CN113620707A - 一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷及其制备工艺 - Google Patents
一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷及其制备工艺 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 36
- BITYAPCSNKJESK-UHFFFAOYSA-N potassiosodium Chemical compound [Na].[K] BITYAPCSNKJESK-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 18
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims description 32
- 235000015895 biscuits Nutrition 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 13
- 239000002994 raw material Substances 0.000 claims description 13
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 10
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 5
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 5
- 229910000449 hafnium oxide Inorganic materials 0.000 claims description 5
- WIHZLLGSGQNAGK-UHFFFAOYSA-N hafnium(4+);oxygen(2-) Chemical compound [O-2].[O-2].[Hf+4] WIHZLLGSGQNAGK-UHFFFAOYSA-N 0.000 claims description 5
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims description 5
- 229910052808 lithium carbonate Inorganic materials 0.000 claims description 5
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 5
- 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 description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 4
- 229910052779 Neodymium Inorganic materials 0.000 claims description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 4
- 229910052772 Samarium Inorganic materials 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 229910052771 Terbium Inorganic materials 0.000 claims description 4
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 229910052746 lanthanum Inorganic materials 0.000 claims description 4
- 238000003754 machining Methods 0.000 claims description 4
- 238000003801 milling Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 230000010287 polarization Effects 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000003786 synthesis reaction Methods 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052797 bismuth Inorganic materials 0.000 abstract description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052735 hafnium Inorganic materials 0.000 abstract description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 239000000543 intermediate Substances 0.000 description 11
- 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 description 4
- 238000000034 method Methods 0.000 description 4
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000036541 health Effects 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
