颗粒级配对选区激光烧结打印结合常压固相烧结制备碳化硅陶瓷性能的影响

doi:10.15541/jim20230582

无机材料学报 ›› 2024, Vol. 39 ›› Issue (7): 754-760.DOI: 10.15541/jim20230582

颗粒级配对选区激光烧结打印结合常压固相烧结制备碳化硅陶瓷性能的影响

王康龙¹^,²(), 殷杰¹(), 陈晓¹, 王力¹, 刘学建¹(), 黄政仁¹^,³

1.中国科学院上海硅酸盐研究所, 上海 200050
2.湖南大学材料科学与工程学院, 长沙 410082
3.中国科学院宁波材料技术与工程研究所, 宁波 315201

收稿日期:2023-12-18 修回日期:2024-02-17 出版日期:2024-02-22 网络出版日期:2024-02-22
通讯作者: 殷杰, 研究员. E-mail: jieyin@mail.sic.ac.cn;
刘学建, 研究员. E-mail: xjliu@mail.sic.ac.cn
作者简介:王康龙(1999-), 男, 硕士研究生. E-mail: wangkanglong@hnu.edu.cn
基金资助:
国家重点研发计划(2022YFB3706300);国家自然科学基金(U22A20129);国家自然科学基金(52073299);国家自然科学基金(52172077)

Effect of Particle Grading on Properties of Silicon Carbide Ceramics Prepared by Selective Laser Sintering Printing Combined with Solid-phase Sintering at Atmospheric Pressure

WANG Kanglong¹^,²(), YIN Jie¹(), CHEN Xiao¹, WANG Li¹, LIU Xuejian¹(), HUANG Zhengren¹^,³

1. Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. College of Materials Science and Engineering, Hunan University, Changsha 410082, China
3. Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, China

Received:2023-12-18 Revised:2024-02-17 Published:2024-02-22 Online:2024-02-22
Contact: YIN Jie, professor. E-mail: jieyin@mail.sic.ac.cn;
LIU Xuejian, professor. E-mail: xjliu@mail.sic.ac.cn
About author:WANG Kanglong (1999-), male, Master candidate. E-mail: wangkanglong@hnu.edu.cn
Supported by:
National Key R&D Program of China(2022YFB3706300);National Natural Science Foundation of China(U22A20129);National Natural Science Foundation of China(52073299);National Natural Science Foundation of China(52172077)

摘要/Abstract

摘要：

SiC陶瓷因其独特的热学、电学性能及优异的力学性能, 被广泛应用于航空航天、核能、化工、半导体等国防与工业重大领域, 但是传统的成型方法无法满足大尺寸复杂构件的制备需求。选区激光烧结(SLS)打印具有无需支撑、材料利用率高、加工效率高等优势, 能高效成型复杂陶瓷结构零部件。本研究采用颗粒级配SiC的方法, 系统研究了冷等静压(CIP)、前驱体浸渍热解(PIP)、CIP结合PIP后常压固相烧结等工艺对级配和中位径82 μm未级配体系SiC陶瓷的影响。研究发现, 级配粉末成型坯体的体积密度和抗弯强度比未级配坯体均提升了20%以上, 级配体系CIP后常压固相烧结体的相对致密度达到了90%以上, 实现了致密化烧结, 而未级配体系烧结体的相对致密度仅为89%, 这是由颗粒级配后坯体的堆积密度提升所致, 且级配烧结体的抗弯强度(136.8 MPa)比未级配(99.4 MPa)提升了37%以上。采用多次重复PIP结合常压固相烧结的方法制备高致密的SiC陶瓷, 发现SLS打印成型的坯体经四次PIP后致密度可达到CIP堆积致密的效果, 但四次PIP后常压固相烧结体的体积密度仅为2.29 g/cm³, 抗弯强度为59.6 MPa。

关键词: 碳化硅陶瓷, 颗粒级配, 选区激光烧结打印, 常压固相烧结

Abstract:

Silicon carbide (SiC) ceramics are widely used in critical industries such as aerospace, nuclear energy, chemical processing, and semiconductor manufacturing due to their unique thermal and electrical properties coupled with excellent mechanical properties. Nevertheless, conventional forming methods often fall short when it comes to producing large-sized and complex components. Selective laser sintering (SLS) printing has the advantages of no support, high material utilization, high processing efficiency, etc., endowing it suitable for the precise fabrication of ceramic structural components with complicated shape. Here, the particle grading approach was employed to systematically investigate the impacts of processes such as cold isostatic pressing (CIP), precursor impregnation pyrolysis (PIP), and the combination of CIP with PIP followed by solid-phase sintering at atmospheric pressure. The results revealed that the graded powders significantly enhanced both the bulk density and the flexural strength of the formed body by over 20% compared to non-graded systems. Relative density of the graded system after CIP and subsequent solid-phase sintering at atmospheric pressure was over 90%, confirming successful densification during sintering. In contrast, the non-graded sintered body only achieved a density of 89%. Implementation of the particle grading led to an increase in bulk density, and it was beneficial for achieving higher densification during sintering. Consequently, the flexural strength of the grading-sintered body was significantly improved, reaching 136.8 MPa—a gain of over 37% compared to the non-graded counterpart whose flexural strength was only 99.4 MPa. Meanwhile, high-density SiC ceramics could be achieved by repeating PIP for four cycles combined with solid-phase sintering of which SiC ceramics density was comparable to that of CIP compacts. However, the bulk density of solid-phase sintered body after four PIP cycles was only 2.29 g/cm³, which was accompanied by a flexural strength of 59.6 MPa.

