Stability and corrosion behavior of AlO<sub><i>x</i></sub> coating on T91 steel and SIMP steel in static liquid Pb-Bi eutectic at 600 ℃

Liao Qing; Li Bing-Sheng; Ge Fang-Fang; Zhang Hong-Peng; Shen Tie-Long; Mao Xue-Li; Wang Ren-Da; Sheng Yan-Bin; Chang Hai-Long; Wang Zhi-Guang; Xu Shuai; Chen Li-Ming; He Xiao-Xun

doi:10.7498/aps.71.20220356

Abstract

Ferritic/martensitic steels, such as T91 steel and SIMP steel, are chosen as the main candidates of structural materials for the Generation IV lead-cooled fast reactors and accelerator driven system. However, the compatibility between container steel and liquid Pb-Bi eutectic (LBE) at high temperature limits their applications. The corrosion of ferritic/martensitic steels is serious in LBE at 600 ℃. In order to avoid corroding the ferritic/martensitic steels in LBE, it is proposed to coat AlO_x (x < 1.5) on the steel surface. The AlO_x coating is conducted on T91 steel and SIMP steel by magnetron sputtering. In this exploratory work, the corrosion results of AlO_x coating steel are compared with the corrosion results of the uncoated steel in LBE with a saturated oxygen concentration at 600 ℃ for 300 h and 700 h. The results show that the AlO_x coating can effectively prevent the iron chromium and oxygen from diffusing, so the oxide scale of the coated steel is thinner than that of the uncoated steel. However, the coating cracks after 700 h corrosion in LBE. Meanwhile, T91 steel and SIMP steel also suffer serious oxidative corrosion, indicating that the coating can protect the substrate from being corroded by 600 ℃ static LBE in a short time. However, the coating cannot keep stable for a long time in LBE at 600 ℃. This may be due to the weak film base bonding force of AlO_x coating prepared under the experimental conditions, or a large number of metal aluminum and structural defects existing in AlO_x coating. It is needed to further study the stability of AlO_x coating in LBE at elevated temperature.

Keywords:

Authors and contacts

1.
State Key Laboratory for Environment-friendly Energy Materials, Southwest University of Science and Technology, Mianyang 621010, China
2.
Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China
3.
Institute of Modern Physics, Chinese Academy of Sciences, Lanzhou 730000, China
4.
School of science, Southwest University of Science and Technology, Mianyang 621010, China
5.
School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621010, China

Corresponding author: Li Bing-Sheng, libingshengmvp@163.com

Funds: Project supported by the National Nature Science Foundation of China (Grant Nos. U1832133, 12075194) and the Scientific Research Fundation of the Science and Technology Department of Sichuan Province, China (Grant No. 2020ZYD055).

