Article(id=1240631734715347724, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631729627648823, articleNumber=null, orderNo=null, doi=10.3969/j.issn.0253-6099.2024.03.029, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1700496000000, receivedDateStr=2023-11-21, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773719255379, onlineDateStr=2026-03-17, pubDate=1717171200000, pubDateStr=2024-06-01, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773719255379, onlineIssueDateStr=2026-03-17, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773719255379, creator=13701087609, updateTime=1773719255379, updator=13701087609, issue=Issue{id=1240631729627648823, tenantId=1146029695717560320, journalId=1235980550691926019, year='2024', volume='44', issue='3', pageStart='1', pageEnd='181', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773719254166, creator=13701087609, updateTime=1773724083554, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1240651985603580488, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631729627648823, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1240651985603580489, tenantId=1146029695717560320, journalId=1235980550691926019, issueId=1240631729627648823, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=135, endPage=139, ext={EN=ArticleExt(id=1240631734987977498, articleId=1240631734715347724, tenantId=1146029695717560320, journalId=1235980550691926019, language=EN, title=Effect of Laser Remelting on Thermal Stability of Ti-6Al-4V Alloy Prepared by Laser Powder Bed Fusion, columnId=1236276108207902848, journalTitle=Mining and Metallurgical Engineering, columnName=MATERIALS, runingTitle=null, highlight=null, articleAbstract=

The effect of laser remelting (LR) on the microstructure property and thermal stability of Ti-6Al-4V alloy prepared by laser powder bed fusion (LPBF) was investigated. The results show that after LR treatment, the thermal stability of the α′ phase within the LRed-Ti-6Al-4V titanium alloy samples is significantly improved, and the temperature at which β-Ti phase appears is up from 500 ℃ to 700 ℃. After heat treatment, the grains in LPBF-Ti-6Al-4V titanium alloy grow continuously, and obviously appear to be “short bar-like” and “coarse lamellar” at the temperature above 700 ℃; while the grains in the melting zone of the surface layer of the LRed-Ti-6Al-4V sample are still maintain equiaxial, and the relatively uniform and fine needle-like microstructure are observed in the melting zone and heat affected zone above 700 ℃. The surface microhardness of those two groups of samples decreases with the increased temperature, especially significant at 700 ℃ and 850 ℃ respectively. It is found that the rapid coarsening of β-Ti grains is the main reason for the falling down of hardness.

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研究了激光重熔(LR)对激光粉末床熔合(LPBF)制备Ti-6Al-4V合金的组织性能和热稳定性的影响。结果表明,LR处理后,LRed-Ti-6Al-4V钛合金样品内α′相热稳定性显著提升,β-Ti相出现的温度点由500 ℃升至700 ℃。热处理后,LPBF-Ti-6Al-4V钛合金内晶粒持续生长,700 ℃以上出现明显的“短棒状”和“粗层片状”特征;而LRed-Ti-6Al-4V样品表层熔化区内晶粒仍维持等轴特征,700 ℃以上的熔化区和热影响区内呈现较为均匀细小的针状组织。两组样品的表面显微硬度值随温度升高而不断降低,并且分别在700 ℃和850 ℃显著下降,β-Ti晶粒的迅速粗化是引起硬度下降的主要原因。

, correspAuthors=null, authorNote=null, correspAuthorsNote=
杨扬(1963—),男,湖南常德人,博士,教授,主要研究方向为材料动态行为。E-mail:
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詹宇星(2001—),女,湖南长沙人,硕士研究生,主要研究方向为增材制造钛合金。E-mail:

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詹宇星(2001—),女,湖南长沙人,硕士研究生,主要研究方向为增材制造钛合金。E-mail:

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詹宇星(2001—),女,湖南长沙人,硕士研究生,主要研究方向为增材制造钛合金。E-mail:

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(a)LPBF-Ti-6Al-4V样品;(b)LRed-Ti-6Al-4V样品

