CN114656245B - 一种氧化铝基复合陶瓷基板及其制备方法 - Google Patents

一种氧化铝基复合陶瓷基板及其制备方法 Download PDF

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CN114656245B
CN114656245B CN202210408276.8A CN202210408276A CN114656245B CN 114656245 B CN114656245 B CN 114656245B CN 202210408276 A CN202210408276 A CN 202210408276A CN 114656245 B CN114656245 B CN 114656245B
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ceramic substrate
alumina
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CN114656245A (zh
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陈琦
李显坪
唐宝发
李刚
吴宇皓
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Jiangsu Zhongtianli Technology Co ltd
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Yangzhou Ztl New Materials Co ltd
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Abstract

本发明涉及陶瓷基板材料技术领域，尤其涉及一种氧化铝基复合陶瓷基板及其制备方法。所述氧化铝基复合陶瓷基板由以下原料组成：氧化铝80~100份、氧化锆15~25份、硼酸铝晶须7~12份、助烧剂10~25份、增塑剂10~15份、分散剂3~5份、粘结剂10~20份、有机溶剂75~105份。本发明通过在氧化铝基基板材料中掺杂钛酸锶和钛酸铋，不仅能改善氧化铝基陶瓷基板抗弯强度、断裂韧性等力学性能，还能进一步提高氧化铝基陶瓷基板对铜、铝、金等不等金属的结合强度，提高了陶瓷基板整体可靠性。

