CN111747743A - 一种球面体压电陶瓷及其制备方法 - Google Patents

一种球面体压电陶瓷及其制备方法 Download PDF

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CN111747743A
CN111747743A CN202010533075.1A CN202010533075A CN111747743A CN 111747743 A CN111747743 A CN 111747743A CN 202010533075 A CN202010533075 A CN 202010533075A CN 111747743 A CN111747743 A CN 111747743A
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piezoelectric ceramic
parts
spherical piezoelectric
spherical
ceramic blank
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CN111747743B (zh
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朱惠祥
汤建海
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Guangzhou Kailitech Electronics Co ltd
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Abstract

本发明公开了一种球面体压电陶瓷及其制备方法,包括如下步骤:按照配比称取原料,将配好的粉料以去离子水和氧化锆球为研磨介质,采用行星球磨机球磨混合;过滤烘干,将粉料于900~1100℃预烧,再用行星球磨机球磨;再次过滤烘干,在粉料中加入8~12wt%的聚乙烯醇溶液进行造粒;干压成型制成所需尺寸的球面体压电陶瓷坯体;将球面体压电陶瓷坯体装进同球面体压电陶瓷坯体尺寸一致的氧化铝坩埚内,上方再放置质量为30~50g的球面体压电陶瓷坯体,一同装进排胶烧结匣钵内排胶烧结,再进行抛光,即得所述的球面体压电陶瓷。本发明能够解决因外力造成对压电陶瓷体的损伤,有利于降低生产成本和不良率,具有优异的压电性能。

