CN113173797A - 一种Al2O3基陶瓷焊接密封元器件及其制备方法 - Google Patents

一种Al2O3基陶瓷焊接密封元器件及其制备方法 Download PDF

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Publication number
CN113173797A
CN113173797A CN202110607217.9A CN202110607217A CN113173797A CN 113173797 A CN113173797 A CN 113173797A CN 202110607217 A CN202110607217 A CN 202110607217A CN 113173797 A CN113173797 A CN 113173797A
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ceramic
parts
oxide
matrix
alumina
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CN113173797B (zh
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曹建平
曹建辉
刘平
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Hunan Jusheng Technology Co ltd
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Xinxing Electronic Ceramics Co ltd
Hunan Xinhuayuan Technology Co ltd
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Abstract

本发明公开一种Al2O3基陶瓷焊接密封元器件及其制备方法，涉及金属化陶瓷加工技术领域。本发明公开的Al 2O3基陶瓷焊接密封元器件，包括陶瓷基体和金属化层，其中陶瓷基体用无机纤维‑氧化铝三维网状基体、氧化钇、氧化硅、氧化钛、添加剂、粘结剂和分散剂等原料，经无机纤维‑氧化铝三维网状基体制备、混料、造粒、一次烧结和二次烧结等步骤而制成；金属化层原料包括钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂，并公开了用金属化层和陶瓷基体组成的密封元器件的制备方法。本发明提供的A l 2O3基陶瓷焊接密封元器件，其具有高的致密度和抗拉强度，具有优异的抗拉强度、韧性和耐高温性能。

Description

一种Al2O3基陶瓷焊接密封元器件及其制备方法
技术领域
本发明属于金属化陶瓷加工技术领域，尤其涉及一种Al2O3基陶瓷焊接密封元器件及其制备方法。
背景技术
随着材料技术的发展，陶瓷材料得到广泛的运用，尤其在密封机构中，陶瓷材料由于其具有良好的耐高温、抗化学腐蚀与导热性，其适用于各类密封元器件。目前，陶瓷焊接密封元器件是由金属化陶瓷构成，而在金属化处理过程中应用的陶瓷材料主要有三氧化二铝、氧化锆、氮化硅、碳化硅、碳化钨及其复合材料，其中碳化硅陶瓷以其优良的强度、硬度、耐化学腐蚀等为特点，应用的最为广泛，性价比远高于一般的金属密封件，且使用寿命大大延长。但氮化硅陶瓷的断裂韧性较低，即脆性较大，易断裂，并且与金属层的封接强度不理想。
