CN111848164B - 一种高横向谐振频率温度稳定性压电陶瓷及其制备方法与应用 - Google Patents

一种高横向谐振频率温度稳定性压电陶瓷及其制备方法与应用 Download PDF

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CN111848164B
CN111848164B CN202010572000.4A CN202010572000A CN111848164B CN 111848164 B CN111848164 B CN 111848164B CN 202010572000 A CN202010572000 A CN 202010572000A CN 111848164 B CN111848164 B CN 111848164B
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凌志远
肖长柳
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South China University of Technology SCUT
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Abstract

本发明公开了一种高横向谐振频率温度稳定性压电陶瓷及其制备方法与应用。所述压电陶瓷材料的化学组成为：0.1Pb(Yb0.5Nb0.5)O3‑0.9Pb(Zr0.48Ti0.52)O3，以主晶相0.1Pb(Yb0.5Nb0.5)O3‑0.9Pb(Zr0.48Ti0.52)O3总重为百分比，MnCO3掺入量为0.2～0.6wt％。以Pb3O4、TiO2、ZrO2、Yb2O3、Nb2O5和MnCO3粉末为原料，采用氧化物固相反应法制备样品，高温烧结得到铌镱锆钛酸铅基压电陶瓷，能满足中小功率压电陶瓷应用对横向谐振频率温度稳定性的要求。

