CN113463053B - 一种钼镍基多元合金旋转靶材及其制备方法 - Google Patents

一种钼镍基多元合金旋转靶材及其制备方法 Download PDF

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CN113463053B
CN113463053B CN202110763518.0A CN202110763518A CN113463053B CN 113463053 B CN113463053 B CN 113463053B CN 202110763518 A CN202110763518 A CN 202110763518A CN 113463053 B CN113463053 B CN 113463053B
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吴宇宁
卿海标
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Nanjing Damai Technology Industry Co ltd
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Abstract

本发明公开了一种钼镍基多元合金旋转靶材及其制备方法,旋转靶材原子组成是Mo100‑x‑y‑ zNixTiyAlz,且X、Y、Z表示原子组成百分比,10≤X≤40,1≤Y≤20,1≤Z≤18;制备先将钼粉、电解镍粉和钛铝预合金粉末按比例混合,然后进行脱氧提纯处理、进行球磨混合、灌粉振实处理、冷等静压成型、脱模、真空卧式烧结、旋锻处理、退火处理得到钼镍钛铝合金管锭,最后通过机加工切片制成钼镍钛铝合金靶材。本发明制备过程能够减少杂质元素的引入,所生产靶材成分均匀、无偏析、晶粒细小,密度可达到理论值99%以上,能够完全满足目前大尺寸溅射靶材的镀膜要求。

Description

一种钼镍基多元合金旋转靶材及其制备方法
技术领域
本发明属于磁控溅射金属靶材,尤其涉及一种大尺寸钼镍钛铝四元合金管状溅射靶材及其制备方法。
背景技术
随着平面显示器的大型化和高精度化,铜作为FPD驱动元件的薄膜晶体管(TFT)的主布线薄膜材料,铜金属化在TFT-LCD工业中得到了广泛的发展,在大面积高频驱动TFT液晶显示器中,由于铜对玻璃基板的附着力较低,因此铜需借助一种粘合金属膜层作为底层或覆盖层,如Mo,Ti,Nb,Ni,Ta,Cr等金属膜层。当不同的金属与铜置于蚀刻液中时,会发生典型的电偶反应,铜在干燥后被削弱或在金属表面产生部分污点,导致薄膜晶体管性能和显示质量变差。因此对金属薄膜材料的抗氧化性和热稳定性,易蚀刻性及较低阻抗要求极高,当前采用的钼钛或钼钛镍合金膜层对玻璃基板虽有良好的附着力,对硅和氧化铟锡的接触电阻较低,但因含钛元素,钛不能很好的溶于磷酸、醋酸、硝酸溶液中,会造成蚀刻不完全有残留物的风险,严重影响TFT制程质量。与钛相比,铝具有优良的抗氧化性能,同时在PAN中具有良好的蚀刻性能,因此,为改善TFT钼合金薄膜的特性,特提出添加一定量Al形成新的合金膜层(钼镍钛铝合金膜层),可确保拥有较好附着力,抗氧化性,耐热性,低电阻率的前提下兼顾易蚀刻的特性薄膜。与之对应的钼镍钛铝合金溅射靶材目前研究相对较少,由于旋转靶镀膜利用率约达75%,远高于平面靶30%的利用率,因此,对钼镍钛铝合金旋转靶材的制备开发将十分重要,所需靶材尺寸也越来越大。