本发明提供一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷及其制备工艺，采用锂、铋、铪等元素掺杂进行相界调控，使材料在室温附近形成多个压电相共存状态，活化压电畴，强化材料压电性能，同时结合稀土元素掺杂，降低材料损耗，使之满足于功率型压电元件的性能要求。
Description
技术领域
本发明属于无铅压电技术及电子陶瓷领域，具体涉及一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷及其制备工艺。
背景技术
功率超声设备已应用于国民经济的各个领域，如超声清洗、超声焊接、超声成型、超声加工、超声手术刀等，近年来在乳化分散、粉碎、除垢、悬浮、萃取等场合也得到了广泛应用。功率超声应用要求材料损耗低，机械品质因数高，矫顽场高，同时仍需较高的机电耦合系数和压电系数，目前使用的功率超声材料绝大多数是锆钛酸铅陶瓷（如PZT-4型和PZT-8型）。
锆钛酸铅陶瓷中铅元素比重超过60％，在其生产、使用以及废弃处理过程中都会给人类健康和生态环境造成严重的铅毒害和铅污染，无铅压电材料及元器件的应用是解决上述问题的唯一途径。然而，对于现阶段的无铅压电材料，同时实现低损耗和高压电常数非常困难，例如对于研究最广的铌酸钾钠无铅压电陶瓷，当其压电系数达到300pC/N时，损耗通常将超过2%甚至3%；又如钛酸铋钠无铅压电陶瓷，其损耗一般较小在1%以下，但压电系数往往不超过200pC/N。因而，对于无铅压电陶瓷来说，如何同时实现高压电系数和低损耗是一个难点。
发明内容
针对上述问题，本发明提供一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷，采用锂、铋、铪等元素掺杂进行相界调控，使材料在室温附近形成多个压电相共存状态，活化压电畴，强化材料压电性能，同时结合稀土元素掺杂，降低材料损耗，使之满足于功率型压电元件的性能要求。
本发明通过以下技术方案来实现：一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷，化学组成为：(1-x-y)(K0.47Na0.47Li0.06)NbO3 + x Bi0.5Li0.5HfO3+yBiREzO3；所述x, y为摩尔百分比，其中0<x≤0.1，0<y≤0.05，RE为稀土元素，至少为La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Er、Yb其中的一种，z表示BiREzO3组元中RE元素的化学计量数，z的数值按电价平衡原则取值。
进一步地，其原料包括：碳酸钾、碳酸钠、碳酸锂、氧化铋、氧化铪、五氧化二铌和辅料，所述辅料为La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Er、Yb的金属氧化物。
本发明采用两步合成法制备铌酸钾钠基无铅压电陶瓷，首先预合成(K0.47Na0.47Li0.06)NbO3、Bi0.5Li0.5HfO3、BiREzO3三种组元作为中间体，再按照上述化学式给定的计量比，将各中间体混合均匀并进行煅烧处理，得到化学组成为(1-x-y)(K0.47Na0.47Li0.06)NbO3 + x Bi0.5Li0.5HfO3+ yBiREzO3的铌酸钾钠基无铅压电陶瓷。
一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷的制备工艺，包括以下步骤：
（1）原料预处理：将碳酸钾、碳酸钠、碳酸锂、氧化铋、氧化铪、五氧化二铌和稀土金属氧化物放入干燥皿，置于烘箱内，在150℃下保温4h烘干；
（2）预合成：按(K0.47Na0.47Li0.06)NbO3、Bi0.5Li0.5HfO3、BiREzO3三种组元的化学式，称取对应原料进行混合，混料均匀后，在750-850℃下进行煅烧，保证各原料成分反应，得到三种组元的中间体粉末；
（3）混料：将三种组元的中间体粉末按所述化学式的计量比进行称取，再通过球磨或搅拌磨的方式使其混合均匀，得到预混粉；
（4）一次煅烧：将预混粉压制成φ80×20mm尺寸的素坯，置于刚玉板上在箱式炉中连续升温至850-900℃，保温4-6h，冷却后得到一次煅烧坯体；
（5）二次煅烧：将一次煅烧坯体进行破碎，过40目筛，然后置于刚玉坩埚中，在箱式炉中连续升温至950-1000℃，保温2-4h，随炉冷却后破碎过筛，得到预烧粉；
（6）细磨：将预烧粉用球磨或砂磨方式进行细化，得到粒径D50为1-2μm的陶瓷粉。
按步骤（1）至（6）制备铌酸钾钠基无铅压电陶瓷粉体后，再经由造粒、干压成型、排胶、烧结、机加工、烧银、极化等步骤，得到上述材料制成的压电陶瓷元件。
本发明采用所述工艺，制备得到致密度高、电性能好的铌酸钾钠基无铅压电陶瓷，压电常数d33不低于300pC/N以上，材料损耗不高于1%，能够满足功率型压电元件的性能要求。
本发明提供的铌酸钾钠基压电陶瓷，元素组成上不含任何有毒有害元素，绿色环保，健康安全，可取代传统的含铅压电材料制作功率型压电元件，有效避免压电陶瓷材料在生产、使用和废弃过程中带来的铅污染，减少对人类健康和环境造成的损害。
附图说明
图1为一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷的制备工艺流程图。
具体实施方式
以下对本发明的具体实施例进行进一步详细说明。应当理解的是，在此提供的附图都是为了说明的目的，并且附图不一定是按比例绘制的。
除非上下文明确要求，否则整个说明书和权利要求书中的“包括”、“包含”等类似词语应当解释为包含的含义，而不是排他或穷举的含义；也就是说，是“包括但不限于”的含义。
实施例1：
