367A CN 111018519 B CN111018519 B CN 111018519B
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任鹏荣
何娇娇
王欣
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Xian University of Technology
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Abstract

本发明公开了一种铌酸钠掺杂钛酸铋钠‑铝酸铋陶瓷的制备方法，通过将Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5按照化学计量比称量混合、球磨干燥、然后将不同组分的混合粉末通过等静压技术挤压成片，最后在不同温度烧结即得。本发明解决了现有技术中陶瓷电容器在‑55℃～300℃的温度范围内介电损耗低的同时，介电常数温度稳定性差的问题。

Description

一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法
技术领域
本发明属于陶瓷材料制备技术领域，涉及一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法。
背景技术
钛酸铋钠(Bi0.5Na0.5TiO3)系列陶瓷自发现以来，大家普遍关注压电性能，对介电性能的关注较少，通过掺杂改性，提高在100℃～300℃高温段介电性能温度稳定性，但这与现有商用多层陶瓷电容器(MLCC)在-55℃～300℃使用温度范围不兼容。“High-temperature dielectrics based on(1-y)[(1-x)Bi0.5Na0.5TiO3-xBiAlO3]-yCaZrO3ternary system with stable permittivity and low dielectric loss in awide temperature range[J].Journal of the European Ceramic Society 39(2019)4160–4167”中公开了一种高温介电陶瓷的制备方法，BiAlO3的掺杂抑制了氧化物离子的导电，显著降低了高温下介电损耗，CaZrO3的掺杂提高了介电性能温度稳定性，在160℃～425℃的温度范围内介电损耗小于0.02，介电常数的温度稳定性(Δε'/ε'200℃)不超过±15％，但是与现有的商用陶瓷电容器-55℃～300℃的温度范围相比，低温温度限过高，具有明显的差异。因此，如何在提高钛酸铋钠基陶瓷介电常数，降低介电损耗的同时，提高温度稳定性，保证其与商用陶瓷电容器的温度兼容性，是一个重要的研究方向。
发明内容
本发明的目的是提供一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，解决了现有商用陶瓷电容器的温度范围内介电损耗高，温度稳定性差的问题。
本发明所采用的技术方案是，一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，其特征在于，具体步骤如下：
步骤1，按照化学计量比(1-x)(0.90Bi0.5Na0.5TiO3-0.10BiAlO3)-xNaNbO3(0.15≤x≤0.30)称量Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5，将0.90Bi0.5Na0.5TiO3-0.10BiAlO3记作BNT-BA，BNT-BA与NaNbO3的摩尔比为85:15～70:30；
步骤2，在球磨机中用酒精为介质，球磨干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体；
步骤3，将步骤2得到的粉体在冷等静压机中，压力成型成圆片；
步骤4，将步骤3成型后的圆片烧结成瓷；
步骤5，将步骤4烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，即得。
本发明的特点还在于，
步骤2中采用行星球磨机，以250～400r/min的转速球磨12～24h。
在步骤3中冷等静压机用200MPa的压力压5min，成为直径10mm，厚度1mm的圆片。
在步骤4中烧结1200℃～1300℃下保温1～5h。
步骤1中的Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5纯度均不小于98.5％。
本发明的有益效果是，本发明一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，通过掺杂铌酸钠(NaNbO3，简称NN)拓宽钛酸铋钠介电陶瓷的温度范围，特别是低温使用温度范围的方法，从而满足其在-55℃～300℃的温度范围内介电损耗低(tanδ≤0.02)、介电常数温度稳定性好(Δε'/ε'200°≤±15％)的性能要求。本发明方法制备的钛酸铋钠-铝酸铋陶瓷温度稳定性能好、介电损耗低、温度兼容性强，利用固相合成法，通过成分设计引入铌酸钠，使得BNT陶瓷的内部极性状态发生变化，从而提升介电温度稳定性(-100～374℃)。该方法成本低、方法简单、可重复性好，所得材料介电性能优异。
附图说明
图1是本发明实施例1-4中制备的BNT-BA-100xNN陶瓷的X射线衍射图谱；
图2是本发明实施例4中所制陶瓷的介电温谱图。
具体实施方式
本发明一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，将Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5按照化学计量比称量、混合球磨干燥，然后将不同组分的混合粉末通过等静压技术挤压成片，最后在不同温度烧结即可。
本发明一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，具体实施步骤如下：
步骤1，按照化学计量比(1-x)(0.90Bi0.5Na0.5TiO3-0.10BiAlO3)-xNaNbO3(0.15≤x≤0.30)称量Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5，将0.90Bi0.5Na0.5TiO3-0.10BiAlO3记作BNT-BA，BNT-BA与NaNbO3的摩尔比为85:15～70:30；
步骤1中的Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5纯度均不小于98.5％。
步骤2，在球磨机中用酒精为介质，球磨干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体；
步骤2中采用行星球磨机，以250～400r/min的转速球磨12～24h。
步骤3，将步骤2得到的粉体在冷等静压机中，压力成型成圆片；
在步骤3中冷等静压机用200MPa的压力压5min，成为直径10mm，厚度1mm的圆片。
步骤4，将步骤3成型后的圆片烧结成瓷；
在步骤4中烧结1200℃～1300℃下保温1～5h。
步骤5，将步骤4烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，即得。
下面结合附图和具体实施方式对本发明进行详细说明。
实施例1
步骤1，称取纯度为98.5％的Bi2O37.7508g、Na2CO32.0123g、TiO24.4366g、Al2O30.3083g和Nb2O51.4187g，使得BNT-BA与NaNbO3的摩尔比为85:15；
步骤2，在行星球磨机中用80ml酒精为介质，以250r/min的转速球磨12h，干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体；
步骤3，将干燥粉体在冷等静压机中，用200MPa的压力压5min成为直径10mm，厚度1mm的圆片；
步骤4，将成型后的圆片在1250℃下保温2h烧结成瓷；
步骤5，将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，然后被银极测试其介电性能。
图1中(a)是实施例1中陶瓷粉体的X射线衍射图谱，从图中可以看出，样品呈单一的钙钛矿相，无第二相出现。
实施例2
步骤1，称取纯度为98.6％的Bi2O37.3921g、Na2CO32.1444g、TiO24.2312g、Al2O30.2941g和Nb2O51.9167g，使得BNT-BA与NaNbO3的摩尔比为80:20。
步骤2，在行星球磨机中用80ml酒精为介质，以260r/min的转速球磨12h，干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体。
步骤3，将干燥粉体在冷等静压机中，用200MPa的压力压5min成为直径10mm，厚度1mm的圆片。
步骤4，将成型后的圆片在1250℃下保温2h烧结成瓷。
步骤5，将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，然后被银极测试其介电性能。
图1中(b)是实施例2中陶瓷粉体的X射线衍射图谱，从图中可以看出，样品呈单一的钙钛矿相，无第二相出现。
实施例3
步骤1，称取纯度为98.7％的Bi2O37.0227g、Na2CO32.2798g、TiO24.0198g、Al2O30.2794g和Nb2O52.4279g，使得BNT-BA与NaNbO3的摩尔比为75:25。
步骤2，在行星球磨机中用80ml酒精为介质，以270r/min的转速球磨12h，干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体。
步骤3，将干燥粉体在冷等静压机中，用200MPa的压力压5min成为直径10mm，厚度1mm的圆片。
步骤4，将成型后的圆片在1250℃下保温2h烧结成瓷。
步骤5，将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，然后被银极测试其介电性能。
图1中(c)是实施例3中陶瓷粉体的X射线衍射图谱，从图中可以看出，样品呈单一的钙钛矿相，无第二相出现。
实施例4
步骤1，称取纯度为98.5％的Bi2O36.6438g、Na2CO32.41902g、TiO23.8029g、Al2O30.2643g和Nb2O52.9532g，使得BNT-BA与NaNbO3的摩尔比为70:30。
步骤2，在行星球磨机中用80ml酒精为介质，以450r/min的转速球磨12h，干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体。
步骤3，将干燥粉体在冷等静压机中，用200MPa的压力压5min成为直径10mm，厚度1mm的圆片。
步骤4，将成型后的圆片在1250℃下保温2h烧结成瓷。
步骤5，将烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，然后被银极测试其介电性能。
图1中(d)是实施例4中陶瓷粉体的X射线衍射图谱，从图中可以看出，样品呈单一的钙钛矿相，无第二相出现。图2是本实施例4中陶瓷在频率为1kHz下的介电温谱曲线图，从图中可以看出，温度稳定性(-100～374℃)最好。
本发明制备出的BNT-BA与NaNbO3的摩尔比为70:30的陶瓷，即实施例4的温度稳定性(-100～374℃)最佳且损耗(tanε≤0.02)最低。
本发明一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，通过将Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5按照化学计量比称量混合、球磨干燥，然后将不同组分的混合粉末通过等静压技术挤压成片，最后在不同温度烧结即得。获得了介电性能温度稳定性好，介电损耗低，温度兼容性好的钛酸铋钠基陶瓷，在宽温电容器领域的实际应用方面提供了一个很好的参考。

