CN116675533A - 一种压电陶瓷材料及其制备方法 - Google Patents
一种压电陶瓷材料及其制备方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 238000000498 ball milling Methods 0.000 claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000010287 polarization Effects 0.000 claims abstract description 12
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000003825 pressing Methods 0.000 claims abstract description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 7
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 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 7
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000007599 discharging Methods 0.000 claims abstract description 5
- 239000003292 glue Substances 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 3
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 46
- 238000000227 grinding Methods 0.000 claims description 16
- 239000011805 ball Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000919 ceramic Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 239000003921 oil Substances 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims 1
- 238000010897 surface acoustic wave method Methods 0.000 abstract description 15
- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 5
- 230000000630 rising effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910020684 PbZr Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 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 1
- 238000003754 machining Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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Abstract
一种压电陶瓷材料及其制备方法，涉及陶瓷材料领域。所述压电陶瓷材料包括氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛，所述压电陶瓷材料的化学式为：(PbO).(MnO2)0.08/3.(Nb2O5)0.04/3.(Sb2O3)0.04/3.(ZrO2)0.828.(TiO2)0.092。所述压电陶瓷材料的制备方法包括：称量→第一次球磨→烘干→预烧→第二次球磨→造粒→烘干→干压成型→排胶与烧结→被银→极化。解决了现有压电陶瓷材料相对介电常数低、介电损耗高的问题。广泛应用于声表面波器件制备领域。
Description
技术领域
本发明涉及陶瓷材料领域，进一步来说，涉及压电陶瓷材料领域，具体来说，涉及一种压电陶瓷材料及其制备方法。
背景技术
压电陶瓷材料广泛应用于声光电以及日常生活和生产的诸多领域，目前压电陶瓷材料应用最广泛的是钙钛矿型的锆钛酸铅(PbZrxTi1-xO3,简写为PZT)或以PZT为基掺入其它组份构成的多元压电陶瓷。从产业结构来看，全世界的声表面波器件市场主要分布在通信、汽车、多媒体、工业、军工等领域，其中通信、汽车、多媒体用声表面波滤波器分别占整个声表面波器件产业的70％、20％、10％的份额。所以制备出一款具有相对介电常数适宜、低介电损耗的特性的压电陶瓷材料是具有很大现实意义与价值的。近年来因为叉指换能器的应用，声表面波器件得到迅速发展，使用压电陶瓷材料制备声表面波器件得到极大研究进展，关键在于找到适宜的压电陶瓷材料的制备方法使材料适用于制备声表面波器件。
传统技术的压电陶瓷材料制备方法是直接通过球磨、压制、烧结、最后加工生成。这样制造的PZT陶瓷材料的缺点是损耗较大(大概4％以上)，表面波衰减较快等。而制备声表面波的压电陶瓷材料主要要求是：①要求材料的介电常数在10<ε<1000；②要求低损耗。因此，传统技术制备的压电陶瓷材料已不能满足声表面波器件迅速发展的要求。
有鉴于此，特提出本发明。
发明内容
本发明要解决的技术问题是现有压电陶瓷材料相对介电常数低、介电损耗高的问题。
本发明的发明构思是：通过探索多元掺杂(包括Mn、Nb、Sb等元素)对PZT基陶瓷组织结构与电性能之间的相互作用规律，实现对声表面波器件用压电陶瓷电性能的精准调控；并通过对球磨、烧结等工艺过程的适当调整，制备适用于声表面波器件的相对介电常数适宜、低介电损耗压电陶瓷材料，以达到声表面波的压电陶瓷材料的主要要求。
为此，本发明提供一种压电陶瓷材料，包括氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛。
所述压电陶瓷材料的化学式为：
(PbO).(MnO2)0.08/3.(Nb2O5)0.04/3.(Sb2O3)0.04/3.(ZrO2)0.828.(TiO2)0.092。
所述一种压电陶瓷材料的制备方法，包括如下方法：
(1)按照化学式计量比分别称取氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛；
(2)按照球、料、水的顺序加入球磨罐中进行混合得到粉体；
