脱脂工艺对光固化3D打印堇青石陶瓷性能的影响

doi:10.15541/jim20210624

无机材料学报 ›› 2022, Vol. 37 ›› Issue (3): 317-324.DOI: 10.15541/jim20210624

所属专题：增材制造专题(2022)；【虚拟专辑】增材制造及3D打印(2021-2022)

脱脂工艺对光固化3D打印堇青石陶瓷性能的影响

朱俊逸(), 张成, 罗忠强, 曹继伟, 刘志远, 王沛, 刘长勇, 陈张伟()

深圳大学增材制造研究所, 深圳 518060

收稿日期:2021-10-08 修回日期:2021-10-21 出版日期:2022-03-20 网络出版日期:2021-11-01
通讯作者: 陈张伟, 教授. E-mail: chen@szu.edu.cn
作者简介:朱俊逸(1996-), 男, 硕士研究生. E-mail: 386398374@qq.com
基金资助:
国家自然科学基金(51975384);广东省自然科学基金(2020A1515011547);深圳市基础研究(JCYJ20190808144009478);深圳市高校稳定支持项目(20200731211324001);深大-台北科大合作项目(2021007)

Influence of Debinding Process on the Properties of Photopolymerization 3D Printed Cordierite Ceramics

ZHU Junyi(), ZHANG Cheng, LUO Zhongqiang, CAO Jiwei, LIU Zhiyuan, WANG Pei, LIU Changyong, CHEN Zhangwei()

Additive Manufacturing Institute, Shenzhen University, Shenzhen 518060, China

Received:2021-10-08 Revised:2021-10-21 Published:2022-03-20 Online:2021-11-01
Contact: CHEN Zhangwei, professor. E-mail: chen@szu.edu.cn
About author:ZHU Junyi (1996-), male, Master candidate. E-mail: 386398374@qq.com
Supported by:
National Natural Science Foundation of China(51975384);Natural Science Foundation of Guangdong Province(2020A1515011547);Basic Research Foundation of Shenzhen(JCYJ20190808144009478);University Support Fund of Shenzhen City(20200731211324001);NTUT-SZU Joint Research Program(2021007)

摘要/Abstract

摘要：

光固化3D打印是制造高度复杂结构陶瓷的一种有效方法。打印的样件需要经历脱脂和烧结等热处理才能成为可用的陶瓷件, 脱脂工艺对打印件性能影响巨大。本工作通过研究脱脂工艺对DLP光固化3D打印制备的堇青石陶瓷性能的影响规律, 建立缺陷抑制策略。比较并分析了脱脂气氛和升温速率对陶瓷样件的表面裂纹和元素分布状态的影响, 还对比进一步烧结后样件显微组织、尺寸收缩率、相对密度和弯曲强度等性能。研究发现脱脂气氛对样件各性能影响最大, 使用氩气脱脂可显著降低表面裂纹, 提高相对密度与弯曲强度; 并确定最佳升温速率为1 ℃/min。最终获得表面完整无裂纹且相对密度为(94.6±0.3)%, 弯曲强度为(94.3±3.2) MPa的堇青石陶瓷样件。本研究为光固化3D打印堇青石陶瓷的无缺陷制造与应用提供了科学依据与技术参考。

关键词: 堇青石陶瓷, 光固化3D打印, 脱脂, 烧结, 性能

Abstract:

Photopolymerization 3D printing method is an effective means for the manufacturing of ceramics with highly complex-shaped structures and exceptional performance. The printed samples need to undergo heat treatment such as debinding and sintering before becoming usable final ceramic parts in various industrial applications, and the debinding process has a great impact on the properties of the printed ceramic parts. In this study, effect of the debinding process on physical properties and mechanical performance of the cordierite ceramics prepared by DLP photopolymerization 3D printing was studied, and defect suppression strategy was established accordingly. The effects of debinding atmosphere and heating rate on surface cracks and material elemental distribution of ceramic samples were compared and analyzed. The microstructure, size shrinkage, relative density, and mechanical performance such as bending strength of the sintered samples were also studied. It is found that the debinding atmosphere has the most significant influence on the properties of the sintered samples, in which the surface cracks can be significantly reduced, and the relative density, and bending strength can be increased when the debinding process is conducted in argon atmosphere at the optimized heating rate of 1 ℃/min. After debinding and sintering, the cordierite ceramic samples with a relative density of (94.6±0.3)% and a bending strength of (94.3±3.2) MPa was obtained. In conclusion, this study provides a scientific basis and technical reference for fabrication and application of cordierite ceramics based on photopolymerization 3D printing method.

Key words: cordierite ceramic, photopolymerization 3D printing, debinding, sintering, properties

中图分类号:

TQ174

朱俊逸, 张成, 罗忠强, 曹继伟, 刘志远, 王沛, 刘长勇, 陈张伟. 脱脂工艺对光固化3D打印堇青石陶瓷性能的影响[J]. 无机材料学报, 2022, 37(3): 317-324.

ZHU Junyi, ZHANG Cheng, LUO Zhongqiang, CAO Jiwei, LIU Zhiyuan, WANG Pei, LIU Changyong, CHEN Zhangwei. Influence of Debinding Process on the Properties of Photopolymerization 3D Printed Cordierite Ceramics[J]. Journal of Inorganic Materials, 2022, 37(3): 317-324.

图/表 8

图1 DLP光固化增材制造原理

Fig. 1 Working principle of DLP 3D printing technology

图2 堇青石陶瓷生坯的热重分析结果与脱脂和烧结曲线

Fig. 2 TG/DSC curves, debinding and sintering curves of printed cordierite green body (a) TG/DSC curves; (b) Debinding curve; (c) Sintering curve

图3 不同升温速率脱脂后的样件表面宏观形貌

Fig. 3 Surface macro-graphs of sample after debinding at different heating rates In air: (a) 0.1 ℃/min; (b) 0.5 ℃/min; (c) 1 ℃/min; (d) 3 ℃/min; (e) 5 ℃/min; In argon: (f) 0.1 ℃/min; (g) 0.5 ℃/min; (h) 1 ℃/min; (i) 3 ℃/min; (j) 5 ℃/min

图4 空气气氛下脱脂后样件的EDS元素分析

Fig. 4 Element analysis of sample after debinding in air (a) SEM image; EDS mappings of (b) Al, (c) Mg, (d) O and (e) Si; (f) EDS spectrum

图5 氩气气氛下脱脂后样件EDS元素分析

Fig. 5 Element analysis after debinding in argon (a) SEM image; EDS mappings of (b) Al, (c) Mg, (d) C and (e) O; (f) Si; (g) EDS spectrum

图6 在氩气气氛下脱脂后的样件表面微观形貌

Fig. 6 Micrographs of sample surfaces after debinding in argon(a) 0.1 ℃/min; (b) 0.5 ℃/min; (c) 1 ℃/min; (d) 3 ℃/min; (e) 5 ℃/min

图7 在不同气氛、不同脱脂升温速率下脱脂并经烧结后样件的性能

Fig. 7 Properties of samples after debinding in different atmospheres followed by sintering (a) Shrinkage rate-debinding in air; (b) Shrinkage rate-debinding in argon; (c) Relative density; (d) Bending strength

图8 优化脱脂策略后烧结的样件

Fig. 8 Final cordierite ceramics prepared with optimized debinding scheme followed by sintering (a, b) Dense rectangular sample; (c) Honeycomb structures with complex inter-crossing channels

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脱脂工艺对光固化3D打印堇青石陶瓷性能的影响

Influence of Debinding Process on the Properties of Photopolymerization 3D Printed Cordierite Ceramics

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