C/C复合材料高熵氧化物涂层抗烧蚀性能

doi:10.15541/jim20230370

无机材料学报 ›› 2024, Vol. 39 ›› Issue (1): 61-70.DOI: 10.15541/jim20230370 CSTR: 32189.14.10.15541/jim20230370

所属专题：【结构材料】热障与环境障涂层(202409)；【结构材料】高熵陶瓷(202409)

C/C复合材料高熵氧化物涂层抗烧蚀性能

郭凌翔(), 唐颖, 黄世伟, 肖博澜, 夏东浩, 孙佳()

西北工业大学超高温结构复合材料国防科技重点实验室, 纤维增强轻质复合材料陕西省重点实验室, 西安 710072

收稿日期:2023-08-14 修回日期:2023-10-18 出版日期:2024-01-20 网络出版日期:2023-10-15
通讯作者: 孙佳, 副教授. E-mail: j.sun@nwpu.edu.cn
作者简介:郭凌翔(1997-), 男, 博士研究生. E-mail: guolingxiang@mail.nwpu.edu.cn
基金资助:
国家重点研发计划(2022YFB3708600);国家重点研发计划(2021YFA0715802);国家自然科学基金(52101098);航空科学基金(2022Z055053004)

Ablation Resistance of High-entropy Oxide Coatings on C/C Composites

GUO Lingxiang(), TANG Ying, HUANG Shiwei, XIAO Bolan, XIA Donghao, SUN Jia()

State Key Laboratory of Ultra High Temperature Composite Materials, Shaanxi Key Laboratory of Fiber Reinforced Light Composite Materials, Northwestern Polytechnical University, Xi’an 710072, China

Received:2023-08-14 Revised:2023-10-18 Published:2024-01-20 Online:2023-10-15
Contact: SUN Jia, associate professor. E-mail: j.sun@nwpu.edu.cn
About author:GUO Lingxiang(1997-), male, PhD candidate. E-mail: guolingxiang@mail.nwpu.edu.cn
Supported by:
National Key R&D Program of China(2022YFB3708600);National Key R&D Program of China(2021YFA0715802);National Natural Science Foundation of China(52101098);Aeronautical Science Foundation of China(2022Z055053004)

摘要/Abstract

摘要：

新一代高超声速飞行器热端部件服役温度不断提高, 对表面防护涂层的相稳定性和抗烧蚀性能提出了更高的要求。本工作针对传统过渡金属氧化物ZrO₂、HfO₂涂层开展高熵化设计, 采用高温固相反应结合超音速大气等离子喷涂制备(Hf_0.125Zr_0.125Sm_0.25Er_0.25Y_0.25)O_2-_δ(M1R3O)、(Hf_0.2Zr_0.2Sm_0.2Er_0.2Y_0.2)O_2-_δ(M2R3O)、(Hf_0.25Zr_0.25- Sm_0.167Er_0.167Y_0.167)O_2-_δ(M3R3O)三种高熵氧化物涂层, 探究稀土组元含量对高熵氧化物涂层的相结构演变规律、相稳定性以及抗烧蚀性能的影响。M2R3O涂层和M3R3O涂层呈现优异的相稳定性和抗烧蚀性能, 涂层经热流密度为2.38~2.40 MW/m²的氧-乙炔焰烧蚀后仍保持物相结构稳定, 未发生固溶体分解或析出稀土组元。其中M2R3O涂层循环烧蚀180 s后的质量烧蚀率与线烧蚀率分别为0.01 mg/s和-1.16 μm/s, 相比M1R3O涂层(0.09 mg/s、-1.34 μm/s)以及M3R3O涂层(0.02 mg/s、-4.51 μm/s), 分别降低了88.9%、13.4%以及50.0%、74.3%, 表现出最优异的抗烧蚀性能。M2R3O涂层的抗烧蚀性能优异归因于其兼具较高的熔点(>2200 ℃)和较低的热导率((1.07±0.09) W/(m·K)), 使其有效防护内部的SiC过渡层以及C/C复合材料免受氧化损伤, 避免了界面SiO₂相形成所导致的界面开裂。