氧化铝陶瓷具有机械强度高，耐磨耐腐蚀性好，热稳定好，绝缘电阻大，膨胀系数与芯片相匹配等特性，是微电子封装领域最常见的基板材料或封装壳体材料。为了使电子器件或封装壳体具有高强度和高气密性，Al2O3陶瓷常需要与各种合金等封装金属进行钎焊。而常见的金属钎料与Al2O3陶瓷润湿性差，所以需要在Al2O3陶瓷表面进行金属化，最常见的方法之一就是在其表面共烧钨金属化层，然后将具有钨金属化层的Al2O3陶瓷进行电镀Ni或Au，这样就可以采用传统的Ag-Cu等钎料钎焊Al2O3陶瓷和合金，从而得到气密封装。传统的氧化铝陶瓷的钨金属化层主要由钨粉和玻璃粉组成，这种金属化层结构不致密、孔隙率高等缺点，影响陶瓷金属化制品的力学性能和使用寿命。氧化铝陶瓷本身具有脆性大、耐冲击能力低、易碎等缺陷，这也影响了氧化铝在密封元器件上的使用，降低了氧化铝陶瓷的使用寿命。
发明内容
本发明提供了一种金属化的氧化铝陶瓷及其制备方法，用于Al2O3基陶瓷焊接密封元器件上，主要目的是提高了密封件的致密度，并大大提高了密封件的弯曲强度和断裂韧性，增大了密封件的抗拉强度，具有优异的耐高温性能。
为了实现本发明的目的，本发明提供了一种Al2O3基陶瓷焊接密封元器件，包括陶瓷基体和金属化层，陶瓷基体是由以下重量份数的原料制备：无机纤维-氧化铝三维网状基体80-90份、氧化钇2-5份、氧化硅1-3份、氧化钛2-4份、添加剂0.5-1.0份、粘结剂3-5份和分散剂1-3份，所述添加剂、粘结剂和分散剂分别为LiYO2、聚乙烯醇缩丁醛和三聚磷酸钠；
所述陶瓷基体的制备方法，依次包括以下步骤：
A1、无机纤维-六方氧化铝三维网状基体的制备：
将无机纤维浸渍于2mol/L的NaOH溶液和有机硅绝缘浸渍剂中，在70-90℃下浸渍3-4h，经过滤，干燥，得到表面改性的无机纤维，所述NaOH溶液和有机硅绝缘浸渍剂的质量比为1:1～2；
将氧化铝和表面改性的无机纤维混合，在惰性气氛下，压力为5-10MPa，温度为80-120℃下反应2-6h，制得无机纤维-氧化铝三维网状基体，所述表面改性的无机纤维与氧化铝的质量比为1:4～8；
A2、混料：将氧化硅、氧化钇和添加剂混合均匀后，加入到步骤A1中制得的无机纤维-氧化铝三维网状基体中，然后加入氧化钛、分散剂和水，高速球磨6-8h；
A3、造粒：将研磨后的浆料抽滤，然后用离心式喷雾干燥机加工成平均粒径为20-40μm的颗粒状陶瓷粉末，备用；
A4、一次烧结：将步骤A3所得的陶瓷粉末装入热压模具中，以氮气为保护气，在1000-1200℃进行常温烧结，保温时间为1-2h，制得陶瓷毛坯；
A5、二次烧结：将步骤A4所得的陶瓷毛坯装入热压模具中，以氮气为保护气，在1600-1800℃进行常压烧结，保温时间为2-3h，随炉冷却至室温后取出，然后在平面磨床上抛光，制得待金属化的陶瓷基体。
进一步的，所述步骤A1中无机纤维为碳化硅纤维、氮化铝纤维或氧化硅纤维中的一种。
进一步的，所述步骤A2的球磨过程中，球磨速率为360r/min，球料比为10:1。
一种Al2O3基陶瓷焊接密封元器件的制备方法，包括以下步骤：
B1、金属化膏的制备：称取钛粉10-20份、钨粉40-60份、氧化钼10-20份、氧化硼10-20份、氧化钇2-4份和有机结合剂2-5份，将钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂一起均匀混合，制得金属化膏；
B2、丝印：将权利要求1中制得的待金属化的陶瓷基体表面用无水乙醇进行超声清洗，然后将金属化膏采用丝网印刷的方法均匀地涂覆在陶瓷基体两端的表面，其中金属化膏的印刷厚度为40-50μm；
B3、金属化处理：上述制备的涂覆有金属化膏的陶瓷基体在真空或惰性气体保护下烧结，烧结温度为1300-1500℃，烧结保温时间为60-90min,即得本发明的Al2O3基陶瓷焊接密封元器件。
