CN107473731B - 一种高能量型压敏电阻及其制造方法 - Google Patents

一种高能量型压敏电阻及其制造方法 Download PDF

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CN107473731B
CN107473731B CN201710737800.5A CN201710737800A CN107473731B CN 107473731 B CN107473731 B CN 107473731B CN 201710737800 A CN201710737800 A CN 201710737800A CN 107473731 B CN107473731 B CN 107473731B
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CN107473731A (zh
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覃远东
梁自伟
栗满谦
朱晓玲
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Guangxi New Future Information Industry Co ltd
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Abstract

本发明主要公开了一种高能量型压敏电阻及其制造方法。该压敏电阻以ZnO为主体，再添加主添加剂预合成超细粉体以及配置好的H3BO3、Al(NO3)·9H2O、AgNO3、Ba(CH3COO)2的混合溶液制备而成。制备方法是采用传统的固相合成法将主添加剂粉料煅烧进行预合成，然后粉碎，并磨细，形成主添加剂预合成超细粉体，然后再与ZnO粉料、配置好的混合溶液一起球磨混合、分散消泡、喷雾造粒、干压成型、排胶、烧结等工序，得到烧结好的瓷片，然后将烧结好的瓷片回火、丝网印刷银电极、还原、焊接、包封，即得到一种高能量型压敏电阻。本发明所制备的压敏电阻烧结温度低，能量密度高，抗老化性能好，耐组合波能力强。

Description

一种高能量型压敏电阻及其制造方法
技术领域
本发明涉及的是一种高能量型压敏电阻及其制造方法，属于压敏电阻制造技术领域。
背景技术
压敏电阻由于具有造价低廉、非欧姆特性优良、响应时间快、漏电流小、通流能量大、能量密度高等优点作为关键保护器件被广泛应用于通讯设备、电力、电器、避雷领域，市场前景十分广阔。随着电子信息技术的迅速发展，人们对压敏电阻的大电流处理和能量吸收能力提出了更高的要求，这一直是科学家们研究的重点和热点，近年来科学家们相继发明了一系列提升产品能量的方法和高能量型的压敏电阻产品，如专利申请号为201410636690.X，高能高电位型氧化锌压敏电阻材料的制备工艺，专利申请号为200910049087.0，高能型氧化锌压敏电阻复合粉体及该压敏电阻的制造方法，专利号为201210554024.2，一种高焦耳型压敏电阻及其制备方法，专利申请号为201510309880.5，一种氧化锌压敏电阻陶瓷及其制备方法等。这些专利在能量型压敏电阻产品的性能提高取得了较大突破和进步，但是还不能够满足日益增长的客户对产品的性能需求，因此从产品的本征结构出发，在材料配方改进和工艺改进方面还有很大的技术突破空间。
发明内容