关键词: 高熵陶瓷, 过渡金属氧化物, 热喷涂, 热防护涂层, 抗烧蚀, C/C复合材料

Abstract:

With improvement in service temperature of thermal structural components for the new generation hypersonic aircraft, higher requirements are put forward for the phase stability and ablation resistance of the thermal protection coatings (TPCs). Carrying out high-entropy design for traditional transition metal oxide ZrO₂ and HfO₂ coatings, solid-phase reaction and supersonic atmosphere plasma spraying (SAPS) were applied to prepare (Hf_0.125Zr_0.125Sm_0.25Er_0.25Y_0.25)O_2-_δ (M1R3O), (Hf_0.2Zr_0.2Sm_0.2Er_0.2Y_0.2)O_2-_δ (M2R3O), (Hf_0.25Zr_0.25Sm_0.167Er_0.167Y_0.167)O_2-_δ (M3R3O) high-entropy oxide (HEO) coatings. The effects of rare earth content on phase structure evolution, phase stability and ablative resistance of HEO coatings were investigated. M2R3O coating and M3R3O coating possessed excellent phase stability and ablation resistance, which maintained stable phase structure after ablation by oxygen-acetylene flame with heat flux density of 2.38-2.40 MW/m², without decomposition of solid solution and precipitation of rare earth components. Mass ablation rate and linear ablation rate of M2R3O coating after cyclic ablation for 180 s are 0.01 mg/s and -1.16 μm/s, respectively. Compared with M1R3O coating (0.09 mg/s, -1.34 μm/s) and M3R3O coating (0.02 mg/s, -4.51 μm/s), the reductions of ablation rate are 88.9%, 13.4%, respectively, and 50.0%, 74.3% for M2R3O coatings, respectively, presenting the best ablation resistance. M2R3O coating exhibits excellent ablation resistance due to its high melting point (>2200 ℃) and low thermal conductivity ((1.07±0.09) W/(m·K)), which effectively protects the internal SiC transition layer and C/C composites from oxidation damage, avoiding interface cracking caused by the formation of SiO₂ phase.

Key words: high-entropy ceramic, transition metal oxide, thermal spray, thermal protection coating, ablation resistance, C/C composite

中图分类号:

TB332

郭凌翔, 唐颖, 黄世伟, 肖博澜, 夏东浩, 孙佳. C/C复合材料高熵氧化物涂层抗烧蚀性能[J]. 无机材料学报, 2024, 39(1): 61-70.

GUO Lingxiang, TANG Ying, HUANG Shiwei, XIAO Bolan, XIA Donghao, SUN Jia. Ablation Resistance of High-entropy Oxide Coatings on C/C Composites[J]. Journal of Inorganic Materials, 2024, 39(1): 61-70.

图/表 19

表1 研究中高熵氧化物的成分及组元摩尔比

Table 1 Compositions and component molar ratios of high-entropy oxides in this study

Label	Constituent	$\frac{n(\text{Hf}+\text{Zr})}{n(\text{Sm}+\text{Er}+\text{Y})}$
M1R3O	(Hf_0.125Zr_0.125Sm_0.25Er_0.25Y_0.25)O_2-_δ	1/3
M2R3O	(Hf_0.2Zr_0.2Sm_0.2Er_0.2Y_0.2)O_2-_δ	2/3
M3R3O	(Hf_0.25Zr_0.25Sm_0.167Er_0.167Y_0.167)O_2-_δ	3/3

表2 高熵氧化物涂层的SAPS参数

Table 2 Parameters of SAPS for high-entropy oxide coatings

Parameter	Value
Current/A	410-430
Voltage/V	100-120
Primary gas Ar/(L·min^-1)	65-70
Second gas H₂/(L·min^-1)	3.5-5.0
Powder flow Ar/(L·min^-1)	5-7
Spray distance/mm	100
Powder feed rate/(g·min^-1)	5-6

图1 高熵氧化物粉体的物相表征

Fig. 1 Phase characterizations of high-entropy oxide powders (a) XRD pattern of M2R3O and standard diffraction peaks for each single-component oxide; (b) XRD patterns of three high-entropy oxides; (c) Ideal crystal structure; (d) Raman spectra of three high-entropy oxides

