CN115159994A - 一种电子陶瓷用陶瓷粉胶黏剂及其制备方法 - Google Patents
一种电子陶瓷用陶瓷粉胶黏剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种电子陶瓷用陶瓷粉胶黏剂，按质量百分比包括以下组分：树脂45％‑55％，溶剂45％‑55％、助粘接剂0.1％‑0.5％、消泡剂0.2％‑0.5％、填料0.5％‑3％，触变剂0.5％‑3％，上述各组分的百分比之和为100％，所述树脂为聚丙烯酸酯、羟基丙烯酸脂、聚氨酯丙烯酸脂、双酚A环氧丙烯酸酯、聚乙烯醇、聚乙烯醇缩丁醛中的至少一种。本发明加入的树脂与醇类溶剂相容性好，可大大降低体系粘度，陶瓷粉能在其中分散均匀，而不发生沉降，有利于后续的陶瓷粉造粒，固化产物收缩性小，且在低温下即可发生分解或碳化，在低温烧结阶段时，在陶瓷板胚料中残留很少，有利于最终获得致密和高强度陶瓷板。
Description
技术领域
本发明涉及陶瓷技术领域，尤其涉及一种电子陶瓷用陶瓷粉胶黏剂及其制备方法。
背景技术
随着现代科技的迅速发展，对陶瓷胶黏剂的需求和质量要求也越来越高，尤其是在电子陶瓷的应用领域，对陶瓷粉胶黏剂的粘度，粘接性能、与陶瓷粉本体的相溶性能等要求越来越严苛。陶瓷粉胶黏剂一方面粘度不能太低，粘度过低时，陶瓷粉分散其中容易沉降；同时粘度也不能偏高，较高的粘度，粉体分散不均，容易粘结成团。以上两种情况均不利于陶瓷粉浆料后续的造粒和成型。陶瓷板成型时均会涉及到烧结脱脂的加工过程，现在的电子陶瓷采用的陶瓷粉大多为纳米或亚微米级别，这种级别的陶瓷粉体相对于其对应的普通粉体，熔点会有较大的降低，可以实现中低温(≤450℃)烧结，因此陶瓷粉胶黏剂也需要在较低温度下能够分解或碳化挥发出去，如果较多残留，会产生较多内气孔、裂纹，这会大大降低陶瓷板的致密度，从而对陶瓷板的机械性能起到较大负面影响。因而，选用粘度合适且能实现低温碳化的粘合剂，已成为电子陶瓷业内亟需解决的问题。
发明内容
本发明的目的在于解决电子陶瓷中陶瓷粉在胶粘剂中难以分布均匀或容易沉降，中低温烧结时难以脱脂完全，在胚体内部产生较多气孔和裂纹，生胚后陶瓷板机械强度变差的问题；而提供一种电子陶瓷用陶瓷粉胶黏剂及其制备方法。
本发明的用于电子陶瓷的陶瓷粉胶黏剂，按质量分数包括：树脂45％-55％，溶剂45％-55％、助粘接剂0.1％-0.5％、消泡剂0.2％-0.5％、填料0.5％-3％，触变剂0.5％-3％，各组分之和为100％。
优选的，其中树脂包括：聚丙烯酸酯(如聚甲基丙烯酸甲酯(PMMA))、羟基丙烯酸脂、聚氨酯丙烯酸脂、双酚A环氧丙烯酸酯、聚乙烯醇、聚乙烯醇缩丁醛，本发明所选用的树脂固化产物收缩性小，与醇类溶剂相容性好，可大大降低体系粘度，低温下即可发生分解或碳化，如PMMA在270℃时即可发生分解。
优选的，溶剂包括：醇类溶剂、醚类溶剂、醇醚类溶剂及酮类溶剂中的一种或多种。其中醇类溶剂包括：乙醇、乙二醇、聚乙二醇、异丙醇、丙三醇中的一种或几种，本发明精选的上述醇类溶剂本身粘度较低，一方面可以起到稀释树脂的作用，一方面又能很好的确保陶瓷粉体在其中有较好的分散性能，同时，沸点不超过300℃，适合于陶瓷粉低温烧结时的低温挥发；醚类溶剂包含：乙醚、环氧丙烷、四氢呋喃及异丙醚中的一种或多种。醇醚类溶剂包括：乙二醇单丁醚、二丙二醇甲醚、二丙二醇丁醚、二乙二醇甲醚、二乙二醇乙醚中的至少一种，上述醇醚类溶剂具有优异的溶解性能，即可溶解亲水性物质，也可以溶解憎水性物质；酮类溶剂包括：丙酮、环己酮、异佛尔酮及甲基异丁基酮中的一种或多种。
优选的，助粘接剂包括：硅烷偶联剂KH450、硅烷偶联剂KH570、硅烷偶联剂KH551中的至少一种，本发明选择的这几种硅烷偶联剂可以偶联主体树脂和陶瓷粉体，提高耐水性能，提升烧结后陶瓷片的抗弯强度、抗压强度、剪切强度等机械性能。
优选的，消泡剂为：聚二甲基硅氧烷，主要指甲基硅油、乙基硅油、甲基含氢硅油、甲基乙氧基硅油、甲基乙烯基硅油、甲基羟基硅油、乙基含氢硅油、羟基含氢硅油中的至少一种，本发明所选用的这几种消泡剂具有良好的润滑消泡性能，可在陶瓷粉体表面包覆光滑油膜，避免陶瓷粉浆料在分散搅拌过程中产生的大量气泡，有助于陶瓷粉的均匀分散有助于后续的陶瓷粉造粒工艺，同时其热分解温度低于350℃，低温烧结时无残留。