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References

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[2]	Sobolev V 2007 J. Nucl. Mater. 362 235 Google Scholar
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[5]	Xu Y C, Zhang Y G, Li X Y, Liu W, Li D D, Liu C S, Pan B C, Wang Z G 2017 Corros. Sci. 118 1 Google Scholar
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[13]	Deloffre P, Balbaud-Célérier F, Terlain A 2004 J. Nucl. Mater. 335 180 Google Scholar
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[20]	Heinzel A, Kondo M, Takahashi M 2006 J. Nucl. Mater. 350 264 Google Scholar
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[24]	Weisenburger A, Jianu A, Doyle S, Bruns M, Fetzer R, Heinzel A, Del Giacco M, An W, Müller G 2013 J. Nucl. Mater 437 282 Google Scholar
[25]	Ferré G, Ormellese M, Fonzo F D, Beghi M G 2013 Corros. Sci. 77 375 Google Scholar
[26]	Sordo F, Abánades A, Lafuente A, Martínez-Val J M, Perlado M 2009 Nucl. Eng. Des. 239 2573 Google Scholar
[27]	Borgstedt H U, Frees G 1995 Liquid Metal Systems. (New York: Springer) p339
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[35]	Comstock M 2009 J. Nucl. Mater. 382 272 Google Scholar
[36]	Tan L, Machut M T, Sridharan K 2007 J. Nucl. Mater. 371 161 Google Scholar
[37]	Li B S, Liao Q, Zhang H P, Shen T L, Ge F F, Nabil D 2021 Corros. Sci. 187 109477 Google Scholar
[38]	Zhang L L, Yan W, Shi Q Q, Li Y F, Shen Y Y, Yang K 2020 Corros. Sci. 167 108519 Google Scholar
[39]	Liu J, Yan W, Sha W, Wang W, Shan Y Y, Yang K 2016 J. Nucl. Mater. 473 189 Google Scholar
[40]	Li Y, Wang S, Sun P, Xu D, Ren M, Guo Y, Lin G 2017 Corros. Sci. 128 241 Google Scholar
[41]	Shi Q, Liu J, Luan H, Yang Z, Wang W, Yan W, Shan Y, Yang K 2015 J. Nucl. Mater. 457 135 Google Scholar
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[44]	Bian L Z, Chen Z Y, Wang L J, Li F S, Chou K C 2017 J. Iron. Steel. Res. Int. 24 77 Google Scholar
[45]	Huntz A M, Maréchal L, Lesage B, Molins R 2006 Appl. Surf. Sci. 252 7781 Google Scholar
[46]	Melander A 1997 Int. J. Fatigue 19 13 Google Scholar
[47]	Wang Q S, Wang W Q, Shi Z M 2018 E. Science. 113 012146 Google Scholar
[48]	Echsler H, Martinez E A, Singheiser L, Quadakkers W J 2004 Mater. Sci. Eng. A 384 1 Google Scholar
[49]	Hayashi H, Watanabe M, Inaba H 2000 Thermochim Acta. 359 77 Google Scholar
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Cited By

图 1 腐蚀实验设备的简单示意图

Figure 1. A simple schematic diagram of the corrosion test equipment.

DownLoad: Full-Size Img PowerPoint

图 2 简化的Ellingham图, 铁、铅、铬和铝氧化物的热力学数据见文献[8]

Figure 2. Experimental condition of thermodynamics in a simplified Ellingham diagram. Thermodynamic data for Fe, Pb, Cr and Al oxides are obtained in Ref. [8].

DownLoad: Full-Size Img PowerPoint

图 3 T91钢和SIMP钢在600 ℃ LBE中暴露300 h和700 h后的X射线衍射图　(a) T91钢; (b) SIMP钢

Figure 3. X-ray diffraction patterns of T91 steel and SIMP steel after exposing in oxygen-saturated static liquid LBE at 600 ℃ for 300 h and 700 h: (a) T91 steel; (b) SIMP.

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图 4 T91钢和SIMP钢在600 ℃的LBE中腐蚀300 h和700 h后的表面SEM图　 (a) LBE中腐蚀300 h后无涂层的T91钢表面; (b) LBE中腐蚀300 h后有涂层的T91钢表面; (c) LBE中腐蚀300 h后无涂层的SIMP钢表面; (d) LBE中腐蚀300 h后有涂层的SIMP钢表面; (e) LBE中腐蚀700 h后无涂层的T91钢表面; (f) LBE中腐蚀700 h后有涂层的T91钢表面; (g) LBE中腐蚀700 h后无涂层的SIMP钢表面; (h) LBE中腐蚀700 h后无涂层的SIMP钢表面

Figure 4. SEM images showing the surface morphology of SIMP and T91 steels after 300 h and 700 h corrosion in LBE at 600 ℃: (a) The uncoated surface of T91 steel in LBE for 300 h; (b) the coated surface of T91 steel in LBE for 300 h; (c) the uncoated surface of SIMP steel in LBE for 300 h; (d) the coated surface of SIMP steel in LBE for 300 h; (e) the uncoated surface of T91 steel in LBE for 700 h; (f) the coated surface of T91 steel in LBE for 700 h; (g) the uncoated surface of SIMP steel in LBE for 700 h; (h) the coated surface of SIMP steel in LBE for 700 h.

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图 5 在600 ℃的LBE中腐蚀300 h后SIMP钢涂层表面的SEM显微照片和表框区域Al, O, Cr和Fe分布图

Figure 5. SEM micrograph of the coated surface of SIMP steel after 300 h corrosion in LBE at 600 ℃ and the elemental mapping images of Al, O, Cr and Fe.

