CN112174659B - 一种钛酸锶压敏电阻及其制备方法 - Google Patents

一种钛酸锶压敏电阻及其制备方法 Download PDF

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CN112174659B
CN112174659B CN202011071967.0A CN202011071967A CN112174659B CN 112174659 B CN112174659 B CN 112174659B CN 202011071967 A CN202011071967 A CN 202011071967A CN 112174659 B CN112174659 B CN 112174659B
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strontium titanate
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furnace
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piezoresistor
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王疆瑛
张景基
刘亚丕
杜汇伟
朱泽洁
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Xinchang China Metrology University Enterprise Innovation Research Institute Co ltd
China Jiliang University
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Abstract

本发明创造提供了一种钛酸锶压敏电阻,其成分为:Sr1‑x‑y‑z TiO3+x(CeO2+Nb2O5)+y(ZnO+1/2NaCO3)+zSiO2,其中x=0.1‑0.5mol%,y=0.2‑0.8mol%,z=0.2‑0.9mol%。制备时,先将称量氯化锶、氯化钛加入盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在105‑130℃烘干,然后,在750℃‑850℃热分解3‑8小时,得到钛酸锶粉体材料;将得到的钛酸锶粉体与x(CeO2+Nb2O5)+y(ZnO+1/2NaCO3)+zSiO2混合球磨6‑12小时,在110℃‑150℃烘干,冲压成片;将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中。本发明创造中粉料直接干压成型,不加粘结剂,不需在进行高温排胶;真空烧结气氛代替气氛炉烧结,氧化烧结过程在空气中进行,实验更加安全,工艺性能好、简单和产品质量容易控制。