进一步的，所述步骤B1中有机结合剂是按照乙基纤维素：松油醇：乙二醇＝2:1:1的重量比例混合而成。
本发明取得了以下有益效果：
1、本发明三聚磷酸钠属于阴离子型亲水基表面活性剂，三聚磷酸钠在水中，会电离形成阴离子，被氧化物(氧化钇、氧化硅和氧化钛)表面所吸附，使得氧化物分子与水接触的界面上形成双电层，氧化物由于表面吸附阴离子，故带负电荷。带有同种电荷的氧化物间受到静电斥力的作用，阻止了粒子间的相互聚集，从而提升氧化物的分散效果。
2、本发明SiO2-Y2O3作为烧结助剂在添加剂的作用下进行高压高温烧结时形成液相，无机纤维-六方氧化铝三维网状基体晶粒在液相中的传质凝聚快，有助于晶界扩散和迁移，故此以SiO2-Y2O3作为烧结助剂对陶瓷基体的致密度及力学性能有显著的提升。
3、本发明金属化膏中钛粉具有很强的化学活泼性，对氧化钼、氧化硼、氧化钇具有很大的亲和力。钛粉很容易在烧结温度下，与氧化钼、氧化硼、氧化钇形成液相活性合金渗透至陶瓷基体表面，形成很致密均匀的金属层，从而使陶瓷基体与金属层进行高强度高气密性的封接，大大提高了陶瓷基体的润湿性。
4、本发明陶瓷基体中的氧化钛能与金属化膏中的氧化物相互作用，使陶瓷基体中的玻璃相粘度降低，并能很好地润湿金属化层中钛颗粒的表面，同时通过毛细作用向金属化层中钛颗粒的间隙中渗透，促使陶瓷基体中的玻璃相向金属化层迁移，提高陶瓷基体的润湿性。
5、本发明利用无机纤维作为增强剂，将氧化铝和表面改性的无机纤维在高温高压下交联制得具有三维网状结构的，该三维网状结构有利于陶瓷基体的致密化，大大提高了陶瓷基体的耐温性能和力学性能；将氧化物在分散剂作用下填充在无机纤维-氧化铝三维网状基体中，进行研磨，无机纤维成分作为球磨介质，可使无机纤维-氧化铝三维网状基体的粒径减小，提高陶瓷基体的致密度和力学性能；并在粘结剂的作用下形成致密的陶瓷基体，由于无机纤维-氧化铝三维网状结构能够分散及消除陶瓷内部及氧化铝引入所产生的各种应力，使得陶瓷基体具有良好的柔韧性，弯曲强度进一步提高。
6、金属化层在烧结过程中，钛粉和氧化钼、氧化硼、氧化钇形成玻璃相，玻璃相向钨粉颗粒中迁移，使钨粉调整位置，重新达到紧密排布，致使金属化层的致密度高；同时钨粉表面的原子会溶解于玻璃相，由于金属化层中的玻璃相会与陶瓷基体中的液相互溶，则促进陶瓷基体中的液相向钨粉孔隙中迁移，同时金属化层中的玻璃相和溶解于玻璃相中的钨粉渗透到陶瓷基体中，且陶瓷基体的三维网络结构能使金属化层的玻璃相更易往陶瓷基体三维网状结构中迁移，加强了陶瓷基体与金属化层的连接，增强了陶瓷基体的润湿性；金属化层组分中的氧化钇高温下易与陶瓷基体中的氧化铝反应生产液相YAP，进一步提高了陶瓷基体对该金属化层的润湿性。
7、本发明采用无机纤维和氧化铝三维网状基体，并使用氧化钇-氧化硅-氧化钛作为烧结助剂，得到了致密度高的陶瓷基体，具有优异的弯曲性、断裂韧性、绝缘性和耐高温性能；采用钛粉、钨粉等作为金属化膏对本发明的陶瓷基体进行金属化处理制得的密封件，具有很好的致密性，并因金属化膏与本发明的陶瓷基体有很好的封接效果，致使其抗拉强度高，耐高温性能优异。
具体实施方式
下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
下面结合具体实施例对本发明的Al2O3基陶瓷焊接密封元器件及其制备方法予以说明。
实施例1：Al2O3基陶瓷焊接密封元器件包括陶瓷基体和金属化层，其中陶瓷基体及其制备方法
密封件中陶瓷基体按重量份数的原料配方组分：无机纤维-氧化铝三维网状基体80份、氧化钇5份、氧化硅3份、氧化钛4份、LiYO21份、聚乙烯醇缩丁醛4.5份和三聚磷酸钠3份；
按照上述配方组分的陶瓷基体的制备方法，包括以下步骤：
A1、碳化硅纤维-氧化铝三维网状基体的制备：
