CN112142474A - 一种水基流延成型高导热氮化铝陶瓷基板的制备方法 - Google Patents
一种水基流延成型高导热氮化铝陶瓷基板的制备方法 Download PDFInfo
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 60
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Abstract
本发明公开了一种水基流延成型高导热氮化铝陶瓷基板的制备方法(1)采用氧化铝磷酸二氢铝对氮化铝粉体进行表面改性；(2)称取改性后的氮化铝粉体、分散剂、增塑剂、粘结剂并混合均匀；(3)真空除泡；(4)生坯的制备，采用流延成型与冷等静压成型相结合工艺；(5)排胶，在180℃～460℃下保温2～3h；(6)氮气气氛下1600℃～1750℃烧结4～6h。本发明采用的溶剂为水，安全、绿色、环保，浆料的稳定性好，制得的陶瓷基板热导率高；工艺简单，且生产成本较低，可用于高功率密度电路、IGBT等领域。
Description
技术领域
本发明公开了一种水基流延成型高导热氮化铝陶瓷基板的制备方法，属于流延成型工艺技术领域。
背景技术
氮化铝(AlN)陶瓷具有高的热导率(接近碳化硅和氧化铍，是氧化铝的5-10倍)、低的介电常数和介质损耗、良好的电绝缘特性以及与硅、砷化镓相匹配的热膨胀系数，是近年来电子工业中一种十分热门的材料。与氧化铍陶瓷相比，氮化铝陶瓷不具有毒性，且生产成本较低，是高功率密度电路、IGBT领域理想的封装材料。
目前，氮化铝陶瓷片主要采用流延成型方法制备，其生产成本低，生产效率高，流延成型主要分为传统非水基流延成型和水基流延成型，由于氮化铝粉体遇水易水解，严重阻碍了其水基流延成型的发展。但非水基流延成型工艺较水基流延成型，成本更高，且挥发的有机物会造成环境污染。此外，大部分有机物都易燃，使用过程中还会存在安全隐患。因此，采用水基流延代替非水基流延是一个不错的选择，水基流延最大的特点是采用水做溶剂，避免使用有毒的有机溶剂，但由于水溶剂的表面张力大，对粉体的浸润性差，容易产生气泡。另外，排胶过程中坯体也容易开裂。专利《一种水性流延浆料及其制备方法》(公布号CN107353030A)，提供了一种水性流延浆料包括水、混合粉体、海藻酸钠、分散剂和水性环氧树脂，制备得到的流延浆料的溶剂为水，安全环保，无气泡，流延后流延膜具有良好的强度和韧性。但其氮化铝陶瓷基片导热系数不理想。
发明内容
本发明主要解决的问题是提供一种水基流延成型高导热氮化铝陶瓷基板的制备方法，本发明提供的氮化铝陶瓷基板是通过水基流延成型法制备的，减少了有机溶剂的使用，安全、绿色、环保。同时，本发明工艺简单，且生产成本较低，制得的浆料稳定性好，陶瓷基板热导率高(180W/m˙K～223W/m˙K)。
为解决上述技术问题，本发明采用的技术方案是：
一种水基流延成型高导热氮化铝陶瓷基板的制备方法，包括以下步骤：
1)氮化铝粉体表面改性：称取原料氮化铝、氧化铝、磷酸二氢铝，球磨12h，得到改性氮化铝粉体；
2)配料：称取改性后的氮化铝粉体、烧结助剂、分散剂、增塑剂、粘结剂，球磨12h～20h，得到流延浆料；
3)真空除泡：向所述流延浆料中加入消泡剂进行真空除泡；
4)生坯的制备：采用流延成型与冷等静压成型相结合工艺获得陶瓷生坯；
5)排胶：将得到的陶瓷生坯200℃～450℃下保温2～3h；
6)烧结：将排胶后的陶瓷生坯在氮气气氛下于1600℃～1750℃烧结4～6h。
其中，步骤1)中氧化铝的质量分数为2wt％，磷酸二氢铝的质量分数为4wt％，研磨介质为无水乙醇，磨球为氧化铝，原料粉体：无水乙醇：磨球质量比＝1:1:4。
所述的氮化铝粉体，氮化铝粉体纯度为95％～99％，粒径为0.8μm～1.2μm，Fe杂质含量小于80ppm，O含量低于1.2％。
步骤2)中烧结助剂为氧化钇、氧化镝、碳酸锂中的一种或几种，分散剂为柠檬酸胺，增塑剂为丙三醇，粘结剂为聚乙烯醇。步骤2)中各物料按照质量份数比为：改性后的氮化铝粉体60份～70份，分散剂0.5份～3.5份，增塑剂6份～12份，粘结剂3份～6份，烧结助剂1份～10份。
步骤3)消泡剂为正丁醇，真空除泡条件为：真空度为-0.04～-0.1MPa，搅拌桨转速20r/min，真空除泡时间为10～20min，粘度在2000～6000cps。