本发明的目的在于提供一种高能量型压敏电阻及其制造方法，提出了利用主添加剂预合成超细粉体替代主添加剂原材料掺杂，可以有效的克服主添加剂原材料由于密度、粒度分布不同，导致在制备浆料过程中引起的沉降速度不同，从而影响ZnO压敏电阻造粒颗粒成分的均匀性，进一步影响瓷体结构的均匀性和瓷体缺陷分布均匀性，最终影响压敏电阻产品能量耐受能力这一现有技术的不足，研制出了一种高能量型压敏电阻及其制造方法。
为了实现上述目的，本发明采取了如下技术方案：一种高能量型压敏电阻，主要由下述摩尔百分比的分析纯原料制备而成：ZnO∶Bi2O3∶Co3O4∶Sb2O3∶MnCO3∶Ni2O3∶ZrO2∶Y2O3∶SiO2∶SnO2∶MgO∶Nb2O5∶H3BO3∶Al(NO3)3·9H2O∶AgNO3∶Ba(CH3COO)2等于96.5%~97.5%∶0.5%~0.65%∶0.3%~0.5%∶0.5%~1.5%∶0.4%~0.5%∶0.35%~0.45%∶0.05%~0.07%∶0.05%~0.1%∶0.05%~0.1%∶0.05%~0.12%∶0.1%~0.3%∶0.01%~0.2%∶0.015%~0.025%∶0.004%~0.006%∶0.01%~0.015%∶0.005%~0.05%；
使用上述原料制造高能量型压敏电阻的步骤如下：
（1）首先将分析纯原料H3BO3、Al(NO3)3·9H2O、AgNO3、Ba(CH3COO)2按摩尔百分比H3BO3∶Al(NO3)3·9H2O∶AgNO3∶Ba(CH3COO)2等于0.015%~0.025%∶0.004%~0.006%∶0.01%~0.015%∶0.005%~0.05%称量好，置入烧杯中，加入去离子水，使之完全溶解，即得到混合溶液，备用；其中H3BO3、Al(NO3)3·9H2O、AgNO3、Ba(CH3COO)2的总重量与去离子水的重量比为1∶10~20；
（2）将分析纯原料Bi2O3、Co3O4、Sb2O3、MnCO3、Ni2O3、ZrO2、Y2O3、SiO2、SnO2、MgO、Nb2O5按摩尔百分比Bi2O3∶Co3O4∶Sb2O3∶MnCO3∶Ni2O3∶ZrO2∶Y2O3∶SiO2∶SnO2∶MgO∶Nb2O5等于0.5%~0.65%∶0.3%~0.5%∶0.5%~1.5%∶0.4%~0.5%∶0.35%~0.45%∶0.05%~0.07%∶0.05%~0.1%∶0.05%~0.1%∶0.05%~0.12%∶0.1%~0.3%∶0.01%~0.2%称量好，置入搅拌球磨罐中，加入锆球、去离子水和分散剂，湿式球磨混合12~24小时，滤出锆球，得到主添加剂混合浆料，然后喷雾造粒，即得到主添加剂造粒粉料颗粒；其中，上述主添加剂Bi2O3、Co3O4、Sb2O3、MnCO3、Ni2O3、ZrO2、Y2O3、SiO2、SnO2、MgO、Nb2O5的总重量、锆球、去离子水、分散剂的重量比为1∶3~4∶1~2∶0.01~0.03；所述分散剂指的是铵盐类阳离子表面活性剂；
（3）将步骤（2）中的主添加剂造粒粉料颗粒置入匣钵中，700oC~900 oC条件下煅烧1~4小时，得到主添加剂预合成粉料颗粒；
（4）将步骤（3）中的主添加剂预合成粉料颗粒粉碎，然后置入球磨罐中，加入锆球、去离子水，湿式球磨混合3~8小时，滤出锆球，即得到主添加剂超细粉体浆料；其中，主添加剂预合成粉料颗粒、锆球、去离子水的重量比为1∶3~4∶1~2；
