CN116253557A - 陶瓷流延浆料及其制备方法和陶瓷流延生带 - Google Patents
陶瓷流延浆料及其制备方法和陶瓷流延生带 Download PDFInfo
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Abstract
本发明提供了一种陶瓷流延浆料及其制备方法和陶瓷流延生带，属于半导体测试材料领域，所述陶瓷流延浆料包括30～55wt％的CBS陶瓷粉体、25～50wt％溶剂、0.5～3wt％分散剂、5～12wt％粘结剂、3～10wt％增塑剂，所述溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为3～6：3～1：4～3，所述粘结剂为低羟基含量PVB树脂，其羟基的含量范围为11～13.5wt％，分子量为50000～80000。通过本公开的处理方案，有效抑制浆料球磨和静置过程中的絮凝现象。
Description
技术领域
本发明涉及半导体测试材料领域，具体涉及一种陶瓷流延浆料及其制备方法和陶瓷流延生带。
背景技术
低温共烧陶瓷(LTCC)技术经过几十年的实际应用，在无线通信、军事装备、卫星定位、汽车传感等领域已经成为将无源元件与高导电性导体(Ag,Au)集成在多层基板中的不可替代技术。在半导体芯片的形成过程中，缩小模块尺寸、增强热扩散、降低介质损耗、调节热膨胀系数等都是非常有利的。CaO-B2O3-SiO2系微晶玻璃由于其优异的宽频介电性能，是十分重要的LTCC材料。
良好的生瓷带性能是制造LTCC共烧材料的基础，高拉伸强度、低形变、高固含量为后续填孔印刷、叠层共烧工艺及产品性能提供保障，而生瓷带性能取决于流延浆料。通过向玻璃陶瓷粉体添加溶剂、分散剂、粘结剂、增塑剂等助剂经二次球磨后，得到一定粘度范围的流延浆料。然而，在没有改性剂的情况下，常用的PVB树脂制备的悬浮浆料表现为高粘流体，没有流动性，容易絮凝成凝胶，这是由于该PVB树脂羟基官能团含量较高，CBS体系玻璃陶瓷粉体中富含B元素，两者发生反应，形成了较强的连接，导致浆料凝胶。因此急需开发一种良好流动性流延浆料且能满足生瓷带性能需求。
发明内容
因此，为了克服上述现有技术的缺点，本发明提供一种解决球磨过程絮凝成胶的陶瓷流延浆料及其制备方法和陶瓷流延生带。
为了实现上述目的，本发明提供一种陶瓷流延浆料，所述陶瓷流延浆料包括30～55wt％的CBS陶瓷粉体、25～50wt％溶剂、0.5～3wt％分散剂、5～12wt％粘结剂、3～10wt％增塑剂，所述溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为3～6：3～1：4～3，所述粘结剂为低羟基含量PVB树脂，其中羟基的含量范围为11～13.5％，分子量为50000～80000。
在其中一个实施例中，所述分散剂为磷酸三乙酯、蓖麻油、三油酸甘油酯中的至少一种。
在其中一个实施例中，所述增塑剂为邻苯二甲酸二丁酯和聚乙二醇中的至少一种。
在其中一个实施例中，还包括1～6wt％改性剂，所述改性剂为2-甲基-2,4-戊二醇(MPD)。
在其中一个实施例中，所述溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为6：2：3。
一种上述陶瓷流延浆料的制备方法，包括：将CBS陶瓷粉体倒入球磨容器，再将混合溶剂、改性剂、分散剂倒入容器与陶瓷粉体混合后，球磨12～24小时，料球比为1：3～4；将所述粘结剂与所述混合溶剂按一定质量配比混合，搅拌均匀直至溶解；将增塑剂和溶解后的粘结剂加入球磨后的混合浆料中，二次球磨4～10小时；将二次球磨后的混合浆料通过100～350目滤网过滤，真空脱泡10～60min，静置陈腐1-5h，得到所述陶瓷流延浆料。
一种陶瓷流延生带，由上述陶瓷流延浆料经流延成型后制得的。
与现有技术相比，本发明的优点在于：通过选用较低分子量、低羟基含量PVB树脂作为粘结剂，减弱PVB与硼的反应，可以有效抑制浆料球磨和静置过程中的絮凝现象，从而解决了CBS体系陶瓷浆料的凝胶现象；并针对宽度大且厚度薄的离型载膜流延工艺，采用异丙醇、二甲苯、乙醇作为三元混合溶剂，提升浆料与离型载膜的润湿性，有效避免干燥过程离型膜翘曲，从而解决了流延烘干过程离型膜翘曲、生瓷脱模等不良现象。
