CN114163233A - 一种高介低损耗压电陶瓷继电器材料及其制备方法 - Google Patents
一种高介低损耗压电陶瓷继电器材料及其制备方法 Download PDFInfo
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- CN114163233A CN114163233A CN202111643699.XA CN202111643699A CN114163233A CN 114163233 A CN114163233 A CN 114163233A CN 202111643699 A CN202111643699 A CN 202111643699A CN 114163233 A CN114163233 A CN 114163233A
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- Compositions Of Oxide Ceramics (AREA)
Abstract
本发明涉及电子陶瓷材料领域，具体为一种高介低损耗压电陶瓷继电器材料及其制备方法，由主体材料和表面镀层组成；所述主体材料的化学式为PbxSm1‑x(MnyNb1‑y)n(ZrzTi1‑z)1‑nO3+awt.％Y2O3+bwt.％Al2O3+cwt.％Sb2O3；其中，0.8≤x＜1，0.4≤y≤0.6，0.5≤z≤0.8，n＝0.15‑0.2，a＝0.55‑0.95，b＝1‑1.25，c＝0.22‑0.30；所述表面镀层为Ni‑Ag‑P层，本发明所制备压电陶瓷材料具有优异的压电性能，表面镀层腐蚀电位高，耐蚀性好，且镀速快，综合性能较好，不仅具有良好的导电性还可以对陶瓷材料起到很好的防护作用。
Description
技术领域
本发明涉及电子陶瓷材料领域，具体涉及一种高介低损耗压电陶瓷继电器材料及其制备方法。
背景技术
电子陶瓷(electronic ceramic)，是指在电子工业中能够利用电、磁性质的陶瓷。其是通过对表面、晶界和尺寸结构的精密控制而最终获得具有新功能的陶瓷，也是目前航天、新能源、新材料、微电子、激光、海洋工程和生物工程等高新技术的重要组成部分和不可缺少的物质基础，是当前高技术竞争的热点之一。
自19世纪80年代，居里兄弟首先在石英晶体上发现压电效应后，压电材料和压电器件的研究和生产发展极为迅速。压电陶瓷作为电子陶瓷材料的一种是实现机械能与电能相互转换的功能材料，作为电子信息材料的一个重要分支，广泛应用于压电振子和压电换能器等领域。
PZT基压电陶瓷材料具有压电常数高、易掺杂改性、稳定性好等特点，烧结温度一般在1200℃以上，虽然目前已经被广泛应用，但是，随着科技的发展，现有的PZT基压电陶瓷材料逐渐不能满足实际应用，需要对其进行改进以提供更多性能更优的压电陶瓷材料。
发明内容
发明目的：针对现有技术的以上缺陷或改进需求，本发明提供了一种高介低损耗压电陶瓷继电器材料及其制备方法。
本发明所采用的技术方案如下：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
所述主体材料的化学式为
PbxSm1-x(MnyNb1-y)n(ZrzTi1-z)1-nO3+awt.％Y2O3+bwt.％Al2O3+cwt.％Sb2O3；
其中，0.8≤x＜1，0.4≤y≤0.6，0.5≤z≤0.8，n＝0.15-0.2，a＝0.55-0.95，b＝1-1.25，c＝0.22-0.30；
所述表面镀层为Ni-Ag-P层。
进一步地，x为0.85、0.9、0.95、0.96或0.98，y为0.4、0.45、0.5、0.55或0.6，z为0.51、0.52、0.53、0.54或0.55。
进一步地，a＝0.55，b＝1，c＝0.25。
进一步地，所述压电陶瓷材料的介电常数2303≤ε≤2330，机电耦合系数0.62≤kp≤0.67，介电损耗0.24×10-2≤tanδ≤0.38×10-2，压电应变常数309≤d33≤343，机械品质因数842≤Qm≤885。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
S1：按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨12-15h后，80-85℃干燥8-10h，800-900℃预烧2-5h，再继续球磨12-15h，加入聚乙烯醇造粒，压片后先以5-10℃/min的速度升温至500-550℃排胶，再以2-4℃/min的速度升温至1250-1320℃烧结4-6h即可，得到主体材料；
