CN116571748A - 一种钛合金制件的粉末热等静压近净成形方法 - Google Patents
一种钛合金制件的粉末热等静压近净成形方法 Download PDFInfo
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Abstract
本发明公开了一种钛合金制件的粉末热等静压近净成形方法,属于钛合金粉末冶金技术领域。该方法包括:(1)采用A3钢制作包套模具,模具内腔经注粉和抽真空后,经氩弧焊形成密闭结构;(2)采用无坩锅感应熔炼超声气体雾化法制备钛合金粉末;(3)采用振动法向包套模具内注入钛合金粉末,并达到钛合金粉末振实密度,真空除气后封焊;(4)热等静压后经机械加工及化学铣,得到目标钛合金制件。本发明得到的钛合金制件,具有均匀细小的微观组织,良好的综合性能,可用于制造高性能、形状复杂的零部件。
Description
技术领域
本发明涉及钛合金及粉末冶金技术领域,具体涉及一种钛合金制件的粉末热等静压近净成形方法。
背景技术
粉末冶金是一种制取金属粉末以及采用成形、烧结和热致密化工件将金属粉末(或金属粉末与非金属粉末)制成材料和制品的工艺技术。它具有悠久的历史,作为粉末冶金雏形的块炼铁技术,在远古时期便是人类制取铁器的唯一手段。粉末冶金成形技术一直处于不断发展演化过程中,特别是近十几年来粉末冶金取得了引人注目的进展,一系列新技术、新工艺相继出现,从传统的单向压制到双向压制,再到热等静压成形,成为材料制备和加工的重要方法之一,现代粉末冶金成形技术正朝着高致密化、高性能化、高生产效率、低成本方向进展。
热等静压粉末冶金技术继承了粉末冶金和热等静压技术的优点,同时借鉴了铸造复杂零件的模壳与型芯组合模具成形技术,因此国外研究者又将该技术称作“粉末铸造技术”,可视为精密铸造的升级版。与传统成形方法相比,热等静压粉末冶金技术具有良好的综合性能,可用来制造性能高、形状复杂的零部件,用以满足航空航天等重要领域的发展需求。国际上,俄罗斯和美国在热等静压粉末冶金技术方面已经非常成熟,并且应用此技术制备了大量复杂高性能零部件应用于航空航天领域。
发明内容
本发明的目的在于提供一种钛合金制件的粉末热等静压近净成形方法,该方法将特定结构、材质的模具与热等静压等工艺相结合,使模具与模具内的钛合金粉末协同变形,从而使获得的钛合金制件具有均匀细小的微观组织,良好的综合性能。
为了实现上述目的,本发明所采用的技术方案如下:
一种钛合金制件的粉末热等静压近净成形方法,该方法是采用金属包套模具进行,具体包括如下步骤:
(1)包套模具的制备:包套模具采用金属制作(A3钢),模具内腔与目标零件形状相似,模具内腔经注粉和抽真空后,经氩弧焊形成密闭结构;
(2)钛合金粉末的制备:采用无坩锅感应熔炼超声气体雾化法(Electrodeinduction melting gas atomization,EIGA)制备钛合金粉末,要求钛合金粉末粒度范围为250μm以下,球形度大于90%,松装密度为理论密度的50~55%;
(3)封装:采用振动法向包套模具内注入钛合金粉末,并达到钛合金粉末振实密度,真空除气后封焊;振实密度为理论密度63~70%;
(4)热等静压:将封装后的包套模具放入热等静压炉中,升温升压至设定温度和压力,保温保压至设定时间;
(5)后处理:经机械加工和/或硝酸浸泡去除模具后,得到目标钛合金制件。
上述步骤(1)中,所述包套模具包括上包套、下包套和真空管;其中:所述下包套为上部开口的圆筒状结构,上包套上设有注粉口,且上包套的底面结构与下包套的顶部能够相配合组装在一起形成空腔;经由注粉口向空腔内注粉后,将真空管焊接于注粉口上方,对空腔抽真空后,将真空管顶部封焊。
上述步骤(1)中,所述包套模具的装配过程为:将包套模具各组成部分依次在石油醚、优级纯酒精中清洗,去除表面灰尘及油污,并对清洗后的包套模具进行干燥处理;采用自动焊机将上包套、下包套和真空管焊接,并检查焊缝质量,并利用氦气质谱检漏仪进行气密闭测试,需达到密封要求。
上述步骤(2)中,钛合金粉末的制备过程为:首先采用预合金法预制钛合金棒料;然后采用无坩锅感应熔炼超声气体雾化法制取洁净预合金粉末,过60目筛取60目筛下的粉末,真空储存,备用;制粉过程中采用高纯氩气;
上述步骤(3)封装过程为:将钛合金粉末填充到密闭模具中,采用振动法增加粉末的流动性,并使粉末达到振实密度;然后将真空管下端焊接到模具注粉口上,并将真空管顶端与外部抽真空装置相连接;在室温条件下将密闭模具抽真空至5.0×10-2Pa以上;再将密闭模具放入马弗炉中加热(温度范围200-400℃),持续4-8h(加热过程中持续抽真空并保持模具内真空度为5.0×10-2Pa以上);加热完成后将模具真空管顶部进行封焊,在真空管外焊接保护套。
