Article(id=1322281997762932752, tenantId=1146029695717560320, journalId=1220038251117760515, issueId=1322281938308677669, articleNumber=null, orderNo=null, doi=10.11868/j.issn.1001-4381.2025.000591, pmid=null, cstr=32421.14.j.issn.1001-4381.2025.000591, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1761235200000, receivedDateStr=2025-10-24, revisedDate=null, revisedDateStr=null, acceptedDate=1763395200000, acceptedDateStr=2025-11-18, onlineDate=1793186195078, onlineDateStr=2026-10-28, pubDate=1784476800000, pubDateStr=2026-07-20, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1793186195078, onlineIssueDateStr=2026-10-28, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1793186195078, creator=13701087609, updateTime=1793186195078, updator=13701087609, issue=Issue{id=1322281938308677669, tenantId=1146029695717560320, journalId=1220038251117760515, year='2026', volume='54', issue='7', pageStart='1', pageEnd='347', issueExtLink='null', onlineDate='null', pubDate='1784476800000', pubDateStr='2026-07-20', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1793186180903, creator='13701087609', updateTime=1793186267843, updator='13701087609', preIssue=null, nextIssue=null, articleTotal=null, ext={EN=IssueExt(id=1322282303045349604, tenantId=1146029695717560320, journalId=1220038251117760515, issueId=1322281938308677669, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1322282303045349605, tenantId=1146029695717560320, journalId=1220038251117760515, issueId=1322281938308677669, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null, downloadFileDto=null}, startPage=222, endPage=230, ext={EN=ArticleExt(id=1322281998144614417, articleId=1322281997762932752, tenantId=1146029695717560320, journalId=1220038251117760515, language=EN, title=Effects of microstructure and properties of powder metallurgy Ti-Fe-O alloy, columnId=1220689384450478826, journalTitle=Journal of Materials Engineering, columnName=RESEARCH ARTICLE, runingTitle=null, highlight=null, articleAbstract=

Ti-Fe-O alloy with excellent comprehensive mechanical properties is prepared using resource rich Fe2O3 as a strengthening agent and pure Ti powder as raw material, based on ball milling powder mixing, electric field assisted hot pressing sintering technology, and hot rolling process. The impacts of Fe₂O₃ content and the particle size of Ti powder on the microstructure and quasi-tatic tensile properties of the Ti-Fe-O alloys is investigated. The research reveals that an increase in Fe₂O₃ content and a decrease in Ti powder size facilitate the formation of the β phase and refine the α phase grains within the alloy. Hot rolling leads to a significant enhancement in the comprehensive mechanical properties of Ti-Fe-O alloys. The strength improvement is attributed to the interstitial solid-solution strengthening by O elements, grain refinement strengthening resulting from the refinement of the α phase, and the precipitation strengthening of nano-scale acicular secondary α phase within the β phase. Under the condition where the pure Ti particle size ranges from 15 μm to 45 μm (D30), the as-rolled Ti-0.71%Fe₂O₃ (Ti-0.58Fe-0.29O) and Ti-1.43% Fe2O3(Ti-1.08Fe-0.62O) alloys achieve an excellent strength-plasticity matching effect. Their tensile strengths and elongations at break reach 975 MPa with 20.6% elongation and 1128 MPa with 18.4% elongation, respectively.

, authors=Biao GUO1, Xuexia LI1, Hongmei ZHANG1, 2, 3, Xiaonan MU1, 2, 3, Xingwang CHENG1, 2, 3, Kefan ZHENG1, authorsList=Biao GUO, Xuexia LI, Hongmei ZHANG, Xiaonan MU, Xingwang CHENG, Kefan ZHENG, authorCompany=null, correspAuthors=Hongmei ZHANG, Xiaonan MU, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, fund=null), CN=ArticleExt(id=1322282001915293731, articleId=1322281997762932752, tenantId=1146029695717560320, journalId=1220038251117760515, language=CN, title=粉末冶金Ti-Fe-O合金组织和性能影响, columnId=1220689384622445292, journalTitle=材料工程, columnName=研究论文, runingTitle=null, highlight=null, articleAbstract=

以储量丰富的Fe2O3为强化剂,纯Ti粉为原料,采用球磨混粉、电场辅助热压烧结技术和热轧工艺制备出综合力学性能优异的Ti-Fe-O合金。系统研究了Fe2O3含量和Ti粉粒径对Ti-Fe-O合金微观组织和准静态拉伸性能的影响规律。研究表明,Fe2O3含量的增加以及Ti粉粒径的减小促进了合金中β相形成、显著细化了α相晶粒。热轧可大幅提升Ti-Fe-O合金综合力学性能,其中,强度提升来源于O元素的间隙固溶强化、α相细晶强化以及β相中纳米针状次生α相的析出强化。在纯Ti粒径为15~45 μm(D30)条件下,热轧态Ti-0.71%Fe2O3(Ti-0.58Fe-0.29O)和Ti-1.43%Fe2O3(Ti-1.08Fe-0.62O)获得了良好的强-塑性匹配效果,两种合金抗拉强度和断后伸长率分别达到975 MPa,20.6%和1128 MPa,18.4%。

