CN114835489B - 一种铌酸钾钠基无铅压电陶瓷及其制备方法 - Google Patents
一种铌酸钾钠基无铅压电陶瓷及其制备方法 Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 32
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000011734 sodium Substances 0.000 claims description 19
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- 238000002156 mixing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
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- 229910052451 lead zirconate titanate Inorganic materials 0.000 description 2
- 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 2
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Abstract
本发明涉及功能陶瓷材料领域,具体涉及一种铌酸钾钠基无铅压电陶瓷及其制备方法。本发明提供的铌酸钾钠基无铅压电陶瓷的制备方法,包括如下步骤:将压电陶瓷粗品在60‑120℃的环境中依次进行交流电场极化和直流电场极化,得到所述压电陶瓷。本发明提供的铌酸钾钠基无铅压电陶瓷的制备方法使压电陶瓷的压电系数有明显提高,而反向压电系数在温度变化过程中稳定性得到提高。
Description
技术领域
本发明涉及功能陶瓷材料领域,具体涉及一种铌酸钾钠基无铅压电陶瓷及其制备方法。
背景技术
压电材料由于具有正、逆压电效应而可实现机械能与电能的相互转换,因此作为一种重要的功能材料被广泛应用于驱动器、传感器等高新技术领域。目前,锆钛酸铅基压电陶瓷因其性能的优越性而成为应用最广泛的压电材料,但是该体系材料中含有大量有毒的铅,在生产、使用及废弃处理过程中均会给人类健康和生态环境带来严重的危害。因此,研发性能优异的无铅压电陶瓷材料成为一项紧迫且具有重大实用意义的课题。
2004年,日本的Saito等人在Nature杂志上报道了利用织构方法制备的经掺杂改性的铌酸钾钠基压电陶瓷,其压电系数d33达416pC/N,可以与含铅压电陶瓷相媲美。该里程碑式的重大突破掀起了研究铌酸钾钠基无铅压电陶瓷的热潮,并使得铌酸钾钠基无铅压电陶瓷被认为是最具潜力替代含铅压电陶瓷的体系之一。目前,大部分关于铌酸钾钠基无铅压电陶瓷的研究仍专注于通过掺杂改性在室温附近形成多晶型相变区以提高其压电性能。但是,由于多晶型相变区的存在,使得铌酸钾钠基无铅压电陶瓷压电性能的温度稳定性很差。例如,对LiSbO3掺杂的铌酸钾钠无铅压电陶瓷,其反向压电系数d33*在室温下为355pm/V,而当温度升高至50℃时急剧下降至250pm/V,降幅达30%。反向压电性能对温度如此强烈的敏感性使铌酸钾钠基无铅压电陶瓷应用受限。
发明内容
因此,本发明要解决的技术问题在于克服现有技术中的铌酸钾钠基无铅压电陶瓷虽具有较优的压电性能,但对温度敏感,热稳定性较差的缺陷,从而提供一种铌酸钾钠基无铅压电陶瓷及其制备方法。
本发明提供一种铌酸钾钠基无铅压电陶瓷的制备方法,包括如下步骤:将压电陶瓷粗品在60-120℃的环境中依次进行交流电场极化和直流电场极化,得到所述压电陶瓷。
优选的,所述交流电场强度为10~30kV/cm,交流电场的频率为0.1-20Hz,极化循环的次数为20-50次,所述直流电场极化的电场强度为20-40kV/cm,极化时间为20~120秒。
优选的,将压电陶瓷粗品置于60-120℃的硅油中依次进行交流电场极化和直流电场极化,得到所述压电陶瓷。
优选的,所述压电陶瓷粗品的制备方法包括如下步骤:
1)按配方比例称取各组分原料,然后将原料混合后依次经一次球磨、一次烘干、一次烧结、二次球磨、二次烘干后得到混合粉料;
2)将混合料粉冷压成型、冷等静压处理后进行二次烧结,得到所述压电陶瓷粗品;
其中,以重量分数计,所述压电陶瓷粗品的原料包括:0.80-3.45份的CaCO3,7.10-12.18份的Na2CO3,8.20-15.90份的K2CO3,0.20-0.71份的Li2CO3,0-3.85份的MnO2,0.60-4.24份的ZrO2,28.50-57.32份的Nb2O5,1.2-13.20份的Ta2O5。
优选的,在步骤1)中,所述一次球磨为湿法球磨,溶剂为无水乙醇;球磨转速为200-300rpm,球磨时间为4-24h;二次球磨为湿法球磨,溶剂为无水乙醇,球磨转速为200-300rpm,球磨时间为4-24h;
在步骤1)中,一次烘干的温度为50-65℃,一次烘干时间为6-24h;二次烘干的温度为50-65℃,二次烘干时间为6-24h。
优选的,在步骤1)中,一次烧结在空气条件进行,烧结温度为700~875℃,烧结时间为2-6h;在步骤2)中,二次烧结在空气条件进行,烧结温度为1060~1160℃,烧结时间为1-6h。
