CN113540001B - 一种微电子封装用可伐/银合金复合材料及其制备方法 - Google Patents
一种微电子封装用可伐/银合金复合材料及其制备方法 Download PDFInfo
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Abstract
一种微电子封装用可伐/银合金复合材料及其制备方法,该复合材料中银合金钎料层中Cu的含量为30~35wt%,Ti的含量为0.1~5.0wt%,Ni的含量为0.1~1.0wt%,余量为Ag;可伐合金层为4J29或4J34。制备方法包括:采用真空加压烧结方法制备钎料锭坯,通过热压扩散方式获得复合锭坯,经冷锻成形、中间退火、精密轧制及成品退火,获得厚度为0.15~1.5mm的层状复合材料,其中可伐合金层厚度为0.1~1mm,银合金钎料层厚度为0.01~0.5mm。本发明的可伐/银合金复合材料与陶瓷热膨胀系数匹配性好,可实现与陶瓷件良好封装。钎焊温度适中,封装工艺简单高效,器件封接后不易发生开裂,成品率高。
Description
技术领域
本发明涉及电子封装材料技术领域,具体涉及一种微电子封装用可伐/银合金复合材料及其制备方法。
背景技术
近年来,随着微电子技术迅猛发展,电子设备、元器件等的微小型化、高密度化、高功率化和多功能化,要求与之配套的封装工艺与封装材料具备高稳定性及高可靠性。封装材料用于支撑和保护半导体芯片和电子电路、辅助散失电子元件热量、传递信号等,对微电子组件寿命至关重要。按照材料组分可将电子封装材料分为塑封封装材料、封装用陶瓷材料和金属封装材料。金属封装材料具有机械强度高、散热性能好等不可替代的特点。传统的金属封装材料包括Cu、Al、Mo、可伐合金等。其中可伐合金具有与无氧铜、陶瓷材料等相近的热膨胀系数,以及良好的真空钎焊性能,广泛应用在电子工业中。它可用来与硬玻璃封接制造高气密性元器件,也可以和陶瓷封接制造高频功率管、整流管,在晶体管和集成电路中用作引出线和引线框架等。然而,采用纯铜作为钎料对可伐进行钎焊,封装温度较高导致芯片损伤,使用银铜合金等焊料时,封接过程常出现无法修复的开裂现象,造成管壳微裂、漏气等问题,严重影响器件可靠性,甚至导致器件失效。应用方尝试采用银铜、可伐合金层叠组装方式封装,但存在成品率低、气密性不佳等问题。
发明内容
本发明的主要目的在于提供一种微电子封装用可伐/银合金复合材料,将钎料和封装材料通过冶金结合形成层状复合材料,从而改善大功率真空管件、半导体器件等在封接过程中因高温、金属层间热应力导致的芯片断裂、管壳微裂、漏气等问题,提高微电子元器件封装成品率及服役可靠性。
本发明的另一目的在于提供上述复合材料的制备方法,该方法操作简便,可实现可伐/银铜钛的高可靠复合,且所制备复合材料厚度适中,利于材料后续预成型。
为了实现上述目的,本发明提供如下技术方案:
一种微电子封装用可伐/银合金复合材料,为可伐合金层与银合金钎料层依靠冶金结合形成的双层层状复合材料;银合金钎料层中Cu的含量为30~35wt%,Ti的含量为0.1~5.0wt%,Ni的含量为0.1~1.0wt%,余量为Ag;可伐合金层的材料为4J29或4J34;该复合材料的厚度为0.15~1.5mm,其中可伐合金层厚度为0.1~1mm,银合金钎料层厚度为0.01~0.5mm。
如上所述的可伐/银合金复合材料,优选地,所述银合金钎料层中Cu的含量为32~34wt%,Ti的含量为0.5~4.5wt%,Ni的含量为0.2~0.8wt%,余量为Ag。
如上所述的可伐/银合金复合材料,优选地,所述可伐合金片厚度为0.2~0.5mm,银合金钎料片厚度为0.02~0.2mm。
