CN111362695A - 一种锆钛酸铅压电陶瓷及其制备方法 - Google Patents
一种锆钛酸铅压电陶瓷及其制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 65
- 229910052451 lead zirconate titanate Inorganic materials 0.000 title claims abstract description 59
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 50
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 claims abstract description 22
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 20
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 17
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 12
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims abstract description 12
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims abstract description 10
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 238000000498 ball milling Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- 238000009275 open burning Methods 0.000 claims description 3
- 230000010287 polarization Effects 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000013078 crystal Substances 0.000 abstract description 12
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 8
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 23
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 230000008878 coupling Effects 0.000 description 6
- 238000010168 coupling process Methods 0.000 description 6
- 238000005859 coupling reaction Methods 0.000 description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 6
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 3
- 229910052808 lithium carbonate Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000010955 niobium Substances 0.000 description 2
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005324 grain boundary diffusion Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009768 microwave sintering Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000034655 secondary growth Effects 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
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Abstract
本发明公开了一种锆钛酸铅压电陶瓷，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅55~75份、硫酸钡0~6份、碳酸锶0.2~8份、五氧化二铌0.1~0.9份、五氧化二锑0.2~1份、二氧化锆15~25份、二氧化钛8~15份。本发明所述的锆钛酸铅压电陶瓷采用二步烧结固相合成的制备方法，制备出优良的锆钛酸铅压电陶瓷材料，既有效缩短了高温烧结时间，又在一定程度上节省了能源和时间和生产成本；本发明所述的二步烧结法通过控制温度的变化，既能够抑制晶界迁移，又能保持晶界扩散处于活跃状态，以实现在晶粒不长大的前提下完成烧结的目的。
Description
技术领域
本发明涉及压电材料技术领域，具体涉及一种锆钛酸铅压电陶瓷及其制备方法。
背景技术
压电陶瓷材料是一种可实现机械能与电能相互转换的功能陶瓷材料，因其稳定的力学性能和优异的电学性能、制备工艺简单、成本低等优点，被广泛引用于激光和医疗、军事信息和航空等方面。继第二次世界大战发现BaTiO3压电陶瓷之后，50年代初锆钛酸铅(PZT)系被发现，发展至今，压电陶瓷材料领域应用的最多、性能最好的就是PZT压电陶瓷。
锆钛酸铅压电陶瓷虽然电性能较优，但其低居里温度点，较高的烧结温度以及高温下有毒元素铅的挥发等缺点一直困扰着众多学者。现有的技术中，主要是通过掺杂改性和工艺改性两种方式来改善PZT陶瓷的性能，前者是在PZT陶瓷的础上对其同时进行A位Ba、Sr等掺杂和B位Nb、Sb等掺杂，利用传统固相烧结法制备，有效地降低了烧结温度，提高了居里温度和各电性能；后者是通过改进PZT陶瓷的制备工艺来提高其各方面性能。
目前，在烧结方面的改进主要集中在放电等离子烧结、热等静压烧结，微波烧结、超高压烧结和真空烧结等。但这些烧结方法的局限性和高成本极大限制了其广泛应用。所以合理地选择烧结工艺，是使PZT压电陶瓷具有理想的结构与预定的性能之关键。烧结温度、保温时间、升温速率及退火工艺都直接影响着陶瓷的结构和致密化，特别是烧结后期易出现的晶粒二次长大往往造成陶瓷性能恶化。
有研究人员提出二步烧结法，即将陶瓷坯体升温到较高温度以获得一定密度，然后快速冷却到一个较低温度，并长时间保温，在此温度下，晶界扩散可继续进行，但晶界迁移却受到抑制。二步烧结法通过控制温度的变化，在抑制晶界迁移的同时，保持晶界扩散处于活跃状态，以实现在晶粒不长大的前提下完成烧结的目的。
中国发明专利申请号201210406289.8公开了“一种铌酸钾钠无铅压电陶瓷及其两步烧结制备方法”，它是以铌酸钾钠压电陶瓷为体，采用两步烧结法制备出性能良好的新型压电陶瓷材料。
中国期刊《中国陶瓷》2018年第54卷第3期，在“两步烧结法制备Mn掺杂Bi4Ti2.85Nb0.15O12陶瓷的微观结构与电性能研究”文章中公开了采用两步烧结法制备铋层状结构压电陶瓷，获得具有均匀细小晶粒结构的致密陶瓷体。
而针对锆钛酸铅压电陶瓷的二步烧结法制备目前不曾报导，因此，本发明是一种采用二步烧结制备锆钛酸铅压电陶瓷的方法，对研究和开发出性能优异的铅压电陶瓷具有一定的实用意义。
发明内容
本发明提供一种锆钛酸铅压电陶瓷及其制备方法，本发明采用二步烧结制备锆钛酸铅压电陶瓷，通过调控第一步烧结温度、第二步烧结温度、升温效率，来获得电性能优异的锆钛酸铅压电陶瓷材料。
本发明解决其技术问题采用以下技术方案：
一种锆钛酸铅压电陶瓷，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅55~75份、硫酸钡0~6份、碳酸锶0.2~8份、五氧化二铌0.1~0.9份、五氧化二锑0.2~1份、二氧化锆15~25份、二氧化钛8~15份。
作为一种优选方案，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅60~68份、硫酸钡0~5份、碳酸锶0.2~6份、五氧化二铌0.1~0.7份、五氧化二锑0.2~0.7份、二氧化锆18~23份、二氧化钛9~13份。
作为一种最优选方案，四氧化三铅63.15份、硫酸钡3份、碳酸锶2份、五氧化二铌0.4份、五氧化二锑0.45份、二氧化锆20份、二氧化钛11份。
本发明还提供了一种锆钛酸铅压电陶瓷的制备方法，包括如下步骤：
（1）称取原料，球磨、烘干、过50~70目筛得粉料；
（2）将上述粉料在900~1100℃预烧成型得料块；
（3）将料块碾碎，再次球磨、烘干、过40~60目筛，加粘结剂并轧膜成型，冲片得到生坯片；
（4）将生坯片在500~700℃下排胶、敞烧，得坯体；
（5）升温1300~1400℃第一次烧结坯体，保温时间为0.5~2min。
（6）降温至1100~1250℃，保温8~12h，再次烧结，自然冷却至室温；
（7）再进行被银、极化处理，即得所述的锆钛酸铅压电陶瓷。
作为一种优选方案，所述步骤（1）、（3）中球磨介质为水，磨球为氧化锆球磨子，工艺为：磨球：水为3~4:0.5~1.5，球磨转速为300~400r/min，球磨时间为5~7h。