, authors=郭彪1, 李雪霞1, 张洪梅1, 2, 3, 穆啸楠1, 2, 3, 程兴旺1, 2, 3, 郑可凡1, authorsList=郭彪, 李雪霞, 张洪梅, 穆啸楠, 程兴旺, 郑可凡, authorCompany=null, correspAuthors=张洪梅, 穆啸楠, authorNote=null, correspAuthorsNote=
穆啸楠(1991—),男,副研究员,博士,研究方向为结构-功能一体化金属基复合材料,联系地址:北京海淀区中关村南大街5号北京理工大学5号教学楼(100081),E-mail:
张洪梅(1979—),女,教授,博士,研究方向为结构-功能一体化金属基复合材料,联系地址:北京海淀区中关村南大街5号北京理工大学5号教学楼(100081),E-mail:
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2.北京理工大学 唐山研究院,河北 唐山 063000
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2.北京理工大学 唐山研究院,河北 唐山 063000
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nanostructured Ti6Al4V alloy, refAbstract=null), Reference(id=1322282014426902672, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, doi=null, pmid=null, pmcid=null, year=2021, volume=11, issue=1, pageStart=163, pageEnd=null, url=null, language=null, rfNumber=[23], rfOrder=25, authorNames=WANG S, LIANG Y L, SUN H, journalName=Metals, refType=null, unstructuredReference=WANG S, LIANG Y L, SUN H,et al.Oxygen induced phase transformation in TC21 alloy with a lamellar microstructure[J].Metals,2021,11(1):163., articleTitle=Oxygen induced phase transformation in TC21 alloy with a lamellar microstructure, refAbstract=null), Reference(id=1322282014506594449, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, doi=null, pmid=null, pmcid=null, year=1996, volume=41, issue=1, pageStart=1, pageEnd=12, url=null, language=null, rfNumber=[24], rfOrder=26, authorNames=WASZ M L, BROTZEN F R, MCLELLAN R B, 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language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.Material Intelligence Research and Development Laboratory,Beijing Institute of Technology(Zhuhai),Zhuhai 519088,Guangdong,China), AuthorCompanyExt(id=1322282002426998828, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, companyId=1322282002406027306, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3.北京理工大学(珠海) 材料智能研发实验室,广东 珠海 519088)])], figs=[ArticleFig(id=1322282006516445275, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=EN, label=Fig.1, caption=XRD profiles of D30 Ti-Fe2O3 in powder,sintered,and rolled states(x=1.43%、2.86%,and 4.29%)(a)powders;(b)as-sintered;(c)as-rolled, figureFileSmall=d1SWHRsBVuWmglgc2kiedQ==, figureFileBig=EWCLp7CroKzdWkWMXPxUbA==, tableContent=null), ArticleFig(id=1322282006596137052, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=CN, label=图1, caption=粉末态、烧结态和热轧态D30 Ti-xFe2O3的XRD图谱(x=1.43%、2.86%和4.29%)(a)粉末态;(b)烧结态;(c)热轧态, figureFileSmall=d1SWHRsBVuWmglgc2kiedQ==, figureFileBig=EWCLp7CroKzdWkWMXPxUbA==, tableContent=null), ArticleFig(id=1322282006772297821, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=EN, label=Fig.2, caption=SEM images of as-sintered D30Ti-xFe2O3(x=0.71%,1.43%,2.14%,2.86%,3.57%,4.29%), figureFileSmall=MAElLOzndht/oBxBsEJ64A==, figureFileBig=Z9kqaccs1zZe1Bd0v8KZJg==, tableContent=null), ArticleFig(id=1322282006826823774, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=CN, label=图2, caption=烧结态D30 Ti-xFe2O3(x=0.71%,1.43%,2.14%,2.86%,3.57%,4.29%)样品SEM图(a)~(f)及D30Ti-3.57%Fe2O3EDS图(g)

(a)-(f) and EDS images of D30Ti-3.57% Fe2O3(g)

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(a)stress-strain curves of as-sintered D30Ti-xFe2O3(x=0.71%-4.29%);(b)stress-strain curves of as-rolled D30Ti-xFe2O3(x=0.71%-4.29%);(c)stress-strain curves of as-rolled(D10,D80)Ti-1.43%Fe2O3;(d)as-rolled Ti-Fe-O alloys in the present work comparing with GB/T 13810—2017 standard

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(a)pure Ti;(b)Ti-1.43%Fe2O3;(c)Ti-4.29%Fe2O3

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Elemental content of pure Ti powder with different particle sizes (mass fraction/%)

, figureFileSmall=null, figureFileBig=null, tableContent=
ElementFeOCNHTi
D100.040.160.0090.0060.001Bal.
D300.080.080.0100.0210.001Bal.
D800.080.050.0100.0140.001Bal.
), ArticleFig(id=1322282007867011180, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=CN, label=表1, caption=