将碳化硅纤维浸渍于2mol/L的NaOH溶液和有机硅绝缘浸渍剂中，在70-90℃下浸渍3-4h，经过滤，干燥，得到表面改性的碳化硅纤维，其中NaOH溶液和有机硅绝缘浸渍剂的质量比为1:1；
将氧化铝和表面改性的碳化硅纤维混合，在惰性气氛下，压力为5-10MPa，温度为80-120℃下反应2-6h，制得碳化硅纤维-氧化铝三维网状基体，其中表面改性的碳化硅纤维与氧化铝的质量比为1:4；
A2、混料：将氧化硅、氧化钇和添加剂混合均匀后，加入到步骤A1中制得的碳化硅纤维-氧化铝三维网状基体中，然后加入氧化钛、分散剂和水，以360r/min的速率球磨6-8h，其中球料比为10:1；
A3、造粒：将研磨后的浆料抽滤，然后用离心式喷雾干燥机加工成平均粒径为20-40μm的颗粒状陶瓷粉末，备用；
A4、一次烧结：将步骤A3所得的陶瓷装入热压模具中，以氮气为保护气，在1000-1200℃进行常温烧结，保温时间为1-2h，制得陶瓷毛坯；
A5、二次烧结：将步骤A4所得的陶瓷毛坯装入热压模具中，以氮气为保护气，在1600-1800℃进行常压烧结，保温时间为2-3h，随炉冷却至室温后取出，然后在平面磨床上抛光，制得待金属化的陶瓷基体。
实施例2：Al2O3基陶瓷焊接密封元器件包括陶瓷基体和金属化层，其中陶瓷基体及其制备方法
密封件中陶瓷基体按重量份数的原料配方组分：无机纤维-氧化铝三维网状基体85份、氧化钇3份、氧化硅2份、氧化钛3份、LiYO20.8份、聚乙烯醇缩丁醛5份和三聚磷酸钠1.2份。
实施例2中陶瓷基体的制备方法与实施例1中相同，具体步骤参照实施例1，值得注意的是，A1步骤中，无机纤维为氮化铝纤维，NaOH溶液和有机硅绝缘浸渍剂的质量比为1:2，表面改性的碳化硅纤维与氧化铝的质量比为1:6。
实施例3：Al2O3基陶瓷焊接密封元器件包括陶瓷基体和金属化层，其中陶瓷基体及其制备方法
密封件中陶瓷基体按重量份数的原料配方组分：无机纤维-氧化铝三维网状基体90份、氧化钇2份、氧化硅1份、氧化钛2份、L iYO21份、聚乙烯醇缩丁醛3份和三聚磷酸钠1份。
实施例3中陶瓷基体的制备方法与实施例1中相同，具体步骤参照实施例1，值得注意的是，A1步骤中，无机纤维为氧化硅纤维，NaOH溶液和有机硅绝缘浸渍剂的质量比为1:1.5，表面改性的碳化硅纤维与氧化铝的质量比为1:8。
实施例4：Al2O3基陶瓷焊接密封元器件包括陶瓷基体和金属化层，其中陶瓷基体及其制备方法
密封件中陶瓷基体按重量份数的原料配方组分：无机纤维-氧化铝三维网状基体82份、氧化钇4.5份、氧化硅3份、氧化钛2.8份、L iYO20.7份、聚乙烯醇缩丁醛5份和三聚磷酸钠2份。
实施例4中陶瓷基体的制备方法与实施例1中相同，具体步骤参照实施例1，值得注意的是，A1步骤中，无机纤维为碳化硅纤维，NaOH溶液和有机硅绝缘浸渍剂的质量比为1:2，表面改性的碳化硅纤维与氧化铝的质量比为1:5.5。
实施例5：Al2O3基陶瓷焊接密封元器件中金属化层的组成以及密封件的制备方法
金属化膏按重量份数的原料配方组分：钛粉10份、钨粉60份、氧化钼10份、氧化硼13份、氧化钇2份和有机结合剂5份，其中有机结合剂是按照乙基纤维素：松油醇：乙二醇＝2:1:1的重量比例混合而成。
Al2O3基陶瓷焊接密封元器件的制备方法包括以下步骤：
B1金属化膏的制备：将上述重量份数的钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂一起均匀混合，制得金属化膏；
B2丝印：将实施例1中制得的待金属化的陶瓷基体表面用无水乙醇进行超声清洗，然后将金属化膏采用丝网印刷的方法均匀地涂覆在陶瓷基体两端的表面，其中金属化膏的印刷厚度为40-50μm；