, figureFileSmall=lkoNPk+lR0ebT1CrRJ5slw==, figureFileBig=W6Fjj6walk7sLQLKrs3a0Q==, tableContent=null), ArticleFig(id=1240651348874686530, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631734715347724, language=EN, label=null, caption=null, figureFileSmall=u2kifsxIwsBk6GkGvTVkmQ==, figureFileBig=UXogjciOn3E2AdsIZ4ReMg==, tableContent=null), ArticleFig(id=1240651349189259353, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631734715347724, language=CN, label=图3, caption=LPBF-Ti-6Al-4V合金热处理前后显微组织形貌

(a),(b)热处理前;(c)500 ℃热处理后;(d)600 ℃热处理后;(e)700 ℃热处理后;(f)850 ℃热处理后

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(a),(b)热处理前;(c)500 ℃热处理后;(d)600 ℃热处理后;(e)700 ℃热处理后;(f)850 ℃热处理后

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(a)LPBF-Ti-6Al-4V样品;(b)LRed-Ti-6Al-4V样品

, figureFileSmall=LWDshfI1eJN2aMitQrTpWA==, figureFileBig=+OEmyrwPFzCQy2AOftNtCA==, tableContent=null), ArticleFig(id=1240651349856153761, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631734715347724, language=EN, label=null, caption=null, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称退火温度/℃β相峰强度α(α′)相峰强度
LPBF-Ti-6Al-4V500 ℃2511 154
600 ℃7391 591
700 ℃8641 766
850 ℃418646
LRed-Ti-6Al-4V500 ℃
600 ℃
700 ℃1051 249
850 ℃2911 460
), ArticleFig(id=1240651349990371507, tenantId=1146029695717560320, journalId=1235980550691926019, articleId=1240631734715347724, language=CN, label=表1, caption=

2组样品内β相、α(α′)相衍射峰强度

, figureFileSmall=null, figureFileBig=null, tableContent=
样品名称退火温度/℃β相峰强度α(α′)相峰强度
LPBF-Ti-6Al-4V500 ℃2511 154
600 ℃7391 591
700 ℃8641 766
850 ℃418646
LRed-Ti-6Al-4V500 ℃
600 ℃
700 ℃1051 249
850 ℃2911 460
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激光重熔对激光粉末床熔合制备Ti-6Al-4V合金热稳定性的影响机制研究
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詹宇星 , 杨扬
矿冶工程杂志 | 材料 2024,44(3): 135-139
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矿冶工程杂志 | 材料 2024, 44(3): 135-139
激光重熔对激光粉末床熔合制备Ti-6Al-4V合金热稳定性的影响机制研究
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詹宇星 , 杨扬
作者信息
  • 中南大学 材料科学与工程学院,湖南 长沙 410083
  • 詹宇星(2001—),女,湖南长沙人,硕士研究生,主要研究方向为增材制造钛合金。E-mail:

通讯作者:

杨扬(1963—),男,湖南常德人,博士,教授,主要研究方向为材料动态行为。E-mail:
Effect of Laser Remelting on Thermal Stability of Ti-6Al-4V Alloy Prepared by Laser Powder Bed Fusion
Yuxing ZHAN , Yang YANG
Affiliations
  • School of Materials Science and Engineering, Central South University, Changsha 410083, Hunan, China
出版时间: 2024-06-01 doi: 10.3969/j.issn.0253-6099.2024.03.029
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研究了激光重熔(LR)对激光粉末床熔合(LPBF)制备Ti-6Al-4V合金的组织性能和热稳定性的影响。结果表明,LR处理后,LRed-Ti-6Al-4V钛合金样品内α′相热稳定性显著提升,β-Ti相出现的温度点由500 ℃升至700 ℃。热处理后,LPBF-Ti-6Al-4V钛合金内晶粒持续生长,700 ℃以上出现明显的“短棒状”和“粗层片状”特征;而LRed-Ti-6Al-4V样品表层熔化区内晶粒仍维持等轴特征,700 ℃以上的熔化区和热影响区内呈现较为均匀细小的针状组织。两组样品的表面显微硬度值随温度升高而不断降低,并且分别在700 ℃和850 ℃显著下降,β-Ti晶粒的迅速粗化是引起硬度下降的主要原因。