不同粒径纯Ti粉的元素含量(质量分数/%)

, figureFileSmall=null, figureFileBig=null, tableContent=
ElementFeOCNHTi
D100.040.160.0090.0060.001Bal.
D300.080.080.0100.0210.001Bal.
D800.080.050.0100.0140.001Bal.
), ArticleFig(id=1322282007942508653, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=EN, label=Table 2, caption=

O and N contents of as-rolled D30 Ti-xFe2O3(mass fraction/%)

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleTiTi-1.43% Fe2O3Ti-2.86% Fe2O3Ti-4.29% Fe2O3
Fet0.081.082.083.08
Ot0.080.510.941.37
Om0.620.951.73
Nm0.030.020.04
), ArticleFig(id=1322282008005423214, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=CN, label=表2, caption=

热轧态D30 Ti-xFe2O3的O和N元素含量(质量分数/%)

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleTiTi-1.43% Fe2O3Ti-2.86% Fe2O3Ti-4.29% Fe2O3
Fet0.081.082.083.08
Ot0.080.510.941.37
Om0.620.951.73
Nm0.030.020.04
), ArticleFig(id=1322282009662173295, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=EN, label=Table 3, caption=

Proportion of β phase in sintered and rolled D30Ti-xFe2O3 alloys

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β phaseTi-0.73%Ti-1.43%Ti-2.14%Ti-2.86%Ti-3.57%Ti-4.29%
Sintered10.312.713.515.221.124.1
Rolled22.125.028.132.237.040.5
), ArticleFig(id=1322282009741865072, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=CN, label=表3, caption=

烧结态和热轧态D30Ti-xFe2O3合金中β相占比

, figureFileSmall=null, figureFileBig=null, tableContent=
β phaseTi-0.73%Ti-1.43%Ti-2.14%Ti-2.86%Ti-3.57%Ti-4.29%
Sintered10.312.713.515.221.124.1
Rolled22.125.028.132.237.040.5
), ArticleFig(id=1322282009808973937, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=EN, label=Table 4, caption=

Tensile properties of as-rolled D30Ti-xFe2O3at room temperature

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleσUTS/MPaσ0.2/MPaεf/%
Ti52039834.8
Ti-0.73%97579020.6
Ti-1.43%112890718.4
Ti-2.14%133111405.0
Ti-2.86%150213981.8
Ti-3.57%1280
Ti-4.29%1045
), ArticleFig(id=1322282009897054322, tenantId=1146029695717560320, journalId=1220038251117760515, articleId=1322281997762932752, language=CN, label=表4, caption=

热轧态D30Ti-xFe2O3合金室温拉伸性能

, figureFileSmall=null, figureFileBig=null, tableContent=
SampleσUTS/MPaσ0.2/MPaεf/%
Ti52039834.8
Ti-0.73%97579020.6
Ti-1.43%112890718.4
Ti-2.14%133111405.0
Ti-2.86%150213981.8
Ti-3.57%1280
Ti-4.29%1045
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粉末冶金Ti-Fe-O合金组织和性能影响
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郭彪 1 , 李雪霞 1 , 张洪梅 1, 2, 3 , 穆啸楠 1, 2, 3 , 程兴旺 1, 2, 3 , 郑可凡 1
材料工程 | 研究论文 2026,54(7): 222-230
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材料工程 |研究论文 2026 , 54 (7) : 222 -230
粉末冶金Ti-Fe-O合金组织和性能影响
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郭彪1, 李雪霞1, 张洪梅1, 2, 3 , 穆啸楠1, 2, 3 , 程兴旺1, 2, 3, 郑可凡1
作者信息
  • 1.北京理工大学 材料学院,北京 100081
  • 2.北京理工大学 唐山研究院,河北 唐山 063000
  • 3.北京理工大学(珠海) 材料智能研发实验室,广东 珠海 519088
通讯作者:
穆啸楠(1991—),男,副研究员,博士,研究方向为结构-功能一体化金属基复合材料,联系地址:北京海淀区中关村南大街5号北京理工大学5号教学楼(100081),E-mail:
张洪梅(1979—),女,教授,博士,研究方向为结构-功能一体化金属基复合材料,联系地址:北京海淀区中关村南大街5号北京理工大学5号教学楼(100081),E-mail:
Effects of microstructure and properties of powder metallurgy Ti-Fe-O alloy
Biao GUO1, Xuexia LI1, Hongmei ZHANG1, 2, 3 , Xiaonan MU1, 2, 3 , Xingwang CHENG1, 2, 3, Kefan ZHENG1
Affiliations
  • 1.School of Materials Science and Engineering,Beijing Institute of Technology,Beijing 100081,China
  • 2.Tangshan Research Institute,Beijing Institute of Technology,Tangshan 063000,Hebei,China
  • 3.Material Intelligence Research and Development Laboratory,Beijing Institute of Technology(Zhuhai),Zhuhai 519088,Guangdong,China
出版时间: 2026-07-20 doi: 10.11868/j.issn.1001-4381.2025.000591
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以储量丰富的Fe2O3为强化剂,纯Ti粉为原料,采用球磨混粉、电场辅助热压烧结技术和热轧工艺制备出综合力学性能优异的Ti-Fe-O合金。系统研究了Fe2O3含量和Ti粉粒径对Ti-Fe-O合金微观组织和准静态拉伸性能的影响规律。研究表明,Fe2O3含量的增加以及Ti粉粒径的减小促进了合金中β相形成、显著细化了α相晶粒。热轧可大幅提升Ti-Fe-O合金综合力学性能,其中,强度提升来源于O元素的间隙固溶强化、α相细晶强化以及β相中纳米针状次生α相的析出强化。在纯Ti粒径为15~45 μm(D30)条件下,热轧态Ti-0.71%Fe2O3(Ti-0.58Fe-0.29O)和Ti-1.43%Fe2O3(Ti-1.08Fe-0.62O)获得了良好的强-塑性匹配效果,两种合金抗拉强度和断后伸长率分别达到975 MPa,20.6%和1128 MPa,18.4%。

