CN105777081B - 一种散热用电子陶瓷基板的制备工艺 - Google Patents

一种散热用电子陶瓷基板的制备工艺 Download PDF

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CN105777081B
CN105777081B CN201610132652.XA CN201610132652A CN105777081B CN 105777081 B CN105777081 B CN 105777081B CN 201610132652 A CN201610132652 A CN 201610132652A CN 105777081 B CN105777081 B CN 105777081B
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赵磊
王宇平
宋德锋
赵小玻
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Abstract

本发明属于电子陶瓷基板技术领域，具体涉及一种散热用电子陶瓷基板的制备工艺。本发明的制备工艺包括：1)复合烧结助剂的制备；2)陶瓷浆料的制备；3)陶瓷成型。本发明的有益效果如下：1)本发明通过采用合适的烧结方法和选取合适的烧结助剂，实现氧化铝陶瓷烧结体的致密化，大大提高了氧化铝陶瓷的热导率。2)本发明的烧结助剂中三聚氰胺在高温下可以生产氮化铝和氮化碳，增加了陶瓷基板表面的硬度和光泽度。3)本发明的烧结助剂可形成低熔点的物相，实现液相烧结，降低烧成温度，促进坯体的致密化。

Description

一种散热用电子陶瓷基板的制备工艺
技术领域
本发明属于电子陶瓷基板技术领域，具体涉及一种散热用电子陶瓷基板的制备工艺。
背景技术
在电子工业中能够利用电、磁性质的陶瓷，称为电子陶瓷。电子陶瓷是通过对表面、晶界和尺寸结构的控制而最终获得具有新功能的陶瓷。在能源、家用电器、汽车等方面可以广泛应用。
广泛用于制作电子功能元件的、多数以氧化物为主成分的烧结体材料。电子陶瓷的制造工艺与传统的陶瓷工艺大致相同。电子陶瓷或称电子工业用陶瓷，它在化学成分、微观结构和机电性能上，均与一般的电力用陶瓷有着本质的区别。这些区别是电子工业对电子陶瓷所提出的一系列特殊技术要求而形成的，其中最重要的是须具有高的机械强度、耐高温高湿、抗辐射、介质常数在很宽的范围内变化、介质损耗角正切值小、电容量温度系数可以调整(或电容量变化率可调整)、抗电强度和绝缘电阻值高以及老化性能优异等。
目前，在电子陶瓷生坯制作时，通常是采用流延成型的方法制作，因此，流延浆料的配置非常关键。氧化铝陶瓷基板因其良好的热传导性能、较高的机械强度和优异的绝缘性能，成为半导体、电子等行业应用最为广泛的无机非金属基板材料。选用陶瓷散热基板替换传统的金属基板，在兼具机械性的基础上相对传统金属基板具有更好的导热性和绝缘性。
因此，将氧化铝陶瓷基板应用于散热用电子陶瓷基板具有非常广阔的应用前景。
发明内容
本发明的目的在于提供一种新的散热用电子陶瓷基板的制备工艺。
为了实现本发明目的而采用的技术方案为：一种散热用电子陶瓷基板的制备工艺，其工艺步骤为：
1)复合烧结助剂的制备
将三聚氰胺、铝粉、高岭土粉、氟化钙分散于无水乙醇中；然后在通风橱中边搅拌、边用热风吹，直至无水乙醇完全烘干而得到混合粉体，即制得复合烧结助剂；
2)陶瓷浆料的制备
依次加入氧化铝粉、羟甲基纤维素、去离子水、硅粉和步骤1)制得的复合烧结助剂进行湿法球磨，制成可凝胶陶瓷浆料，对该陶瓷浆料进行真空搅拌除泡；
3)陶瓷成型
将步骤2)制得的陶瓷浆料由模具底部压入模具中，自然放置完成凝胶过程；取出陶瓷坯片进行干燥处理，放入热压模具中置于热压炉中进行烧结压制，再降温冷却得到陶瓷基板。
其中，按质量份数计，步骤1)中三聚氰胺10～30份、铝粉50份、高岭土粉10～20份、氟化钙5～15份。
其中，按质量份数计，步骤2)中的氧化铝粉50份、羟甲基纤维素3～6份、去离子水15～20份和复合烧结助剂15～25份。
其中，步骤3)中陶瓷坯片采用至少2层层叠后进行高温烧结，烧结温度为1280～1540℃，烧结时间2～5小时，干燥处理温度为60～95℃，干燥时间2～12小时。
其中，所述的氧化铝粉为平均粒度1～4μm微观晶型呈片状或短柱状高温煅烧α-氧化铝粉。
本发明的有益效果如下：
(1)本发明通过采用合适的烧结方法和选取合适的烧结助剂，实现氧化铝陶瓷烧结体的致密化，大大提高了氧化铝陶瓷的热导率。
(2)本发明的烧结助剂中三聚氰胺在高温下可以生产氮化铝和氮化碳，增加了陶瓷基板表面的硬度和光泽度。
(3)本发明的烧结助剂可形成低熔点的物相，实现液相烧结，降低烧成温度，促进坯体的致密化。
具体实施方式
下面结合实施例对本发明作进一步的描述。
实施例1
1)复合烧结助剂的制备
将三聚氰胺10克、铝粉50克、高岭土粉10克、氟化钙5克分散于75毫升无水乙醇中，浸泡20分钟；然后在通风橱中边搅拌、边用热风吹，直至无水乙醇完全烘干而得到混合粉体，即制得复合烧结助剂；
2)陶瓷浆料的制备
依次加入平均粒度3.5μm片状微观晶型高温煅烧α-氧化铝粉100克、羟甲基纤维素6克、去离子水15克、硅粉10克和步骤(1)制得的复合烧结助剂15克进行湿法球磨，球磨2小时，制成可凝胶陶瓷浆料，对该陶瓷浆料进行真空搅拌除泡；
3)陶瓷成型
将步骤(2)制得的陶瓷浆料由模具底部压入模具中，自然放置完成凝胶过程；取出陶瓷坯片在温度60℃条件下干燥12小时，然后将陶瓷坯体单片铺撒氧化铝粉叠2层放置承烧板上，放入热压模具中置于热压炉中在1280℃下烧结5小时，最后降温冷却得到陶瓷基板。
实施例2
1)复合烧结助剂的制备
将三聚氰胺20克、铝粉50克、高岭土粉15克、氟化钙10克分散于150毫升无水乙醇中，浸泡20分钟；然后在通风橱中边搅拌、边用热风吹，直至无水乙醇完全烘干而得到混合粉体，即制得复合烧结助剂；
2)陶瓷浆料的制备
依次加入平均粒度1.0μm短柱状微观晶型高温煅烧α-氧化铝粉100克、羟甲基纤维素5克、去离子水18克、硅粉8克和步骤(1)制得的复合烧结助剂25克进行湿法球磨，球磨3小时，制成可凝胶陶瓷浆料，对该陶瓷浆料进行真空搅拌除泡；
3)陶瓷成型
将步骤(2)制得的陶瓷浆料由模具底部压入模具中，自然放置完成凝胶过程；取出陶瓷坯片在温度80℃条件下干燥6小时，然后将陶瓷坯体单片铺撒氧化铝粉叠3层放置承烧板上，放入热压模具中置于热压炉中在1400℃下烧结3小时，最后降温冷却得到陶瓷基板。
实施例3
1)复合烧结助剂的制备
将三聚氰胺30克、铝粉50克、高岭土粉20克、氟化钙15克分散于225毫升无水乙醇中，浸泡20分钟；然后在通风橱中边搅拌、边用热风吹，直至无水乙醇完全烘干而得到混合粉体，即制得复合烧结助剂；
2)陶瓷浆料的制备
依次加入平均粒度4.0μm片状微观晶型高温煅烧α-氧化铝粉100克、羟甲基纤维素6克、去离子水20克和步骤(1)制得的复合烧结助剂25克进行湿法球磨，球磨4小时，制成可凝胶陶瓷浆料，对该陶瓷浆料进行真空搅拌除泡；
3)陶瓷成型
将步骤(2)制得的陶瓷浆料由模具底部压入模具中，自然放置完成凝胶过程；取出陶瓷坯片在温度95℃条件下干燥2小时，然后将陶瓷坯体单片铺撒氧化铝粉叠5层放置承烧板上，放入热压模具中置于热压炉中在1540℃下烧结2小时，最后降温冷却得到陶瓷基板。
对实施例1～3所制得的陶瓷基板进行检测，密度约3.8g/cm3，弯曲强度约240MPa，表面粗糙度约0.5μm，翘曲量＜0.2％。

