CN106495684A - 一种无铅压电陶瓷材料的制备方法 - Google Patents

一种无铅压电陶瓷材料的制备方法 Download PDF

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CN106495684A
CN106495684A CN201610876103.3A CN201610876103A CN106495684A CN 106495684 A CN106495684 A CN 106495684A CN 201610876103 A CN201610876103 A CN 201610876103A CN 106495684 A CN106495684 A CN 106495684A
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吴蓉蓉
薛荣飞
蒋玉芳
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TRUSYN CHEM-TECH Co Ltd
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Abstract

本发明涉及一种无铅压电陶瓷材料的制备方法,属于压电陶瓷制备技术领域。本发明首先以硝酸铝、异丙醇铝等物质为原料,制备得到水解液,再将其与聚乙烯醇混合,得到前驱体凝胶粉末,接着将Bi2O3、硝酸溶液、碳酸钾等物质进行混合,得到混合液1,再将乙酰丙酮和钛酸四丁酯等物质进行混合,并加入无水乙醇,得到混合液2,并将其与混合液1、前驱体凝胶粉末混合陈化,得到混合凝胶,最后依次对其进行预烧结和煅烧,即可得到无铅压电陶瓷材料。本发明制备的无铅压电陶瓷材料无需高烧结温度,只需120~130℃,能够节约时间和能耗;且无铅压电陶瓷材料居里温度高,居里温度为370~385℃。

