CN107922275A - 在水性环境中制造无铅压电陶瓷 - Google Patents

在水性环境中制造无铅压电陶瓷 Download PDF

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CN107922275A
CN107922275A CN201680046152.2A CN201680046152A CN107922275A CN 107922275 A CN107922275 A CN 107922275A CN 201680046152 A CN201680046152 A CN 201680046152A CN 107922275 A CN107922275 A CN 107922275A
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piezoelectric property
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CN107922275B (zh
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H-J.施赖纳
T.艾因黑林格-米勒
F.阿斯曼
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Abstract

本发明涉及用于在主要为水性的悬浮剂中制造具有压电性能的陶瓷的方法。

Description

在水性环境中制造无铅压电陶瓷
本发明涉及用于在主要为水性的悬浮剂中制造具有压电性能的陶瓷的方法。
在现有技术中，已知其中使用有机悬浮剂的用于制造压电陶瓷的方法。在压电陶瓷如钛酸铋钠-(BNT)或钛酸铋钠-钛酸钡-(BNT-BT)陶瓷的制造中，水性分散体本身同样是已知的。
现有技术已知的使用水性分散体的方法的缺点是可溶性成分如碱可能在这些水性分散体的预处理(Aufbereitung)中溶解出来并会在干燥过程中分离。这导致的问题是溶解的物质不均匀地分布在陶瓷中，陶瓷由此具有差的压电值。
本发明的目的是开发不具有上述缺点的方法。所述目的通过用于制造具有压电性能的陶瓷的本发明方法得以实现，其中使用主要为水性的悬浮剂。所制造的具有压电性能的陶瓷优选无铅，特别优选地，所制造的具有压电性能的陶瓷为钛酸铋钠-(BNT)、钛酸铋钠-钛酸钡-(BNT-BT)、铌酸钾钠-(KNN)或钛酸铋钠-铌酸钾钠-(BNT-KNN)陶瓷或其混合物。
根据本发明，所述用于制造具有压电性能的陶瓷的方法包括原料的混合、碾磨、压制颗粒(Pressgranulat)的制造，以及其它的步骤，如各向同性分布的冷冻，和随后的温度处理。
用于制造压电元件的本发明方法包括以下步骤：
a) 混合原料；
b)碾磨原料；
c)将碾磨的原料混合物造粒，如喷雾冷冻造粒；
d)煅烧；
e)制造包含所述煅烧产物的泥浆；
f)将所述泥浆造粒；
g)制造压制品；
h)脱脂和烧结；
i)金属化和极化。
原料混合和碾磨的方法步骤在主要为水性的悬浮剂(悬浮剂中水的含量> 80%，优选> 90%)中进行，并且通过工艺控制而防止可溶性成分与不溶性成分的分离，该分离导致不均匀的材料。
根据本发明，由此制备的用于制造无铅压电陶瓷的悬浮体包含40-60%的陶瓷、40-60%的水和<20%，优选<5%的(有机)添加剂，该陶瓷优选选自钛酸铋钠-(BNT)、钛酸铋钠-钛酸钡-(BNT-BT)、铌酸钾钠-(KNN)或钛酸铋钠-铌酸钾钠-(BNT-KNN)陶瓷或其混合物。
特别地，通过将存在于水性悬浮体中的各向同性分布定型并随后在没有发生脱混(“分离”)的情况下除去悬浮介质，防止可溶性成分与不溶性成分的分离。
例如通过冷冻所述悬浮体，可以实现各向同性分布的定型。所述冷冻优选在其温度低于所述悬浮体熔化温度的冷冻介质(液态、固态或气态)中进行。所述冷冻介质的温度优选远低于所述悬浮体的熔化温度，特别是低于所述悬浮体熔化温度> 10K，并且使得所述悬浮体能够急速冷冻。
所述冷冻介质选自液态或气态的氮、液态或气态的空气、液态或气态的氧、其它液态或气态的有机或无机介质，优选液氮。