因钼的熔点高达2620℃,密度10.2g/cm3,而铝的熔点660℃,密度2.7g/cm3,两者熔点和密度差别较大,采用真空熔炼法很容易缩孔及偏析,无法保证产品组织与成分均匀性,且产生多种脆性相,产品易开裂,无法制备大尺寸靶材。若采用热压烧结方式制备,该方法虽在一定程度在可避免合金成分偏析,但热压过程无法将氧,氮等气体杂质元素脱除,会导致产品杂质及氧含量的超标,导致溅射镀膜过程中打弧;另外,因热压烧结设备限制,难以制备长度超过1.5米靶材。
发明内容
发明目的:本发明的第一目的是提供一种大尺寸,高密度,高纯度且成分均匀无偏析钼镍钛铝多元合金旋转溅射靶材;本发明的第二目的在于提供上述钼镍钛铝多元合金旋转溅射靶材的制备方法。
技术方案:本发明的一种钼镍基多元合金旋转靶材,所述旋转靶材原子组成是Mo100-x-y-zNixTiyAlz,且X、Y、Z表示原子组成百分比,10≤X≤40,1≤Y≤20,1≤Z≤18。
本发明通过Mo、Ni、Ti和Al进行复配制备旋转靶材,使得金镀膜层易蚀刻不会产生残留,拥有较好附着力,抗氧化性,耐湿性及低电阻率,完全满足TFT制程中主导线膜层需求。其中Ti、Al的加入不仅能够去除合金粉末中部分残余的氧,亦可与Ni形成微量的Ti3Al(γ+α)、Ni2TiAl、Ni3Al金属间化合物,从而提高合金的室温强度、韧性,抑制Ni的富集。所述成分中,由于Ni与Mo相比容易向Cu热扩散,若成为富Ni合金,则会向主布线膜的Cu扩散Ni,从而使电阻值增加,因此Ni的添加量控制在40at%以下。而Ti主要影响整体合金的耐氧化性及耐湿性,当Ti的添加量超过20at%时,耐氧化性及耐湿性效果饱和,蚀刻性会下降;其次,为确保较好耐氧化性的前提下还能拥有较好蚀刻性,所添加Al的含量不超过18at%较好,因为铝含量过多会造成腐蚀过快,耐湿性较低缺陷。
进一步的,本发明的合金靶材内气体等杂质元素含量尽可能的少,具体体现在原料的选择上,Mo由钼粉提供,钼粉粒度为3~7μm,氧含量≤1000ppm,纯度大于99.95%;Ni由电解镍粉提供,电解镍粉粒度为6~12μm,氧含量≤2000ppm,纯度大于99.9%;Ti和Al由钛铝预合金粉末提供,钛铝预合金粉末的粒度为35~60μm,氧含量≤3000ppm。还有其他如碳≤50ppm,钾≤50ppm等,气体杂质元素过多会导致溅射镀膜过程中打弧,影响镀膜质量。
本发明还保护所述的钼镍基多元合金旋转靶材的制备方法,包括以下步骤:
步骤一、将钼粉、电解镍粉和钛铝预合金粉末按比例混合,然后置于真空炉内进行脱氧提纯处理,然后将脱氧提纯处理的粉体进行球磨混合;
步骤二、将球磨后的粉体灌入管状模腔内,灌粉全程采用振动平台振实粉体,灌粉完成后抽真空并密封,然后进行冷等静压成型,最终脱模压制成相对密度为68~70%的合金管坯;
步骤三、将脱模后的合金管坯放于真空烧结炉内进行卧式烧结,得到相对密度大于98%的合金管坯;
步骤四、将烧结后的合金管坯进行旋锻处理;
步骤五、将锻造后的管坯放入真空炉进行去应力退火处理,得到钼镍钛铝合金管锭,最后通过机加工切片,与铜背板焊合绑定,经过清洗及干燥制成钼镍钛铝合金靶材。
进一步的,所述步骤二中,卧式烧结的参数为:首段按4~6℃/min的升温速率至950℃保温2~5h,第二段按2~4℃/min的升温速率至1150~1280℃保温烧结3~7h,之后随炉降温,烧结期间真空度不小于3*10-3pa。在卧式烧结放置合金管坯时,采用球形氧化铝陶瓷颗粒将整管填埋,控制氧化铝陶瓷颗粒的粒径2~5mm。这里采用氧化铝陶瓷颗粒使内孔及四周均填埋好,因高温烧结收缩时,由于管坯较长壁厚较大,径向上端因自重会变形凹陷,采用填粉方式可确保在烧结过程中管坯正常收缩同时,避免径向变形过大发生椭圆弯曲现象,烧结后合金管变形均匀,内孔无椭圆凹陷发生。