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图 6 涂层T91钢和SIMP钢在600 ℃的 LBE中腐蚀300 h后表面扫描电子显微镜显微照片　(a) T91钢; (b) SIMP钢

Figure 6. SEM micrograph of the coated surface of T91 and SIMP steels after 300 h corrosion in LBE at 600 ℃: (a) T91 steel; (b) SIMP steel

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图 7 在600 ℃的LBE中腐蚀300 h后T91钢和SIMP钢的横截面SEM图像和EDS线性分析(扫描方向从左到右)　(a), (b)涂层T91钢; (c), (d)无涂层T91钢; (e), (f)涂层SIMP钢; (g), (h)无涂层SIMP钢

Figure 7. Cross-sectional SEM images and EDS linear analysis of T91 and SIMP steels after 300 h corrosion in LBE at 600 ℃: (a), (b) The coated T91; (c), (d) the uncoated T91; (e), (f) the coated SIMP; (g), (h) the uncoated SIMP.

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图 8 在600 ℃的LBE中腐蚀LBE中腐蚀300 h后T91钢和SIMP钢的SEM 图和EDS图谱　(a)涂层T91钢; (b)涂层SIMP钢

Figure 8. Cross-sectional SEM image and EDS mapping of T91 and SIMP steels after 300 h corrosion in LBE at 600 ℃ : (a) The coated T91 steel; (b) coated SIMP steel.

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图 9 T91钢和SIMP钢在600℃的LBE中腐蚀700 h后的横截面SEM图像和EDS线性分析(扫描方向从左到右)　(a), (b)涂层T91钢; (c), (d)无涂层T91钢; (e), (f)涂层SIMP钢; (g), (h)无涂层SIMP钢.

Figure 9. Cross-sectional SEM images and EDS linear analysis of T91 and SIMP steels after 700 h corrosion in LBE at 600 ℃: (a), (b) The coated T91; (c), (d) the uncoated T91; (e), (f) the coated SIMP; (g), (h) the uncoated SIMP.

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表 1 研究钢材的化学成分(质量分数)

Table 1. Chemical compositions of the studied steels (mass fraction%)

元素	Fe	Cr	Ni	Mo	V	Si	C	Nb	N	Ta	W
T91	Bal	8.50	0.25	0.95	0.19	0.20	0.10	0.067	0.05	—	—
SIMP	Bal	10.50	—	—	0.20	1.40	0.20	0.01	—	0.15	1.50

DownLoad: CSV

表 2 磁控溅射制备AlO_x薄膜的典型工艺参数(1 sccm = 1 mL/min)

Table 2. Typical process parameters of the AlO_x films prepared by magnetron sputtering

靶功率/W	频率 /kHz	O₂ 流量/sccm	氩气流量/sccm	靶温度/℃	沉积速率/(nm·min^–1)
400	350	8.6	32	25	9

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表 3 T91钢和SIMP钢在600 ℃静态LBE下表面氧化物在图4标记位置的EDS点分析

Table 3. EDS analyses of the surface oxides of T91 and SIMP steel exposed to static LBE at 600 ℃ in Fig. 4.

原子分数/%	元素
原子分数/%	Fe	Cr	O	Al	Pb	Si
Point A	43.89	—	55.12	—	0.34	0.65
Point B	0.89	—	61.9	36.4	—	0.81
Point C	42.7	—	54.37	—	0.38	2.55
Point D	3.01	—	58.63	34.6	—	3.76
Point E	44.21	—	54.30	—	0.88	0.61
Point F	41.17	—	58.26	—	—	0.57
Point G	40.59	—	55.23	—	0.60	3.58
Point H	32.51	—	63.80	—	—	3.69