粉末冶金  /  Ti-Fe-O合金  /  Fe2O3粉末  /  微观组织  /  力学性能

Ti-Fe-O alloy with excellent comprehensive mechanical properties is prepared using resource rich Fe2O3 as a strengthening agent and pure Ti powder as raw material, based on ball milling powder mixing, electric field assisted hot pressing sintering technology, and hot rolling process. The impacts of Fe₂O₃ content and the particle size of Ti powder on the microstructure and quasi-tatic tensile properties of the Ti-Fe-O alloys is investigated. The research reveals that an increase in Fe₂O₃ content and a decrease in Ti powder size facilitate the formation of the β phase and refine the α phase grains within the alloy. Hot rolling leads to a significant enhancement in the comprehensive mechanical properties of Ti-Fe-O alloys. The strength improvement is attributed to the interstitial solid-solution strengthening by O elements, grain refinement strengthening resulting from the refinement of the α phase, and the precipitation strengthening of nano-scale acicular secondary α phase within the β phase. Under the condition where the pure Ti particle size ranges from 15 μm to 45 μm (D30), the as-rolled Ti-0.71%Fe₂O₃ (Ti-0.58Fe-0.29O) and Ti-1.43% Fe2O3(Ti-1.08Fe-0.62O) alloys achieve an excellent strength-plasticity matching effect. Their tensile strengths and elongations at break reach 975 MPa with 20.6% elongation and 1128 MPa with 18.4% elongation, respectively.