进一步的,所述步骤三中,冷等静压成型的压力为230~330MPa,保压时间为240~500s;振实粉体时振动平台的振幅为3~6mm,激振力为110~130KN。优选的,在压制过程中,压制模具结构为:内芯为实心钢棒,其表面经过高频淬火并抛光至Ra0.2,并带有1~2mm锥度,有利于后续坯管脱模;外层套有厚度5~15mm的圆柱形聚氨酯类胶套,该胶套内径底部较小,上端较大结构,两端采用圆形胶塞配合密封。胶套外层套有304不锈钢圆桶,其表面均匀开有若干导流孔,孔径10-30mm,利用其刚性来固定和控制装料过程粉坯不变形,同时导流孔可保证冷等静压时粉坯各个点受力均匀。
进一步的,所述步骤一中,真空炉内的处理温度为950~1100℃,脱氧提纯处理的时间为2~5h;球磨的转速为120~210R/M,氩气保护球磨时间为8~12h。由于市场上原料粉末氧含量普遍较高,氧含量超标会导致溅射镀膜过程中打弧,影响镀膜质量,通过前期真空脱氧处理可去除初始粉体的氧、氮,氢及低熔点物质等异相杂质,减低氧含量,提升粉体的纯度,确保最终靶材纯度。在球磨过程中,球料比3:1,球磨机内衬及磨球均采用纯钼材质,可有效避免杂质元素的引入,确保粉末纯度,因钼粉与铝粉比重相差过大极易造成混料不均匀,且铝粉球磨过程有***风险,铝粉球磨时延展性较好,易形成片状大颗粒导致粉体分层现象。由于铝能大量溶于α-Ti内,采用预先雾化造粒的钛铝合金粉体与钼粉及镍粉混合机械球磨处理,可有效避免粉体混合不均匀,同时球磨粉末的部分粉体颗粒被挤压成较大的扁长片状,部分粉末颗粒加工硬化冷焊层破碎变成较小的颗粒,球磨后粉末粒度分布变宽,粉体在球磨后原子处于高能状态,加速烧结过程中的原子扩散,有利于烧结密度的提高。
进一步的,所述步骤四中,旋锻处理的锻造力为18~22MN,锻造温度为1030~1100℃,保温时间2~4h。在旋锻处理前,还包括对合金管坯内衬TZM钢棒的步骤,TZM钢棒为钼合金棒材,具体过程为:在TZM钢棒钢棒内部通冷却水,旋锻时TZM钢棒与合金管坯相对反向旋转,相互垂直的四个锤砧,两两对击,控制锻造速度为190~250次/min。
进一步的,所述步骤五中,退火温度为980~1130℃,保温时间为2~4h,真空度不小于3*10-3pa;钼镍钛铝合金靶材的长度为1300~3000mm。
本发明的制备原理:本发明依次通过真空脱氧、灌粉振实、冷等静压成型、卧式真空烧结、旋锻、退火、外加工和绑定焊合的过程,制备得到大尺寸的钼镍钛铝合金靶材。其中,通过灌粉振实、冷等静压成型、卧式真空烧结、旋锻四个步骤的先后的协同作用可以实现大尺寸的制备,灌粉振实过程中采用震动平台大幅度激振,有利于形成较大松装密度,提高成型密度及均匀性;冷等静压成型过程中采用特定结构胶套模具可有效避免因装粉时粉体自重问题造成底部堆积严重,密度过大,压制后变形不均产生底部粗大现象;卧式真空烧结过程中可最大限度的去除粉体颗粒内部气体等杂质含量,降低氧含量,确保靶材产品较高纯度,真空烧结时用氧化铝填粉方式可确保在烧结过程中管坯正常收缩同时,避免径向变形过大发生椭圆弯曲现象,烧结后合金管变形均匀;旋锻过程中利用四锤头快速旋锻可使坯管在一个近似封闭的径向受压型腔内变形,具有良好的工艺塑性,可闭合及消除气孔等缺陷,并能使晶粒充分破碎细化,进一步提高管坯密度达99.5%以上。由锤砧入口角产生的轴向分力,有利于工件沿轴向延伸,进而使管坯锻造延长,延长率约5%~15%,可确保管坯笔直度及减少加工余量,大大降低生产成本,并为最后形成大尺寸奠定基础。
