CN105819854A - 一种降低铅基压电陶瓷烧结温度的添加物及其应用方法 - Google Patents

一种降低铅基压电陶瓷烧结温度的添加物及其应用方法 Download PDF

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CN105819854A
CN105819854A CN201610129089.0A CN201610129089A CN105819854A CN 105819854 A CN105819854 A CN 105819854A CN 201610129089 A CN201610129089 A CN 201610129089A CN 105819854 A CN105819854 A CN 105819854A
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lead
piezoelectric ceramics
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周佳骏
童兴野
刘红
方敬忠
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Abstract

本发明公开了一种降低铅基压电陶瓷烧结温度的添加物及其应用方法，涉及电子陶瓷技术领域，特别涉及一种添加物可以降低铅基压电陶瓷烧结温度的用途。采用的铅基基体配方体系分别为铌镁酸‑钛酸铅(PMN‑PT)和锰锑‑铌镍‑锆钛酸铅(PMS‑PNN‑PZT)。在基本体系中，添加质量分数为0.1‑2.0％的LiF，可以将陶瓷的烧结温度从1250℃降低至1100℃左右，并保持相对优异的性能。本发明可以有效降低共烧电极的成本，同时降低PbO的挥发，减少对环境的影响。

Description

一种降低铅基压电陶瓷烧结温度的添加物及其应用方法
技术领域
本发明涉及一种用于电子元器件行业的压电陶瓷材料，特别是涉及铅基压电陶瓷及其制备方法。
背景技术
压电陶瓷是一类极其重要的电子功能材料，基于该材料的元器件如微位移驱动器、传感器、换能器等，在航空航天、光学和信息技术等领域得到的广泛的应用。
压电陶瓷的性能优劣直接影响到器件的性能，因此关于原材料的性能研究非常重要。上世纪40年代人们发现了钛酸钡压电陶瓷陶瓷(BaTiO3)，它是最早发现的压电陶瓷材料。但是，BaTiO3较低的居里温度(TC＝120℃)限制了其使用的温度范围。1955年，B.Jaffe等发现了一种二元系钛锆酸铅(Pb(Zr,Ti)O3，PZT)，这种材料的压电性能更为优越。PZT是由铁电相PbTiO3和反铁电相PbZrO3构成的连续固溶体，其结构同BaTiO3一样，均为ABO3钙钛矿型。1965年，日本学者HiromuOuchi等通过在PZT中添加第三种组分铌镁酸铅Pb(Mg1/3Nb2/3)O3，研制成第一种商用三元系压电陶瓷材料(PMN-PZT)。目前市场上使用的压电陶瓷原材料大多数都是含铅的多元系陶瓷。
传统铅基压电陶瓷的烧结温度一般在1250℃左右，这样高的烧结温度会带来一些问题。首先是环境方面，铅基压电陶瓷中PbO的含量超过60wt％，而PbO在高于800℃就开始挥发，高温烧结将带来的严重的PbO挥发。而PbO是一种对自然界生物有毒性的物质。其次，大量PbO的挥发会使得陶瓷本身组分产生偏离，产品性能不稳定。另外，在多层压电陶瓷器件中，为了达到高的烧结温度，共烧的Ag-Pd电极中Pd的含量将会急剧上升，这样极大地增加了电极的成本。最后，低的烧结温度可以降低能耗。
综上，低温烧结铅基压电陶瓷将会有效降低元器件制造成本，提高产品竞争力。许多学者已经研究过PZT基压电陶瓷的低温烧结技术。以往的一些低温烧结技术中，通常会用到CdO或者V2O5，而这两类物质均为强毒性物质。同时，过度追求低的烧结温度，反而对陶瓷的性能造成恶化。本发明将铅基压电陶瓷烧结温度降低到1100℃附近，同时具有优异的电学性能；而且添加物对环境影响较小。
发明内容
本发明的目的是提供一种能够降低铅基压电陶瓷烧结温度的添加物，适合于该类陶瓷在微位移驱动器、传感器、蜂鸣片等器件中的应用。采用LiF添加物来降低压电陶瓷的烧结温度，得到低温烧结陶瓷；不仅可以降低成本，而且符合环保的要求。该类陶瓷可以应用在多层压电陶瓷器件、电声转换器件等领域。
本发明通过以下技术方案来实现：一种添加物，单一化合物LiF，在铅基压电陶瓷中的质量分数为0.1—2％。
所述的一种添加物在降低压电陶瓷烧结温度的用途，以铌镁-钛酸铅(PMN-PT)为基体配方，在基体配方中加入基本配方体系重量为0.1—2％的添加物。采用常规的压电陶瓷制备工艺，可以获得低温烧结的压电陶瓷。
所述的一种添加物在降低压电陶瓷烧结温度中的用途，所述铌镁-钛酸铅为：Pb(Mg1/3Nb2/3)O3-PbTiO3，其中PbTiO3的最佳含量不超过20mol％。
所述的一种添加物在降低压电陶瓷烧结温度中的用途，以锰锑-铌镍-锆钛酸铅(PMS-PNN-PZT)为基体配方，在基体配方中加入基本配方体系重量为0.1—2％的添加物。采用常规的压电陶瓷制备工艺，可以获得低温烧结的压电陶瓷。
所述的一种添加物在降低压电陶瓷烧结温度中的用途，所述锰锑-铌镍-锆钛酸铅为：Pb(Mn1/3Sb2/3)O3–Pb(Ni1/3Nb2/3)0.5Zr0.14Ti0.36O3。，其中Pb(Mn1/3Sb2/3)O3的最佳含量不超过3mol％。
一种低温烧结铅基压电陶瓷，包含所述的一种添加物，具有单一的钙钛矿结构。
铅基压电陶瓷的基体配方采用以下两种方式：
(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3+ywt％LiF，其中0≤x≤0.2，0≤y≤2。
(1-z)Pb(Mn1/3Sb2/3)O3–zPb(Ni1/3Nb2/3)0.5Zr0.14Ti0.36O3+ywt％LiF，其中0≤z≤0.03，0≤y≤2。
压电陶瓷制造方式为传统固相烧结工艺。按化学计量比称量后，将原料粉球磨混合，烘干，过40目筛后，压片，在860℃烧结2h；将烧结得到的原料块，碾碎，球磨，烘干，过筛后，加入一定量的的PVA水溶液造粒得到的陶瓷粉体，然后模压成型，得到生坯片。生坯片先在600℃脱脂，然后在1100℃烧结2h，陶瓷片进行抛光、表面被银和极化处理。
本发明的有益效果是：添加物简单，成本低；在与电极的共烧过程中采用Ag70-Pd30电极，降低了成本；本发明采用的是常规陶瓷工艺，适合大规模生产。
具体实施方式
实施例1
表1给出了本例中所实施的6个试样的配方。本发明以分析纯级Pb3O4、TiO2、MgO、LiF、和Nb2O5为原材料，按照化学式(1-x)Pb(Mg1/3Nb2/3)O3-xPbTiO3+ywt％LiF，(Pb3O4过量1.8wt％)称取原材料之后，放入球磨罐中，以无水乙醇为介质，球磨24h后，将得到的浆料放入烘箱烘干，过40目筛，在860℃预烧2h。将预烧得到的粉料破碎，球磨，烘干之后过120目筛，然后加入一定量的3wt％PVA水溶液造粒，模压成型，在600℃停留2h排胶，然后在1100-1230℃烧结2h。将烧好的陶瓷片抛光，烧银电极之后静置24h之后，进行电学性能测试。
表1
试样编号 X Y 烧结温度 Tm(℃) εr loss d33 *(1kV/mm) 迟滞
1 0.10 0 1230 47 29190 0.080 1114 23％
2 0.10 0.25 1170 43 23195 0.072 871 10％
3 0.10 0.50 1150 30 16492 0.056 406 3％
4 0.10 0.75 1100 24 14548 0.030 348 3％
5 0.14 0.5 1150 54 21503 0.077 883 14％
6 0.14 0.75 1100 42 18251 0.079 625 6％
实施例2
表2给出了本例中所实施的4个试样的配方。本发明以分析纯级Pb3O4、ZrO2、TiO2、MnO2、Sb2O3、NiO、LiF和Nb2O5为原材料，按照化学式(1-z)Pb(Mn1/3Sb2/3)O3–zPb(Ni1/3Nb2/3)0.5Zr0.14Ti0.36O3+ywt％LiF(Pb3O4过量1.8wt％)称取原材料之后，放入球磨罐中，以无水乙醇为介质，球磨24h后，将得到的浆料放入烘箱烘干，过40目筛，在860℃预烧2h。将预烧得到的粉料破碎，球磨，烘干之后过120目筛，然后加入一定量的3wt％PVA水溶液造粒，模压成型，在600℃停留2h排胶，然后在1100-1250℃烧结2h。将烧好的片抛光，烧银电极之后，在75℃极化15min。静置24h之后，进行电学性能测试。
表2
试样编号 Z Y 烧结温度 Tc(℃) Qm loss d33 *(1kV/mm) d33(pC/N)
1 0.01 0 1250 147 118 0.007 1058 620
2 0.02 0 1250 139 163 0.004 1036 550
3 0.01 0.5 1100 156 109 0.003 824 473
4 0.02 0.5 1100 143 63 0.004 779 431
以上所述仅为本发明较好的实施案例，并不用于限制本发明。熟悉本领域的技术人员可以容易对以上这些实例进行修改，并把一般原理应用到其它实例中而不通过创造性的劳动。故凡本领域技术人员根据本发明之提示，对本发明进行的修改和改进均在本发明的保护之内。

