Please wait a minute...
材料研究学报  2026, Vol. 40 Issue (4): 295-304    DOI: 10.11901/1005.3093.2025.137
  研究论文 本期目录 | 过刊浏览 |
Ti含量对奥氏体15Cr-ODS合金硬度的影响
曹意1,2, 李静2(), 熊良银2, 刘实2, 张春华1()
1.沈阳工业大学材料科学与工程学院 沈阳 110870
2.中国科学院金属研究所 师昌绪先进材料创新中心 沈阳 110016
Effect of Ti Content on Microstructure and Hardness of an Austenitic 15Cr-ODS Alloy
CAO Yi1,2, LI Jing2(), XIONG Liangyin2, LIU Shi2, ZHANG Chunhua1()
1.School of Materials Science and Engineering, Shenyang University of Technology, Shenyang 110870, China
2.Shi -changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
引用本文:

曹意, 李静, 熊良银, 刘实, 张春华. Ti含量对奥氏体15Cr-ODS合金硬度的影响[J]. 材料研究学报, 2026, 40(4): 295-304.
Yi CAO, Jing LI, Liangyin XIONG, Shi LIU, Chunhua ZHANG. Effect of Ti Content on Microstructure and Hardness of an Austenitic 15Cr-ODS Alloy[J]. Chinese Journal of Materials Research, 2026, 40(4): 295-304.

全文: PDF(23617 KB)   HTML
摘要: 

用机械合金化制备Fe-15Ni-15Cr-2.0Mo-1.0Mn-(0.2, 0.8, 1.5)Ti-0.4Y2O3合金并使用SEM、EBSD、TEM和显微硬度仪等手段对其表征,研究了Ti含量对其微观组织和显微硬度的影响。结果表明,Ti含量的提高使这种合金中生成的Y-Ti-O复合纳米氧化物显著增加。Ti含量为0.8% (质量分数)的合金中纳米氧化物颗粒的尺寸范围为2~7 nm,氧化物主要由烧绿石结构的Y2Ti2O7和正交结构的Y2TiO5组成。纳米氧化物对晶界的强钉扎和合金晶粒的细化,使其显微硬度从302.7HV0.5(0.2%Ti)提高到401.3HV0.5。但是,Ti含量提高到1.5%的合金,过量的Ti在其内生成粗大的TiO2颗粒而使晶粒增大和硬度下降。大约0.8%的Ti含量与0.4% (质量分数)的Y2O3配合,可在15Cr-FeCrNi合金中生成弥散分布、尺寸较小的纳米强化相,使其显微硬度较高。

关键词 材料合成与加工工艺15Cr-ODS奥氏体合金热等静压Ti含量微观结构显微硬度    
Abstract

An austenitic oxide dispersion strengthened (ODS) alloy with the composition of Fe-15Ni-15Cr-2.0Mo-1.0Mn-(0.2, 0.8, 1.5) Ti-0.4Y2O3 was fabricated using mechanical alloying and hot isostatic pressing (HIP). The effect of Ti content on the microstructure and microhardness of austenitic 15Cr-ODS alloy was studied through SEM, EBSD, TEM, and microhardness tester. The results show that the increase of Ti content significantly facilitates the formation of Y-Ti-O complex oxide particles. When the Ti content approaches 0.8% (mass fraction), the size of oxide particles in the matrix is mainly concentrated in the range from 2 nm to 7 nm. These nano oxideparticles nanoparticles are mainly composed of Y2Ti2O7 with pyrochlore structure and Y2TiO5 with orthogonal structure. Due to the strong pinning effect of nano oxide-particles to grain boundaries, the grain refinement is achieved in the ODS alloy with 0.8% addition of Ti. At the same time, the microhardness of the alloy is increased from 302.7HV0.5(0.2%Ti) to 401.3HV0.5 (0.8%Ti). However, when Ti increases to 1.5%, the excessive Ti leads to the formation of coarse TiO2 particles in addition to Y2Ti2O7 and Y2TiO5, which leads to increased grain size and decreased hardness of the alloy. It is proven that the nano oxideparticles with homogenous distribution and fine size can be obtained in the 15Cr-FeCrNi ODS alloy when the contents of Ti and Y2O3 are about 0.8% and 0.4% (mass fraction), respectively, thus providing better mechanical properties.