Claims (5)

1.一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，其特征在于，具体步骤如下：
步骤1，按照化学计量比(1-x)(0.90Bi0.5Na0.5TiO3-0.10BiAlO3)-xNaNbO3(0.15≤x≤0.30)称量Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5，将0.90Bi0.5Na0.5TiO3-0.10BiAlO3记作BNT-BA，BNT-BA与NaNbO3的摩尔比为85:15～70:30；
步骤2，在球磨机中用酒精为介质，球磨干燥得到掺杂NaNbO3的0.90Bi0.5Na0.5TiO3-0.10BiAlO3粉体；
步骤3，将步骤2得到的粉体在冷等静压机中，压力成型成圆片；
步骤4，将步骤3成型后的圆片烧结成瓷；
步骤5，将步骤4烧结后的陶瓷片打磨、抛光后用无水乙醇洗涤，即得。
2.根据权利要求1所述的一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，其特征在于，所述步骤2中采用行星球磨机，以250～400r/min的转速球磨12～24h。
3.根据权利要求1所述的一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，其特征在于，所述在步骤3中冷等静压机用200MPa的压力压5min，成为直径10mm，厚度1mm的圆片。
4.根据权利要求1所述的一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，其特征在于，所述在步骤4中烧结1200℃～1300℃下保温1～5h。
5.根据权利要求1所述的一种铌酸钠掺杂钛酸铋钠-铝酸铋陶瓷的制备方法，其特征在于，所述步骤1中的Bi2O3、Na2CO3、TiO2、Al2O3和Nb2O5纯度均不小于98.5％。
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