增材制造  /  3D打印  /  激光粉末床熔合  /  激光重熔  /  Ti-6Al-4V  /  退火热处理  /  热稳定性

The effect of laser remelting (LR) on the microstructure property and thermal stability of Ti-6Al-4V alloy prepared by laser powder bed fusion (LPBF) was investigated. The results show that after LR treatment, the thermal stability of the α′ phase within the LRed-Ti-6Al-4V titanium alloy samples is significantly improved, and the temperature at which β-Ti phase appears is up from 500 ℃ to 700 ℃. After heat treatment, the grains in LPBF-Ti-6Al-4V titanium alloy grow continuously, and obviously appear to be “short bar-like” and “coarse lamellar” at the temperature above 700 ℃; while the grains in the melting zone of the surface layer of the LRed-Ti-6Al-4V sample are still maintain equiaxial, and the relatively uniform and fine needle-like microstructure are observed in the melting zone and heat affected zone above 700 ℃. The surface microhardness of those two groups of samples decreases with the increased temperature, especially significant at 700 ℃ and 850 ℃ respectively. It is found that the rapid coarsening of β-Ti grains is the main reason for the falling down of hardness.

additive manufacturing  /  3D printing  /  laser powder bed fusion (LPBF)  /  laser remelting (LR)  /  Ti-6Al-4V  /  annealing heat treatment  /  thermal stability
詹宇星, 杨扬. 激光重熔对激光粉末床熔合制备Ti-6Al-4V合金热稳定性的影响机制研究. 矿冶工程杂志, 2024 , 44 (3) : 135 -139 . DOI: 10.3969/j.issn.0253-6099.2024.03.029
Yuxing ZHAN, Yang YANG. Effect of Laser Remelting on Thermal Stability of Ti-6Al-4V Alloy Prepared by Laser Powder Bed Fusion[J]. Mining and Metallurgical Engineering, 2024 , 44 (3) : 135 -139 . DOI: 10.3969/j.issn.0253-6099.2024.03.029