Key wordssynthesizing and processing technics for materials    15Cr-ODS austenitic alloy    hot isostatic pressing    Ti content    microstructure    microhardness
收稿日期: 2025-04-14     
ZTFLH:  TG142.7  
基金资助:中核科研领创项目(CNNC-LCKY-2024-094)
通讯作者: 李静,副研究员,jingli@imr.ac.cn,研究方向为氧化物弥散强化合金;
张春华,教授,zhangchunhua5858@126.com,研究方向为材料表面工程;
Corresponding author: LI Jing, Tel: 15140168377, E-mail: jingli@imr.ac.cn;
ZHANG Chunhua, Tel: 13709840616, E-mail: zhangchunhua5858@126.com
作者简介: 曹 意,女,1998年生,硕士生
图1  不同Ti含量热等静压态ODS合金的晶粒IPF图和晶粒尺寸分布
图2  不同Ti含量ODS合金的晶粒核平均取向差KAM图
图3  不同Ti含量ODS合金的TEM明场像和纳米氧化物尺寸分布
图4  0.2Ti合金内氧化物颗粒的HRTEM照片和相应的FFT衍射斑点
图5  0.8Ti合金内氧化物颗粒的HRTEM照片和相应的FFT衍射斑点
图6  1.5Ti合金内氧化物颗粒的HRTEM照片和相应的FFT衍射斑点
Fig.4ad1{2¯2¯2¯} / nmd2{400} / nmd3{22¯2¯} / nmα12α23α13
Measured0.28620.25520.2808123.88°53.60°69.43°
Y2Ti2O70.29120.25220.2912125.26°54.73°70.52°
Fig.4bd1{2¯1¯1¯} / nmd2{403} / nmd3{21¯2} / nmα12α23α13
Measured0.30030.21560.2646127.07°45.20°81.86°
Y2TiO50.29070.21290.2653127.53°46.36°81.16°
Fig.4cd1{4¯2¯2¯} / nmd2{1¯1¯2} / nmd3{5¯3¯0} / nmα12α23α13
Measured0.23930.43110.185881.89°54.16°24.73°
Y2O30.23630.43270.181780.40°55.93°24.46°
表1  图4中氧化物颗粒晶面间距(d)和角度(α)的测量值和理论值
Fig.5ad1{4¯00} / nmd2{22¯2¯} / nmd3{2¯2¯2¯} / nmα12α23α13
Measured0.25780.28030.2819125.57°70.34°54.32°
Y2Ti2O70.25220.29120.2912125.26°70.52°54.73°
Fig.5bd1{4¯1¯1¯} / nmd2{012¯} / nmd3{4¯03¯} / nmα12α23α13
Measured0.20580.30010.1980110.74°71.12°39.61°
Y2TiO50.20830.30910.2029111.63°71.81°39.82°
表2  图5中氧化物颗粒晶面间距(d)和角度(α)的测量值和理论值
Fig.6ad1{2¯2¯2¯} / nmd2{400} / nmd3{22¯2¯} / nmα12α23α13
Measured0.30700.25410.2964126.27°53.65°69.61°
Y2Ti2O70.29120.25220.2912125.26°54.73°70.52°
Fig.6bd1{2¯1¯2¯} / nmd2{2¯21} / nmd3{4¯11¯} / nmα12α23α13
Measured0.26900.17210.2135123.52°38.99°84.53°
Y2TiO50.26530.17210.2083124.68°40.21°84.46°
Fig.6cd1{1¯00} / nmd2{001¯} / nmd3{1¯01¯} / nmα12α23α13
Measured0.45920.28920.257689.55°33.34°56.77°
TiO20.45940.29590.248790.00°32.78°57.21°
表3  图6中氧化物颗粒晶面间距(d)和角度(α)的测量值和理论值
AlloysY2TiO5Y2Ti2O7Y2O3TiO2
0.2Ti61.1%16.6%22.3%0
0.8Ti35.0%65.0%00
1.5Ti14.2%76.3%09.5%
表4  三种合金中氧化物粒子的种类和数量占比
图7  ODS合金的显微硬度
图8  不同Ti含量奥氏体ODS钢中氧化物生成的示意图
AlloyTypes of oxideδ / %rst / J·m-2
0.2TiY2Ti2O75.10.42
Y2TiO54.20.36
Y2O310.60.71
0.8TiY2Ti2O75.60.45
Y2TiO50.20.02
1.5TiY2Ti2O75.50.44
Y2TiO53.90.34
TiO2--
表5  3种合金中氧化物颗粒的δ和rst值
[1] Oka H, Watanabe M, Kinoshita H, et al. In situ observation of damage structure in ODS austenitic steel during electron irradiation [J]. J. Nucl. Mater., 2011, 417(1-3): 279
[2] Velikodnyi A N, Voyevodin V N, Kalchenko A S, et al. Impact of nano-oxides and injected gas on swelling and hardening of 18Cr10NiTi stainless steel during ion irradiation [J]. J. Nucl. Mater., 2022, 565: 153666
[3] Zhao Q, Yu L M, Liu Y C, et al. Morphology and structure evolution of Y2O3 nanoparticles in ODS steel powders during mechanical alloying and annealing [J]. Adv. Powder Technol., 2015, 26: 1578
[4] Ukai S, Harada M, Okada H, et al. Alloying design of oxide dispersion strengthened ferritic steel for long life FBRs core materials [J]. J. Nucl. Mater., 1993, 204: 65
[5] Kim I S, Choi B Y, Kang C Y, et al. Effect of Ti and W on the mechanical properties and microstructure of 12%Cr base mechanical-alloyed nano-sized ODS ferritic alloys [J]. ISIJ Int., 2003, 43: 1640
[6] Oksiuta Z, Baluc N L. Role of Cr and Ti contents on the microstructure and mechanical properties of ODS ferritic steels [J]. Adv. Mater. Res., 2008, 59: 308