有益效果:与现有技术相比,本发明的显著优点为:(1)本发明配比下的合金靶材其溅射镀膜层拥有较好附着力,抗氧化性,耐湿性,低电阻率以及易蚀刻性;本发明的制备方法能够减少杂质元素的引入,所生产管靶成分均匀、无偏析、平均晶粒细小(≤50微米),氧含量较低,密度可达到理论值99%以上,完全满足目前大尺寸溅射靶材的镀膜要求。(2)采用采用卧式真空烧结方式可制备较大规格靶材产品,不受设备限制(例如用热压或热等静压方式烧结,设备限制较大,成品长度不超过2米),同时烧结成本也大幅度降低。(3)所述方法生产的管靶规格为1300~3000mm,完全满足高端液晶面板厂商的需求,具有明显的市场竞争力,进一步提高了的钼镍基多元合金旋转靶材的综合性能。
附图说明
图1为实施例1制备的钼镍钛铝多元合金旋转靶成品金相图;
图2为实施例1制备的2.4米钼镍钛铝多元合金旋转靶C-SCAN检测图;
图3为实施例2制备的钼镍钛铝多元合金旋转靶成品金相图;
图4为实施例2制备的3米钼镍钛铝多元合金旋转靶C-SCAN检测图;
图5为实施例3制备的钼镍钛铝合金靶材与铜背板焊合绑定制备镀膜层结构示意图。
具体实施方式
下面结合实施例对本发明的技术方案作进一步详细说明。
实施例1
制备Mo40Ni30Ti15Al15
S1、采用Mo粉粒度3~7um,氧含量≤1000ppm,纯度大于99.95%;Ni粉为电解镍粉,纯度大于99.9%,粒度6~12um,氧含量≤2000ppm;雾化造粒的Ti50Al50合金粉末,粒度35-60um,氧含量≤3000ppm。按上述的原子比混合,置于真空炉内1000℃,真空度不小于10-2pa进行真空脱氧提纯处理2h。
S2、将真空处理后粉体进行机械球磨混合,球料比3:1,转速为170R/M,氩气保护球磨混合12h,球磨机内衬及磨球均采用纯钼材质。
S3、将球磨粉末灌入管状模腔内,灌粉全程采用振动平台不间断的振实粉体,振幅3~6mm,激振力120KN,灌粉完成后用细管抽真空(不小于0.1pa)并密封上胶塞,然后用冷等静压机压力250MPa,保压300s,最终脱模压制成长度2500mm的空心管坯,制得相对密度68%的合金管坯。
S4、将长管坯放于卧式真空烧结炉内,采用球形氧化铝陶瓷颗粒(粒径2~5mm)将整管填埋,使内孔及四周均填埋好,烧结真空度不低于3*10-3pa,烧结参数为:首段按3℃/min的升温速率至930℃保温3h,第二段按2℃/min的升温速率至1200℃保温烧结4h,之后随炉降温,可获得长度2350mm,相对密度≥98%的钼镍钛铝合金管。
S5、采用奥地利GFM四锤头精锻机对烧结管坯进行旋锻处理,锻造力20MN,加热锻造温度1020℃,保温2h,空心管坯内孔衬有TZM钢棒,钢棒内部通有冷却水,旋锻时内芯钢棒与空心管坯相对反向旋转,相互垂直的四个锤砧,两两对击,锻造速度220次/min,最终锻造成长度为2510mm的钼镍钛铝合金管。
S6、将锻造管坯放入真空炉退火处理,退火温度为990℃,真空度不小于3*10-3pa,保温2h。
S7、通过镗孔机加工内外圆及端面,加工成长度2400mm的钼镍钛铝合金管,通过与钛背管绑定焊合,C-SCAN检测及经过超声波清洗及干燥,最终制备成为长度2400mm钼镍钛铝旋转靶材。
参见图1,为制备的钼镍钛铝多元合金旋转靶成品金相图,可看出,合金晶粒均匀,排列紧密,孔洞缺陷较少。经检测,本实施例制备靶材相对密度为99.3%,平均晶粒度≤50um,靶材纯度≥99.97%。参加图2,钼镍钛铝多元合金旋转靶内部无气孔裂纹等缺陷,绑定焊合率≥98%,完全达到了高端溅射靶材的要求。
实施例2
制备Mo52Ni25Ti15Al8
