CN115231928A - 一种氮化铝陶瓷基板及其制备方法 - Google Patents

一种氮化铝陶瓷基板及其制备方法 Download PDF

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CN115231928A
CN115231928A CN202210614093.1A CN202210614093A CN115231928A CN 115231928 A CN115231928 A CN 115231928A CN 202210614093 A CN202210614093 A CN 202210614093A CN 115231928 A CN115231928 A CN 115231928A
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aluminum nitride
ceramic substrate
sintering aid
nitride ceramic
main phase
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杨治华
贺云鹏
周国相
张砚召
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Chongqing Research Institute of Harbin Institute of Technology
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Abstract

本发明提供一种氮化铝陶瓷基板，其由无机粉体烧结获得，无机粉体包括主相材料和烧结助剂，主相材料为氮化铝粉体，其粒径分布按体积百分比包括：0.05‑0.2μm 16.26‑18.93％、0.2‑0.5μm 17.10‑18.21％、0.5‑1μm17.94‑17.96％、1‑2μm 22.55‑23.84％、2‑3.5μm 22.37‑24.86％。上述氮化铝陶瓷基板的制备方法包括如下步骤：将主相材料和烧结助剂球磨获得流延浆料；将流延浆料成型、排胶，在0.1‑0.3MPa的保护气压力下以1760‑1800℃保温烧结4‑6h。本发明通过主相材料和烧结助剂的配合提高了氮化铝陶瓷基板的热导率。

Description

一种氮化铝陶瓷基板及其制备方法
技术领域
本发明涉及半导体封装的技术领域，具体涉及一种氮化铝陶瓷基板及其制备方法。
背景技术
随着功率器件特别是第三代半导体的崛起与应用，半导体器件逐渐向大功率、小型化、集成化、多功能等方向发展，对封装基板性能也提出了更高要求。功率器件几乎用于所有的电子制造业，目前功率半导体的应用范围已从传统的工业控制和4C产业(计算机、通信、消费类电子产品和汽车)，扩展到新能源、轨道交通、智能电网等新领域。而功率器件的制造离不开电子封装，电子封装为芯片和电子元件提供机械支撑和环境保护，实现电互联和信号传输，提供快速散热通道，让器件能更好的发挥各项性能。
电子封装用基板材料要求具有成本低、易加工、高导热性与绝缘性等特性，而陶瓷基板材料由于具有耐高温、耐腐蚀、机械强度高以及高膨胀系数的优点，成为电子封装材料的首选。但是航空航天、武器装备、深海钻探、汽车电子领域等的封装陶瓷基板的使用环境恶劣，对封装陶瓷基板的性能提出了新要求。
