CN107399974A - 一种添加氟化物制备高导热氮化硅陶瓷的方法 - Google Patents
一种添加氟化物制备高导热氮化硅陶瓷的方法 Download PDFInfo
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Abstract
该发明属于陶瓷材料制备技术领域,涉及一种添加氟化物制备高导热氮化硅陶瓷的方法。本发明中以α‑Si3N4为原料,以氮化硅镁和稀土氟化物的混合物为烧结助剂,助剂的添加量为1~15wt%。首先用纳米TiC对Si3N4粉末进行表面改性的预处理,将处理后的原料、助剂、粘结剂、晶种、消泡剂、溶剂放入球磨罐中混合均匀,再加入分散剂进行二次球磨,球磨后的混合浆料经过烘干、造粒、成型、烧结、热处理过程制备得到高导热氮化硅陶瓷。本发明通过添加稀土金属氟化物来避免助剂中的氧进入氮化硅陶瓷的晶格中,减少了晶格氧杂质含量对陶瓷热导率的不利影响,制备得到的氮化硅陶瓷具有较高的热导率,在电子封装材料领域具有巨大的应用潜力。
Description
技术领域
本发明属于陶瓷材料制备技术领域,具体涉及一种添加氟化物制备高导热氮化硅陶瓷的方法。
背景技术
随着集成电路和功能器件的不断发展,人们对电路工作温度的散热问题提出了更高的要求。要解决这一严重的问题,必须采用新材料通过衬底进行散热。目前可用作电子基片的陶瓷材料有Al2O3、BeO、AlN等,其中Al2O3的热导率最高仅为31.7W/(m·K),难以满足集成技术快速发展的要求。陶瓷中BeO的导热率最高,但BeO的一个致命弱点就是其毒性很大,对于生产操作人员带来了不便,在工业生产中的使用受到了很大的限制。AlN陶瓷是一种优良的高导热材料,其热导率的理论值与BeO(320W/(m·K))相近,但AlN存在易氧化、抗水性差等问题,这影响了其应用范围。在不断寻找高导热陶瓷的研究中,Haggerty 等人计算得出Si3N4晶体的热导率可高达 320 W/(m·K),并有着比AlN更高的机械强度。抗水性比AlN好,可以水基处理,降低了生产成本。此外具有电绝缘性好、无毒、强度高、抗氧化性好、线膨胀系数小、热稳定性好等优异的性能,能够在诸多恶劣的环境中使用,是一种理想的电子封装材料。
Si3N4是共健化合物,自扩散系数低,固相烧结很难得到高致密度的Si3N4陶瓷。目前Si3N4多采用液相烧结方式,在烧结过程中添加烧结助剂,使其在高温下与Si3N4表面的二氧化硅生成液相促进Si3N4的致密化。Si3N4陶瓷的中的杂质含量、晶界相、晶格缺陷等都是影响导热率的重要因素,其中晶格氧对声子散射十分显著,是影响Si3N4陶瓷热导率最主要的因素。要获得高热导率的氮化硅陶瓷,应选择合适的助剂、减少晶界相含量、提高原料的纯度、促进晶粒长大与发育完整等。要减小烧结助剂对氮化硅陶瓷热导率的影响,应选择合适的助剂量,过多的助剂会引入过多的杂质。同时避免引入Al元素,因为β-Si3N4有一定的溶Al能力,Al溶入晶格后生成固溶体,加剧了对声子的散射,降低热导率。本文采用氮化硅镁和稀土金属的氟化物作为烧结助剂,减少了传统陶瓷中氧化物助剂的氧杂质对陶瓷热导率的影响。
发明内容
本发明提供一种添加氟化物制备高导热氮化硅陶瓷的方法,该方法通过添加稀土金属氟化物来避免助剂中的氧进入氮化硅陶瓷的晶格中,减少了晶格氧杂质含量对陶瓷的热导率产生的不利影响,制备得到的氮化硅陶瓷具有较高的热导率,在电子封装材料领域具有巨大的应用潜力。本发明所采用的技术方案是:
(1)以α-Si3N4为原料,以氮化硅镁和稀土氟化物的混合物为烧结助剂,助剂的添加量为1~15wt%;
(2)首先用纳米TiC对原料Si3N4粉末进行表面改性的预处理,将处理后的原料、烧结助剂、粘结剂、晶种、消泡剂、溶剂放入球磨罐中混合均匀,再加入分散剂进行二次球磨,球磨后的混合浆料经过烘干、造粒、成型、烧结、热处理过程制备得到高导热氮化硅陶瓷。
进一步的,所述的Si3N4原料的α相>90%,纯度>99%,粒度为0.4~1.2μm。
进一步的,所述的稀土金属氟化物为YF3、LaF3、YbF3、EuF3、SmF3、CeF3或NdF3中的任一种或一种以上。
进一步的,所述粘结剂为聚乙烯醇缩丁醛或聚乙烯醇中的任一种,晶种为β- Si3N4粉末,消泡剂为磷酸三丁酯,分散剂为丙烯酸树脂,用来调节pH值使浆料具有良好的流动性,溶剂为无水乙醇和丁酮,上述试剂的纯度均为分析纯以上。
进一步的,聚乙烯醇缩丁醛或聚乙烯醇中任一种的添加量为0.5~4wt%,β-Si3N4的添加量为0.2~10wt%,粒度为1.5~5μm, β相>70%,纯度>99%,无水乙醇和丁酮的比例为1:1。
进一步的,所述成型方式为干压成型、等静压成型或流延成型中的任一种,烧结条件为1750~1900℃保温2~24h,烧结过程采用Si3N4-BN的混合粉末进行埋粉,热处理条件为1400~1700℃保温4~48h,烧结和热处理过程中始终以氮气气氛进行保护,热处理结束后随炉冷却至室温。