另一方面,本发明提供如上所述的可伐/银合金复合材料的制备方法,采用“钎料混粉-钎料锭坯制备-锭坯表面处理-锭坯复合-冷锻成形-中间退火-精密轧制-成品退火”的工艺流程,包括以下步骤:
(1)钎料混粉
按照质量百分比称取几种原材料粉末,其中Cu的含量为30~35wt%,Ti的含量为0.1~5.0wt%,Ni的含量为0.1~1.0wt%,余量为Ag,在球磨机中进行混粉;
(2)钎料锭坯制备:采用真空加压烧结方法将球磨后的钎料合金粉末制备成锭坯;
(3)锭坯表面处理:使用双面研磨机对钎料锭坯与可伐合金进行表面处理;
(4)锭坯复合:采用热压扩散方法将表面处理后的银合金锭坯与4J29或4J34可伐合金基体层叠进行初步复合;
(5)冷锻成形:采用小型液压冷锻机对复合锭坯进行冷锻;
(6)中间退火:将冷锻后的复合坯料放入真空炉中进行退火;
(7)精密轧制:将退火后复合坯料进行多道次精密轧制,直至达到成品尺寸;
(8)成品退火:将复合片材放置真空炉中进行退火。
如上所述的方法,优选地,所述步骤(1)中原材料中Cu粉、Ni粉、Ag粉纯度为99.99%,Ti粉纯度为99.9%,粉末粒度均为200目~400目,球磨速度100~200rad/min,球磨时间2小时~4小时。
如上所述的方法,优选地,所述步骤(2)中,真空加压烧结压力为40MPa~60MPa,真空度为1.0×10-3Pa~1.0×10-4pa,烧结温度为700℃~750℃。
如上所述的方法,优选地,所述步骤(4)中可伐合金锭坯厚度为1~8mm,银合金钎料锭坯厚度为0.1~1mm;复合压力为30MPa~50MPa,扩散温度为700℃~750℃,扩散时间为5min~15min。
如上所述的方法,优选地,所述步骤(5)中冷锻变形量为20%~40%,锻压速率为1~2mm·s-1。
如上所述的方法,优选地,所述步骤(6)中真空度为1.0×10-3pa~1.0×10-4Pa,退火温度为580℃~600℃,保温时间为60min~120min;
如上所述的方法,优选地,所述步骤(7)中单道次轧制变形率为20~35%,总变形率小于90%;
如上所述的方法,优选地,所述步骤(8)中真空度为1.0×10-3Pa~1.0×10-4Pa,退火温度为550℃~580℃,保温时间为60min~90min。
本发明的有益效果在于以下几个方面:
(1)本发明的复合材料适用于微电子封装中与陶瓷件直接连接,有效解决传统陶瓷与可伐间接连接工艺复杂、耗时耗资、批次稳定性不佳等问题。
(2)本发明的复合材料包括钎料层与可伐基体层,二者厚度配比适中,可加工成所需形状尺寸后与陶瓷器件快速装配,有效解决目前封装过程中因装配错位等原因导致焊合率低等问题,提高封装效率。
(3)本发明的复合材料钎料层成分中含有活性元素Ti及元素Ni,在钎焊过程中Ti元素可与陶瓷发生反应形成金属间化合物,可改善银合金钎料对陶瓷的润湿,Ni元素的添加可提高钎料层与可伐合金的相似相溶性,通过Fe、Ni元素反应促进钎料层与可伐层界面扩散作用,有利于银合金钎料与可伐合金形成良好的冶金结合,从而增强陶瓷/可伐界面结合强度。
(4)本发明的复合材料制备方法,采用冷锻工艺可改善复合材料的成形性能,有利于后续轧制成形,保证复合材料的尺寸稳定性。中间退火与成品退火两次退火工艺,一方面使得复合材料的成分充分均匀化,结合界面实现元素扩散,另一方面可消除材料在加工过程中产生的残余应力,保证复合材料与陶瓷连接时的可靠复合。
(5)本发明的复合材料与陶瓷热膨胀系数匹配性好,器件封接后不易发生开裂,提高器件封装成品率。