Description

一种球面体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,具体涉及一种球面体压电陶瓷及其制备方法。
背景技术
压电陶瓷是一种新兴的陶瓷材料,迄今已有一百多年的发展历史。 上世纪中期,PZT 系压电陶瓷的发明,促进了电子技术的飞速发展,从而使各种电子产品出现在我们的面前,压电陶瓷作为其内部精密的元件,可以将电能转换成机械能或者将机械能转换成电能,在电子产品中起到了关键作用。
目前的球面体压电陶瓷的制备方法,经过机械磨外圆、机械磨平面、机械铣拋凸面、机械铣抛凹面对陶瓷体的损伤大,导致产品不良率高,对后期的产品电性能有一定的风险,且介电性能不能满足需求。
发明内容
本发明提供一种球面体压电陶瓷及其制备方法,所述的球面体压电陶瓷本无需经过过多的机械加工,具有优异的介电性能。
本发明解决其技术问题采用以下技术方案:
一种球面体压电陶瓷,所述球面体压电陶瓷由以下重量份原料组成:60~80份四氧化三铅、2~4份氧化镍、1~3份氧化钕、0.1~6份碳酸钡、0.1~5份碳酸锶、0.1~0.9份五氧化二铌、0.1~0.8份五氧化二锑、16~25份二氧化锆、8~15份改性二氧化钛。
优选的,所述球面体压电陶瓷由以下重量份原料组成:65~75份四氧化三铅、2~3份氧化镍、1~2份氧化钕、0.1~1份碳酸钡、0.2~2份碳酸锶、0.2~0.7份五氧化二铌、0.2~0.6份五氧化二锑、18~22份二氧化锆、9~14份改性二氧化钛。
最优选的,所述球面体压电陶瓷由以下重量份原料组成:70份四氧化三铅、2.5份氧化镍、1.5份氧化钕、0.5份碳酸钡、0.6份碳酸锶、0.4份五氧化二铌、0.45份五氧化二锑、20份二氧化锆、10份改性二氧化钛。
优选的,所述改性二氧化钛的制备方法为:将4~8份硝酸银溶在4~8份氨水中,加入6~10份金红石型二氧化钛,超声处理10~30min,过滤,放入球磨机内,加入0.4~1份碳酸钙、0.5~0.9份碳纤维、0.5~1.5份氯化钠、0.4~0.8份二氧化锰、1~2份氧化镁,在1000~1200r/min的转速下研磨30~50min,再与4~6份脱盐水混合均匀,过滤,干燥,研磨至400~600目即得所述改性二氧化钛。
最优选的,所述改性二氧化钛的制备方法为:将6份硝酸银溶在6份氨水中,加入8份金红石型二氧化钛,超声处理20min,过滤,放入球磨机内,加入0.7份碳酸钙、0.6份碳纤维、1份氯化钠、0.6份二氧化锰、1.5份氧化镁,在1100r/min的转速下研磨40min,再与5份脱盐水混合均匀,过滤,干燥,研磨至500目即得所述改性二氧化钛。
本发明还提供了一种球面体压电陶瓷的制备方法,包含如下步骤:
(1)按照配比称取原料,将配好的粉料以去离子水和氧化锆球为研磨介质,采用行星球磨机球磨混合;
(2)过滤烘干,将粉料于900~1100℃预烧,预烧后的料体再次用行星球磨机球磨;
(3)再次过滤烘干,在粉料中加入8~12wt%的聚乙烯醇溶液进行造粒;
(4)造粒后装料至模具中,干压成型制成所需尺寸的球面体压电陶瓷坯体,所述模具尺寸为D=21mm,R=22mm,T=1.1mm;
(5)将球面体压电陶瓷坯体装进同球面体压电陶瓷坯体尺寸一致的氧化铝坩埚内,上方再放置质量为30~50g的球面体压电陶瓷坯体,一同装进排胶烧结匣钵内排胶烧结,匣钵尺寸为L=115mm,B=115mm,H=50mm;
(6)排胶烧结完成得到所需球面体压电陶瓷粗糙体,进行抛光,即得所述的球面体压电陶瓷。
优选的,所述步骤(1)中料体:球:水=1:2~4:0.5~1.5。
优选的,所述步骤(1)、(2)中球磨转速为300~400r/min,球磨时间为3~5h。
优选的,所述步骤(3)中聚乙烯醇溶液的质量分数为15~25wt%。
优选的,所述步骤(4)中干压成型压力为10~14MPa,保压时间为4~6秒。
优选的,所述步骤(5)中排胶温度为500~600℃,保温时间为1.5~2.5h;所述烧结温度为1150~1310℃,保温1.5~3h。
本发明的有益效果:(1)本发明所述的球面体压电陶瓷将造粒好的压电陶瓷粉料直接干压成型制成所需的压电陶瓷球面坯体,同时把排胶烧结的氧化铝坩埚也一同制作成同干压模具尺寸一致球面体,同干压成型的压电陶瓷球面体整体装载在匣钵内一起进行排胶烧结;待烧结好后的压电陶瓷球面体进行最后的抛光;(2)本发明所述的球面体压电陶瓷无需经过过多的机械加工,解决因多次机械技工的外力造成对压电陶瓷体的损伤,有利于降低生产成本和不良率;(3)本发明所述的球面体压电陶瓷具有优异的压电介电性能。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面将对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
一种球面体压电陶瓷,所述球面体压电陶瓷由以下重量份原料组成:70份四氧化三铅、0.5份碳酸钡、0.6份碳酸锶、0.4份五氧化二铌、0.45份五氧化二锑、20份二氧化锆、10份改性二氧化钛。
所述改性二氧化钛的制备方法为:将6份硝酸银溶在6份氨水中,加入8份金红石型二氧化钛,超声处理20min,过滤,放入球磨机内,加入0.7份碳酸钙、0.6份碳纤维、1份氯化钠、0.6份二氧化锰、1.5份氧化镁,在1100r/min的转速下研磨40min,再与5份脱盐水混合均匀,过滤,干燥,研磨至500目即得所述改性二氧化钛。
一种球面体压电陶瓷的制备方法,包含如下步骤:
(1)按照配比称取原料,将配好的粉料以去离子水和氧化锆球为研磨介质,采用行星球磨机球磨混合;
(2)过滤烘干,将粉料于1000℃预烧,预烧后的料体再次用行星球磨机球磨;
(3)再次过滤烘干,在粉料中加入10wt%的聚乙烯醇溶液进行造粒;