也可以通过借助物理方法如压力变化、固体介质或类似方法冷冻所述悬浮体，通过相变将各向同性分布定型。所述定型也可以通过凝胶化过程等进行，如通过改变pH值(ζ电位)。另一方面，也可以通过絮凝进行定型，如通过改变所述分散体的pH值(ζ电位)。也可以加入一种或多种添加剂以实现定型。
根据本发明，在排除毛细力并且不产生显著液相的情况下进行悬浮剂的除去，由此保持冷冻分布。所述悬浮剂优选通过在合适的压力(<1bar，优选<100mbar)/温度条件下使主要为水性的悬浮剂升华至一定的低残留水分含量(<5%，优选<3%)而除去。
在根据本发明的教导的一个优选的实施方案中，所述冷冻通过喷入到冷冻介质，优选液氮中来进行，由此同时产生原生颗粒(Protogranulat)。由于冷冻干燥，这些原生颗粒变成可进一步加工的颗粒。
然而，所述悬浮剂也可以通过化学方法，如通过分解除去。
所述定型的分布通过反应程序转移到所需的压电陶瓷材料中。该反应程序优选为所述定型分布的温度处理(煅烧/混合氧化物法)，由此形成煅烧产物。
可以由如此形成的煅烧产物制造可压缩(pressfähig)粉末。为此，首先制造泥浆。根据本发明，由此制备的用于制造无铅压电陶瓷的悬浮体包含40-60%的陶瓷、40-60%的水和<20%，优选<5%的(有机)添加剂，该陶瓷优选选自钛酸铋钠-(BNT)、钛酸铋钠-钛酸钡-(BNT-BT)、铌酸钾钠-(KNN)或钛酸铋钠-铌酸钾钠-(BNT-KNN)陶瓷或其混合物。
通过喷雾干燥或其它造粒方法由所述泥浆制造粉末。由所述煅烧产物制造可压缩粉末的此类造粒方法优选为喷雾冷冻造粒或喷雾干燥。
下文基于制造钛酸铋钠-钛酸钡-陶瓷(BNT-BT)的实施例1描述本发明的方法，但本发明不应受其限制。
实施例1：
所述方法基于以下方法步骤进行：
1)制造Bi2O3-Na2CO3-TiO2-悬浮体
将Bi2O3、Na2CO3、TiO2、水和研磨球称入容器中。随后将该悬浮体均化或解附聚。
2)将Bi2O3-Na2CO3-TiO2-悬浮体进行喷雾冷冻造粒
将所述陶瓷悬浮体喷洒在装有液氮的托盘中并由此急速冷冻。通过经由储料槽的软管连接，供应泥浆。在每次喷雾操作开始时，用液氮装填产物托盘。由于液氮的蒸发，定期检查喷雾单元之间的料位，并任选补充氮气。这用于确保冷冻的液滴被液氮连续覆盖，从而防止泥浆再次熔化。在喷雾操作之后，将含有冷冻的泥浆液滴和液氮的产物托盘放入冷冻干燥设备中。一旦液氮除了少量残留物外完全蒸发，冷冻干燥过程就开始，即冷冻干燥设备中的压力降低。对于颗粒的主要干燥，确定大概24小时的时间。省去后干燥步骤。
3)制造Bi2O3-Na2CO3-TiO2-BaTiO3-粉末混合物
对于所述Bi2O3-Na2CO3-TiO2-BaTiO3-粉末混合物，将所述喷雾冷冻颗粒和BaTiO3粉末以不同含量(表1)称入容器中。在加入若干研磨球之后，将所述容器放在辊式破碎机上并干燥混合，以产生均匀的粉末混合物。
表 1:原料的摩尔比
4)煅烧
将Bi2O3-Na2CO3-TiO2-BaTiO3-粉末混合物分散在托盘中。在900℃下进行煅烧所述粉末混合物以产生BNT-BT。
5)制造BNT-BT-泥浆
煅烧后，使用行星式球磨机碾磨BNT-BT粉末。分离出研磨球之后，向所述泥浆中加入有机添加剂。将所述泥浆再次在辊式破碎机上均化。
6)BNT-BT泥浆的喷雾冷冻造粒
与步骤2)类似
7)BNT-BT-部件的压制
借助于单轴压机在大约200MPa的压制压力下制造压制品。
8)脱脂和烧结
在800℃下将所述坯件脱脂。之后，将所述压制体置于壳囊中并烧结。
9)金属化和极化
通过研磨表面，将烧结的片材的厚度设定为1mm。使用银糊在两面上金属化，其通过丝网印刷施涂并在700至900℃下烘烤。对于极化，施加梯形电压分布，其中最大电压在2至5kV之间变化。
为了更好理解，实施例1的方法流程作为流程图示于图1中。
通过这种方式，制造不同压电陶瓷，其特征参数通过DIN 50324 1-3(截至2002年12月)中定义的方法测定。
表 2:本发明的压电陶瓷的测试结果
BNT-BT6 BNT
d33 (pC/N) 200 87
kp (%) 30 16
kt (%) 50 44
εT 33/ε0 1000 460
ρ (g/cm³) 5.8 5.8