图2 M2R3O粉体的TEM测试分析

Fig. 2 TEM analyses of M2R3O powders (a) Morphology; (b) High-resolution TEM (HRTEM) image; (c) Selective area electron diffraction (SAED) pattern; (d) High-angle annular dark field (HAADF) image and corresponding element mappings

图3 高熵氧化物涂层表面和截面的微观形貌

Fig. 3 Surface and cross-section morphologies of high-entropy oxide coatings (a, d) M1R3O coating; (b, e) M2R3O coating; (c, f) M3R3O coating

图4 高熵氧化物涂层的XRD图谱

Fig. 4 XRD patterns of high-entropy oxide coatings (a) Full spectrum diffraction; (b) M1R3O coating and refinement pattern; (c) M2R3O coating and refinement pattern; (d) M3R3O coating and refinement pattern

图5 HfO2-RE2O3和ZrO2-RE2O3 (RE=Sm、Er、Y)二元相图[30]

Fig. 5 Binary phase diagrams of HfO2-RE2O3 and ZrO2-RE2O3 (RE=Sm, Er and Y)[30] (a) HfO2-Sm2O3; (b) HfO2-Er2O3; (c) HfO2-Y2O3; (d) ZrO2-Sm2O3; (e) ZrO2-Er2O3; (f) ZrO2-Y2O3

图6 高熵氧化物涂层烧蚀过程的表面温度曲线

Fig. 6 Surface temperature curves of high-entropy oxide coatings during ablation

图7 高熵氧化物涂层烧蚀后的宏观形貌

Fig. 7 Macro morphologies of high-entropy oxide coatings after ablation

图8 高熵氧化物涂层的质量烧蚀率与线烧蚀率

Fig. 8 Mass ablation ratios and line ablation ratios of high- entropy oxide coatings

图9 高熵氧化物涂层烧蚀后的XRD图谱

Fig. 9 XRD patterns of high-entropy oxide coatings after ablation (a) M1R3O; (b) M2R3O; (c) M3R3O

图10 涂层循环烧蚀180 s后的截面微观形貌以及EDS分析

Fig. 10 Cross-section morphologies and EDS analyses of high-entropy oxide coatings after cyclic ablation for 180 s(a-c) M1R3O; (d-f) M2R3O; (g-i) M3R3O

图11 高熵氧化物涂层与其他涂层在相同烧蚀环境中的抗烧蚀性能比较

Fig. 11 Comparison of ablation resistances between high-entropy oxide coatings and other coatings in the same ablation environment

图S1 M1R3O粉体的TEM测试分析

Fig. S1 TEM analysis of M1R3O powders (a) Morphology; (b) HRTEM image; (c) SAED pattern; (d) HAADF image and its corresponding element mappings

图S2 M3R3O粉体的TEM测试分析

Fig. S2 TEM analysis of M3R3O powders (a) Morphology; (b) HRTEM image; (c) SAED pattern; (d) HAADF image and its corresponding element mappings

图S3 高熵氧化物粉体的XRD精修图谱

Fig. S3 XRD refinement patterns of high-entropy oxide powders (a) M1R3O; (b) M2R3O; (c)M3R3O

图S4 高熵氧化物的热导率

Fig. S4 Thermal conductivities of high-entropy oxides

图S5 高熵氧化物涂层烧蚀后的表面微观形貌

Fig. S5 Surface microstructures of high-entropy oxide coatings after ablation (a-c) M2R3O coatings; (d-f) M3R3O coatings

表S1 EDS元素点扫描分析

Tabel S1 EDS element point scanning analysis

	Hf	Zr	Sm	Er	Y	Si	O
Spot A/(%, in atom)	10.5	5.6	9.3	8.5	8.4	—	57.7
Spot B/(%, in atom)	5.6	4.7	5.1	8.7	10.4	3.8	61.7

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C/C复合材料高熵氧化物涂层抗烧蚀性能

Ablation Resistance of High-entropy Oxide Coatings on C/C Composites

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