硅酸盐学报

石墨烯含量对墨水直写SiC基复合材料微观结构及性能的影响

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李保岩 ¹ , 刘洪军 ¹^,² , 任骏 ¹ , 刘一林 ¹ , 李亚敏 ¹^,²

硅酸盐学报 | 研究论文 2026,54(9): 2961-2973

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硅酸盐学报 |研究论文 2026 , 54 (9) : 2961 -2973

石墨烯含量对墨水直写SiC基复合材料微观结构及性能的影响

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李保岩¹, 刘洪军¹^,², 任骏¹, 刘一林¹, 李亚敏¹^,²

作者信息

^1．兰州理工大学材料科学与工程学院，兰州 730050

^2．兰州理工大学，省部共建有色金属先进加工与再利用国家重点实验室，兰州 730050

通讯作者:

刘洪军（1974—），男，博士，教授。

作者简介:

李保岩（1999—），男，硕士研究生。

Graphene Content-Dependent Microstructure and Properties in Direct-Ink-Writing of SiC Composites

Baoyan LI¹, Hongjun LIU¹^,², Jun REN¹, Yilin LIU¹, Yamin LI¹^,²

Affiliations

^1.School of Materials Science and Engineering, Lanzhou University of Technology, Lanzhou 730050, China

^2.State Key Laboratory for Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, China

Corresponding Author:

{LIU} Hongjun (1974-), Male, Ph. D., Professor. E-mail: liuhongjun@lut.edu.cn

LI Baoyan (1999-), Male, Master candidate. E-mail: 15612967399@163.com

出版时间: 2026-08-19 doi: 10.14062/j.issn.0454-5648.20250896

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摘要

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为克服陶瓷及其复合材料在复杂结构成型与微观孔隙调控方面的困难，本工作采用墨水直写结合高温热解方法制备了石墨烯/SiC基复合材料。石墨烯的含量、分布与取向是影响其性能的关键因素，因此，本工作系统探究了石墨烯含量对石墨烯/SiC_p/PCS浆料打印成形性、挤出丝微观结构、点阵结构热解收缩行为、力学性能与导电性的影响，为实现结构设计、制备工艺和性能的一体化调控提供保障。结果表明：随着石墨烯含量增加，素坯打印精度与结构成形性提高；石墨烯片层在挤出丝中形成从中心至边缘的梯度取向分布，点阵结构热解收缩率随石墨烯含量提高而逐渐降低；当石墨烯/SiC_p复合粉体中石墨烯含量为25%时，所制备的复合材料综合性能最优，挤出丝抗拉强度、点阵抗压强度和单根丝电导率分别达到1.855 MPa、8.65 MPa和247.1 S/m，本工作为开发适用于极端工作环境的多功能轻质陶瓷材料提供了新的工艺方案。

关键词

3D打印 / 墨水直写 / 多孔陶瓷 / 碳化硅基复合材料 / 石墨烯

Abstract

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Introduction

Graphene/SiC composites are widely used in the fields of filtration, biomedicine, catalysis, microwave absorption, energy storage and chemical sensing. 3D printing technology can realize the design of fine feature change and integrated molding complex geometric structure in the preparation of porous ceramic materials, especially the slurry direct writing process (DIW). The physical properties and other functions of composites strongly depend on the microstructure obtained during processing, so these phenomena must be systematically investigated to design and produce reliable materials, especially for 3D printing applications. In this paper, graphene/SiC matrix composites were prepared by DIW technology, and their printing accuracy, microstructure, pyrolysis behavior, mechanical properties and electrical properties were investigated.