Description

一种氧化铝基复合陶瓷基板及其制备方法
技术领域
本发明涉及陶瓷基板材料技术领域，尤其涉及一种氧化铝基复合陶瓷基板及其制备方法。
背景技术
常用的半导体封装用陶瓷基板材料主要有：氧化铍基板、氧化铝基板、氮化铝基板和氮化硅基板。其中，氧化铍基板虽然具有较高的热导率，但是其粉体有毒，会引起中毒且造成环境污染。氧化铝陶瓷基板是目前制作和加工技术最成熟的陶瓷基板材料，具有介电损耗低，电性能与温度相关性低，机械强度较高，化学稳定性好的优点，但因其热导率低，热膨胀系数高，目前只能应用与低端或者小功率器件。氮化硅陶瓷基板具有硬度大、强度高、热膨胀系数小、高温蠕动小、抗氧化性能好、热腐蚀性能良好、摩擦系数小等诸多优异性能，但是其制备工艺条件复杂苛刻，对设备要求极高，良品率较低且生产成本高。氮化铝陶瓷基板的热导率高，可达150W/(m•K)以上，且热膨胀系数为(3.8～4 .4)× 10-6/℃，与硅、碳化硅等半导体芯片材料的热膨胀系数匹配性较好，但是氮化铝陶瓷的力学性能较差，抗弯强度只有300MPa，在大电流、高温度的使用环境下极容易发生损坏，从而对半导体寿命造成不良影响。
同时，陶瓷基板表面金属化工艺是实现陶瓷在功率型电子元器件封装中使用的重要环节，金属化方法决定了陶瓷基板的性能、制造成本、产品良率与使用范围。
基于上述情况，本发明提出了一种氧化铝基复合陶瓷基板及其制备方法，可有效解决以上问题。
发明内容
本发明的目的在于提供一种氧化铝基复合陶瓷基板及其制备方法。
为实现上述目的，本发明提供了一种氧化铝基复合陶瓷基板，所述氧化铝基复合陶瓷基板由以下原料组成：氧化铝80~100份、氧化锆15~25份、硼酸铝晶须7~12份、助烧剂10~25份、增塑剂10~15份、分散剂3~5份、粘结剂10~20份、有机溶剂75~105份。
优选地，所述助烧剂为稀土氧化物，包括氧化钇、氧化钙、氧化铌、氧化铈、氧化钐、氧化镧中的至少一种或两种以上的组合。
优选地，所述增塑剂包括邻苯二甲酸二丁酯、丙三醇的至少一种或两种以上的组合。
优选地，所述分散剂包括三油酸甘油酯、磷酸三乙酯、聚丙烯酸钠、聚乙烯酸酯、蓖麻油中的至少一种或两种以上的组合。
优选地，所述粘结剂为聚乙烯醇缩丁醛、丙烯酸酯、聚乙烯醇中的至少一种或两种以上的组合。
优选地，所述有机溶剂包括无水乙醇、丙酮、异丙醇、乙酸乙酯的至少一种或两种以上的组合。
优选地，所述氧化铝基复合陶瓷基板的原料还包括钛酸金属。
优选地，所述钛酸金属为钛酸锶与钛酸铋的组合。
优选地，所述氧化铝基复合陶瓷基板由以下原料组成：氧化铝80~100份、氧化锆15~25份、钛酸锶2~6份、钛酸铋3~5份、硼酸铝晶须7~12份、氧化钇4~10份、氧化镧6~15份、邻苯二甲酸二丁酯10~15份、三油酸甘油酯3~5份、聚乙烯醇缩丁醛10~20份、异丙醇50~70份、乙酸乙酯25~35份。
优选地，所述氧化铝基复合陶瓷基板由以下原料组成：氧化铝80份、氧化锆15份、钛酸锶2份、钛酸铋3份、硼酸铝晶须7份、氧化钇4份、氧化镧6份、邻苯二甲酸二丁酯10份、三油酸甘油酯3份、聚乙烯醇缩丁醛10份、异丙醇50份、乙酸乙酯25份。
优选地，所述氧化铝基复合陶瓷基板由以下原料组成：氧化铝100份、氧化锆25份、钛酸锶6份、钛酸铋5份、硼酸铝晶须12份、氧化钇10份、氧化镧15份、邻苯二甲酸二丁酯15份、三油酸甘油酯5份、聚乙烯醇缩丁醛20份、异丙醇70份、乙酸乙酯35份。
本发明还提供一种氧化铝基复合陶瓷基板的制备方法，所述制备方法包括以下步骤：
(1)将氧化铝、氧化锆、钛酸锶、钛酸铋、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散18~20h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散10~12h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以6～8℃/min的升温速率升至在1400℃~1450℃的温度下保温8~10h，即得。
与现有技术相比，本发明具有如下有益效果：
1.本发明通过在氧化铝基基板材料中掺杂钛酸锶和钛酸铋，不仅能改善氧化铝基陶瓷基板抗弯强度、断裂韧性等力学性能，还能进一步提高氧化铝基陶瓷基板对铜、铝、金等不等金属的结合强度，提高了陶瓷基板整体可靠性。
2.本发明原材料在国内充足，价格适宜，使其规模化生产没有太高的成本限制；其次，本发明组合适用范围广，可满足氧化铝基复合陶瓷基板背胶层的生产要求；同时，制备工艺方法简单，总体生产成本不高，有利于工业的大规模生产。
具体实施方式
实施例1
按表1称量具体原料，其余步骤制备步骤如下：
(1)将氧化铝、氧化锆、钛酸锶、钛酸铋、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散18h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散10h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以6℃/min的升温速率升至在1400℃℃的温度下保温10h，即得。
实施例2
按表1称量具体原料，其余步骤制备步骤如下：
(1)将氧化铝、氧化锆、钛酸锶、钛酸铋、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散20h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散12h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以8℃/min的升温速率升至在1450℃的温度下保温8h，即得。
实施例3
按表1称量具体原料，其余步骤制备步骤如下：
(1)将氧化铝、氧化锆、钛酸锶、钛酸铋、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散20h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散12h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以8℃/min的升温速率升至在1450℃的温度下保温10h，即得。
对比例1
按表1称量具体原料，其余步骤制备步骤如下：
(1)将氧化铝、氧化锆、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散20h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散12h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以8℃/min的升温速率升至在1450℃的温度下保温10h，即得。
对比例2
按表1称量具体原料，其余步骤制备步骤如下：
(1)将氧化铝、氧化锆、钛酸锶、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散20h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散12h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以8℃/min的升温速率升至在1450℃的温度下保温10h，即得。。
对比例3
按表1称量具体原料，其余步骤制备步骤如下：
(1)将氧化铝、氧化锆、钛酸铋、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散20h，得混合物A；
(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散12h，得混合物B；
(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；
(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以8℃/min的升温速率升至在1450℃的温度下保温10h，即得。
表1
物料组成 实施例1 实施例2 实施例3 对比例1 对比例2 对比例3
氧化铝 80 90 100 100 100 100
氧化锆 15 20 25 25 25 25
钛酸锶 2 4 6 / 6 /
钛酸铋 3 4 5 / / 5
硼酸铝晶须 7 9 12 12 12 12
氧化钇 4 8 10 10 10 10
氧化镧 6 10 15 15 15 15
邻苯二甲酸二丁酯 10 12 15 15 15 15
三油酸甘油酯 3 4 5 5 5 5
聚乙烯醇缩丁醛 10 15 20 20 20 20
异丙醇 50 60 70 70 70 70
乙酸乙酯 25 30 35 35 35 35 
实施例 4性能测试
将实施例1~3以及对比例1~3制备得到的复合陶瓷基板进行热导率、抗弯强度、断裂韧性、反射率进行测试；分别以铜、铝、金作为金属原料，通过溅射法，在实施例1~3以及对比例1~3制备得到的复合陶瓷基板上形成一层10μm的金属薄膜，同时测定其结合强度。测试结果见表2。
表2性能测试结果
  实施例1 实施例2 实施例3 对比例1 对比例2 对比例3
热导率 (W/m·K) 182 179 181 175 172 186
抗弯强度 （MPa） 798 792 812 753 762 785
断裂韧性 （MPa·m1/2） 8.7 8.5 9.1 6.9 7.2 8.3
发射率% 99.3 99.5 99.2 99.6 99.4 99.1
结合强度 （铜/MPa） 25.2 26.8 27.3 26.5 15.2 27.4
结合强度 （铝/MPa） 45.6 44.3 46.8 22.6 45.6 21.8
结合强度 （金/MPa） 51.3 52.6 53.5 30.2 31.5 42.4 
前述对本发明的具体示例性实施方案的描述是为了说明和例证的目的。这些描述并非想将本发明限定为所公开的精确形式，并且很显然，根据上述教导，可以进行很多改变和变化。对示例性实施例进行选择和描述的目的在于解释本发明的特定原理及其实际应用，从而使得本领域的技术人员能够实现并利用本发明的各种不同的示例性实施方案以及各种不同的选择和改变。本发明的范围意在由权利要求书及其等同形式所限定。