现有的氮化铝陶瓷由于具有高热导率、低介电常数和优良的电绝缘性、耐腐蚀性、无毒、比强度高的优点，且具有与硅相匹配的热膨胀系数、机械、电学性能优良，被认为是新一代大规模集成电路、半导体模块电路及大功率期间的理想散热和封装材料。但是，目前市场上已推出的氮化铝陶瓷基板产品的最大热导率约在170W/(m·K)左右，与其319W/(m·K)的理论热导率值相差较多，限制了氮化铝陶瓷基板的使用。
发明内容
本发明要解决的技术问题在于克服现有技术中氮化铝陶瓷基板产品的最大热导率约在170W/(m·K)左右，与其319W/(m·K)的理论热导率值相差较多，限制了氮化铝陶瓷基板的使用，氮化铝陶瓷基板热导率有待进一步提升的缺陷。
为此，本发明提供一种氮化铝陶瓷基板，其由无机粉体烧结获得，所述无机粉体包括体积占比为94.2-96.8％的主相材料和体积占比为3.2-5.8％的烧结助剂，所述主相材料为氮化铝粉体，所述氮化铝粉体的粒径分布按体积百分比包括：
Figure BDA0003672958320000021
可选的，所述烧结助剂包括体积占比分别为22-44％、56-78％的碱金属和/或碱土金属化合物、稀土金属化合物。
可选的，所述烧结助剂的D50粒径为0.2-0.5μm。
可选的，所述碱金属和/或碱土金属化合物选自CaO、CaC2、CaF2、SrO及Li2CO3中的至少一种。
可选的，所述稀土金属化合物选自Y2O3、Dy2O3、Gd2O3及YF3中的至少一种。
本发明还提供前述的一种氮化铝陶瓷基板的制备方法，包括如下步骤：
将主相材料和烧结助剂球磨获得流延浆料；
将流延浆料成型、排胶，然后在0.1-0.3MPa的保护气压力下以1760-1800℃烧结4-6h。
可选的，所述排胶时间为4-8h，排胶温度为600℃。
可选的，球磨的步骤包括：将无机粉体、分散剂和溶剂球磨分散12-20h，然后依次加入粘接剂和增塑剂球磨20-30h获得流延浆料。
可选的，所述溶剂为乙醇和丁酮的二元共沸混合物；
和/或，所述溶剂占主相材料和烧结助剂总重量的35-45％。
可选的，所述分散剂选自油酸和/或鱼油；
和/或，所述分散剂占主相材料和烧结助剂总重量的1-2％。
可选的，前述的氮化铝陶瓷基板的制备方法满足以下(1)-(4)中的至少一项：
(1)所述粘接剂选自聚乙烯醇缩丁醛和/或聚甲基丙烯酸甲酯；
(2)所述粘接剂占主相材料和烧结助剂总重量的6.5-10％；
(3)所述增塑剂选自邻苯二甲酸丁苄酯和/或邻苯二甲酸二丁酯；
(4)所述增塑剂占主相材料和烧结助剂总重量的4-7％。
本发明技术方案，具有如下优点：
1.本发明提供的一种氮化铝陶瓷基板，通过搭配不同尺寸的氮化铝粉体颗粒以及采用烧结助剂获得，通过本发明中特定配比的氮化铝粉体颗粒和烧结助剂的配合，提高了氮化铝陶瓷基板的热导率。其中氮化铝粉体的粒径分布有益于实现密致的堆积状态；烧结助剂一方面与氮化铝颗粒表面的氧形成低共熔液相，实现液相烧结，促进致密化，另一方面通过与氮化铝中的氧杂质反应，实现晶格的净化。
2.本发明提供的一种氮化铝陶瓷基板的制备方法，采用气压烧结方式，保护气既作为保护气氛也作为传递压力的介质，以便于抑制氮化铝在高温下的分解和失重，从而提高氮化铝陶瓷基板的力学、热学性能。
3.本发明提供的一种氮化铝陶瓷基板的制备方法，现有技术在制备氮化铝陶瓷基板时，由于杂质的存在容易产生与氮化铝基体连续的第二相，限制氮化铝陶瓷基体的热导率的提高，而碱金属和/或碱土金属化合物和稀土金属化合物的复合烧结助剂的添加，能够使第二相减少至成为孤立相或完全消除第二相，有助于氮化铝陶瓷基板热导率的提高。
附图说明