Description

一种高横向谐振频率温度稳定性压电陶瓷及其制备方法与 应用
技术领域
本发明属于压电陶瓷材料领域，具体涉及一种高横向谐振频率温度稳定性压电陶瓷及其制备方法与应用。
背景技术
压电陶瓷可以实现机械能与电能之间的高效转换，目前已被广泛应用于超声探测，移动通信，人工智能等高新技术领域，而在不同应用领域对压电陶瓷性能有不同的要求，如在航空航天、能源开发等领域需要压电陶瓷能同时具有高的居里温度与好的谐振频率温度稳定性，以保证压电陶瓷不会因温度变化而性能劣化。典型的三元系压电陶瓷，如Pb(Mg1/3Nb2/3)O3-Pb(Zr,Ti)O3、Pb(Ni1/3Nb2/3)O3-Pb(Zr,Ti)O3等，居里温度TC都低于250℃，若按照压电陶瓷的实际使用温度为TC的一半计算，其实际使用温度低于130℃。而Ohuchi等研究的Pb(Yb0.5Nb0.5)O3-Pb(Zr,Ti)O3(PYN-PZT)三元系压电陶瓷(Piezoelectric andstructural properties of Pb(Yb1/2Nb1/2)O3-PbTiO3-PbZrO3 ceramics,Journal of theEuropean Ceramic Society,19(6):1191-1195,1999)，TC可达390℃，其实际使用温度接近200℃，因此PYN-PZT陶瓷具有在高温领域应用的潜力。
然而，压电陶瓷在使用过程中，性能参数会随着温度改变而发生变化，其中谐振频率随温度的波动十分敏感。Wersing认为(Temperature coefficient of resonancefrequencies and permittivity in PZT ceramics near the morphotropic phaseboundary.Ferroelectrics,37(1):611-614,1981)作为功率压电器件所用的压电陶瓷，其谐振频率常数温度系数应该控制在100ppm/K之间，因为谐振频率常数的变化将直接导致压电陶瓷的谐振频率发生漂移。对于谐振器、超声电机等压电器件，它们的工作频率为其谐振频率点，如果谐振频率发生漂移将会导致驱动电路需额外增设频率自动追踪回路，从而使驱动电路更加复杂、成本更高，不利于器件的应用，因此亟需一种具有高谐振频率温度稳定性的压电陶瓷材料。
发明内容
为解决现有技术的缺点和不足之处，本发明的首要目的在于提供一种高横向谐振频率温度稳定性压电陶瓷，该压电陶瓷满足中小功率压电陶瓷应用对横向谐振频率温度稳定性的要求。
本发明的另一目的在于提供上述一种高横向谐振频率温度稳定性压电陶瓷的制备方法。
本发明的再一目的在于提供上述一种高横向谐振频率温度稳定性压电陶瓷的应用。
本发明目的通过以下技术方案实现：
一种高横向谐振频率温度稳定性压电陶瓷，其配方组成为：
0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3+xMnCO3，其中，MnCO3占主晶相0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3总质量的0.2～0.6％，即x为0.2～0.6％。
优选的，所述x为0.4％。
上述一种高横向谐振频率温度稳定性压电陶瓷的制备方法，包括以下步骤：
(1)将Pb3O4、TiO2、ZrO2、Yb2O3、Nb2O5和MnCO3按化学计量比0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3+xMnCO3配料，球磨混合均匀，烘干，过筛，煅烧，得到煅烧粉体；
(2)将煅烧粉体球磨混合均匀，烘干，加入粘结剂混均并过筛，干压成型，得到陶瓷生坯；
(3)将陶瓷生坯排胶后在1250～1290℃下烧结2～3h，得到的陶瓷涂覆银浆，烧银，极化，得到铌镱锆钛酸铅基压电陶瓷。
优选的，步骤(1)所述煅烧的条件为：800～900℃下煅烧3～4h。
优选的，步骤(1)和(2)所述过筛均指过60～80目筛。
优选的，步骤(1)和(2)所述球磨混合均匀的条件均为：以水为溶剂，氧化锆球为球磨介质，其中料、球和水的质量比为1:2:1，在300～350rpm/min下球磨90～120min。
优选的，步骤(1)和(2)所述烘干的条件均为：在100～130℃下干燥8～12h。
优选的，步骤(2)所述粘结剂为聚乙烯醇，所述粘结剂的加入量占煅烧粉体质量的1～1.5％。
优选的，步骤(2)所述干压成型的条件为：在20～40MPa的轴向压力下保压20～40s。
优选的，步骤(2)所述陶瓷生坯的直径为20～25mm，厚度为1.5～2.5mm。
优选的，步骤(3)所述排胶的条件为：在700～800℃保温1～2h。
优选的，步骤(3)所述涂覆银浆指在陶瓷上通过丝网印刷上银电极。
优选的，步骤(3)所述烧银的条件为：700～800℃下烧制15～30min。
优选的，步骤(3)所述极化的条件为：在100～140℃硅油中、3～4kV/mm直流电场下极化20～40min。
上述一种高横向谐振频率温度稳定性压电陶瓷的应用。
优选在功率器件中的应用。
与现有技术相比，本发明具有以下优点及有益效果：
(1)本发明具有工艺简单、成本低廉、重复性好等优势。
(2)本发明通过加入MnCO3，所制备的压电陶瓷在-25～85℃范围内，横向谐振频率的斜率值最低值在-3～13Hz/℃之间，能满足中小功率压电陶瓷器件应用的要求。
附图说明
图1为实施例1～3所得压电陶瓷在密闭氧化铝坩埚中1290℃下烧结2h样品在28～400℃间的介电温谱，测试频率为1kHz，测试电平为1V。
图2为实施例1～3所得压电陶瓷在密闭的氧化铝坩埚中1290℃烧结2h样品在-25～85℃间的横向谐振频率温谱斜率值，测试电平为1V。
具体实施方式
下面结合实施例和附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
本发明实施例中未注明具体条件者，按照常规条件或者制造商建议的条件进行。所用未注明生产厂商者的原料、试剂等，均为可以通过市售购买获得的常规产品。
实施例1
步骤一：将高纯的Pb3O4、TiO2、ZrO2、Yb2O3、Nb2O5按照化学计量比为0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3总共称量100g，再加入0.2g的MnCO3和0.3g的Pb3O4。称量好的粉体放入球磨罐中，以去离子水为溶剂，氧化锆球为球磨介质，料、球和水的质量比为1:2:1，球磨90min(转速为300rpm/min)，在110℃下烘10h至干燥后研磨过80目筛，得到的粉体在900℃下煅烧4h。
步骤二：以去离子水为溶剂，氧化锆球为球磨介质，将煅烧过的粉体在研钵中磨碎后再次球磨，其中料、球和水的质量比为1:2:1，球磨90min(转速为300rpm/min)，得到的浆料在在110℃下烘10h至干燥后，加入10wt％的聚乙烯醇溶液(水为溶剂，质量浓度为12％)混合磨细并过60目筛。然后将磨细的粉体在22MPa的轴向压力下保压30s，压制成直径大约25mm、厚度大约2.5mm的陶瓷生坯。
步骤三：陶瓷生坯在750℃烧制1h排除有机物后，放置于密闭的氧化铝坩埚中，在1290℃下烧结2h。将烧结后样品涂覆银浆(丝网印刷法)，并在750℃下烧制15min，得到的陶瓷样品置于130℃硅油中，在30kV/cm的直流电场下极化30min。最后，将极化后的样品(压电陶瓷)切割成17mm×5mm×1.5～2mm长条片。
实施例2
将实施例步骤一中MnCO3粉末的用量改成0.4g，其他条件参照实施例1，得到压电陶瓷样品。
实施例3
将实施例步骤一中MnCO3粉末的用量改成0.6g，其他条件参照实施例1，得到压电陶瓷样品。
对比例1
将实施例步骤一中MnCO3粉末的用量改成0g，其他条件参照实施例1，得到压电陶瓷样品。
对比例2
将实施例步骤一中Zr/Ti改为0.50:0.50(摩尔比)，MnCO3粉末的用量改成0.2g，其他条件参照实施例1，得到压电陶瓷样品。
对比例3
将实施例步骤一中Zr/Ti改为0.50:0.50(摩尔比)，MnCO3粉末的用量改成0.4g，其他条件参照实施例1，得到压电陶瓷样品。
采用ZX80A阻抗分析仪测试实施例1～3和对比例1～3压电陶瓷样品的横向谐振频率温谱，样品置于环境试验箱中，测试温度范围为-25～85℃，升温速率为1℃/min，每间隔2℃测试一组数据。
对谐振频率温谱数据进行三次样条插值，每隔5个数据点取一个插值点，再计算每个插值点上的斜率值。
采用TH 2186A数字电桥测试实施例1～3压电陶瓷样品的电容C(1kHz、1V)随温度变化情况，通过计算相对介电常数
Figure BDA0002549963820000051
得到介电温谱，
Figure BDA0002549963820000052
计算公式如下：
Figure BDA0002549963820000053
其中Cs表示串联电容，单位：F；t表示样品厚度，单位：m；A表示有效电极面积单位：m2；ε0表示绝对介电常数，ε0＝8.85×10-12F/m。
采用Agilent 4294A阻抗分析仪测试实施例1～3压电陶瓷样品在室温下的横向谐振频率fr和谐振阻抗R、横向反谐振频率fa。机械品质因数Qm和横向机电耦合系数k31的计算公式如下：
Figure BDA0002549963820000061
其中fr和fa单位：Hz；
Figure BDA0002549963820000062
其中Δf＝fa-fr。
利用阿基米德原理测量样品体积密度，记录测试温度，分别测量样品的饱和重水m1，悬浮重m2和干重m0，根据测量水温得到水的密度ρ水，样品的体积密度ρ计算公式如下：
Figure BDA0002549963820000063
其中m0、m1和m2单位：kg；ρ和ρ水单位：kg/m3。
根据以上得到数据再计算出样品的弹性柔顺系数
Figure BDA0002549963820000064
和压电应变常数d31，公式如下：
Figure BDA0002549963820000065
其中l表示样品长度，单位m；
Figure BDA0002549963820000066
单位：m2/N；
Figure BDA0002549963820000067
其中d31单位：C/N。
测试的结果如表一所示，当MnCO3的引入量为0.4wt％时，TC＝376℃，Qm＝490，
Figure BDA0002549963820000071
温度在-25～85℃范围内，横向谐振频率的斜率值在-3～13Hz/℃之间，表明此时横向谐振频率随温度变化非常缓慢，能满足中小功率压电陶瓷器件应用的要求。
表一
Figure BDA0002549963820000072
表二
Figure BDA0002549963820000073
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (9)

