高熵碳化物超高温陶瓷的研究进展

doi:10.15541/jim20230562

无机材料学报 ›› 2024, Vol. 39 ›› Issue (6): 591-608.DOI: 10.15541/jim20230562

高熵碳化物超高温陶瓷的研究进展

蔡飞燕¹^,²^,³(), 倪德伟¹^,²^,⁴(), 董绍明¹^,²()

1.中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海200050
2.中国科学院上海硅酸盐研究所, 结构陶瓷及复合材料工程研究中心, 上海200050
3.中国科学院大学, 北京100049
4.国科大杭州高等研究院, 杭州310024

收稿日期:2023-12-06 修回日期:2024-01-19 出版日期:2024-06-20 网络出版日期:2024-01-22
通讯作者: 倪德伟, 研究员. E-mail: deweini@mail.sic.ac.cn;
董绍明, 研究员. E-mail: smdong@mail.sic.ac.cn
作者简介:蔡飞燕(1998-), 女, 博士研究生. E-mail: caifeiyan19@mails.ucas.ac.cn
基金资助:
国家重点研发计划(2022YFB3707700);上海市优秀学术/技术带头人计划(23XD1424300);国家自然科学基金(52332003)

Research Progress of High-entropy Carbide Ultra-high Temperature Ceramics

CAI Feiyan¹^,²^,³(), NI Dewei¹^,²^,⁴(), DONG Shaoming¹^,²()

1. State Key Laboratory of High Performance Ceramics & Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. Structural Ceramics and Composites Engineering Research Center, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
3. University of Chinese Academy of Sciences, Beijing 100049, China
4. Hangzhou Institute for Advanced Study, University of Chinese Academy of Sciences, Hangzhou 310024, China

Received:2023-12-06 Revised:2024-01-19 Published:2024-06-20 Online:2024-01-22
Contact: NI Dewei, professor. E-mail: deweini@mail.sic.ac.cn;
DONG Shaoming, professor. E-mail: smdong@mail.sic.ac.cn
About author:CAI Feiyan (1998-), female, PhD candidate. E-mail: caifeiyan19@mails.ucas.ac.cn
Supported by:
National Key R&D Program of China(2022YFB3707700);Program of Shanghai Academic/Technology Research Leader(23XD1424300);National Natural Science Foundation of China(52332003)

摘要/Abstract

摘要：

高速飞行技术的发展对高性能热结构材料提出了迫切需求。高熵碳化物(HECs)陶瓷作为近年来发展迅速的一类新型材料, 兼具高熵陶瓷与超高温陶瓷的优良特性, 在极端服役环境中具有广阔的应用前景, 因此得到国内外学者的广泛关注。相比仅含有一种或两种过渡金属元素的传统超高温碳化物陶瓷, HECs综合性能有所提升, 且具有更强的组成和性能可设计性, 因此具备较大的发展潜力。经过对HECs的不断探索, 研究人员获得了许多有趣的结果, 开发了多种HECs的制备方法, 对HECs的显微结构和性能的认识也更加深入。本文综述了HECs的基本理论以及从实验过程中获得的规律; 对HECs粉体、HECs块体、HECs涂层及薄膜, 以及纤维增强HECs基复合材料的制备方法进行了梳理和归纳; 并对HECs的力学、热学等性能, 尤其是与高温应用相关的抗氧化、抗烧蚀性能的研究进展进行了综述和讨论。最后, 针对HECs研究中有待进一步完善的科学问题, 对HECs的未来发展提出了展望。

关键词: 高熵碳化物, 超高温陶瓷, 力学性能, 抗氧化性能, 抗烧蚀性能, 综述

Abstract:

The development of high-speed flight technology has put forward an urgent demand for high- performance thermal structure materials. High-entropy carbides (HECs) ceramics are a fast-emerging family of materials that combine the excellent properties of high-entropy ceramics and ultra-high temperature ceramics. HECs have a broad application prospect in extreme service environments, which has received extensive attention from scholars in recent years. Compared with traditional ultra-high temperature carbides containing only one or two transition metal elements, HECs have a greater potential for development because of their improved comprehensive performance and greater designability of composition and properties. After successive exploration of HECs in recent years, researchers have obtained many interesting results, developed a variety of preparation methods, and gained comprehensive understanding of microstructure and properties. The basic theories and the laws on HECs obtained from experimental process are reviewed in this paper. Preparation methods of HECs including powders, blocks, coatings and films, as well as fiber-reinforced HECs-based composites are summarized. Research progress on the properties of HECs, such as the mechanical properties, thermal properties, and especially the oxidation and ablation resistance related to high-temperature applications, is reviewed and discussed. Finally, the scientific issues that need to be further explored in this area are emphasized, and the prospects are proposed.

