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Acta Metall Sin  2026, Vol. 62 Issue (8): 1385-1394    DOI: 10.11900/0412.1961.2024.00353
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Effect of Heat Treatment on Flame Retardant Property of GH4169 Alloy Fabricated by Selective Laser Melting
ZHOU Jiaxuan1,2, SI Hongli2, ZHANG Guilin2, ZHANG Shaohua2(), ZHANG Jian2(), TIAN Yanzhong1, PANG Xueyong1
1 School of Materials Science and Engineering, Northeastern University, Shenyang 110819, China
2 Shi -changxu Innovation Center for Advanced Materials, Institute of Metal Research, Chinese Academy of Sciences, Shenyang 110016, China
Cite this article: 

ZHOU Jiaxuan, SI Hongli, ZHANG Guilin, ZHANG Shaohua, ZHANG Jian, TIAN Yanzhong, PANG Xueyong. Effect of Heat Treatment on Flame Retardant Property of GH4169 Alloy Fabricated by Selective Laser Melting. Acta Metall Sin, 2026, 62(8): 1385-1394.

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Abstract  

With the advancement of high-thrust liquid rocket engine toward higher chamber pressure and specific impulse, the turbine pump system of the gas generator is being increasingly exposed to extreme high-temperature and high-pressure oxygen-enriched environments. This exacerbates the risk of metal-oxidation combustion failure of superalloy components. The production of high-performance and complex-structured superalloy parts via selective laser melting technology has emerged as a key research area in the manufacture of critical aerospace components. Therefore, the investigation of the oxygen-enriched combustion mechanism of high-temperature alloy materials fabricated using the selective laser melting technology is of great practical significance. This study investigated the effect of heat treatment on the flame retardant property of GH4169 alloy produced via selective laser melting using self-developed experimental equipment designed for oxygen-enriched combustion testing of metal materials. A high-speed camera was used to observe and record the combustion process. The microstructure and combustion morphology of the alloy were analyzed using OM, SEM, and EDS. The as-deposited sample exhibited a typical fish-scale molten pool morphology, with numerous low-melting-point Laves phases precipitating in the interdendritic regions and grain boundaries. Following heat treatment at 980 oC, most Laves phases dissolved, and needle-like and short rod-like δ-Ni3Nb phases precipitated at the grain boundaries and in the interdendritic regions. Upon increasing the solution temperature to 1080 oC, the volume fraction of precipitated phases was significantly reduced. Consequently, only a small number of nano-sized Laves particles were formed within the grains and a certain amount of blocky carbides were located at the grain boundaries. Combustion resistance testing revealed that the as-deposited sample exhibited the poorest resistance, whereas samples heat-treated at 1080 oC demonstrated the highest resistance. Further, microstructural analysis confirmed that the combustion behavior was closely related to the type and volume fraction of the precipitates within the matrix. Laves phases with high Nb content melted early in the combustion, thereby accelerating the reaction owing to the high combustion heat of Nb. The δ phases formed after heat treatment at 980 oC also promoted combustion. Thus, these findings suggest that eliminating the low-melting-point phases and controlling the types of precipitated phases are key strategies for enhancing the flame retardant properties of GH4169 alloy.

Key words:  metal combustion      GH4169 alloy      selective laser melting      precipitated phase      flame retardant property     
Received:  21 October 2024     
ZTFLH:  TG146.15  
Fund: National Natural Science Foundation of China(52150233);Key Research Program of Chinese Academy of Sciences(ZDRW-CN-2021-2-1)
Corresponding Authors:  ZHANG Shaohua, associate professor, Tel: (024)23748882, E-mail: zhangshaohua@imr.ac.cn; ZHANG Jian, professor, Tel: (024)23971196, E-mail: jianzhang@imr.ac.cn

URL: 

https://www.ams.org.cn/EN/10.11900/0412.1961.2024.00353     OR     https://www.ams.org.cn/EN/Y2026/V62/I8/1385

