CN106892653A - 氧化锌基压敏陶瓷粉体及其制备方法 - Google Patents

氧化锌基压敏陶瓷粉体及其制备方法 Download PDF

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CN106892653A
CN106892653A CN201510954792.0A CN201510954792A CN106892653A CN 106892653 A CN106892653 A CN 106892653A CN 201510954792 A CN201510954792 A CN 201510954792A CN 106892653 A CN106892653 A CN 106892653A
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zinc oxide
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citric acid
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张莹莹
杨殿来
许壮志
薛健
张明
李磊
许成
周岩
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LIAONING PROV ACADEMY OF LIGHT INDUSTRY SCIENCES
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Abstract

一种氧化锌基压敏陶瓷粉体，各组分摩尔量百分比如下：Zn：83.0～92.0％、Bi：6.5～10.0％、Sb：4～8％、Co：1.5～1.8％、Ni：0.01～0.009％、Mn：0.5～1.0％、Cr：0.5～1.1％、Al：0.01～0.09％、Y：1.0～2.0％、Ho：1.0～2.0％、Si：0.5～1.0％、Ba：0.5～1.0％和B：0.3～0.5％。本发明通过两步法柠檬酸凝胶技术在ZnO表面包覆一层柠檬酸层。本发明在粉体合成方法上打破了常规的固相法及常规液相法，而是采用新颖操作简单的两步法柠檬酸凝胶技术方法制备了氧化锌基陶瓷粉体，制得的粉体具有成分均匀、粒度细、分布范围窄、分散性好等优点，进而保证了后续制备压敏电阻器件的高可靠性。