S2：将主体材料除油、粗化、敏化、活化、还原后浸入镀液中，60-70℃施镀100-120min，所述镀液由以下重量百分数的成分组成：
NiSO4·6H2O 2-2.5％、Ag2SO4 1-1.5％、NaH2PO2 2-3％、柠檬酸钠4-5％、EDTA 1-3％、硼酸0.1-1％、表面活性剂BS-12 0.5-1％、余量为水；
S3：将上述镀件水洗、乙醇洗后，65-80℃干燥5-10h即可。
进一步地，除油操作如下：
将主体材料放入除油液中，80-85℃除油20-40min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：
除油剂FW 3-5％、NaOH 1-1.5％、Na2CO3 1-1.5％、Na3PO4 0.8-1％、余量为水。
进一步地，粗化操作如下：
将主体材料放入HF、水按质量比1：1-3组成的粗化液中，室温浸渍5-10min。
进一步地，敏化操作如下：
将主体材料放入SnCl2、HCl、水按质量比1-1.5：2-2.5：80-100组成的敏化液中，室温浸渍5-10min后水洗至无Cl-，烘干。
进一步地，活化操作如下：
将主体材料放入质量浓度为0.1-0.2％的PdCl2溶液中，室温浸渍5-10min后水洗，烘干。
进一步地，还原操作如下：
将主体材料放入质量浓度为0.4-1％的NaH2PO2溶液中，室温浸渍5-10min后水洗，烘干。
本发明的有益效果：
本发明提供了一种高介低损耗压电陶瓷继电器材料，是发明人在PZT基压电陶瓷材料基础上通过多元复合掺杂改性所获得的，通常认为，介电常数是晶粒和晶界的共同作用的结果，晶粒尺寸较小，晶界所占的比例越大，介电常数就越高，本发明所制备的压电陶瓷材料晶粒生长良好，瓷体的致密度高，气孔小，气孔率低，这是因为适量的Sm、Mn、Nb固熔到晶格内部，降低界面能，促进晶粒的生长和细化，增加了晶界的比例，提升了介电常数，本发明所制备压电陶瓷材料具有优异的压电性能，其中，介电常数2303≤ε≤2330，机电耦合系数0.62≤kp≤0.67，介电损耗0.24×10-2≤tanδ≤0.38×10-2，压电应变常数309≤d33≤343，机械品质因数842≤Qm≤885，完全能够满足压电振子、压电换能器、压电驱动器对陶瓷材料的应用要求，表面镀层腐蚀电位高，耐蚀性好，且镀速快，综合性能较好，不仅具有良好的导电性还可以对陶瓷材料起到很好的防护作用。
附图说明
图1为本发明实施例1所制备的压电陶瓷材料断面形貌的SEM图。
图2为本发明实施例1所制备的压电陶瓷材料主体材料和表面镀层界面处的SEM图。
具体实施方式
实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
主体材料的化学式为
Pb0.85Sm0.15(Mn0.4Nb0.6)0.15(Zr0.51Ti0.49)0.85O3+0.55wt.％Y2O3+1wt.％Al2O3+0.25wt.％Sb2O3；
表面镀层为Ni-Ag-P层。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨14h后，80℃干燥10h，850℃预烧5h，再继续球磨15h，加入聚乙烯醇造粒，压片后先以5℃/min的速度升温至500℃排胶，再以2℃/min的速度升温至1280℃烧结5h即可，得到主体材料；将主体材料放入除油液中，85℃除油30min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：除油剂FW 3％、NaOH 1％、Na2CO3 1.2％、Na3PO4 0.8％、余量为水，再将主体材料放入HF、水按质量比1：1组成的粗化液中，室温浸渍粗化10min，再将主体材料放入SnCl2、HCl、水按质量比1.5：2：80组成的敏化液中，室温浸渍10min后水洗至无Cl-，烘干，放入质量浓度为0.1％的PdCl2溶液中，室温浸渍10min后水洗，烘干，放入质量浓度为0.4％的NaH2PO2溶液中，室温浸渍10min后水洗，烘干后浸入镀液中，605℃施镀120min，所述镀液由以下重量百分数的成分组成：NiSO4·6H2O 2％、Ag2SO4 1％、NaH2PO2 2.5％、柠檬酸钠5％、EDTA 1％、硼酸0.2％、表面活性剂BS-12 0.6％、余量为水，将上述镀件水洗、乙醇洗后，80℃干燥5h即可。
实施例2：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
主体材料的化学式为
Pb0.85Sm0.15(Mn0.5Nb0.5)0.15(Zr0.51Ti0.49)0.85O3+0.55wt.％Y2O3+1wt.％Al2O3+0.25wt.％Sb2O3
