CN113213944A - 一种BN纳米片强韧化高导热AlN陶瓷基板和制备方法 - Google Patents
一种BN纳米片强韧化高导热AlN陶瓷基板和制备方法 Download PDFInfo
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Abstract
本发明提供了一种BN纳米片强韧化高导热AlN陶瓷基板和制备方法,包括以下步骤:步骤S01:制备BN纳米片强韧化高导热AlN陶瓷流延浆料;步骤S02:制备BN纳米片强韧化高导热AlN陶瓷素片;步骤S03:将步骤S02制得的陶瓷素片氮气气氛下烧结6‑8h,得产品。本发明采用机械球磨法剥离氮化硼纳米片,一步法制备氮化硼纳米片强韧化氮化铝陶瓷的浆料,通过流延、排胶和烧结等工艺得到陶瓷基板。BN纳米片的添加旨在不影响氮化铝基板导热性能的基础上,通过片状纳米颗粒的钉扎和裂纹偏转效应,大幅提高陶瓷基板对断裂能的消耗,从而改善氮化铝陶瓷的力学性能,扩大氮化铝陶瓷基板的应用领域。
Description
技术领域
本发明属于纳米强韧化陶瓷基片材料领域,涉及一种BN纳米片强韧化高导热AlN陶瓷基板和制备方法。
背景技术
大多数陶瓷材料是离子键或共价键极强的材料,具有较高的绝缘性能和优异的高频特性,同时线膨胀系数与电子元器件非常相近,化学性能非常稳定且热导率高,凭借其优异的综合性能,陶瓷材料正逐步成为电子封装中常用的基片材料。长期以来,绝大多数大功率混合集成电路的基板材料一直沿用Al2O3和BeO陶瓷,但Al2O3基板的热导率低,热膨胀系数和Si不太匹配;BeO虽然具有优良的综合性能,但其较高的生产成本和剧毒的缺点限制了它的应用推广。
氮化铝(AlN)作为一种综合性能优良新型的先进陶瓷材料,其理论热导率高达320W/(m·K),工业上实际制备的多晶氮化铝的热导率也可达100~250 W/(m),该数值是传统基片材料氧化铝热导率的5倍~10倍。与其它几种陶瓷材料相较,氮化铝陶瓷综合性能优良,非常适用于半导体基片和结构封装材料,在电子工业中的应用潜力非常巨大。但是,其力学性能较差,弯曲强度为350MPa左右,断裂韧性为3 MPa·m1/2左右,这使氮化铝基板的可加工性较差,且在应对冷热交换频繁的环境时的可靠性较低,成为限制其应用的重要因素。
发明内容
1、所要解决的技术问题:
氮化铝(AlN)作为一种综合性能优良新型的先进陶瓷材料,但是,其力学性能较差,这使氮化铝基板的可加工性较差,且在应对冷热交换频繁的环境时的可靠性较低。
2、技术方案:
为了解决以上问题,本发明提供了一种BN纳米片强韧化高导热AlN陶瓷基板的制备方法,包括以下步骤:步骤S01:制备BN纳米片强韧化高导热AlN陶瓷流延浆料;步骤S02:制备BN纳米片强韧化高导热AlN陶瓷素片;步骤S03:将步骤S02制得的陶瓷素片氮气气氛下烧结6-8h,得产品。
步骤S01具体为:将氮化硼粉体、聚乙二醇、蔗糖、无水乙醇进行湿法球磨,球磨转速为300r/min,球磨时间18h;随后加入氮化铝粉、烧结助剂氧化钇粉、聚乙烯醇缩丁醛和无水乙醇混合后再次球磨,二次球磨转速为200r/min,球磨时间为6h,球磨后料浆进行过筛除泡后得到流延浆料。
所述氮化铝粉的平均粒径为1μm。
所述烧结助剂氧化钇粉的平均粒径为800nm。
所述聚乙烯醇缩丁醛的聚合度为2000。
氮化硼粉体、聚乙二醇、蔗糖、无水乙醇按质量比为1:0.1:0.1:20;氮化铝粉、氧化钇粉、聚乙烯醇缩丁醛和乙醇按照1:0.04:3: 20;纳米BN的质量比为2wt%。
