CN111215623A - 一种Ti-Al系合金的粉末冶金致密化无压烧结方法 - Google Patents
一种Ti-Al系合金的粉末冶金致密化无压烧结方法 Download PDFInfo
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- CN111215623A CN111215623A CN202010134399.8A CN202010134399A CN111215623A CN 111215623 A CN111215623 A CN 111215623A CN 202010134399 A CN202010134399 A CN 202010134399A CN 111215623 A CN111215623 A CN 111215623A
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- 229910021330 Ti3Al Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound 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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making alloys
- C22C1/04—Making alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium, hafnium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
Abstract
本发明属于合金技术领域,具体涉及一种Ti‑Al系合金的粉末冶金致密化无压烧结方法。本发明提供了一种Ti‑Al系合金的粉末冶金致密化无压烧结方法,本发明采用程序升温的方式进行无压烧结,通过在烧结的不同升温阶段采用不同的保护气氛和气体流速,能够得到致密度较高的Ti‑Al系合金。实施例结果表明,本发明制备的Ti‑Al系合金致密度高达98%以上;准静态压缩强度达到1100MPa以上,临界破坏应变超过0.4。另外,本发明提供的粉末冶金无压烧结方法生产成本低,可以实现Ti‑Al系合金异形件的批量化生产。
Description
技术领域
本发明属于合金技术领域,具体涉及一种Ti-Al系合金的粉末冶金致密化无压烧结方法。
背景技术
Ti-Al系合金具有比强度高、高温强度高、高温塑性好以及抗蠕变性能优异等特点,是在600~800℃条件下服役的非常有潜力的轻质结构材料,可用于航空、航天发动机零部件的制造生产。
目前,Ti-Al系合金零部件的制备方法主要包括:熔炼铸造和粉末冶金,熔炼铸造具体包括铸锭冶金和精密铸造两种方式,其中铸锭冶金是先熔炼得到Ti-Al系合金铸锭,然后对铸锭进行热加工和热处理,最后通过机加工的方式从铸锭中掏取零部件;精密铸造是先制备出接近零部件形状的型模,将熔炼好的Ti-Al系合金液体浇铸到型模内,对得到的零件毛坯进行热处理,最后机加工得到。其中,铸锭冶金配合车削掏取的方法虽然可以获得组织致密均匀的零部件,但锻造工艺成本较高,且车削掏取会造成严重的材料浪费,因此,不适用于Ti-Al系合金零部件的大批量工业化生产;而精密铸造虽然避免了材料大量浪费的问题,但由于Ti-Al系合金熔融液体在异形铸模中流动性不足,制得的零部件质量均一性不够理想,成品率不高,目前规模化生产也面临较大困难。
粉末冶金法是以金属粉末作为原料,经过成型和烧结工艺,制造金属材料零部件的技术。根据成型烧结工艺的不同,粉末冶金法主要包括放电等离子烧结和热等静压烧结,两者都是在一定压力下烧结,可以制备出高致密度的Ti-Al系合金。但是,放电等离子烧结只能生产特定形状的小块材料,难以制备复杂形状的大体积零部件;热等静压烧结需要制备特定形状的包套,生产成本较高。冷等静压+无压烧结技术可以实现各种尺寸的异形件的批量化生产,但现有冷等静压+无压烧结技术制备出的Ti-Al系合金,材料致密度低,约为90~94%,无法满足产品的使用要求。
发明内容