步骤4)控制流延机刮刀高度为0.3～5mm，流延速度为100～500mm/min，得到0.2～1mm的坯体，然后在等静压机经压力50～120Mpa，保压5～10min。
步骤5)排胶工艺为200℃之前升温速率为1℃/min；200℃～450℃为0.3℃/min；450℃保温1h；450℃～600℃为1℃/min。最后在600℃处保温3h。
与现有技术相比，本发明具有以下优点：
1)本发明采用水基流延法制备，此方法制备工艺简单，采用水代替有机溶剂，安全、绿色，环保；
2)本发明采用三氧化二铝和磷酸二氢铝对氮化铝粉体进行表面改性，通过在氮化铝粉体表面形成一层薄膜，阻止氮化铝的水解，得到的氮化铝粉体分散性好，抗水解性能优；
3)本发明采用丙三醇作为流延浆料的增塑剂，可使流延浆料有良好的润湿性，得到的流延浆料气泡少，稳定性好，并且没有裂纹。
4)本发明制备的氮化铝陶瓷基片热导率高180W/m˙K～223W/m˙K。
具体实施方式
结合实施例说明本发明的具体技术方案。
实施例1
一种水基流延成型高导热氮化铝陶瓷基板的制备方法，该制备方法包括如下步骤：
1)氮化铝粉体表面改性：按比例称取氮化铝、2wt％氧化铝、4wt％磷酸二氢铝，加入无水乙醇进行球磨，粉体：无水乙醇：氧化铝磨球＝1:1:4，球磨12h，干燥后得到改性氮化铝粉体；
2)配料：称取改性后的氮化铝粉体(固含量为60wt％)、氧化钇(5wt％)、柠檬酸胺(2wt％)、丙三醇(8wt％)、聚乙烯醇(4wt％)，加入去离子水中，球磨12h～20h，得到流延浆料；
3)真空除泡：向上述流延浆料中加入消泡剂正丁醇，设置真空度为-0.1MPa，搅拌桨转速为20r/min，真空除泡时间15min，粘度2000～6000cps；
4)生坯的制备：将除泡后的浆料经流延机流延得到0.2～1mm的生坯坯体，流延过程中控制流延机刮刀高度为2mm，流延速度为300mm/min。再将得到的坯体用等静压机进行压制，提高陶瓷坯体的密度，压为100Mpa，保压时间为10min；
5)排胶：将得到的陶瓷生坯体首先以1℃/min的升温速率升至200℃；再以0.3℃/min的升温速率升温至450℃并保温1h；然后以1℃/min的升温速率至600℃，最后在600℃处保温3h；
6)烧结：将排胶后的陶瓷生坯在氮气气氛下于1700℃烧结6h，得到氮化铝陶瓷基片。
通过此工艺制得的流延浆料粘度为46.5mPa.s，制得的氮化铝陶瓷基片热导率为198W/m˙K。
实施例2
一种水基流延成型高导热氮化铝陶瓷基板的制备方法，该制备方法包括如下步骤：
1)氮化铝粉体表面改性：按比例称取氮化铝、2wt％氧化铝、4wt％磷酸二氢铝，加入无水乙醇进行球磨，粉体：无水乙醇：氧化铝磨球＝1:1:4，球磨12h，干燥后得到改性氮化铝粉体；
2)配料：称取改性后的氮化铝粉体(固含量为65wt％)、氧化钇(5wt％)、柠檬酸胺(2wt％)、丙三醇(8wt％)、聚乙烯醇(4wt％)，加入去离子水中，球磨12h～20h，得到流延浆料；
3)真空除泡：向上述流延浆料中加入消泡剂正丁醇，设置真空度为-0.1MPa，搅拌桨转速为20r/min，真空除泡时间15min，粘度2000～6000cps；
4)生坯的制备：将除泡后的浆料经流延机流延得到0.2～1mm的生坯坯体，流延过程中控制流延机刮刀高度为2mm，流延速度为300mm/min。再将得到的坯体用等静压机进行压制，提高陶瓷坯体的密度，压为100Mpa，保压时间为10min；
5)排胶：将得到的陶瓷生坯体首先以1℃/min的升温速率升至200℃；再以0.3℃/min的升温速率升温至450℃并保温1h；然后以1℃/min的升温速率至600℃，最后在600℃处保温3h；
6)烧结：将排胶后的陶瓷生坯在氮气气氛下于1700℃烧结6h，得到氮化铝陶瓷基片。
通过此工艺制得的流延浆料粘度为92.8mPa.s，制得的氮化铝陶瓷基片热导率为221W/m˙K。
实施例3
一种水基流延成型高导热氮化铝陶瓷基板的制备方法，该制备方法包括如下步骤：
1)氮化铝粉体表面改性：按比例称取氮化铝、2wt％氧化铝、4wt％磷酸二氢铝，加入无水乙醇进行球磨，粉体：无水乙醇：氧化铝磨球＝1:1:4，球磨12h，干燥后得到改性氮化铝粉体；
2)配料：称取改性后的氮化铝粉体(固含量为70wt％)、氧化钇(5wt％)、柠檬酸胺(2wt％)、丙三醇(8wt％)、聚乙烯醇(4wt％)，加入去离子水中，球磨12h～20h，得到流延浆料；