作为一种优选方案，所述步骤（3）中粘结剂为聚乙烯醇水溶液。
作为一种优选方案，所述步骤（5）中升温速率为5~20℃/min。
作为一种优选方案，所述步骤（6）中降温速率为5~20℃/min。
本发明的有益效果：（1）本发明所述的锆钛酸铅压电陶瓷采用二步烧结固相合成的制备方法，制备出优良的锆钛酸铅压电陶瓷材料，既有效缩短了高温烧结时间，又节省了能源，时间和生产成本；（2）本发明所述的二步烧结法通过控制温度的变化，既能够抑制晶界迁移，又能保持晶界扩散处于活跃状态，以实现在晶粒不长大的前提下完成烧结的目的；（3）本发明通过调控第一步烧结温度、第二步烧结温度、保温时间、升温速率，来获得电性能优异的PZT压电陶瓷，提高了陶瓷致密度，综合性能可达到：相对介电常数3210~3700，介电损耗≤2.0%，平面机电耦合系数70~75%，机械品质因素63~77。同时，操作简单，原料易获得，可实现批量生产，具有一定工业实用性。
附图说明
图1为实施例1所制的样品金相图；
图2为对比例1所制的样品金相图。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明一部分实施例，而不是全部的实施例。于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种锆钛酸铅压电陶瓷，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅63.15份、硫酸钡3份、碳酸锶2份、五氧化二铌0.4份、五氧化二锑0.45份、二氧化锆20份、二氧化钛11份。
所述的锆钛酸铅压电陶瓷的制备方法，包括如下步骤：
（1）称取原料，球磨、烘干、过60目筛得粉料；
（2）将上述粉料在1030℃预烧成型得料块；
（3）将料块碾碎，再次球磨、烘干、过50目筛，加粘结剂并轧膜成型，冲片得到生坯片；
（4）将生坯片在600℃下排胶、敞烧，得坯体；
（5）升温1300℃第一次烧结坯体，保温时间为1min。
（6）降温至1100~1250℃，保温8~12h，再次烧结，自然冷却至室温；
（7）再进行被银、极化处理，即得所述的锆钛酸铅压电陶瓷。
所述步骤（1）、（3）中球磨介质为水，磨球为氧化锆球磨子，工艺为：磨球：水为3.6:0.8，球磨转速为350r/min，球磨时间为6h。
所述步骤（3）中粘结剂为聚乙烯醇水溶液。
所述步骤（5）中升温速率为15℃/min。
所述步骤（6）中降温速率为15℃/min。
实施例2
实施例2与实施例1不同之处在于，实施例2与实施例1的锆钛酸铅压电陶瓷原料配比不同，其它都相同。
所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅55份、硫酸钡6份、碳酸锶0.2份、五氧化二铌0.9份、五氧化二锑0.2份、二氧化锆25份、二氧化钛8份。
实施例3
实施例3与实施例1不同之处在于，实施例3与实施例1的锆钛酸铅压电陶瓷原料配比不同，其它都相同。
所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅75份、硫酸钡1份、碳酸锶8份、五氧化二铌0.1份、五氧化二锑1份、二氧化锆15份、二氧化钛15份。
实施例4
实施例4与实施例1不同之处在于，实施例4第一次烧结温度为1400℃，第二次烧结温度为1100℃，其它都相同。
实施例5
实施例5与实施例1不同之处在于，实施例5第一次烧结温度为1350℃，第二次烧结温度为1250℃，其它都相同。
实施例6
实施例6与实施例1不同之处在于，实施例6的升温和降温速率为5℃/min，其它都相同。
实施例7
实施例7与实施例1不同之处在于，实施例7的升温和降温速率为20℃/min，其它都相同。
对比例1
对比例1与实施例1不同之处在于，对比例1两次烧结温度都为1250℃，其它都相同。
对比例2
对比例2与实施例不同之处在于，对比例2第一次烧结温度为1130，第二次烧结温度为950℃，其它都相同。
对比例3
对比例3与实施例1不同之处在于，对比例3第一次烧结温度为1150℃，第二次烧结温度为1000℃，其它都相同。
对比例4
对比例4与实施例1不同之处在于，对比例4与实施例1的锆钛酸铅压电陶瓷原料配比不同，其它都相同。
所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅63.15份、碳酸钠 3份、碳酸钾 2份、碳酸锂2份、五氧化二铌0.4份、五氧化二锑0.45份、二氧化锆20份、二氧化钛11份。
对比例5
对比例5与实施例1不同之处在于，对比例5与实施例1的锆钛酸铅压电陶瓷原料配比不同，其它都相同。
所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅63.15份、碳酸钠 3份、碳酸钾 2份、碳酸锂2份、三氧化二锑1份、五氧化二铌0.4份、五氧化二钽 0.45份、二氧化锆20份、二氧化钛11份。
