非氧化物陶瓷光固化增材制造研究进展及展望

doi:10.15541/jim20210705

无机材料学报 ›› 2022, Vol. 37 ›› Issue (3): 267-277.DOI: 10.15541/jim20210705 CSTR: 32189.14.10.15541/jim20210705

所属专题：增材制造专题(2022)；【制备方法】3D打印(202409)

非氧化物陶瓷光固化增材制造研究进展及展望

杨勇¹^,²(), 郭啸天¹^,³, 唐杰¹^,², 常浩天¹^,³, 黄政仁¹^,², 胡秀兰³()

1.中国科学院上海硅酸盐研究所, 高性能陶瓷和超微结构国家重点实验室, 上海 200050
2.中国科学院大学材料科学与光电技术学院, 北京 100049
3.南京工业大学材料科学与工程学院, 南京 211816

收稿日期:2021-11-15 修回日期:2021-12-23 出版日期:2022-03-20 网络出版日期:2022-01-06
通讯作者: 胡秀兰, 教授. E-mail: whoxiulan@163.com
作者简介:杨勇(1974-), 男, 研究员. E-mail: yangyong@mail.sic.ac.cn
基金资助:
国家重点研发计划(2021YFB3701500);中国科学院科研装备研制项目(YZQT014)

Research Progress and Prospects of Non-oxide Ceramic in Stereolithography Additive Manufacturing

YANG Yong¹^,²(), GUO Xiaotian¹^,³, TANG Jie¹^,², CHANG Haotian¹^,³, HUANG Zhengren¹^,², HU Xiulan³()

1. State Key Laboratory of High Performance Ceramics and Superfine Microstructures, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China
2. College of Materials Science and Opto-Electronic Technology, University of Chinese Academy of Sciences, Beijing 100049, China
3. College of Materials Science and Engineering, Nanjing Tech University, Nanjing 211816, China

Received:2021-11-15 Revised:2021-12-23 Published:2022-03-20 Online:2022-01-06
Contact: HU Xiulan, professor. E-mail: whoxiulan@163.com
About author:YANG Yong (1974-), male, professor. E-mail: yangyong@mail.sic.ac.cn
Supported by:
National Key Research and Development Project(2021YFB3701500);Research Instrument Development Project of Chinese Academy of Sciences(YZQT014)

摘要/Abstract

摘要：

目前光固化3D打印技术因打印成型精度高而被广泛应用于陶瓷增材制造, 其中非氧化物陶瓷如碳化硅、氮化硅等因打印材料粉体折射率和吸光度比较高, 光固化陶瓷浆料存在分散稳定性差、入射光难穿透并产生光固化反应的固化层厚度低等问题, 导致其固含量很难提高甚至于无法打印成型。高固含量的非氧化物陶瓷打印成型成为光固化3D打印的主要难点, 吸引了广大学者对其光固化机理、粉体调控等机制进行研究。本文系统地总结了几种非氧化物陶瓷光固化浆料的制备、光固化成型、有机物去除及烧结致密化的研究工作, 并就如何对光敏树脂组成进行调节、对陶瓷粉体进行改性的几种方法进行分析与讨论, 针对性地提出创新方案来改善非氧化物陶瓷的浆料性能、光固化打印优化和致密化缺陷修复及性能提升, 最终推动大尺寸、复杂结构的非氧化物陶瓷部件光固化增材制造高精度制备技术的进步。

关键词: 光固化, 3D打印, 非氧化物, 致密化, 综述

Abstract:

At present, stereolithography 3D printing technology is widely used in ceramic additive manufacturing because of its high printing accuracy. Among them, the stereolithography ceramic slurry of non-oxide ceramics such as silicon carbide, silicon nitride, etc., has problems such as poor dispersion stability and low curing layer thickness because the incident light is difficult to penetrate and produce light curing reaction for printing high-solid-loading slurry. This is all because the refractive index and optical absorbance of the non-oxide ceramic printing material powder are relatively high. Therefore, printing and molding of high-solid-content non-oxide ceramics have become main challenges in stereolithography 3D printing, and the technology has attracted a large number of researchers to study its light-curing mechanism, powder control and other mechanisms. This paper systematically summarizes the research works of several non-oxide ceramics such as light-curing slurry preparation, light-curing molding, organic matter removal, and sintering densification. It also analyzes and discusses several methods of adjusting composition of photosensitive resin and modifying ceramic powder, and proposes innovative solutions to improve the slurry performance of non-oxide ceramics, optimize its light-curing printing, repair its densification defects and improve its performance. And the ultimate goal is to promote the advancement of high-precision preparation technology for light-curing additive manufacturing of large-size, complex-structure non-oxide ceramic parts.

Key words: stereolithography, 3D printing, non-oxide, densification, review

中图分类号:

TQ174

杨勇, 郭啸天, 唐杰, 常浩天, 黄政仁, 胡秀兰. 非氧化物陶瓷光固化增材制造研究进展及展望[J]. 无机材料学报, 2022, 37(3): 267-277.

YANG Yong, GUO Xiaotian, TANG Jie, CHANG Haotian, HUANG Zhengren, HU Xiulan. Research Progress and Prospects of Non-oxide Ceramic in Stereolithography Additive Manufacturing[J]. Journal of Inorganic Materials, 2022, 37(3): 267-277.