Key words: high-entropy carbide, ultra-high temperature ceramic, mechanical property, oxidation resistance, ablation resistance, review

中图分类号:

TQ174

蔡飞燕, 倪德伟, 董绍明. 高熵碳化物超高温陶瓷的研究进展[J]. 无机材料学报, 2024, 39(6): 591-608.

CAI Feiyan, NI Dewei, DONG Shaoming. Research Progress of High-entropy Carbide Ultra-high Temperature Ceramics[J]. Journal of Inorganic Materials, 2024, 39(6): 591-608.

图/表 14

表1 经实验验证的9种HECs的EFA值[31]

Table 1 EFA values of 9 experimentally validated HECs[31]

Composition	EFA/(eV/atom)^-1	Phase
(VNbTaMoW)C	125	Single-phase
(TiZrHfNbTa)C	100	Single-phase
(TiHfVNbTa)C	100	Single-phase
(TiVNbTaW)C	77	Single-phase
(TiHfNbTaW)C	67	Single-phase
(TiZrHfTaW)C	50	Single-phase
(ZrHfTaMoW)C	45	Multi-phase
(TiZrHfMoW)C	38	Multi-phase
(ZrHfVMoW)C	37	Multi-phase

表2 典型的HECs粉体合成方法及特点

Table 2 Typical HECs synthesis methods and characteristics

Synthesizing method	Composition (lattice parameter)	Starting materials	Synthesizing conditions	Grain size	Oxygen content/ % (in mass)
Mechanical alloying^[32-33]	(TiZrHfVNb)C (0.4496 nm) (TiZrHfVTa)C (0.4495 nm) (TiZrHfNbTa)C (0.4526 nm) (TiZrVNbTa)C (0.4440 nm) (TiHfVNbTa)C (0.4425 nm) (ZrHfVNbTa)C (0.4493 nm)	Transition metals + Graphite powder	50-70 h	2.5 nm 2.4 nm 3.3 nm 4.0 nm 3.2 nm 3.0 nm	-
Carbothermal reduction method^[34-35]	(TiZrHfNbTa)C (0.4524 nm)	Metal oxides + Graphite powder or carbon black	Carbothermal reduction (CTR) 1600 ℃, 1 h; Solid solution (SS) 2000 ℃, 1.5 h	550 nm	0.2
Carbothermal reduction method^[34-35]	(TiZrHfNbTa)C (0.4503 nm)		2200 ℃, 1 h	0.5-2 μm	-
Molten salt synthesis^[36]	(TiVNbTa)C (0.4468 nm)	Metal carbides + Molten salt media KCl	1300 ℃, 1 h	50-110 nm	-
Liquid precursors method^[37-38]	(TiZrHfNbTa)C (-)	Metal chlorides + Furfuryl alcohol	CTR 1400 ℃, 1 h; SS 2000 ℃, 1 h	132 nm	0.22
Liquid precursors method^[37-38]	(TiZrHfTa)C (0.4529 nm)	Equiatomic metal containing monomers + Allyl-functional novolac resin	1800 ℃, 2 h	~100 nm	-
Direct synthetic method^[39]	(TiZrHfNbTa)C (0.4508 nm)	Metal carbides	1950 ℃, 5 min (SPS)	~2 μm	-

图1 几种典型方法合成的HECs粉体的形貌

Fig. 1 Morphologies of HECs powders synthesized by several typical methods (a) Liquid precursor method[37]; (b) Molten salt synthesis[36]; (c) Carbothermal reduction method[35]; (d) Direct synthesis method[39]

