CN107117964B - 一种不同温度预烧料混合的pzt压电陶瓷及其制备方法 - Google Patents

一种不同温度预烧料混合的pzt压电陶瓷及其制备方法 Download PDF

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CN107117964B
CN107117964B CN201710339829.8A CN201710339829A CN107117964B CN 107117964 B CN107117964 B CN 107117964B CN 201710339829 A CN201710339829 A CN 201710339829A CN 107117964 B CN107117964 B CN 107117964B
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尚勋忠
周桃生
古雪姣
郭健
吴静
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Youchuangtai Wuhan Technology Co ltd
Hubei University
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Hubei University
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Abstract

本发明公开了一种不同温度预烧料混合的PZT压电陶瓷及其制备方法,其化学式Pb(Zr1‑ xTix)O3+Ywt%La2O3+Zwt%Nb2O5,其中0.44≤x≤0.47,0.2≤Y≤0.4,0.1≤Z≤0.3。先按化学计量式比配料、球磨、烘干,然后分别在830℃,860℃,890℃三种温度下预烧;再经过二次球磨、烘干得到三种预烧温度不同的陶瓷粉体,然后以不同的配合比混合,压制成型;1250℃烧结、烧银、极化。本发明提高了压电系数、平面机电耦合系数、厚度机电耦合系数及介电常数,综合性能更好,可应用于对压电性能有较高要求的器件。

Description

一种不同温度预烧料混合的PZT压电陶瓷及其制备方法
技术领域
本发明涉及压电陶瓷技术领域,尤其涉及一种不同温度预烧料混合的PZT压电陶瓷及其制备方法。
背景技术
PZT压电陶瓷作为一种能实现机械能与电能相互转换新型的功能材料,广泛的应用于能源、机械、电子、国防等高技术领域。目前PZT压电陶瓷作为最为重要的商用功能陶瓷之一,近年来在大功率器件超声换能、超声马达、压电变压器、水声换能器及医用超声探头等方面得到了广泛使用。
随着各行各业的不断发展,对PZT压电陶瓷的性能要求也越来越高。因此如何提高PZT压电陶瓷的各项性能以满足日益提高的要求成为了热点。近年来,国内外的专家学者对PZT压电陶瓷的掺杂改性做了许多的研究,使其具备了更优异、更稳定的性能,使PZT陶瓷进入了一个新的发展阶段。但是,对于PZT陶瓷的预烧温度的研究报道却不是很多。
对于一般的PZT压电陶瓷而言,其制备工艺中的预烧过程十分重要,预烧是通过原料中原子或离子之间在加热作用下的扩散来完成固相化学反应,预烧过程中可以使各原料的固相化学反应充分均匀,生成固溶体,形成主晶相。不仅如此,预烧温度对压电陶瓷的压电性能和介电性能有十分重要的影响,这是因为合适的预烧温度能使原料之间的反应更加充分,有利于形成主晶相,使其在烧结过程中减小收缩率,形成的结构更为致密,进而使PZT压电陶瓷的性能提高。
发明内容
本发明的目的是为了进一步的提高PZT压电陶瓷的压电介电性能,使其能够满足相关领域对PZT压电陶瓷的要求,提供一种便于大规模生产的制备方法。
为了达到上述目的,本发明通过如下方案予以实现:
本发明的不同温度预烧料混合的PZT压电陶瓷的化学式是:Pb(Zr1-xTix)O3+Ywt%La2O3+Zwt%Nb2O5,其中0.44≤x≤0.47,0.2≤Y≤0.4,0.1≤Z≤0.3。
优选本发明的PZT压电陶瓷的化学式是:Pb(Zr0.53Ti0.47)O3+0.3wt%La2O3+0.2wt%Nb2O5,x=0.47,Y=0.3,Z=0.2。
本发明的不同温度预烧料混合的PZT压电陶瓷的制备方法的具体步骤如下:
(1)配料
将原料Pb3O4、ZrO2、TiO2、La2O3、Nb2O5按化学计量比配料,球磨并烘干;
(2)合成
将步骤(1)中混合均匀粉料分为三份,分别置于坩埚中并压实,加盖密封,在750℃~950℃范围内以三种不同的温度预烧2h;
(3)造粒及成型
将步骤(2)的合成料混合,每种预烧温度合成料加入混合配比的范围为10%~90%,球磨后烘干,得到陶瓷粉体;再加PVA粘合剂造粒,取造粒后的粉体放入模具中,压制成压电陶瓷坯体;
(4)排胶
将步骤(3)获得的压电陶瓷坯体置于加热炉,升温至600-800℃并保温0.5-2h,排出有机物;
(5)烧结
将步骤(4)排胶后的陶瓷坯体放在坩埚中并密封;将坩埚置于高温炉里,升温至1000-1500℃,保温1-4h,自然冷却至室温;
(6)烧银
将步骤(5)烧结后的压电陶瓷片在砂纸上研磨,采用丝网印刷工艺在其上下表面印刷银浆,置于加热炉中,升温至600-800℃并保温1-10min,自然冷却至室温;
(7)极化
将步骤(6)的烧银制品置于硅油中,施加直流电场,极化,然后自然冷却,得到本发明的PZT压电陶瓷。
步骤(1)中,优选球磨时间是2h。
步骤(2)中,优选分等量三份,预烧时间是2h。
步骤(3)中,优选球磨时间是4h,PVA粘合剂的加入量是5%(质量分数)。
步骤(4)中,优选升温至700℃并保温1h。
步骤(5)中,优选升温至1250℃,保温2.5h。
步骤(6)中,优选升温至680℃并保温5min。
步骤(7)中,优选烧成样品置于150℃的硅油中,以外加4kV/cm的直流电场极化10min;极化后的样品放置24h以消除局部剩余应力。
本发明的积极效果如下:
本发明通过不同温度预烧料混合的PZT压电陶瓷,提高了压电系数、机电耦合系数及介电常数。其中厚度机电耦合系数提高9.8%,平面机电耦合系数提高5%,压电系数提高11.5%,介电常数提高了17%。
具体实施方式
下面的实施例是对本发明的进一步详细描述。
实施例1
(1)配料
将原料Pb3O4、ZrO2、TiO2、La2O3、Nb2O5、按Pb(Zr0.53Ti0.47)O3+0.3wt%La2O3+0.2wt%Nb2O5(x=0.47,Y=0.3,Z=0.2)的化学计量比配料,并放于球磨罐中,加30%的去离子水,在行星式球磨机上球磨2h,球磨转速为250r/min;球磨后烘干。
(2)合成
将步骤(1)混合均匀的粉料分为等量三份,分别置于坩埚中并压实,并加盖密封,以830℃、860℃、890℃温度预烧,保温2h。
(3)造粒及成型
将步骤(2)的合成料按830℃:860℃:890℃=1:2:3的配比混合,球磨4h后烘干,得到陶瓷粉体;再加5%PVA粘合剂(质量分数为5wt%)造粒,使其具有良好的流动性,取适量造粒后的粉体放入模具中,通过液压机加压制成直径为12mm,厚度为1.2mm的圆片压电陶瓷坯体。
(4)排胶
将步骤(3)获得的压电陶瓷坯体置于加热炉,升温至700℃并保温1h,排出有机物。
(5)烧结
将步骤(4)排胶后的陶瓷坯体放在氧化铝坩埚中并用氧化锆粉密封;将坩埚置于高温炉里,升温至1250℃,保温2.5h,自然冷却至室温。
(6)烧银
将步骤(5)烧结后的压电陶瓷片在砂纸上研磨,采用丝网印刷工艺在其上下表面印刷银浆,置于加热炉中,升温至680℃并保温5min,自然冷却至室温。
(7)极化
将步骤(6)的烧银制品置于150℃的硅油中,施加4kv/cm的直流电场,极化10min,然后自然冷却,放置24h后测试性能。
实施例2
本例PZT压电陶瓷的制备方法大体上与实例1中一致,但是在具体制备中,将步骤(2)的合成料按3:2:1的比例混合,随后执行步骤(3)~(7)。
实施例3
本例PZT压电陶瓷的制备方法大体上与实例1中一致,但是在具体制备中,将步骤(2)的合成料按1:2:1的比例混合,随后执行步骤(3)~(7)。
对比实施例1
本例PZT压电陶瓷的制备方法大体上与实例1中一致,但是在具体制备中,将步骤(1)所得的粉体只进行860℃预烧并保温2h,随后执行步骤(3)~(7);
上述实例的测试结果详见表1。
表1
通过对比可知,不同温度预烧料混合PZT压电陶瓷在压电性能和介电性能都有所提高,且综合性能更好。
尽管已经示出和描述了本发明的实施例,对于本领域的普通技术人员而言,可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型,本发明的范围由所附权利要求及其等同物限定。