(4)造粒后装料至模具中,干压成型制成所需尺寸的球面体压电陶瓷坯体,所述模具尺寸为D=21mm,R=22mm,T=1.1mm;
(5)将球面体压电陶瓷坯体装进同球面体压电陶瓷坯体尺寸一致的氧化铝坩埚内,上方再放置质量为40g的球面体压电陶瓷坯体,一同装进排胶烧结匣钵内排胶烧结,匣钵尺寸为L=115mm,B=115mm,H=50mm;
(6)排胶烧结完成得到所需球面体压电陶瓷粗糙体,进行抛光,即得所述的球面体压电陶瓷。
所述步骤(1)中料体:球:水=1:3:1。
所述步骤(1)、(2)中球磨转速为350r/min,球磨时间为4h。
所述步骤(3)中聚乙烯醇溶液的质量分数为19wt%。
所述步骤(4)中干压成型压力为12MPa,保压时间为5秒。
所述步骤(5)中排胶温度为550℃,保温时间为2h;所述烧结温度为1230℃,保温2h。
实施例2
实施例2与实施例1不同之处在于,球面体压电陶瓷的配比不同,其它都相同。
一种球面体压电陶瓷,所述球面体压电陶瓷由以下重量份原料组成:60份四氧化三铅、4份碳酸钡、0.1份碳酸锶、0.9份五氧化二铌、0.1份五氧化二锑、25份二氧化锆、8份改性二氧化钛。
实施例3
实施例3与实施例1不同之处在于,球面体压电陶瓷的配比不同,其它都相同。
一种球面体压电陶瓷,所述球面体压电陶瓷由以下重量份原料组成:80份四氧化三铅、0.1份碳酸钡、5份碳酸锶、0.1份五氧化二铌、0.8份五氧化二锑、16份二氧化锆、15份改性二氧化钛。
实施例4
实施例4与实施例1不同之处在于,实施例4与实施例1的制备参数不同,其它都相同。
一种球面体压电陶瓷的制备方法,包含如下步骤:
(1)按照配比称取原料,将配好的粉料以去离子水和氧化锆球为研磨介质,采用行星球磨机球磨混合;
(2)过滤烘干,将粉料于900℃预烧,预烧后的料体再次用行星球磨机球磨;
(3)再次过滤烘干,在粉料中加入8wt%的聚乙烯醇溶液进行造粒;
(4)造粒后装料至模具中,干压成型制成所需尺寸的球面体压电陶瓷坯体,所述模具尺寸为D=21mm,R=22mm,T=1.1mm;
(5)将球面体压电陶瓷坯体装进同球面体压电陶瓷坯体尺寸一致的氧化铝坩埚内,上方再放置质量为30g的球面体压电陶瓷坯体,一同装进排胶烧结匣钵内排胶烧结,匣钵尺寸为L=115mm,B=115mm,H=50mm;
(6)排胶烧结完成得到所需球面体压电陶瓷粗糙体,进行抛光,即得所述的球面体压电陶瓷。
所述步骤(1)中料体:球:水=1:2:0.5。
所述步骤(1)、(2)中球磨转速为300r/min,球磨时间为3h。
所述步骤(3)中聚乙烯醇溶液的质量分数为15wt%。
所述步骤(4)中干压成型压力为10MPa,保压时间为4秒。
所述步骤(5)中排胶温度为500℃,保温时间为1.5h;所述烧结温度为1150℃,保温1.5h。
实施例5
一种球面体压电陶瓷的制备方法,包含如下步骤:
(1)按照配比称取原料,将配好的粉料以去离子水和氧化锆球为研磨介质,采用行星球磨机球磨混合;
(2)过滤烘干,将粉料于1100℃预烧,预烧后的料体再次用行星球磨机球磨;
(3)再次过滤烘干,在粉料中加入12wt%的聚乙烯醇溶液进行造粒;
(4)造粒后装料至模具中,干压成型制成所需尺寸的球面体压电陶瓷坯体,所述模具尺寸为D=21mm,R=22mm,T=1.1mm;
(5)将球面体压电陶瓷坯体装进同球面体压电陶瓷坯体尺寸一致的氧化铝坩埚内,上方再放置质量为50g的球面体压电陶瓷坯体,一同装进排胶烧结匣钵内排胶烧结,匣钵尺寸为L=115mm,B=115mm,H=50mm;
(6)排胶烧结完成得到所需球面体压电陶瓷粗糙体,进行抛光,即得所述的球面体压电陶瓷。
所述步骤(1)中料体:球:水=1: 4: 1.5。
所述步骤(1)、(2)中球磨转速为400r/min,球磨时间为5h。
所述步骤(3)中聚乙烯醇溶液的质量分数为25wt%。
所述步骤(4)中干压成型压力为14MPa,保压时间为6秒。
所述步骤(5)中排胶温度为600℃,保温时间为2.5h;所述烧结温度为1310℃,保温3h。
对比例1
对比例1与实施例1不同之处在于,对比例1不含有四氧化三铅,其它都相同,
对比例2
对比例2与实施例1不同之处在于,对比例2用的是没有改性的二氧化钛,其它都相同。
对比例3
对比例3与实施例1不同之处在于,对比例3不含有改性二氧化钛,其它都相同。
对比例4
对比例4与实施例1不同之处在于,步骤(5)中上方没有再放置质量为40g的球面体压电陶瓷坯体,结果排胶烧结出来的球面体压电陶瓷体严重变形,达不到使用要求。
为了进一步证明本发明的效果,提供了以下测试方法:
1.检测实施例1~5、对比例1~3的锆钛酸铅压电陶瓷的性能(表1 )。
表1 性能参数
Figure 863476DEST_PATH_IMAGE001
通过表1可看出,本发明所述的球面体压电陶瓷的综合性能:相对介电常数2810~3300,介电损耗≤1.9%,平面机电耦合系数65~70%,机械品质因素63~75。其中实施例1为最佳实施方式;通过对比实施例1~3可看出,球面体压电陶瓷的原料配比影响着球面体压电陶瓷的性能,实施例1为最佳配比,有着最佳的相对介电常数、介电损耗、耦合常数、品质因数;通过对比实施例1与实施例4、实施例5,不同的制备参数也影响着球面体压电陶瓷的性能,实施例1为最佳参数;
通过对比实施例1与对比例1~3可知,改性二氧化钛和四氧化三铅显著影响着本发明的球面体压电常数的相对介电常数、介电损耗、耦合常数、品质因数。
以上述依据本发明的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本发明技术思想的范围内,进行多样的变更以及修改。本发明的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。