powder metallurgy  /  Ti-Fe-O alloy  /  Fe2O3 powder  /  microstructure  /  mechanical property
郭彪, 李雪霞, 张洪梅, 穆啸楠, 程兴旺, 郑可凡. 粉末冶金Ti-Fe-O合金组织和性能影响. 材料工程, 2026 , 54 (7) : 222 -230 . DOI: 10.11868/j.issn.1001-4381.2025.000591
Biao GUO, Xuexia LI, Hongmei ZHANG, Xiaonan MU, Xingwang CHENG, Kefan ZHENG. Effects of microstructure and properties of powder metallurgy Ti-Fe-O alloy[J]. Journal of Materials Engineering, 2026 , 54 (7) : 222 -230 . DOI: 10.11868/j.issn.1001-4381.2025.000591
Ti及Ti合金具有比强度高、耐腐蚀性好、生物相容性优良等特性,在骨植入材料市场占比已达70%~80%,是现阶段生物医用领域应用的理想植入体材料[1-2]。纯Ti与人骨密度、强度相近,但纯Ti的力学性能较差,且硬度不高,材料在使用过程中可能会发生疲劳磨损、微动磨损等问题引发感染[3]。国内外研究者尝试通过添加合金元素的方法来提高纯Ti强度,其中应用最广泛的Ti合金有以Ti-6Al-4V(TC4)和Ti-6Al-7Nb为代表的α+β型Ti合金[4],具有较高的强度、塑性、耐蚀性和成型性,但Al元素会引起骨质疏松和精神紊乱等病症,V元素可引起恶性组织反应,对人体产生毒副作用[5]。此外,Ti合金植入体还存在价格昂贵等问题。
Fe属于置换固溶的强β稳定元素,具有良好的β相稳定效果[6]。Umeda等[7]通过粉末冶金工艺制备Ti-Fe合金,详细分析了Fe在Ti基体中的固溶行为、β相的形成机制以及α-Ti晶粒的细化过程。对Ti-Fe合金的强化机制进行了定量分析,指出Ti-Fe合金的主要强化机制是α-Ti晶粒细化和β-Ti硬质相的分散强化。Guo等[8]通过在Ti中添加不同含量的Fe(1%~5%,质量分数,下同),调控增材制造Ti合金的微观结构,Fe的加入显著促进了柱状晶向等轴晶的转变,提高了β-Ti相的比例,细化了α板条宽度。此外,Niu等[9]研究了不同Fe含量(0%~4%)对Ti-Fe合金的微观结构、力学性能、腐蚀行为和细胞响应的影响。研究结果表明,Ti-Fe合金与纯Ti具有相似的细胞活性和增殖能力,由此表明Fe的加入对细胞响应没有负面影响,具有良好的生物相容性。O属于间隙固溶的强α稳定元素,溶质O通过与螺位错核心的强相互作用对α-Ti有着显著的强化效果[10],但应用难点在于O元素的脆化效应[11-12],当O元素含量超过0.32%,Ti合金的塑性会急剧下降[13-14]。近年来,研究者尝试通过改进制备技术和处理工艺,使O元素在Ti基体中获得了较好的应用效果。如Luo等[15]采用粉末冶金法和热挤压工艺制备出Ti-O合金,成功将O元素含量提升至0.62%,其拉伸屈服强度达到800 MPa,同时保持了良好的塑性(断后伸长率>20%)。Ding等[16]采用激光粉末床熔融3D打印技术,配合定制高氧钛粉(氧含量0.65%,表面氧化层约30 nm),制备出了抗拉强度为1193.3 MPa、断后伸长率为23.3%的Ti-0.67%O合金,实现了强度与塑性的理想平衡。
本工作通过廉价无毒的元素设计,以纯Ti基体中添加Fe、O元素的方式,用Fe元素代替V等元素、O元素代替Al元素[17],在纯Ti中引入Fe2O3。其中Fe2O3作为Fe源和O源,资源丰富,原料成本低,甚至可以利用废料回收获取[18]。采用电场辅助热压烧结结合热轧工艺制备α+β双相高性能Ti-Fe-O合金,系统分析Fe2O3含量和纯Ti颗粒尺寸对Ti-Fe-O合金微观组织和力学性能的影响规律。
采用3种粒径(0~15、15~45 μm和53~105 μm,中位粒径为10、30 μm和80 μm,分别标记为D10、D30和D80)的纯Ti球形粉末为原料,购自中航迈特增材科技(北京)有限公司,其粒度分布和元素含量如表1所示。三氧化二铁(Fe2O3)粉末采用水热法制备[19],其纯度为99.9%,中位粒径为20 nm,原料来源于工业粉末Fe2O3·nH2O。