表面镀层为Ni-Ag-P层。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨12h后，80℃干燥8h，800℃预烧2h，再继续球磨12h，加入聚乙烯醇造粒，压片后先以5℃/min的速度升温至500℃排胶，再以2℃/min的速度升温至1250℃烧结4h即可，得到主体材料；将主体材料放入除油液中，80℃除油20min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：除油剂FW 3％、NaOH 1％、Na2CO3 1％、Na3PO4 0.8％、余量为水，再将主体材料放入HF、水按质量比1：1组成的粗化液中，室温浸渍粗化5min，再将主体材料放入SnCl2、HCl、水按质量比1：2：80组成的敏化液中，室温浸渍5min后水洗至无Cl-，烘干，放入质量浓度为0.1％的PdCl2溶液中，室温浸渍5min后水洗，烘干，放入质量浓度为0.4％的NaH2PO2溶液中，室温浸渍5min后水洗，烘干后浸入镀液中，60℃施镀100min，所述镀液由以下重量百分数的成分组成：NiSO4·6H2O 2％、Ag2SO4 1％、NaH2PO2 2％、柠檬酸钠4％、EDTA 1％、硼酸0.1％、表面活性剂BS-12 0.5％、余量为水，将上述镀件水洗、乙醇洗后，65℃干燥5h即可。
实施例3：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
主体材料的化学式为
Pb0.9Sm0.1(Mn0.4Nb0.6)0.15(Zr0.51Ti0.49)0.85O3+0.55wt.％Y2O3+1wt.％Al2O3+0.25wt.％Sb2O3
表面镀层为Ni-Ag-P层。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨15h后，85℃干燥10h，900℃预烧5h，再继续球磨15h，加入聚乙烯醇造粒，压片后先以10℃/min的速度升温至550℃排胶，再以4℃/min的速度升温至1320℃烧结6h即可，得到主体材料；将主体材料放入除油液中，85℃除油40min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：除油剂FW 5％、NaOH 1.5％、Na2CO3 1.5％、Na3PO4 1％、余量为水，再将主体材料放入HF、水按质量比1：3组成的粗化液中，室温浸渍粗化10min，再将主体材料放入SnCl2、HCl、水按质量比1.5：2.5：100组成的敏化液中，室温浸渍10min后水洗至无Cl-，烘干，放入质量浓度为0.2％的PdCl2溶液中，室温浸渍10min后水洗，烘干，放入质量浓度为1％的NaH2PO2溶液中，室温浸渍10min后水洗，烘干后浸入镀液中，70℃施镀120min，所述镀液由以下重量百分数的成分组成：NiSO4·6H2O 2.5％、Ag2SO4 1.5％、NaH2PO2 3％、柠檬酸钠5％、EDTA 3％、硼酸1％、表面活性剂BS-12 1％、余量为水，将上述镀件水洗、乙醇洗后，80℃干燥10h即可。
实施例4：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
主体材料的化学式为
Pb0.85Sm0.15(Mn0.4Nb0.6)0.15(Zr0.55Ti0.45)0.85O3+0.55wt.％Y2O3+1wt.％Al2O3+0.25wt.％Sb2O3
表面镀层为Ni-Ag-P层。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨12h后，85℃干燥8h，900℃预烧2h，再继续球磨15h，加入聚乙烯醇造粒，压片后先以5℃/min的速度升温至550℃排胶，再以2℃/min的速度升温至1320℃烧结4h即可，得到主体材料；将主体材料放入除油液中，85℃除油20min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：除油剂FW 5％、NaOH 1％、Na2CO3 1.5％、Na3PO4 0.8％、余量为水，再将主体材料放入HF、水按质量比1：3组成的粗化液中，室温浸渍粗化5min，再将主体材料放入SnCl2、HCl、水按质量比1.5：2：100组成的敏化液中，室温浸渍5min后水洗至无Cl-，烘干，放入质量浓度为0.2％的PdCl2溶液中，室温浸渍5min后水洗，烘干，放入质量浓度为1％的NaH2PO2溶液中，室温浸渍5min后水洗，烘干后浸入镀液中，70℃施镀100min，所述镀液由以下重量百分数的成分组成：NiSO4·6H2O 2.5％、Ag2SO4 1％、NaH2PO2 3％、柠檬酸钠4％、EDTA 3％、硼酸0.1％、表面活性剂BS-12 1％、余量为水，将上述镀件水洗、乙醇洗后，65℃干燥10h即可。