Methods

SiC powder with an average particle size of 3.2 μm was used as a matrix of the composite. A graphene powder with average particle size of 8 μm, bulk density of 0.08-0.13 g/mL, thickness of 1-3 layers and purity of 99% was a reinforced phase. Polycarbosilane (PCS) with a molar mass of about 1500 g/mol was used as a precursor to prepare ceramic slurry. The diameter of extrusion nozzle was 0.55 mm, the layer thickness was 0.48 mm, and the printing speed was 6 mm/s, which was used for DIW. The morphology and distribution characteristics of graphene in the cross section of graphene/SiC_p composite extruded wire were characterized by scanning electron microscopy (SEM). The phase composition of graphene/SiC matrix composites after pyrolysis was determined by X-ray diffraction (XRD) with Cu K_α - ray (λ), the scanning rate of 10 °/min, and the scanning angle (2θ) of 20°-80°. The Raman spectra of graphene/SiC matrix composite samples were analyzed by Raman spectroscopy in a scanning range of 1000-2000 cm^-1, power of 10 MW, and laser wavelength of 532 nm. The resistance of single wire after pyrolysis was measured by inductance capacitance meter (LCR) and the conductivity was calculated. The tensile test was carried out in an electronic universal testing machine, the tensile rate was 0.1 mm/min, and the tensile strength was calculated. A universal testing machine was used to carry out compression test on the pyrolytic frame samples, and the displacement speed was 0.2 mm/min. The compressive strength was calculated.

Results and discussion

The experimental results of single-layer printing and dot matrix structure printing show that all three slurries exhibit a good extrusion forming ability. In addition, increasing the graphene content in the slurry can suppress the spreading deformation of extruded filaments, reduce the line width, and make it closer to the extrusion diameter, which is helpful for high-precision printing. The SEM images of the extruded filament cross-section show that the graphene layers form a certain degree of orientation in the matrix. In the central region, there is a relatively random and irregular arrangement, and the orientation of graphene sheets is most pronounced in the edge region. At the central axis, the shear rate is rather low, the orientation torque is weak, and the graphene layers are randomly distributed mainly due to the non-uniform shear flow field experienced by the slurry in the extrusion port. In the edge region, the shear rate is extremely high, forcing the graphene layers to deflect and arrange along the streamline direction. The pyrolysis process forms a porous structure, and the graphene layers are well preserved. In the Raman spectra, the I_D/I_G value of 25G is the smallest, and the higher the graphene content, the lower the average defect density of graphene. The higher the graphene content, the higher the tensile strength of the extruded filament and the compressive strength of the lattice structure.

Conclusions

The DIW process using graphene/SiC_p/PCS composite slurry could achieve the preparation of lattice grid structure green bodies. The printing ability of the slurry improved with the increase of graphene content. In the DIW printing process, graphene layers were oriented and arranged along the extrusion direction in the extrusion filament, forming an orientation gradient structure from the center to the edge, and the higher the content, the more significant the orientation characteristics and gradient. Graphene improved the strength of composite materials via constructing gradient orientation distribution, enhancing interfacial bonding, and exerting crack bridging effect. Also, it significantly improved the conductivity of porous SiC based composite materials. At the graphene content of 25%, the tensile strength of the extruded filament and the compressive strength of the lattice structure could be the maximum values, and the electrical conductivity of a single filament reached 247.1 S/m, providing a feasible material system and technical path for the development of multifunctional lightweight ceramic materials for extreme environmental applications.

Key words

3D printing / slurry direct writing / porous ceramics / silicon carbide-based composites / graphene

引用本文

李保岩, 刘洪军, 任骏, 刘一林, 李亚敏. 石墨烯含量对墨水直写SiC基复合材料微观结构及性能的影响. 硅酸盐学报, 2026 , 54 (9) : 2961 -2973 . DOI: 10.14062/j.issn.0454-5648.20250896

Baoyan LI, Hongjun LIU, Jun REN, Yilin LIU, Yamin LI. Graphene Content-Dependent Microstructure and Properties in Direct-Ink-Writing of SiC Composites[J]. Journal of the Chinese Ceramic Society, 2026 , 54 (9) : 2961 -2973 . DOI: 10.14062/j.issn.0454-5648.20250896

基金

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国家自然科学基金(52062029)
甘肃省自然科学基金(25JRRA094)

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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.0454-5648.20250896

接收时间：2025-12-08
首发时间：2026-10-22
出版时间：2026-08-19

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出版历史

收稿日期：2025-12-08
修回日期：2026-01-07

基金

国家自然科学基金(52062029)

甘肃省自然科学基金(25JRRA094)

作者信息

^1．兰州理工大学材料科学与工程学院，兰州 730050

^2．兰州理工大学，省部共建有色金属先进加工与再利用国家重点实验室，兰州 730050

通讯作者:

刘洪军（1974—），男，博士，教授。

参考文献

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https://castjournals.cast.org.cn/joweb/gsyxb/CN/10.14062/j.issn.0454-5648.20250896

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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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