Ti-6Al-4V合金具有比强度高、延展性和耐腐蚀性优良等特性,广泛应用于航空航天和海洋船舶等领域。采用传统加工工艺制备Ti-6Al-4V合金,能耗高、材料损耗大[1-3];目前采用增材制造技术制备Ti-6Al-4V合金已经成为研究热点。激光粉末床熔合(LPBF)是一种典型的增材制造工艺,该技术采用高能激光束对金属粉末进行照射扫描,使其熔化后快速凝固,采用“逐层叠加”的方式进行成型制备[4],结合计算机编程技术可以实现精准高效的生产制造[5-6],完成复杂零件的快速批量成型[7]。但由于LPBF过程中存在极大的冷速(>104K/s),会导致部件内部存在明显的组织结构问题[8],使其在高温环境下呈现不稳定的综合性能。本文采用激光重熔(LR)技术作为LPBF-Ti-6Al-4V打印样的辅助后处理工艺[9-12],探讨激光重熔处理对增材制造钛合金热稳定性的作用机制。
LPBF过程使用无锡飞而康公司生产的Ti-6Al-4V粉末作为原料。Ti-6Al-4V粉末呈球状,颗粒中值尺寸为33.0 μm。
LPBF制备过程在恒定气压的高纯度氩气保护下进行,采用往复式反平行旋转扫描策略,激光束的扫描方向每次旋转67°。设定激光功率(P)为225 W,粉末层厚度(t)为30 μm,扫描速率(vs)为1 000 mm/s,扫描间距(h)为0.12 mm,焦距为2 mm。样品制备完成后,在2 h内将基材缓慢冷却至室温。所得样品命名为LPBF-Ti-6Al-4V。相应的能量密度由式(1)计算[13],得到LPBF过程中单位体积能量密度(VED)为62.5 J/mm3
LR过程采用往复式S形扫描策略,选用氩气为保护气氛。设定激光功率(P)为1 kW,扫描速率(v)为20 mm/s,光斑直径(ξ)为4 mm,搭接率为50%。所得样品命名为LRed-Ti-6Al-4V。由式(2)[14]计算得到LR实验中能量密度(E)为12.5 J/mm3
对2组样品进行保温2 h的退火热处理,设置退火温度分别为500,600,700及850 ℃,然后炉冷至室温。对热处理前后所有样品进行XRD测试,选用Cu-Kα进行扫描,扫描速度为8°/min。使用Jade软件对X射线衍射所得数据进行物相定性分析。各试样在经过研磨抛光后,使用Kroll试剂作为腐蚀液,腐蚀55 s,对样品进行金相组织观察。使用HV-1000Z型数字显微维氏硬度计测量硬度,设定外加载荷为0.2 kg(1.96 N)、加载时间为15 s,每次打6个点,计算硬度平均值。测量热处理前后LPBF-Ti-6Al-4V样品的表面硬度和LRed-Ti-6Al-4V样品的表层显微硬度。
图1为LPBF-Ti-6Al-4V和LRed-Ti-6Al-4V样品热处理前的XRD图像。由图1可知,2组样品的X射线衍射图谱都以α(α′)相为主,均没有出现明显的β峰。由Bragg定律计算可以得出,LPBF-Ti-6Al-4V样品的晶格参数ac分别为(0.292 803 3±0.000 12)nm和(0.466 507 3±0.000 21)nm,LRed-Ti-6Al-4V样品的晶格参数ac分别为(0.294 318 6±0.000 15)nm和(0.469 857 3±0.000 20)nm。将计算结果与PDF卡片(№44-1294)中α(α′)相的晶格参数(a=0.292 nm,c=0.463 nm)对比,晶格参数基本保持一致,可以认为这2组样品中都是α(α′)相。由于LPBF和LR过程都伴随着快速升温熔化-急速冷却凝固特征,β-Ti主要发生非扩散型相变转变为α′相[15-16],因此认为2组样品的物相成分都是α′-Ti。
图2是2组样品经过退火热处理后的XRD图像,对应的样品内β相、α(α′)相衍射峰强度见表1。由图2可以看出,所有样品衍射图像中主要的α(α′)相衍射峰所在位置并未发生太大变化。已知在500 ℃以上,增材制造过程产生的亚稳相α′马氏体会发生分解[17]
结合α-β双相转变知识可知,α相转变为β相的温度点大概在950 ℃左右[18],而本次实验设定的温度范围为500~850 ℃,并未到达α-β相变的温度点。因此认为本次退火热处理实验中主要发生α′相的分解反应,新产生的β相对应XRD图谱上出现的β峰。综合分析微观组织形貌和XRD图谱,LPBF-Ti-6Al-4V样品经过500 ℃保温处理后出现β-Ti相,而LRed-Ti-6Al-4V钛合金样品在700 ℃时才开始出现β-Ti相;同时由表1可以看到,以衍射峰作为标准,相同温度下LPBF-Ti-6Al-4V样品β相的相对峰高均明显高于LRed-Ti-6Al-4V样品,说明LPBF-Ti-6Al-4V样品发生α′分解所需要的温度更低,且在相同温度下α′相分解的程度更大。即在无氧受热环境下,LRed-Ti-6Al-4V合金能更好地保留原有的α′相成分,说明LRed-Ti-6Al-4V样品内α′相的热稳定性更高。