上述步骤(4)热等静压过程中,设定温度为800-1000℃,设定压力为80-150MPa,设定时间为2-6h;热等静压中使用高纯氩气作为加压介质,且采用先加压后升温的方式进行热等静压。
上述步骤(4)热等静压处理过程中,包套模具与钛合金粉末协同变形。
上述步骤(5)中,所述化学铣选用硝酸(浓度为1~2mol/L)为腐蚀基液,化学铣通过石墨板与目标件(装有钛合金制件的包套模具)短接构成原电池对模具进行腐蚀。
经步骤(5)化学铣处理后,依次进行清洗喷砂和热处理调质。
采用本发明方法成形的钛合金制件具有均匀细小的微观组织,良好的综合性能。
本发明设计机理如下:
本发明设计的包套材料满足以下要求:(1)不与粉末发生化学反应;(2)焊接性能良好;(3)具有良好的加工性;(4)材质为无孔隙或者其他缺陷的锻料;(5)成本低廉,并且去除容易;(6)强度与粉末压坯相匹配,综合考虑包套材质选用A3钢。
全粒度粉末的振实密度为68%左右,因而粉末体在热等静压过程中的体积收缩超过30%。如此大的收缩量会给包套设计带来很大考验,包套不仅需要顺利容纳粉末热等静压致密化导致的体积收缩,还要确保收缩均匀,特别是保证局部发生大变形的部位不会发生撕裂引起热等静压失败。
本发明通过包套材质及成型过程中工艺设计及相应参数控制协同作用,实现了包套应与粉末体在高温高压下发生协调变形,促使粉末体完成致密化过程,同时保证成形件关键尺寸的精确控制,从而实现了粉末构件的近净成形。
本发明的优点和有益效果如下:
1、本发明利用优化设计的包套模具成形,零件尺寸精度和表面粗糙度可以达到或超过精密铸造件水平。
2、与精密铸件相比,零件的致密度高,成分均匀,组织中没有宏观成分偏析,综合力学性能优异。
3、与传统机械加工方法相比,材料利用率高,工艺过程相对简单,工艺周期短。
附图说明
图1为本发明包套模具的下包套。
图2为本发明包套模具的上包套。
图3为上包套与下包套组装后。
图4为包套模具的真空管。
图5为将真空管下端焊接到上包套的注粉口上。
图6为将真空管顶端封焊并进行热等静压。
图7为热等静压前后包套模具对比。
图8为实施例的超声气体雾化法制得的钛合金粉末。
图9为实施例制备的钛合金粉末的扫描电镜照片;其中:(a)和(b)为不同放大倍数。
图10为实施例制备的钛合金柱状钛合金制件的显微组织图。
具体实施方式
下面通过实施例对本发明技术方案进行清楚、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。
实施例1:
本实施例采用NNS-HIP技术制备柱状钛合金制件,该钛合金制件的粉末热等静压近净成形方法制备,包括如下步骤:
(1)包套模具的制备:包套模具包括上包套、下包套和真空管;其中:所述下包套为上部开口的圆筒状结构,上包套上设有注粉口,且上包套的底面结构与下包套的顶部能够相配合组装,经氩弧焊后密封并形成空腔,如图1-4所示;包套模具采用金属A3钢制作,模具内腔与目标零件形状相似,使用前将包套模具各组成部件依次在石油醚、优级纯酒精中清洗,去除表面灰尘及油污,并对清洗后的各部件进行干燥处理;
(2)钛合金粉末的制备:首先采用预合金法预制钛合金棒料;然后采用无坩锅感应熔炼超声气体雾化法制取洁净预合金粉末,过60目筛取60目筛下的粉末,真空储存;制粉过程中采用纯度为99.995%以上的高纯氩气;所制备的钛合金粉末粒度小于250μm,球形度大于90%,松装密度为理论密度的50~55%(图8-9)。
(3)封装:将钛合金粉末填充到模具内腔中,采用振动法增加粉末的流动性,并使粉末达到振实密度,振实密度为理论密度63~70%;然后将真空管下端焊接到模具注粉口上(图5),并将真空管顶端通过管路与抽真空装置相连接;在室温条件下将密闭模具抽真空至5.0×10-2Pa以上,再将密闭模具放入马弗炉中加热至200-400℃,持续4-8h,加热过程中持续抽真空并保持模具内真空度为5.0×10-2Pa以上;加热完成后将模具真空管顶部进行封焊(图6),检查焊缝质量,并利用氦气质谱检漏仪进行气密闭测试,需达到密封要求。在真空管外焊接保护套。
(4)热等静压:将封装后的包套模具放入热等静压炉中,升温升压至设定温度和压力,保温保压至设定时间;具体地,设定温度为940℃,设定压力为140MPa,设定时间为4h;热等静压中使用高纯氩气作为加压介质,且采用先加压后升温的方式进行热等静压。热等静压处理过程中,包套模具与钛合金粉末协同变形,如图7所示。
