CN101508016B - 一种用于键合金丝的中间合金制备新方法 - Google Patents
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Abstract
本发明公开了一种生产键合金丝用的中间合金制备方法。其制备过程为,将纯度不低于5N的高纯金与添加量不大于1%的微合金元素置于真空感应熔炼炉内,在高真空条件下(10-3Pa),通入保护气体,利用真空中频感应加热,采用漏浇工艺使合金液体在高温下快速激冷,形成小颗粒(近似球状)状中间合金。该中间合金颗粒成分均匀,不存在偏析,无污染不需加工,方便使用。利用此法制备的中间合金来生产键合金丝,解决了控制微量添加组分烧损不易控制及合金元素均匀分布等问题,为超细丝的后续加工提供了优质坯料。
Description
技术领域
本发明涉及一种用于键合金丝生产的中间合金制备方法——漏浇-激冷法。
背景技术
在金属材料冶炼和铸造时,常常先把一些添加元素与基体元素做成中间合金,再将其加入基体中进行熔铸,其目的是使添加的元素合金化更充分,添加元素的分布更均匀,烧损更小。中间合金传统的制作方法是将添加元素按大量加入原则配比,与母体金属直接熔合铸成块,再分析合金成分后轧成片或碎块待用。在有色金属加工中,常见的中间合金有Cu-P8~14%,熔点714~1022℃;Cu-Be3~4%,熔点864℃;Ni-Mg17%熔点1082℃;Au-Ge8~12%熔点400~500℃;Ag-Mg10%熔点759℃等,这些中间合金大都是在熔铸车间自行熔制的,无标准遵循,一般中间合金具备如下技术条件:1、熔化温度低于或者接近合金的熔化温度;2、添加元素含量尽量提高;3、化学成分均匀一致,夹杂物少;4、希望中间合金铸块有脆性,方便破碎;5、能够抵抗大气腐蚀作用,保存期间不会氧化碎成粉末。
在微电子封装材料领域,键合金丝是一种综合性能要求极高的精密合金材料,其关键技术之一就是添加适量的中间合金进行微合金化。目前国内外对键合金丝的专利权限主要公知了微合金元素的配方组成,如日本专利:Japanese PatentApplication 074421(US Patent No.4752442)、Japanese Patent Application6-311524、Japanese Patent Application 06/160302(US Patent No.4330329);欧洲专利European Patent Application 0743697 A2。而对中间合金的制备工艺未涉及。
发明内容
本发明的目的是提供一种用于键合金丝生产的中间合金制备方法——漏浇-激冷法。该方法可以解决微合金元素易氧化、易挥发、易燃、易损等问题,通过此法所得中间合金,添加到母体金属液中,合金化速度快,分散性好,在高真空精密连铸过程中,组分烧损可控、强化元素分布均匀,铸锭组织均一。
本发明是在高真空条件下(10-3Pa),通入惰性保护气体,利用中频感应加热及漏浇方法来制备中间合金。其制备步骤为:
(1)备料:将高纯金(≥99.999%)在真空条件下,使用高纯度坩埚及模具浇铸成坯料,轧制该坯料成薄带材,用5%的稀盐酸加热煮15分钟备用。
(2)配料:将一定量的高纯金带材与添加量≤1%的微合金元素(微合金元素的纯度≥99.95%)进行配料,配料过程中需注意污染及微合金元素的氧化问题。
(3)制备:用轧制好的高纯金薄带材将微合金元素紧紧地包裹起来,对准激冷塔和漏浇口,放置于真空感应熔炼炉内。预抽真空到1×101Pa,并充入惰性气体Ar反复清洗,然后抽高真空达到1×10-3Pa,再充入氩气,立即升温熔炼。当温度达到浇铸温度1200~1400℃时,保温1~5分钟后,以80~120g/min的速度通过漏浇口浇注于激冷塔上(激冷条件为:水流量≥10L/min,水压≥2MPa,水温≤20℃),形成大小基本一致,呈近似球状的合金颗粒。
申请人发明的漏浇-激冷法制备的中间合金,与传统方法比较,具有添加元素含量分布均匀、成份可控性好、对金微合金化作用明显(提高再结晶温度、晶粒细化作用显著、提高抗拉强度、改善可加工性)等特点。利用此法制备的中间合金来生产键合金丝,解决了控制微量添加组分烧损不易控制及合金元素均匀分布等问题,为超细丝的后续加工提供了优质坯料。
具体实施方式
1、工艺过程
(1)备料:将高纯金(≥99.999%)在真空条件下,使用高纯度坩埚及模具浇铸成坯料,轧制该坯料成薄带材,用5%的稀盐酸加热煮15分钟备用。
(2)配料:称取99g高纯金带材与1gCa、或1g Be、或1g Ce、或1g Ga等微合金元素(微合金元素纯度≥99.95%)进行配料,过程中需注意污染及微合金元素的氧化问题。
(3)制备:用轧制好的高纯金薄带材将微合金元素紧紧地包裹起来,对准激冷塔和漏浇口,放置于真空感应熔炼炉内。预抽真空到1×101Pa,并充入惰性气体Ar反复清洗,然后抽高真空达到1×10-3Pa,再充入氩气,立即升温熔炼。当温度达到浇铸温度1200~1400℃时,保温1~5分钟后,以80~120g/min的速度通过漏浇口浇注于激冷塔上(激冷条件为:水流量≥10L/min,水压≥2MPa,水温≤20℃),形成大小基本一致,呈近似球状的合金颗粒。
2、实施例情况
运用该方法制备中间合金,其合金成份如下表:
采用本法所制的中间合金制备键合金丝已有74批次232公斤,拉伸加工性能优良,5000m以上单丝长丝率达到74%,φ15μm超细键合金丝单丝长度最长达到20000m,综合成品率达到86.7%,产品性能优良,产销率100%。
Claims (4)
1.一种生产键合金丝用中间合金的制备方法,其特征在于包括以下步骤:
(1)将高纯金在真空条件下脱气铸成坯料并轧成薄带材,之后用质量百分比为5%的稀盐酸煮15分钟并烘干;
(2)按微合金元素添加量的质量百分比≤1%的配料方案进行配料;
(3)用轧制好的高纯金薄带材将微合金元素紧紧地包裹起来,对准激冷塔和漏浇口,放置于真空感应熔炼炉内;
(4)预抽真空并充氩气反复清洗后,抽高真空达1×10-3Pa,再充入氩气达0.05MPa,升温熔炼;
(5)当温度达到浇注温度1200~1400℃时,保温1~5分钟后,以80~120g/min的速度通过漏浇口浇注于激冷塔上。
2.根据权利要求1所述的生产键合金丝用中间合金制备方法,其特征在于所述的微合金元素为Be、Mg、Ca、Cu、Ag、Ce、La、Sc中的任意一种元素。
3.根据权利要求1所述的生产键合金丝用中间合金制备方法,其特征在于制备中间合金用的高纯金纯度≥99.999%的质量百分比,微合金元素纯度≥99.95%的质量百分比。
4.根据权利要求1所述的生产键合金丝用中间合金制备方法,其特征在于激冷塔的激冷条件为:水流量≥10L/min,水压≥2MPa,水温≤20℃。
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