实施例5：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
主体材料的化学式为
Pb0.85Sm0.15(Mn0.4Nb0.6)0.15(Zr0.51Ti0.49)0.85O3+0.55wt.％Y2O3+1wt.％Al2O3+0.25wt.％Sb2O3
表面镀层为Ni-Ag-P层。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨15h后，80℃干燥10h，800℃预烧5h，再继续球磨12h，加入聚乙烯醇造粒，压片后先以10℃/min的速度升温至500℃排胶，再以4℃/min的速度升温至1250℃烧结6h即可，得到主体材料；将主体材料放入除油液中，80℃除油40min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：除油剂FW 3％、NaOH 1.5％、Na2CO3 1％、Na3PO4 1％、余量为水，再将主体材料放入HF、水按质量比1：1组成的粗化液中，室温浸渍粗化10min，再将主体材料放入SnCl2、HCl、水按质量比1：2.5：80组成的敏化液中，室温浸渍10min后水洗至无Cl-，烘干，放入质量浓度为0.1％的PdCl2溶液中，室温浸渍10min后水洗，烘干，放入质量浓度为0.4％的NaH2PO2溶液中，室温浸渍10min后水洗，烘干后浸入镀液中，60℃施镀120min，所述镀液由以下重量百分数的成分组成：NiSO4·6H2O 2％、Ag2SO4 1.5％、NaH2PO2 2％、柠檬酸钠5％、EDTA 1％、硼酸1％、表面活性剂BS-12 0.5％、余量为水，将上述镀件水洗、乙醇洗后，80℃干燥5h即可。
实施例6：
一种高介低损耗压电陶瓷继电器材料，由主体材料和表面镀层组成；
主体材料的化学式为
Pb0.85Sm0.15(Mn0.4Nb0.6)0.15(Zr0.51Ti0.49)0.85O3+0.55wt.％Y2O3+1wt.％Al2O3+0.25wt.％Sb2O3
表面镀层为Ni-Ag-P层。
上述高介低损耗压电陶瓷继电器材料的制备方法如下：
按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨15h后，80℃干燥10h，880℃预烧5h，再继续球磨12h，加入聚乙烯醇造粒，压片后先以10℃/min的速度升温至520℃排胶，再以2℃/min的速度升温至1250℃烧结5h即可，得到主体材料；将主体材料放入除油液中，85℃除油30min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：除油剂FW 3％、NaOH 1.2％、Na2CO3 1％、Na3PO4 0.8％、余量为水，再将主体材料放入HF、水按质量比1：2组成的粗化液中，室温浸渍粗化10min，再将主体材料放入SnCl2、HCl、水按质量比1：2：100组成的敏化液中，室温浸渍5min后水洗至无Cl-，烘干，放入质量浓度为0.2％的PdCl2溶液中，室温浸渍5min后水洗，烘干，放入质量浓度为1％的NaH2PO2溶液中，室温浸渍5min后水洗，烘干后浸入镀液中，70℃施镀110min，所述镀液由以下重量百分数的成分组成：NiSO4·6H2O 2％、Ag2SO4 1％、NaH2PO2 2.5％、柠檬酸钠4％、EDTA 3％、硼酸0.2％、表面活性剂BS-12 1％、余量为水，将上述镀件水洗、乙醇洗后，70℃干燥10h即可。
对比例1：
对比例1与实施例1基本相同，区别在于，原料中不加入Sm2O3。
对比例2：
对比例2与实施例1基本相同，区别在于，原料中不加入MnO2。
对比例3：
对比例3与实施例1基本相同，区别在于，原料中不加入Nb2O3。
对比例4：
对比例4与实施例1基本相同，区别在于，原料中不加入Y2O3。
对比例5：
对比例5与实施例1基本相同，区别在于，原料中不加入Al2O3。
对比例6：
对比例6与实施例1基本相同，区别在于，原料中不加入Sb2O3。
性能测试：
①将实施例1-6及对比例1-6所制备的压电陶瓷材料在TH2828S阻抗分析仪上采用电桥法测量元件的共振频率和反共振频率，计算压电应变常数d33、介电系数ε和机械品质因数Qm及介电损耗tanδ，通过CB/T4314-2013计算求出机电耦合系数kp，压电应变常数d33越大表示压电性能越高，机械品质因数Qm越大表示陶瓷在共振振动时的损失约小。
表1：
