Effect of C-to-SiC Ratio on the Microstructure and Properties of SiC Ceramics Prepared by a Hybrid Method of DIW and RMI

Abstract

Silicon carbide (SiC) ceramic materials were fabricated via the combination of direct ink writing (DIW) and reactive melting infiltration (RMI) techniques. The effects of the carbon black-to-silicon carbide (C-to-SiC) ratio on the rheological properties of the slurry, as well as the microstructure and mechanical performance of the resulting SiC ceramics were systematically investigated. The experimental results demonstrate that, as the carbon black content increases from 9vol% to 18vol%, the viscosity, yield stress, and equilibrium modulus of the slurry all exhibit a corresponding increase, contributing to enhanced dimensional precision of the green body. After high-temperature heat treatment, the linear shrinkage in the vertical direction decreases from 8.59% to 6.88%. The prepared SiC ceramic materials display densities in the range of 2.70 – 2.85 g/cm³ and porosities ranging from 0.39vol% to 3.99vol%, indicating an improvement in densification. With the increase in carbon black content, the free silicon content in the ceramics decrease, while the residual carbon content increase. Mechanical testing results reveal that the SiC ceramics fabricated from slurries with 12vol% and 15vol% carbon black content achieve the highest flexural strength and modulus, reaching 287.74 MPa and 274.10 GPa, respectively. A reasonable C-to-SiC ratio helps to generate more SiC content (especially nanoscale β-SiC) and retain less residual Si, thereby forming a finer microstructure. Combined with less residual C, higher mechanical properties can be obtained.

Keywords

SiC ceramics / direct ink writing / reactive melting infiltration / microstructure / mechanical properties

References

[1] Bhuvanesh KM, Sathiya P. Methods and Materials for Additive Manufacturing: A Critical Review on Advancements and Challenges[J]. Thin-Walled Structures, 2021, 159: 107 228

[2] Wang KL, Yin J, Chen X, et al. . Advances on Direct Selective Laser Printing of Ceramics: An Overview[J]. Journal of Alloys and Compounds, 2024, 975: 172 821

[3] Alghamdi SS, John S, Choudhury NR, et al. . Additive Manufacturing of Polymer Materials: Progress, Promise and Challenges[J]. Polymers, 2021, 13(5): 753

[4] Zhang Y, Wu LM, Guo XY, et al. . Additive Manufacturing of Metallic Materials: A Review[J]. Journal of Materials Engineering and Performance, 2018, 27(1): 1-13

[5] Dai JL, Xue BY, Qian Q, et al. . 3D-printable Boron Nitride/Polyacrylic Hydrogel Composites with High Thermal Conductivities[J]. Journal of Wuhan University of Technology-Mater. Sci. Ed., 2024, 39(5): 1 303-1 310

[6] Fu H, Zhu W, Xu ZF, et al. . Effect of Silicon Addition on the Microstructure, Mechanical and Thermal Properties of C_f/SiC Composite Prepared via Selective Laser Sintering[J]. Journal of Alloys and Compounds, 2019, 792: 1 045-1 053

[7] Zhu SX, Michael HC, Singh M. Additive Manufacturing of Silicon Carbide-based Ceramics by 3-D Printing Technologies[J]. The American Ceramic Society, 2015, 138: 956 193

[8] Mei H, Yan YK, Feng LP, et al. . First Printing of Continuous Fibers into Ceramics[J]. Journal of the American Ceramic Society, 2019, 102(6): 3 244-3 255

[9] Klosterman DA, Chartoff RP, Osborne NR, et al. . Development of a Curved Layer LOM Process for Monolithic Ceramics and Ceramic Matrix Composites[J]. Papid Prototyping Journal, 1999, 5(2): 61-71

[10] Wang CL, Zhang JY, Lei LW. Effect of Particle Size on Silicon Nitride Ceramic Slurry by Stereolithography[J]. Journal of Wuhan University of Technology-Mater. Sci. Ed., 2023, 38(3): 514-519

[11] Lu ZL, Xia YL, Miao K, et al. . Microstructure Control of Highly Oriented Short Carbon Fibres in SiC Matrix Composites Fabricated by Direct Ink Writing[J]. Ceramics International, 2019, 45(14): 17 262-17 267

[12] Qian Q, Xue BY, He WH, et al. . Bioprocessing Inspired Enzyme-induced Mineralization of 3D Printed Hydrogels[J]. Journal of Wuhan University of Technology-Mater. Sci. Ed., 2025, 40(4): 939-945

[13] Wang WQ, Bai XJ, Zhang L, et al. . Additive Manufacturing of C_sf/SiC Composites with High Fiber Content by Direct Ink Writing and Liquid Silicon Infiltration[J]. Ceramics International, 2022, 48(3): 3 895-3 903

[14] Xia YL, Lu ZL, Cao JW, et al. . Microstructure and Mechanical Property of C_f/SiC Core/shell Composite Fabricated by Direct Ink Writing [J]. Scripta Materialia, 2019, 165: 84-88

[15] Xiong HW, Chen HH, Chen ZK, et al. . 3D-SiC Decorated with SiC Whiskers: Chemical Vapor Infiltration on the Porous 3D-SiC Lattices Derived from Polycarbosilane-based Suspensions[J]. Ceramics International, 2020, 46(5): 6 234-6 242

[16] Li W, Cui CC, Bao JX, et al. . Properties Regulation of SiC Ceramics Prepared via Stereolithography Combined with Reactive Melt Infiltration Techniques[J]. Ceramics International, 2021, 47(24): 33 997-34 004

[17] Lu J, Ni DW, Liao CJ, et al. . Fabrication and Microstructure Evolution of C_sf/ZrB₂-SiC Composites via Direct Ink Writing and Reactive Melt Infiltration[J]. Journal of Advanced Ceramics, 2021, 10(6): 1 371-1 380