Description

一种钛酸锶压敏电阻及其制备方法
技术领域
本发明属于电子信息工程技术领域,具体涉及一种钛酸锶压敏电阻及其制备方法。
背景技术
随着我国工业生产的快速发展,集成、大规模集成电路在电子设备中的广泛使用,电子元件和设备也日益向微型、轻量、集成、多功能、高可靠高稳定性方向发展,这要求对低压化的微集成装置加强保护。压敏陶瓷可以用于抑制电压浪涌和过电压保护,并且普遍的应用于在航空、航天、电力、国防、交通和家用电器等各种领域。由于钛酸锶(SrTiO3)陶瓷既具有较大的介电常数,又具有相对较高的非线性系数与较低的压敏电压,所以它在低压领域的应用前景是不能够被取代的。SrTiO3压敏电阻器具有电容-压敏双功能特性,优异的消噪作用和过电压保护功能,可应用于各类电子设备和电子系统中,大大提高电子设备和电子系统的电磁兼容性、可靠性及寿命。在实际应用中的研究价值日益增加。
发明内容
本发明的目的是提供一种钛酸锶压敏电阻及其制备方法。所提供的钛酸锶压敏电阻其成分为:Sr1-x-y-zTiO3+x(CeO2+Nb2O5)+y(ZnO+1/2NaCO3)+zSiO2,其中x=0.1-0.5mol%,y=0.2-0.8mol%,z=0.2—0.9mol%。
一种钛酸锶压敏电阻的制备方法,包括以下步骤:,
a)将称量氯化锶(SrCl4)、氯化钛(TiCl4)加入(HCl)盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在105-130℃烘干,然后,在750℃-850℃热分解,得到钛酸锶(Sr1-x-y-zTiO3)粉体材料。
b)将得到的钛酸锶(Sr1-x-y-zTiO3)粉体与x(CeO2+Nb2O5)+y(ZnO+1/2NaCO3)+zSiO2混合球磨6-12小时,在110℃-150℃烘干,冲压成Φ8mm,厚度1.0mm的圆片。
c)将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中,在真空气氛下,在温度1250-1500℃,保温4-8小时,然后随炉自然冷却。将冷却后的样品取出并放入马弗炉或箱式电阻炉中,在800-1000℃氧化温度下保温20-30min,随后随炉自然冷却。经两面研磨,超声波清洗,烘干,将清洗抛光后的样品的上下两个表面均匀的涂覆导电银装然后放入马弗炉中于550℃保温5分钟,随后随炉自然冷却,得到钛酸锶压敏电阻,压敏电压V10mA=4-7V,非线性指数α=4-5,损耗系数tgδ=0.02-0.03,电容55-70nF。
本发明具有以下主要特点:
粉料直接干压成型,不加入粘结剂,不需要在进行高温排胶;真空烧结气氛代替气氛炉烧结,氧化烧结过程在空气中进行,实验更加安全简练,具有制备方法工艺性能好、简单和产品质量容易控制。
具体实施方式
实施例1
根据钛酸锶压敏电阻成分为:
Sr0.98TiO3+0.5mol%(CeO2+Nb2O5)+0.6mol%(ZnO+1/2NaCO3)+0.9mol%SiO2
钛酸锶压敏电阻的制备方法,包括以下步骤:,
a)一种钛酸锶(Sr0.98TiO3)粉体材料的制备
按照实施例1要求的配比,将称量氯化锶(SrCl4)、氯化钛(TiCl4)加入(HCl)盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在110℃烘干,然后,在800℃热分解4小时,得到钛酸锶(Sr0.98TiO3)粉体材料。
b)将得到的钛酸锶(Sr0.98TiO3)粉体与0.6mol%(ZnO+1/2NaCO3)+0.9mol%SiO2混合球磨8小时,在120℃烘干,冲压成Φ8mm,厚度1.0mm的圆片。
c)将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中,在真空气氛下,在温度1350℃,保温4小时,然后随炉自然冷却。将冷却后的样品取出并放入马弗炉或箱式电阻炉中,在900℃氧化温度下保温30min,随后随炉自然冷却。经两面研磨,超声波清洗,烘干,将清洗抛光后的样品的上下两个表面均匀的涂覆导电银装然后放入马弗炉中于550℃保温5分钟,随后随炉自然冷却,得到钛酸锶压敏电阻,压敏电压V10mA=4.2V,非线性指数α=4,损耗系数tgδ=0.02,电容68nF。
实施例2
根据钛酸锶压敏电阻成分为:
Sr0.988TiO3+0.3mol%(CeO2+Nb2O5)+0.4mol%(ZnO+1/2NaCO3)+0.5mol%SiO2
钛酸锶压敏电阻的制备方法,包括以下步骤:,
b)一种钛酸锶(Sr0.988TiO3)粉体材料的制备
按配比,将称量氯化锶(SrCl4)、氯化钛(TiCl4)加入(HCl)盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在110℃烘干,然后,在850℃热分解6小时,得到钛酸锶(Sr0.98TiO3)粉体材料。
b)将得到的钛酸锶(Sr0.98TiO3)粉体与0.3mol%(CeO2+Nb2O5)+0.4mol%(ZnO+1/2NaCO3)+
0.5mol%SiO2混合球磨10小时,在120℃烘干,冲压成Φ8mm,厚度1.0mm的圆片。
c)将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中,在真空气氛下,在温度1400℃,保温6小时,然后随炉自然冷却。将冷却后的样品取出并放入马弗炉或箱式电阻炉中,在950℃氧化温度下保温20min,随后随炉自然冷却。经两面研磨,超声波清洗,烘干,将清洗抛光后的样品的上下两个表面均匀的涂覆导电银装然后放入马弗炉中于550℃保温5分钟,随后随炉自然冷却,得到钛酸锶压敏电阻,压敏电压V10mA=4.5V,非线性指数α=5,损耗系数tgδ=0.02,电容64nF。
实施例3
根据钛酸锶压敏电阻成分为:
Sr0.984TiO3+0.5mol%(CeO2+Nb2O5)+0.5mol%(ZnO+1/2NaCO3)+0.6mol%SiO2
钛酸锶压敏电阻的制备方法,包括以下步骤:
c)一种钛酸锶(Sr0.988TiO3)粉体材料的制备
按配比,将称量氯化锶(SrCl4)、氯化钛(TiCl4)加入(HCl)盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在110℃烘干,然后,在850℃热分解6小时,得到钛酸锶(Sr0.984TiO3)粉体材料。
b)将得到的钛酸锶(Sr0.984TiO3)粉体与0.5mol%(CeO2+Nb2O5)+
0.5mol%(ZnO+1/2NaCO3)+0.6mol%SiO2混合球磨10小时,在120℃烘干,冲压成Φ8mm,厚度1.0mm的圆片。
c)将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中,在真空气氛下,在温度1350℃,保温8小时,然后随炉自然冷却。将冷却后的样品取出并放入马弗炉或箱式电阻炉中,在900℃氧化温度下保温30min,随后随炉自然冷却。经两面研磨,超声波清洗,烘干,将清洗抛光后的样品的上下两个表面均匀的涂覆导电银装然后放入马弗炉中于550℃保温5分钟,随后随炉自然冷却,得到钛酸锶压敏电阻,压敏电压V10mA=4.7V,非线性指数α=4.5,损耗系数tgδ=0.02,电容61nF。。
实施例4
根据钛酸锶压敏电阻成分为:
Sr0.99TiO3+0.3mol%(CeO2+Nb2O5)+0.3mol%(ZnO+1/2NaCO3)+0.4mol%SiO2
钛酸锶压敏电阻的制备方法,包括以下步骤:,
d)一种钛酸锶(Sr0.99TiO3)粉体材料的制备
按配比,将称量氯化锶(SrCl4)、氯化钛(TiCl4)加入(HCl)盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在120℃烘干,然后,在900℃热分解4小时,得到钛酸锶(Sr0.99TiO3)粉体材料。
b)将得到的钛酸锶(Sr0.99TiO3)粉体与0.3mol%(CeO2+Nb2O5)+0.3mol%(ZnO+1/2NaCO3)+
0.4mol%SiO2混合球磨10小时,在130℃烘干,冲压成Φ8mm,厚度1.0mm的圆片。
c)将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中,在真空气氛下,在温度1400℃,保温4小时,然后随炉自然冷却。将冷却后的样品取出并放入马弗炉或箱式电阻炉中,在930℃氧化温度下保温30min,随后随炉自然冷却。经两面研磨,超声波清洗,烘干,将清洗抛光后的样品的上下两个表面均匀的涂覆导电银装然后放入马弗炉中于550℃保温5分钟,随后随炉自然冷却,得到钛酸锶压敏电阻,压敏电压V10mA=5.1V,非线性指数α=5,损耗系数tgδ=0.03,电容58nF。

