Effect of Ageing Treatment at 650 ℃ on Microstructure and Properties of 9Cr-ODS Steel

doi:10.11900/0412.1961.2019.00445

Acta Metall Sin

2020, Vol. 56

Issue (8): 1075-1083 DOI: 10.11900/0412.1961.2019.00445

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Effect of Ageing Treatment at 650 ℃ on Microstructure and Properties of 9Cr-ODS Steel

PENG Yanyan, YU Liming(

), LIU Yongchang, MA Zongqing, LIU Chenxi, LI Chong, LI Huijun

Tianjin Key Lab of Composite and Functional Materials, School of Materials Science and Engineering, Tianjin University, Tianjin 300072, China

Cite this article:

PENG Yanyan, YU Liming, LIU Yongchang, MA Zongqing, LIU Chenxi, LI Chong, LI Huijun. Effect of Ageing Treatment at 650 ℃ on Microstructure and Properties of 9Cr-ODS Steel. Acta Metall Sin, 2020, 56(8): 1075-1083.

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Abstract

Oxide dispersion strengthened (ODS) steel has excellent high-temperature performance and corrosion resistance. It has broad application prospect and development space in the key field of high temperature structural materials for nuclear power. 9Cr-ODS steel has become one of the most promising candidate materials in advanced nuclear reactors because of its excellent high temperature mechanical properties and radiation resistance. In this work, 9Cr-ODS steel was designed and prepared by powder metallurgy process. The as-hot isostatically pressed (HIPed) microstructure of the steel was studied and analyzed, including matrix grain distribution characteristics, micron-scale large size precipitated phase, and nanoscale oxide particles. In addition, the high temperature microstructure thermal stability of 9Cr-ODS steel aged at 650 ℃ for different time was researched by means of XRD, SEM, TEM and hardness test, and the microstructure change of matrix and hardness properties were analyzed. Based on the contrast analysis of the matrix microstructure and hardness properties, the hardness change of the austenitic ODS steel at high temperature was obtained. The results showed that the original as-HIPed microstructure of 9Cr-ODS steel is mainly composed of martensite lath and large amount of Y₂O₃. During ageing process, the lath martensite of 9Cr-ODS steel gradually coarsens and the number of dislocations decreases with ageing time increasing, and the Cr₂₃C₆ carbides begin to precipitate along the grain boundary and grow up. At the same time, the Laves phases with large size begin to precipitate in ageing and then grow with the increase of ageing time. Meanwhile, ageing treatment makes Y₂O₃ phase with larger size further grow, while Y₂O₃ phase with smaller size precipitate increase. This phenomenon can probably be associated with the dissolution of the fine particles induced from the particle coarsening, generally called the Ostwald-Ripening mechanism. The change of microhardness during ageing was related to the size of lath martensite and the number and density of the second phase precipitation, especially Cr₂₃C₆. The hardness test results show that the microhardness first decreases and then tends to be stable with the increase of ageing time.

Key words: 9Cr-ODS steel ageing thermal stability

Received: 24 December 2019

ZTFLH:

TG142.1

Fund: National Natural Science Foundation of China(51974199);National Natural Science Foundation of China(U1960204)

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	Yanyan PENG
	Liming YU
	Yongchang LIU
	Zongqing MA
	Chenxi LIU
	Chong LI
	Huijun LI

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https://www.ams.org.cn/EN/10.11900/0412.1961.2019.00445 OR https://www.ams.org.cn/EN/Y2020/V56/I8/1075

Fig.1 XRD spectra of 9Cr-ODS steel under different ageing time at 650 ℃

Fig.2 TEM bright-field images of 9Cr-ODS steel with different ageing time at 650 ℃
(a) 0 h (b) 200 h (c) 500 h (d) 1000 h (e) 2000 h (f) 4000 h

Fig.3 Statistical histogram of martensite laths size (a) and average size of laths (b) in 9Cr-ODS steel with different ageing time at 650 ℃

Fig.4 TEM Bright-field images of oxides with different ageing time at 650 ℃
(a) 0 h (b) 200 h (c) 500 h (d) 1000 h (e) 2000 h (f) 4000 h

