CN107188567B - 一种高热导率氮化铝陶瓷的制备方法 - Google Patents

一种高热导率氮化铝陶瓷的制备方法 Download PDF

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CN107188567B
CN107188567B CN201710438497.9A CN201710438497A CN107188567B CN 107188567 B CN107188567 B CN 107188567B CN 201710438497 A CN201710438497 A CN 201710438497A CN 107188567 B CN107188567 B CN 107188567B
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aluminum nitride
nitride ceramic
sintering
thermal conductivity
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CN107188567A (zh
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贺智勇
张启富
王峰
千粉玲
刘秋元
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Beijing Cisri Nmt Advanced Materials & Technology Co ltd
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Abstract

一种高热导率氮化铝陶瓷的制备方法，属于氮化铝陶瓷制备技术领域。以氮化铝粉体为主要原料，以无水乙醇为溶剂，通过引入2～6wt％三元烧结助剂经湿法球磨、干燥、造粒、干压、冷等静压、脱脂、烧结后制备得到高热导率氮化铝陶瓷，所得氮化铝陶瓷的热导率在180～230W·m‑1·K‑1，致密度≥99.3％。优点在于，制备得到的氮化铝陶瓷显微结构均匀；制备工艺简单，便于批量化生产。引入的三元烧结助剂可以较好的对氮化铝陶瓷结构性能进行调控，进而实现高热导率氮化铝陶瓷无压烧结的制备。

Description

一种高热导率氮化铝陶瓷的制备方法
技术领域
本发明属于氮化铝陶瓷制备技术领域，涉及一种高热导率氮化铝陶瓷的制备方法。
背景技术
氮化铝陶瓷具有优异的导热性能，电绝缘性能与耐高温性能，同时也具有较低的介电常数，与硅匹配的线膨胀系数及无毒等特性，从而使其成为目前最理想的基本材料与电子器件封装材料。
高热导率是氮化铝陶瓷工业应用的优势所在。要想实现高热导率陶瓷的制备，必须要满足两个条件：一是氮化铝陶瓷要具有较高的致密度；二是氮化铝陶瓷晶格中的固溶氧含量要尽可能的低。在实际生产中，一般是通过引入稀土化合物(氧化钇、氧化钐、氧化镝、氟化钇、氟化钐等)或碱土金属化合物(氧化钙、氧化硼、氟化钙等)等烧结助剂，在高温下通过与氧化铝反应生成第二相来降低晶格中固溶氧含量，同时促进烧结，进而实现高热导率氮化铝陶瓷的制备。中国专利(CN102030538B)公开了一种氮化铝陶瓷的制备方法及采用该方法制备的氮化铝陶瓷，以氧化钇、氧化钙、氟化钙、氧化镝中的一种或多种作为烧结助剂，制备得到了系列氮化铝陶瓷，其中以氧化钇与氧化钙作为复合烧结助剂时制备得到的氮化铝陶瓷的热导率最高(180W·m-1·K-1)。Tohru等(Scripta Materialia,2005,52:583-586)以氧化钇作为烧结助剂，制备得到了热导率为164.7W·m-1·K-1的氮化铝陶瓷。YU等(Journal of the European Ceramic Society,2002,22:247-250)以氧化钇与氟化钙作为烧结助剂，制备得到了热导率为147W·m-1·K-1的氮化铝陶瓷。可见，氮化铝陶瓷的热导率与烧结助剂选择具有很重要的关系。因此，寻找、开发适用于氮化铝陶瓷的多元体系烧结助剂对于高热导率氮化铝陶瓷的制备至关重要。
发明内容
本发明的目的在于提供一种可用于氮化铝陶瓷制备用三元烧结助剂(氧化铈+其它稀土化合物中的一种+碱土金属化合物中的一种)及其制备方法，可以实现高热导率氮化铝陶瓷的无压烧结制备。在相同的条件下，通过引入三元烧结助剂制备得到氮化铝陶瓷的性能优于引入单一及二元复合烧结助剂制备得到氮化铝陶瓷的性能。
本发明的技术方案是：一种高热导率氮化铝陶瓷的制备方法，具体工艺过程包括以下步骤：
1)配料：将氮化铝粉与烧结助剂按比例称取后置于球磨罐中，加入无水乙醇与氧化锆磨球，经球磨后获得混合均匀浆料，其中球磨转速为150～180r/min；
2)成型：将浆料置于50～70℃的低温烘箱内，干燥后研磨、破碎，然后加入适量的粘结剂混合均匀，再将粉体过筛。将粉体装入钢制模具中于压力机上进行一次成型，然后再将成型的生坯塑封后放入冷等静压机内二次加压成型，最终得到氮化铝陶瓷生坯；
3)脱脂：将氮化铝生坯放置于马弗炉内，在空气气氛下进行脱脂；
4)烧结：将脱脂后生坯放置于高温烧结炉中，于氮气氛围下于1800～1900℃对样品进行烧结，保温时间为2～6h。烧结结束后以1～5℃/min降温速率降至1600～1700℃后，再随炉冷却至室温，得到氮化铝陶瓷。
优选的是，步骤(1)所述的烧结助剂为三元复合烧结助剂，其中必含有氧化铈，稀土化合物氧化钇、氧化钐、氧化镝、氟化钇、氟化钐等中的一种，碱土金属化合物氧化钙、氧化硼、氟化钙等中的一种。其中，氧化铈、其它稀土化合物及碱土金属化合物引入质量分别占粉体总质量的0.5～1.5％，1～3％，0.5～1.5％；
优选的是，步骤(1)所述的配料过程中，为实现陶瓷粉料快速混合均匀，一般陶瓷粉料、磨球及无水乙醇的质量比应为1:1:1～1:2:3；
优选的是，步骤(2)成型过程中为保证成型坯体结构的均匀性，成型工艺如下：一次成型压力为20～40MPa，保压时间1～3min；二次成型过程中，在80～120MPa保压1-6min，在200～240MPa保压1～6min；升、降压速率均在10-20MPa/min范围内；
优选的是，步骤(3)中所述的脱脂工艺必须要保证脱脂过程中坯体内不能产生裂纹等缺陷，以保证后继烧结样品显微结构的均匀性；脱脂后坯体内的粘结剂要完全分解，分解残留碳的含量要尽可能的低，以减少对样品结构及性能的影响，鉴于以上考虑，坯体的脱脂温度范围一般在450～600℃，升温速率≤4℃/min，保温时间2～6h；
优选的是，步骤(4)中所述的烧结工艺必须要保证坯体的致密化烧结，同时也要避免烧结过程中发生弯曲变形等，一般烧结温度应控制在1800～1900℃，升温速率≤8℃/min，保温时间2～6h；保温结束后先温控降温至1600～1700℃，降温速率为1～5℃/min，再随炉冷却至室温。得到氮化铝陶瓷的热导率在180～230W·m-1·K-1，致密度≥99.3％。
本发明的优点在于，所得氮化铝陶瓷的热导率在180～230W·m-1·K-1，致密度≥99.3％。制备得到的氮化铝陶瓷显微结构均匀；制备工艺简单，便于批量化生产。引入的三元烧结助剂可以较好的对氮化铝陶瓷结构性能进行调控，进而实现高热导率氮化铝陶瓷无压烧结的制备。
附图说明
图1为高热导率氮化铝陶瓷显微结构图。
具体实施方式
1按质量比96:2.5:1:0.5依次准确称取氮化铝粉、氧化钐、氧化铈、氟化钙粉末置于尼龙球磨罐中，同时添加质量比0.3％硬脂酸作为分散剂，加入无水乙醇及氧化锆球为球磨介质，湿法球磨4h。其中粉料、无水乙醇及氧化锆球的质量比为1:1:2，球磨转速为160r/min。浆料干燥后的得到混合均匀的物料；
2添加聚乙烯醇缩丁醛溶液为粘结剂，与混合物料混合均匀，过80目网筛后，将粉体置于钢制模具中于压力机上压制成生坯，成型压力为40MPa；然后将生坯塑封包装，置于冷等静压机中进行二次压制，压制成型压力为100MPa保压60s，220MPa保压时间为180s；
3将成型后生坯置于脱脂炉内于空气气氛中进行排胶。升温速率为2℃/min，胶温度为500℃，保温时间为4h；
4脱脂后生坯放入坩埚中，置于高温烧结炉内氮气氛围下进行烧结，以一定的速率升温至1860℃，保温时间为4h，烧结结束后再以一定的速率降温至1700℃后再随炉冷却至室温，得到高热导率氮化铝陶瓷样品；
采用此工艺制备得到的氮化铝陶瓷样品显微结构致密(见附图1)，体积密度为3.3g/cm3，气孔率为0.6％，致密度为99.4％，热导率为201.3W·K-1·m-1，较相同条件下单一(4wt％氧化钐)及二元助烧剂(3wt％氧化钐-1wt％氧化铈；3.5wt％氧化钐-0.5wt％氟化钙)制备得到的氮化铝陶瓷样品的热导率高。