B3金属化处理：上述制备的涂覆有金属化膏的陶瓷基体在真空或惰性气体保护下烧结，烧结温度为1300-1500℃，烧结保温时间为60-90min，即得本发明的Al2O3基陶瓷焊接密封元器件C1。
实施例6：Al2O3基陶瓷焊接密封元器件中金属化层的组成以及密封件的制备方法
金属化膏按重量份数的原料配方组分：钛粉15份、钨粉55份、氧化钼13份、氧化硼10份、氧化钇3份和有机结合剂4份，其中有机结合剂是按照乙基纤维素：松油醇：乙二醇＝2:1:1的重量比例混合而成。
Al2O3基陶瓷焊接密封元器件的制备方法包括以下步骤：
B1金属化膏的制备：将上述重量份数的钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂一起均匀混合，制得金属化膏；
B2丝印：将实施例2中制得的待金属化的陶瓷基体表面用无水乙醇进行超声清洗，然后将金属化膏采用丝网印刷的方法均匀地涂覆在陶瓷基体两端的表面，其中金属化膏的印刷厚度为40-50μm；
B3金属化处理：上述制备的涂覆有金属化膏的陶瓷基体在真空或惰性气体保护下烧结，烧结温度为1300-1500℃，烧结保温时间为60-90min，即得本发明的Al2O3基陶瓷焊接密封元器件C2。
实施例7：Al2O3基陶瓷焊接密封元器件中金属化层的组成以及密封件的制备方法
金属化膏按重量份数的原料配方组分：钛粉18份、钨粉50份、氧化钼10份、氧化硼15份、氧化钇4份和有机结合剂3份，其中有机结合剂是按照乙基纤维素：松油醇：乙二醇＝2:1:1的重量比例混合而成。
Al2O3基陶瓷焊接密封元器件的制备方法包括以下步骤：
B1金属化膏的制备：将上述重量份数的钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂一起均匀混合，制得金属化膏；
B2丝印：将实施例3中制得的待金属化的陶瓷基体表面用无水乙醇进行超声清洗，然后将金属化膏采用丝网印刷的方法均匀地涂覆在陶瓷基体两端的表面，其中金属化膏的印刷厚度为40-50μm；
B3金属化处理：上述制备的涂覆有金属化膏的陶瓷基体在真空或惰性气体保护下烧结，烧结温度为1300-1500℃，烧结保温时间为60-90min，即得本发明的Al2O3基陶瓷焊接密封元器件C3。
实施例8：Al2O3基陶瓷焊接密封元器件中金属化层的组成以及密封件的制备方法
金属化膏按重量份数的原料配方组分：钛粉20份、钨粉40份、氧化钼20份、氧化硼15份、氧化钇3份和有机结合剂2份，其中有机结合剂是按照乙基纤维素：松油醇：乙二醇＝2:1:1的重量比例混合而成。
Al2O3基陶瓷焊接密封元器件的制备方法包括以下步骤：
B1金属化膏的制备：将上述重量份数的钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂一起均匀混合，制得金属化膏；
B2丝印：将实施例4中制得的待金属化的陶瓷基体表面用无水乙醇进行超声清洗，然后将金属化膏采用丝网印刷的方法均匀地涂覆在陶瓷基体两端的表面，其中金属化膏的印刷厚度为40-50μm；
B3金属化处理：上述制备的涂覆有金属化膏的陶瓷基体在真空或惰性气体保护下烧结，烧结温度为1300-1500℃，烧结保温时间为60-90min，即得本发明的Al2O3基陶瓷焊接密封元器件C4。
对实施例5-8制得的Al2O3基陶瓷焊接密封元器件进行抗拉强度检测，其检测方法如下：
抗拉强度检测采用三点法，即在密封件一个端面均匀取三点，分别在其上放置一Ф3mm厚0.1mm的银铜焊料片，再用夹具分别将三根Ф3mm×30mm的铁镍钴瓷封合金杆垂直、平稳的压在焊料片上，放入真空钎焊炉中进行钎焊，最后将封接好的测试件在材料试验机上进行拉力测试，通过公式E＝10P/F计算出抗拉强度数值，其中:E--抗拉强度(MPa)，P--拉断时的力(KN)，F--试样的封接面积cm2。测试设备为CSS-44100万能材料试验机。