具体实施方式
下面对本公开实施例进行详细描述。
以下通过特定的具体实例说明本公开的实施方式，本领域技术人员可由本说明书所揭露的内容轻易地了解本公开的其他优点与功效。显然，所描述的实施例仅仅是本公开一部分实施例，而不是全部的实施例。本公开还可以通过另外不同的具体实施方式加以实施或应用，本说明书中的各项细节也可以基于不同观点与应用，在没有背离本公开的精神下进行各种修饰或改变。需说明的是，在不冲突的情况下，以下实施例及实施例中的特征可以相互组合。基于本公开中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本公开保护的范围。
要说明的是，下文描述在所附权利要求书的范围内的实施例的各种方面。应显而易见，本文中所描述的方面可体现于广泛多种形式中，且本文中所描述的任何特定结构及/或功能仅为说明性的。基于本公开，所属领域的技术人员应了解，本文中所描述的一个方面可与任何其它方面独立地实施，且可以各种方式组合这些方面中的两者或两者以上。举例来说，可使用本文中所阐述的任何数目个方面来实施设备及/或实践方法。另外，可使用除了本文中所阐述的方面中的一或多者之外的其它结构及/或功能性实施此设备及/或实践此方法。
另外，在以下描述中，提供具体细节是为了便于透彻理解实例。然而，所属领域的技术人员将理解，可在没有这些特定细节的情况下实践所述方面。
本公开实施例提供一种陶瓷流延浆料，陶瓷流延浆料包括30～55wt％的CBS陶瓷粉体、25～50wt％溶剂、0.5～3wt％分散剂、5～12wt％粘结剂、3～10wt％增塑剂。在本申请中如无特殊指出，均为质量百分数。
CBS陶瓷粉体是Ca-B-Si-O体系LTCC陶瓷粉体。陶瓷粉体的平均粒径可为0.5～5um。Ca-B-Si-O体系中CaO的范围是25～35wt％，B2O3的范围是35～50wt％，SiO2的范围是20～30wt％。
溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为3～6：3～1：4～3。
粘结剂为低羟基含量PVB树脂，其中羟基的含量范围为11～13.5wt％，分子量50000～80000。
分散剂可分散难溶于溶剂的陶瓷粉体，同时也能抑制粉体颗粒的沉降和凝聚，形成稳定悬浮液。在其中一个实施例中，分散剂为磷酸三乙酯、蓖麻油、三油酸甘油酯中的至少一种。
增塑剂可以降低浆料的粘度，增强生瓷带的韧性。在其中一个实施例中，增塑剂为邻苯二甲酸二丁酯和聚乙二醇中的至少一种。
在其中一个实施例中，还包括1～6wt％改性剂，改性剂能够进一步提升浆料的固含量，从而提升生瓷带的性能。改性剂为2-甲基-2,4-戊二醇(MPD)。改性剂可以吸附于粉体颗粒表面，使凝聚的颗粒表面易于润湿，使体系均匀，悬浮性能增加。
一种陶瓷流延浆料的制备方法，包括以下步骤：
将CBS陶瓷粉体倒入球磨容器，再将混合溶剂、改性剂、分散剂倒入容器与陶瓷粉体混合后，球磨12～24小时，料球比为1：3～4；
将粘结剂与混合溶剂按一定质量配比混合，搅拌均匀直至溶解；
将增塑剂和溶解后的粘结剂加入球磨后的混合浆料中，二次球磨4～10小时；
将二次球磨后的混合浆料通过100～350目滤网过滤，真空脱泡10～60min，静置陈腐1-5h，得到陶瓷流延浆料。
将上述陶瓷流延浆料经流延成型后制得陶瓷流延生带。本发明获得的陶瓷流延生带的厚度可为50～150微米，优选为90～120微米。调整所需刮刀间隙，将上述浆料经流延成型、干燥、揭膜等工艺制备的生瓷带，表面均匀、平整、光滑，无裂纹，无皱皮，无气泡，韧性好，强度高，不易形变。
实施例一
一种陶瓷流延浆料的制备方法，包括以下步骤：
步骤一，将50wt％CBS陶瓷粉体倒入球磨容器，将混合溶剂、2wt％改性剂、3wt％分散剂倒入容器与陶瓷粉体混合后，球磨12～24小时，料球比为1：3；溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为6：2：3。分散剂为蓖麻油。改性剂为2-甲基-2,4-戊二醇(MPD)。