Claims (3)

1.一种散热用电子陶瓷基板的制备工艺，其特征在于：包括如下步骤：
1)复合烧结助剂的制备
将三聚氰胺、铝粉、高岭土粉、氟化钙分散于无水乙醇中；然后在通风橱中边搅拌、边用热风吹，直至无水乙醇完全烘干而得到混合粉体，即制得复合烧结助剂；按质量份数计，三聚氰胺10～30份、铝粉50份、高岭土粉10～20份、氟化钙5～15份；
2)陶瓷浆料的制备
依次加入氧化铝粉、羟甲基纤维素、去离子水、硅粉和步骤1)制得的复合烧结助剂进行湿法球磨，制成可凝胶陶瓷浆料，对该陶瓷浆料进行真空搅拌除泡；按质量份数计，氧化铝粉50份、羟甲基纤维素3～6份、去离子水15～20份和复合烧结助剂15～25份；
3)陶瓷成型
将步骤2)制得的陶瓷浆料由模具底部压入模具中，自然放置完成凝胶过程；取出陶瓷坯片进行干燥处理，放入热压模具中置于热压炉中进行烧结压制，再降温冷却得到陶瓷基板。
2.根据权利要求1所述的一种散热用电子陶瓷基板的制备工艺，其特征在于：步骤3)中陶瓷坯片采用至少2层层叠后进行高温烧结，烧结温度为1280～1540℃，烧结时间2～5小时，干燥处理温度为60～95℃，干燥时间2～12小时。
3.根据权利要求1所述的一种散热用电子陶瓷基板的制备工艺，其特征在于：所述的氧化铝粉为平均粒度1～4μm微观晶型呈片状或短柱状高温煅烧α-氧化铝粉。
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