图3为热处理前后LPBF-Ti-6Al-4V合金的金相组织。从图3(a)~(b)可以看出,LPBF-Ti-6Al-4V样品内呈现明显的α′柱状晶特征,归因为LPBF过程具有极大的冷却速率(>104K/s),导致β相来不及转变为α相,而是通过非扩散相变的方式转变为α′相马氏体[19]。LPBF-Ti-6Al-4V样品内部出现明显的不规则孔隙,推测是熔合成型过程中激光束的移动速度很快,导致每层合金粉末未能发生完全熔合;同时LPBF-Ti-6Al-4V样品内存在一定的孔洞缺陷,这是由于LPBF过程中激光扫描速率较大,在高能束聚焦下粉末熔化产生大量金属蒸气,熔池内极大的冷却速率会造成蒸气挥发性的减弱,致使其无法在成型前扩散排出,在试样内部以气泡孔洞形式存在[20]。从图3(c)~(f)可以看出,经过退火热处理后,样品内晶粒不断长大。在较低退火温度下(500 ℃,600 ℃),合金内部马氏体逐渐粗化,纵横比不断减小,且出现弥散分布的细小β相晶粒;退火温度达到700 ℃时,部分位置的α(α′)相板条马氏体被其他板条α相或新长大的β相晶粒截断分割,进而呈现“短棒状”特征;退火温度达到850 ℃时,LPBF-Ti-6Al-4V样品内呈现大尺寸层片状α相和层间β相交织排布的特征。由于LPBF过程具有高冷却速率特征,LPBF-Ti-6Al-4V样品组织结构具有显著各向异性,经过退火热处理后样品各向异性特征更明显,原始β晶界处的α′马氏体大多以相互平行、相近取向的生长方式形成集束生长的粗大板条组织,这种强择优取向组织会对样品整体性能造成不利影响。
图4为LRed-Ti-6Al-4V样品热处理前后的金相组织。如图4(a)~(b)所示,LRed-Ti-6Al-4V合金表层约150 μm深度范围内晶粒组织发生改变,并且出现组织分层。重熔层组织由熔化区的等轴晶粒(约60~70 μm)以及热影响区的精细针状晶粒(约80~90 μm)构成。较LPBF-Ti-6Al-4V样品,LRed-Ti-6Al-4V样品表层组织中孔洞间隙问题得到明显改善,说明激光重熔形成的新熔池能够更好地填补原有的成型缺陷,能有效提升样品表层组织的致密度、优化合金表层成型质量。较低退火温度下(500 ℃,600 ℃),LRed-Ti-6Al-4V样品表层等轴晶粒趋于向针状形态转变,在晶粒尺寸上仍保持原有水平,并未发生显著粗化,稍深处的马氏体晶粒呈现高纵横比的针状特征;热处理温度700 ℃以上时,LRed-Ti-6Al-4V样品表层的等轴晶粒完全转化为纵横比更大的针状晶粒,重熔层呈现均匀且较为精细的针状晶粒组织,并以针状形态持续生长。
采用维氏硬度计对热处理前后打印样品进行硬度测定,退火热处理前后LPBF-Ti-6Al-4V样品的显微硬度如图5(a)所示。随着退火温度升高,LPBF-Ti-6Al-4V合金显微硬度呈现持续降低趋势。退火前样品显微硬度为323.1HV0.2,当退火温度升至850 ℃时,表面显微硬度降至282.5HV0.2
退火热处理前后LRed-Ti-6Al-4V样品的显微硬度如图5(b)所示。激光重熔后钛合金的显微硬度变化趋势与重熔处理前保持一致。且在相同处理条件下,LRed-Ti-6Al-4V样品表层0~150 μm内的显微硬度均高于LPBF-Ti-6Al-4V样品。
LRed-Ti-6Al-4V样品表层150 μm深度范围内的硬度均高于LPBF-Ti-6Al-4V样品,证明激光重熔对钛合金硬度的作用深度在150 μm范围内。对比2组样品热处理前后的表面硬度降幅,LPBF-Ti-6Al-4V样品经700 ℃退火处理后的表面显微硬度降幅(3.9%)显著高于500 ℃以及600 ℃退火后降幅(2.3%,2.4%),而LRed-Ti-6Al-4V样品经500 ℃,600 ℃以及700 ℃退火处理后的表面显微硬度降幅都较为接近(8.4%,9.0%和9.2%),850 ℃时硬度降幅达到15.0%。即2组钛合金样品在退火过程中会出现表面显微硬度下降的明显转折点分别为700 ℃和850 ℃。