Key words: SiC ceramic, particle grading, selective laser sintering printing, solid-phase sintering at atmospheric pressure

中图分类号:

TQ174

王康龙, 殷杰, 陈晓, 王力, 刘学建, 黄政仁. 颗粒级配对选区激光烧结打印结合常压固相烧结制备碳化硅陶瓷性能的影响[J]. 无机材料学报, 2024, 39(7): 754-760.

WANG Kanglong, YIN Jie, CHEN Xiao, WANG Li, LIU Xuejian, HUANG Zhengren. Effect of Particle Grading on Properties of Silicon Carbide Ceramics Prepared by Selective Laser Sintering Printing Combined with Solid-phase Sintering at Atmospheric Pressure[J]. Journal of Inorganic Materials, 2024, 39(7): 754-760.

图/表 9

表1 SLS打印参数

Table 1 Parameters for SLS printing

Laser power/ W	Hatch distance/ μm	Scanning speed/ (mm·s^-1)	Preheating temperature/ ℃	Layer thickness/ mm	Energy density / (J·mm^-3)
35	80	7620	60	0.1	0.057

表2 实验工艺制度缩写

Table 2 Abbreviations for experimental procedures

Abbreviation	Experimental procedure
SLS-SSiC	Solid-phase sintering at atmospheric pressure after SLS
CIP-SSiC	Solid-phase sintering at atmospheric pressure after SLS and CIP
CIP-PIP-1-SSiC	Solid-phase sintering at atmospheric pressure after SLS and CIP followed by PIP once
CIP-PIP-2-SSiC	Solid-phase sintering at atmospheric pressure after SLS and CIP followed by PIP twice
PIP-4-SSiC	Solid-phase sintering at atmospheric pressure after SLS and PIP four times

图1 SLS打印制备SiC陶瓷的工艺流程

Fig. 1 Flow chart of SiC ceramics preparation by SLS printing

图2 SLS打印成型SiC素坯脱黏后的性能

Fig. 2 Properties of SLS printed SiC green bodies after debonding (a) Bulk density; (b) Flexural strength

表3 不同工艺对级配和D50=82 μm体系SiC陶瓷性能的影响

Table 3 Effect of different processes on properties of SiC ceramics with gradation and D50=82 μm systems

Sample		Bulk density/ (g·cm^-3)	Open porosity/%	Flexural strength/MPa	Elastic modulus/GPa	Fracture toughness/(MPa·m^1/2)
SLS-SSiC	Gradation	1.41	52.16	3.49	—	—
SLS-SSiC	D₅₀=82 μm	1.30	54.23	3.12	—	—
CIP-SSiC	Gradation	2.54	6.37	136.8	127	1.98
CIP-SSiC	D₅₀=82 μm	2.29	10.01	99.4	111	1.72
CIP-PIP-1-SSiC	Gradation	2.67	7.43	142.1	118	2.16
CIP-PIP-1-SSiC	D₅₀=82 μm	2.53	7.05	120.5	107	2.09
CIP-PIP-2-SSiC	Gradation	2.69	7.27	150.3	106	2.04
CIP-PIP-2-SSiC	D₅₀=82 μm	2.51	7.59	123.9	113	2.11
PIP-4-SSiC	Gradation	2.29	20.2	59.6	89	1.37
PIP-4-SSiC	D₅₀=82 μm	2.15	19.8	55.7	75	1.19

图3 样品的孔径分布及对应SEM照片

Fig. 3 Pore size distribution and corresponding SEM images of the samples D50=82 μm system: (a) SLS, (c) CIP, (e) CIP-PIP-1, (g) CIP-PIP-2, (i) PIP-4 Graded system: (b) SLS, (d) CIP, (f) CIP-PIP-1, (h) CIP-PIP-2, (j) PIP-4

图4 级配和D50=82 μm体系CIP-PIP-2-SSiC烧结体的X、Y、Z轴收缩率

Fig. 4 X, Y, and Z-axis shrinkage rate of CIP-PIP-2-SSiC for gradation and D50=82 μm systems Colorful figure is available on website

图5 各阶段烧结体SEM照片

Fig. 5 SEM images of sintered bodies in each stage D50=82 μm system: (a) SLS-SSiC, (c) CIP-SSiC, (e) CIP-PIP-2-SSiC, (g) PIP-4-SSiC Graded system: (b) SLS-SSiC, (d) CIP-SSiC, (f) CIP-PIP-2-SSiC, (h) PIP-4-SSiC

表4 本工作制备的SiC陶瓷致密度和抗弯强度与文献报道对比

Table 4 Comparison of densities and flexural strengths of SiC ceramics prepared in this work with literature reports

Sample	Bulk density / (g·cm^-3)	Open porosity/%	Flexural strength/MPa	Ref.
CIP-SSiC PIP-4-SSiC	2.67	6.37	136.8	This work
CIP-SSiC PIP-4-SSiC	2.29	20.2	59.6	This work
CIP-SSiC	—	7.02	56.2	[20]
CIP	2.12	33.88	59.47	[21]
PIP-7	—	10	20	[22]
PIP-8	2.45	5.05	152.6	[23]

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颗粒级配对选区激光烧结打印结合常压固相烧结制备碳化硅陶瓷性能的影响

Effect of Particle Grading on Properties of Silicon Carbide Ceramics Prepared by Selective Laser Sintering Printing Combined with Solid-phase Sintering at Atmospheric Pressure

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