S1、采用Mo粉粒度3~7um,氧含量≤1000ppm,纯度大于99.95%;Ni粉为电解镍粉,纯度大于99.9%,粒度6~12um,氧含量≤2000ppm;雾化造粒的Ti70Al30合金粉末,粒度35-60um,氧含量≤3000ppm。按上述的原子比例混合,置于真空炉内1030℃,真空度不小于10- 2pa进行真空脱氧提纯处理5h。
S2、将真空处理后粉体进行机械球磨混合,球料比3:1,转速为180R/M,氩气保护球磨混合10h,球磨机内衬及磨球均采用纯钼材质。
S3、将球磨粉末灌入管状模腔内,灌粉全程采用振动平台不间断的振实粉体,振幅3~6mm,激振力110KN,灌粉完成后用细管抽真空(不小于0.1pa)并密封上胶塞,然后用冷等静压机压力300MPa,保压300s,最终脱模压制成长度3200mm的空心管坯,制得相对密度70%的合金管坯。
S4、将长管坯放于卧式真空烧结炉内,采用球形氧化铝陶瓷颗粒(粒径2~5mm)将整管填埋,使内孔及四周均填埋好,烧结真空度不低于3*10-3pa,烧结参数为:首段按4℃/min的升温速率至950℃保温3h,第二段按2℃/min的升温速率至1230℃保温烧结4h,之后随炉降温,可获得长度2920mm,相对密度≥98%的钼镍钛铝合金管。
S5、采用奥地利GFM四锤头精锻机对烧结管坯进行旋锻处理,锻造力18MN,加热锻造温度1050℃,保温2h,空心管坯内孔衬有TZM钢棒,钢棒内部通有冷却水,旋锻时内芯钢棒与空心管坯相对反向旋转,相互垂直的四个锤砧,两两对击,锻造速度240次/min,最终锻造成长度为3130mm的钼镍钛铝合金管。
S6、将锻造管坯放入真空炉退火处理,退火温度为1020℃,真空度不小于3*10-3pa,保温3h。
S7、通过镗孔机加工内外圆及端面,加工成长度3000mm的钼镍钛铝合金管,通过与钛背管绑定焊合,C-SCAN检测及经过超声波清洗及干燥,最终制备成为长度3000mm钼镍钛铝旋转靶材。
如图3所示,为制备的钼镍钛铝多元合金旋转靶成品金相图,可看出,合金晶粒均匀,排列紧密,孔洞缺陷较少。经检测,本实施例制备靶材相对密度为99.5%,平均晶粒度≤50um,靶材纯度≥99.98%。图示4为制备的3米钼镍钛铝多元合金旋转靶C-SCAN检测图,内部无气孔裂纹等缺陷,绑定焊合率≥98%,完全达到了高端溅射靶材的要求。
实施例3
制备镀膜样品,其中靶材为Mo45-Ni30-Ti15-Al10
S1、采用Mo粉粒度3~7um,氧含量≤1000ppm,纯度大于99.95%;Ni粉为电解镍粉,纯度大于99.9%,粒度6~12um,氧含量≤2000ppm;雾化造粒的Ti50AL50at%合金粉末,粒度35-60um,氧含量≤3000ppm。按原子比Mo45-Ni30-Ti15-Al10at%混合,置于真空炉内1000℃,真空度不小于10-2pa进行真空脱氧提纯处理1H。
S2、将真空处理后粉体进行机械球磨混合,球料比3:1,转速为170R/M,氩气保护球磨混合8h,球磨机内衬及磨球均采用纯钼材质。
S3、将球磨粉末灌入管状模腔内,灌粉全程采用振动平台不间断的振实粉体,振幅3~6mm,激振力130KN,灌粉完成后用细管抽真空(不小于0.1pa)并密封胶塞,然后用冷等静压机压力230MPa,保压300s,压制成高度50mm*直径180mm小圆坯锭。
S4、将小坯锭放于卧式真空烧结炉内,烧结真空度不低于3*10-3pa,烧结参数为:首段按4℃/min的升温速率至930℃保温2h,第二段按3℃/min的升温速率至1200℃保温烧结3h,之后随炉降温,制备成高度42mm*直径165mm的小钼镍钛铝合金锭。
S5、再经过旋锻处理,锻造力20MN,加热锻造温度1050℃,保温2h,然后进行退火处理,退火温度为1000℃,真空度不小于3*10-3pa,保温3h.