3)真空除泡：向上述流延浆料中加入消泡剂正丁醇，设置真空度为-0.1MPa，搅拌桨转速为20r/min，真空除泡时间15min，粘度2000～6000cps；
4)生坯的制备：将除泡后的浆料经流延机流延得到0.2～1mm的生坯坯体，流延过程中控制流延机刮刀高度为2mm，流延速度为300mm/min。再将得到的坯体用等静压机进行压制，提高陶瓷坯体的密度，压为100Mpa，保压时间为10min；
5)排胶：将得到的陶瓷生坯体首先以1℃/min的升温速率升至200℃；再以0.3℃/min的升温速率升温至450℃并保温1h；然后以1℃/min的升温速率至600℃，最后在600℃处保温3h；
6)烧结：将排胶后的陶瓷生坯在氮气气氛下于1700℃烧结6h，得到氮化铝陶瓷基片。
通过此工艺制得的流延浆料粘度为349.6mPa.s，制得的氮化铝陶瓷基片热导率为184W/m˙K。
Claims (9)
1.一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于，包括以下步骤：
1)氮化铝粉体表面改性：称取原料氮化铝、氧化铝、磷酸二氢铝，球磨12h，得到改性氮化铝粉体；
2)配料：称取改性后的氮化铝粉体、烧结助剂、分散剂、增塑剂、粘结剂，球磨12h～20h，得到流延浆料；
3)真空除泡：向所述流延浆料中加入消泡剂进行真空除泡；
4)生坯的制备：采用流延成型与冷等静压成型相结合工艺获得陶瓷生坯；
5)排胶：将得到的陶瓷生坯200℃～450℃下保温2～3h；
6)烧结：将排胶后的陶瓷生坯在氮气气氛下于1600℃～1750℃烧结4～6h。
2.根据权利要求1所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤1)中氧化铝的质量分数为2wt％，磷酸二氢铝的质量分数为4wt％，研磨介质为无水乙醇，磨球为氧化铝，原料粉体：无水乙醇：磨球的质量比1:1:4。
3.根据权利要求2所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤1)所述的氮化铝粉体，氮化铝粉体纯度为95％～99％，粒径为0.8μm～1.2μm，Fe杂质含量小于80ppm，O含量低于1.2％。
4.根据权利要求1所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤2)中烧结助剂为氧化钇、氧化镝、碳酸锂中的一种或几种，分散剂为柠檬酸胺，增塑剂为丙三醇，粘结剂为聚乙烯醇。
5.根据权利要求1所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤2)中各物料按照质量份数比为：改性后的氮化铝粉体60份～70份，分散剂0.5份～3.5份，增塑剂6份～12份，粘结剂3份～6份，烧结助剂1份～10份。
6.根据权利要求1所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤3)消泡剂为正丁醇，真空除泡条件为：真空度为-0.04～-0.1MPa，搅拌桨转速20r/min，真空除泡时间为10～20min，粘度在2000～6000cps。
7.根据权利要求1所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤4)流延成型中，流延机刮刀高度为0.3～5mm，流延速度为100～500mm/min。
8.根据权利要求7所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤4)冷等静压成型的等静压压力为50～120Mpa，保压时间为5～10min。
9.根据权利要求1所述的一种水基流延成型高导热氮化铝陶瓷基板的制备方法，其特征在于：所述步骤5)排胶工艺为200℃之前升温速率为1℃/min；200℃～450℃为0.3℃/min；450℃保温1h；450℃～600℃为1℃/min。最后在600℃处保温3h。
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Application publication date: 20201229 |