CN107285755A - 一种稳定耐高温电子陶瓷及其制备方法 - Google Patents

一种稳定耐高温电子陶瓷及其制备方法 Download PDF

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CN107285755A
CN107285755A CN201710652906.5A CN201710652906A CN107285755A CN 107285755 A CN107285755 A CN 107285755A CN 201710652906 A CN201710652906 A CN 201710652906A CN 107285755 A CN107285755 A CN 107285755A
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aluminium hydroxide
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齐慧
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Hefei Easthigh Rui Electronic Technology Co Ltd
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Abstract

本发明公开了一种稳定耐高温电子陶瓷及其制备方法，涉及电子材料技术领域，该电子陶瓷包括以下原料：改性氢氧化铝、纳米二氧化硅、氮化铝、三氧化二硼、二氧化钼、氧化镁、氧化锆、氧化钍、碳酸锰、氟锆酸钾、聚乙烯缩丁醛、氢氧化铌、酒石酸锑钾、硬脂酸锌、增塑剂、分散剂和抗氧剂。其制备方法是通过对上述原料分阶段研磨混匀、压制造型、固化干燥以及烧结处理制得的。本发明的电子陶瓷制备简单方便，原料成本低廉，具有良好的耐高温性，随温度的升高，电容变化率小而稳定，介电损耗低，使用寿命长，适宜推广应用。