(5)后处理:经机械加工及化学腐蚀,得到目标钛合金制件。化学腐蚀选用浓度1~2mol/L的硝酸为腐蚀液,将零件表面模具材料腐蚀掉;化学铣过后,经清洗喷砂和热处理调质后,得到钛合金制件。
本实施例粉末采用钛合金牌号为TA7 ELI。热等静压处理前后,包套模具体积收缩为35%左右,零件表面粗糙度小于Ra3.2,零件致密度高,室温相对密度>99.75%,成分均匀,组织中没有宏观成分偏析,综合力学性能优异,本实施力产品在室温和-253℃力学性能如表1-2所示。
表1室温力学性能数据
表2 -253℃力学性能数据
Claims (10)
1.一种钛合金制件的粉末热等静压近净成形方法,其特征在于:该方法是使用金属包套模具进行,具体包括如下步骤:
(1)包套模具的制备:包套模具采用A3钢制作,模具内腔经注粉和抽真空后,经氩弧焊形成密闭结构;
(2)钛合金粉末的制备:采用无坩锅感应熔炼超声气体雾化法制备钛合金粉末,要求钛合金粉末粒度范围为250μm以下,球形度大于90%,松装密度为理论密度的50~55%;
(3)封装:采用振动法向包套模具内注入钛合金粉末,并达到钛合金粉末振实密度,真空除气后封焊;振实密度为理论密度63~70%;
(4)热等静压:将封焊后的包套模具放入热等静压炉中,升温升压至设定温度和压力,保温保压至设定时间;
(5)后处理:经机械加工和/或硝酸浸泡去除模具后,得到目标钛合金制件。
2.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(1)中,所述包套模具包括上包套、下包套和真空管;其中:所述下包套为上部开口的圆筒状结构,上包套上设有注粉口,且上包套的底面结构与下包套的顶部能够相配合组装在一起形成空腔;经由注粉口向空腔内注粉后,将真空管焊接于注粉口上方,对空腔抽真空后,将真空管顶部封焊。
3.根据权利要求2所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(1)中,所述包套模具的装配过程为:将包套模具各组成部分依次在石油醚、优级纯酒精中清洗,去除表面灰尘及油污,并对清洗后的包套模具进行干燥处理;采用自动焊机将上包套、下包套和真空管焊接,并检查焊缝质量,并利用氦气质谱检漏仪进行气密闭测试,需达到密封要求。
4.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(2)中,钛合金粉末的制备过程为:首先采用预合金法预制钛合金棒料;然后采用无坩锅感应熔炼超声气体雾化法制取洁净预合金粉末,过60目筛取60目筛下的粉末,真空储存,备用;制粉过程中采用高纯氩气。
5.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(3)封装过程为:将钛合金粉末填充到模具内腔中,采用振动法增加粉末的流动性,并使粉末达到振实密度;然后将真空管下端焊接到模具注粉口上,并将真空管顶端与外部抽真空装置相连接;在室温条件下将密闭模具抽真空至5.0×10-2Pa以上,再将密闭模具放入马弗炉中加热(温度范围200-400℃),持续4-8h(加热过程中持续抽真空并保持模具内真空度为5.0×10-2Pa以上);加热完成后将模具真空管顶部进行封焊,在真空管外焊接保护套。
6.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(4)热等静压过程中,设定温度为800-1000℃,设定压力为80-150MPa,设定时间为2-6h;热等静压中使用高纯氩气作为加压介质,且采用先加压后升温的方式进行热等静压。
7.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(4)热等静压处理过程中,包套模具与钛合金粉末协同变形。
8.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(5)中,所述化学铣选用硝酸为腐蚀基液,化学铣通过石墨板与目标件(装有钛合金制件的包套模具)短接构成原电池对包套模具进行腐蚀。
9.根据权利要求7所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:步骤(5)中,化学铣过后,依次进行清洗喷砂和热处理调质。
10.根据权利要求1所述的钛合金制件的粉末热等静压近净成形方法,其特征在于:该方法成形的钛合金制件具有均匀细小的微观组织,良好的综合性能。
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