Claims (1)

1.一种不同温度预烧料混合的PZT压电陶瓷,其特征在于:所述的PZT压电陶瓷的化学式是:Pb(Zr0.53Ti0.47)O3+0.3wt%La2O3+0.2wt%Nb2O5
制备方法的具体步骤如下:
(1)配料
将原料Pb3O4、ZrO2、TiO2、La2O3、Nb2O5、按Pb(Zr0.53Ti0.47)O3+0.3wt%La2O3+0.2wt%Nb2O5的化学计量比配料,并放于球磨罐中,加30%的去离子水,在行星式球磨机上球磨2h,球磨转速为250r/min;球磨后烘干;
(2)合成
将步骤(1)混合均匀的粉料分为等量三份,分别置于坩埚中并压实,并加盖密封,以830℃、860℃、890℃温度预烧,保温2h;
(3)造粒及成型
将步骤(2)的合成料按830℃:860℃:890℃=1:2:3的配比混合,球磨4h后烘干,得到陶瓷粉体;再加5%PVA粘合剂,质量分数为5wt%,造粒,使其具有良好的流动性,取适量造粒后的粉体放入模具中,通过液压机加压制成直径为12mm,厚度为1.2mm的圆片压电陶瓷坯体;
(4)排胶
将步骤(3)获得的压电陶瓷坯体置于加热炉,升温至700℃并保温1h,排出有机物;
(5)烧结
将步骤(4)排胶后的陶瓷坯体放在氧化铝坩埚中并用氧化锆粉密封;将坩埚置于高温炉里,升温至1250℃,保温2.5h,自然冷却至室温;
(6)烧银
将步骤(5)烧结后的压电陶瓷片在砂纸上研磨,采用丝网印刷工艺在其上下表面印刷银浆,置于加热炉中,升温至680℃并保温5min,自然冷却至室温;
(7)极化
将步骤(6)的烧银制品置于150℃的硅油中,施加4kv/cm的直流电场,极化10min,然后自然冷却,得到PZT压电陶瓷。
CN201710339829.8A 2017-05-15 2017-05-15 一种不同温度预烧料混合的pzt压电陶瓷及其制备方法 Expired - Fee Related CN107117964B (zh)

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