ElementMass fraction / %Hc / (kJ·mol-1)
Ni53.00240
Cr19.50565
Nb5.10967
Mo3.05751
Ti0.90912
Al0.90842
C0.05-
FeBal.364
Table 1  Chemical compositions of the processed GH4169 powder and heat of combustion of metal elements (Hc)
SampleSolution treatmentAge hardening
ASNoneNone
980SDA980 oC, 1 h (AC)720 oC, 8 h (FC, 50 oC·h-1) + 620 oC, 8 h (AC)
1080SDA1080 oC, 1 h (AC)720 oC, 8 h (FC, 50 oC·h-1) + 620 oC, 8 h (AC)
Table 2  Heat treatment schedule of GH4169 alloy fabricated by selective laser melting
Fig.1  Experimental setup in promoted ignition-combustion (PIC) test chamber (a), and combustion processes of the 1080SDA sample at an oxygen pressure of 5.0 MPa (b-k)
Fig.2  Low (a-c) and high (a1-c1) magnified SEM images of samples suffering different heat treatments (Insets in Figs.2b1 and c1 are the locally enlarged images of square regions showing γ'/γ" strengthening phases) (a, a1) AS (b, b1) 980SDA (c, c1) 1080SDA
Fig.3  DSC heating curves of samples suffering different heat treatments
Fig.4  Macroscopic morphologies of samples suffering different heat treatments after combustions at different oxygen pressures (Inset in Fig.4a shows the combustion zone)
Fig.5  Average combustion lengths (a) and average combustion rates (b) of samples suffering different heat treatments after combustion at different oxygen pressures
Fig.6  Cross sectional OM images of combustion zone of samples suffering different heat treatments after combustion at an oxygen pressure of 5.0 MPa (HAZ—heat affected zone)
Fig.7  Low (a-c) and locally high (d-f) magnified SEM images of the HAZ of samples suffering different heat treatments after combustion at an oxygen pressure of 5.0 MPa (a, d) AS (b, e) 980SDA (c, f) 1080SDA
Fig.8  OM (a-c) and SEM (d-f) images of the transition zone of samples suffering different heat treatments after combustion at an oxygen pressure of 5.0 MPa (Circles in Figs.8d-f show dendritic hole morphologies) (a, d) AS (b, e) 980SDA (c, f)1080SDA
Fig.9  SEM images (a-c) and EDS analysis results (a1-c1) of typical spherical oxides in the melting zone of samples suffering different heat treatments after combustion at an oxygen pressure of 5.0 MPa (a, a1) AS (b, b1) 980SDA (c, c1) 1080SDA
Fig.10  Low (a) and locally high (b) magnified SEM images of oxide morphology and corresponding EDS elemental distribution mappings of 1080SDA sample at the combustion front after combustion at an oxygen pressure of 5.0 MPa
[1] Huang J F, Zhao G P, Jiao L Y, et al. Combustion failure analysis of GH202 and GH586 superalloys for rocket engine [J]. J. Iron Steel Res., 2005, 17(3): 68
黄进峰, 赵光普, 焦兰英 等. 火箭发动机用合金GH202和GH586燃烧事故分析 [J]. 钢铁研究学报, 2005, 17(3): 68
[2] Harrison P L, Yoffe A D. The burning of metals [J]. Proc. Roy. Soc., 1961, 261A: 357
[3] Monroe R W, Bates C E, Pears C D. Metal combustion in high-pressure flowing oxygen [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres [C]. Phoenix: ASTM, 1983: 126
[4] Hill P R, Adamson D, Foland D H, et al. High temperature oxidation and ignition of metals [R]. Washington: National Advisory Committee for Aeronautics, 1956
[5] Benz F J, Shaw R C, Homa J M. Burn propagation rates of metals and alloys in gaseous oxygen [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres: Second Volume [C]. Philadelphia: ASTM, 1986: 135
[6] Wehr-Aukland A K, White J E, Cook K M. Failure analysis of an oxygen transfer hose flash fire [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres: 15th Volume [C]. Philadelphia: ASTM, 2021: 207
[7] Zabrenski J S, Werley B L, Slusser J W. Pressurized flammability limits of metals [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres: Fourth Volume [C]. Philadelphia: ASTM, 1989: 178
[8] Slusser J W, Miller K A. Selection of metals for gaseous oxygen service [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres [C]. Philadelphia: ASTM, 1983: 25
[9] Shao L, Xie G L, Zhang C, et al. Combustion of metals in oxygen-enriched atmospheres [J]. Metals, 2020, 10: 128
[10] Zawierucha R, McIlroy K M, Mazzarella R. Promoted ignition-combustion behavior of engineering alloys at elevated temperatures and pressures in oxygen gas mixtures [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres: Fourth Volume [C]. West Conshohocken: ASTM, 1991: 18
[11] Million J F, Samant A, Zawierucha R. Promoted ignition-combustion behavior of cobalt and nickel alloys in oxygen-enriched atmospheres [A]. Twelfth International Symposium on Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres [C]. Berlin: ASTM, 2009: 10
[12] Huang J F, Yu H Y, Li Y B, et al. Oxidation characteristic and mechanism of superalloys in oxygen-enriched atmosphere [J]. J. Iron Steel Res., 2009, 21(3): 51
黄进峰, 余红燕, 李永兵 等. 富氧气氛下高温合金氧化特征及机理 [J]. 钢铁研究学报, 2009, 21(3): 51
