Preparation of High-entropy Diboride Ceramic Powders by Sol-Gel Method and Their Pyrolysis Behavior

XING Shu-wen; GONG Wei-lu; YE Li; CUI Hai-feng; ZHAO Tong

doi:10.14028/j.cnki.1003-3726.2025.25.066

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Preparation of High-entropy Diboride Ceramic Powders by Sol-Gel Method and Their Pyrolysis Behavior

更新时间：2025-06-25

- Preparation of High-entropy Diboride Ceramic Powders by Sol-Gel Method and Their Pyrolysis Behavior
- Polymer Bulletin Vol. 38, Issue 7, Pages: 1124-1132(2025)
- 作者机构：
  
  1.中国科学院化学研究所，极端环境高分子材料重点实验室，北京 100190
  2.中国科学院大学，北京 100049
- 作者简介：
- 基金信息：
- DOI：10.14028/j.cnki.1003-3726.2025.25.066
  CLC：
- Received：27 February 2025，
  
  Accepted：29 March 2025，
  
  Published Online：22 May 2025，
  
  Published：20 July 2025
- 稿件说明：
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邢叔文, 弓伟露, 叶丽, 崔海峰, 赵彤. 溶胶-凝胶法制备高熵二硼化物陶瓷粉体及其裂解行为研究. 高分子通报, 2025, 38(7), 1124–1132.

Xing S. W.; Gong W. L.; Ye L.; Cui H. F.; Zhao T. Preparation of high-entropy diboride ceramic powders by sol-gel method and their pyrolysis behavior. Polym. Bull. (in Chinese), 2025, 38(7), 1124–1132.
邢叔文, 弓伟露, 叶丽, 崔海峰, 赵彤. 溶胶-凝胶法制备高熵二硼化物陶瓷粉体及其裂解行为研究. 高分子通报, 2025, 38(7), 1124–1132. DOI： 10.14028/j.cnki.1003-3726.2025.25.066.

Xing S. W.; Gong W. L.; Ye L.; Cui H. F.; Zhao T. Preparation of high-entropy diboride ceramic powders by sol-gel method and their pyrolysis behavior. Polym. Bull. (in Chinese), 2025, 38(7), 1124–1132. DOI： 10.14028/j.cnki.1003-3726.2025.25.066.

摘要

以山梨糖醇为碳源、硼酸为硼源、金属配位共聚物(PNME)为金属源，采用溶胶-凝胶法制备出高熵二硼化物陶瓷前驱体，随后经固化和高温裂解得到元素分布均匀的(Ti

Ta)B

高熵二硼化物陶瓷粉体。为深入探究所得高熵二硼化物陶瓷前驱体的裂解行为，对前驱体在600~1900 ℃范围内热解产物的晶相组成进行了表征，并结合热力学理论计算推导出裂解反应的顺序，从而验证实验结果。实验结果显示，在前驱体裂解过程中，碳热还原反应与硼碳热还原反应同时发生，二者互为竞争反应；随着温度升高，硼碳热还原反应占据优势，所以产物中的碳化物最终转化为二硼化物，并通过固溶反应转变为单相高熵二硼化物。本研究不仅为高熵二硼化物陶瓷粉体的制备提供了新方法，而且为深入探究其裂解行为及机理提供了理论依据，对高性能陶瓷材料的应用与优化具有重要的参考价值。

Abstract

In this study

high-entropy diboride ceramic precursor was prepared by sol-gel method using sorbitol as the carbon source

boric acid as the boron source and coordinated-metal copolymer (PNME) as the metal source. Subsequently

high-entropy diboride ceramic powders (Ti

Ta)B

with uniform elemental distributions were obtained by curing and high-temperature pyrolysis. To further investigate the pyrolysis behavior of the obtained high-entropy diboride ceramic precursors

the crystalline phase compositions of the pyrolysis products obtained at 600 ℃ to 1900 ℃ were characterized

and the sequence of the pyrolysis reactions was deduced by combining with theoretical calculations of the thermodynamics theory to validate the experimental results. The results showed that during the pyrolysis process of precursors

both carbothermal reduction and boron-carbothermal reduction reactions occurred and competed with each other. With the temperature increased

the boron-carbothermal reduction reaction became dominant. Consequently

the carbides in the product were ultimately transformed into diborides and further converted into a single-phase high-entropy diboride through solid solution reaction. This study not only provides a new method for the preparation of high-entropy diborid

e ceramic powders but also offers theoretical insights into the pyrolysis behavior and mechanisms of high-entropy diboride ceramic precursors

which holds significant reference value for the application and optimization of high-performance ceramic materials.

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references

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