优选的,在步骤2)中,所述冷压成型的压力为30-50MPa,压制时间为30-60s;所述冷等静压的压力为200-300MPa,压制时间为5-20min。
本发明还提供一种铌酸钾钠基无铅压电陶瓷,由上述所述的铌酸钾钠基无铅压电陶瓷的制备方法制备得到。
优选的,所述铌酸钾钠基无铅压电陶瓷的通式为:
(1-x)(KaNaaLibCac)(NbdTaeZrf)O3-xMnO2,其中2a+b+c=1,d+e+f=1,0.44≤a≤0.48,0.01≤b≤0.05,0.02≤c≤0.07,0<d≤0.97,0.06≤e≤0.2,0.02≤f≤0.07;0≤x≤0.08,其中x为铌酸钾钠基无铅压电陶瓷中的MnO2与铌酸钾钠基无铅压电陶瓷的质量比。
优选的,所述铌酸钾钠基无铅压电陶瓷的压电常数d33为310~380pC/N;
在外加电场作用下,其反向压电常数d33*在室温至160℃的温度范围内的波动不超过10%。
本发明技术方案,具有如下优点:
本发明提供的铌酸钾钠基无铅压电陶瓷的制备方法,包括将压电陶瓷粗品在60-120℃的环境中依次进行交流电场极化和直流电场极化,得到所述压电陶瓷。本发明通过在直流电场极化前进行交流电场极化,使压电陶瓷粗品中的电畴结构在温度变化过程中稳定性得到提高,从而使压电陶瓷的压电系数有明显提高,而反向压电系数在温度变化过程中稳定性得到提高。从测试例的结果中可以发现铌酸钾钠基无铅压电陶瓷的具有优异的压电常数d33和机电耦合因素kp,同时反向压电常数d33*在室温至160℃的温度范围内的波动≤10%。
进一步,本发明通过所述压电陶瓷粗品的制备方法包括如下步骤:1)按配方比例称取各组分原料,然后将原料混合后依次经一次球磨、一次烘干、一次烧结、二次球磨、二次烘干后得到混合粉料;2)将混合料粉冷压成型、冷等静压处理后进行二次烧结,得到所述压电陶瓷粗品;其中,以重量分数计,所述压电陶瓷粗品的原料包括:0.80-3.45份的CaCO3,7.10-12.18份的Na2CO3,8.20-15.90份的K2CO3,0.20-0.71份的Li2CO3,00-3.85份的MnO2,0.60-4.24份的ZrO2,28.50-57.32份的Nb2O5,1.2-13.20份的Ta2O5。利用该方法制备得到的铌酸钾钠基无铅压电陶瓷粗品,在外加电场作用下可以进一步提高铌酸钾钠基无铅压电陶瓷的压电性能的温度稳定性。
进一步,本发明通过所述压电陶瓷粗品的制备方法中包括一次球磨和二次球磨,球磨介质均为无水乙醇,一次球磨时间为4-24h,二次球磨时间为4-24h,经过一次球磨和二次球磨后,得到成分均匀且细化的粉体,由此可以进一步提高铌酸钾钠基无铅压电陶瓷的综合性能。
进一步,本发明通过所述压电陶瓷粗品的制备方法中一次烧结是在空气条件700~875℃的温度下进行的,由此可以使得碳化物和氧化物中的碳元素和部分氧元素烧蚀掉,以便制备得到具有上述化学组成的铌酸钾钠基无铅压电陶瓷,并且利用该方法可以进一步提高铌酸钾钠基无铅压电陶瓷的压电性能的温度稳定性。
进一步,本发明通过所述压电陶瓷粗品的制备方法中冷压成型的压力为30-50MPa,压制时间为30-60s;冷等静压的压力为200-300MPa,压制时间为5-20分钟,由此可以进一步提高铌酸钾钠基无铅压电陶瓷的温度稳定性。
进一步,本发明通过所述压电陶瓷粗品的制备方法中是在空气条件1060~1160℃的温度下进行的,由此可以进一步提高铌酸钾钠基无铅压电陶瓷的温度稳定性。
具体实施方式
提供下述实施例是为了更好地进一步理解本发明,并不局限于所述最佳实施方式,不对本发明的内容和保护范围构成限制,任何人在本发明的启示下或是将本发明与其他现有技术的特征进行组合而得出的任何与本发明相同或相近似的产品,均落在本发明的保护范围之内。
实施例中未注明具体实验步骤或条件者,按照本领域内的文献所描述的常规实验步骤的操作或条件即可进行。所用试剂或仪器未注明生产厂商者,均为可以通过市购获得的常规试剂产品。
实施例1
本实施例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2211g的Li2CO3,7.7958g的Na2CO3,10.1654g的K2CO3,37.0924g的Nb2O5,4.6422g的Ta2O5,1.4818g的CaCO3,1.8359g的ZrO2和1.5938g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm;球磨后将物料在60℃烘干24h,将烘干后的物料在875℃空气条件下烧结6h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm,球磨后将物料在60℃烘干12h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为60s,将粉料压制为直径15mm、厚度1.0mm的圆片,之后在300MPa下进行冷等静压处理20min,冷等静压处理后在空气条件下1105℃烧结3h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于120℃的硅油中依次进行交流电场极化和直流电场极化,所述交流电场极化电场强度为40kV/cm,交流电场的频率为1Hz,极化循环50次,所述直流电场极化的电场强度为30kV/cm,极化时间为20秒,得到所述铌酸钾钠基无铅压电陶瓷。