附图说明
图1为实施例1制备的AgCuTiNi/4J29层状复合材料的金相显微镜照片。
具体实施方式
下面对本发明的较优的实施例作进一步的详细说明。应当理解的是,此处所描述的具体实施例仅用于解释本发明,不构成对本发明的限制。
实施例1:制备AgCuTiNi/4J29层状复合材料
步骤1:钎料配料混粉
分别称取粉末粒度200目~400目,纯度为99.99%的Ag粉126克,Cu粉64克,Ni粉1.0克,纯度为99.9%的Ti粉9.0克,在球磨机中进行混粉,球磨速度150rad/min,球磨时间2小时。
步骤2:制坯
将球磨后的粉末进行真空加压烧结,真空度1.0×10-4Pa,温度730℃,压力40MPa,锭坯直径为100mm。
步骤3:锭坯表面处理
将厚度为0.62mm的烧结锭坯与直径为100mm、厚度为4mm的4J29可伐合金放置双面研磨机中进行表面处理。
步骤4:锭坯复合
将表面研磨后的AgCuTiNi与4J29坯料层叠组坯后进行热扩散压力复合,复合压力为40MPa,扩散温度为720℃,扩散时间为10min。
步骤5:冷锻成形
将扩散复合后的锭坯利用小型液压冷锻机进行冷锻,冷锻变形量为20%~30%,锻压速率为1~2mm·s-1。
步骤6:中间退火
将冷锻后的复合坯料放入真空炉中进行退火,真空度为1.0×10-4pa,退火温度为580℃,保温时间为60min。
步骤7:精密轧制
采用精密轧机对退火后复合坯料进行多道次轧制,单道次轧制变形率为20%~25%,直至成品尺寸0.35mm。
步骤8:成品退火
将轧制后的层状复合片材放置在真空炉中,真空度为1.0×10-3Pa,退火温度为550℃,保温时间为60min。
获得的AgCuTiNi/4J29层状复合材料的金相显微镜照片如图1所示,照片可见,银合金层与可伐合金层结合良好,无孔洞、缝隙等缺陷。
实施例2:制备AgCuTiNi/4J29层状复合材料
步骤1:钎料配料混粉
分别称取粉末粒度200目~400目,纯度为99.99%的Ag粉124克,Cu粉68克,Ni粉1.0克,纯度为99.9%的Ti粉7.0克,在球磨机中进行混粉,球磨速度150rad/min,球磨时间2小时。
步骤2:制坯
将球磨后的粉末进行真空加压烧结,真空度1.0×10-4Pa,温度720℃,压力50MPa,锭坯直径为100mm。
步骤3:锭坯表面处理
将厚度为0.60mm的烧结锭坯与直径为100mm、厚度为5mm的4J29可伐合金放置双面研磨机中进行表面处理。
步骤4:锭坯复合
将表面研磨后的AgCuTiNi与4J29坯料层叠组坯后进行热扩散压力复合,复合压力为50MPa,扩散温度为710℃,扩散时间为5min。
步骤5:冷锻成形
将扩散复合后的锭坯利用小型液压冷锻机进行冷锻,冷锻变形量为30%~40%,锻压速率为1~2mm·s-1。
步骤6:中间退火
将冷锻后的复合坯料放入真空炉中进行退火,真空度为1.0×10-4Pa,退火温度为590℃,保温时间为60min。
步骤7:精密轧制
采用精密轧机对退火后复合坯料进行多道次轧制,单道次轧制变形率为30%~35%,直至成品尺寸0.5mm。
步骤8:成品退火
将轧制后的层状复合片材放置在真空炉中,真空度为1.0×10-3pa,退火温度为560℃,保温时间为60min。
实施例3:制备AgCuTiNi/4J34层状复合材料
步骤1:钎料配料混粉
分别称取粉末粒度200目~400目,纯度为99.99%的Ag粉132克,Cu粉66克,Ni粉0.8克,纯度为99.9%的Ti粉1.2克,在球磨机中进行混粉,球磨速度150rad/min,球磨时间2小时。