步骤二，将陶瓷粉质量的6wt％PVB树脂与混合三元溶剂按一定质量配比混合，充分搅拌均匀，实现PVB树脂的充分溶解，避免浆料的团聚导致生瓷带开裂。PVB树脂，羟基含量11％-13.5％，分子量50000-80000。步骤一和步骤二中所有三元溶剂在整个体系中质量百分比为30wt％。
步骤三，将增塑剂和溶解后的粘结剂加入球磨后的混合浆料中，二次球磨4～10小时。增塑剂为邻苯二甲酸二丁酯。
步骤四，将二次球磨后的混合浆料通过100～350目滤网过滤，真空脱泡10～60min，静置陈腐1-5h，得到陶瓷流延浆料。滤网是尼龙滤网。
实施例二
一种陶瓷流延浆料的制备方法，包括以下步骤：
步骤一，将35wt％CBS陶瓷粉体倒入球磨容器，将混合溶剂、2wt％改性剂、1wt％分散剂倒入容器与陶瓷粉体混合后，球磨12～24小时，料球比为1：3；溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为6：2：3。分散剂为蓖麻油。改性剂为2-甲基-2,4-戊二醇(MPD)。
步骤二，将陶瓷粉质量的9wt％PVB树脂与混合三元溶剂按一定质量配比混合，充分搅拌均匀，实现PVB树脂的充分溶解，避免浆料的团聚导致生瓷带开裂。PVB树脂，羟基含量11％-13.5％，分子量50000-80000。步骤一和步骤二中所有三元溶剂在整个体系中质量百分比为52％。
步骤三，将4％增塑剂和溶解后的粘结剂加入球磨后的混合浆料中，二次球磨4～10小时。增塑剂为邻苯二甲酸二丁酯。
步骤四，将二次球磨后的混合浆料通过200目滤网过滤，真空脱泡20min，静置陈腐1h，得到陶瓷流延浆料。滤网是尼龙滤网。
上述两种实施例制备的浆料都无絮凝现象，且制备的浆料流延干燥过程无离型膜翘曲，生瓷脱模现象；流延制备的生瓷带外观无不良，拉伸强度较佳，均超过2MPa，具体参数如下表1所示。
以上所述，仅为本公开的具体实施方式，但本公开的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本公开揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本公开的保护范围之内。因此，本公开的保护范围应以权利要求的保护范围为准。
Claims (7)
1.一种陶瓷流延浆料，其特征在于，所述陶瓷流延浆料包括30～55wt％的CBS陶瓷粉体、25～50wt％溶剂、0.5～3wt％分散剂、5～12wt％粘结剂、3～10wt％增塑剂，
所述溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为3～6：3～1：4～3，
所述粘结剂为低羟基含量PVB树脂，其中羟基的含量范围为11～13.5wt％，分子量为50000～80000。
2.根据权利要求1所述的陶瓷流延浆料，其特征在于，所述分散剂为磷酸三乙酯、蓖麻油、三油酸甘油酯中的至少一种。
3.根据权利要求1所述的陶瓷流延浆料，其特征在于，所述增塑剂为邻苯二甲酸二丁酯和聚乙二醇中的至少一种。
4.根据权利要求1所述的陶瓷流延浆料，其特征在于，还包括1～6wt％改性剂，所述改性剂为2-甲基-2,4-戊二醇。
5.根据权利要求1所述的陶瓷流延浆料，其特征在于，所述溶剂为异丙醇、二甲苯、乙醇三元混合溶剂，质量比为6：2：3。
6.一种如权利要求1-5中任一项所述陶瓷流延浆料的制备方法，其特征在于，包括：
将CBS陶瓷粉体倒入球磨容器，再将混合溶剂、分散剂倒入容器与陶瓷粉体混合后，球磨12～24小时，料球比为1：3～4；
将所述粘结剂与所述混合溶剂按一定质量配比混合，搅拌均匀直至溶解；
将增塑剂和溶解后的粘结剂加入球磨后的混合浆料中，二次球磨4～10小时；
将二次球磨后的混合浆料通过100～350目滤网过滤，真空脱泡10～60min，静置陈腐1-5h，得到所述陶瓷流延浆料。
7.一种陶瓷流延生带，其特征在于，由权利要求1-5中任一项所述陶瓷流延浆料经流延成型后制得的。
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