Fig.5 TEM image (a) and EDS (b) of oxides in 9Cr-ODS steel (Inset shows the SAED pattern of oxides)

Fig.6 SAED pattern of matrix and Y₂O₃

Fig.7 Statistical histogram (a) and average size (b) of Y₂O₃ in 9Cr-ODS steel with different ageing time at 650 ℃

Fig.8 TEM bright-field images of carbides in 9Cr-ODS steel with different ageing time at 650 ℃
(a) 0 h (b) 200 h (c) 500 h (d) 1000 h (e) 2000 h (f) 4000 h

Fig.9 TEM image (a) and EDS (b) of carbides in 9Cr-ODS steel (Inset shows the SAED pattern of carbides)

Fig.10 TEM bright-field images of Lavesphases in 9Cr-ODS steel with different ageing time at 650 ℃
(a) 50 h (b) 200 h (c) 500 h (d) 1000 h (e) 2000 h

Fig.11 TEM image (a) and EDS (b) of Laves phases in 9Cr-ODS steel (Inset shows the SAED pattern of Laves phases)

Fig.12 Vickers hardness change of 9Cr-ODS steel during ageing at 650 ℃

[1]	Abram T, Ion S. Generation-IV nuclear power: A review of the state of the science [J]. Energy Policy, 2008, 36: 4323 doi: 10.1016/j.enpol.2008.09.059
[2]	Mansur L K, Rowcliffe A F, Nanstad P K, et al. Materials needs for fusion, Generation IV fission reactors and spallation neutron sources-similarities and differences [J]. J. Nucl. Mater., 2004, 329-333: 166 doi: 10.1016/j.jnucmat.2004.04.016
[3]	Xu M. The development of fast reactor technology, to ensure the sustainable development of nuclear energy [J]. China Nucl. Power, 2012, 5: 98
	(徐銤. 发展快堆技术, 保证核能可持续发展 [J]. 中国核电, 2012, 5: 98)
[4]	Bloom E E, Busby J T, Duty C E, et al. Critical questions in materials science and engineering for successful development of fusion power [J]. J. Nucl. Mater., 2007, 367-370: 1 doi: 10.1016/j.jnucmat.2007.02.007
[5]	Marques J G. Evolution of nuclear fission reactors: Third generation and beyond [J]. Energy Conv. Manag., 2010, 51: 1774 doi: 10.1016/j.enconman.2009.12.043
[6]	Zhang Z, Chen D L. Consideration of Orowan strengthening effect in particulate-reinforced metal matrix nanocomposites: A model for predicting their yield strength [J]. Scr. Mater., 2006, 54: 1321 doi: 10.1016/j.scriptamat.2005.12.017
[7]	Jiang Y, Smith J R, Odette G R. Formation of Y-Ti-O nanoclusters in nanostructured ferritic alloys: A first-principles study [J]. Phys. Rev., 2009, 79B: 064103
[8]	Hirata A, Fujita T, Wen Y R, et al. Atomic structure of nanoclusters in oxide-dispersion-strengthened steels [J]. Nat. Mater., 2011, 10: 922 doi: 10.1038/nmat3150 pmid: 22019943
[9]	Zhao Q, Yu L M, Liu Y C, et al. Microstructure and tensile properties of a 14Cr ODS ferritic steel [J]. Mater. Sci. Eng., 2017, A680: 347
[10]	Ijiri Y, Oono N, Ukai S, et al. Oxide particle-dislocation interaction in 9Cr-ODS steel [J]. Nucl. Mater. Energy, 2016, 9: 378
[11]	Zhang L, Ukai S, Hoshino T, et al. Y₂O₃ evolution and dispersion refinement in Co-base ODS alloys [J]. Acta Mater., 2009, 57: 3671 doi: 10.1016/j.actamat.2009.04.033
[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, A767: 138419