结合LPBF-Ti-6Al-4V和LRed-Ti-6Al-4V合金样品热处理后的物相组分和组织结构变化,对不同温度下样品的显微硬度变化曲线进行分析。由于重熔后样品表层组织发生顶部晶粒的等轴化和整体结构的精细化,且有效改善了表层粉末熔合不足和熔池内气体逸出造成的孔洞缺陷,LRed-Ti-6Al-4V样品表层硬度较LPBF-Ti-6Al-4V样品显著提升。
LPBF-Ti-6Al-4V样品经500 ℃退火处理即发生α′相的分解,随着温度不断升高,β相含量进一步提升。由于β相强度低于α相[21],LPBF-Ti-6Al-4V样品表面硬度的下降是α′相分解和晶粒生长共同作用的结果。退火温度700 ℃以上时,LPBF-Ti-6Al-4V样品出现表面显微硬度的显著下降。双相钛合金内的β-Ti晶粒在(700±5)℃保温处理条件下生长速度明显加快[22],即在700 ℃以上退火会产生显著粗化的β-Ti晶粒,进而引起Ti-6Al-4V钛合金样品显微硬度发生较大程度的降低。而LRed-Ti-6Al-4V样品在较低温度(500,600 ℃)下均能维持较为细小的α(α′)相晶粒组织,这一阶段样品显微硬度的降低主要是由熔化区内等轴晶粒的形态转变以及重熔层晶粒尺寸的增大引起的;退火温度700 ℃以上时,LRed-Ti-6Al-4V样品内才开始产生β相晶粒,且重熔层晶粒组织仍维持在较为精细的尺寸范围,因此经700 ℃退火处理并不会引起LRed-Ti-6Al-4V样品表面显微硬度值的大幅下降。
1)激光粉末床熔合和激光重熔过程都伴随有高温度梯度和高冷却速率,β相来不及向α相转变,而是通过非扩散型相变转变为α′马氏体。激光重熔处理后,Ti-6Al-4V合金表层晶粒发生显著细化,并且有效填补了表层内的孔洞间隙,大幅提升了样品的显微硬度。
2)对比2组样品热处理前后的组织结构变化,LRed-Ti-6Al-4V样品内分解产生β相的温度点更高,且晶粒尺寸相对更为稳定;而LPBF-Ti-6Al-4V样品在500 ℃下即出现β相衍射峰,且加热后呈现明显的晶粒粗大和截断现象,证实激光重熔处理能有效提升LPBF-Ti-6Al-4V样品物相成分和晶粒尺寸的热稳定性。
3)2组样品的表面显微硬度值均随温度升高呈现不同程度的降低趋势,并且都存在明显下降的转折温度点,激光重熔前后钛合金的转折温度点分别为700 ℃和850 ℃。β相的生长以及整体晶粒的粗化是造成硬度变化的原因。
  • 国家自然科学基金(51871243; 51574290)
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2024年第44卷第3期
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doi: 10.3969/j.issn.0253-6099.2024.03.029
  • 接收时间:2023-11-21
  • 首发时间:2026-03-17
  • 出版时间:2024-06-01
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  • 收稿日期:2023-11-21
基金
国家自然科学基金(51871243; 51574290)
作者信息
    中南大学 材料科学与工程学院,湖南 长沙 410083

通讯作者:

杨扬(1963—),男,湖南常德人,博士,教授,主要研究方向为材料动态行为。E-mail:
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2种不同金属材料的力学参数

Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)

Genus
种数
Number of
species
占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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