journal article·2026-07Open access

Ultrafast low-temperature fabrication of strong and tough high-entropy boride-based ceramics via reactive ZrSi 2 -assisted heavy direct current sintering

Lehao Liu, Yingjun Liu, Yuhan Yao, Yufei Zu, Zhaofu Zhang, Jianjun Sha, Yang Zhang, Hongfeng Dong, Nan Zhang, Shujing Zhang, Ning Zhang, Wenhao Yue, Yibo Zhang, Wuhao Cao, Yuan Hu, Ruiheng An, Wenhu Li, Luyi Zhu, Taotao Ai

Journal of Advanced Ceramics· Volume 15· Issue 7

Abstract

Abstract The ultrahigh sintering temperatures required for high-entropy borides (HEBs) pose a significant challenge to their processing and practical application. This study introduces an efficient low-temperature fabrication route for dense HEB-based ceramics using reactive ZrSi2-assisted heavy direct current sintering, with a maximum heating rate exceeding 3700 °C/min. A porosity of 1.60%±0.61% can be achieved at a sintering temperature of 1000 °C, which is reduced by 600–1000 °C compared to state-of-the-art spark plasma sintering (SPS)/field-assisted sintering technique (FAST) processing of HEBs. Microstructural analysis revealed interdiffusion between HEB and ZrSi2, leading to a core–shell HEB architecture and layered high-entropy silicides (HESs). Meanwhile, dislocations and nonuniform stress fields were observed within the HEB grains. These microstructural features synergistically inhibit crack propagation and promote crack deflection and branching. Consequently, both flexural strength and fracture toughness (KIC) are significantly enhanced. A flexural strength of 963 MPa was attained at 1400 °C, and a KIC of 7.4 MPa·m1/2 was achieved at 1500 °C, surpassing most reported HEB-based ceramics. These results demonstrate that reactive ZrSi2-assisted heavy direct current sintering is a profoundly effective approach for the low-temperature manufacturing of high-performance HEB-based ceramics.
Source: crossref · Quality: baseline

Research context

OpenAlex topics: Advanced ceramic materials synthesis · High Entropy Alloys Studies · Advanced materials and composites

SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.

References (53)