优选的，填料包括：熔融二氧化硅、气相二氧化硅、硅酸铝、硅酸钾、改性碳酸钙、活性氧化铝中的至少一种；本发明选择这几种填料的作用是：降低热膨胀系数(CTE)，提高强度，提高耐水性，吸湿稳定性，防止沉降，与陶瓷本体粉兼容性好，在压片时即可和陶瓷本体粉压成整体，在烧结时进一步得到致密的胚料。
优选的，触变剂包括:有机膨润土、氢化蓖麻油、聚酰胺、羟乙基纤维素及甲基纤维素中的一种或多种；本发明的所选择的上述触变剂能够防止粘合剂发生流淌，使浆料具有触变性，能够防止陶瓷粉及填料发生沉降及湿膜产生流挂，提升陶瓷粉粘合剂的施工性能和储存时间。
本发明还提供了上述电子陶瓷片用陶瓷粉胶黏剂的制备方法，包括以下：
1，将树脂、溶剂按配方比例加入30L真空搅拌机搅拌，搅拌15～30分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min)；；
2，将填料按配方比例加入30L真空搅拌机搅拌(搅拌15～45分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min)；
3，将助粘接剂、触变剂、消泡剂按配方比例加入30L真空搅拌机搅拌，搅拌15～45分钟(搅拌速度为1500-2500r/min，分散速度为1000-2000r/min)；
4，最后将分散均匀的胶黏剂采用150-200目滤网通过挤出机进行分装过滤。
本发明加入的聚丙烯酸酯(如聚甲基丙烯酸甲酯(PMMA))、羟基丙烯酸脂、聚氨酯丙烯酸脂、双酚A环氧丙烯酸酯、聚乙烯醇、聚乙烯醇缩丁醛与醇类溶剂相容性好，可大大降低体系粘度，陶瓷粉能在其中分散均匀，而不发生沉降，有利于后续的陶瓷粉造粒，固化产物收缩性小，且在低温下即可发生分解或碳化，在低温烧结阶段时，在陶瓷板胚料中残留很少，有利于最终获得致密和高强度陶瓷板。而醇类溶剂的加入可使树脂体系的粘度保持在较低状态，有利于陶瓷粉体在浆料体系中的分散，同时加入的醇类溶剂沸点低，适合陶瓷板的低温烧结工艺。而加入聚二甲基硅氧烷消泡剂具有良好的润滑与消泡性能，可在陶瓷粉表面形成光滑包覆膜，能避免搅拌分散过程中产生的气泡，有利于后续的造粒工艺，同时，其热分解温度低于低温烧结温度，在烧结时能够挥发完全。通过加入二氧化硅、气相二氧化硅、硅酸铝、硅酸钾、改性碳酸钙、活性氧化铝等填料，可以降低体系热膨胀系数(CTE)，提高耐水性，吸湿稳定性，调节粘度，防止陶瓷粉体的沉降，同时该系列填料与陶瓷本体粉兼容性好，在压片时即可和陶瓷本体粉压成整体，在烧结时进一步得到致密、高强度的胚料。
综上所述，本发明生产工艺简单，市场需求量大，制备成本较低，满足工业化生产需求。
具体实施方式
下面将结合具体实施例对本发明实施例中的技术方案进行清楚、完整地描述。
陶瓷粉胶黏剂及电子陶瓷板的相关性能检测
1.粘度测试
粘度测试采用NDJ-79旋转式粘度计(上海维菱科学仪器有限公司)，遵照ASTMD1084标准测试；
2.密度测试
陶瓷粉胶黏剂密度的测试采用重量杯法，遵循GB/T 13354-92标准，陶瓷板采用，遵循GB/T4100.5-1999标准。
3.三点弯曲强度测试
采用材料万能试验机测试陶瓷板的三点弯曲强度，遵循GB/T 14452一1993标准。
本发明电子陶瓷片用陶瓷粉胶黏剂的制备方法，包括以下步骤：
1，将树脂、溶剂按配方比例加入30L真空搅拌机搅拌，搅拌15～30分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min)；；
2，将填料按配方比例加入30L真空搅拌机搅拌(搅拌15～45分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min)；
3，将助粘接剂、触变剂、消泡剂按配方比例加入30L真空搅拌机搅拌，搅拌15～45分钟(搅拌速度为1500-2500r/min，分散速度为1000-2000r/min)；
4，最后将分散均匀的胶黏剂采用150-200目滤网通过挤出机进行分装过滤。
