journal article·2026-03Open access

Synthesis and microstructure of binary (Zr0.5Hf0.5)C nanoparticles via stepwise thermo-carburization and carbothermal reduction processes

Eui Seon Lee, Jongmin Byun, Sung-Tag Oh

Abstract

A novel strategy for synthesizing (Zr 0.5 Hf 0.5 )C nano-powders was proposed, and their synthesis behavior was investigated by varying the processing temperatures and durations. The (Zr 0.5 Hf 0.5 )C nanoparticles were prepared from a mixture of zirconium hydride (ZrH 2 ), hafnium oxide (HfO 2 ), and activated charcoal using a pressure-free spark plasma sintering system. The synthesis behaviors for stepwise thermo-carburization, carbothermal reduction, and solid solution processes were examined using a thermogravimetric differential thermal analysis (TG-DTA) with the derivative DTA method. The (Zr 0.5 Hf 0.5 )C powder exhibits significant particle refinement behavior, resulting in a more homogeneous size distribution without necking compared to the individual single-component mono-carbides. Furthermore, the compositional homogeneity and structural characteristics were elucidated by Raman and TEM analyses. Consequently, (Zr 0.5 Hf 0.5 )C powder with a size of 150±34 nm and a low oxygen content of 0.437±0.126 wt% was successfully synthesized at 1600 °C for 60 min.
Source: openalex_inverted_index · Quality: baseline

Research context

OpenAlex topics: MXene and MAX Phase Materials · Advanced ceramic materials synthesis · Advanced materials and composites

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

References (43)

Show source-provided references
1. Synthesis, pyrolysis mechanism, and ceramic ablation performance of a TaC precursor with unsaturated bonds10.26599/JAC.2025.9221176 ↗
2. Compositional optimization for enhanced oxidation resistance of high-entropy carbide ceramics10.1016/j.actamat.2024.120463 ↗
3. Melting point of group IV and V transition metal diborides10.1111/jace.70299 ↗
4. In-situ phase evolution of multi-component boride to high-entropy ceramic upon ultra-high temperature ablation10.1016/j.jeurceramsoc.2022.11.019 ↗
5. The oxidation resistance and plasma ablation performance at 3000 K of HfC-TiC ultra-high temperature ceramics10.1016/j.jeurceramsoc.2025.117530 ↗
6. Fabrication and characterization of HfCZrCTiC composites: role of carbonaceous and metallic additives10.1007/s43207-024-00444-3 ↗
7. Phase stability and mechanical properties of carbide solid solutions with 2-5 principal metals10.1016/j.commatsci.2021.110869 ↗
8. Arc melting: a novel method to prepare homogeneous solid solutions of transition metal carbides (Zr, Ta, Hf)10.1016/j.ceramint.2019.01.238 ↗
9. Low temperature synthesis of an equiatomic (TiZrHfVNb)C5 high entropy carbide by a mechanically-induced carbon diffusion route10.1016/j.ceramint.2019.07.195 ↗
10. Solid solution synthesis of tantalum carbide-hafnium carbide by spark plasma sintering10.1111/jace.14778 ↗
11. Synthesis and densification of nano-crystalline hafnium carbide powder10.1016/j.jeurceramsoc.2015.08.004 ↗
12. Synthesis and densification of ultra-fine ZrC powders-effects of C/Zr ratio10.1016/j.ijrmhm.2019.03.001 ↗
13. Thermal erosion characteristics of vacuum hot-pressed NbC-modified ZrC ultra-high temperature ceramics ranging from 1500 to 2500°C10.1016/j.jeurceramsoc.2025.117835 ↗
14. Fabrication and characterization of polymer-derived high-entropy carbide ceramic powders10.1111/jace.17134 ↗
15. Low-temperature sintering of single-phase, high-entropy carbide ceramics10.1111/jace.16672 ↗
16. Dense HfB2 ceramics fabricated by high-energy ball milling and spark plasma sintering
17. Reactive laser synthesis of ultra-high-temperature ceramics HfC, ZrC, TiC, HfN, ZrN, and TiN for additive manufacturing10.1016/j.ceramint.2022.11.319 ↗
18. Preparation of ZrC by self-propagating high-temperature synthesis10.1016/j.ceramint.2010.03.013 ↗
19. Ultra-fast high-temperature synthesis and densification of high-entropy diborides and diboride-carbide ceramics10.1016/j.jeurceramsoc.2023.05.042 ↗
20. One-step synthesis of high-entropy diborides with hierarchy structure and high hardness via aluminum-melt reaction method10.1080/21663831.2023.2292079 ↗
21. Microwave sintering of ZrB2-based ceramics: a review10.53063/synsint.2023.33129 ↗
22. Producing high performance TiB2 ceramics by high-pressure sintering forging10.1016/j.ceramint.2025.02.175 ↗
23. Preparation of high-entropy carbides by different sintering techniques10.1007/s10853-021-06004-y ↗
24. Ultrafast pressure sintering: a one-step route to dense high-entropy carbide from precursors10.1016/j.jeurceramsoc.2024.117095 ↗
25. Mechanical properties and rapid consolidation of binderless niobium carbide10.1016/j.jallcom.2009.03.036 ↗
26. Nano-TaC powder synthesized using modified spark plasma sintering apparatus and its densification10.1016/j.ceramint.2015.05.124 ↗
27. Nano-sized zirconium carbide powder: synthesis and densification using a spark plasma sintering apparatus10.1016/j.ijrmhm.2017.01.006 ↗
28. High-entropy carbide: a novel class of multicomponent ceramics10.1016/j.ceramint.2018.08.100 ↗
29. TEM study of the reaction mechanisms involved in the carbothermal reduction of zirconia10.1016/j.jeurceramsoc.2012.07.024 ↗
30. Synthesis and characterization of nano-crystalized HfC based on an aqueous solution-derived precursor
31. Synthesis of ZrCx with controlled carbon stoichiometry by low temperature solid state reaction10.1016/j.jeurceramsoc.2019.03.004 ↗
32. Sluggish diffusion in Co–Cr–Fe–Mn–Ni high-entropy alloys10.1016/j.actamat.2013.04.058 ↗
33. Diffusion and solid solution formation between the binary carbides of TaC, HfC and ZrC10.1016/j.ijrmhm.2013.03.009 ↗
34. Gao · 2016
35. Heat-treatment of carbon blacks obtained by pyrolysis of used tires. Effect on the surface chemistry, porosity and electrical conductivity10.1016/S0165-2370(02)00017-7 ↗
36. Synthesis of MAX phase-based ceramics from early transition metal hydride powders10.1016/j.jeurceramsoc.2022.09.025 ↗
37. Synthesis of single-phase high-entropy carbide powders10.1016/j.scriptamat.2018.10.049 ↗
38. Critical assessment and thermodynamic calculation of the ternary system C-Hf-Zr (carbon-zirconium-hafnium)10.1361/105497102770331703 ↗
39. In-situ formation of titanium carbide in copper-titanium-carbon system: a review10.1016/j.powtec.2022.117389 ↗
40. High fracture toughness of HfC through nano‐scale templating and novel sintering aids10.1111/jace.15956 ↗
41. Vacancy‐induced and two‐phonon raman scattering in ZrCx, NbCx, HfCx, and TaCx10.1002/pssb.2221080225 ↗
42. Phonon spectra in TaC and HfC10.1103/PhysRevLett.25.1611 ↗
43. Synthesis and oxidation behavior of Ti-Zr-Ta (Hf) high entropy carbide nanopowders by sol-gel method10.1016/j.ceramint.2024.10.095 ↗