CN113073295B - 一种钨溅射靶材坯料的制备方法及应用 - Google Patents
一种钨溅射靶材坯料的制备方法及应用 Download PDFInfo
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Abstract
本发明提供一种钨溅射靶材坯料的制备方法及应用,所述方法包括:对钨板坯进行交叉轧制使柱状晶破碎、然后进行再结晶退火使晶粒等轴化,其中,所述钨板坯通过化学气相沉积法制得,其纯度≥6N。本发明方法制备的钨溅射靶材坯料的纯度、致密度等性能指标理想,且作为集成电路制造的原料进行真空溅射成膜时,溅射速率稳定,薄膜均匀一致,降低薄膜电阻率,提高成品良率,同时,该方法可操作性强,具有广泛的应用前景。
Description
技术领域
本发明涉及溅射靶材技术领域,尤其涉及一种钨溅射靶材坯料的制备方法及应用。
背景技术
溅射是利用一定能量的粒子(离子或中性原子、分子)轰击靶材表面,使靶材表面的原子或分子获得足够大的能量而最终脱离靶材并沉积在基体表面,形成微米尺度(甚至纳米尺度)薄膜,是目前应用十分广泛的薄膜制备方法。溅射靶材是粒子轰击的对象,是溅射法沉积薄膜的原材料,很大程度上决定薄膜的性能、制备效率以及产品良率。溅射作为一种先进的薄膜材料制备技术,广泛应用于微电子、光电子等现代高科技领域。
钨是典型的难熔金属,熔点高(3410℃),具有稳定的高温特性、抗电子迁移能力和较高的电子发射系数等诸多优点,在集成电路(主要是存储芯片和射频芯片)制备等行业中具有广泛的应用前景,因而钨溅射靶材的需求量日益扩大。
目前钨溅射靶材坯料主要采用粉末冶金技术,主要有以下两种方案:其一,采用热等静压或SPS放电等离子烧结致密化处理;其二,采用常压烧结,再进行轧制致密化。采用上述方案制备的钨溅射靶材坯料的纯度可达到5N5,密度为19.10~19.15g/cm3,同时作为集成电路制造的原料进行真空溅射成膜时,溅射速率不稳定,薄膜电阻率较理论电阻率偏高,并最终导致芯片的良率较低,亟需高性能钨溅射靶材,而靶材的性能根本上取决于靶材坯料的性能,因此坯料的制备方法仍需深入研究。
发明内容
本发明提供一种钨溅射靶材坯料的制备方法及应用,该方法制备的钨溅射靶材坯料的纯度、致密度等性能指标理想,且作为集成电路制造的原料进行真空溅射成膜时,溅射速率稳定,所得薄膜均匀一致,降低薄膜电阻率,提高成品良率,同时,该方法可操作性强,具有广泛的应用前景。
根据本发明的第一方面,提供了一种钨溅射靶材坯料的制备方法,所述方法包括:对钨板坯进行交叉轧制使柱状晶破碎、然后进行再结晶退火使晶粒等轴化,其中,所述钨板坯通过化学气相沉积法制备得到,其纯度可达到6N甚至8N。
发明人在钨溅射靶材坯料的研发过程中发现,采用化学气相沉积法能够制得纯度高、致密度大的钨溅射靶材坯料,但是由于气相沉积钨材料在进行真空溅射成膜时,经常出现溅射速率不稳定问题,究其原因是化学气相沉积的钨涂层为柱状晶结构组织,距离基体远的位置晶粒尺寸偏大,与此同时基体近表面的致密性问题也会造成薄膜质量不佳问题。通过采用特定的轧制工艺使柱状晶破碎,保证在厚度方向具有均匀的结构性能和微观组织,然后通过再结晶退火使晶粒等轴化,能够获得细小均匀的晶粒结构,在真空溅射成膜时,表现出优异的溅射性能和溅射薄膜的品质,溅射速率的波动小,成膜均匀一致,降低薄膜电阻率,提高成品良率。
进一步地,所述交叉轧制为垂直交叉,包括至少一道次换向,第一道次轧制压下量为20~50%,总压下量不低于75%,两个方向的压下量差异≤20%,初始轧制温度1550℃~1800℃,道次间保温温度≥1500℃。其中,所述两个方向分别指:第一轧制方向,即垂直于晶粒生长的方向;第二轧制方向即垂直于第一轧制方向。
进一步地,所述再结晶退火在氢气炉、惰性气体保护炉或真空炉中进行;所述再结晶退火的温度为1700~2200℃,时间为1~10h。