Show source-provided references
1. S Divilov. Disordered enthalpy-entropy descriptor for high-entropy ceramics discovery. 2024, 625: 66-73.10.1038/s41586-023-06786-y ↗
2. AB Peters. Materials design for hypersonics. 2024, 15: 3328.10.1038/s41467-024-46753-3 ↗
3. F Wang. Will high-entropy carbides and borides be enabling materials for extreme environments. 2023, 5: 022002.10.1088/2631-7990/acbd6e ↗
4. HM Xiang. High-entropy ceramics: Present status, challenges, and a look forward. 2021, 10: 385-441.10.1007/s40145-021-0477-y ↗
5. T Qureshi. Review: High-entropy borides—challenges and opportunities. 2024, 59: 15921-15991.10.1007/s10853-024-10064-1 ↗
6. SH Qiu. Achieving superhardness and enhanced toughness in high-entropy boride-based composites by tailoring their multi-scale microstructures. 2025, 21: 2404632.10.1002/smll.202404632 ↗
7. S Zhang. Optimized preparation and mechanical properties of high-entropy boride ceramics. 2025, 44: 111926.10.1016/j.mtcomm.2025.111926 ↗
8. FW Wang. Pressureless densification and properties of high-entropy boride ceramics with B 4 C additions. 2024, 190: 1-9.10.1016/j.jmst.2024.01.007 ↗
9. Y Zhang. Fabrication of textured (Hf 0.2 Zr 0.2 Ta 0.2 Cr 0.2 Ti 0.2 )B 2 high-entropy ceramics. 2021, 41: 1015-1019.10.1016/j.jeurceramsoc.2020.08.071 ↗
10. SM Smith. Intermediate stage densification kinetics of high-entropy ceramics during spark plasma sintering. 2025, 45: 117136.10.1016/j.jeurceramsoc.2024.117136 ↗
11. S Volodko. Heterogeneous microstructures in dual-phase high-entropy carbide/boride ceramics. 2025, 945: 149045.10.1016/j.msea.2025.149045 ↗
12. BW Yuan. Fabrication and oxidation resistance of metallic Ta-reinforced high-entropy (Ti,Zr,Hf,Nb,Ta)B 2 ceramics. 2025, 18: 4642.10.3390/ma18194642 ↗
13. V Kombamuthu. Effect of SiC on densification, microstructure and mechanical properties of high entropy diboride (Ti 0.2 Zr 0.2 Hf 0.2 Nb 0.2 Ta 0.2 )B 2 . 2024, 44: 5358-5369.10.1016/j.jeurceramsoc.2023.12.072 ↗
15. FL Huang. Improved damage tolerance and oxidation resistance of (Ti 0.2 Zr 0 . 2 Hf 0.2 Nb 0.2 Ta 0.2 )B 2 –SiC by introducing chopped carbon fibers. 2024, 13: 101-112.10.26599/JAC.2024.9220844 ↗
16. L Feng. Strength retention of single-phase high-entropy diboride ceramics up to 2000 °C. 2024, 107: 1895-1904.10.1111/jace.19438 ↗
17. B Li. Densification and mechanical properties of Al 2 O 3 reinforced high-entropy diboride ceramics. 2025, 124: 112-120.10.1177/17436753251380041 ↗
18. CC Ji. Microstructure and mechanical properties of high-entropy diboride-based ceramic assisted by Ti 3 AlC 2 additive. 2024, 50: 30810-30820.10.1016/j.ceramint.2024.05.386 ↗
19. EW Awin. Tailoring crystal structure of high-entropy carbides in Si-based ceramic nanocomposites through precursor engineering. 2024, 44: 6901-6910.10.1016/j.jeurceramsoc.2024.05.013 ↗
20. B Du. Novel synthesis of (Hf 0.25 Zr 0.25 Ti 0.25 Ta 0.25 )C–SiC biphasic ceramic micro-powders using single-source-precursor route. 2024, 50: 46166-46172.10.1016/j.ceramint.2024.08.459 ↗
21. N Gilli. Design of ultra-high temperature ceramic nano-composites from multi-scale length microstructure approach. 2021, 226: 109344.10.1016/j.compositesb.2021.109344 ↗
22. RR Hao. Theoretical prediction of structural stability, electronic and elastic properties of ZrSi 2 under pressure. 2015, 5: 36779-36786.10.1039/C5RA01964H ↗
23. AY Potanin. Combustion synthesis of the (Ti,Zr)B 2 –(Zr,Ti)C eutectic composites: Structure formation and properties. 2024, 50: 47433-47444.10.1016/j.ceramint.2024.09.094 ↗
24. BX Wei. Dual plate-like grains of (Ti,Zr)B 2 and W 2 B 5 toughened solid solution composites fabricated via in-situ reaction spark plasma sintering of (Ti,W)C and ZrB 2 powders. 2024, 44: 6206-6222.10.1016/j.jeurceramsoc.2024.03.066 ↗
25. D Liu. Synthesis of superfine high-entropy metal diboride powders. 2019, 167: 110-114.10.1016/j.scriptamat.2019.03.038 ↗
26. YJ Liu. Phase composition, densification behavior and high-temperature strength of carbon-doped ZrB 2 –ZrSi 2 ceramics. 2023, 49: 39083-39089.10.1016/j.ceramint.2023.09.246 ↗
27. YJ Liu. Ultrafast preparation of dense textured ZrB 2 -based ceramics via heavy continuous DC Joule heating and pressing. 2025, 14: 9221074.10.26599/JAC.2025.9221074 ↗