为了更清楚地说明本发明具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本发明的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1是本发明实施例3的氮化铝陶瓷基板的断面二次电子微观结构图；
图2是本发明实施例3的氮化铝陶瓷基板的背散射电子微观结构图。
具体实施方式
提供下述实施例是为了更好地进一步理解本发明，并不局限于所述最佳实施方式，不对本发明的内容和保护范围构成限制，任何人在本发明的启示下或是将本发明与其他现有技术的特征进行组合而得出的任何与本发明相同或相近似的产品，均落在本发明的保护范围之内。
实施例中未注明具体实验步骤或条件者，按照本领域内的文献所描述的常规实验步骤的操作或条件即可进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规试剂产品。
乙醇和丁酮的二元共沸混合中乙醇和丁酮的质量比为46:54；其中乙醇为无水乙醇，无水乙醇型号为AR(沪试)，≥99.7％，购自国药试剂；丁酮型号为AR(沪试)，≥99.0％，购自国药试剂；
油酸型号为AR(沪试)，购自国药试剂；
鱼油购自国药试剂；
聚乙烯醇缩丁醛粘度为15-35mm2/s，购自国药试剂；
聚甲基丙烯酸甲酯为高流动型，购自阿拉丁；
邻苯二甲酸丁苄酯购自毛博士实验室；
邻苯二甲酸二丁酯的型号为AR(沪试)，≥99.5％，购自国药试剂。
实施例1
本实施例提供一种氮化铝陶瓷基板，其无机粉体中主相材料(氮化铝粉体)的体积占比为94.2％、烧结助剂的体积占比为5.8％；烧结助剂的D50粒径为0.5μm，烧结助剂中碱金属和/或碱土金属化合物为体积占比22％的CaO，烧结助剂中稀土金属化合物为体积占比78％的YF3；氮化铝粉体的粒径分布按体积百分比包括：0.05-0.2μm 18.93％、0.2-0.5μm18.21％、0.5-1μm 17.94％、1-2μm 22.55％、2-3.5μm 22.37％。
上述的氮化铝陶瓷基板的制备方法，包括如下步骤：
将上述的氮化铝粉体、烧结助剂以及乙醇和丁酮的二元共沸混合物、分散剂球磨分散12h，然后依次加入粘接剂和增塑剂球磨20h获得粘度为24000mPa·s的流延浆料；其中乙醇和丁酮的二元共沸混合物分散剂占主相材料和烧结助剂总重量的35％，分散剂为占主相材料和烧结助剂总重量的1％的油酸，粘接剂为占主相材料和烧结助剂总重量的6.5％的聚甲基丙烯酸甲酯，增塑剂为占主相材料和烧结助剂总重量的4％的邻苯二甲酸丁苄酯，
将流延浆料在流延机上成型获得流延生坯片，将流延生坯片经裁切后在600℃的空气气氛下排胶4h，然后转移至烧结炉中在0.2MPa的氮气压力下以1760℃保温烧结4h，获得120×120×0.5mm规格的氮化铝陶瓷基板。
实施例2
本实施例提供一种氮化铝陶瓷基板，其无机粉体中主相材料(氮化铝粉体)的体积占比为95.5％、烧结助剂的体积占比为4.5％；烧结助剂的D50粒径为0.3μm，烧结助剂中碱金属和/或碱土金属化合物为体积占比30％的CaF2和Li2CO3混合物，其中CaF2和Li2CO3的体积比为2:1；烧结助剂中稀土金属化合物为体积占比70％的Y2O3；氮化铝粉体的粒径分布按体积百分比包括：0.05-0.2μm 17.57％、0.2-0.5μm 17.66％、0.5-1μm 17.96％、1-2μm23.21％、2-3.5μm 23.60％。
上述的氮化铝陶瓷基板的制备方法，包括如下步骤：