Claims (10)

1.一种球面体压电陶瓷,其特征在于,所述球面体压电陶瓷由以下重量份原料组成:60~80份四氧化三铅、2~4份氧化镍、1~3份氧化钕、0.1~6份碳酸钡、0.1~5份碳酸锶、0.1~0.9份五氧化二铌、0.1~0.8份五氧化二锑、16~25份二氧化锆、8~15份改性二氧化钛。
2.根据权利要求1所述的球面体压电陶瓷,其特征在于,所述球面体压电陶瓷由以下重量份原料组成:65~75份四氧化三铅、2~3份氧化镍、1~2份氧化钕、0.1~1份碳酸钡、0.2~2份碳酸锶、0.2~0.7份五氧化二铌、0.2~0.6份五氧化二锑、18~22份二氧化锆、9~14份改性二氧化钛。
3.根据权利要求1所述的球面体压电陶瓷,其特征在于,所述球面体压电陶瓷由以下重量份原料组成:70份四氧化三铅、2.5份氧化镍、1.5份氧化钕、0.5份碳酸钡、0.6份碳酸锶、0.4份五氧化二铌、0.45份五氧化二锑、20份二氧化锆、10份改性二氧化钛。
4.根据权利要求1所述的球面体压电陶瓷,其特征在于,所述改性二氧化钛的制备方法为:将4~8份硝酸银溶在4~8份氨水中,加入6~10份金红石型二氧化钛,超声处理10~30min,过滤,放入球磨机内,加入0.4~1份碳酸钙、0.5~0.9份碳纤维、0.5~1.5份氯化钠、0.4~0.8份二氧化锰、1~2份氧化镁,在1000~1200r/min的转速下研磨30~50min,再与4~6份脱盐水混合均匀,过滤,干燥,研磨至400~600目即得所述改性二氧化钛。
5.一种球面体压电陶瓷的制备方法,其特征在于,包含如下步骤:
(1)按照配比称取原料,将配好的粉料以去离子水和氧化锆球为研磨介质,采用行星球磨机球磨混合;
(2)过滤烘干,将粉料于900~1100℃预烧,预烧后的料体再次用行星球磨机球磨;
(3)再次过滤烘干,在粉料中加入8~12wt%的聚乙烯醇溶液进行造粒;
(4)造粒后装料至模具中,干压成型制成所需尺寸的球面体压电陶瓷坯体,所述模具尺寸为D=21mm,R=22mm,T=1.1mm;
(5)将球面体压电陶瓷坯体装进同球面体压电陶瓷坯体尺寸一致的氧化铝坩埚内,上方再放置质量为30~50g的球面体压电陶瓷坯体,一同装进排胶烧结匣钵内排胶烧结,匣钵尺寸为L=115mm,B=115mm,H=50mm;
(6)排胶烧结完成得到所需球面体压电陶瓷粗糙体,进行抛光,即得所述的球面体压电陶瓷。
6.根据权利要求5所述的球面体压电陶瓷的制备方法,其特征在于,所述步骤(1)中料体:球:水=1:2~4:0.5~1.5。
7.根据权利要求5所述的球面体压电陶瓷的制备方法,其特征在于,所述步骤(1)、(2)中球磨转速为300~400r/min,球磨时间为3~5h。
8.根据权利要求5所述的球面体压电陶瓷的制备方法,其特征在于,所述步骤(3)中聚乙烯醇溶液的质量分数为15~25wt%。
9.根据权利要求5所述的球面体压电陶瓷的制备方法,其特征在于,所述步骤(4)中干压成型压力为10~14MPa,保压时间为4~6秒。
10.根据权利要求5所述的球面体压电陶瓷的制备方法,其特征在于,所述步骤(5)中排胶温度为500~600℃,保温时间为1.5~2.5h;所述烧结温度为1150~1310℃,保温1.5~3h。
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