步骤2:制坯
将球磨后的粉末进行真空加压烧结,真空度1.0×10-4pa,温度740℃,压力40MPa,锭坯直径为100mm。
步骤3:锭坯表面处理
将厚度为0.64mm的烧结锭坯与直径为100mm、厚度为5.8mm的4J34可伐合金放置双面研磨机中进行表面处理。
步骤4:锭坯复合
将表面研磨后的AgCuTiNi与4J34坯料层叠组坯后进行热扩散压力复合,复合压力为40MPa,扩散温度为730℃,扩散时间为15min。
步骤5:冷锻成形
将扩散复合后的锭坯利用小型液压冷锻机进行冷锻,冷锻变形量为30%~40%,锻压速率为1~2mm·s-1。
步骤6:中间退火
将冷锻后的复合坯料放入真空炉中进行退火,真空度为1.0×10-4Pa,退火温度为580℃,保温时间为90min。
步骤7:精密轧制
采用精密轧机对退火后复合坯料进行多道次轧制,单道次轧制变形率为30%~35%,直至成品尺寸0.8mm。
步骤8:成品退火
将轧制后的层状复合片材放置在真空炉中,真空度为1.0×10-3Pa,退火温度为550℃,保温时间为90min。
实施例4:制备AgCuTiNi/4J34层状复合材料
步骤1:钎料配料混粉
分别称取粉末粒度200目~400目,纯度为99.99%的Ag粉129.6克,Cu粉62克,Ni粉0.4克,纯度为99.9%的Ti粉8克,在球磨机中进行混粉,球磨速度150rad/min,球磨时间2小时。
步骤2:制坯
将球磨后的粉末进行真空加压烧结,真空度1.0×10-4Pa,温度750℃,压力60MPa,锭坯直径为100mm。
步骤3:锭坯表面处理
将厚度为0.62mm的烧结锭坯与直径为100mm、厚度为5mm的4J34可伐合金放置双面研磨机中进行表面处理。
步骤4:锭坯复合
将表面研磨后的AgCuTiNi与4J34坯料层叠组坯后进行热扩散压力复合,复合压力为30MPa,扩散温度为740℃,扩散时间为5min。
步骤5:冷锻成形
将扩散复合后的锭坯利用小型液压冷锻机进行冷锻,冷锻变形量为20%~30%,锻压速率为1~2mm·s-1。
步骤6:中间退火
将冷锻后的复合坯料放入真空炉中进行退火,真空度为1.0×10-4Pa,退火温度为600℃,保温时间为120min。
步骤7:精密轧制
采用精密轧机对退火后复合坯料进行多道次轧制,单道次轧制变形率为30%~35%,直至成品尺寸0.6mm。
步骤8:成品退火
将轧制后的层状复合片材放置在真空炉中,真空度为1.0×10-3Pa,退火温度为580℃,保温时间为90min。
实验例1性能检测
分别对实施例1~4制备的复合材料进行力学性能测试与界面分析,并与Al2O3陶瓷进行钎焊封接后进行气密性测试,结果见表1。
表1
钎焊温度 | 剥离强度 | 银合金/可伐层厚比 | 气密性 | |
实施例1 | 850℃ | 6.5N/m | 1∶6 | <1.0×10-13Pa·m3/s |
实施例2 | 850℃ | 6.0N/m | 1∶8 | <1.0×10-13Pa·m3/s |
实施例3 | 850℃ | 5.9N/m | 1∶9 | <1.0×10-13Pa·m3/s |
实施例4 | 850℃ | 6.1N/m | 1∶8 | <1.0×10-13Pa·m3/s |
以上实验结果表明,本发明的可伐/银合金复合材料与陶瓷热膨胀系数匹配性好,可实现与陶瓷件良好封装。钎焊温度适中,封装工艺简单高效,器件封接后不易发生开裂,成品率高。
上述实施例中仅仅举出本发明可伐/银合金复合材料及其制备方法部分的实施例,在上述本发明的技术方案中:所述的合金组分Ag、Cu、Ni、Ti的含量在规定范围内可自由选择,此处不再一一列举,故以上的说明所包含的技术方案应视为例示性,而非用以限制本发明申请专利的保护范围。