本发明的目的在于提供一种Ti-Al系合金的粉末冶金致密化无压烧结方法,本发明提供的无压烧结方法能够克服Ti-Al系合金产品生产工艺复杂,成本高的缺陷,实现Ti-Al系合金的高致密度、低成本批量化生产,以满足先进航空发动机零部件对轻质Ti-Al系合金材料的需求。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种Ti-Al系合金的粉末冶金致密化无压烧结方法,包括以下步骤:
(1)将Ti-Al系合金原料混合,进行冷等静压成型,得到压坯;
(2)将所述压坯进行无压烧结,得到Ti-Al系合金;所述无压烧结的程序包括以下步骤:
以100~400mL/min的速率通入流动氢气,在氢气气氛中,将所述压坯从室温第一升温至500~600℃;
停止通入流动氢气,对炉膛内进行抽真空;
密封炉膛,在500~600℃保温1~2h;
保持炉膛密封状态,将所述保温后的压坯第二升温至750~850℃;
以500~2000mL/min的速率通入流动氩气,在所述氩气气氛中,将所述第二升温后的压坯第三升温至烧结温度;所述烧结温度为1400~1600℃;
调整流动氩气的流速为100~400mL/min,在所述氩气气氛中,将所述升温程序后的压坯在所述烧结温度保温2~5h后降温,得到高致密度Ti-Al系合金。
优选地,所述第一升温的升温速率为2~5℃/min。
优选地,所述第一升温结束后,停止通入流动氢气,对炉膛内抽真空,所述真空度优选至真空度为1×10-3~5×10-2Pa。
优选地,所述第二升温的升温速率为5~8℃/min。
优选地,所述第三升温的升温速率为1~3℃/min。
优选地,所述降温的速率为1~5℃/min。
优选地,按质量百分比计,所述Ti-Al系合金原料包括Ti粉30~60%、TiH2粉10~20%、Al粉10~30%、Nb粉10~50%和X粉0~10%;其中X粉为Mo粉、W粉、Ta粉和V粉中的一种或多种;所述Ti-Al系合金原料的质量百分比之和为100%。
优选地,所述Ti-Al系合金原料的粒径独立地为5~50μm。
优选地,所述冷等静压成型的温度为5~30℃,压力为200~400MPa,保压时间为10~60min。
本发明提供了一种Ti-Al系合金的粉末冶金致密化无压烧结方法,本发明采用程序升温的方式进行无压烧结,通过在烧结的不同升温阶段采用不同的保护气氛和气体流速,能够得到致密度较高的Ti-Al系合金。本发明在较低温度升温过程中通入流动氢气,使得炉膛内氢气分压较高,因此氢气能扩散进Ti-Al系合金压坯,与压坯内的氧气反应,从而防止Ti-Al系合金原料的氧化;本发明在抽真空后密封炉膛,使得炉膛内氢气分压降低,固溶于Ti-Al系合金压坯内的氢气将从压坯内逸出,另外,在500~750℃时TiH2剧烈分解,活性氢原子将促进合金元素的扩散,同时释放出氢气,与压坯内释放出的固溶的氢气共同构成炉膛内微弱的氢气气氛,防止合金氧化;本发明在500~600℃保温1~2h,一方面能够使TiH2充分分解,另一方面使Ti和固态Al先反应生成TiAl3,避免Al熔融,从而减少材料孔隙;本发明在升温至750~850℃过程中,保持炉膛密封状态不动,未反应的Ti继续与TiAl3发生化学反应,生成Ti3Al,此时炉膛内存在微弱的氢气气氛,避免合金氧化;在升温至1400~1600℃过程中需要通入较大流速的氩气带走炉膛内的氢气,降低炉膛内的氢气分压,使合金中残余的固溶氢气逸出,防止氢脆发生;在1400~1600℃的保温烧结阶段,合金中的固溶氢气已排净,减小氩气流速可以避免高温烧结时温度波动对合金的影响,降温后完成致密化无压烧结过程。实施例结果表明,本发明制备的Ti-Al系合金致密度高达98%以上;准静态压缩强度达到1100MPa以上,临界破坏应变超过0.4。另外,本发明提供的粉末冶金无压烧结方法生产成本低,可以实现Ti-Al系合金异形件的批量化生产。
附图说明
图1为本发明无压烧结程序的示意图;
图2为本发明实施例1制备的Ti-Al系合金的光镜图;
图3为本发明实施例1制备的Ti-Al系合金的准静态压缩真应力-应变曲线。
具体实施方式
本发明提供了一种Ti-Al系合金的粉末冶金致密化无压烧结方法,包括以下步骤:
(1)将Ti-Al系合金原料混合,进行冷等静压成型,得到压坯;
(2)将所述压坯进行无压烧结,得到Ti-Al系合金;所述无压烧结的程序包括以下步骤:
以100~400mL/min的速率通入流动氢气,在氢气气氛中,将所述压坯从室温第一升温至500~600℃;
停止通入流动氢气,对炉膛内进行抽真空;
密封炉膛,在500~600℃保温1~2h;
保持炉膛密封状态,将所述保温后的压坯第二升温至750~850℃;
以500~2000mL/min的速率通入流动氩气,在所述氩气气氛中,将所述第二升温后的压坯第三升温至烧结温度;所述烧结温度为1400~1600℃;
调整流动氩气的流速为100~400mL/min,在所述氩气气氛中,将所述升温程序后的压坯在所述烧结温度保温2~5h后降温,得到高致密度Ti-Al系合金。
本发明将Ti-Al系合金原料混合,进行冷等静压成型,得到压坯。在本发明中,所述Ti-Al系合金原料的粒径独立地优选为5~50μm。在本发明中,所述Ti-Al系合金原料的具体组成根据Ti-Al系合金的成分进行确定。
在本发明中,按质量百分比计,所述Ti-Al系合金原料优选包括钛粉30~60%。在本发明中,所述钛粉的纯度优选为99.5%,所述钛粉的粒径优选为5~50μm。
在本发明中,按质量百分比计,所述Ti-Al系合金原料优选包括TiH2粉10~20%。在本发明中,所述TiH2粉的粒径优选为5~50μm。所述TiH2粉在无压烧结过程中会分解,促进合金中原子之间的扩散,可以有效提高烧结材料的致密度。
在本发明中,按质量百分比计,所述Ti-Al系合金原料优选包括铝粉10~30%。在本发明中,所述铝粉的纯度优选为99.5%,所述铝粉的粒径优选为5~50μm。
在本发明中,按质量百分比计,所述Ti-Al系合金原料优选包括Nb粉10~50%。在本发明中,所述Nb粉的纯度优选为99.9%,所述Nb粉的粒径优选为5~50μm。
在本发明中,按质量百分比计,所述Ti-Al系合金原料优选包括X粉0~10%。在本发明中,所述X粉优选为Mo粉、W粉、Ta粉和V粉中的一种或多种。在本发明中,所述X粉的粒径优选为5~50μm。
在本发明中,所述Ti-Al系合金原料的质量百分比之和为100%。
本发明对所述Ti-Al系合金原料的混合方式没有特殊的限定,采用本领域技术人员所熟知的混合方式即可,以各原料粉末混合均匀为宜。
在本发明中,所述冷等静压成型的温度优选为5~30℃,更优选为10~25℃;所述冷等静压成型的压力优选为200~400MPa;所述冷等静压成型的保压时间优选为10~60min。在本发明中,采用冷等静压成型能够制备得到具有一定强度、和Ti-Al系合金产品形状尺寸接近的压坯。
得到压坯后,本发明将所述压坯进行无压烧结,得到Ti-Al系合金。在本发明中,所述无压烧结程序的示意图如图1所示。在本发明中,所述无压烧结优选在箱式电阻炉或管式炉中进行。
本发明以100~400mL/min的速率通入流动氢气,在氢气气氛中,将所述压坯从室温第一升温至500~600℃,所述第一升温过程如图1中的(I)所示。在本发明中,所述第一升温的升温速率优选为2~5℃/min。在本发明中,所述第一升温过程中的压力优选为50~90kPa。本发明在进行所述第一升温前,优选先将体系进行抽真空至1×10-2~5×10-3Pa,然后充入氩气;重复抽真空和充入氩气步骤2~3次,最后抽真空,通入流动氢气。本发明在充入氢气前先充入氩气的作用是清洗炉膛,排净其中的空气。本发明在第一升温过程中通入流动氢气,使得炉膛内氢气分压较高,因此氢气能扩散进Ti-Al系合金压坯,与压坯内的氧气反应,从而防止Ti-Al系合金原料的氧化。
完成所述第一升温后,本发明停止通入流动氢气,对炉膛内进行抽真空,然后密封炉膛,在500~600℃保温1~2h,所述保温过程如图1中的(II)所示。在本发明中,所述抽真空优选至真空度为1×10-3~5×10-2Pa。本发明在抽真空后密封炉膛,使得炉膛内氢气分压降低,过量固溶于Ti-Al系合金压坯内的氢气将从压坯内逸出,另外,在500~750℃时TiH2剧烈分解,活性氢原子将促进合金元素的扩散,同时释放出氢气,与压坯内释放出的过量固溶的氢气共同构成炉膛内微弱的氢气气氛,防止合金氧化;本发明在500~600℃保温1~2h,一方面能够使TiH2充分分解,另一方面使Ti和固态Al先反应生成TiAl3,避免Al熔融,从而减少材料孔隙,提高致密度。本发明在所述保温过程中,发生如下反应:Ti+3Al(s)→TiAl3/Ti+3Al(l)→TiAl3,TiAl3+Ti→Ti3Al。