本实施例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为:0.945(K0.467Na0.467Li0.019Ca0.047)(Nb0.886Ta0.0667Zr0.0473)O3-0.055MnO2。
实施例2
本实施例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2276g的Li2CO3,8.0227g的Na2CO3,10.4612g的K2CO3,38.1718g的Nb2O5,4.7773g的Ta2O5,1.5249g的CaCO3,1.8893g的ZrO2和0.7969g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为24h,球磨转速为200rpm;球磨后将物料在65℃烘干12h,将烘干后的物料在900℃空气条件下烧结5h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为24h,球磨转速为200rpm,球磨后将物料在65℃烘干12h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为30s,将粉料压制为直径10mm、厚度1.5mm的圆片,之后在300MPa下进行冷等静压处理15min,冷等静压处理后在空气条件下1115℃烧结3h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于90℃的硅油中依次进行交流电场极化和直流电场极化,所述交流电场极化的电场强度为30kV/cm,交流电场的频率为1Hz,极化循环50次,所述直流电场极化的电场强度为30kV/cm,极化时间为20秒,得到所述铌酸钾钠基无铅压电陶瓷。
本实施例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为:0.9725(K0.467Na0.467Li0.019Ca0.047)(Nb0.886Ta0.0667Zr0.0473)O3-0.0275MnO2。x=0.05y=0.01
实施例3
本实施例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2156g的Li2CO3,7.6020g的Na2CO3,9.9126g的K2CO3,36.17002g的Nb2O5,4.5267g的Ta2O5,1.4450g的CaCO3,1.7903g的ZrO2和2.2748g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为24h,球磨转速为250rpm;球磨后将物料在60℃烘干24h,将烘干后的物料在900℃空气条件下烧结2h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为24h,球磨转速为250rpm,球磨后将物料在60℃烘干24h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为40s,将粉料压制为直径10mm、厚度1.5mm的圆片,之后在200MPa下进行冷等静压处理15min,冷等静压处理后在空气条件下1085℃烧结3h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于120℃的硅油中依次进行交流电场极化和直流电场极化,所述交流电场极化的电场强度为40kV/cm,交流电场的频率为1Hz,极化循环40次,所述直流电场极化的电场强度为40kV/cm,极化时间为20秒,得到所述铌酸钾钠基无铅压电陶瓷。
本实施例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为:0.9215(K0.467Na0.467Li0.019Ca0.047)(Nb0.886Ta0.0667Zr0.0473)O3-0.0785MnO2。
实施例4
本实施例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2283g的Li2CO3,8.2051g的Na2CO3,10.6990g的K2CO3,38.6040g的Nb2O5,5.5768g的Ta2O5,1.5301g的CaCO3,1.1663g的ZrO2和0.7013g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm;球磨后将物料在65℃烘干12h,将烘干后的物料在900℃空气条件下烧结6h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm,球磨后将物料在65℃烘干12h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为45s,将粉料压制为直径10mm、厚度1.5mm的圆片,之后在200MPa下进行冷等静压处理15min,冷等静压处理后在空气条件下1120℃烧结2h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于90℃的硅油中依次进行交流电场极化和直流电场极化,所述交流电场极化的电场强度为30kV/cm,交流电场的频率为2Hz,极化循环40次,所述直流电场极化的电场强度为30kV/cm,极化时间为20秒,得到所述铌酸钾钠基无铅压电陶瓷。