由上表1可知，本发明所制备压电陶瓷材料具有优异的压电性能，其中，介电常数2303≤ε≤2330，机电耦合系数0.62≤kp≤0.67，介电损耗0.24×10-2≤tanδ≤0.38×10-2，压电应变常数309≤d33≤343，机械品质因数842≤Qm≤885，完全能够满足压电振子、压电换能器、压电驱动器对陶瓷材料的应用要求。
②通过称重法计算实施例1-6表面镀层镀速；通过电化学方法检测镀层腐蚀情况(以3.5％氯化钠溶液为腐蚀溶液，以饱和甘汞电极为参比电极，铂电极为辅助电极，扫描速度0.05V/s，等待时间10s)，结果如表2所示：
表2
由表2可知，本发明压电陶瓷材料表面镀层腐蚀电位高，耐蚀性好，且镀速快，所得镀层的综合性能较好，不仅具有良好的导电性还可以对陶瓷材料起到很好的防护作用。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (10)
1.一种高介低损耗压电陶瓷继电器材料，其特征在于，所述压电陶瓷材料由主体材料和表面镀层组成；
所述主体材料的化学式为
PbxSm1-x(MnyNb1-y)n(ZrzTi1-z)1-nO3+awt.％Y2O3+bwt.％Al2O3+cwt.％Sb2O3；
其中，0.8≤x＜1，0.4≤y≤0.6，0.5≤z≤0.8，n＝0.15-0.2，a＝0.55-0.95，b＝1-1.25，c＝0.22-0.30；
所述表面镀层为Ni-Ag-P层。
2.如权利要求1所述的高介低损耗压电陶瓷继电器材料，其特征在于，x为0.85、0.9、0.95、0.96或0.98，y为0.4、0.45、0.5、0.55或0.6，z为0.51、0.52、0.53、0.54或0.55。
3.如权利要求1所述的高介低损耗压电陶瓷继电器材料，其特征在于，a＝0.55，b＝1，c＝0.25。
4.如权利要求1所述的高介低损耗压电陶瓷继电器材料，其特征在于，所述压电陶瓷材料的介电常数2303≤ε≤2330，机电耦合系数0.62≤kp≤0.67，介电损耗0.24×10-2≤tanδ≤0.38×10-2，压电应变常数309≤d33≤343，机械品质因数842≤Qm≤885。
5.如权利要求1-4中任一项所述的高介低损耗压电陶瓷继电器材料的制备方法，其特征在于，具体如下：
S1：按照化学式配比称量PbO、Sm2O3、MnO2、Nb2O3、ZrO2、TiO2、Y2O3、Al2O3、Sb2O3，烘干后，加入球磨罐，以乙醇、柠檬酸铵、水组成的混合分散剂中，球磨12-15h后，80-85℃干燥8-10h，800-900℃预烧2-5h，再继续球磨12-15h，加入聚乙烯醇造粒，压片后先以5-10℃/min的速度升温至500-550℃排胶，再以2-4℃/min的速度升温至1250-1320℃烧结4-6h即可，得到主体材料；
S2：将主体材料除油、粗化、敏化、活化、还原后浸入镀液中，60-70℃施镀100-120min，所述镀液由以下重量百分数的成分组成：
NiSO4·6H2O 2-2.5％、Ag2SO4 1-1.5％、NaH2PO2 2-3％、柠檬酸钠4-5％、EDTA 1-3％、硼酸0.1-1％、表面活性剂BS-12 0.5-1％、余量为水；
S3：将上述镀件水洗、乙醇洗后，65-80℃干燥5-10h即可。
6.如权利要求5所述的高介低损耗压电陶瓷继电器材料的制备方法，其特征在于，除油操作如下：
将主体材料放入除油液中，80-85℃除油20-40min，取出后热水洗涤后烘干即可，所述除油液由以下重量百分数的成分组成：
除油剂FW 3-5％、NaOH 1-1.5％、Na2CO3 1-1.5％、Na3PO4 0.8-1％、余量为水。
7.如权利要求5所述的高介低损耗压电陶瓷继电器材料的制备方法，其特征在于，粗化操作如下：
将主体材料放入HF、水按质量比1：1-3组成的粗化液中，室温浸渍5-10min。
8.如权利要求5所述的高介低损耗压电陶瓷继电器材料的制备方法，其特征在于，敏化操作如下：
将主体材料放入SnCl2、HCl、水按质量比1-1.5：2-2.5：80-100组成的敏化液中，室温浸渍5-10min后水洗至无Cl-，烘干。
9.如权利要求5所述的高介低损耗压电陶瓷继电器材料的制备方法，其特征在于，活化操作如下：
将主体材料放入质量浓度为0.1-0.2％的PdCl2溶液中，室温浸渍5-10min后水洗，烘干。
10.如权利要求5所述的高介低损耗压电陶瓷继电器材料的制备方法，其特征在于，还原操作如下：
将主体材料放入质量浓度为0.4-1％的NaH2PO2溶液中，室温浸渍5-10min后水洗，烘干。
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