1.一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，其配方组成为：
0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3+xMnCO3，其中，MnCO3占主晶相0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3总质量的0.2~0.6%，即x为0.2~0.6%。
2.权利要求1所述一种高横向谐振频率温度稳定性压电陶瓷的制备方法，其特征在于，包括以下步骤：
（1）将Pb3O4、TiO2、ZrO2、Yb2O3、Nb2O5和MnCO3按化学计量比0.1Pb(Yb0.5Nb0.5)O3-0.9Pb(Zr0.48Ti0.52)O3+xMnCO3配料，球磨混合均匀，烘干，过筛，煅烧，得到煅烧粉体；
（2）将煅烧粉体球磨混合均匀，烘干，加入粘结剂混均并过筛，干压成型，得到陶瓷生坯；
（3）将陶瓷生坯排胶后在1250~1290℃下烧结2~3h，得到的陶瓷涂覆银浆，烧银，极化，得到铌镱锆钛酸铅基压电陶瓷。
3.根据权利要求2所述一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，步骤（1）所述煅烧的条件为：800~900℃下煅烧3~4h。
4.根据权利要求2所述一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，步骤（3）所述极化的条件为：在100~140℃硅油中、3~4kV/mm直流电场下极化20~40min。
5.根据权利要求2所述一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，步骤（2）所述粘结剂为聚乙烯醇，所述粘结剂的加入量占煅烧粉体质量的1~1.5%。
6.根据权利要求2所述一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，步骤（1）和（2）所述过筛均指过60~80目筛。
7.根据权利要求2所述一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，步骤（1）和（2）所述球磨混合均匀的条件均为：以水为溶剂，氧化锆球为球磨介质，其中料、球和水的质量比为1:2:1，在300~350rpm/min下球磨90~120min；
步骤（2）所述干压成型的条件为：在20~40MPa的轴向压力下保压20~40s；
步骤（3）所述烧银的条件为：700~800℃下烧制15~30min。
8.根据权利要求2所述一种高横向谐振频率温度稳定性压电陶瓷，其特征在于，步骤（3）所述排胶的条件为：在700~800℃保温1~2h；步骤（1）和（2）所述烘干的条件均为：在100~130℃下干燥8~12h。
9.权利要求1所述一种高横向谐振频率温度稳定性压电陶瓷在功率器件中的应用。
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