(3)通过一次球磨、烘干、预烧、二次球磨制备出所需的压电陶瓷粉体；
(4)将压电陶瓷粉体放入烘箱烘干；
(5)将烘干所得的料先经过40目筛，接着进行人工造粒；
(6)将人工造粒所制得材料放入模具，进行干压成型；
(7)将干压成型后的材料进行排胶烧结、被银、极化、得到压电陶瓷材料。
本发明的有益效果：
压电陶瓷材料的压电常数达到591pC/N-605pC/N，介电损耗在2.5％-2.8％。
相对介电常数适宜、介电损耗低，满足声表面波器件对压电陶瓷材料的主要要求。
广泛应用于声表面波器件制备领域。
附图说明
图1为本发明新型压电陶瓷材料制备流程示意图。
具体实施方式
一种相对介电常数适宜、低介电损耗的新型压电陶瓷材料的制备方法，具体方法如下：
(1)按照化学式计量比分别称取氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛，对其进行一次球磨，以锆球∶料∶去离子水＝2∶1∶1(质量比)比例，按照球、料、水的顺序加入磨罐中进行混合，放入球磨机，转速350rpm，球磨时间8h，进行球磨；
(2)将一次球磨所得的磨料放入80℃的常规烘箱中进行烘干，烘干时间为12h；
(3)将所得烘干磨料放入马弗炉中进行预烧，预烧时，20℃到960℃，升温速率为2.0℃/min，时间470min，升温至960℃之后，保温240分钟，然后自然冷却到室温；
(4)将所得烘干磨料放入马弗炉中进行预烧，预烧时，20℃到100℃，升温时间为90min，升温至100℃之后，继续升温至850℃，升温时间为320min，升温至850℃后保温180分钟，然后自然冷却到室温。升温过程中不用冲入惰性气体；
(5)将预烧所得的预烧料进行二次球磨，以锆球：料：去离子水＝2:1:1比例，按照球、料、水的顺序加入磨罐中，放入球磨机，转速350rpm，球磨时间6h，进行球磨；
(6)将二次球磨所得的磨料放入100摄氏度烘箱中烘6h；
(7)将烘干所得的料先经过40目筛，再加入10％质量比的PVA，进行人工造粒；
(8)将材料放入模具，再将模具装到压机上，然后加压10MPa，加压时间15秒；
(9)将干压成型后的材料进行排胶烧结，室温升至550℃，升温时间450min；550℃下保温3小时，550℃升温至1250℃，升温时间600min；1250℃下保温6小时，自然冷却；
(10)将所得材料进行被银，印银方式为手刷；
(11)将所得材料进行极化，极化方式为硅油极化，极化电压和时间分别为3.5KV/mm，20min，极化温度为110℃。
对上述制备方法所制的压电陶瓷材料进行性能测试，结果如表1所示。
对制备出的新型压电陶瓷材料的性能测试结果：
表1压电陶瓷材料性能参数测试表
| 测试参数 | 测试数据 |
| 相对介电常数 | 600-650 |
| 介电损耗 | 2.5％-2.8％ |
| 压电系数d33 | 591pC/N-605pC/N |
| 体电阻率 | 0.41GΩ·m-0.43GΩ·m |
| 居里温度 | 165℃-170℃ |
从上表的数据可以看出，采用本发明的制备方法制备的压电陶瓷材料具有相对介电常数适宜、低介电损耗的特性，满足声表面波器件对压电陶瓷材料的主要要求。
最后应说明的是：上述实施例仅仅是为清楚地说明所作的举例，本发明包括但不限于以上实施例,这里无需也无法对所有的实施方式予以穷举。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。凡符合本发明要求的实施方案均属于本发明的保护范围。
Claims (6)
1.一种压电陶瓷材料，其特征在于，组份包括：氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛；
所述压电陶瓷材料的化学式为：
(PbO).(MnO2)0.08/3.(Nb2O5)0.04/3.(Sb2O3)0.04/3.(ZrO2)0.828.(TiO2)0.092。
2.如权利要求1所述的一种压电陶瓷材料的制备方法，其特征在于，包括如下方法：
(1)按照化学式计量比分别称取氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛；
(2)按照球、料、水的顺序加入球磨罐中进行混合得到粉体；
(3)通过一次球磨、烘干、预烧、二次球磨制备出所需的压电陶瓷粉体；
(4)将压电陶瓷粉体放入烘箱烘干；
(5)将烘干所得的料先经过40目筛，接着进行人工造粒；
(6)将人工造粒所制得材料放入模具，进行干压成型；
(7)将干压成型后的材料进行排胶烧结、被银、极化、得到压电陶瓷材料。
3.如权利要求2所述的一种压电陶瓷材料的制备方法，其特征在于，具体方法如下：
(1)按照化学式计量比分别称取氧化铅、二氧化锰、五氧化二铌、三氧化二锑、二氧化锆、二氧化钛，对其进行一次球磨，按质量比，以锆球∶料∶去离子水＝2∶1∶1，按照球、料、水的顺序加入磨罐中进行混合，放入球磨机，转速350rpm，球磨时间8h，进行球磨；
(2)将一次球磨所得的磨料放入80℃的常规烘箱中进行烘干，烘干时间为12h；
(3)将所得烘干磨料放入马弗炉中进行预烧，预烧温度从20℃到960℃，升温速率为2.0℃/min，时间470min，升温至960℃之后，保温240分钟，然后自然冷却到室温；
(4)将所得烘干磨料放入马弗炉中进行预烧，预烧温度从20℃到100℃，升温时间为90min，升温至100℃之后，继续升温至850℃，升温时间为320min，升温至850℃后保温180分钟，然后自然冷却到室温，升温过程中不用冲入惰性气体；
(5)将预烧所得的预烧料进行二次球磨，以锆球：料：去离子水＝2:1:1比例，按照球、料、水的顺序加入磨罐中，放入球磨机，转速350rpm，球磨时间6h，进行球磨；
(6)将二次球磨所得的磨料放入100摄氏度烘箱中烘6h；
(7)将烘干所得的料先经过40目筛，再加入10％质量比的PVA，进行人工造粒；
(8)将造粒后的材料放入模具，再将模具装到压机上，然后加压10MPa，加压时间15秒；
(9)将干压成型后的材料进行排胶烧结，室温升至550℃，升温时间450min；550℃下保温3小时，550℃升温至1250℃，升温时间600min；1250℃下保温6小时，自然冷却；
(10)将所得材料进行被银；
(11)将所得材料进行极化。
4.如权利要求3所述的一种压电陶瓷材料的制备方法，其特征在于，所述被银为手刷印银方式。
5.如权利要求3所述的一种压电陶瓷材料的制备方法，其特征在于，所述极化的极化方式为硅油极化，极化电压和时间分别为3.5KV/mm，20min，极化温度为110℃。
6.如权利要求1所述的一种压电陶瓷材料，其特征在于，所述压电陶瓷材料的性能参数为：
。
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