Claims (1)

1.一种氧化铝基复合陶瓷基板，其特征在于，所述氧化铝基复合陶瓷基板由以下原料组成：氧化铝80～100份、氧化锆15～25份、钛酸锶2～6份、钛酸铋3～5份、硼酸铝晶须7～12份、氧化钇4～10份、氧化镧6～15份、邻苯二甲酸二丁酯10～15份、三油酸甘油酯3～5份、聚乙烯醇缩丁醛10～20份、异丙醇50～70份、乙酸乙酯25～35份；所述氧化铝基复合陶瓷基板的制备方法包括如下步骤：(1)将氧化铝、氧化锆、钛酸锶、钛酸铋、硼酸铝晶须、氧化钇、氧化镧搅拌均匀，然后加入异丙醇、三油酸甘油酯和乙酸乙酯，将其搅拌均匀后，球磨分散18～20h，得混合物A；(2)向混合物A中加入邻苯二甲酸二丁酯和聚乙烯醇缩丁醛，搅拌均匀后，球磨分散10～12h，得混合物B；(3)将混合物B进行抽真空脱泡得流延浆料，然后经流延成型，制得流延生坯片；(4)将步骤(3)制得的流延生坯片进行烧结，在惰性气氛中，以6～8℃/min的升温速率升至在1400℃～1450℃的温度下保温8～10h，即得。
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