28. HZ Shen. Ultrafast high-temperature sintering: Principles, advantages, and applications. 2025, 45: 117653.10.1016/j.jeurceramsoc.2025.117653 ↗
29. Z Liu. Large-diameter ceramic room-temperature flash sintering technology based on new carbon electrodes. 2025, 14: 9221094.10.26599/JAC.2025.9221094 ↗
30. M Sakkaki. Numerical simulation of heat transfer during spark plasma sintering of zirconium diboride. 2020, 46: 4998-5007.10.1016/j.ceramint.2019.10.240 ↗
31. M Biesuz. Ultrafast high-temperature sintering (UHS) vs. conventional sintering of 3YSZ: Microstructure and properties. 2024, 44: 4741-4750.10.1016/j.jeurceramsoc.2024.01.064 ↗
32. Bona E De. Ultrafast high-temperature sintering (UHS) of ZrB 2 -based materials. 2024, 44: 567-573.10.1016/j.jeurceramsoc.2023.09.007 ↗
33. HR Mao. Ultrafast high-temperature synthesis and densification of high-entropy carbides. 2022, 42: 4053-4065.10.1016/j.jeurceramsoc.2022.03.054 ↗
34. F Zuo. Scalable and efficient consolidation of Al 2 O 3 and SiC ceramics using a powder medium-based ultrafast high-temperature sintering (P-UHS). 2025, 266: 116768.10.1016/j.scriptamat.2025.116768 ↗
35. F Lebas. Exploration of UHS scalability by SPS approach: Multiphysics simulation, critical dimensions, mechanisms and properties. 2026, 46: 117865.10.1016/j.jeurceramsoc.2025.117865 ↗
36. J Gild. A high-entropy silicide: (Mo 0.2 Nb 0.2 Ta 0.2 Ti 0.2 W 0.2 )Si 2 . 2019, 5: 337-343.10.1016/j.jmat.2019.03.002 ↗
37. JJ Sha. Mechanical properties and toughening mechanism of WC-doped ZrB 2 –ZrSi 2 ceramic composites by hot pressing. 2014, 62: 199-204.10.1016/j.matdes.2014.04.083 ↗
38. JC Li. High-entropy (Ti 0.2 V 0.2 Nb 0.2 Mo 0.2 W 0.2 )Si 2 with excellent high-temperature wear resistance. 2024, 107: 2750-2764.10.1111/jace.19592 ↗
39. FL Huang. Reactive sintered dense carbon fiber reinforced high-entropy boride composite using high-entropy silicide as reactant. 2025, 108: 20212.10.1111/jace.20212 ↗
40. Y Qin. A high entropy silicide by reactive spark plasma sintering. 2019, 8: 148-152.10.1007/s40145-019-0319-3 ↗
41. Y Qin. High-entropy silicide ceramics developed from (TiZrNbMoW)Si 2 formulation doped with aluminum. 2020, 40: 2752-2759.10.1016/j.jeurceramsoc.2020.02.059 ↗
42. G Yao. Electronic structures and strengthening mechanisms of superhard high-entropy diborides. 2023, 42: 614-628.10.1007/s12598-022-02152-5 ↗
43. Q Zheng. Transient liquid-phase to guide multiphase evolution in reactive-hot-pressed ZrB 2 –SiC–ZrC ceramics. 2020, 6: 607-617.10.1016/j.jmat.2020.05.001 ↗
44. H Xie. Rapid liquid phase-assisted ultrahigh-temperature sintering of high-entropy ceramic composites. 2022, 8: 8241.10.1126/sciadv.abn8241 ↗
45. LJ Qiao. First-principles prediction, fabrication and characterization of (Hf 0.2 Nb 0.2 Ta 0.2 Ti 0.2 Zr 0.2 )B 2 high-entropy borides. 2022, 48: 17234-17245.10.1016/j.ceramint.2022.02.281 ↗
46. JX Liu. Mechanical properties of hot-pressed high-entropy diboride-based ceramics. 2020, 9: 503-510.10.1007/s40145-020-0383-8 ↗
47. JC Li. High-entropy diboride: A novel high-temperature self-lubricating ceramic with enhanced mechanical and tribological properties. 2025, 14: 9221085.10.26599/JAC.2025.9221085 ↗
48. AC Murchie. Room-temperature mechanical properties of a high-entropy diboride. 2022, 19: 2293-2299.10.1111/ijac.14026 ↗
49. D Wang. Microstructure and mechanical properties of in-situ B 4 C–(TiZrHfNbTa)B 2 composite by reactive spark plasma sintering. 2022, 74: 4129-4137.10.1007/s11837-022-05377-y ↗
50. MX Mao. A new route to fabricate dual-phase compositionally complex ceramics. 2024, 44: 116726.10.1016/j.jeurceramsoc.2024.116726 ↗
51. L Silvestroni. A simple route to fabricate strong boride hierarchical composites for use at ultra-high temperature. 2020, 183: 107618.10.1016/j.compositesb.2019.107618 ↗
52. W Luo. Formation and strengthening mechanism of kink bands in an ultra-coarse-grained Fe–Cr–Al alloy. 2024, 186: 1-14.10.1016/j.jmst.2023.11.017 ↗
53. P Liu. Superior strength–plasticity synergy in a heterogeneous lamellar Ti 2 AlC/TiAl composite with unique interfacial microstructure. 2023, 159: 21-32.10.1016/j.jmst.2023.03.011 ↗