步骤S02具体为:将步骤S01制得的流延浆料经过流延工艺后得到复相陶瓷胶片,之后进入脱脂炉内进行排胶,排胶时间8h,后得到复相陶瓷素片。
步骤S03中烧结过程为:陶瓷基板素片于氮气气氛0.2MPa、1850℃条件下烧结6-8h。
升温速度为0-1400℃,升温速率为10℃/分钟,1400-1600℃升温速率为3℃/分钟,1600℃以上升温速率为1℃/分钟。
一种BN纳米片强韧化高导热AlN陶瓷基板,通过权利要求1-9任一项权利要求所述的方法制得。
3、有益效果:
本发明选取层状氮化硼粉体作为原料,通过机械球磨进行层间剥离获得纳米片状BN,可以显著降低纳米颗粒的原料成本;同时,一步法球磨的工艺可以优化BN纳米片的分散情况,减少其大面积团聚的发生。
本发明利用层间剥离法引入的BN纳米片具有较高的纯度和导热系数,且具有优异的增强特性,与基体AlN颗粒结合良好,借助纳米颗粒钉扎和裂纹偏转作用,可以显著提高氮化铝陶瓷的力学性能。
本发明通过对原料制备和烧结工艺进行控制,掌握BN纳米片的组织形貌和分散情况,以及其在氮化铝基体中的分布情况,进而对复相陶瓷的显微组织结构实现调控,最终制得结构致密、导热性能和力学性能优异的陶瓷基板。
附图说明
图1为本发明所述BN纳米片强韧化高导热AlN陶瓷基板的制备工艺流程。
图2为实施例1中BN纳米片强韧化高导热AlN陶瓷的低倍SEM图。
图3为实施例1中BN纳米片强韧化高导热AlN陶瓷的高倍SEM图。
具体实施方式
下面通过实施例来对本发明进行详细说明。
实施例1
将氮化硼粉体(平均粒径为1μm)、聚乙二醇(聚合度4000)、蔗糖、无水乙醇按质量比为1:0.1:0.1:20进行湿法球磨,球磨转速为300r/min,球磨时间18h;随后加入氮化铝粉(平均粒径为1μm)、烧结助剂氧化钇粉(平均粒径为800nm)、聚乙烯醇缩丁醛(聚合度为2000)和无水乙醇按照1:0.04:3: 20质量比进行混合再次球磨,二次球磨转速为200r/min,球磨时间为6h,球磨后料浆进行过筛除泡后得到流延浆料;其中氮化硼的质量比为2wt%;流延排胶完成后的陶瓷素片于氮气气氛0.2MPa、1850℃条件下烧结6h,得产品;升温速度为0-1400℃升温速率为10℃/分钟,1400-1600℃升温速率为3℃/分钟, 1600℃以上升温速率为1℃/分钟。工艺流程如图1所示,所得BN纳米片强韧化高导热AlN陶瓷基板的性能为:相对密度为99.7%;抗弯强度为422.3MPa;断裂韧性为:5.71MPa·m1/2;热导率为186.1W/(m·K)。图2和图3为BN纳米片强韧化高导热AlN陶瓷基板的断口SEM图,基板组织结构致密,在高倍放大图片中有许多片状纳米BN,其钉扎效应、裂纹偏转和裂纹延长会改善陶瓷基板对应力的耐受能力,改善基板材料的力学性能。
实施例2
将氮化硼粉体(平均粒径为1μm)、聚乙二醇(聚合度4000)、蔗糖、无水乙醇按质量比为1:0.1:0.1:20进行湿法球磨,球磨转速为300r/min,球磨时间18h;随后加入氮化铝粉(平均粒径为1μm)、烧结助剂氧化钇粉(平均粒径为800nm)、聚乙烯醇缩丁醛(聚合度为2000)和无水乙醇按照1:0.04:3: 20质量比进行混合再次球磨,二次球磨转速为200r/min,球磨时间为6h,球磨后料浆进行过筛除泡后得到流延浆料;其中氮化硼的质量比为3wt%;流延排胶完成后的陶瓷素片于氮气气氛0.2MPa、1800℃条件下烧结8h,得产品;升温速度为0-1400℃升温速率为10℃/分钟,1400-1600℃升温速率为3℃/分钟, 1600℃以上升温速率为1℃/分钟。工艺流程如图1所示,所得BN纳米片强韧化高导热AlN陶瓷基板的性能为:相对密度为99.3%;抗弯强度为376.78MPa;断裂韧性为:5.21MPa·m1/2;热导率为176.9W/(m·K)。