Description

一种无铅压电陶瓷材料的制备方法
技术领域
本发明涉及一种无铅压电陶瓷材料的制备方法,属于压电陶瓷制备技术领域。
背景技术
压电陶瓷是一种能够将机械能和电能互相转化的功能陶瓷材料,它的应用十分广泛,而且是应用在与人们的生活密切相关的许多领域,以实现能量转化,传感驱动,频率控制等功能。在能量转换方面,可制造压电点火器、移动X光机电源、炮弹引爆装置、压电变压器、压电拾音器、压电蜂鸣器、压电喇叭,还可以做成金属探伤器、超声清洗、超声医疗、超声切割器。在传感方面,可应用于声纳系统、汽车倒车传感、气象探测、遥测环境保护、家用电器。在驱动方面,可用于精确的控制机构-压电驱动器、谐振器、滤波器等控制装置时决定通讯设备性能的关键器件。随着人们生活水平不断的提高,此类产品的需求量也越来越多。
目前常见的无铅压电陶瓷体系主要有:钛酸钡基、含铋层状结构、钨青铜结构、碱金属铌酸盐系无铅压电陶瓷。这些无机压电陶瓷因为组成和结构不同,其性能也各具特色:钛酸钡基陶瓷材料压电性能中等,但居里温度偏低;含铋层状结构和钨青铜结构陶瓷材料的居里温度高但压电活性低;碱金属铌酸盐系陶瓷则存在难以烧结致密的问题。尽管传统固相合成工艺对提高无铅压电陶瓷压电性能具有一定成效,但是其粉体的制备预烧结温度高,组分不均,且需长时间保温,耗时耗能。
发明内容
本发明所要解决的技术问题:针对无铅压电陶瓷材料预烧结温度高,组分不均,且需长时间保温,耗时耗能的问题,本发明首先以硝酸铝、异丙醇铝等物质为原料,制备得到水解液,再将其与聚乙烯醇混合,得到前驱体凝胶粉末,接着将Bi2O3、硝酸溶液、碳酸钾等物质进行混合,得到混合液1,再将乙酰丙酮和钛酸四丁酯等物质进行混合,并加入无水乙醇,得到混合液2,并将其与混合液1、前驱体凝胶粉末混合陈化,得到混合凝胶,最后依次对其进行预烧结和煅烧,即可得到无铅压电陶瓷材料。本发明制备的无铅压电陶瓷材料无需高预烧结温度,节约时间和能耗,且得到的无铅压电陶瓷材料居里温度和压电活性高,可广泛应用于谐振器、滤波器等控制装置等领域。
为解决上述技术问题,本发明采用的技术方案是:
(1)按重量份数计,分别称量10~15份硝酸铝、45~50份去离子水、5~10份异丙醇铝和15~20份正硅酸乙酯置于烧杯中,在室温下搅拌混合20~24h后,制备得水解液,随后按质量比1:10,将聚乙烯醇与水解液搅拌混合,在85~90℃下水浴加热6~8h后,再在75~80℃下旋转蒸发至干,制备得干燥前驱凝胶,随后将干燥前驱凝胶置于球磨罐中,在250~300r/min球磨3~5h,随后过100~120目筛,制备得前驱体凝胶粉末,备用;
(2)称取1.2~1.3gBi2O3,将其与45~50mL质量分数60%硝酸溶液混合并置于烧杯中,搅拌10~15min,随后将1.2~1.5g碳酸钾、0.2~0.3g碳酸锂和45~50mL冰醋酸添加至烧杯中,在45~50℃下搅拌混合25~30min,制备得混合液1,备用;
(3)按乙酰丙酮与钛酸四丁酯摩尔比1:8,将乙酰丙酮与钛酸四丁酯搅拌混合并置于烧杯中,随后添加乙酰丙酮质量10倍的无水乙醇至烧杯中,在200~300W下超声分散10~15min,制备得混合液2;
(4)按质量比1:3:8,将步骤(1)备用的前驱体凝胶粉末、混合液2和步骤(2)备用混合液1搅拌混合,在室温下陈化6~8h后,用质量分数18%氨水调节pH至2.5~3.0,随后搅拌混合并置于65~70℃下干燥3~5h,收集得混合凝胶;
(5)将上述制备的混合凝胶置于120~130℃马弗炉中预烧结1~2h,随后收集预烧结粉末并置于550~600℃下煅烧1~2h,收集煅烧后的材料,将其移至管式气氛炉中,在温度为600~700℃,氮气气氛下预热25~30min,随后按15℃/min升温至1100~1200℃,保温煅烧1~2h后,静置冷却至室温,碾磨即可制备得无铅压电陶瓷材料。
本发明制备的无铅压电陶瓷材料居里温度为370~385℃,介电损耗为0.3~0.5%,相对介电常数为1340~1450,纵向压电应变常数为252~275PC·N-1,横向压电应变常数为-150~-36PC·N-1
本发明与其他方法相比,有益技术效果是:
(1)本发明制备的无铅压电陶瓷材料无需高预烧结温度,只需120~130℃,能够节约时间和能耗;
(2)本发明制备的无铅压电陶瓷材料居里温度高,居里温度为370~385℃;
(3)本发明制备的无铅压电陶瓷材料制备步骤简单,所需成本低。
具体实施方式
首先按重量份数计,分别称量10~15份硝酸铝、45~50份去离子水、5~10份异丙醇铝和15~20份正硅酸乙酯置于烧杯中,在室温下搅拌混合20~24h后,制备得水解液,随后按质量比1:10,将聚乙烯醇与水解液搅拌混合,在85~90℃下水浴加热6~8h后,再在75~80℃下旋转蒸发至干,制备得干燥前驱凝胶,随后将干燥前驱凝胶置于球磨罐中,在250~300r/min球磨3~5h,随后过100~120目筛,制备得前驱体凝胶粉末,备用;再称取1.2~1.3gBi2O3,将其与45~50mL质量分数60%硝酸溶液混合并置于烧杯中,搅拌10~15min,随后将1.2~1.5g碳酸钾、0.2~0.3g碳酸锂和45~50mL冰醋酸添加至烧杯中,在45~50℃下搅拌混合25~30min,制备得混合液1,备用;按乙酰丙酮与钛酸四丁酯摩尔比1:8,将乙酰丙酮与钛酸四丁酯搅拌混合并置于烧杯中,随后添加乙酰丙酮质量10倍的无水乙醇至烧杯中,在200~300W下超声分散10~15min,制备得混合液2;接着按质量比1:3:8,将备用的前驱体凝胶粉末、混合液2和备用混合液1搅拌混合,在室温下陈化6~8h后,用质量分数18%氨水调节pH至2.5~3.0,随后搅拌混合并置于65~70℃下干燥3~5h,收集得混合凝胶;最后将上述制备的混合凝胶置于120~130℃马弗炉中预烧结1~2h,随后收集预烧结粉末并置于550~600℃下煅烧1~2h,收集煅烧后的材料,将其移至管式气氛炉中,在温度为600~700℃,氮气气氛下预热25~30min,随后按15℃/min升温至1100~1200℃,保温煅烧1~2h后,静置冷却至室温,碾磨即可制备得无铅压电陶瓷材料。