本发明实施例1-3电子陶瓷片用陶瓷粉胶黏剂的具体配方和相关性能(1)，如下表1所示：
表1
本发明实施例4-6电子陶瓷片用陶瓷粉胶黏剂的具体配方和相关性能(2)，如下表2所示：
表2
本发明实施例7-9电子陶瓷片用陶瓷粉胶黏剂的具体配方和相关性能，如下表3所示：
表3
采用本发明的陶瓷粉胶黏剂制备电子陶瓷板的工艺过程如下：
1，将陶瓷粉、陶瓷粉胶黏剂、分散剂按配方比例加入30L真空搅拌机搅拌，搅拌90～240分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min)；
2，将分散好的陶瓷粉浆料加入离心式喷雾造粒机，进行喷雾造粒；
3，将造粒好的陶瓷粉加入分级振动筛中，按粉体粒径进行陶瓷粉体的分级收集；
4，将分级好的一定质量的陶瓷粉加入压片机中，进行干压成型；
5，将压好的陶瓷板放入马弗炉中，进行低温(400～450℃)烧结脱脂，即可得成品电子陶瓷板。
将本发明的制得的电子陶瓷板与国内外同类产品相比，其结果如下表所示：
以上所述是本发明的优选实施方式，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也视为本发明的保护范围。
Claims (10)
1.一种电子陶瓷用陶瓷粉胶黏剂，其特征在于，按质量百分比包括以下组分：树脂45％-55％，溶剂45％-55％、助粘接剂0.1％-0.5％、消泡剂0.2％-0.5％、填料0.5％-3％，触变剂0.5％-3％，上述各组分的百分比之和为100％，所述树脂为聚丙烯酸酯、羟基丙烯酸脂、聚氨酯丙烯酸脂、双酚A环氧丙烯酸酯、聚乙烯醇、聚乙烯醇缩丁醛中的至少一种。
2.如权利要求1所述的一种电子陶瓷用陶瓷粉胶黏剂，其特征在于：所述溶剂包括：醇类溶剂、醚类溶剂、醇醚类溶剂及酮类溶剂中的一种或多种。
3.如权利要求2所述的一种电子陶瓷用陶瓷粉胶黏剂，其特征在于：所述醇类溶剂包括：乙醇、乙二醇、聚乙二醇、异丙醇、丙三醇中的一种或几种；醚类溶剂包含：乙醚、环氧丙烷、四氢呋喃及异丙醚中的一种或多种；醇醚类溶剂包括：乙二醇单丁醚、二丙二醇甲醚、二丙二醇丁醚、二乙二醇甲醚、二乙二醇乙醚中的至少一种；酮类溶剂包括：丙酮、环己酮、异佛尔酮及甲基异丁基酮中的一种或多种。
4.如权利要求1所述的一种电子陶瓷用陶瓷粉胶黏剂，其特征在于：所述助粘接剂包括：硅烷偶联剂KH450、硅烷偶联剂KH570、硅烷偶联剂KH551中的至少一种。
5.如权利要求1所述的一种电子陶瓷用陶瓷粉胶黏剂，其特征在于：所述消泡剂为：聚二甲基硅氧烷，主要指甲基硅油、乙基硅油、甲基含氢硅油、甲基乙氧基硅油、甲基乙烯基硅油、甲基羟基硅油、乙基含氢硅油、羟基含氢硅油中的至少一种。
6.如权利要求1所述的一种电子陶瓷用陶瓷粉胶黏剂，其特征在于：所述填料包括：熔融二氧化硅、气相二氧化硅、硅酸铝、硅酸钾、改性碳酸钙、活性氧化铝中的至少一种。
7.如权利要求1所述的一种电子陶瓷用陶瓷粉胶黏剂，其特征在于：所述触变剂包括:有机膨润土、氢化蓖麻油、聚酰胺、羟乙基纤维素及甲基纤维素中的一种或多种。
8.一种制备如权利要求1-7任一项所述的电子陶瓷用陶瓷粉胶黏剂的方法，其特征在于，包括以下步骤：
(1)，将树脂、溶剂按配方比例加入30L真空搅拌机搅拌；
(2)，将填料按配方比例加入30L真空搅拌机搅拌；
(3)，将助粘接剂、触变剂、消泡剂按配方比例加入30L真空搅拌机搅拌，搅拌15～45分钟(搅拌速度为1500-2500r/min，分散速度为1000-2000r/min；
(4)，最后将分散均匀的胶黏剂采用150-200目滤网通过挤出机进行分装过滤。
9.如权利要求1所述的制备方法，其特征在于：步骤(1)中搅拌时间为15～30分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min。
10.如权利要求1所述的制备方法，其特征在于：步骤(2)中搅拌时间为15～45分钟，搅拌速度为1000-3000r/min，分散速度为1000-2000r/min。
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