本实施例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为:0.9758(K0.476Na0.476Li0.019Ca0.029)(Nb0.893Ta0.0776Zr0.0291)O3-0.0242MnO2。
实施例5
本实施例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2284g的Li2CO3,8.0259g的Na2CO3,10.4653g的K2CO3,32.8593g的Nb2O5,13.6548g的Ta2O5,2.1611g的CaCO3,2.6647g的ZrO2和0.2318g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为24h,球磨转速为200rpm;球磨后将物料在60℃烘干24h,将烘干后的物料在850℃空气条件下烧结6h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为24h,球磨转速为200rpm,球磨后将物料在60℃烘干24h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为30s,将粉料压制为直径10mm、厚度1.5mm的圆片,之后在200MPa下进行冷等静压处理20min,冷等静压处理后在空气条件下1125℃烧结2h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于120℃的硅油中依次进行交流电场极化和直流电场极化,所述交流电场极化的电场强度为30kV/cm,交流电场的频率为1Hz,极化循环40次,所述直流电场极化的电场强度为30kV/cm,极化时间为60秒,得到所述铌酸钾钠基无铅压电陶瓷。
本实施例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为:0.992(K0.458Na0.458Li0.0187Ca0.0653)(Nb0.7477Ta0.1869Zr0.0654)O3-0.008MnO2。
对比例1
本对比例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2211g的Li2CO3,7.7958g的Na2CO3,10.1654g的K2CO3,37.0924g的Nb2O5,4.6422g的Ta2O5,1.4818g的CaCO3,1.8359g的ZrO2和1.5938g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm;球磨后将物料在60℃烘干24h,将烘干后的物料在875℃空气条件下烧结6h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm,球磨后将物料在60℃烘干12h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为60s,将粉料压制为直径15mm、厚度1.0mm的圆片,之后在300MPa下进行冷等静压处理20min,冷等静压处理后在空气条件下1105℃烧结3h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于120℃的硅油中进行直流电场极化,所述直流电场极化的电场强度为30kV/cm,极化时间为20秒,得到铌酸钾钠基无铅压电陶瓷。
本对比例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为:0.945(K0.467Na0.467Li0.019Ca0.047)(Nb0.886Ta0.0667Zr0.0473)O3-0.055MnO2。
对比例2
本对比例提供一种铌酸钾钠基无铅压电陶瓷的制备方法,如下步骤:
1)将0.2211g的Li2CO3,7.7958g的Na2CO3,10.1654g的K2CO3,37.0924g的Nb2O5,4.6422g的Ta2O5,1.4818g的CaCO3,1.8359g的ZrO2和1.5938g的MnO2混合后在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm;球磨后将物料在60℃烘干24h,将烘干后的物料在875℃空气条件下烧结6h;将烧结后的物料在球磨机中进行湿法球磨,球磨溶剂为无水乙醇,球磨时间为12h,球磨转速为250rpm,球磨后将物料在60℃烘干12h,得到混合粉料;