Claims (1)

1.一种钛酸锶压敏电阻的制备方法,其特征在于,包括以下步骤:
a)将称量氯化锶、氯化钛加入盐酸和水溶液,搅拌加热60℃,加入等摩尔量的草酸和少量无水乙醇的水溶液,用盐酸调成PH值为1,混合沉淀,清洗过滤,得到沉淀物,将沉淀物在105-130℃烘干,然后,在750℃-850℃热分解3-8小时,得到钛酸锶粉体材料;
b)将得到的钛酸锶粉体与x(CeO2+Nb2O5)+y(ZnO+1/2NaCO3)+zSiO2混合球磨6-12小时,在110℃-150℃烘干,冲压成Φ8mm,厚度1.0mm的圆片;
c)将成型后的样品放在刚玉方舟中,然后放入真空烧结炉中,在真空气氛下,在温度1250-1450℃,保温4-8小时,然后随炉自然冷却;将冷却后的样品取出并放入马弗炉或箱式电阻炉中,在800-1000℃氧化温度下保温20-30min,随后随炉自然冷却;
经两面研磨,超声波清洗,烘干,将清洗抛光后的样品的上下两个表面均匀的涂覆导电银装然后放入马弗炉中于550℃保温5分钟,随后随炉自然冷却,得到钛酸锶压敏电阻,压敏电压V10mA=4-7V,非线性指数α=4-5,损耗系数tgδ=0.02-0.03,电容55-70nF;
所述钛酸锶压敏电阻的成分为:Sr1-x-y-z TiO3+x(CeO2+Nb2O5)+y(ZnO+1/2Na CO3)+zSiO2,其中x=0.1-0.5mol%,y=0.2-0.8mol%,z=0.2-0.9mol%。
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