图/表 10

图1 光固化成型原理图[1]

Fig. 1 Prototyping mechanism of stereolithography[1]

表1 陶瓷材料的折射率和吸光度

Table 1 Refractive index and absorbance of ceramic materials

Material	Absorbance (d/μm, λ/nm)	Refractive index (d/μm, λ/nm)
Al₂O₃^{[3,4,5,6,7,8]}	0.044 (10, 405)	1.787 (2.3, 365)
ZrO₂^{[9,10,11,12,13]}	0.003 (10, 405)	Low
ZTA^[14,15,16]	Low	Low
SiO₂^[17,18,19]	Low	1.564 (2.25, 365)
SiC^{[20,21,22,23]}	0.479 (10, 405)	2.553 (12.25, 467-691)
Si₃N₄^{[20,21,22,23]}	0.180 (5, 405)	2.023 (-, 632.8)
TiO₂^{[20,21,22,23]}	Low	2.493 (-, 632.8)
BN^{[20,21,22,23]}	High	High

图2 陶瓷浆料中光传递示意图[29]

Fig. 2 Schematic drawing of the light transferring among ceramic slurry[29]

表2 不同制造方式SiC陶瓷的结构与性能

Table 2 Structure and properties of SiC ceramics obtained by different manufacturing methods

Material	Flexural strength/MPa	Elasticity modulus/GPa	Fracture toughness/ (MPa·m^1/2)
RB-SiC^[42]	≥330	≥340	≥4.1
S-SiC^[43]	349-431	308-342	3.77
RB-SiC^[44]	(305±15)	-	-
RB-SiC*^[45]	210.4	-	-
(C_f)/SiC*^[46]	262.6	-	-

图3 剪切应力下不同粒径分布SiC浆料流动示意图[49]

Fig. 3 Schematic diagram of flow of SiC slurry with different particle size distributions under shear stress[49]

图4 光固化成型制备SiC陶瓷基复合材料[52]

Fig. 4 Preparation of SiC ceramic-based composite by stereolithography[52] (a) Prepared schematic of SiC ceramic-based composite by stereolithography; (b) SEM image of SiC ceramic-based composite with a diamond volume fraction of 15%; (c) SiC ceramic-based composite

图5 数字光处理技术和液态硅渗透工艺制备Cf/SiC陶瓷复合材料[46]

Fig. 5 Preparation of Cf/SiC ceramic composites by digital light processing technology and liquid silicon infiltration process[46] (a) Prepared schematic of SiC composites; (b, c) SEM images of cross section and horizontal plane of Cf/SiC composite; (d) Sintered Cf/SiC composites

图6 数字光处理成型技术制备Si3N4-SiO2陶瓷[58]

Fig. 6 Preparation of Si3N4-SiO2 ceramics by digital light processing (DLP) technology[58] (a) Schematic synthetic reaction process of oxidation of silicon nitride at high temperature; (b) SEM image of fracture surface of Si3N4-SiO2 ceramics sintered at 1350 ℃; (c) Si3N4-SiO2 ceramics with lattice structure

图7 基于数字光处理的立体光刻法制备表面氧化氮化硅粉末复杂形状陶瓷零件[60]

Fig. 7 Fabrication of complex shaped ceramic parts with surface- oxidized Si3N4 powder via digital light processing based stereolithography method[60] (a) Green Si3N4 body of a blade; (b) Green Si3N4 body of a vertebrae; (c) Sintered body of a Si3N4 gear; (d) SEM image of sintered body of a Si3N4 gear

表3 高折射率、高吸光度陶瓷的光固化成型和烧结性能比较

Table 3 Comparison of molding and sintering performances in stereolithography of high refractive index and high absorbance ceramics

Material	Technology	Resin+photoinitiator	Dispersant	Powder	Cured thickness /μm	Solid content/% (in volume)	Bending strength /MPa	Ref.
SiC	DLP	HDDA+DVE-3+ TPO	KOS110	15 μm SiC	78	30	-	[29]
SiC	DLP	HDDA+TMPTA+TPO	KOS110+ 17000	15 μm SiC+ ~40 nm SiC	-	45	165.2	[48]
SiC	DLP	ACMO+HDDA+ TMPTA+BAPO	4200	10 μm SiC	≈60	40	50.18	[49]
Al₂O₃-Si₃N₄	SLA	TMPTA+HDDA+ Irgacure 184	PEG200+ glycerol	1 μm Al₂O₃+ 200 nm Si₃N₄	40	47	-	[57]
SiO₂-Si₃N₄	DLP	TMPTA+Irgacure 184	-	3.45 μm Si₃N₄+ Y₂O₃+Al₂O₃	50-60	50	(77±5)	[58]
Si₃N₄	DLP	HDDA+TMPTA+819	Copolymer	200 nm oxidized Si₃N₄	51	-	-	[60]
Si₃N₄	DLP	EA+819+HDDA+184	Darvan	800 nm (KH-560)Si₃N₄	50	45	-	[62]

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非氧化物陶瓷光固化增材制造研究进展及展望

Research Progress and Prospects of Non-oxide Ceramic in Stereolithography Additive Manufacturing

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