[7] He P, Klimenkov M, Lindau R, et al. Characterization of precipitates in nano structured 14%Cr ODS alloys for fusion application [J]. J. Nucl. Mater., 2012, 428: 131
[8] Fan L L, Xiong Y K, Zeng Y, et al. The strength-ductility synergy of magnesium matrix nanocomposite achieved by a dual-heterostructure [J]. J. Mater. Sci. Technol., 2025, 215: 296
[9] Wang M, Sun H Y, Zou L, et al. Structural evolution of oxide dispersion strengthened austenitic powders during mechanical alloying and subsequent consolidation [J]. Powder Technol., 2015, 272: 309
[10] Ratti M, Leuvrey D, Mathon M H, et al. Influence of titanium on nano-cluster (Y, Ti, O) stability in ODS ferritic materials [J]. J. Nucl. Mater., 2009, 386-388: 540
[11] Zhang J R, Li Y F, Bao F Y, et al. Study on the formation mechanism of Y-Ti-O oxides during mechanical milling and annealing treatment [J]. Adv. Powder Technol., 2021, 32(2): 582
[12] Peng Y Y, Yu L M, Liu Y C, et al. Microstructures and tensile properties of an austenitic ODS heat resistance steel [J]. Mater. Sci. Eng., 2019, 767A: 138419
[13] Singh R, Prakash U, Kumar D, et al. Nano oxide particles in 18Cr oxide dispersion strengthened (ODS) steels with high yttria contents [J]. Mater. Charact., 2022, 189: 111936
[14] Courtin L, Urvoy S, Bossu D, et al. Comparison of 15Cr-15Ni austenitic steel cladding tubes obtained by HPTR Cold Pilgering or by cold drawing [J]. Key Eng. Mater., 2015, 651-653: 38
[15] Zhao R L, Jia H D, Yin C X, et al. Effects of cold rolling and heat treatment on microstructure and mechanical properties of 15Cr-15Ni ODS austenitic steel [J]. Mater. Today Commun., 2023, 37: 106941
[16] Yan F Z, Li J, Xiong L Y, et al. Effect of explosive compaction on microstructure of ODS FeCrAl alloy fabricated by oxidation method [J]. Mater. Res. Express, 2021, 8: 046504
[17] Chen C L, Zeng Y. Influence of Ti content on synthesis and characteristics of W-Ti ODS alloy [J]. J. Nucl. Mater., 2016, 469: 1
[18] London A J, Santra S, Amirthapandian S, et al. Effect of Ti and Cr on dispersion, structure and composition of oxide nano-particles in model ODS alloys [J]. Acta Mater., 2015, 97: 223
[19] Ukai S, Ohtsuka S. Nano-mesoscopic structure control in 9Cr-ODS ferritic steels [J]. Energy Mater., 2007, 2: 26
[20] Chinnappan R. Thermodynamic stability of oxide phases of Fe-Cr based ODS steels via quantum mechanical calculations [J]. Calphad, 2014, 45: 188
[21] Fu C L, Krčmar M, Painter G S, et al. Vacancy mechanism of high oxygen solubility and nucleation of stable oxygen-enriched clusters in Fe [J]. Phys. Rev. Lett., 2007, 99: 225502
[22] Mao X D, Oh K H, Kang S H, et al. On the coherency of Y2Ti2O7 particles with austenitic matrix of oxide dispersion strengthened steel [J]. Acta Mater., 2015, 89: 141
[23] Oono N, Tang Q X, Ukai S. Oxide particle refinement in Ni-based ODS alloy [J]. Mater. Sci. Eng., 2016, 649A: 250
[24] Mao X D, Kang S H, Kim T K, et al. Microstructure and mechanical properties of ultrafine-grained austenitic oxide dispersion strengthened steel [J]. Metall. Mater. Trans., 2016, 47A(11): 5334
[25] Tang Q X, Hoshino T, Ukai S, et al. Refinement of oxide particles by addition of Hf in Ni-0.5 mass%Al-1 mass%Y2O3 alloys [J]. Mater. Trans., 2010, 51(11): 2019
[26] Yang T X, Dou P, Li Z X, et al. Effects of Hf and/or Ti addition on the morphology, crystal, and metal/oxide interface structures of nanoparticles in FeCrAl-ODS steels [J]. Vacuum, 2024, 228: 113507
[1] 代宇航, 王月苗, 白英伯, 张瑞, 张伟红, 周子荐, 陶稀鹏, 崔传勇. GH4151高强镍基高温合金的热压缩变形[J]. 材料研究学报, 2026, 40(3): 169-178.