实例1
首先按重量份数计,分别称量15份硝酸铝、50份去离子水、10份异丙醇铝和20份正硅酸乙酯置于烧杯中,在室温下搅拌混合24h后,制备得水解液,随后按质量比1:10,将聚乙烯醇与水解液搅拌混合,在90℃下水浴加热8h后,再在80℃下旋转蒸发至干,制备得干燥前驱凝胶,随后将干燥前驱凝胶置于球磨罐中,在300r/min球磨5h,随后过120目筛,制备得前驱体凝胶粉末,备用;再称取1.3gBi2O3,将其与50mL质量分数60%硝酸溶液混合并置于烧杯中,搅拌15min,随后将1.5g碳酸钾、0.3g碳酸锂和50mL冰醋酸添加至烧杯中,在50℃下搅拌混合30min,制备得混合液1,备用;按乙酰丙酮与钛酸四丁酯摩尔比1:8,将乙酰丙酮与钛酸四丁酯搅拌混合并置于烧杯中,随后添加乙酰丙酮质量10倍的无水乙醇至烧杯中,在300W下超声分散15min,制备得混合液2;接着按质量比1:3:8,将备用的前驱体凝胶粉末、混合液2和备用混合液1搅拌混合,在室温下陈化8h后,用质量分数18%氨水调节pH至3.0,随后搅拌混合并置于70℃下干燥5h,收集得混合凝胶;最后将上述制备的混合凝胶置于130℃马弗炉中预烧结2h,随后收集预烧结粉末并置于600℃下煅烧2h,收集煅烧后的材料,将其移至管式气氛炉中,在温度为700℃,氮气气氛下预热30min,随后按15℃/min升温至1200℃,保温煅烧2h后,静置冷却至室温,碾磨即可制备得无铅压电陶瓷材料。
经检测,本发明制备的无铅压电陶瓷材料居里温度为385℃,介电损耗为0.5%,相对介电常数为1450,纵向压电应变常数为275PC·N-1,横向压电应变常数为-36PC·N-1
实例2
首先按重量份数计,分别称量10份硝酸铝、45份去离子水、5份异丙醇铝和15份正硅酸乙酯置于烧杯中,在室温下搅拌混合20h后,制备得水解液,随后按质量比1:10,将聚乙烯醇与水解液搅拌混合,在85℃下水浴加热6h后,再在75℃下旋转蒸发至干,制备得干燥前驱凝胶,随后将干燥前驱凝胶置于球磨罐中,在250r/min球磨3h,随后过100目筛,制备得前驱体凝胶粉末,备用;再称取1.2gBi2O3,将其与45mL质量分数60%硝酸溶液混合并置于烧杯中,搅拌10min,随后将1.2g碳酸钾、0.2g碳酸锂和45mL冰醋酸添加至烧杯中,在45℃下搅拌混合25min,制备得混合液1,备用;按乙酰丙酮与钛酸四丁酯摩尔比1:8,将乙酰丙酮与钛酸四丁酯搅拌混合并置于烧杯中,随后添加乙酰丙酮质量10倍的无水乙醇至烧杯中,在200W下超声分散10min,制备得混合液2;接着按质量比1:3:8,将备用的前驱体凝胶粉末、混合液2和备用混合液1搅拌混合,在室温下陈化6h后,用质量分数18%氨水调节pH至2.5,随后搅拌混合并置于65℃下干燥3h,收集得混合凝胶;最后将上述制备的混合凝胶置于120℃马弗炉中预烧结1h,随后收集预烧结粉末并置于550℃下煅烧1h,收集煅烧后的材料,将其移至管式气氛炉中,在温度为600℃,氮气气氛下预热25min,随后按15℃/min升温至1100℃,保温煅烧1h后,静置冷却至室温,碾磨即可制备得无铅压电陶瓷材料。 经检测,本发明制备的无铅压电陶瓷材料居里温度为370℃,介电损耗为0.3%,相对介电常数为1340,纵向压电应变常数为252PC·N-1,横向压电应变常数为-150PC·N-1
实例3
首先按重量份数计,分别称量12份硝酸铝、47份去离子水、7份异丙醇铝和17份正硅酸乙酯置于烧杯中,在室温下搅拌混合22h后,制备得水解液,随后按质量比1:10,将聚乙烯醇与水解液搅拌混合,在87℃下水浴加热7h后,再在77℃下旋转蒸发至干,制备得干燥前驱凝胶,随后将干燥前驱凝胶置于球磨罐中,在270r/min球磨4h,随后过110目筛,制备得前驱体凝胶粉末,备用;再称取1.2gBi2O3,将其与47mL质量分数60%硝酸溶液混合并置于烧杯中,搅拌12min,随后将1.3g碳酸钾、0.25g碳酸锂和47mL冰醋酸添加至烧杯中,在47℃下搅拌混合27min,制备得混合液1,备用;按乙酰丙酮与钛酸四丁酯摩尔比1:8,将乙酰丙酮与钛酸四丁酯搅拌混合并置于烧杯中,随后添加乙酰丙酮质量10倍的无水乙醇至烧杯中,在250W下超声分散12min,制备得混合液2;接着按质量比1:3:8,将备用的前驱体凝胶粉末、混合液2和备用混合液1搅拌混合,在室温下陈化7h后,用质量分数18%氨水调节pH至2.7,随后搅拌混合并置于67℃下干燥4h,收集得混合凝胶;最后将上述制备的混合凝胶置于125℃马弗炉中预烧结2h,随后收集预烧结粉末并置于570℃下煅烧1h,收集煅烧后的材料,将其移至管式气氛炉中,在温度为650℃,氮气气氛下预热27min,随后按15℃/min升温至1150℃,保温煅烧1h后,静置冷却至室温,碾磨即可制备得无铅压电陶瓷材料。
经检测,本发明制备的无铅压电陶瓷材料居里温度为375℃,介电损耗为0.4%,相对介电常数为1430,纵向压电应变常数为260PC·N-1,横向压电应变常数为-100PC·N-1