表3 HECs陶瓷及涂层的常见制备方法和性能

Table 3 Common Preparation methods and properties of H ECs ceramics and coatings

图2 通过三种典型过程制备的(TiZrNbTaW)C陶瓷的形貌及元素分布图[67]

Fig. 2 SEM images and corresponding EDS element mappings of (TiZrNbTaW)C ceramics prepared by three typical processes[67] (a, d) Using metallic powders and graphite as raw materials (HEC-M); (b, e) Using metal carbides as raw materials (HEC-C); (c, f) Using metal oxides and graphite as raw materials (HEC-O)

图3 在300和600 ℃沉积的近等摩尔比(TiNbTaCrW)C薄膜的(a, b)表面SEM和(c~e)TEM照片[71]

Fig. 3 (a, b) SEM and (c-e) TEM images of nearly equimolar (TiNbTaCrW)C films deposited at 300 and 600 ℃[71]

图4 (ZrHfNbTa)C陶瓷和单组元、二组元碳化物陶瓷的硬度-位移曲线[18]

Fig. 4 Hardness-depth curves of the (ZrHfNbTa)C and mono, binary carbides ceramics[18]

图5 HECs的断裂韧性、维氏硬度与一些相关材料的对比[19]

Fig. 5 Fracture toughness and Vickers hardness of HECs compared to related materials[19]

图6 不同金属组元数量的碳化物在室温条件下的热导率[15]

Fig. 6 Thermal conductivity of carbides with different numbers of metals at room temperature[15]

图7 (TiZrHfNbTa)C和ZrC在1200 ℃水氧条件下的增重曲线[125]

Fig. 7 Weight gain curves for (TiZrHfNbTa)C and ZrC at 1200 ℃ in water vapor condition[125]

图8 (ZrHfNbTa)C、ZrC、NbC、HfC、TaC和(Hf-Ta)C粉体的TG-DSC氧化曲线及氧化后的形貌[15]

Fig. 8 TG-DSC curves and SEM images after oxidation of (ZrHfNbTa)C, ZrC, NbC, HfC, TaC and (Hf-Ta)C powders[15]

图9 (TiZrHfNbTa)C0.8N0.2陶瓷烧蚀过渡区的元素富集现象[129]

Fig. 9 Elemental enrichment in the ablation transition region of (TiZrHfNbTa)C0.8N0.2[129] (a, b) Highly dense oxide scale embedded in oval Hf/Zr-rich grains; (c) Initial oval grains in the areas away from ablation surface

图10 (TiZrHfNbTa)C陶瓷在氧-乙炔焰烧蚀(2000 ℃)过程中的物相形成机理示意图[56]

Fig. 10 Schematic diagram of the ablation mechanism of (TiZrHfNbTa)C during oxyacetylene ablation flame (2000 ℃)[56] (a) Ablation center; (b) Ablation edge

表4 基于相图总结的HECs体系中可能形成的复合氧化物

Table 4 Complex oxides that could form in the HECs systems based on a review of available phase diagrams

Element	Ti	Zr	Hf	Nb	Ta
Ti	TiO₂		HfTiO₄^[137]
Zr	ZrTiO₄^[138]	ZrO₂	(Hf, Zr)O₂^[139]
Hf			HfO₂
V		ZrV₂O₇		VNb₉O₂₅^[140]	VTa₉O₂₅^[141]
Nb	Nb₂TiO₇^[142] Nb₁₀Ti₂O₂₉^[142] Nb₆Ti₂O₁₉^[142] TiNb₆O₁₇^[143]	Zr₆Nb₂O₁₇^[135]	Hf₆Nb₂O₁₇^[119]	Nb₂O₅
Ta	TiTa₂O₇^[144]	ZrTa₆O₁₇^[145] Zr₆Ta₂O₁₉^[145]	Hf₆Ta₂O₁₇^[134]	Nb₄Ta₂O₁₅^[146]	Ta₂O₅
Mo
W		ZrW₂O₈^[147]	HfW₂O₈^[147]

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高熵碳化物超高温陶瓷的研究进展

Research Progress of High-entropy Carbide Ultra-high Temperature Ceramics

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