上述实施例5-8所得Al2O3基陶瓷焊接密封元器件与发明专利CN109336564B公开的一种高铝陶瓷的制备方法及利用该方法制备的高铝陶瓷相比，其抗拉强度对比检测结果见表1。
表1密封件的抗拉强度检测结果
C1 C2 C3 C4 对比项
抗拉强度(MPa) 204 216 210 208 162
对实施例1-4中的陶瓷基体进行致密度、弯曲强度和断裂韧性的测试。
(1)陶瓷基体致密度的测试方法：
体积密度的测试：
1)将待测试样置于100±5℃烘箱中干燥直至衡重，用分析天平称量待测试样室温下的干重m1，精确到0.001g；
2)将步骤1)称量后的待测试样放入沸水中煮沸不少于3h，且煮沸过程中使试样始终处于液面以下，冷却到室温后，用分析天平称量待测试样在水中的浮重m2，精确到0.001g；
3)将步骤2)称量后的待测试样从水中取出，用纱布将试样表面的水擦干，然后迅速称量待测试样的湿重m3，精确到0.001g。
4)重复上述步骤各3次取均值。
陶瓷基体的体积密度ρs按公式κ＝m1ρw/(m3-m2)计算，式中：m1为试样干燥后的重量(g)；m2为试样充分吸水后在水中的浮重(g)；m3为试样充分吸水后在空气中的重量(g)；ρw为水的密度，取1.0g/cm3。
陶瓷基体的理论密度ρth按公式ρth＝1/Σ(wi/ρi)计算，式中：wi为第i组分的重量百分比；ρi第i组分的理论密度(g/cm3)。
陶瓷基体的致密度，即相对密度ρr按公式ρr＝ρs/ρth计算。
(2)陶瓷基体的弯曲强度，采用三点弯曲法测定：
1)将制得的陶瓷试样，在平面磨床磨双面打磨至4mm左右；
2)利用内圆切割机将试样加工成尺寸为3×4×36mm的长方体样条，再利用金刚石研磨膏磨倒角；
3)采用型号为YRWT-D型微机控制电子万能实验机进行测试。测试条件为跨距20mm，加载速度为0.5mm/min，垂直加压。陶瓷的弯曲强度σf按公式σf＝3FL/2bd2计算，式中：σf为计算的陶瓷弯曲强度(MPa)；b为测试样条的宽度(mm)；L为设定的试验机跨距(mm)；d为测试样条的高度(mm)；F为陶瓷试样断裂时的试验机显示的加载力(N)。
同一陶瓷试样，准备3根样条，测试后取平均值作为其弯曲强度
(3)陶瓷基体的断裂韧性，采用三点弯曲法测试：
1)将烧结后的陶瓷试样，在平面磨床上双面平磨至4mm左右，以金刚石研磨膏精密抛光；
2)利用内圆切割机将试样加工成尺寸为3×4×40mm的长方体样条，金刚石研磨膏磨倒角；
3)利用金刚石内圆切割机在样条平行于外力加载方向上加工宽度约0.22mm，深度1.4-1.6mm的切口；
4)采用型号为YRWT-D型微机控制电子万能实验机进行测试，跨距为20mm，加载速度为0.05mm/min，试样的断裂韧性下列公式计算。
Figure BDA0003094324720000121
式中：KIC为陶瓷试样的断裂韧性(MPa.m1/2)；a为样条切口深度(mm)；b为样条的宽度(mm)；w为样条的高度(mm)；P为样条断裂时施加的负载(N)；L为设定的试验机跨距(mm)。
同一试样，准备3根样条，测试后取平均值作为其断裂韧性值。
上述实施例1-4所得陶瓷基体的致密度、弯曲强度、断裂韧性与发明专利CN109336564B中的高铝陶瓷相比，其对比试验结果见表2。
表2陶瓷基体性能的对比试验结果表
实施例1 实施例2 实施例3 实施例4 对比项
致密度(％) 95.9 98.6 97.3 96.2 88.2
弯曲强度(MPa) 336 357 368 349 172