（5）取去离子水、分散剂、硬脂酸、无水乙醇、工业优级ZnO粉料依次置入乳化混合罐中，湿式乳化混合20分钟~40分钟，再依次加入步骤（4）中的主添加剂超细粉体浆料、步骤（1）中的混合溶液，湿式乳化混合0.5~2小时，再添加粘结剂和消泡剂，继续乳化混合3~5小时，制成喷雾浆料备用；其中，去离子水、分散剂、硬脂酸、无水乙醇、粘结剂、消泡剂、工业优级ZnO粉料的重量比为0.3～0.55 : 0.01～0.05 : 0.002～0.01 : 0.002～0.01 : 0.1～0.5 : 0.001～0.004 : 1；上述工业优级ZnO粉料与步骤（2）中的Bi2O3、Co3O4、Sb2O3、MnCO3、Ni2O3、ZrO2、Y2O3、SiO2、SnO2、MgO、Nb2O5和步骤（1）中的H3BO3、Al(NO3)3·9H2O、AgNO3、Ba(CH3COO)2的摩尔百分比为96.5%~97.5%∶0.5%~0.65%∶0.3%~0.5%∶0.5%~1.5%∶0.4%~0.5%∶0.35%~0.45%∶0.05%~0.07%∶0.05%~0.1%∶0.05%~0.1%∶0.05%~0.12%∶0.1%~0.3%∶0.01%~0.2%∶0.015%~0.025%∶0.004%~0.006%∶0.01%~0.015%∶0.005%~0.05%；上述粘结剂是质量浓度为5%的聚乙烯醇水溶液，上述分散剂是铵盐类阳离子表面活性剂，上述消泡剂是纯度为99%以上的磷酸三丁酯或正辛醇；
（6）将步骤（5）中的喷雾浆料喷雾干燥成含水量0.35%～0.55%的造粒粉料；
（7）将造粒粉料按常规方法干压成型，制成陶瓷生坯体；
（8）将陶瓷生坯体经550℃～650℃排胶后进行烧结，烧结温度为1050℃～1250℃，得到烧结好的瓷片；
（9）然后将烧结好的瓷片550℃～850℃回火、丝网印刷银电极、还原、焊接、包封，即得到一种高能量型压敏电阻。所述印银采用的工艺是常规丝网印刷工艺，印银所用的银电极浆料含银量为80%。
采取上述措施的本发明具有以下特点：
1.本发明所采用的产品配方是利用主添加剂预合成超细粉体替代主添加剂原材料掺杂，可以有效的克服主添加剂原材料由于密度、粒度分布不同，导致在制备浆料过程中引起的沉降速度不同，从而影响ZnO压敏电阻造粒颗粒成分的均匀性，进一步影响瓷体结构的均匀性和瓷体缺陷分布均匀性，最终影响压敏电阻产品的能量耐受能力这一现有技术的不足，从而实现该产品的高通流、高能量耐受能力；
2. 本发明所采用的产品配方是利用主添加剂预合成超细粉体替代主添加剂原材料掺杂，可以有效的降低瓷体烧结温度；
3.本发明所采用的产品配方未添加任何的Pb、Cr元素，绿色环保；
4.本发明产品压敏电压梯度200～230V/mm，压敏电压稳定，通流能力达到9.5 kA/cm2，脉冲能量耐受能力达到950J/cm3，而且耐组合波能力强，抗老化性能好；
5.本发明的制备方法工艺简单，制造成本低，并且能够实现大批量生产。
具体实施方式
下面结合实施例对本发明作进一步描述。需要指出的是，按照本发明的技术方案，下述实施例还可以举出许多，根据申请人大量的实验结果证明，在本发明的权利要求书所提出的范围，均可以达到本发明的目的。
实施例1
一种高能量型压敏电阻的制备方法按下列步骤进行：
1. 首先称量分析纯原料H3BO3 30克、Al(NO3)3·9H2O 46.858克、AgNO3 59.262克、Ba(CH3COO)2 66.666克置入烧杯中，加入2.5千克去离子水，使之完全溶解，即得到混合溶液；
2. 然后称量分析纯原料Bi2O3 6861.6克、Co3O4 3060.5克、Sb2O3 6957.3克、MnCO31337.2克、Ni2O3 1652.7克、ZrO2 200.5克、Y2O3 573.3克、SiO2 152.5克、SnO2 382.7克、MgO106.7克、Nb2O5 133.3克，置入搅拌球磨罐中，加入80千克锆球、30千克去离子水和430克分散剂，湿式球磨混合12小时，滤出锆球，得到主添加剂混合浆料，然后在添加剂喷雾干燥塔喷雾干燥成含水量小于0.3%的主添加剂造粒粉料颗粒；