图1中的(II)所示保温后,本发明保持炉膛密封状态,将所述保温后的压坯第二升温至750~850℃,所述第二升温过程如图1中的(III)所示,在本发明中,所述第二升温的升温速率优选为5~8℃/min。在第二升温过程中,未反应的Ti继续与TiAl3发生化学反应,生成Ti3Al,避免合金氧化;此反应速率快,因此可以选择较高的升温速率,提高烧结效率。
完成所述第二升温后,本发明以500~2000mL/min的速率通入流动氩气,在所述氩气气氛中,将所述第二升温后的压坯第三升温至烧结温度;所述烧结温度为1400~1600℃,所述第三升温过程如图1中的(IV)所示。在本发明中,所述第三升温的升温速率优选为1~3℃/min;在本发明中,所述氩气的流速优选为400~500mL/min。在第三升温过程中,Nb向Ti3Al中固溶,生成Ti2AlNb,此反应速率慢,需要缓慢升温,使反应充分进行,以得到目标组织状态的合金;本发明在所述第三升温过程中,需要通入较大流速的氩气带走炉膛内的氢气,降低炉膛内的氢气分压,使合金中残余的固溶氢气逸出,防止氢脆发生。
所述第三升温完成后,本发明调整流动氩气的流速为100~400mL/min,在1400~1600℃条件下保温烧结2~5h,所述保温过程如图1中的(V)所示。所述保温时间根据在1400~1600℃烧结温度下Ti、Al、Nb及X元素之间互扩散系数D的最小值确定,以Ti-Al-Nb合金为例,根据文献可知,Ti、Al、Nb三种元素粉末之间互扩散速率最慢的是Ti和Nb,根据原料粉末的粒径RNb和RTi,代入式I:
计算烧结保温时间t;其中D通过文献查阅得到。
在本发明中,所述氩气的流速为100~200mL/min。在图1中(V)所示的保温阶段,氢气已排净,减小氩气流速可以避免高温烧结时温度波动对合金的影响。
图1中的(V)所示保温完成后,本发明将保温所得压坯进行降温,保持流动氩气的流速为100~400mL/min不变,所述降温过程如图1中的(VI)所示。本发明优选降温至室温。在本发明中,所述降温的速率优选为1~5℃/min。
采用本发明提供的无压烧结方法制备得到的Ti-Al系合金,致密度为98%以上。在本发明中,按重量百分比计,所述Ti-Al系合金的化学成分优选包括Ti 40~80%;优选包括Al 10~30%;优选包括Nb 10~50%;优选包括X 0~10%,其中X为Mo、W、Ta和V中的一种或多种。
下面将结合本发明中的实施例,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他实施例,都属于本发明保护的范围。
实施例1
按质量百分比,称取Ti粉45%,TiH2粉18%、Al粉17%、Nb粉20%,其中Ti粉粒径40μm、TiH2粉粒径40μm、Al粉粒径20μm、Nb粉粒径30μm;将上述粉末混合均匀,进行冷等静压成型,得到压坯;其中,冷等静压成型的参数为:温度20℃,压力200MPa,保压时间30min;
将所述压坯放入密封的管式炉中,进行无压烧结,所述无压烧结的烧结程序为:
(1)抽真空,至真空度为1×10-2~5×10-3Pa,充入氩气;
(2)重复步骤(1)2~3次;
(3)抽真空,以230mL/min的速率通入流动H2,保持炉膛内压力为50~90kPa;以3℃/min的升温速率从室温加热至550℃;
(4)停止通入流动氢气,对炉膛内进行抽真空,至真空度1×10-3~5×10-2Pa,密封炉膛;在550℃保温1.5h;
(5)保持炉膛密封状态,以7℃/min的升温速率加热至800℃;
(6)通流动氩气,流速600mL/min,以2℃/min的升温速率加热至1500℃;
(7)调整氩气流速为150mL/min,在1500℃保温烧结3h;
(8)以2℃/min的降温速率冷却至室温,得到Ti-Al系合金,合金组成为Ti-17Al-20Nb(wt.%)。