Description

一种稳定耐高温电子陶瓷及其制备方法
技术领域
本发明涉及电子材料技术领域，具体涉及一种稳定耐高温电子陶瓷及其制备方法。
背景技术
电子陶瓷材料主要是指的一类具有电磁等功能的陶瓷，它的介电性能和导电性能调节范围较宽，是特种陶瓷材料中最具活力的材料之一，被人们广为关注。它可以应用在电子、通讯、自动控制、信息计算机、汽车、航空等众多领域当中，具有显著的社会效益和经济效益。当前电子信息的发展越来越迅速，对电子元器件的要求也越来越高，微型化、薄膜化、多功能等成为未来发展的方向，而目前电子陶瓷产品存在耐高温性不足的问题，导致其介电损耗大，电容变化率大且不稳定，严重影响电子陶瓷产品的使用，因此，需要改善。
发明内容
针对现有技术中存在的问题，本发明提供了一种稳定耐高温电子陶瓷及其制备方法，该种电子陶瓷制备简单方便，原料成本低廉，具有良好的耐高温性，随温度的升高，电容变化率小而稳定，介电损耗低，使用寿命长，适宜推广应用。
为了达到上述目的，本发明通过以下技术方案来实现的：
一种稳定耐高温电子陶瓷，包括以下按重量份计的原料：改性氢氧化铝30-40份、纳米二氧化硅25-35份、氮化铝10-20份、三氧化二硼5-15份、二氧化钼8-12份、氧化镁5-15份、氧化锆6-10份、氧化钍4-8份、碳酸锰3-5份、氟锆酸钾2-4份、聚乙烯缩丁醛2-4份、氢氧化铌2-6份、酒石酸锑钾2-6份、硬脂酸锌1-5份、增塑剂1-3份、分散剂1-3份和抗氧剂1-5份；
所述改性氢氧化铝通过以下步骤制得：取适量氢氧化铝研磨至粒径小于等于500μm，再向其中加入相当氢氧化铝重量1-3％的环氧大豆油、相当氢氧化铝重量4-6％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量3-5％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在85-95℃，搅拌反应2-3h，干燥后，粉碎即得。
进一步地，所述电子陶瓷包括以下按重量份计的原料：改性氢氧化铝35份、纳米二氧化硅30份、氮化铝15份、三氧化二硼10份、二氧化钼10份、氧化镁10份、氧化锆8份、氧化钍6份、碳酸锰4份、氟锆酸钾3份、聚乙烯缩丁醛3份、氢氧化铌4份、酒石酸锑钾4份、硬脂酸锌3份、增塑剂2份、分散剂2份和抗氧剂3份。
进一步地，所述改性氢氧化铝通过以下步骤制得：取适量氢氧化铝研磨至粒径小于等于300μm，再向其中加入相当氢氧化铝重量2％的环氧大豆油、相当氢氧化铝重量5％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量4％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在90℃，搅拌反应2.5h，干燥后，粉碎即得。
优选地，所述增塑剂为五氯硬脂酸甲酯或氯甲氧基油酸甲酯。
优选地，所述分散剂为十二烷基硫酸钠、聚丙烯酰胺或古尔胶中的一种。
优选地，所述抗氧剂为抗氧剂1010、抗氧剂1076或抗氧剂TNP中的一种。
上述的一种稳定耐高温电子陶瓷的制备方法，按照以下步骤进行：
(1)按所述重量份配比称取原料；
(2)先将除增塑剂、分散剂和抗氧剂的其它原料混合加入重量比为30-40％、温度为45-55℃的去离子水在球磨机中研磨混匀，得浆料；再将剩余原料加入到浆料中继续研磨混匀，得混料；
(3)之后将混料注入模具中，通过压力机压制成型，随后将模具放置于空气干燥箱中固化处理1-2h，固化后脱模得到湿坯，将湿坯置于真空干燥箱中干燥2-3h，得素坯；
(4)最后将素坯放置于烧结炉中加热烧结，烧结完毕随炉温冷却至室温即可。
进一步地，在步骤(4)中，所述烧结炉的烧结温度为580-620℃，烧结时间为2-3h。
本发明具有如下的有益效果：本发明的电子陶瓷制备简单方便，原料成本低廉，原料中无铅无钡，绿色环保；通过对生产原料及工艺的改进优化，在降低原料输出成本及简化制备工艺的同时，依然能使制得成品电子陶瓷性能提升，对于现有技术中，出现的电容随温度上升变化大、不稳定的问题得以解决，本发明的电子陶瓷具有良好的耐高温性，随温度的升高，电容变化率小而稳定，经检测，其可在320℃的高温下均有良好的温度稳定性(TCC＜10％)，电容变化率可控制在2-4ppm/℃，介电损耗低，达到了0.04以下，使用寿命长，适宜推广应用。
具体实施方式
下面结合实施例对本发明的具体实施方式作进一步描述，以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。
实施例1
一种稳定耐高温电子陶瓷，预备以下原料待用：改性氢氧化铝30kg、纳米二氧化硅25kg、氮化铝10kg、三氧化二硼5kg、二氧化钼8kg、氧化镁5kg、氧化锆6kg、氧化钍4kg、碳酸锰3kg、氟锆酸钾2kg、聚乙烯缩丁醛2kg、氢氧化铌2kg、酒石酸锑钾2kg、硬脂酸锌1kg、增塑剂1kg、分散剂1kg和抗氧剂1kg；
上述的改性氢氧化铝通过以下步骤制得：取30kg的氢氧化铝研磨至粒径小于等于500μm，再向其中加入相当氢氧化铝重量1％的环氧大豆油、相当氢氧化铝重量4％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量3％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在85℃，搅拌反应2h，干燥后，粉碎即制得本发明原料所需的改性氢氧化铝。
其中，上述的增塑剂采用五氯硬脂酸甲酯；
分散剂采用十二烷基硫酸钠；
抗氧剂采用抗氧剂1010。
上述的一种稳定耐高温电子陶瓷的制备方法，按照以下步骤进行：
(1)先将除增塑剂、分散剂和抗氧剂的其它原料混合加入重量比为30％、温度为45℃的去离子水在球磨机中研磨混匀，得浆料；再将剩余原料加入到浆料中继续研磨混匀，得混料；
(2)之后将混料注入模具中，通过压力机压制成型，随后将模具放置于空气干燥箱中固化处理1h，固化后脱模得到湿坯，将湿坯置于真空干燥箱中干燥2h，得素坯；
(3)最后将素坯放置于烧结炉中加热烧结处理2h，烧结温度控制在580℃，烧结完毕后随炉温冷却至室温即制得本发明的稳定耐高温电子陶瓷。
实施例2
一种稳定耐高温电子陶瓷，预备以下原料待用：改性氢氧化铝35kg、纳米二氧化硅30kg、氮化铝15kg、三氧化二硼10kg、二氧化钼10kg、氧化镁10kg、氧化锆8kg、氧化钍6kg、碳酸锰4kg、氟锆酸钾3kg、聚乙烯缩丁醛3kg、氢氧化铌4kg、酒石酸锑钾4kg、硬脂酸锌3kg、增塑剂2kg、分散剂2kg和抗氧剂3kg；
上述的改性氢氧化铝通过以下步骤制得：取35kg的氢氧化铝研磨至粒径小于等于500μm，再向其中加入相当氢氧化铝重量2％的环氧大豆油、相当氢氧化铝重量5％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量4％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在90℃，搅拌反应2.5h，干燥后，粉碎即制得本发明原料所需的改性氢氧化铝。
其中，上述的增塑剂采用氯甲氧基油酸甲酯；
分散剂采用聚丙烯酰胺；
抗氧剂采用抗氧剂1076。
上述的一种稳定耐高温电子陶瓷的制备方法，按照以下步骤进行：
(1)先将除增塑剂、分散剂和抗氧剂的其它原料混合加入重量比为35％、温度为50℃的去离子水在球磨机中研磨混匀，得浆料；再将剩余原料加入到浆料中继续研磨混匀，得混料；
(2)之后将混料注入模具中，通过压力机压制成型，随后将模具放置于空气干燥箱中固化处理1.5h，固化后脱模得到湿坯，将湿坯置于真空干燥箱中干燥2.5h，得素坯；
(3)最后将素坯放置于烧结炉中加热烧结处理2.5h，烧结温度控制在600℃，烧结完毕后随炉温冷却至室温即制得本发明的稳定耐高温电子陶瓷。
实施例3
一种稳定耐高温电子陶瓷，预备以下原料待用：改性氢氧化铝40kg、纳米二氧化硅35kg、氮化铝20kg、三氧化二硼15kg、二氧化钼12kg、氧化镁15kg、氧化锆10kg、氧化钍8kg、碳酸锰5kg、氟锆酸钾4kg、聚乙烯缩丁醛4kg、氢氧化铌6kg、酒石酸锑钾6kg、硬脂酸锌5kg、增塑剂3kg、分散剂3kg和抗氧剂5kg；
上述的改性氢氧化铝通过以下步骤制得：取40kg的氢氧化铝研磨至粒径小于等于500μm，再向其中加入相当氢氧化铝重量3％的环氧大豆油、相当氢氧化铝重量6％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量5％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在95℃，搅拌反应3h，干燥后，粉碎即制得本发明原料所需的改性氢氧化铝。
其中，上述的增塑剂采用五氯硬脂酸甲酯；
分散剂采用古尔胶；
抗氧剂采用抗氧剂TNP。
上述的一种稳定耐高温电子陶瓷的制备方法，按照以下步骤进行：
(1)先将除增塑剂、分散剂和抗氧剂的其它原料混合加入重量比为40％、温度为55℃的去离子水在球磨机中研磨混匀，得浆料；再将剩余原料加入到浆料中继续研磨混匀，得混料；
(2)之后将混料注入模具中，通过压力机压制成型，随后将模具放置于空气干燥箱中固化处理2h，固化后脱模得到湿坯，将湿坯置于真空干燥箱中干燥3h，得素坯；
(3)最后将素坯放置于烧结炉中加热烧结处理3h，烧结温度控制在620℃，烧结完毕后随炉温冷却至室温即制得本发明的稳定耐高温电子陶瓷。
以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。

