CN107117958A - 一种钛酸锶压敏陶瓷的制备工艺 - Google Patents

一种钛酸锶压敏陶瓷的制备工艺 Download PDF

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CN107117958A
CN107117958A CN201710324462.2A CN201710324462A CN107117958A CN 107117958 A CN107117958 A CN 107117958A CN 201710324462 A CN201710324462 A CN 201710324462A CN 107117958 A CN107117958 A CN 107117958A
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strontium titanates
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赵大鹏
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Bengbu Harvest Electromechanical Equipment Manufacturing Co Ltd
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Abstract

本发明属于压敏电阻原料制备技术领域，具体涉及一种钛酸锶压敏陶瓷的制备工艺，包括提高配料精度、利用γ辐射源预处理原料，并经过两次混料后，控制各步骤条件，得到产品。本发明相比现有技术具有以下优点：一次混料用60Coγ辐射源辐照，能够使其部分原料提前反应，再通过升温使原料进一步反应，得到晶粒叫大的钛酸锶晶相，在不添加锂盐的条件下降低了烧结温度，能够使晶体微观结构得到明显改善，晶界致密，通过各部条件的控制综合作用，提高产品的主要性能。

Description

一种钛酸锶压敏陶瓷的制备工艺
技术领域
本发明属于压敏电阻原料制备技术领域，具体涉及一种钛酸锶压敏陶瓷的制备工艺。
背景技术
压敏陶瓷最早出现于20世纪30年代，当时以SiC为基料制成供避雷器使用的压敏陶瓷，随着技术的逐渐完善，逐渐出现了以氧化锌为基料的压敏陶瓷和以钛酸锶为基料的多功能压敏陶瓷，其制成的压敏变阻器既具有很强的稳压和瞬态浪涌抑制功能，又具有较强的滤波和消噪功能，但其对电流浪涌的抑制能力低，而且烧结过程要求苛刻，工艺复杂，导致其成本较高，其晶粒的半导体化是在高温还原气氛中实现的，所以，这样的元件在空气中长期使用容易发生老化而使性能蜕变，还限制了其在高压条件下的使用寿命，因此，应当对钛酸锶压敏陶瓷的制备工艺进行进一步研究和完善。
发明内容
本发明的目的是针对现有的问题，提供了一种钛酸锶压敏陶瓷的制备工艺。
本发明是通过以下技术方案实现的：一种钛酸锶压敏陶瓷的制备工艺，包括以下步骤：
（1）使用高精度秤按以下重量份配料：碳酸锶15份、二氧化钛18份、五氧化二铌2.8份、碳酸锰2.2份、氧化镧1.6份；
（2）将一次混料加入相当于其重量2倍质量浓度为16.5%的尿素溶液中，用11.8×1014Bq60Coγ辐射源辐照，剂量率为60Gy/min，吸收剂量为3.2Gy，完成后静置分离出沉淀，用水冲洗干净后烘干，将上述处理后的一次混料：水：球按重量比1:2:3进行球磨6小时；
（3）将球磨好的料在135℃烘干后过150目筛；
（4）以8-10℃/min的升温速度升温，在1100℃保温4小时，然后随炉冷却；
（5）在上述所得混合料里加入以下重量份的配料：钠硼硅玻璃4.6份、氧化铝2.5份、氧化钷0.3份、银0.6份、铜0.1份、镍0.24份，得到二次混料；
（6）将二次混料：水：球按重量比1:1.5:4进行球磨4小时，干燥后加入相当于其重量8%的聚乙烯醇，研磨后搅拌均匀，以65MPa的压力预压成块，将块打碎后过60目筛，其中40%的碎料可过100目筛，得到混合粉料；
（7）在油压机上，用675MPa的压力将混合粉料放入内径为10mm的模具中压制成型，然后在马沸炉中，以6℃/min的升温速度，升至600℃后保持4小时，进行排胶；
（8）将排胶完的中间样放入管式炉中，加入相当于其重量2%的石墨粉，以6-8℃/min的升温速度升温至750℃，保温30粉红后，通入氮气，在1150-1200℃的条件下烧结，在烧结温度下保温3小时，随炉冷却，同时继续通入氮气，直到炉内温度将至800℃后关掉氮气，随炉冷却，完成烧结；
（9）按常规方法上电极后测试相关数据即可。
作为对上述方案的进一步改进，所述高精度秤的称重精度为0.1g。
作为对上述方案的进一步改进，所述上电极的具体操作步骤为：在试样两端涂覆铝电极，用松油醇调节铝浆浓稠度，涂覆完毕后放入电阻炉中，在600℃的条件下保温20分钟，冷却至200℃后将其取出，在空气中自然冷却即可。
作为对上述方案的进一步改进，所述各原料的纯度不低于98%。
本发明相比现有技术具有以下优点：一次混料用60Coγ辐射源辐照，能够使其部分原料提前反应，再通过升温使原料进一步反应，得到晶粒叫大的钛酸锶晶相，在不添加锂盐的条件下降低了烧结温度，能够使晶体微观结构得到明显改善，晶界致密，通过各部条件的控制综合作用，提高产品的主要性能。
具体实施方式
实施例1
一种钛酸锶压敏陶瓷的制备工艺，包括以下步骤：
（1）使用高精度秤按以下重量份配料：碳酸锶15份、二氧化钛18份、五氧化二铌2.8份、碳酸锰2.2份、氧化镧1.6份；
（2）将一次混料加入相当于其重量2倍质量浓度为16.5%的尿素溶液中，用11.8×1014Bq60Coγ辐射源辐照，剂量率为60Gy/min，吸收剂量为3.2Gy，完成后静置分离出沉淀，用水冲洗干净后烘干，将上述处理后的一次混料：水：球按重量比1:2:3进行球磨6小时；
（3）将球磨好的料在135℃烘干后过150目筛；
（4）以8-10℃/min的升温速度升温，在1100℃保温4小时，然后随炉冷却；
（5）在上述所得混合料里加入以下重量份的配料：钠硼硅玻璃4.6份、氧化铝2.5份、氧化钷0.3份、银0.6份、铜0.1份、镍0.24份，得到二次混料；
（6）将二次混料：水：球按重量比1:1.5:4进行球磨4小时，干燥后加入相当于其重量8%的聚乙烯醇，研磨后搅拌均匀，以65MPa的压力预压成块，将块打碎后过60目筛，其中40%的碎料可过100目筛，得到混合粉料；
（7）在油压机上，用675MPa的压力将混合粉料放入内径为10mm的模具中压制成型，然后在马沸炉中，以6℃/min的升温速度，升至600℃后保持4小时，进行排胶；
（8）将排胶完的中间样放入管式炉中，加入相当于其重量2%的石墨粉，以6-8℃/min的升温速度升温至750℃，保温30粉红后，通入氮气，在1150-1200℃的条件下烧结，在烧结温度下保温3小时，随炉冷却，同时继续通入氮气，直到炉内温度将至800℃后关掉氮气，随炉冷却，完成烧结；
（9）在试样两端涂覆铝电极，用松油醇调节铝浆浓稠度，涂覆完毕后放入电阻炉中，在600℃的条件下保温20分钟，冷却至200℃后将其取出，在空气中自然冷却即可，然后测试相关数据即可。
已知现有的钛酸锶陶瓷的性能达到如下水平：非线性系数α在3-35之间，压敏电压在3-250V/mm之间，介电常数达到105，介电损耗达到10-2-10-3，在低电压下具有较大的电容器功能（大于0.01μF），能吸收1000-3000A/cm²的浪涌。
本实施例中不用氢气作还原气氛，得到的钛酸锶压敏陶瓷性能好，压敏电压最低可达到5.36V/mm，非线性系数α最高可达32.5，介电常数最高可达94386.45，介电损耗最低可达0.0194。