为了进一步证明本发明的效果，提供了以下测试方法：
1.实施例1（图1）和对比例1（图2）在显微镜下的金相图。
从图1和图2可看出，实施例1制得的锆钛酸铅压电陶瓷没有出现晶粒，而对比例1制得的锆钛酸铅压电陶瓷出现了晶粒，晶粒会导致锆钛酸铅压电陶瓷的性能恶化，实施例1制得的锆钛酸铅压电陶瓷具有更好的致密度。
2.检测实施例1~7、对比例1~3的锆钛酸铅压电陶瓷的性能（表1 ）。
表1 性能参数
通过表1可看出，本发明所述的锆钛酸铅压电陶瓷综合性能：相对介电常数3210~3700，介电损耗≤2.0%，平面机电耦合系数70~75%，机械品质因素63~77。其中实施例1为最佳实施方式；通过对比实施例1~3可看出，锆钛酸铅压电陶瓷的原料配比影响着锆钛酸铅压电陶瓷的性能，实施例1为最佳配比，有着最佳的相对介电常数、介电损耗、耦合常数、品质因数；通过对比实施例1与实施例4、实施例5、对比例1、对比例2、对比例3可知，两次烧结温度对于本发明来说至关重要，影响着本发明的锆钛酸铅压电陶瓷的相对介电常数、介电损耗、耦合常数、品质因数；通过对比实施例1与实施例6、实施例7可知，两次烧结的升温和降温速率也会影响着本发明的锆钛酸铅压电陶瓷的相对介电常数、介电损耗、耦合常数、品质因数，通过对比实施例1与对比例4、5可知，本发明所述的锆钛酸铅压电陶瓷中的成分当采用其它如：碳酸钠、碳酸钾、碳酸锂、五氧化二钽、三氧化二锑替代时，锆钛酸铅压电陶瓷的相对介电常数、介电损耗、耦合常数、品质因数都会相应变差。
以上述依据本发明的理想实施例为启示，通过上述的说明内容，相关工作人员完全可以在不偏离本发明技术思想的范围内，进行多样的变更以及修改。本发明的技术性范围并不局限于说明书上的内容，必须要根据权利要求范围来确定其技术性范围。
Claims (8)
1.一种锆钛酸铅压电陶瓷，其特征在于，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅55~75份、硫酸钡0~6份、碳酸锶0.2~8份、五氧化二铌0.1~0.9份、五氧化二锑0.2~1份、二氧化锆15~25份、二氧化钛8~15份。
2.根据权利要求1所述的锆钛酸铅压电陶瓷，其特征在于，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅60~68份、硫酸钡0~5份、碳酸锶0.2~6份、五氧化二铌0.1~0.7份、五氧化二锑0.2~0.7份、二氧化锆18~23份、二氧化钛9~13份。
3.根据权利要求1所述的锆钛酸铅压电陶瓷，其特征在于，所述锆钛酸铅压电陶瓷由以下重量份原料组成：四氧化三铅63.15份、硫酸钡3份、碳酸锶2份、五氧化二铌0.4份、五氧化二锑0.45份、二氧化锆20份、二氧化钛11份。
4.权利要求1~3任一所述的锆钛酸铅压电陶瓷的制备方法，其特征在于，包括如下步骤：
（1）称取原料，球磨、烘干、过50~70目筛得粉料；
（2）将上述粉料在900~1100℃预烧成型得料块；
（3）将料块碾碎，再次球磨、烘干、过40~60目筛，加粘结剂并轧膜成型，冲片得到生坯片；
（4）将生坯片在500~700℃下排胶、敞烧，得坯体；
（5）升温1300~1400℃第一次烧结坯体，保温时间为0.5~2min；
（6）降温至1100~1250℃，保温8~12h，再次烧结，自然冷却至室温；
（7）再进行被银、极化处理，即得所述的锆钛酸铅压电陶瓷。
5.根据权利要求4所述的锆钛酸铅压电陶瓷的制备方法，其特征在于，所述步骤（1）、（3）中球磨介质为水，磨球为氧化锆球磨子，工艺为：磨球：水为3~4:0.5~1.5，球磨转速为300~400r/min，球磨时间为5~7h。
6.根据权利要求4所述的锆钛酸铅压电陶瓷的制备方法，其特征在于，所述步骤（3）中粘结剂为聚乙烯醇。
7.根据权利要求4所述的锆钛酸铅压电陶瓷的制备方法，其特征在于，所述步骤（5）中升温速率为5~20℃/min。
8.根据权利要求4所述的锆钛酸铅压电陶瓷的制备方法，其特征在于，所述步骤（6）中降温速率为5~20℃/min。
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| CN114591082A (zh) * | 2022-04-19 | 2022-06-07 | 东莞理工学院 | 一种pzt-pnn-psn-pmn压电陶瓷及其制备方法 |
| CN115477538A (zh) * | 2022-10-05 | 2022-12-16 | 西南大学 | 一种两步烧结制备铌酸钾钠基压电陶瓷的方法 |
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