[18] Xiong HW, Chen HH, Zhao LZ, et al. . SiC_w/SiCp Reinforced 3D-SiC Ceramics Using Direct Ink Writing of Polycarbosilane-based Solution: Microstructure, Composition and Mechanical Properties[J]. Journal of the European Ceramic Society, 2019, 39(8): 2 648-2 657

[19] Shahzad A, Lazoglu I. Direct Ink Writing (DIW) of Structural and Functional Ceramics: Recent Achievements and Future Challenges[J]. Composites Part B-Engineering, 2021, 225: 109 249

[20] Zhang H, Yang Y, Liu B, et al. . The Preparation of SiC-based Ceramics by one Novel Strategy Combined 3D Printing Technology and Liquid Silicon Infiltration Process[J]. Ceramics International, 2019, 45(8): 10 800-10 804

[21] Yin YH, Wan F, Zhen M, et al. Effect of ISOBAM Content in Slurry on Preparation, Microstructure, and Mechanical Properties of SiC Ceramics Fabricated by Combining Direct Ink Writing and Liquid Silicon Infiltration[J]. Ceramics International, 2023: 5 083–5 091

[22] Wan F, Pirzada TJ, Liu RJ, et al. . Microstructure Characterization by X-Ray Computed Tomography of C/C-SiC Ceramic Composites Fabricated with Different Carbon Fiber Architectures[J]. Applied Composite Materials, 2019, 26(4): 1 247-1 260

[23] Del MBL, Ginebra MP. Rheological Characterisation of Ceramic Inks for 3D Direct Ink Writing: A Review[J]. Journal of the European Ceramic Society, 2021, 41(16): 18-33

[24] Larson CM, Choi JJ, Gallardo PA, et al. . Direct Ink Writing of Silicon Carbide for Microwave Optics[J]. Advanced Engineering Materials, 2016, 18(1): 39-45

[25] Smay JE, Nadkarni Sarosh S, Xu J. Direct Writing of Dielectric Ceramics and Base Metal Electrodes[J]. International Journal of Applied Ceramic Technology, 2007, 4(1): 47-52

[26] Sun QL, Peng Y, Cheng H, et al. . Direct Ink Writing of 3D Cavities for Direct Plated Copper Ceramic Substrates with Kaolin Suspensions[J]. Ceramics International, 2019, 45(9): 12 535-12 543

[27] An T, Hwang KT, Kim JH, et al. . Extrusion-based 3D Direct Ink Writing of NiZn-ferrite Structures with Viscoelastic Ceramic Suspension [J]. Ceramics International, 2020, 46(5): 6 469-6 476

[28] Raghavan SR, Khan SA. Shear-Thickening Response of Fumed Silica Suspensions under Steady and Oscillatory Shear[J]. Journal of colloid and interface science, 1997, 185(1): 57-67

[29] Roman MB, Moyano JJ, Perez-Coll D, et al. . Polymer-derived Ceramic/graphene Oxide Architected Composite with High Electrical Conductivity and Enhanced Thermal Resistance[J]. Journal of the European Ceramic Society, 2018, 38(5): 2 265-2 271

[30] Lamon J. A Micromechanics-based Approach to the Mechanical Behavior of Brittle-matrix Composites[J]. Composites Science and Technology, 2001, 61(15): 2 259-2 272

[31] Li S, Zhang Y, Han JC, et al. . Effect of Carbon Particle and Carbon Fiber on the Microstructure and Mechanical Properties of Short Fiber Reinforced Reaction Bonded Silicon Carbide Composite[J]. Journal of the European Ceramic Society, 2013, 33(4): 887-896

[32] Kumar S, Kumar A, Devi R, et al. . Capillary Infiltration Studies of Liquids into 3D-stitched C-C Preforms Part B: Kinetics of Silicon Infiltration[J]. Journal of the European Ceramic Society, 2009, 29(12): 2 651-2 657

[33] Tang WZ, Zhao T, Dou R, et al. . Fabrication of High-strength Si/SiC Composites with Low Shrinkage Rates via Vat Photopolymerization Technology and Liquid Silicon Infiltration[J]. Additive Manufacturing, 2022, 59: 103 168

[34] Zhang JX, Jiang DL, Qin SY, et al. . Fracture Behavior of Laminated SiC Composites[J]. Ceramics International, 2004, 30(5): 697-703

[35] Gilbert CJ, Cao JJ, De Jonghe LC, et al. . Crack-growth Resistance-curve Behavior in Silicon Carbide: Small Versus Long Cracks[J]. Journal of the American Ceramic Society, 1997, 80(9): 2 253-2 261

[36] Chen Z, Zeng LF. Pressurelessly Sintering Silicon Carbide with Additives of Holmium Oxide and Alumina[J]. Materials Research Bulletin, 1995, 30(3): 265-270

[37] Ma RZ, Wu J, Wei BQ, et al. . Processing and Properties of Carbon Nanotubes-nano-SiC Ceramic[J]. Journal of Materials Science, 1998, 33(21): 5 243-5 246

[38] Singh M, Salem JA. Mechanical Properties and Microstructure of Biomorphic Silicon Carbide Ceramics Fabricated from Wood Precursors [J]. Journal of the European Ceramic Society, 2002, 22(14–15): 2 709-2 717

[39] Li CR, Li S, An D, et al. . Microstructure and Mechanical Properties of Spark Plasma Sintered SiC Ceramics Aided by B₄C[J]. Ceramics International, 2020, 46(8): 10 142-10 146

RIGHTS & PERMISSIONS

Wuhan University of Technology and Springer-Verlag GmbH Germany, Part of Springer Nature