将纯Ti粉末和Fe2O3粉末按照D30 Ti-xFe2O3(x=0.71%、1.43%、2.14%、2.86%、3.57%和4.29%)、D10 Ti-1.43%Fe2O3和D80 Ti-1.43%Fe2O3的比例与球磨球(直径为3 mm)以球粉质量比5∶1放入球磨罐中,在行星式球磨机中以280 r·min-1球磨4 h,得到Ti-Fe2O3混合粉末。将Ti-Fe2O3混合粉末装入外径为55 mm、内径为25 mm的石墨模具中,通过电场辅助热压烧结炉(FAST,FHP-828)进行真空烧结。烧结参数设定为升温速率为100 ℃/min,烧结温度为900 ℃,压力为50 MPa,保温时间为5 min,真空度为5 Pa,烧结完成后随炉冷却至室温。烧结得到的样品在900 ℃下进行热轧,变形量为75%,首道次保温10 min,每道次回炉1~3 min,共10道次,轧后空冷,最终获得Ti-Fe-O合金。采用X射线衍射仪(Rigaku Ultima IV)用于确定样品的晶相组成,采用Cu Kα辐射(波长λ=0.154 nm),管电压为40 kV,管电流为40 mA,扫描速度为1 (°)/min。采用氧氮氢分析仪(NOH836)测量热轧态试样中N、O元素含量。为了研究Fe2O3含量和纯Ti颗粒尺寸对微观组织的影响,采用600#~3000# SiC砂纸对烧结态和热轧态样品进行打磨和机械抛光,通过扫描电子显微镜(HITACHI S-4800 N)对其微观形貌进行表征,并配合能谱仪表征其表面元素分布。采用透射电子显微镜(FEI Tecnai 20 G2)对样品纳观尺度微结构进行表征,透射试样首先经线切割后打磨至厚度为30 μm,然后通过离子减薄仪(Gatan 691,Ar气环境),电压为3.5 kV,时间为25 min。采用配备LasterXtens激光引伸计的万能试验机(Zwick,Roell Z050)对烧结态和热轧态试样进行准静态拉伸性能测试,热轧态试样标距方向与热轧方向平行,应变速率为5×10-4 s-1,拉伸试样的标距为12 mm,厚度为1.5 mm,每种材料测试3个平行样品,得到拉伸数据。
实验过程中粉末态、烧结态和热轧态D30 Ti-xFe2O3(x=1.43%、2.86%和4.29%)的XRD图谱如图1所示。图1(a)为混合粉体以及D30纯Ti粉末的衍射峰,在混合粉体中存在Fe2O3峰(Fe2O3(104)),表明球磨过程中Fe2O3未发生分解,仍保持较好的晶体结构。烧结得到的Ti-xFe2O3坯体中并未发现Fe2O3衍射峰(图1(b)),说明Fe2O3在烧结过程中发生了一定程度的分解,源自Fe2O3的Fe和O开始扩散固溶于Ti基体中,部分O元素间隙固溶于α-Ti晶胞八面体空隙中,促使晶格产生膨胀[20],导致α-Ti的(0002)和(1011)峰衍射峰发生小角度的偏移。此外,3种不同Fe2O3含量的样品中均未观察到明显的β相衍射峰。
热轧态Ti-xFe2O3(图1(c))出现明显的β相衍射峰(β(100))。Fe2O3分解温度约1200 ℃[21],900 ℃的烧结条件下未能使Fe2O3完全分解,导致Fe和O原子的扩散程度受到一定限制,β相未完全形成。热轧的高温塑性变形过程进一步促进Fe2O3分解,变形引入的位错和空位作为元素扩散的快速通道,加速Fe2O3分解后Fe和O元素的扩散,缺陷的产生和晶格畸变提高了Ti基体的固溶度,推动Fe与Ti原子发生置换固溶,β相的比例进一步上升,衍射峰强度增大。
对热轧后D30纯Ti和Ti-xFe2O3(x=1.43%、2.86%和4.29%)的O和N元素含量进行测量,如表2所示。O元素的含量随着Fe2O3含量的增加而成比例的上升。测得O元素含量(表中Om)普遍高于理论O(表中Ot)含量(高于0.01%~0.36%),这可能与钛合金球磨过程中常见的吸氧过程有关[22],而球磨后样品的N含量增加相对较少(均低于0.05%)。当Fe2O3达到2.86 %后所测得的O含量已高达0.95%。
图2为D30 Ti-xFe2O3(x=0.71%~4.29%)样品的SEM微观组织照片。从图中可以看出,烧结态样品中存在少量的烧结微孔(图中虚线圆圈标记),致密度约为96%,这是Fe2O3未完全分解导致的。随着Fe2O3含量的增加,白亮的β相比例增大,α相晶粒呈现细化趋势。其中,D30 Ti-0.71%Fe2O3(图2(a))和D30 Ti-1.43% Fe2O3(图2(b))中的α相晶粒呈现较为粗大的板条状(α相平均晶粒尺寸约30~50 μm)。随着Fe2O3含量的增加,如图2(c)~(f)所示,D30 Ti-(2.14%~4.29%)Fe2O3烧结态样品中α相晶粒逐渐细化为等轴状(α相平均晶粒尺寸约10~15 μm),晶粒尺寸明显减小,数量增多。在烧结过程中,Fe元素置换固溶于Ti基体,使β相转变温度下降,随着β相的生长,α相周围的β相逐渐连接在一起,将α相隔断,包裹住α相晶粒,使α相晶粒呈现细化后的等轴状。
图3(a)~(f)为对应图2(a)~(f)样品热轧后的SEM微观组织照片。根据前文的相组成和成分分析结果,热轧态D30Ti-xFe2O3样品中Fe2O3完全分解,Fe和O元素已完全固溶进入Ti基体,此时可称为热轧态Ti-Fe-O合金。与烧结态的形貌相比,热轧后合金的微观形貌发生显著变化,无明显的缺陷和孔隙,合金致密度更高,达到99%以上。α相晶粒沿轧制方向拉长,形成平行于轧制方向的条带状结构,并且在热轧过程中发生破碎,形成亚微米级残余棒状α相。如图3(b)和图3(d)~(f)右上角局部放大照片对比,随着Fe2O3含量升高,较为粗大的棒状α相逐渐细化,呈现细密的状态,并且析出了特别细小的针状次生α相(αs)。