将上述的氮化铝粉体、烧结助剂以及乙醇和丁酮的二元共沸混合物、分散剂球磨分散18h，然后依次加入粘接剂和增塑剂球磨24h获得粘度为25000mPa·s的流延浆料；其中乙醇和丁酮的二元共沸混合物分散剂占主相材料和烧结助剂总重量的35％，分散剂为占主相材料和烧结助剂总重量的1.5％的油酸，粘接剂为占主相材料和烧结助剂总重量的8％的聚乙烯醇缩丁醛，增塑剂为占主相材料和烧结助剂总重量的6％的邻苯二甲酸丁苄酯，
将流延浆料在流延机上成型获得流延生坯片，将流延生坯片经裁切后在600℃的空气气氛下排胶6h，然后转移至烧结炉中在0.2MPa的氮气压力下以1780℃保温烧结6h，获得120×120×0.5mm规格的氮化铝陶瓷基板。
实施例3
本实施例提供一种氮化铝陶瓷基板，其无机粉体中主相材料(氮化铝粉体)的体积占比为96.8％、烧结助剂的体积占比为3.2％；烧结助剂的D50粒径为0.2μm，烧结助剂中碱金属和/或碱土金属化合物为体积占比37％的CaC2，烧结助剂中稀土金属化合物为体积占比63％的Y2O3；氮化铝粉体的粒径分布按体积百分比包括：0.05-0.2μm 17.57％、0.2-0.5μm17.66％、0.5-1μm 17.96％、1-2μm 23.21％、2-3.5μm 23.60％。
上述的氮化铝陶瓷基板的制备方法，包括如下步骤：
将上述的氮化铝粉体、烧结助剂以及乙醇和丁酮的二元共沸混合物、分散剂球磨分散20h，然后依次加入粘接剂和增塑剂球磨30h获得粘度为27000mPa·s的流延浆料；其中乙醇和丁酮的二元共沸混合物分散剂占主相材料和烧结助剂总重量的40％，分散剂为占主相材料和烧结助剂总重量的1.8％的鱼油，粘接剂为占主相材料和烧结助剂总重量的10％的聚乙烯醇缩丁醛，增塑剂为占主相材料和烧结助剂总重量的6％的邻苯二甲酸二丁酯，
将流延浆料在流延机上成型获得流延生坯片，将流延生坯片经裁切后在600℃的空气气氛下排胶8h，然后转移至烧结炉中在0.2MPa的氮气压力下以1790℃保温烧结5h，获得120×120×0.5mm规格的氮化铝陶瓷基板。
实施例4
本实施例提供一种氮化铝陶瓷基板，其无机粉体中主相材料(氮化铝粉体)的体积占比为95％、烧结助剂的体积占比为5％；烧结助剂的D50粒径为0.4μm，烧结助剂中碱金属和/或碱土金属化合物为体积占比44％的CaO和SrO混合物，其中CaO和SrO体积比为1:1，烧结助剂中稀土金属化合物为体积占比56％的Y2O3和Dy2O3混合物，其中Y2O3和Dy2O3的体积比为1:1；氮化铝粉体的粒径分布按体积百分比包括：0.05-0.2μm 16.26％、0.2-0.5μm17.10％、0.5-1μm 17.94％、1-2μm 23.84％、2-3.5μm 24.86％。
上述的氮化铝陶瓷基板的制备方法，包括如下步骤：
将上述的氮化铝粉体、烧结助剂以及乙醇和丁酮的二元共沸混合物、分散剂球磨分散20h，然后依次加入粘接剂和增塑剂球磨30h获得粘度为25000mPa·s的流延浆料；其中乙醇和丁酮的二元共沸混合物分散剂占主相材料和烧结助剂总重量的42％，分散剂为占主相材料和烧结助剂总重量的2％的鱼油，粘接剂为占主相材料和烧结助剂总重量的9.2％的聚甲基丙烯酸甲酯，增塑剂为占主相材料和烧结助剂总重量的7％的邻苯二甲酸二丁酯，
将流延浆料在流延机上成型获得流延生坯片，将流延生坯片经裁切后在600℃的空气气氛下排胶6h，然后转移至烧结炉中在0.2MPa的氮气压力下以1800℃保温烧结6h，获得120×120×0.5mm规格的氮化铝陶瓷基板。
实施例5