Description

氧化锌基压敏陶瓷粉体及其制备方法
技术领域
本发明涉及一种压敏电阻无源电子器件原材料及其制备方法，尤其是一种氧化锌基压敏陶瓷粉体及其制备方法。
背景技术
氧化锌基压敏陶瓷是以氧化锌为主体，添加若干其他氧化物改性的烧结体材料，由于氧化锌压敏电阻具有非线性系数高、响应时间快、漏电流小、制造成本低廉等优点，广泛应用于电力线路、电子通信、集成电路以及其它领域。压敏电阻主要用于半导体器件的过压保护，在电路中与用电器并联，当工作电压正常时，其电阻值很高，对电路设备几乎没有影响；当工作电压过载时，其阻值急剧降低、分流作用急剧增强，对电子和电器设备的安全起到保护作用。现有的氧化锌压敏电阻具有烧结温度过高，非线性系数小等不足。
ZnO压敏电阻粉体作为压敏电阻器件的主体材料，其传统的制备方法以固相法为主，采用固相法制得的粉体均匀性较差，粉体粒度较大，进而影响了后续器件的稳定性与可靠性。采用常规液相法制得的氧化锌基压敏电阻粉体在均匀性上有了很大的提高，但存在着粉体易团聚、分散性差等缺点。
发明内容
针对上述现有技术的缺点，本发明提供了一种可靠性高的氧化锌基压敏陶瓷粉体及其制备方法。
为实现上述目的，本发明采用的技术方案是：一种氧化锌基压敏陶瓷粉体，各组分摩尔量百分比如下：Zn：83.0～92.0％、Bi：6.5～10.0％、Sb：4～8％、Co：1.5～1.8％、Ni：0.01～0.009％、Mn：0.5～1.0％、Cr：0.5～1.1％、Al：0.01～0.09％、Y：1.0～2.0％、Ho：1.0～2.0％、Si：0.5～1.0％、Ba：0.5～1.0％和B：0.3～0.5％。
一种氧化锌基压敏陶瓷粉体的制备方法，具体步骤为：
(1)按照上述的摩尔百分比，将掺杂剂CO、Mn、Al、Ni、Cr、Y、Ho采用金属盐溶液形式引入，上述每种金属盐形式的掺杂剂分别溶于柠檬酸水溶液中，每一种含有掺杂剂的柠檬酸溶液按顺序加入到ZnO悬浮液中，悬浮溶液为去离子水；将上述混合后的溶液采用锯齿型搅拌器进行强力搅拌12-24h后，进行50-80℃低温烘干，再进行450-500℃低温煅烧，保温时间在2-5小时，得到氧化锌基粉体。
(2)将Ba盐和B盐溶于柠檬酸中，将Si(OEt)4溶于乙醇溶液中，将乙酸锑直接加入柠檬酸中，搅拌30min，将Bi(NO3)3·5H2O加入到柠檬酸中，通过氨水来调节溶液的PH值至7左右，得到Bi的盐溶液。
(3)将步骤(1)获得的氧化锌基粉体加入到步骤(2)制得的Bi的盐溶液中，搅拌至均匀后，将Ba、B、Si的柠檬酸溶液迅速加入到上述溶液中搅拌12-24h，后采用真空冷冻干燥技术进行干燥，最后进行450-500℃低温煅烧，得到外面包覆掺杂剂的氧化锌基压敏陶瓷粉体；再向粉体中添加占粉体质量为5％～10％的聚乙烯醇(PVA)后造粒、压片成型。成型后的圆片经过2°/min升温至600℃进行排胶处理，在950～1150℃温度下烧结成瓷。
本发明在粉体合成方法上打破了常规的固相法及常规液相法，而是采用新颖操作简单的两步法柠檬酸凝胶技术方法制备了氧化锌基陶瓷粉体，制得的粉体具有成分均匀、粒度细、分布范围窄、分散性好等优点，进而保证了后续制备压敏电阻器件的高可靠性。
具体实施方式
实施例1
(1)将CO(摩尔量百分比1.5％)、Mn(摩尔量百分比0.5％)、Al(摩尔量百分比0.05％)、Ni(摩尔量百分比0.05％)、Cr(摩尔量百分比1.1％)、Y(摩尔量百分比1.0％)、Ho(摩尔量百分比1.0％)等掺杂剂均采用金属盐溶液形式引入，上述每种金属盐形式的掺杂剂分别溶于柠檬酸水溶液中，每一种含有掺杂剂的柠檬酸溶液按顺序加入到ZnO(摩尔量百分比83％)悬浮液中，悬浮溶液为去离子水。将上述混合后的溶液采用锯齿型搅拌器进行强力搅拌12h，再进行60℃低温烘干后，进行450℃低温煅烧，保温时间为3小时，得到氧化锌基粉体。
(2)将Ba盐(摩尔量百分比0.5％)和B盐(摩尔量百分比0.3％)溶于柠檬酸中；将Si(OEt)4(摩尔量百分比0.5％)溶于乙醇溶液中；将乙酸锑(摩尔量百分比4％)直接加入柠檬酸中，搅拌30min；将Bi(NO3)3·5H2O(摩尔量百分比6.5％)加入到柠檬酸中，通过氨水来调节溶液的PH至7左右，得到Bi的盐溶液。
(3)将第一步获得的掺杂后氧化锌基粉体加入到Bi的盐溶液中，搅拌至均匀后，将Ba、B、Si的柠檬酸溶液迅速加入到上述溶液中搅拌20h，然后采用真空冷冻干燥技术进行干燥，最后进行450℃低温煅烧，得到外面包覆掺杂剂的氧化锌基压敏陶瓷粉体。再向粉体中添加占粉体质量为5％的PVA后造粒、压片成型。压制成型后的圆片经过2°/min升温至600℃进行排胶处理，进行1150℃烧结成瓷，在进行热处理后，进行表面电极涂覆进行电学性能测试。电位梯度高达700V/mm，漏电流为1.5μA，非线性系数为60。
实施例2
(1)将CO(摩尔量百分比0.9％)、Mn(摩尔量百分比0.3％)、Al(摩尔量百分比0.02％)、Ni(摩尔量百分比0.03％)、Cr(摩尔量百分比0.8％)、Y(摩尔量百分比0.2％)、Ho(摩尔量百分比0.35％)等掺杂剂均采用金属盐溶液形式引入，上述每种金属盐形式的掺杂剂分别溶于柠檬酸水溶液中，每一种含有掺杂剂的柠檬酸溶液按顺序加入到ZnO(摩尔量百分比87％)悬浮液中，悬浮溶液为去离子水。将上述混合后的溶液采用锯齿型搅拌器进行强力搅拌20h，再进行70℃低温烘干后，进行470℃低温煅烧，保温时间为2小时，得到氧化锌基粉体。
(2)将Ba盐(摩尔量百分比0.4％)和B盐(摩尔量百分比0.2％)溶于柠檬酸中；将Si(OEt)4(摩尔量百分比0.3％)溶于乙醇溶液中；将乙酸锑(摩尔量百分比3.5％)直接加入柠檬酸中，搅拌30min；将Bi(NO3)3·5H2O(摩尔量百分比6.0％)加入到柠檬酸中，通过氨水来调节溶液的PH至7左右，得到Bi的盐溶液。
(3)将第一步获得的掺杂后氧化锌基粉体加入到Bi的盐溶液中，搅拌至均匀后，将Ba、B、Si的柠檬酸溶液迅速加入到上述溶液中搅拌24h，然后采用真空冷冻干燥技术进行干燥，最后进行460℃低温煅烧，得到外面包覆掺杂剂的氧化锌基压敏陶瓷粉体。再向粉体中添加占粉体质量为8％的PVA后造粒、压片成型。压制成型后的圆片经过2°/min升温至600℃进行排胶处理，进行960℃烧结成瓷，在进行热处理后，进行表面电极涂覆进行电学性能测试。电位梯度高达680V/mm，漏电流为1.3μA，非线性系数为56。
实施例3
(1)CO(摩尔量百分比1.0％)、Mn(摩尔量百分比0.5％)、Al(摩尔量百分比0.05％)、Ni(摩尔量百分比0.05％)、Cr(摩尔量百分比0.6％)、Y(摩尔量百分比0.2％)、Ho(摩尔量百分比0.3％)等掺杂剂均采用金属盐溶液形式引入，上述每种金属盐形式的掺杂剂分别溶于柠檬酸水溶液中，每一种含有掺杂剂的柠檬酸溶液按顺序加入到ZnO(摩尔量百分比90％)悬浮液中，悬浮溶液为去离子水。将上述混合后的溶液采用锯齿型搅拌器进行强力搅拌22h，再进行75℃低温烘干后，进行480℃低温煅烧，保温时间为4小时，得到氧化锌基粉体。
(2)将Ba盐(摩尔量百分比0.3％)和B盐(摩尔量百分比0.1％)溶于柠檬酸中；将Si(OEt)4(摩尔量百分比0.4％)溶于乙醇溶液中；将乙酸锑(摩尔量百分比2％)直接加入柠檬酸中，搅拌30min；将Bi(NO3)3·5H2O(摩尔量百分比4.5％)加入到柠檬酸中，通过氨水来调节溶液的PH至7左右，得到Bi的盐溶液。
(3)将第一步获得的掺杂后氧化锌基粉体加入到Bi的盐溶液中，搅拌至均匀后，将Ba、B、Si的柠檬酸溶液迅速加入到上述溶液中搅拌18h，然后采用真空冷冻干燥技术进行干燥，最后进行480℃低温煅烧，得到外面包覆掺杂剂的氧化锌基压敏陶瓷粉体。再向粉体中添加占粉体质量为10％的PVA后造粒、压片成型。压制成型后的圆片经过2°/min升温至600℃进行排胶处理，进行950℃烧结成瓷，在进行热处理后，进行表面电极涂覆进行电学性能测试。电位梯度高达650V/mm，漏电流为1.4μA，非线性系数为62。

