硅酸盐学报

烧结温度对碳纳米纤维/陶瓷复合电阻材料性能的影响

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孙文星 ¹ , 李端姣 ¹ , 王云龙 ² , 钟振鑫 ² , 丁宇东 ³ , 丁冬海 ³ , 种小川 ³ , 肖国庆 ³

硅酸盐学报 | 研究论文 2026,54(9): 3150-3160

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硅酸盐学报 |研究论文 2026 , 54 (9) : 3150 -3160

烧结温度对碳纳米纤维/陶瓷复合电阻材料性能的影响

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孙文星¹, 李端姣¹, 王云龙², 钟振鑫², 丁宇东³, 丁冬海³, 种小川³, 肖国庆³

作者信息

^1．广东电网有限责任公司，广州 510699

^2．广东电网有限责任公司惠州供电局，广东惠州 516000

^3．西安建筑科技大学材料科学与工程学院，西安 710055

通讯作者:

肖国庆（1967—），男，博士，教授。

作者简介:

孙文星（1987—），博士，正高级工程师。

Effect of Sintering Temperature on Properties of Carbon Nanofiber/Ceramic Composite Resistive Materials

Wenxing SUN¹, Duanjiao LI¹, Yunlong WANG², Zhenxin ZHONG², Yudong DING³, Donghai DING³, Xiaochuan CHONG³, Guoqing XIAO³

Affiliations

^1.Guangdong Power Grid Co., Ltd., Guangzhou 510699, China

^2.Huizhou Power Supply Bureau, Guangdong Power Grid Co., Ltd., Huizhou 516000, Guangdong, China

^3.School of Materials Science and Engineering, Xi'an University of Architecture and Technology, Xi'an 710055, China

Corresponding Author:

{XIAO} Guoqing (1967-), male, Ph.D., Professor. E-mail: xiaoguoqing@xauat.edu.cn

SUN Wenxing (1987-), male, Ph.D., Senior Engineer. E-mail: 13922724599@139.com

出版时间: 2026-08-18 doi: 10.14062/j.issn.0454-5648.20250855

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摘要

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采用预合成的碳纳米纤维/铝酸钙复合粉（CNFs/CAC）为导电填料，经干法球磨、造粒、成型及埋碳烧结工艺，制备了碳纳米纤维/陶瓷复合电阻材料，系统研究了烧结温度（1300~1500 ℃）对复合电阻材料物相组成、微观结构、致密度、力学性能及导电性能的影响。结果显示：随着烧结温度的升高，材料致密度和抗压强度逐渐提高，电阻率呈先减小后增大的趋势，1400 ℃烧结后样品综合性能最佳，体积密度为2.23 g/cm³，抗压强度达189 MPa，电阻率为476 Ω·cm，电阻温度系数为-0.14%/℃，I_D/I_G值最小为0.85。预合成的碳纳米纤维/铝酸钙复合粉不仅在陶瓷基体中形成均匀连续的导电网络，而且通过促进裂纹偏转、分支提升了导电陶瓷的力学性能，这对复合电阻材料中高分散性碳系导电填料的引入及其综合性能的提升提供了新的思路。

关键词

碳纳米纤维/铝酸钙复合粉 / 复合导电陶瓷 / 烧结温度 / 力学性能 / 电性能

Abstract

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Introduction

Carbon-ceramic composite materials, which seamlessly integrate the exceptional mechanical strength, high-temperature tolerance, corrosion resistance, and thermal shock resistance of ceramics with the superior electrical conductivity of carbon-based materials, exhibit an immense application potential in various fields. They are particularly critical in the manufacturing of closing resistors for ultra-high voltage (UHV) circuit breakers. Under extreme service environments characterized by high temperatures, high pressures, intense electromagnetic fields, and the corrosive byproducts of SF₆ decomposition, these key components face stringent performance requirements, including high mechanical strength, controllable and stable resistivity, a low temperature coefficient of resistance (TCR), and remarkable thermal shock resistance. Conventional conductive ceramics predominantly utilize nano-carbon fillers such as carbon black, carbon nanotubes, carbon fibers, and graphene. However, these nano-sized carbon materials typically suffer from severe agglomeration, poor interfacial wettability with the ceramic matrix, and high susceptibility to oxidation during the high-temperature sintering process, severely limiting their structural integrity and functional stability. To overcome these bottlenecks, this study was to introduce a pre-synthesized carbon nanofiber/calcium aluminate composite powder (CNFs/CAC) as an innovative conductive filler. The implementation of CNFs/CAC could effectively mitigate the agglomeration of nano-sized carbons. Furthermore, the unique microstructural architecture of CNFs/CAC could facilitate the construction of a robust three-dimensional carbon conductive network and leverage calcium aluminate as an efficient sintering aid to promote particle rearrangement and matrix densification, thereby lowering the required sintering temperature. Crucially, the CAC shell encapsulating the carbon nanofibers significantly retarded their oxidation at elevated temperatures. Sintering temperature acts as a paramount thermodynamic variable governing densification kinetics, phase transformations, and microstructural evolution. Inadequate temperatures fail to provide a sufficient driving force for grain boundary migration, resulting in excessive porosity and deteriorated mechanical properties. Conversely, excessive temperatures provoke abnormal grain growth, disruption of the percolation network, and pronounced oxidation of the carbon phase. Therefore, this study was to investigate the evolution mechanisms of phase composition, microstructure, mechanical strength, and electrical properties of CNF/ceramic composites at a sintering temperature range of 1300-1500 ℃, to optimize processing parameters and provide a robust theoretical foundation for the fabrication of high-performance composite conductive ceramics.