所得Ti-Al系合金的光镜图如图2所示,本发明制备的Ti-Al系合金的致密度较高,为98.6%;
所得Ti-Al系合金的准静态压缩真应力-应变曲线如图3所示,由图3可以看出,本发明制备的Ti-Al系合金的准静态压缩强度为1400MPa,临界破坏应变为0.5,具有较高的强度,能够满足航天航空技术领域的要求。
实施例2
按质量百分比,称取Ti粉40%,TiH2粉13%、Al粉17%、Nb粉20%、Mo粉5%,其中Ti粉粒径35μm、TiH2粉粒径35μm、Al粉粒径10μm、Nb粉粒径15μm、Mo粉粒径10μm;将上述粉末混合均匀,进行冷等静压成型,得到压坯;其中,冷等静压成型的参数为:温度25℃,压力300MPa,保压时间20min;
将所述压坯放入密封的管式炉中,进行无压烧结,所述无压烧结的烧结程序为:
(1)抽真空,至真空度为1×10-2~5×10-3Pa,充入氩气;
(2)重复步骤(1)2~3次;
(3)抽真空,以150mL/min的速率通入流动H2,保持炉膛内压力为50~90kPa;以4℃/min的升温速率从室温加热至500℃;
(4)停止通入流动氢气,对炉膛内进行抽真空,密封炉膛;在500℃保温2h;
(5)保持炉膛密封状态,以6℃/min的升温速率加热至820℃;
(6)通流动氩气,流速850mL/min,以1.5℃/min的升温速率加热至1450℃;
(7)调整氩气流速为130mL/min,在1450℃保温烧结3.5h;
(8)以3℃/min的降温速率冷却至室温,得到Ti-Al系合金,合金组成为Ti-17Al-20Nb-5Mo(wt.%)。
所得Ti-Al系合金的致密度为98.3%,准静态压缩强度为1300MPa,临界破坏应变为0.48。
实施例3
按质量百分比,称取Ti粉40%,TiH2粉15%、Al粉10%、Nb粉25%、W粉6%,其中Ti粉粒径35μm、TiH2粉粒径35μm、Al粉粒径10μm、Nb粉粒径15μm、W粉粒径8μm;将上述粉末混合均匀,进行冷等静压成型,得到压坯;其中,冷等静压成型的参数为:温度10℃,压力400MPa,保压时间10min;
将所述压坯放入密封的箱式炉中,进行无压烧结,所述无压烧结的烧结程序为:
(1)抽真空,至真空度为1×10-2~5×10-3Pa,充入氩气;
(2)重复步骤(1)2~3次;
(3)抽真空,以270mL/min的速率通入流动H2,保持炉膛内压力为50~90kPa;以5℃/min的升温速率从室温加热至600℃;
(4)停止通入流动氢气,对炉膛内进行抽真空,至真空度1×10-3~5×10-2Pa,密封炉膛;在600℃保温1h;
(5)保持炉膛密封状态,以5℃/min的升温速率加热至850℃;
(6)通流动氩气,流速1100mL/min,以2.5℃/min的升温速率加热至1600℃;
(7)调整氩气流速为160mL/min,在1550℃保温烧结4h;
(8)以3.5℃/min的降温速率冷却至室温,得到Ti-Al系合金,合金组成为Ti-10Al-25Nb-6W(wt.%)。
所得Ti-Al系合金的致密度为98.5%,准静态压缩强度为1360MPa,临界破坏应变为0.51。
实施例4
按质量百分比,称取Ti粉40%,TiH2粉15%、Al粉18%、Nb粉21%、V粉6%,其中Ti粉粒径40μm、TiH2粉粒径40μm、Al粉粒径5μm、Nb粉粒径20μm、V粉粒径15μm;将上述粉末混合均匀,进行冷等静压成型,得到压坯;其中,冷等静压成型的参数为:温度25℃,压力350MPa,保压时间15min;
将所述压坯放入密封的箱式炉中,进行无压烧结,所述无压烧结的烧结程序为:
(1)抽真空,至真空度为1×10-2~5×10-3Pa,充入氩气;
(2)重复步骤(1)2~3次;
(3)抽真空,以160mL/min的速率通入流动H2,保持炉膛内压力为50~90kPa;以4℃/min的升温速率从室温加热至500℃;
(4)停止通入流动氢气,对炉膛内进行抽真空,至真空度1×10-3~5×10-2Pa,密封炉膛;在500℃保温2h;
(5)保持炉膛密封状态,以6℃/min的升温速率加热至830℃;
(6)通流动氩气,流速800mL/min,以1.5℃/min的升温速率加热至1450℃;