对烧结态和热轧态D30Ti-3.57%Fe2O3样品进行EDS面扫分析,如图2(g)和图3(g)所示。代表Fe元素的绿色比较集中分布在白亮的β相区域,代表O元素的蓝色均匀分布在整个测试区域,表明Fe元素有较高的β相稳定能力,在稳定β相中起主导作用。表3统计了烧结态和热轧态样品中β相占比,热轧态样品中β相占比对比烧结态样品提高了超过10%,原本在烧结态中集中分布于β相内的未完全分解的Fe2O3,在热轧的作用下进一步分解、扩散并固溶,产生的O元素在β相内激活了次生α相的形核,Fe元素固溶于Ti基体,降低了β相转变温度,促进了β相形成,扩大了β相区。
为了进一步分析热轧态Ti-Fe-O合金β相中αs的析出行为,采用TEM对轧制态D30Ti-1.43%Fe2O3(D30Ti-1.08Fe-0.62O)和D30Ti-2.86%Fe2O3(D30Ti-2.08 Fe-0.95O)样品进行表征。如图4(a)所示,在Fe2O3含量为1.43%的Ti-1.08 Fe-0.62O合金中,αs尺寸较大(亚微米级)。随着Fe2O3含量增加,αs尺寸明显减小,在Fe2O3含量为2.86%的D30Ti-2.08Fe-0.95 O合金中,观察到β相区域内(对应图3(d)白亮区域)产生高密度纳米αs相,αs相平均宽度约10 nm,长度约85 nm。图4(b)局部区域的选区电子衍射斑点显示沿[21¯1¯0]晶带轴的hcp-αs与[1¯11]晶带轴的bcc-β之间满足Burgers取向关系。
以不同粒径纯Ti粉(D10和D80)为基体,分别制备的热轧态Ti-1.43%Fe2O3样品SEM微观组织照片如图5所示。结合图4(b)可以看出,3种合金的初生α相形态类似,均呈现出沿轧制方向的条带状分布,且β相占比接近30%。但值得注意的是,由于D10纯Ti粉粒径较小(更容易在球磨中吸氧),且不同纯Ti粉含氧量存在差异(见表1),因此D10纯Ti粉制备的合金相比其他样品,尽管Fe含量相同,但含氧量相对更高。以往研究表明,O元素会较大程度增加αs的形核位点,促进αs形成[23]。因此,3种合金β相转变区形貌和尺寸存在明显的差异,其中D10纯Ti粉制备的合金β相转变区不仅产生亚微米棒状α相,还存在较高密度的纳米αs相。
对不同Fe2O3含量的烧结态和热轧态Ti-Fe-O合金进行室温准静态拉伸性能测试,得到工程应力-应变曲线如图6(a),(b)所示。热轧使低Fe2O3含量的Ti-Fe-O合金综合力学性能得到进一步提升,热轧态D30Ti-0.71%Fe2O3(Ti-0.58 Fe-0.29O)抗拉强度和断后伸长率达到975 MPa,20.6%(抗拉强度和断后伸长率相比烧结态样品分别提升了28.9%和37.3%)。热轧态D30Ti-1.43%Fe2O3(Ti-1.08 Fe-0.62O)抗拉强度和断后伸长率达到1128 MPa,18.4%(抗拉强度和断后伸长率相比烧结态样品分别提升了15.1%和275.5%)。可以看出,D30Ti-(0.71%,1.43%)Fe2O3合金呈现出优异的强塑性匹配效果。热轧态D30Ti-2.14%Fe2O3和D30Ti-2.86%Fe2O3的抗拉强度对比烧结态提升均超过了20%,达到1331 MPa和1502 MPa,但断后伸长率低于5.0%,塑性相对较差。随着Fe2O3含量进一步升高,Ti-3.57%Fe2O3和Ti-4.29% Fe2O3表现出强烈的脆性现象,与合金中O含量过高有关(O含量分别达到1.15%和1.73%)。过高的O含量不仅会严重扭曲晶格,阻碍位错运动,还会抑制孪生变形模式,导致Ti的塑性大幅下降[24-25]。结合图6(c)中热轧态(D10,D80)Ti-1.43%Fe2O3合金和图6(b)中D30Ti-1.43%Fe2O3合金的室温准静态拉伸测试结果,可以发现D30Ti-1.43%Fe2O3和D80Ti-1.43% Fe2O3力学性能接近,而D10Ti-1.43%Fe2O3合金抗拉强度达到1447 MPa,接近高强Ti合金水平,但塑性较差,断后伸长率只有5.8%。主要是由于D10Ti-1.43%Fe2O3合金纯Ti粉体中O含量较高,O间隙固溶强化效应强,且αs相比(D30、D80)1.43% Fe2O3合金更加细小,细晶强化作用明显。图6(d)对比了本工作所制备的Ti-Fe-O合金与GB/T 13810—2017中的TA1G、TA2G、TA3G、TA4G和TC4合金材料的抗拉强度和断后伸长率。对比发现热轧态D30Ti-0.71% Fe2O3和D30Ti-1.43%Fe2O3具有良好的强度和塑性的平衡,对比纯Ti和TC4合金展现出一定优势。良好的强塑性匹配和廉价无毒的元素设计使得Ti-Fe-O合金在生物医用材料领域具有潜在的应用价值。
表4统计了热轧态D30Ti-xFe2O3(x=0.71%~4.29%)合金的抗拉强度(σUTS)、屈服强度(σ0.2)和断后伸长率(εf),图7展示了屈服强度(σ0.2)随Fe2O3、Fe和O含量变化的关系。固溶强化对屈服强度的影响分别为328.6 MPa/xFe2O3(图7(a))、470.0 MPa/xFe(图7(b))和1058.2 MPa/xO(图7(c)),对应的R2值(评估拟合质量)分别为0.9665、0.9671和0.9288,均高于0.9,表明实验数据与拟合曲线的偏差非常小。上述结果表明,O的间隙固溶对强度提升的贡献非常明显,是Ti-Fe-O合金强度提升的主要原因。O原子半径较小(约0.066 nm),易填入α-Ti晶胞八面体空隙中,促使晶格发生畸变,产生应力场阻碍位错运动,增加位错滑移阻力,提升抗拉强度,并且随着O元素含量的提高,强化作用增强。