3. 将步骤2中的主添加剂造粒粉料颗粒置入匣钵中，750oC条件下煅烧2小时，升温速率2.5 oC/min，随炉降温，得到主添加剂预合成粉料颗粒；
4. 将步骤3中的主添加剂预合成粉料颗粒粉碎，然后置入球磨罐中，加入80千克锆球、30千克去离子水，湿式球磨混合4小时，滤出锆球，即得到主添加剂超细粉体浆料；
5. 称量去离子水70千克、分散剂2.5千克、硬脂酸500克、无水乙醇1.5千克、工业优级ZnO粉料200千克依次置入乳化混合罐中，湿式乳化混合20分钟~40分钟，再依次加入步骤4中的主添加剂超细粉体浆料、步骤1中的混合溶液，湿式乳化混合0.5~2小时，再添加55千克质量浓度为5%的聚乙烯醇水溶液和0.8千克纯度为99%以上的磷酸三丁酯，继续乳化混合3小时，制成喷雾浆料备用；
6. 采用浆料喷雾干燥塔将步骤5中的喷雾浆料喷雾干燥成含水量0.35%～0.55%的造粒粉料；
7. 将造粒粉料按常规方法干压成型，制成直径16.6毫米、厚度3.75~3.85毫米，重量2.69~2.77克的陶瓷生坯体；
8. 将步骤7中的陶瓷生坯体在550℃条件下保温4小时排胶，排胶后进行烧结，烧结温度为1090℃，保温3小时，得到烧结好的瓷片；
9. 然后将烧结好的瓷片800℃回火2小时、采用含银量为80%的银电极浆料丝网印刷银电极，自由边为0.5毫米、还原、焊接、包封，即得到一种高能量型压敏电阻。
实施例2
一种高能量型压敏电阻的制备方法按下列步骤进行：
1. 首先称量分析纯原料H3BO3 29.927克、Al(NO3)3·9H2O 46.744克、AgNO3 59.118克、Ba(CH3COO)2 66.505克置入烧杯中，加入2.5千克去离子水，使之完全溶解，即得到混合溶液；
2. 然后称量分析纯原料Bi2O3 7329.6克、Co3O4 2749.2克、Sb2O3 6286.7克、MnCO31166.5克、Ni2O3 1678.4克、ZrO2 203.2克、Y2O3 458.3克、SiO2 137.2克、SnO2 381.7克、MgO15.3克、Nb2O5 337.2克，置入搅拌球磨罐中，加入80千克锆球、30千克去离子水和430克分散剂，湿式球磨混合18小时，滤出锆球，得到主添加剂混合浆料，然后在添加剂喷雾干燥塔喷雾干燥成含水量小于0.3%的主添加剂造粒粉料颗粒；
3. 将步骤2中的主添加剂造粒粉料颗粒置入匣钵中，750oC条件下煅烧2小时，升温速率2.5 oC/min，随炉降温，得到主添加剂预合成粉料颗粒；
4. 将步骤3中的主添加剂预合成粉料颗粒粉碎，然后置入球磨罐中，加入80千克锆球、30千克去离子水，湿式球磨混合4小时，滤出锆球，即得到主添加剂超细粉体浆料；
5. 称量去离子水70千克、分散剂2.5千克、硬脂酸500克、无水乙醇1.5千克、工业优级ZnO粉料200千克依次置入乳化混合罐中，湿式乳化混合20分钟~40分钟，再依次加入步骤4中的主添加剂超细粉体浆料、步骤1中的混合溶液，湿式乳化混合0.5~2小时，再添加55千克质量浓度为5%的聚乙烯醇水溶液和0.8千克纯度为99%以上的磷酸三丁酯，继续乳化混合3小时，制成喷雾浆料备用；
6. 采用浆料喷雾干燥塔将步骤5中的喷雾浆料喷雾干燥成含水量0.35%～0.55%的造粒粉料；
7. 将造粒粉料按常规方法干压成型，制成直径16.6毫米、厚度3.75~3.85毫米，重量2.69~2.77克的陶瓷生坯体；
8. 将步骤7中的陶瓷生坯体在550℃条件下保温4小时排胶，排胶后进行烧结，烧结温度为1060℃，保温3小时，得到烧结好的瓷片；