Claims (4)

1.一种钛酸锶压敏陶瓷的制备工艺，其特征在于，包括以下步骤：
（1）使用高精度秤按以下重量份配料：碳酸锶15份、二氧化钛18份、五氧化二铌2.8份、碳酸锰2.2份、氧化镧1.6份；
（2）将一次混料加入相当于其重量2倍质量浓度为16.5%的尿素溶液中，用11.8×1014Bq60Coγ辐射源辐照，剂量率为60Gy/min，吸收剂量为3.2Gy，完成后静置分离出沉淀，用水冲洗干净后烘干，将上述处理后的一次混料：水：球按重量比1:2:3进行球磨6小时；
（3）将球磨好的料在135℃烘干后过150目筛；
（4）以8-10℃/min的升温速度升温，在1100℃保温4小时，然后随炉冷却；
（5）在上述所得混合料里加入以下重量份的配料：钠硼硅玻璃4.6份、氧化铝2.5份、氧化钷0.3份、银0.6份、铜0.1份、镍0.24份，得到二次混料；
（6）将二次混料：水：球按重量比1:1.5:4进行球磨4小时，干燥后加入相当于其重量8%的聚乙烯醇，研磨后搅拌均匀，以65MPa的压力预压成块，将块打碎后过60目筛，其中40%的碎料可过100目筛，得到混合粉料；
（7）在油压机上，用675MPa的压力将混合粉料放入内径为10mm的模具中压制成型，然后在马沸炉中，以6℃/min的升温速度，升至600℃后保持4小时，进行排胶；
（8）将排胶完的中间样放入管式炉中，加入相当于其重量2%的石墨粉，以6-8℃/min的升温速度升温至750℃，保温30粉红后，通入氮气，在1150-1200℃的条件下烧结，在烧结温度下保温3小时，随炉冷却，同时继续通入氮气，直到炉内温度将至800℃后关掉氮气，随炉冷却，完成烧结；
（9）按常规方法上电极后测试相关数据即可。
2.如权利要求1所述一种钛酸锶压敏陶瓷的制备工艺，其特征在于，所述高精度秤的称重精度为0.1g。
3.如权利要求1所述一种钛酸锶压敏陶瓷的制备工艺，其特征在于，所述上电极的具体操作步骤为：在试样两端涂覆铝电极，用松油醇调节铝浆浓稠度，涂覆完毕后放入电阻炉中，在600℃的条件下保温20分钟，冷却至200℃后将其取出，在空气中自然冷却即可。
4.如权利要求1所述一种钛酸锶压敏陶瓷的制备工艺，其特征在于，所述各原料的纯度不低于98%。
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CN113185280A (zh) * 2021-04-27 2021-07-30 四川海祥电子科技有限公司 一种高Qf微波介质材料制备方法

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* Cited by examiner, † Cited by third party
Title
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113185280A (zh) * 2021-04-27 2021-07-30 四川海祥电子科技有限公司 一种高Qf微波介质材料制备方法
CN113185280B (zh) * 2021-04-27 2022-06-28 四川海祥电子科技有限公司 一种高Qf微波介质材料制备方法

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