[13]	Peng Y Y. Study on precipitation behavior of strengthening phase and microstructure thermal stability of austenitic ODS steel [D]. Tianjin: Tianjin University, 2019
	(彭艳艳. 奥氏体ODS钢的强化相析出行为及其组织热稳定性研究 [D]. 天津: 天津大学, 2019)
[14]	Ren J, Yu L M, Liu Y C, et al. Effects of Zr addition on strengthening mechanisms of Al-alloyed high-Cr ODS steels [J]. Materials, 2018, 11: 118 doi: 10.3390/ma11010118
[15]	Dong H Q, Yu L M, Liu Y C, et al. Effect of hafnium addition on the microstructure and tensile properties of aluminum added high-Cr ODS steels [J]. J. Alloys Compd., 2017, 702: 538 doi: 10.1016/j.jallcom.2017.01.298
[16]	Muroga T, Nagasaka T, Li Y, et al. Fabrication and characterization of reference 9Cr and 12Cr-ODS low activation ferritic/martensitic steels [J]. Fusion Eng. Des., 2014, 89: 1717 doi: 10.1016/j.fusengdes.2014.01.010
[17]	Li Y F, Abe H, Li F, et al. Grain structural characterization of 9Cr-ODS steel aged at 973 K up to 10,000 h by electron backscatter diffraction [J]. J. Nucl. Mater., 2014, 455: 568 doi: 10.1016/j.jnucmat.2014.08.047
[18]	Yan P Y, Yu L M, Liu Y C, et al. Effects of Hf addition on the thermal stability of 16Cr-ODS steels at elevated aging temperatures [J]. J. Alloys Compd., 2018, 739: 368 doi: 10.1016/j.jallcom.2017.12.245
[19]	Li Y F, Nagasaka T, Muroga T, et al. High-temperature mechanical properties and microstructure of 9Cr oxide dispersion strengthened steel compared with RAFMs [J]. Fusion Eng. Des., 2011, 86: 2495 doi: 10.1016/j.fusengdes.2011.03.004
[20]	Zhou X S, Liu Y C, Yu L M, et al. Microstructure characteristic and mechanical property of transformable 9Cr-ODS steel fabricated by spark plasma sintering [J]. Mater. Des., 2017, 132: 158 doi: 10.1016/j.matdes.2017.06.063
[21]	Yamamoto M, Ukai S, Hayashi S, et al. Formation of residual ferrite in 9Cr-ODS ferritic steels [J]. Mater. Sci. Eng., 2010, A527: 4418
[22]	Ohtsuka S, Ukai S, Fujiwara M. Nano-mesoscopic structural control in 9Cr ODS ferritic/martensitic steels [J]. J. Nucl. Mater., 2006, 351: 241 doi: 10.1016/j.jnucmat.2006.02.006
[23]	Zhang G M. Study on strengthening mechanism and performance evaluation of 9Cr oxide dispersion strengthened steel [D]. Beijing: University of Science and Technology Beijing, 2016
	(张广明. 9Cr氧化物弥散强化的强化机理研究及性能评价 [D]. 北京: 北京科技大学, 2016)
[24]	Dong H Q, Yu L M, Liu Y C, et al. Enhancement of tensile properties due to microstructure optimization in ODS steels by zirconium addition [J]. Fusion Eng. Des., 2017, 125: 402 doi: 10.1016/j.fusengdes.2017.03.170
[25]	Abe F. Precipitate design for creep strengthening of 9% Cr tempered martensitic steel for ultra-supercritical power plants [J]. Sci. Technol. Adv. Mater., 2008, 9: 013002 doi: 10.1088/1468-6996/9/1/013002 pmid: 27877920
[26]	Mukhopadhyay D K. Development of oxide dispersion strengthened ferritic steels for fusion [J]. J. Nucl. Mater., 1998, 258-263: 1209 doi: 10.1016/S0022-3115(98)00188-3
[27]	Zhang L Y, Yu L M, Liu Y C, et al., Influence of Zr addition on the microstructures and mechanical properties of 14Cr ODS steels [J], Mater. Sci. Eng., 2017, A695:66