S6、通过机加工切片制成外径140mm*厚度8mm的钼镍钛铝合金靶材。
S7、最后与铜背板焊合绑定,C-SCAN检测及经过超声波清洗及干燥,最终制备成为Mo45-Ni30-Ti15-Al10合金靶材镀膜样品。
参见图1的镀膜层结构,其中膜层1为基材玻璃,膜层2为底部合金镀膜层,膜层3为主导电铜层,膜层4为顶部合金覆盖层,基材玻璃面积为100*100mm,镀膜层厚度分别为:膜层2=600A,膜层3=5000A,膜层4=600A。
对比例1
按照实施例3的方法,分别制备Mo35-Ni30-Ti15-Al20,Mo75-Ti25和Mo60-Ni20-Ti20镀膜样品靶,结构与图1相同。
然后与实施例3中的镀膜样品进行抗氧化性,附着力,电阻率,高温耐湿性及耐腐蚀性等检测对比,数据参见下表1和表2。
表1
表2
膜层抗氧化性检测:采用分光测试计测定膜层在大气中于室温,150℃、250℃、350℃加热1h后的反射率的变化,由表1可知,常规1#钼钛二元合金薄膜随着温度升高,其反射率大幅度降低,波动值最大,耐氧化性最差。通过添加一定配比镍及铝后反射率波动微小,尤其含有铝的膜层3#/和4#其抗氧化性比2#较佳,高温耐氧化非常稳定。
高温耐湿性检测则将上述4种薄膜在(温度85℃+湿度85%)环境下放置100小时,200小时后通过目视确认薄膜表面有无变色。由表2可知,4#当添加Al过多至20at%时,在高温高湿下铝过多会降低其耐腐蚀性能,随着时间的延长,表面发生气孔缺陷,耐湿性变差导致薄膜表面颜色变暗。3#铝含量10at%,膜层暴露在高温高湿环境中也无变色、具有高耐湿性。故优选的,铝原子添加量小于18at%较好。
电阻率采用薄膜电阻仪测定,随着钼及钛的含量降低以及镍的添加,其电阻率逐渐降低,当添加铝元素后3#及4#膜层的电阻率大大降低。附着力检测采用3M胶带撕剥法,评价有无薄膜残留。通过测试4种膜层材料均无剥落残留,说明都具有高附着力。蚀刻性检测:将样品浸渍于Cu蚀刻液内一定时间,然后用纯水清洗基板,再使之干燥,用光学显微镜观察基板上是否残留有金属薄膜。由于钛具有较强耐腐蚀性,1#含钛较高其蚀刻后发现基板上金属膜层无变化,无法蚀刻。相比较2#含钛20at%,虽能发生一定腐蚀反应,但基板上仍有少量膜层残渣,说明蚀刻不充分。发现通过减少钛含量,添加一定量易腐蚀的铝元素后,3#和4#样品基板上无膜层残留,蚀刻效果较理想。
综上检测对比,3#样品Mo45-Ni30-Ti15-Al10综合性能最佳。由于钛有含量过高蚀刻后有残留,优选的钛含量<20at%。铝元素具有良好的抗氧化性及蚀刻性能,铝含量过多会造成腐蚀过快,高温耐湿性较低缺陷,优选的铝含量控制在18at%之内。故提出较优选的合金膜层材料:Mo100-x-y-zNixTiyAlz(10≤X≤40,1≤Y≤20,1≤Z≤18),以上优选配比合金靶材其溅射镀膜层拥有较好附着力,抗氧化性,耐湿性,低电阻率以及易蚀刻性。

Claims (10)

1.一种钼镍基多元合金旋转靶材,其特征在于,所述旋转靶材原子组成是Mo100-x-y- zNixTiyAlz,且X、Y、Z表示原子组成百分比,10≤X≤40,1≤Y≤20,1≤Z≤18。