进一步地,所述方法还包括对所述再结晶退火后的钨板坯进行磨削加工;可选地,所述磨削加工的总加工余量为2~5mm,正面加工余量≥0.5mm,底面加工余量≥1mm。
进一步地,在对所述钨板坯进行交叉轧制之前,对所述钨板坯进行保温处理;可选地,所述保温处理的温度为1550~1650℃,时间为30~60min。
进一步地,所述钨板坯通过将WF6和H2通入常压反应室进行化学气相沉积,在基体上沉积钨涂层制得;可选地,所述WF6和H2的纯度均不低于5N;和/或,所述基体包括紫铜、不锈钢、钼、不锈钢镀铜中的至少一种。
进一步地,所述沉积的温度为450~600℃,沉积速度为0.1~0.8mm/h,所述钨板坯的厚度为20~50mm。
进一步地,所述方法包括以下步骤:
(1)以WF6和H2为原料,通入常压反应室进行化学气相沉积,在基体上沉积钨涂层,得到纯度≥6N的钨板坯;
(2)将步骤(1)中得到的钨板坯进行退火处理;
(3)将步骤(2)中得到的钨板坯进行交叉轧制处理;
(4)将步骤(3)中得到的钨板坯进行再结晶退火处理;
(5)将步骤(4)中得到的钨板坯进行磨削加工处理,得到钨溅射靶材坯料。
根据本发明的第二方面,提供了由前面所述的制备方法得到的钨溅射靶材坯料。
根据本发明的第三方面,提供了前面所述的钨溅射靶材坯料在集成电路制备中的应用。
本发明提供的一种钨溅射靶材坯料的制备方法及应用,具有如下效果:
(1)本发明方法制备的钨溅射靶材坯料纯度达到8N,密度大于19.15g/cm3,具有更优异的纯度和致密性的性能指标,在提高组织均匀性的同时,降低晶粒尺寸,在真空溅射成膜时,表现出优异的溅射性能和溅射薄膜的品质,溅射速率稳定,成膜均匀一致,降低薄膜电阻率,提高成品良率,且该方法可操作性强,具有广泛的应用前景。
(2)本发明通过化学气相沉积法得到的钨板坯经交叉轧制、再结晶退火后,其力学性能有显著提升,同时塑性明显提高,延伸率可达40%,有助于后续的磨削加工以提高靶材表面质量。
(3)本发明方法基于化学气相沉积法,通过调整基体的尺寸和连续气相沉积反应,能够实现大尺寸靶材的批量生产,提高了生产效率,节省了生产成本。
附图说明
图1是实施例1中常压化学气相沉积得到的钨板坯的三维金相组织,箭头方向为生长方向;
图2是实施例1中钨溅射靶材坯料的金相组织,箭头方向为轧制方向,垂直箭头方向为生长方向;
图3是实施例1中钨溅射靶材坯料的C扫描照片;
图4是应用于8英寸基台的钨靶材坯料;
图5是实施例3中钨溅射靶材坯料的组织照片,(a)代表RD-ND面,(b)代表TD-ND面;
图6是实施例1和实施例3的钨溅射靶材坯料的三点弯曲力学特性的对比图。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚,下面将结合本发明中的附图,对本发明中的技术方案进行清楚、完整地描述,显然,所描述的实施例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作出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
实施例1
本实施例的钨溅射靶材坯料的制备方法包括:
常压化学气相沉积过程:以电子级99.9995%纯度WF6为原料,99.9995%纯度H2为原料,紫铜为基体,沉积温度580℃,沉积速度0.4mm/h,获得长度380mm、宽度190mm、厚度35mm的钨板坯,纯度8N,密度19.18g/cm3;
保温及交叉轧制过程:氢气炉1600℃保温40min,沿长度方向进入轧机,第一道次,压下量30%,1570℃保温30min,第二道次,压下量30%,1570℃保温20min,轧制方向转90°,第三道次,压下量30%,1570℃保温10min,第4道次,压下量30%,最终长度775mm,宽度387mm,厚度8.4mm,可制备直径332mm靶材两块。