(7)调整氩气流速为130mL/min,在1450℃保温烧结4h;
(8)以3℃/min的降温速率冷却至室温,得到Ti-Al系合金,合金组成为Ti-18Al-21Nb-6V(wt.%)。
所得Ti-Al系合金的致密度为98.6%,准静态压缩强度为1300MPa,临界破坏应变为0.48。
实施例5
按质量百分比,称取Ti粉40%,TiH2粉15%、Al粉17%、Nb粉20%、Ta粉8%,其中Ti粉粒径35μm、TiH2粉粒径35μm、Al粉粒径10μm、Nb粉粒径15μm、Ta粉粒径10μm;将上述粉末混合均匀,进行冷等静压成型,得到压坯;其中,冷等静压成型的参数为:温度25℃,压力380MPa,保压时间20min;
将所述压坯放入密封的箱式炉中,进行无压烧结,所述无压烧结的烧结程序为:
(1)抽真空,至真空度为1×10-2~5×10-3Pa,充入氩气;
(2)重复步骤(1)2~3次;
(3)抽真空,以170mL/min的速率通入流动H2,保持炉膛内压力为50~90kPa;以4℃/min的升温速率从室温加热至500℃;
(4)停止通入流动氢气,对炉膛内进行抽真空,至真空度1×10-3~5×10-2Pa,密封炉膛;在500℃保温2h;
(5)保持炉膛密封状态,以6℃/min的升温速率加热至800℃;
(6)通流动氩气,流速750mL/min,以2℃/min的升温速率加热至1600℃;
(7)调整氩气流速为150mL/min,在1550℃保温烧结2h;
(8)以3℃/min的降温速率冷却至室温,得到Ti-Al系合金,合金组成为Ti-17Al-20Nb-8Ta(wt.%)。
所得Ti-Al系合金的致密度为98.2%,准静态压缩强度为1330MPa,临界破坏应变为0.45。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (9)
1.一种Ti-Al系合金的粉末冶金致密化无压烧结方法,其特征在于,包括以下步骤:
(1)将Ti-Al系合金原料混合,进行冷等静压成型,得到压坯;
(2)将所述压坯进行无压烧结,得到Ti-Al系合金;所述无压烧结的程序包括以下步骤:
以100~400mL/min的速率通入流动氢气,在氢气气氛中,将所述压坯从室温第一升温至500~600℃;
停止通入流动氢气,对炉膛内进行抽真空;
密封炉膛,在500~600℃保温1~2h;
保持炉膛密封状态,将所述保温后的压坯第二升温至750~850℃;
以500~2000mL/min的速率通入流动氩气,在所述氩气气氛中,将所述第二升温后的压坯第三升温至烧结温度;所述烧结温度为1400~1600℃;
调整流动氩气的流速为100~400mL/min,在所述氩气气氛中,将所述升温程序后的压坯在所述烧结温度保温2~5h后降温,得到高致密度Ti-Al系合金。
2.根据权利要求1所述的无压烧结方法,其特征在于,所述第一升温的升温速率为2~5℃/min。
3.根据权利要求1所述的无压烧结方法,其特征在于,所述第一升温结束后,停止通入流动氢气,对炉膛内抽真空,所述真空度优选至真空度为1×10-3~5×10-2Pa。
4.根据权利要求1所述的无压烧结方法,其特征在于,所述第二升温的升温速率为5~8℃/min。
5.根据权利要求1所述的无压烧结方法,其特征在于,所述第三升温的升温速率为1~3℃/min。
6.根据权利要求1所述的无压烧结方法,其特征在于,所述降温的速率为1~5℃/min。
7.根据权利要求1所述的无压烧结方法,其特征在于,按质量百分比计,所述Ti-Al系合金原料包括Ti粉30~60%、TiH2粉10~20%、Al粉10~30%、Nb粉10~50%和X粉0~10%;其中X粉为Mo粉、W粉、Ta粉和V粉中的一种或多种;所述Ti-Al系合金原料的质量百分比之和为100%。
8.根据权利要求7所述的无压烧结方法,其特征在于,所述Ti-Al系合金原料的粒径独立地为5~50μm。
9.根据权利要求1所述的无压烧结方法,其特征在于,所述冷等静压成型的温度为5~30℃,压力为200~400MPa,保压时间为10~60min。
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