本发明的有益效果:本发明以氮化硅镁和稀土金属氟化物的为烧结助剂,避免了助剂中的氧进入到氮化硅晶格中,减少了晶格氧对氮化硅陶瓷热导率的影响。制备得到的氮化硅陶瓷不仅具有较高的热导率,同时具有高机械强度、耐水性、抗氧化性等优点,成为电子封装领域具有巨大潜力的一种材料。
具体实施方式
下面结合实施例对本发明的技术方案做详细说明。
实施例
1
将纳米TiC处理的α-Si3N4(α=92%,D50=0.55μm)89.5g、氮化硅镁5g、氟化钇5g、β- Si3N4
(D50=1.5μm) 0.5g、聚乙烯醇、磷酸三丁脂、无水乙醇与丁酮的混合溶液放入尼龙球磨罐中球磨24h,磨介球为氮化硅球。再加入丙烯酸树脂进行二次球磨24h,球磨结束后65℃烘干、过40目筛。将造粒粉进行等静压成型,压力为400MPa。将坯体在1900℃保温8h,之后在1400℃热处理24h。随炉冷却后得到氮化硅陶瓷,导热率达102W/(m·K)。
实施例
2
将87g处理后的α- Si3N4粉末(α=93.7%,D50=0.67μm)、5g氮化硅镁、3g氟化铷、3g氟化钐、2g β-Si3N4
(D50=2.5μm)粉末、聚乙烯醇缩丁醛、磷酸三丁脂、无水乙醇与丁酮的混合溶液的混合物在球磨罐中磨18h后加入丙烯酸树脂再磨20h。将浆料在60℃的温度下干燥后过40目筛。先20MPa干压成型后再200PMa等静压。放入烧结炉中,在1950℃的温度下保温15h,之后降温至1300℃保温10h,随炉冷却。得到的氮化硅陶瓷的热导率高达143 W/(m·K)。
实施例
3
87g处理后的α-Si3N4粉末(α=94.2%,D50=0.89μm)、4g氮化硅镁、4g氟化镱、5g β-Si3N4
(D50=4.5μm)粉末、聚乙烯醇缩丁醛、磷酸三丁脂、无水乙醇与丁酮的混合溶液的混合物放入尼龙球磨罐中球磨20h,再放入丙烯酸树脂后二次球磨20h得到混合浆料。将浆料经流延成型后放入烧结炉中1750℃保温24h,之后将温度降至1650℃热处理40h后随炉冷却。得到的氮化硅陶瓷的热导率为125 W/(m·K)。
Claims (8)
1.一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于:
(1)以α-Si3N4为原料,以氮化硅镁和稀土氟化物的混合物为烧结助剂,助剂的添加量为1~15wt%;
(2)首先用纳米TiC对原料Si3N4粉末进行表面改性的预处理,将处理后的原料、烧结助剂、粘结剂、晶种、消泡剂、溶剂放入球磨罐中混合均匀,再加入分散剂进行二次球磨,球磨后的混合浆料经过烘干、造粒、成型、烧结、热处理过程制备得到高导热氮化硅陶瓷。
2.按照权利要求1所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,所述的Si3N4原料的α相>90%,纯度>99%,粒度为0.4~1.2μm。
3.按照权利要求1所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,所述的稀土氟化物为YF3、LaF3、YbF3、EuF3、SmF3、CeF3或NdF3中的任一种或一种以上。
4.按照权利要求1所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,所述粘结剂为聚乙烯醇缩丁醛或聚乙烯醇中的任一种,晶种为β相氮化硅粉末,消泡剂为磷酸三丁酯,分散剂为丙烯酸树脂,用来调节pH值使浆料具有良好的流动性,溶剂为无水乙醇和丁酮。
5.按照权利要求4所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,聚乙烯醇缩丁醛或聚乙烯醇中任一种的添加量为0.5~4wt%,β相氮化硅的添加量为0.2~10wt%。
6.按照权利要求4所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,所述β相氮化硅晶种的粒度为1.5~5μm, β相>70%,纯度>99%。
7.按照权利要求4所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,所述无水乙醇和丁酮的比例为1:1。
8.按照权利要求1所述的一种添加氟化物制备高导热氮化硅陶瓷的方法,其特征在于,成型方式为干压成型、等静压成型或流延成型中的任一种,烧结条件为1750~1900℃保温2~24h,烧结过程采用Si3N4-BN的混合粉末进行埋粉,热处理条件为1400~1700℃保温4~48h,烧结和热处理过程中始终以氮气气氛进行保护,热处理结束后随炉冷却至室温。
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