所述实施例1、2中所得的BN纳米片强韧化高导热AlN陶瓷基板的相对密度均大于99%,热导率均大于175W/(m·K),抗弯强度均高于370MPa;断裂韧性高于5.0MPa·m1/2,且微观组织结构良好,完全达到了商用高导热基板的要求,断裂韧性更是远高于市售的氮化铝基板,改善了氮化铝陶瓷基板的可加工性和可靠性,因此本发明提供了一种BN纳米片强韧化高导热AlN陶瓷基板的制备方法。
对比例1
将氮化铝粉(平均粒径为1μm)、烧结助剂氧化钇粉(平均粒径为800nm)、聚乙烯醇缩丁醛(聚合度为2000)和无水乙醇按照1:0.04:3: 20质量比进行混合球磨,球磨转速为200r/min,球磨时间为12h,球磨后料浆进行过筛除泡后得到流延浆料;流延排胶完成后的陶瓷素片于氮气气氛0.2MPa、1850℃条件下烧结8h,得产品;升温速度为0-1400℃升温速率为10℃/分钟,1400-1600℃升温速率为3℃/分钟, 1600℃以上升温速率为1℃/分钟。所得高导热AlN陶瓷基板的性能为:相对密度为98.2%;抗弯强度为321.42MPa;断裂韧性为:2.76MPa·m1/2;热导率为168.2W/(m·K)。相比较实施例1中的陶瓷基板的各项性能,未添加BN纳米片作为强韧化手段的纯氮化铝基板的力学性能和热学性能均较低,断裂韧性更是几乎为实施例1中的一半。
Claims (10)
1.一种BN纳米片强韧化高导热AlN陶瓷基板的制备方法,包括以下步骤:步骤S01:制备BN纳米片强韧化高导热AlN陶瓷流延浆料;步骤S02:制备BN纳米片强韧化高导热AlN陶瓷素片;步骤S03:将步骤S02制得的陶瓷素片氮气气氛下烧结6-8h,得产品。
2.如权利要求1所述的方法,其特征在于:步骤S01具体为:将氮化硼粉体、聚乙二醇、蔗糖、无水乙醇进行湿法球磨,球磨转速为300r/min,球磨时间18h;随后加入氮化铝粉、烧结助剂氧化钇粉、聚乙烯醇缩丁醛和无水乙醇混合后再次球磨,二次球磨转速为200r/min,球磨时间为6h,球磨后料浆进行过筛除泡后得到流延浆料。
3.如权利要求2所述的方法,其特征在于:所述氮化铝粉的平均粒径为1μm。
4.如权利要求2所述的方法,其特征在于:所述烧结助剂氧化钇粉的平均粒径为800nm。
5.如权利要求2所述的方法,其特征在于;所述聚乙烯醇缩丁醛的聚合度为2000。
6.如权利要求2-5任一项权利要求所述的方法,其特征在于:氮化硼粉体、聚乙二醇、蔗糖、无水乙醇按质量比为1:0.1:0.1:20;氮化铝粉、氧化钇粉、聚乙烯醇缩丁醛和乙醇按照1:0.04:3: 20;纳米BN的质量比为2wt%。
7.如权利要求1所述的方法,其特征在于:步骤S02具体为:将步骤S01制得的流延浆料经过流延工艺后得到复相陶瓷胶片,之后进入脱脂炉内进行排胶,排胶时间8h,后得到复相陶瓷素片。
8.如权利要求1所述的方法,其特征在于:步骤S03中烧结过程为:陶瓷基板素片于氮气气氛0.2MPa、1850℃条件下烧结6-8h。
9.如权利要求8所述的方法,其特征在于:升温速度为0-1400℃,升温速率为10℃/分钟,1400-1600℃升温速率为3℃/分钟, 1600℃以上升温速率为1℃/分钟。
10.一种BN纳米片强韧化高导热AlN陶瓷基板,其特征在于:通过权利要求1-9任一项权利要求所述的方法制得。
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