Claims (1)

1.一种无铅压电陶瓷材料的制备方法,其特征在于具体制备步骤为:
(1)按重量份数计,分别称量10~15份硝酸铝、45~50份去离子水、5~10份异丙醇铝和15~20份正硅酸乙酯置于烧杯中,在室温下搅拌混合20~24h后,制备得水解液,随后按质量比1:10,将聚乙烯醇与水解液搅拌混合,在85~90℃下水浴加热6~8h后,再在75~80℃下旋转蒸发至干,制备得干燥前驱凝胶,随后将干燥前驱凝胶置于球磨罐中,在250~300r/min球磨3~5h,随后过100~120目筛,制备得前驱体凝胶粉末,备用;
(2)称取1.2~1.3gBi2O3,将其与45~50mL质量分数60%硝酸溶液混合并置于烧杯中,搅拌10~15min,随后将1.2~1.5g碳酸钾、0.2~0.3g碳酸锂和45~50mL冰醋酸添加至烧杯中,在45~50℃下搅拌混合25~30min,制备得混合液1,备用;
(3)按乙酰丙酮与钛酸四丁酯摩尔比1:8,将乙酰丙酮与钛酸四丁酯搅拌混合并置于烧杯中,随后添加乙酰丙酮质量10倍的无水乙醇至烧杯中,在200~300W下超声分散10~15min,制备得混合液2;
(4)按质量比1:3:8,将步骤(1)备用的前驱体凝胶粉末、混合液2和步骤(2)备用混合液1搅拌混合,在室温下陈化6~8h后,用质量分数18%氨水调节pH至2.5~3.0,随后搅拌混合并置于65~70℃下干燥3~5h,收集得混合凝胶;
(5)将上述制备的混合凝胶置于120~130℃马弗炉中预烧结1~2h,随后收集预烧结粉末并置于550~600℃下煅烧1~2h,收集煅烧后的材料,将其移至管式气氛炉中,在温度为600~700℃,氮气气氛下预热25~30min,随后按15℃/min升温至1100~1200℃,保温煅烧1~2h后,静置冷却至室温,碾磨即可制备得无铅压电陶瓷材料。
CN201610876103.3A 2016-10-08 2016-10-08 一种无铅压电陶瓷材料的制备方法 Pending CN106495684A (zh)

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