Claims (17)

1.用于制造具有压电性能的陶瓷的方法，其特征在于：使用主要为水性的悬浮剂。
2.根据权利要求1所述的用于制造具有压电性能的陶瓷的方法，其特征在于：在第一方法步骤中，将原料在主要为水性的悬浮剂中混合并碾磨，由此产生具有各向同性分布的悬浮体。
3.根据权利要求2所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述悬浮体的各向同性分布在随后的方法步骤中被定型。
4.根据权利要求3所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述各向同性分布的定型通过冷冻所述悬浮体进行。
5.根据权利要求4所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述冷冻在液态、固态或气态的冷冻介质中进行。
6.根据权利要求5所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述冷冻介质的温度低于所述悬浮体的熔化温度，优选远低于所述熔化温度。
7.根据权利要求6所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述悬浮体被急速冷冻。
8.根据权利要求5至7中任一项所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述冷冻介质选自液态或气态的氮、液态或气态的空气、液态或气态的氧、或其它液态或气态的有机或无机介质。
9.根据权利要求4至7中任一项所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述冷冻通过喷入到冷冻介质中进行，由此产生原生颗粒。
10.根据权利要求3所述的用于制造具有压电性的能陶瓷的方法，其特征在于：所述各向同性分布的定型通过物理方法如压力变化、固体介质等，通过胶凝化方法，通过分散体的絮凝，或通过加入添加剂进行。
11.根据前述权利要求中任一项所述的用于制造具有压电性能的陶瓷的方法，其特征在于：在排除毛细力并且不产生显著液相的情况下除去悬浮剂。
12.根据权利要求11所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述悬浮剂的除去通过升华进行。
13.根据权利要求3至12中任一项所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述定型的各向同性分布通过反应程序转移到压电材料中。
14.根据权利要求13所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述反应程序是温度处理(煅烧)，由此获得煅烧产物。
15.根据权利要求14所述的用于制造具有压电性能的陶瓷的方法，其特征在于：通过造粒方法由所述煅烧产物制造可压缩粉末。
16.根据权利要求15所述的用于制造具有压电性能的陶瓷的方法，其特征在于：所述造粒方法是喷雾干燥或喷雾冷冻造粒。
17.用于制造具有压电性能的陶瓷的悬浮体，其特征在于：所述悬浮体包含40-60%的陶瓷、40-60%的水和<20%，优选<5%的(有机)添加剂，所述陶瓷优选选自钛酸铋钠-(BNT)、钛酸铋钠-钛酸钡-(BNT-BT)、铌酸钾钠-(KNN)或钛酸铋钠-铌酸钾钠-(BNT-KNN)陶瓷或其混合物。
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