Claims (6)

1.一种添加物，其特征在于：单一化合物LiF，在铅基压电陶瓷中的质量分数为0.1—2％。
2.根据权利要求1所述的一种添加物在降低压电陶瓷烧结温度中的用途，其特征在于：以铌镁-钛酸铅(PMN-PT)为基体配方，在基体配方中加入基本配方体系重量为0.1—2％的添加物。采用常规的压电陶瓷制备工艺，可以获得低温烧结的压电陶瓷。
3.根据权利要求2所述的一种添加物在降低压电陶瓷烧结温度中的用途，其特征在于：所述铌镁-钛酸铅为：Pb(Mg1/3Nb2/3)O3-PbTiO3，其中PbTiO3的最佳含量不超过20mol％。
4.根据权利要求1所述的一种添加物在降低压电陶瓷烧结温度中的用途，其特征在于：以锰锑-铌镍-锆钛酸铅(PMS-PNN-PZT)为基体配方，在基体配方中加入基本配方体系重量为0.1—2％的添加物；采用常规的压电陶瓷制备工艺，可以获得低温烧结的压电陶瓷。
5.根据权利要求4所述的一种添加物在降低压电陶瓷烧结温度中的用途，其特征在于：所述锰锑-铌镍-锆钛酸铅为：Pb(Mn1/3Sb2/3)O3–Pb(Ni1/3Nb2/3)0.5Zr0.14Ti0.36O3，其中Pb(Mn1/3Sb2/3)O3的最佳含量不超过3mol％。
6.一种低温烧结铅基压电陶瓷，其特征在于：包含权利要求1所述的一种添加物，具有单一的钙钛矿结构。
CN201610129089.0A 2016-03-07 2016-03-07 一种降低铅基压电陶瓷烧结温度的添加物及其应用方法 Pending CN105819854A (zh)

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