2.根据权利要求1所述的钼镍基多元合金旋转靶材,其特征在于:Mo由钼粉提供,钼粉粒度为3~7 μm,氧含量≤1000ppm,纯度大于99.95%;Ni由电解镍粉提供,电解镍粉粒度为6~12 μm,氧含量≤2000ppm,纯度大于99.9%;Ti和Al由钛铝预合金粉末提供,钛铝预合金粉末的粒度为35~60 μm,氧含量≤3000ppm。
3.权利要求1-2任一项所述的钼镍基多元合金旋转靶材的制备方法,其特征在于,包括以下步骤:
步骤一、将钼粉、电解镍粉和钛铝预合金粉末按比例混合,然后置于真空炉内进行脱氧提纯处理,然后将脱氧提纯处理的粉体进行球磨混合;
步骤二、将球磨后的粉体灌入管状模腔内,灌粉全程采用振动平台振实粉体,灌粉完成后抽真空并密封,然后进行冷等静压成型,最终脱模压制成相对密度为68~70%的合金管坯;
步骤三、将脱模后的合金管坯放于真空烧结炉内进行卧式烧结,得到相对密度大于98%的合金管坯;
步骤四、将烧结后的合金管坯进行旋锻处理;
步骤五、将锻造后的管坯放入真空炉进行去应力退火处理,得到钼镍钛铝合金管锭,最后通过机加工切片制成钼镍钛铝合金靶材。
4.根据权利要求3所述的钼镍基多元合金旋转靶材的制备方法,其特征在于:所述步骤三中,卧式烧结的参数为:首段按4~6℃/min的升温速率至930~950℃保温2~5h,第二段按2~4℃/min的升温速率至1150~1280℃保温烧结3~7h,之后随炉降温。
5.根据权利要求4所述的钼镍基多元合金旋转靶材的制备方法,其特征在于:在卧式烧结放置合金管坯时,采用球形氧化铝陶瓷颗粒将整管填埋,控制氧化铝陶瓷颗粒的粒径2~5mm。
6.根据权利要求3所述的钼镍基多元合金旋转靶材的制备方法,其特征在于:所述步骤二中,冷等静压成型的压力为230~330MPa,保压时间为240~500s;振实粉体时振动平台的振幅为3~6mm,激振力为110~130 KN。
7.根据权利要求3所述的钼镍基多元合金旋转靶材的制备方法,其特征在于:所述步骤一中,真空炉内的处理温度为950~1100℃,脱氧提纯处理的时间为2~5 h;球磨的转速为120~210 R/M,球磨时间为8~12 h。
8.根据权利要求3所述的钼镍基多元合金旋转靶材的制备方法,其特征在于:所述步骤四中,旋锻处理的锻造力为18~22 MN,锻造温度为1030~1100℃,保温时间2~4 h。
9.根据权利要求8所述的镍基多元合金旋转靶材的制备方法,其特征在于:在旋锻处理前,还包括对合金管坯内衬TZM钢棒的步骤,具体为:在TZM钢棒内部通冷却水,旋锻时TZM钢棒与合金管坯相对反向旋转,控制锻造速度为190~250次/min。
10.根据权利要求3所述的钼镍基多元合金旋转靶材的制备方法,其特征在于:所述步骤五中,退火温度为980~1130℃,保温时间为2~4 h;钼镍钛铝合金靶材的长度为1300~3000mm。
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