9. 然后将烧结好的瓷片800℃回火2小时、采用含银量为80%的银电极浆料丝网印刷银电极，自由边为0.5毫米、还原、焊接、包封，即得到一种高能量型压敏电阻。
实施例3
一种高能量型压敏电阻的制备方法按下列步骤进行：
1. 首先称量分析纯原料H3BO3 29.927克、Al(NO3)3·9H2O 46.744克、AgNO3 59.117克、Ba(CH3COO)2 66.504克置入烧杯中，加入2.5千克去离子水，使之完全溶解，即得到混合溶液；
2. 然后称量分析纯原料Bi2O3 6502克、Co3O4 2749.2克、Sb2O3 6582.5克、MnCO31254克、Ni2O3 1594.5克、ZrO2 156.3克、Y2O3 286.5克、SiO2 152.2克、SnO2 381.7克、MgO106.4克、Nb2O5 101.2克，置入搅拌球磨罐中，加入75千克锆球、30千克去离子水和430克分散剂，湿式球磨混合18小时，滤出锆球，得到主添加剂混合浆料，然后在添加剂喷雾干燥塔喷雾干燥成含水量小于0.3%的主添加剂造粒粉料颗粒；
3. 将步骤2中的主添加剂造粒粉料颗粒置入匣钵中，750oC条件下煅烧2小时，升温速率2.5 oC/min，随炉降温，得到主添加剂预合成粉料颗粒；
4. 将步骤3中的主添加剂预合成粉料颗粒粉碎，然后置入球磨罐中，加入75千克锆球、30千克去离子水，湿式球磨混合4小时，滤出锆球，即得到主添加剂超细粉体浆料；
5. 称量去离子水70千克、分散剂2.5千克、硬脂酸500克、无水乙醇1.5千克、工业优级ZnO粉料200千克依次置入乳化混合罐中，湿式乳化混合20分钟~40分钟，再依次加入步骤4中的主添加剂超细粉体浆料、步骤1中的混合溶液，湿式乳化混合0.5~2小时，再添加55千克质量浓度为5%的聚乙烯醇水溶液和0.8千克纯度为99%以上的磷酸三丁酯，继续乳化混合3小时，制成喷雾浆料备用；
6. 采用浆料喷雾干燥塔将步骤5中的喷雾浆料喷雾干燥成含水量0.35%～0.55%的造粒粉料；
7. 将造粒粉料按常规方法干压成型，制成直径16.6毫米、厚度3.75~3.85毫米，重量2.69~2.77克的陶瓷生坯体；
8. 将步骤7中的陶瓷生坯体在550℃条件下保温4小时排胶，排胶后进行烧结，烧结温度为1020℃，保温3小时，得到烧结好的瓷片；
9. 然后将烧结好的瓷片800℃回火2小时、采用含银量为80%的银电极浆料丝网印刷银电极，自由边为0.5毫米、还原、焊接、包封，即得到一种高能量型压敏电阻。
为了检测本发明的性能，对本发明进行了性能测试，测试结果如下表所示：
Figure DEST_PATH_IMAGE002AA
注：组合波冲击次数±20次，表示正方向连续冲击20次后，反方向连续冲击20次。
从上述测试结果可知,本发明的性能指标均优于现有同类产品。

Claims (1)

1.一种高能量型压敏电阻的制造方法，其特征在于，所述的制造方法的具体步骤是：
（1）首先将分析纯原料H3BO3、Al(NO3)3·9H2O、AgNO3、Ba(CH3COO)2按摩尔百分比H3BO3∶Al(NO3)3·9H2O∶AgNO3∶Ba(CH3COO)2等于0.015%~0.025%∶0.004%~0.006%∶0.01%~0.015%∶0.005%~0.05%称量好，置入烧杯中，加入去离子水，使之完全溶解，即得到混合溶液，备用；其中H3BO3、Al(NO3)3·9H2O、AgNO3、Ba(CH3COO)2的总重量与去离子水的重量比为1∶10~20；