本实施例提供一种氮化铝陶瓷基板，其无机粉体中主相材料(氮化铝粉体)的体积占比为96.8％、烧结助剂的体积占比为3.2％；烧结助剂的D50粒径为0.2μm，烧结助剂中碱金属和/或碱土金属化合物为体积占比37％的CaC2，烧结助剂中稀土金属化合物为体积占比63％的Y2O3；氮化铝粉体的粒径分布按体积百分比包括：0.05-0.2μm 17.57％、0.2-0.5μm17.66％、0.5-1μm 17.96％、1-2μm 23.21％、2-3.5μm 23.60％。
上述的氮化铝陶瓷基板的制备方法，包括如下步骤：
将上述的氮化铝粉体、烧结助剂以及乙醇和丁酮的二元共沸混合物、分散剂球磨分散20h，然后依次加入粘接剂和增塑剂球磨30h获得粘度为22000mPa·s的流延浆料；其中乙醇和丁酮的二元共沸混合物分散剂占主相材料和烧结助剂总重量的45％，分散剂为占主相材料和烧结助剂总重量的1.8％的油酸，粘接剂为占主相材料和烧结助剂总重量的10％的聚乙烯醇缩丁醛，增塑剂为占主相材料和烧结助剂总重量的6％的邻苯二甲酸二丁酯，
将流延浆料在流延机上成型获得流延生坯片，将流延生坯片经裁切后在600℃的空气气氛下排胶8h，然后转移至烧结炉中在0.1MPa的氮气压力下以1790℃保温烧结5h，获得120×120×0.5mm规格的氮化铝陶瓷基板。
实施例6
本实施例提供一种氮化铝陶瓷基板，其无机粉体中主相材料(氮化铝粉体)的体积占比为96.8％、烧结助剂的体积占比为3.2％；烧结助剂的D50粒径为0.2μm，烧结助剂中碱金属和/或碱土金属化合物为体积占比37％的CaC2，烧结助剂中稀土金属化合物为体积占比63％的Y2O3；氮化铝粉体的粒径分布按体积百分比包括：0.05-0.2μm 17.57％、0.2-0.5μm17.66％、0.5-1μm 17.96％、1-2μm 23.21％、2-3.5μm 23.60％。
上述的氮化铝陶瓷基板的制备方法，包括如下步骤：
将上述的氮化铝粉体、烧结助剂以及乙醇和丁酮的二元共沸混合物、分散剂球磨分散20h，然后依次加入粘接剂和增塑剂球磨30h获得粘度为22000mPa·s的流延浆料；其中乙醇和丁酮的二元共沸混合物分散剂占主相材料和烧结助剂总重量的45％，分散剂为占主相材料和烧结助剂总重量的1.8％的油酸，粘接剂为占主相材料和烧结助剂总重量的10％的聚乙烯醇缩丁醛，增塑剂为占主相材料和烧结助剂总重量的6％的邻苯二甲酸二丁酯，
将流延浆料在流延机上成型获得流延生坯片，将流延生坯片经裁切后在600℃的空气气氛下排胶8h，然后转移至烧结炉中在0.3MPa的氮气压力下以1790℃保温烧结5h，获得120×120×0.5mm规格的氮化铝陶瓷基板。
对比例1
本对比例提供一种氮化铝陶瓷基板，其与实施例1的陶瓷基板的唯一区别在于：在制备过程中未添加烧结助剂。
对比例2
本对比例提供一种氮化铝陶瓷基板，其与实施例1的陶瓷基板的唯一区别在于：制备所用氮化铝粉体的粒径分布按体积百分比包括0.5-1μm 23.5％，1-2μm 34.2％，2-5μm42.3％。
对比例3
本对比例提供一种氮化铝陶瓷基板，其与实施例1的陶瓷基板的唯一区别在于：在制备过程中烧结助剂的体积比为6％。
对比例4
本对比例提供一种氮化铝陶瓷基板，其与实施例1的陶瓷基板的唯一区别在于：在制备过程中烧结助剂的体积比为3％。
试验例1
使用扫描电镜观察实施例3的氮化铝陶瓷基板的微观结构，其微观结构图见图1和图2。图2中的白色晶粒为第二相，由图可知，在氮化铝陶瓷的三叉晶界结构处，晶界洁净，局部位置存在有孤立分布的第二相，在晶界处未发现有形成的连续第二相存在。
试验例2
按照GB/T 25995-2010精细陶瓷密度和显气孔率试验方法标准测试实施例、对比例的氮化铝陶瓷基板的相对密度，测试结果见表1。