DownLoad: CSV

map

[1]	Sar F, Mhiaoui S, Gasser J G 2007 J. Non. Cryst. Solids. 353 3622 Google Scholar
[2]	Sobolev V 2007 J. Nucl. Mater. 362 235 Google Scholar
[3]	Zhang J 2014 Adv. Eng. Mater. 16 349 Google Scholar
[4]	Zhang J, Ning L 2008 J. Nucl. Mater. 373 351 Google Scholar
[5]	Xu Y C, Zhang Y G, Li X Y, Liu W, Li D D, Liu C S, Pan B C, Wang Z G 2017 Corros. Sci. 118 1 Google Scholar
[6]	Barbier F, Rusanov A 2001 J. Nucl. Mater. 296 231 Google Scholar
[7]	Martinelli L, Jean-Louis C, Fanny B C 2011 Nucl. Eng. Des. 241 1288 Google Scholar
[8]	Concetta F 2015 Handbook on Lead-bismuth Eutectic Alloy and Lead Properties, Materials Compatibility, Thermal-hydraulics and Technologies (2015 Edition-Introduction) (OECD Nuclear Energy Agency)
[9]	Zhang J 2009 Corros. Sci. 51 1207 Google Scholar
[10]	Takaya S, Furukawa T, Müller G, Heinzel A, Jianu A, Weisenburger A, Aoto K, Inoue M, Okuda T, Abe F, Ohnuki S, Fujisawa T, Kimura A 2012 J. Nucl. Mater. 428 125 Google Scholar
[11]	Srinivasan P B, Kumar M 2009 Mater. Chem. Phys. 115 179 Google Scholar
[12]	Müller G, Schumacher G, Zimmermann F 2000 J. Nucl. Mater. 278 85 Google Scholar
[13]	Deloffre P, Balbaud-Célérier F, Terlain A 2004 J. Nucl. Mater. 335 180 Google Scholar
[14]	Weisenburger A, Heinzel A, Müller G, Muscher H, Rousanov A 2008 J. Nucl. Mater. 376 274 Google Scholar
[15]	Fetzer R, Weisenburger A, Jianu A, Müller G 2012 Corros. Sci. 55 213 Google Scholar
[16]	Short M P, Ballinger R G, Hänninen H E 2013 J. Nucl. Mater. 434 259 Google Scholar
[17]	Hosemann P, Thau H T, Johnson A L, Maloy S A, Li N 2008 J. Nucl. Mater. 373 246 Google Scholar
[18]	Takaya S, Furukawa T, Aoto K, Müller G, Weisenburger A, Heinzel A, Inoue M, Okuda T, Abe F, Ohnuki S, Fujisawa T and Kimura A 2009 J. Nucl. Mater. 386–388 507 Google Scholar
[19]	Takaya S, Furukawa T, Inoue M, Fujisawa T, Okuda T, Abe F, Ohnuki S, Kimura A 2010 J. Nucl. Mater. 398 132 Google Scholar
[20]	Heinzel A, Kondo M, Takahashi M 2006 J. Nucl. Mater. 350 264 Google Scholar
[21]	Kurata Y, Futakawa M, Saito S 2004 J. Nucl. Mater. 335 501 Google Scholar
[22]	Ferré F G, Mairov A, Iadicicco D, Vanazzi M, Bassini S, Utili M, Tarantino M, Bragaglia M, Lamastra F R, Nanni F, Ceseracciu L, Serruys Y, Trocellier P, Beck L, Sridharan K, Beghi M G , Di Fonzo F 2017 Corros. Sci. 124 80 Google Scholar
[23]	Glasbrenner H, Gröschel F 2006 J. Nucl. Mater. 356 213 Google Scholar
[24]	Weisenburger A, Jianu A, Doyle S, Bruns M, Fetzer R, Heinzel A, Del Giacco M, An W, Müller G 2013 J. Nucl. Mater 437 282 Google Scholar
[25]	Ferré G, Ormellese M, Fonzo F D, Beghi M G 2013 Corros. Sci. 77 375 Google Scholar
[26]	Sordo F, Abánades A, Lafuente A, Martínez-Val J M, Perlado M 2009 Nucl. Eng. Des. 239 2573 Google Scholar
[27]	Borgstedt H U, Frees G 1995 Liquid Metal Systems. (New York: Springer) p339
[28]	Ellingham H J T 1994 J. Soc. Chem. Ind. 63 125
[29]	Yeliseyeva O, Tsisar V, Zhou Z 2013 J. Nucl. Mater. 442 434 Google Scholar