但过量的O固溶易导致合金脆化,降低塑性。根据图3中微观组织照片分析,热轧后产生的微米级残余棒状α相有效提高了合金的强度。细小的棒状α相有效增加了晶界面积,使位错在晶界处塞积,滑移受阻,进而提高了合金的强度。在β相中析出的弥散分布的细小纳米级针状αs也是提高合金抗拉强度的重要因素。纳米级αs相尺寸小、分布密集且均匀,可提供更强的钉扎作用,阻碍位错运动,强化Ti-Fe-O合金。αs相的形成还可能伴随β相中溶质元素的再分配,导致β相基体固溶度变化,间接影响力学性能。考虑到合金烧结和热轧过程中涉及快速升降、温过程,Fe2O3热分解时间较短,O元素未完全均匀扩散至基体内部,而主要集中分布在β相中,并在热轧过程中激活αs的形核,因而在O元素含量超过0.32%的条件下,合金仍保持较好的塑性。此外,引入适当含量的Fe2O3,热轧后析出的αs相存在一定的塑性变形能力(如图4(a)中棒状αs相内部产生的高密度位错),可使合金变形更均匀,减少局部应力集中,延长均匀变形阶段,有利于均匀的塑性变形。
图8为热轧态纯钛与典型Ti-Fe-O合金拉伸断口形貌。纯Ti的断口出现密集的大韧窝(如图8(a)圆圈所示),属于韧性断裂,当在Ti基体中加入Fe2O3,断裂行为发生改变,拉伸断裂模式逐渐由韧性向脆性转变,D30Ti-1.43%Fe2O3合金的断口呈现韧窝和解理的混合(如图8(b)圆圈和矩形圈所示),为准解理混合型断裂,随着Fe2O3含量的增加,D30Ti-4.29%Fe2O3合金的断口没有韧窝等韧性断裂特征,几乎由解理组成(如图8(c)所示),为脆性断裂。
(1)通过低速球磨、电场辅助热压烧结和热轧工艺成功将Fe2O3引入纯Ti中,制备出了具有α+β双相结构和纳米级αs相的Ti-Fe-O合金。Fe2O3在烧结和热轧过程中完成分解,产生的Fe集中分布于β相,对稳定β相有促进作用。Fe2O3含量的增高和Ti粉粒径的减小对促进β相的产生以及细化α相晶粒有重要作用。
(2)低Fe2O3含量和中等粒径Ti粉制备出了具有高强度和高塑性的Ti-Fe-O合金。15~45 μm粒径(D30)纯Ti粉的Ti-0.71%Fe2O3(Ti-0.58Fe-0.29O)和Ti-1.43%Fe2O3(Ti-1.08 Fe-0.62O)抗拉强度和断后伸长率分别达到975 MPa,20.6%和1128 MPa,18.4%。在医用外科植入物用Ti及Ti合金方面具有潜在应用价值。
(3)Fe2O3对Ti-Fe-O合金的增强效果为328.6 MPa/xFe2O3。强化机制主要包括O元素间隙固溶强化、α相细化以及β相中纳米级αs的析出强化。
  • 国家自然科学基金项目(52301186)
  • 国家自然科学基金项目(52471114)
  • 冲击环境材料技术重点实验室基金项目(6142902240401)
  • 河北省自然科学基金项目(E2024105014)
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2026年第54卷第7期
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doi: 10.11868/j.issn.1001-4381.2025.000591
  • 接收时间:2025-10-24
  • 首发时间:2026-10-28
  • 出版时间:2026-07-20
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  • 收稿日期:2025-10-24
  • 录用日期:2025-11-18
基金
国家自然科学基金项目(52301186)
国家自然科学基金项目(52471114)
冲击环境材料技术重点实验室基金项目(6142902240401)
河北省自然科学基金项目(E2024105014)
作者信息
    1.北京理工大学 材料学院,北京 100081
    2.北京理工大学 唐山研究院,河北 唐山 063000
    3.北京理工大学(珠海) 材料智能研发实验室,广东 珠海 519088

通讯作者:

穆啸楠(1991—),男,副研究员,博士,研究方向为结构-功能一体化金属基复合材料,联系地址:北京海淀区中关村南大街5号北京理工大学5号教学楼(100081),E-mail:
张洪梅(1979—),女,教授,博士,研究方向为结构-功能一体化金属基复合材料,联系地址:北京海淀区中关村南大街5号北京理工大学5号教学楼(100081),E-mail:
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2种不同金属材料的力学参数
科
Family
属数
Number of
genus
种数
Number of
species
占总种数比例
Percentage of
total species (%)
属
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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