2)将步骤1)中得到的混合粉料冷压成型,冷压成型的压力为50MPa,压制时间为60s,将粉料压制为直径15mm、厚度1.0mm的圆片,之后在300MPa下进行冷等静压处理20min,冷等静压处理后在空气条件下1105℃烧结3h,得到压电陶瓷粗品;
3)将压电陶瓷粗品置于120℃的硅油中进行交流电场极化,所述交流电场极化电场强度为40kV/cm,交流电场的频率为1Hz,极化循环50次,得到所述铌酸钾钠基无铅压电陶瓷。
本对比例提供的铌酸钾钠基无铅压电陶瓷的制备方法制备的铌酸钾钠基无铅压电陶瓷的通式为0.945(K0.467Na0.467Li0.019Ca0.047)(Nb0.886Ta0.0667Zr0.0473)O3-0.055MnO2。
测试例
对实施例1-5和对比例1和2得到的铌酸钾钠基无铅压电陶瓷进行压电常数d33、机电耦合因素kp、相对介电常数ε33/ε0、居里温度Tc和反向压电常数d33*进行测试。
压电常数d33采用中国科学院声学所的ZJ-6A型准静态压电常数测试仪进行测试;
机电耦合因素kp采用北京邦联时代电子科技有限公司的PV80阻抗分析仪进行测试;
相对介电常数ε33/ε0采用是德4980AL型LCR表进行测试;
居里温度Tc采用武汉佰力博科技有限公司的DMS-1000系列高温介电阻抗温谱仪进行测试;
压电常数d33、机电耦合因素kp、相对介电常数ε33/ε0、居里温度Tc的测试结果见表1,反向压电常数d33*的测试结果见表1。
反向压电常数d33*采用德国aixACCT公司的TF ANALYZER 1000型铁电分析仪进行测试,其中测试温度范围为20-160℃,测试结果见表2。
表1
表2
显然,上述实施例仅仅是为清楚地说明所作的举例,而并非对实施方式的限定。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。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (7)
1.一种铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于,包括如下步骤:
将压电陶瓷粗品在60-120℃的环境中依次进行交流电场极化和直流电场极化,得到所述压电陶瓷;所述交流电场强度为10~30kV/cm,交流电场的频率为0.1-20Hz,极化循环的次数为20-50次,所述直流电场极化的电场强度为20-40kV/cm,极化时间为20~120秒;
其中,以重量分数计,所述压电陶瓷粗品的原料包括:1.4818份的CaCO3,7.7958份的Na2CO3,10.1654份的K2CO3,0.2211份的Li2CO3,1.5938份的MnO2,1.8359份的ZrO2,37.0924份的Nb2O5,4.6422份的Ta2O5。
2.根据权利要求1所述的铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于,将压电陶瓷粗品置于60-120℃的硅油中依次进行交流电场极化和直流电场极化,得到所述压电陶瓷。
3.根据权利要求1或2所述的铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于,所述压电陶瓷粗品的制备方法包括如下步骤:
1)按配方比例称取各组分原料,然后将原料混合后依次经一次球磨、一次烘干、一次烧结、二次球磨、二次烘干后得到混合粉料;
2)将混合料粉冷压成型、冷等静压处理后进行二次烧结,得到所述压电陶瓷粗品;
其中,以重量分数计,所述压电陶瓷粗品的原料包括:1.4818份的CaCO3,7.7958份的Na2CO3,10.1654份的K2CO3,0.2211份的Li2CO3,1.5938份的MnO2,1.8359份的ZrO2,37.0924份的Nb2O5,4.6422份的Ta2O5。
4.根据权利要求3所述的铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于,在步骤1)中,所述一次球磨为湿法球磨,溶剂为无水乙醇;球磨转速为200-300rpm,球磨时间为4-24h;二次球磨为湿法球磨,溶剂为无水乙醇,球磨转速为200-300rpm,球磨时间为4-24h;
在步骤1)中,一次烘干的温度为50-65℃,一次烘干时间为6-24h;二次烘干的温度为50-65℃,二次烘干时间为6-24h。
5.根据权利要求3所述的铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于,在步骤1)中,一次烧结在空气条件进行,烧结温度为700~875℃,烧结时间为2-6h;在步骤2)中,二次烧结在空气条件进行,烧结温度为1060~1160℃,烧结时间为1-6h。
6.根据权利要求3所述的铌酸钾钠基无铅压电陶瓷的制备方法,其特征在于,在步骤2)中,所述冷压成型的压力为30-50MPa,压制时间为30-60s;所述冷等静压的压力为200-300MPa,压制时间为5-20min。
7.一种铌酸钾钠基无铅压电陶瓷,其特征在于,由权利要求1-6任一项所述的铌酸钾钠基无铅压电陶瓷的制备方法制备得到。
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