再结晶退火过程:氢气炉1800℃保温4h,获得完全再结晶钨板坯。
机械加工过程:线切割下料,外圆磨和平面磨,正面磨削量1mm,底面磨削量1.1mm,最终板厚6.3mm。
实施例2
本实施例的钨溅射靶材坯料的制备方法包括:
常压化学气相沉积过程:以电子级99.9995%纯度WF6为原料,99.9995%纯度H2为原料,紫铜为基体,沉积温度550℃,沉积速度0.3mm/h,获得长度和宽度均为240mm、厚度35mm的钨板坯,纯度8N,密度19.21g/cm3;
保温及交叉轧制过程:氢气炉1580℃保温40min,沿长度方向进入轧机,第一道次,压下量30%,1580℃保温30min,第二道次,压下量30%,1580℃保温20min,轧制方向转90°,第三道次,压下量30%,1580℃保温10min,第4道次,压下量30%,最终长度和宽度为490mm,厚度8.4mm,可制备直径450mm靶材1块。
再结晶退火过程:氢气炉2000℃保温1h,获得完全再结晶钨板坯。
机械加工过程:线切割下料,外圆磨和平面磨,正面磨削量1mm,底面磨削量1.1mm,最终板厚6.3mm。
实施例3
本实施例的钨溅射靶材坯料的制备方法与实施例1的区别在于轧制过程不同,具体地,本实施例的轧制过程包括:氢气炉1600℃保温40min,沿长度方向进入轧机,第一道次,压下量30%,1570℃保温30min,第二道次,压下量20%,1570℃保温20min,第三道次,压下量10%,1570℃保温10min,第4道次,压下量10%。
参见图2和图5,及图6,与实施例1相比,本实施例制得的钨溅射靶材坯料的微观组织均匀性明显较差,力学性能也明显降低。
测试例1
将实施例1和实施例3的钨溅射靶材坯料进行低膜厚成膜,溅射条件及结果见表1。
表1
结果显示,以本发明实施例制备的钨溅射靶材坯料为原料进行溅射成膜时,溅射薄膜的品质优良。同时,在基本相同的溅射条件且所得薄膜厚度基本相同的条件下,实施例1的钨溅射靶材坯料的膜阻较实施例3明显降低,约为其1/6~1/2,具有更优异的溅射薄膜的品质。
最后应说明的是:以上实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的精神和范围。
Claims (4)
1.一种钨溅射靶材坯料的制备方法,其特征在于,对钨板坯进行垂直交叉轧制使柱状晶破碎、然后进行再结晶退火使晶粒等轴化,其中,所述钨板坯通过化学气相沉积法制备得到,包括以下步骤:
(1)以WF6和H2为原料,通入常压反应室进行化学气相沉积,以紫铜为基体,在基体上沉积钨涂层,沉积温度580℃,沉积速度0.4mm/h,获得长度380mm、宽度190mm、厚度35mm的钨板坯,纯度为8N,密度为19.18g/cm3;所述WF6和H2的纯度均不低于5N;
(2)将步骤(1)中得到的钨板坯进行退火处理:氢气炉1600℃保温40min;
(3)将步骤(2)中得到的钨板坯进行垂直交叉轧制处理:沿长度方向进入轧机,第一道次,压下量30%,1570℃保温30min,第二道次,压下量30%,1570℃保温20min,轧制方向转90°,第三道次,压下量30%,1570℃保温10min,第4道次,压下量30%;
(4)将步骤(3)中得到的钨板坯进行再结晶退火处理:氢气炉1800℃保温4h,获得完全再结晶钨板坯;
(5)将步骤(4)中得到的钨板坯进行磨削加工处理,得到钨溅射靶材坯料。
2.根据权利要求1所述的钨溅射靶材坯料的制备方法,其特征在于,所述磨削加工的总加工余量为2~5mm,正面加工余量≥0.5mm,底面加工余量≥1mm。
3.权利要求1或2所述的制备方法得到的钨溅射靶材坯料。
4.权利要求3所述的钨溅射靶材坯料在集成电路芯片制造中的应用。
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