[13] Shi L F, Huang J F, Zhao G P, et al. Research on combustion characteristics and properties of superalloy in high-pressure and oxygen-enriched atmosphere [J]. Hot Working Technol., 2007, 36(4): 26
施立发, 黄进峰, 赵光普 等. 高压富氧下几种高温合金的燃烧特征和性能研究 [J]. 热加工工艺, 2007, 36(4): 26
[14] Wang H L, Huang J F, Lian Y, et al. Combustion behavior of GH4169 and GH4202 superalloys in oxygen-enriched atmosphere [J]. Chin. J. Eng., 2016, 38: 1288
王宏亮, 黄进峰, 连 勇 等. 高温合金GH4169与GH4202在富氧气氛中的燃烧行为 [J]. 工程科学学报, 2016, 38: 1288
[15] Shao L, Li Z B, Yu J B, et al. Combustion behavior and mechanisms of Ti2AlNb compared to an α + β Ti alloy [J]. Corros. Sci., 2021, 192: 109868
[16] Shao L, Li W S, Li D Y, et al. A review on combustion behavior and mechanism of Ti alloys for advanced aero-engine [J]. J. Alloys Compd., 2023, 960: 170584
[17] Shao L, Xie G L, Liu X H, et al. Combustion behavior and mechanism of Ti-25V-15Cr compared to Ti-6Al-4V alloy [J]. Corros. Sci., 2022, 194: 109957
[18] Shao L, Xie G L, Liu X H, et al. Combustion behaviour and mechanism of TC4 and TC11 alloys [J]. Corros. Sci., 2020, 168: 108564
[19] Cao S T, Zhang S H, Zhang J. Combustion behavior of GH4061 alloy in high pressure and oxygen-enriched atmosphere [J]. Acta Metall. Sin., 2023, 59: 547
曹姝婷, 张少华, 张 健. GH4061合金在高压富氧环境下的燃烧行为 [J]. 金属学报, 2023, 59: 547
[20] Liu S Y, Shin Y C. Additive manufacturing of Ti6Al4V alloy: A review [J]. Mater. Des., 2019, 164: 107552
[21] Zhao R X, Zhao Z Y, Bai P K, et al. Effect of heat treatment on the microstructure and properties of Inconel 718 alloy fabricated by selective laser melting [J]. J. Mater. Eng. Perform., 2022, 31: 353
[22] Moussaoui K, Rubio W, Mousseigne M, et al. Effects of selective laser melting additive manufacturing parameters of Inconel 718 on porosity, microstructure and mechanical properties [J]. Mater. Sci. Eng., 2018, A735: 182
[23] Zhang S Y, Wang L L, Lin X, et al. The formation and dissolution mechanisms of Laves phase in Inconel 718 fabricated by selective laser melting compared to directed energy deposition and cast [J]. Composites, 2022, 239B: 109994
[24] Amato K N, Gaytan S M, Murr L E, et al. Microstructures and mechanical behavior of Inconel 718 fabricated by selective laser melting [J]. Acta Mater., 2012, 60: 2229
[25] Sui S, Zhong C L, Chen J, et al. Influence of solution heat treatment on microstructure and tensile properties of Inconel 718 formed by high-deposition-rate laser metal deposition [J]. J. Alloys Compd., 2018, 740: 389
[26] Wan H Y, Zhou Z J, Li C P, et al. Effect of scanning strategy on grain structure and crystallographic texture of Inconel 718 processed by selective laser melting [J]. J. Mater. Sci. Technol., 2018, 34: 1799
[27] Chlebus E, Gruber K, Kuźnicka B, et al. Effect of heat treatment on the microstructure and mechanical properties of Inconel 718 processed by selective laser melting [J]. Mater. Sci. Eng., 2015, A639: 647
[28] Huang W P, Yang J J, Yang H H, et al. Heat treatment of Inconel 718 produced by selective laser melting: Microstructure and mechanical properties [J]. Mater. Sci. Eng., 2019, A750: 98
[29] Li X, Shi J J, Wang C H, et al. Effect of heat treatment on microstructure evolution of Inconel 718 alloy fabricated by selective laser melting [J]. J. Alloys Compd., 2018, 764: 639
[30] Zhang D Y, Niu W, Cao X Y, et al. Effect of standard heat treatment on the microstructure and mechanical properties of selective laser melting manufactured Inconel 718 superalloy [J]. Mater. Sci. Eng., 2015, A644: 32
[31] Li J, Zhao Z Y, Bai P K, et al. Microstructural evolution and mechanical properties of IN718 alloy fabricated by selective laser melting following different heat treatments [J]. J. Alloys Compd., 2019, 772: 861
[32] Bransford J W. Ignition and combustion temperatures determined by laser heating [A]. Flammability and Sensitivity of Materials in Oxygen-Enriched Atmospheres: Second Volume [C]. Philadelphia: ASTM, 1986: 78
[33] Yu J B, Wang H, Liu X J, et al. Flame retardancy of face-centred-cubic structured NiCo-based medium-entropy alloys in high-pressure oxygen atmospheres [J]. J. Alloys Compd., 2023, 944: 169231
[34] Shao L, Xie G L, Liu X H, et al. Combustion behaviour and mechanism of a Cu-Ni-Mn alloy in an oxygen enriched atmosphere [J]. Corros. Sci., 2020, 163: 108253
[35] Liu Y M, Zhao M L, Feng H, et al. Dynamic in-situ study on phase transition of GH4169 superalloy during homogenization process [J]. Rare Met. Mater. Eng., 2021, 50: 1334
刘艳梅, 赵美兰, 冯 辉 等. GH4169合金均匀化过程中相变动态原位研究 [J]. 稀有金属材料与工程, 2021, 50: 1334
[36] Rao G A, Kumar M, Srinivas M, et al. Effect of standard heat treatment on the microstructure and mechanical properties of hot isostatically pressed superalloy Inconel 718 [J]. Mater. Sci. Eng., 2003, A355: 114
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