Claims (2)

1.一种氧化锌基压敏陶瓷粉体，其特征在于，各组分摩尔量百分比如下：Zn：83.0～92.0％、Bi：6.5～10.0％、Sb：4～8％、Co：1.5～1.8％、Ni：0.01～0.009％、Mn：0.5～1.0％、Cr：0.5～1.1％、Al：0.01～0.09％、Y：1.0～2.0％、Ho：1.0～2.0％、Si：0.5～1.0％、Ba：0.5～1.0％和B：0.3～0.5％。
2.如权利要求1所述的氧化锌基压敏陶瓷粉体的制备方法，其特征在于，具体步骤为：
(1)按照权利要求1所述的摩尔百分比，将掺杂剂CO、Mn、Al、Ni、Cr、Y、Ho采用金属盐溶液形式引入，上述每种金属盐形式的掺杂剂分别溶于柠檬酸水溶液中，每一种含有掺杂剂的柠檬酸溶液按顺序加入到ZnO悬浮液中，悬浮溶液为去离子水；将上述混合后的溶液采用锯齿型搅拌器进行强力搅拌12-24h后，进行50-80℃低温烘干，再进行450-500℃低温煅烧，保温时间在2-5小时，得到氧化锌基粉体；
(2)将Ba盐和B盐溶于柠檬酸中，将Si(OEt)4溶于乙醇溶液中，将乙酸锑直接加入柠檬酸中，搅拌30min，将Bi(NO3)3·5H2O加入到柠檬酸中，通过氨水来调节溶液的PH值至7左右，得到Bi的盐溶液；
(3)将步骤(1)获得的氧化锌基粉体加入到步骤(2)制得的Bi的盐溶液中，搅拌至均匀后，将Ba、B、Si的柠檬酸溶液迅速加入到上述溶液中搅拌12-24h，后采用真空冷冻干燥技术进行干燥，最后进行450-500℃低温煅烧，得到外面包覆掺杂剂的氧化锌基压敏陶瓷粉体；再向粉体中添加占粉体质量为5％～10％的％聚乙烯醇后造粒、压片成型，成型后的圆片经过2°/min升温至600℃进行排胶处理，在950～1150℃温度下烧结成瓷。
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