（2）将分析纯原料Bi2O3、Co3O4、Sb2O3、MnCO3、Ni2O3、ZrO2、Y2O3、SiO2、SnO2、MgO、Nb2O5按摩尔百分比Bi2O3∶Co3O4∶Sb2O3∶MnCO3∶Ni2O3∶ZrO2∶Y2O3∶SiO2∶SnO2∶MgO∶Nb2O5等于0.5%~0.65%∶0.3%~0.5%∶0.5%~1.5%∶0.4%~0.5%∶0.35%~0.45%∶0.05%~0.07%∶0.05%~0.1%∶0.05%~0.1%∶0.05%~0.12%∶0.1%~0.3%∶0.01%~0.2%称量好，置入搅拌球磨罐中，加入锆球、去离子水和分散剂，湿式球磨混合12~24小时，滤出锆球，得到主添加剂混合浆料，然后喷雾造粒，即得到主添加剂造粒粉料颗粒；其中，上述主添加剂Bi2O3、Co3O4、Sb2O3、MnCO3、Ni2O3、ZrO2、Y2O3、SiO2、SnO2、MgO、Nb2O5的总重量、锆球、去离子水、分散剂的重量比为1∶3~4∶1~2∶0.01~0.03；所述分散剂指的是铵盐类阳离子表面活性剂；
（3）将步骤（2）中的主添加剂造粒粉料颗粒置入匣钵中，700℃～900℃条件下煅烧1~4小时，得到主添加剂预合成粉料颗粒；
（4）将步骤（3）中的主添加剂预合成粉料颗粒粉碎，然后置入球磨罐中，加入锆球、去离子水，湿式球磨混合3~8小时，滤出锆球，即得到主添加剂超细粉体浆料；其中，主添加剂预合成粉料颗粒、锆球、去离子水的重量比为1∶3~4∶1~2；
（5）取去离子水、分散剂、硬脂酸、无水乙醇、工业优级ZnO粉料依次置入乳化混合罐中，湿式乳化混合20分钟~40分钟，再依次加入步骤（4）中的主添加剂超细粉体浆料、步骤（1）中的混合溶液，湿式乳化混合0.5~2小时，再添加粘结剂和消泡剂，继续乳化混合3~5小时，制成喷雾浆料备用；其中，去离子水、分散剂、硬脂酸、无水乙醇、粘结剂、消泡剂、工业优级ZnO粉料的重量比为0.3～0.55 : 0.01～0.05 : 0.002～0.01 : 0.002～0.01 : 0.1～0.5 :0.001～0.004 : 1；上述工业优级ZnO粉料与步骤（2）中的Bi2O3、Co3O4、Sb2O3、MnCO3、Ni2O3、ZrO2、Y2O3、SiO2、SnO2、MgO、Nb2O5和步骤（1）中的H3BO3、Al(NO3)3·9H2O、AgNO3、Ba(CH3COO)2的摩尔百分比为96.5%~97.5%∶0.5%~0.65%∶0.3%~0.5%∶0.5%~1.5%∶0.4%~0.5%∶0.35%~0.45%∶0.05%~0.07%∶0.05%~0.1%∶0.05%~0.1%∶0.05%~0.12%∶0.1%~0.3%∶0.01%~0.2%∶0.015%~0.025%∶0.004%~0.006%∶0.01%~0.015%∶0.005%~0.05%；上述粘结剂是质量浓度为5%的聚乙烯醇水溶液，上述分散剂是铵盐类阳离子表面活性剂，上述消泡剂是纯度为99%以上的磷酸三丁酯或正辛醇；
（6）将步骤（5）中的喷雾浆料喷雾干燥成含水量0.35%～0.55%的造粒粉料；
（7）将造粒粉料按常规方法干压成型，制成陶瓷生坯体；
（8）将陶瓷生坯体经550℃～650℃排胶后进行烧结，烧结温度为1050℃～1250℃，得到烧结好的瓷片；
（9）然后将烧结好的瓷片550℃～850℃回火、丝网印刷银电极、还原、焊接、包封，即得到一种高能量型压敏电阻，所述丝网印刷银电极采用的工艺是常规丝网印刷工艺，所用的银电极浆料含银量为80%。
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