Claims (10)
1.一种微电子封装用可伐/银合金复合材料,其特征在于:该可伐/银合金复合钎料为可伐合金层与银合金钎料层依靠冶金结合形成的双层层状复合材料;银合金钎料层中Cu的含量为30~35 wt%,Ti的含量为0.1~5.0 wt%,Ni的含量为0.1~1.0 wt%,余量为Ag;可伐合金层的材料为4J29或4J34;该复合材料的厚度为0.15~ 1.5mm,其中可伐合金层厚度为0.1~1mm,银合金钎料层厚度为0.01~0.5mm。
2. 根据权利要求1所述的可伐/银合金复合材料,其特征在于:所述银合金钎料层中Cu的含量为32~34 wt%,Ti的含量为0.5~4.5 wt%,Ni的含量为0.2~0.8 wt%,余量为Ag。
3.根据权利要求1所述的可伐/银合金复合材料,其特征在于:所述可伐合金层厚度为0.2~0.5mm,银合金钎料层厚度为0.02~0.2mm。
4. 根据权利要求1所述的可伐/银合金复合材料的制备方法,其特征在于:采用“钎料混粉-钎料锭坯制备-锭坯表面处理-锭坯复合-冷锻成形-中间退火-精密轧制-成品退火”的工艺流程,包括以下步骤:
(1)钎料混粉
按照质量百分比称取几种原材料粉末,其中Cu的含量为30~35 wt%,Ti的含量为0.1~5.0 wt%,Ni的含量为0.1~1.0 wt%,余量为Ag,在球磨机中进行混粉;
(2)钎料锭坯制备:采用真空加压烧结方法将球磨后的钎料合金粉末制备成锭坯;
(3)锭坯表面处理:使用双面研磨机对钎料锭坯与可伐合金进行表面处理;
(4)锭坯复合:采用热压扩散方法将表面处理后的银合金锭坯与4J29或4J34可伐合金基体层叠进行初步复合;
(5)冷锻成形:采用小型液压冷锻机对复合锭坯进行冷锻;
(6)中间退火:将冷锻后的复合坯料放入真空炉中进行退火;
(7)精密轧制:将退火后复合坯料进行多道次精密轧制,直至达到成品尺寸;
(8)成品退火:将复合片材放置真空炉中进行退火。
5.根据权利要求4中所述的方法,其特征在于,所述步骤(1)中原材料中Cu粉、Ni粉、Ag粉纯度为99.99%,Ti粉纯度为99.9%,粉末粒度均为200目~400目,球磨速度100~200rad/min,球磨时间2小时~4小时。
6.根据权利要求4中所述的方法,其特征在于,所述步骤(2)中,真空加压烧结压力为40MPa~60MPa,真空度为1.0×10-3Pa~1.0×10-4Pa,烧结温度为700℃~750℃。
7.根据权利要求4中所述的方法,其特征在于,所述步骤(4)中,可伐合金锭坯厚度为1~8mm,银合金钎料锭坯厚度为0.1~1mm;复合压力为30MPa~50MPa,扩散温度为700℃~750℃,扩散时间为5min~15min。
8.根据权利要求4中所述的方法,其特征在于,所述步骤(5)中冷锻变形量为 20%~40%,锻压速率为1~2mm·s-1。
9.根据权利要求4中所述的方法,其特征在于,所述步骤(6)中真空度为1.0×10-3Pa~1.0×10-4Pa,退火温度为580℃~600℃,保温时间为60min~120min。
10.根据权利要求4中所述的方法,其特征在于,所述步骤(7)中单道次轧制变形率为20~35%,总变形率小于90%;
所述步骤(8)中真空度为1.0×10-3Pa~1.0×10-4Pa,退火温度为550℃~580℃,保温时间为60min~90min。
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