Claims (8)

1.一种稳定耐高温电子陶瓷，其特征在于，包括以下按重量份计的原料：改性氢氧化铝30-40份、纳米二氧化硅25-35份、氮化铝10-20份、三氧化二硼5-15份、二氧化钼8-12份、氧化镁5-15份、氧化锆6-10份、氧化钍4-8份、碳酸锰3-5份、氟锆酸钾2-4份、聚乙烯缩丁醛2-4份、氢氧化铌2-6份、酒石酸锑钾2-6份、硬脂酸锌1-5份、增塑剂1-3份、分散剂1-3份和抗氧剂1-5份；
所述改性氢氧化铝通过以下步骤制得：取适量氢氧化铝研磨至粒径小于等于500μm，再向其中加入相当氢氧化铝重量1-3％的环氧大豆油、相当氢氧化铝重量4-6％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量3-5％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在85-95℃，搅拌反应2-3h，干燥后，粉碎即得。
2.根据权利要求1所述的一种稳定耐高温电子陶瓷，其特征在于，包括以下按重量份计的原料：改性氢氧化铝35份、纳米二氧化硅30份、氮化铝15份、三氧化二硼10份、二氧化钼10份、氧化镁10份、氧化锆8份、氧化钍6份、碳酸锰4份、氟锆酸钾3份、聚乙烯缩丁醛3份、氢氧化铌4份、酒石酸锑钾4份、硬脂酸锌3份、增塑剂2份、分散剂2份和抗氧剂3份。
3.根据权利要求1所述的一种稳定耐高温电子陶瓷，其特征在于，所述改性氢氧化铝通过以下步骤制得：取适量氢氧化铝研磨至粒径小于等于300μm，再向其中加入相当氢氧化铝重量2％的环氧大豆油、相当氢氧化铝重量5％的氨基硅烷偶联剂KH-550和相当氢氧化铝重量4％的聚亚苯基砜树脂，共同输送至捏合釜中，温度控制在90℃，搅拌反应2.5h，干燥后，粉碎即得。
4.根据权利要求1所述的一种稳定耐高温电子陶瓷，其特征在于，所述增塑剂为五氯硬脂酸甲酯或氯甲氧基油酸甲酯。
5.根据权利要求1所述的一种稳定耐高温电子陶瓷，其特征在于，所述分散剂为十二烷基硫酸钠、聚丙烯酰胺或古尔胶中的一种。
6.根据权利要求1所述的一种稳定耐高温电子陶瓷，其特征在于，所述抗氧剂为抗氧剂1010、抗氧剂1076或抗氧剂TNP中的一种。
7.一种如权利要求1-6任意一项所述的稳定耐高温电子陶瓷的制备方法，其特征在于，包括以下步骤：
(1)按所述重量份配比称取原料；
(2)先将除增塑剂、分散剂和抗氧剂的其它原料混合加入重量比为30-40％、温度为45-55℃的去离子水在球磨机中研磨混匀，得浆料；再将剩余原料加入到浆料中继续研磨混匀，得混料；
(3)之后将混料注入模具中，通过压力机压制成型，随后将模具放置于空气干燥箱中固化处理1-2h，固化后脱模得到湿坯，将湿坯置于真空干燥箱中干燥2-3h，得素坯；
(4)最后将素坯放置于烧结炉中加热烧结，烧结完毕随炉温冷却至室温即可。
8.根据权利要求7所述的一种稳定耐高温电子陶瓷的制备方法，其特征在于，在步骤(4)中，所述烧结炉的烧结温度为580-620℃，烧结时间为2-3h。
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