Claims (4)

1.一种高热导率氮化铝陶瓷的制备方法，其特征在于，包括如下步骤：
1)配料：按重量百分数比例称取氮化铝粉与以氧化铈0.5～1％+其它稀土化合物1～2.5％+碱土金属化合物0.5～1.5％组成的三元烧结助剂，然后采用湿法混料工艺制备得到混合均匀的浆料，其中湿法混料用的液体介质为无水乙醇，球磨转速为150～180r/min；
所述的三元烧结助剂中的其它稀土化合物为氧化钇、氧化钐、氧化镝、氟化钇、氟化钐中的一种；碱土金属化合物为氟化钙；
2)成型：将步骤1)中所得浆料置于50～70℃的低温烘箱内干燥，然后加入粘结剂造粒、过筛、干压后再经分步加压等静压成型工艺制得生坯；
3)脱脂：将步骤2)中所得生坯置于马弗炉中，于450～600℃保温2～6h；
4)烧结：将步骤3)中热处理后生坯置于高温烧结炉中，于氮气氛围下在1860～1900℃保温2～4h；烧结结束后温控降温至1600～1700℃，降温速率为1～5℃/min，再随炉冷却至室温，得到氮化铝陶瓷；采用该工艺制备的氮化铝陶瓷的热导率在180～220W·m-1·K-1，致密度≥99.3％。
2.根据权利要求1所述的方法，其特征在于，步骤1)中烧结助剂的质量比均是针对混合粉体而言，混合粉体为三元烧结助剂与氮化铝粉体的混合。
3.根据权利要求1所述的方法，其特征在于，所述步骤2)中所用粘结剂包括但不限于石蜡、聚乙烯醇缩丁醛有机粘结剂，引入质量比占混合粉体质量的1～3％。
4.根据权利要求1所述的方法，其特征在于，所述步骤2)中所用的分步加压冷等静压工艺参数为：在80～120MPa保压1～6min，200～240MPa保压1～6min，其中升压与降压速率均在10～20MPa/min范围内。
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