[28]	Bentley J, Hoelzer D T, Coffey D W, et al. EFTEM and spectrum imaging of mechanically alloyed oxide-dispersion-strengthened 12YWT and 14YWT ferritic steels [J]. Microsc. Microanal., 2004, 10(S02): 662
[29]	Sugino Y, Ukai S, Hayashi Q, et al. Directional recrystallization of ODS alloys by means of zone annealing [J]. J. Nucl. Mater., 2011, 417: 171 doi: 10.1016/j.jnucmat.2011.01.062
[30]	Ren J, Yu L M, Liu Y C, et al., Microstructure evolution and tensile properties of an Al added high-Cr ODS steel during thermal aging at 650 ℃ [J]. Fusion Eng. Des., 2020, 157: 111700 doi: 10.1016/j.fusengdes.2020.111700
[31]	Miller M K, Hoelzer D T, Kenik E A, et al. Stability of ferritic MA/ODS alloys at high temperatures [J]. Intermetallics, 2015, 13: 387 doi: 10.1016/j.intermet.2004.07.036
[32]	Huang J D，Mei J P，Yan J L. Microstructure degradation and properties evolution of T91 steel during aging[J]. Heat Treat. Met., 2016, 42(11): 45
	(黄金督, 梅建平, 晏井利等. T91钢时效过程中的组织老化和性能变化[J]. 金属热处理, 2016, 41(11): 45)
[33]	Ren J, Yu L M, Liu Y C, et al., Corrosion behavior of an Al added high-Cr ODS steel in supercritical water at 600 ℃ [J]. Appl. Sur. Sci., 2019, 480: 969 doi: 10.1016/j.apsusc.2019.03.019
[34]	Xie R, Lü Z, Lu C Y, et al. Characterization of nanosized precipitates in 9Cr-ODS steels by SAXS and TEM [J]. Acta Metall. Sin., 2016, 52: 1053 doi: 10.11900/0412.1961.2016.00164
	(谢锐, 吕铮, 卢晨阳等. 9Cr-ODS钢中纳米析出相的SAXS和TEM研究 [J]. 金属学报, 2016, 52: 1053) doi: 10.11900/0412.1961.2016.00164
[35]	Shigeharu U, Takeji K, Satoshi O. Production and properties of nano-scale oxide dispersion strengthened (ODS) 9Cr martensitic steel claddings [J]. ISIJ Int., 2003, 43: 2038 doi: 10.2355/isijinternational.43.2038
[36]	He J C, Wan F R. The research of nano-scale particles in the oxide dispersion strengthened steels [J]. J. Funct. Mater., 2014, 45: 17029
	(贺建超, 万发荣. ODS钢中纳米氧化物颗粒成分与结构研究 [J]. 功能材料, 2014, 45: 17029)
[37]	Zhang C H, Kimura A, Kasada R, et al. Characterization of the oxide particles in Al-added high-Cr ODS ferritic steels [J]. J. Nucl. Mater., 2011, 417: 221 doi: 10.1016/j.jnucmat.2010.12.063
[38]	Li B, Xu X W. Microstructure and mechanical properties of aged T/P92 steel [J]. Heat Treat. Met., 2014, 39(12): 110 doi: 10.13251/j.issn.0254-6051.2014.12.029
	(李斌, 徐晓伟. T/P92钢的时效组织与性能 [J]. 金属热处理, 2014, 39(12): 110) doi: 10.13251/j.issn.0254-6051.2014.12.029
[39]	Ma W J, Lu Q, Shi Q Q, et al. Structure stability of a newly designed martensitic heat-resistant steel [J]. Heat Treat. Met., 2017, 42(5): 27
	(马文杰, 卢奇, 石全强等. 新设计的马氏体耐热钢的组织稳定性 [J]. 金属热处理, 2017, 42(5): 27)
[40]	Hu P, Yan W, Shan Y Y, et al. Study on structural evolution and mechanical properties of high Cr ferritic heat-resistant steel in ageing process [J]. Guangdong Electr. Power, 2011, 24(11): 6
	(胡平, 严伟, 单以银等. 高Cr铁素体耐热钢时效过程中的组织演变与力学性能研究 [J]. 广东电力, 2011, 24(11): 6)

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