Methods

The ceramic matrix raw materials comprised bauxite, kaolin, and potassium feldspar, while the conductive filler was a laboratory-synthesized CNFs/CAC powder. The introduction of CaO via the CAC into the Al₂O₃-SiO₂ system deliberately promoted the formation of anorthite, subsequently generating a liquid phase that substantially enhanced the liquid-phase sintering process. The preparation commenced with mixing the raw materials (i.e., 60% bauxite, 22% kaolin, 18% potassium feldspar, and 1.5% CNFs/CAC) by dry ball milling in a ball-to-material mass ratio of 2∶1 at 320 r/min for 9 h. The homogeneous mixture was then granulated through a 20-mesh sieve to obtain granules of approximately 0.85 mm in diameter. These granules were uniaxially pressed into cylindrical green bodies (20 mm in diameter and 20 mm in height) at 50 MPa, followed by cold isostatic pressing (CIP) at 200 MPa for 300 s to ensure initial uniformity. The compacts were dried at 300 ℃ for 2 h and subsequently sintered in a carbon-embedded graphite crucible atmosphere. The sintering profile was systematically varied from 1300 ℃ to 1500 ℃. The phase compositions were analyzed by X-ray diffraction (XRD), and microstructural morphology alongside elemental carbon distribution was determined by field emission scanning electron microscopy (FESEM) with energy dispersive spectrometry (EDS). The macroscopic physical properties, including apparent porosity and bulk density, were measured by the Archimedes method. The compressive strength was tested by a universal testing machine, while the volume resistivity and TCR were evaluated by a precise digital LCR meter coupled with a controlled electro-thermal drying oven.

Results and discussion

The sintering temperature fundamentally dictates the structural evolution and functional performance of carbon nanofiber/ceramic composite resistive materials at 1300-1500 ℃. Elevated temperatures facilitate a liquid-phase formation, drastically reducing apparent porosity from 31% to 23% and boosting bulk density from 2.11 g/cm³ to 2.31 g/cm³. Nevertheless, exceeding 1400 ℃ exacerbates carbon depletion via the Boudouard reaction, irreversibly disrupting the conductive pathways and spiking resistivity. The material achieves its optimal comprehensive properties precisely at 1400 ℃, yielding a compressive strength of 189 MPa, a minimal resistivity of 476 Ω·cm, a highly stable NTC behavior with a TCR of -0.14%/℃, and a lowest I_D/I_G ratio of 0.85, reflecting an exceptional graphitic ordering. The incorporation of the pre-synthesized CNFs/CAC filler serves a dual purpose. It establishes a highly uniform and continuous conductive percolating network at minimal doping levels, and it synergistically has fracture toughness via inducing sophisticated crack deflection and bridging mechanisms, offering a robust paradigm for advanced composite electro-ceramics.

Key words

carbon nanofiber/calcium aluminate composite powder / composite conductive ceramics / sintering temperature / mechanical properties / electrical properties

引用本文

孙文星, 李端姣, 王云龙, 钟振鑫, 丁宇东, 丁冬海, 种小川, 肖国庆. 烧结温度对碳纳米纤维/陶瓷复合电阻材料性能的影响. 硅酸盐学报, 2026 , 54 (9) : 3150 -3160 . DOI: 10.14062/j.issn.0454-5648.20250855

Wenxing SUN, Duanjiao LI, Yunlong WANG, Zhenxin ZHONG, Yudong DING, Donghai DING, Xiaochuan CHONG, Guoqing XIAO. Effect of Sintering Temperature on Properties of Carbon Nanofiber/Ceramic Composite Resistive Materials[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (9) : 3150 -3160 . DOI: 10.14062/j.issn.0454-5648.20250855

基金

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高压断路器用国产化合闸电阻研制与应用(031300KC23110008)

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2026年第54卷第9期

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文章信息

doi: 10.14062/j.issn.0454-5648.20250855

接收时间：2025-11-19
首发时间：2026-10-22
出版时间：2026-08-18

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收稿日期：2025-11-19
修回日期：2025-12-14

基金

高压断路器用国产化合闸电阻研制与应用(031300KC23110008)

作者信息

^1．广东电网有限责任公司，广州 510699

^2．广东电网有限责任公司惠州供电局，广东惠州 516000

^3．西安建筑科技大学材料科学与工程学院，西安 710055

通讯作者:

肖国庆（1967—），男，博士，教授。

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20250855

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
				栓菌属 Trametes	5	2.39

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