试验例3
使用GB/T 6569-2006精细陶瓷弯曲强度试验方法测试实施例、对比例的氮化铝陶瓷基板的抗弯强度，测试结果见表1。
试验例4
使用GB/T 22588闪光法测量热扩散系数或导热系数的方法测试实施例、对比例的氮化铝陶瓷基板的热导率，测试结果见表1。
试验例5
使用GB/T 5594.5电子元器件结构陶瓷材料性能测试体积电阻率测试的方法测试实施例、对比例的氮化铝陶瓷基板的体积电阻率，测试结果见表1。
试验例6
使用GB/T 5594.4-2015电子元器件结构陶瓷材料性能测试方法第4部分：介电常数和介质损耗角正切值测试的方法方法测试实施例、对比例的氮化铝陶瓷基板的介电常数，测试结果见表1。
表1.实施例、对比例测试结果
Figure BDA0003672958320000121
由表1可知，本发明制备出的氮化铝陶瓷基板热导率可达到223W/m·K。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明创造的保护范围之中。

Claims (10)

1.一种氮化铝陶瓷基板，其特征在于，其由无机粉体烧结获得，所述无机粉体包括体积占比为94.2-96.8％的主相材料和体积占比为3.2-5.8％的烧结助剂，所述主相材料为氮化铝粉体，所述氮化铝粉体的粒径分布按体积百分比包括：
Figure FDA0003672958310000011
2.根据权利要求1所述的一种氮化铝陶瓷基板，其特征在于，所述烧结助剂包括体积占比分别为22-44％、56-78％的碱金属和/或碱土金属化合物、稀土金属化合物。
3.根据权利要求1或2所述的一种氮化铝陶瓷基板，其特征在于，所述烧结助剂的D50粒径为0.2-0.5μm。
4.根据权利要求2或3所述的一种氮化铝陶瓷基板，其特征在于，所述碱金属和/或碱土金属化合物选自CaO、CaC2、CaF2、SrO及Li2CO3中的至少一种。
5.根据权利要求2-4任一项所述的一种氮化铝陶瓷基板，其特征在于，所述稀土金属化合物选自Y2O3、Dy2O3、Gd2O3及YF3中的至少一种。
6.权利要求1-5任一项所述的一种氮化铝陶瓷基板的制备方法，其特征在于，包括如下步骤：
将无机粉体球磨获得流延浆料；
将流延浆料成型、排胶，然后在0.1-0.3MPa的保护气压力下以1760-1800℃烧结4-6h。
7.根据权利要求6所述的一种氮化铝陶瓷基板的制备方法，其特征在于，球磨的步骤包括：将无机粉体、分散剂和溶剂球磨分散12-20h，然后依次加入粘接剂和增塑剂球磨20-30h获得流延浆料。
8.根据权利要求7所述的一种氮化铝陶瓷基板的制备方法，其特征在于，所述溶剂为乙醇和丁酮的二元共沸混合物；
和/或，所述溶剂占主相材料和烧结助剂总重量的35-45％。
9.根据权利要求7或8所述的一种氮化铝陶瓷基板的制备方法，其特征在于，所述分散剂选自油酸和/或鱼油；
和/或，所述分散剂占主相材料和烧结助剂总重量的1-2％。
10.根据权利要求7-9任一项所述的一种氮化铝陶瓷基板的制备方法，其特征在于，满足以下(1)-(4)中的至少一项：
(1)所述粘接剂选自聚乙烯醇缩丁醛和/或聚甲基丙烯酸甲酯；
(2)所述粘接剂占主相材料和烧结助剂总重量的6.5-10％；
(3)所述增塑剂选自邻苯二甲酸丁苄酯和/或邻苯二甲酸二丁酯；
(4)所述增塑剂占主相材料和烧结助剂总重量的4-7％。
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