[30]	Weisenburger A, Schroer C, Jianu A, Heinzel A, Konys J, Steiner H, Müller G, Fazio C, Gessi A, Babayan S, Kobzova A, Martinelli L, Ginestar K, Balbaud-Célerier F, Martín-Muñoz F J, Soler Crespo L 2011 J. Nucl. Mater. 415 260 Google Scholar
[31]	Weisenburger A, Mansani L, Schumacher G, Müller G 2014 Nucl. Eng. Des. 273 584 Google Scholar
[32]	Martinelli L, Balbaud-Célérier F, Terlain A, Bosonnet S, Picard G, Santarini G 2008 Corros. Sci. 50 2537 Google Scholar
[33]	Martinelli L, Balbaud-Célérier F, Picard G, Santarini G 2008 Corros. Sci. 50 2549 Google Scholar
[34]	Miorin E, Montagner F, Zin V, Giuranno D, Deambrosis S M 2019 Surf. Coat. Technol. 377 124890 Google Scholar
[35]	Comstock M 2009 J. Nucl. Mater. 382 272 Google Scholar
[36]	Tan L, Machut M T, Sridharan K 2007 J. Nucl. Mater. 371 161 Google Scholar
[37]	Li B S, Liao Q, Zhang H P, Shen T L, Ge F F, Nabil D 2021 Corros. Sci. 187 109477 Google Scholar
[38]	Zhang L L, Yan W, Shi Q Q, Li Y F, Shen Y Y, Yang K 2020 Corros. Sci. 167 108519 Google Scholar
[39]	Liu J, Yan W, Sha W, Wang W, Shan Y Y, Yang K 2016 J. Nucl. Mater. 473 189 Google Scholar
[40]	Li Y, Wang S, Sun P, Xu D, Ren M, Guo Y, Lin G 2017 Corros. Sci. 128 241 Google Scholar
[41]	Shi Q, Liu J, Luan H, Yang Z, Wang W, Yan W, Shan Y, Yang K 2015 J. Nucl. Mater. 457 135 Google Scholar
[42]	Behnamian Y, Mostafaei A, Kohandehghan A, Amirkhiz B S, Serate D, Sun Y, Liu S, Aghaie E, Zeng Y, Chmielus M, Zheng W, Guzonas D 2016 Corros. Sci. 106 188 Google Scholar
[43]	Martinelli L, Balbaud-Célérier F, Terlian A, Delpech S, Santarini G, Favergeon J, Moulin G, Tabarant M, Picard G 2008 Corros. Sci. 50 2523 Google Scholar
[44]	Bian L Z, Chen Z Y, Wang L J, Li F S, Chou K C 2017 J. Iron. Steel. Res. Int. 24 77 Google Scholar
[45]	Huntz A M, Maréchal L, Lesage B, Molins R 2006 Appl. Surf. Sci. 252 7781 Google Scholar
[46]	Melander A 1997 Int. J. Fatigue 19 13 Google Scholar
[47]	Wang Q S, Wang W Q, Shi Z M 2018 E. Science. 113 012146 Google Scholar
[48]	Echsler H, Martinez E A, Singheiser L, Quadakkers W J 2004 Mater. Sci. Eng. A 384 1 Google Scholar
[49]	Hayashi H, Watanabe M, Inaba H 2000 Thermochim Acta. 359 77 Google Scholar
[50]	Mavko G, Mukerji T, Dvorkin J 2009 The Rock Physics Handbook: Elasticity and Hooke's law 2 21 Google Scholar

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Vol. 71, Issue 15 - 2022-08-05

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Stability and corrosion behavior of AlO_x coating on T91 steel and SIMP steel in static liquid Pb-Bi eutectic at 600 ℃

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Stability and corrosion behavior of AlOx coating on T91 steel and SIMP steel in static liquid Pb-Bi eutectic at 600 ℃

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Stability and corrosion behavior of AlO_x coating on T91 steel and SIMP steel in static liquid Pb-Bi eutectic at 600 ℃