一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷，化学组成为：(1-x-y) (K0.47Na0.47Li0.06)NbO3 + x Bi0.5Li0.5HfO3+ yBiREzO3；所述x, y为摩尔百分比，其中0<x≤0.1，0<y≤0.05，RE为稀土元素，至少为La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Er、Yb其中的一种，z表示BiREzO3组元中RE元素的化学计量数，z的数值按电价平衡原则取值，具体为BiLaO3、BiCe0.75O3、BiPrO3、BiNdO3、BiPmO3、BiSmO3、BiEuO3、BiGdO3、BiTbO3、BiErO3、BiYbO3。
实施例2：
一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷的制备工艺，工艺步骤如附图1，包括：
（1）原料预处理：将碳酸钾、碳酸钠、碳酸锂、氧化铋、氧化铪、五氧化二铌和稀土金属氧化物放入干燥皿，置于烘箱内，在150℃下保温4h烘干；
（2）预合成：按(K0.47Na0.47Li0.06)NbO3、Bi0.5Li0.5HfO3、BiREzO3三种组元的化学式，称取对应原料进行混合，混料均匀后，在750-850℃下进行煅烧，保证各原料成分反应，得到三种组元的中间体粉末；
（3）混料：将三种组元的中间体粉末按所述化学式的计量比进行称取，再通过球磨或搅拌磨的方式使其混合均匀，得到预混粉；
（4）一次煅烧：将预混粉压制成φ80×20mm尺寸的素坯，置于刚玉板上在箱式炉中连续升温至850-900℃，保温4-6h，冷却后得到一次煅烧坯体；
（5）二次煅烧：将一次煅烧坯体进行破碎，过40目筛，然后置于刚玉坩埚中，在箱式炉中连续升温至950-1000℃，保温2-4h，随炉冷却后破碎过筛，得到预烧粉；
（6）细磨：将预烧粉用球磨或砂磨方式进行细化，得到粒径D50为1-2μm的陶瓷粉。
按步骤（1）至（6）制备铌酸钾钠基无铅压电陶瓷粉体后，再经由造粒、干压成型、排胶、烧结、机加工、烧银、极化等步骤，得到上述材料制成的压电陶瓷元件。
实施例3：
一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷，化学组成为：(0.94) (K0.47Na0.47Li0.06)NbO3 + 0.03 Bi0.5Li0.5HfO3+ 0.03BiCe0.75O3；其制备工艺如附图1，包括：
（1）原料预处理：将碳酸钾、碳酸钠、碳酸锂、氧化铋、氧化铪、五氧化二铌和氧化铈放入干燥皿，置于烘箱内，在150℃下保温4h烘干；
（2）预合成：按(K0.47Na0.47Li0.06)NbO3、Bi0.5Li0.5HfO3、BiCe0.75O3三种组元的化学式，称取对应原料进行混合，混料均匀后，在750-850℃下进行煅烧，保证各原料成分反应，得到三种组元的中间体粉末；
（3）混料：将三种组元的中间体粉末按所述化学式的计量比进行称取，再通过球磨或搅拌磨的方式使其混合均匀，得到预混粉；
（4）一次煅烧：将预混粉压制成φ80×20mm尺寸的素坯，置于刚玉板上在箱式炉中连续升温至850-900℃，保温4-6h，冷却后得到一次煅烧坯体；
（5）二次煅烧：将一次煅烧坯体进行破碎，过40目筛，然后置于刚玉坩埚中，在箱式炉中连续升温至950-1000℃，保温2-4h，随炉冷却后破碎过筛，得到预烧粉；
（6）细磨：将预烧粉用球磨或砂磨方式进行细化，得到粒径D50为1-2μm的陶瓷粉。
按步骤（1）至（6）制备铌酸钾钠基无铅压电陶瓷粉体后，再经由造粒、干压成型、排胶、烧结、机加工、烧银、极化等步骤，得到上述材料制成的压电陶瓷元件。制得压电元件的压电常数不低于300pC/N，损耗不高于1%。
以上仅为本发明的较佳实施例，并不用于局限本发明的保护范围，任何在本发明精神内的修改、等同替换或改进等，都涵盖在本发明的权利要求范围内。
Claims (2)
1.一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷，化学组成为：(1-x-y) (K0.47Na0.47Li0.06)NbO3 + x Bi0.5Li0.5HfO3 + yBiREzO3；所述x, y为摩尔百分比，其中0<x≤0.1，0<y≤0.05，RE为稀土元素，至少为La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Er、Yb其中的一种，z表示BiREzO3组元中RE元素的化学计量数，z的数值按电价平衡原则取值。
2.一种用于功率型压电元件的稀土掺杂铌酸钾钠基无铅压电陶瓷的制备工艺，包括以下步骤：
（1）原料预处理：将碳酸钾、碳酸钠、碳酸锂、氧化铋、氧化铪、五氧化二铌和稀土金属氧化物放入干燥皿，置于烘箱内，在150℃下保温4h烘干；
（2）预合成：按(K0.47Na0.47Li0.06)NbO3、Bi0.5Li0.5HfO3、BiREzO3三种组元的化学式，称取对应原料进行混合，混料均匀后，在750-850℃下进行煅烧，保证各原料成分反应，得到三种组元的中间体粉末；
（3）混料：将三种组元的中间体粉末按所述化学式的计量比进行称取，再通过球磨或搅拌磨的方式使其混合均匀，得到预混粉；
（4）一次煅烧：将预混粉压制成φ80×20mm尺寸的素坯，置于刚玉板上在箱式炉中连续升温至850-900℃，保温4-6h，冷却后得到一次煅烧坯体；
（5）二次煅烧：将一次煅烧坯体进行破碎，过40目筛，然后置于刚玉坩埚中，在箱式炉中连续升温至950-1000℃，保温2-4h，随炉冷却后破碎过筛，得到预烧粉；
（6）细磨：将预烧粉用球磨或砂磨方式进行细化，得到粒径D50为1-2μm的陶瓷粉；
按步骤（1）至（6）制备铌酸钾钠基无铅压电陶瓷粉体后，再经由造粒、干压成型、排胶、烧结、机加工、烧银、极化等步骤，得到上述材料制成的压电陶瓷元件。
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