断裂韧性(MPa.m<sup>1/2</sup>) 3.0 3.3 3.5 3.1 1.5
根据以上实施例1-8的对比试验结果，可以看出，密封件的抗拉强度高，即陶瓷基体与金属化层之间具有很好的封接效果，陶瓷基体的润湿性能好；陶瓷基体的致密度高，弯曲强度和断裂韧性值较高，即陶瓷基体得致密度和力学性能很好，适合作为Al2O3基陶瓷焊接密封元器件基体材料。
以上所述实施例的各技术特征可以进行任意组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。

Claims (5)

1.一种Al2O3基陶瓷焊接密封元器件，包括陶瓷基体和金属化层，其特征在于，陶瓷基体是由以下重量份数的原料制备：无机纤维-氧化铝三维网状基体80-90份、氧化钇2-5份、氧化硅1-3份、氧化钛2-4份、添加剂0.5-1.0份、粘结剂3-5份和分散剂1-3份，所述添加剂、粘结剂和分散剂分别为LiYO2、聚乙烯醇缩丁醛和三聚磷酸钠；
所述陶瓷基体的制备方法，依次包括以下步骤：
A1、无机纤维-六方氧化铝三维网状基体的制备：
将无机纤维浸渍于2mol/L的NaOH溶液和有机硅绝缘浸渍剂中，在70-90℃下浸渍3-4h，经过滤，干燥，得到表面改性的无机纤维，所述NaOH溶液和有机硅绝缘浸渍剂的质量比为1:1～2；
将氧化铝和表面改性的无机纤维混合，在惰性气氛下，压力为5-10MPa，温度为80-120℃下反应2-6h，制得无机纤维-氧化铝三维网状基体，所述表面改性的无机纤维与氧化铝的质量比为1:4～8；
A2、混料：将氧化硅、氧化钇和添加剂混合均匀后，加入到步骤A1中制得的无机纤维-氧化铝三维网状基体中，然后加入氧化钛、分散剂和水，高速球磨6-8h；
A3、造粒：将研磨后的浆料抽滤，然后用离心式喷雾干燥机加工成平均粒径为20-40μm的颗粒状陶瓷粉末，备用；
A4、一次烧结：将步骤A3所得的陶瓷粉末装入热压模具中，以氮气为保护气，在1000-1200℃进行常温烧结，保温时间为1-2h，制得陶瓷毛坯；
A5、二次烧结：将步骤A4所得的陶瓷毛坯装入热压模具中，以氮气为保护气，在1600-1800℃进行常压烧结，保温时间为2-3h，随炉冷却至室温后取出，然后在平面磨床上抛光，制得待金属化的陶瓷基体。
2.根据权利要求1所述Al2O3基陶瓷焊接密封元器件，其特征在于，所述步骤A1中无机纤维为碳化硅纤维、氮化铝纤维或氧化硅纤维中的一种。
3.根据权利要求1所述Al2O3基陶瓷焊接密封元器件，其特征在于，所述步骤A2的球磨过程中，球磨速率为360r/min，球料比为10:1。
4.根据权利要求1-3任一所述的Al2O3基陶瓷焊接密封元器件的制备方法，其特征在于，包括以下步骤：
B1、金属化膏的制备：称取钛粉10-20份、钨粉40-60份、氧化钼10-20份、氧化硼10-20份、氧化钇2-4份和有机结合剂2-5份，将钛粉、钨粉、氧化钼、氧化硼、氧化钇和有机结合剂一起均匀混合，制得金属化膏；
B2、丝印：将权利要求1中制得的待金属化的陶瓷基体表面用无水乙醇进行超声清洗，然后将金属化膏采用丝网印刷的方法均匀地涂覆在陶瓷基体两端的表面，其中金属化膏的印刷厚度为40-50μm；
B3、金属化处理：上述制备的涂覆有金属化膏的陶瓷基体在真空或惰性气体保护下烧结，烧结温度为1300-1500℃，烧结保温时间为60-90min,即得本发明的Al2O3基陶瓷焊接密封元器件。
5.根据权利要求4所述的一种Al2O3基陶瓷焊接密封元器件的制备方法，其特征在于，所述步骤B1中有机结合剂是按照乙基纤维素：松油醇：乙二醇＝2:1:1的重量比例混合而成。
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