[2] 王权, 李一磊, 庞建超, 高崇, 姚迪, 张辉, 李守新, 张哲峰. 奥氏体不锈钢的显微硬度与拉伸性能的关系[J]. 材料研究学报, 2026, 40(3): 188-200.
[3] 刘俏君, 周键, 张航飞, 黄魁. PPy-GO共沉积改性阴离子交换膜的制备和性能[J]. 材料研究学报, 2026, 40(3): 225-233.
[4] 魏佳雨, 王敬忠, 翟亚中, 朱瑞, 车洪艳. 制粉工艺对新型镍基ODS合金组织和性能的影响[J]. 材料研究学报, 2026, 40(1): 48-58.
[5] 段玉, 王倩, 刘宏臣, 车远军, 石磊, 白慧娟. 油页岩灰基磁性分子筛的制备及其对亚甲基蓝的吸附性能[J]. 材料研究学报, 2025, 39(6): 463-473.
[6] 钟伟杰, 焦东玲, 刘仲武, 刘娜, 许文勇, 李周, 张国庆. 热等静压态镍基高温合金的高温氧化[J]. 材料研究学报, 2025, 39(3): 172-184.
[7] 胡彭钦, 王栋, 卢玉章, 张健. 热工艺对一种镍基单晶高温合金蠕变性能的影响[J]. 材料研究学报, 2025, 39(3): 161-171.
[8] 臧涛, 杨朋飞, 赵元, 高英, 鄂世举, 刘洋, 齐山贺, 张烨, 张嘉振. 热等静压SLM Ti-6Al-4V合金的缺口敏感性[J]. 材料研究学报, 2025, 39(10): 791-800.
[9] 韩珩, 李洪峤, 李鹏, 马国政, 郭伟玲, 刘明. 冷喷涂温度对Ni-Ti3AlC2复合涂层摩擦学性能的影响[J]. 材料研究学报, 2025, 39(1): 44-54.
[10] 尹一峰, 卢正冠, 徐磊, 吴杰. GH4099合金粉末的热等静压成形和薄壁筒体的制造[J]. 材料研究学报, 2024, 38(9): 669-679.
[11] 李沅沅, 梁健, 熊自柳, 苗斌, 田秀刚, 齐建军, 郑士建. 新型热镀锌双相钢的合金成分对界面层和镀层结构的影响[J]. 材料研究学报, 2024, 38(6): 446-452.
[12] 王俊, 王炫力, 刘爽, 宋蕊, 宋希文. Mn掺杂对(Y0.4Er0.6)3Al5O12 热障涂层材料的微观结构和导热性能的影响[J]. 材料研究学报, 2024, 38(6): 463-470.
[13] 赵勇, 刘腾远, 贾春妮, 杨朕聃, 陈响军, 王培, 李殿中. 冷拉拔钢丝横截面应变不均匀性的晶体塑性研究[J]. 材料研究学报, 2024, 38(2): 81-91.
[14] 张泽疆, 李新梅. 激光熔覆CoCrFeNiSi x 高熵合金涂层的耐磨和耐蚀性能[J]. 材料研究学报, 2024, 38(10): 741-750.
[15] 文锋, 张东勋, 王韡, 滕心跃, 楚鑫新. 316L不锈钢表面Fe-Al渗层的制备及其机理[J]. 材料研究学报, 2024, 38(10): 759-767.