3D打印氧化铝陶瓷的气氛脱脂热处理工艺研究

doi:10.15541/jim20210634

无机材料学报 ›› 2022, Vol. 37 ›› Issue (3): 333-337.DOI: 10.15541/jim20210634

所属专题：【虚拟专辑】增材制造及3D打印(2021-2022)

3D打印氧化铝陶瓷的气氛脱脂热处理工艺研究

曾勇¹^,²^,³(), 张子佳¹^,²^,³, 孙立君¹^,²^,³, 姚海华¹^,²^,³, 陈继民¹^,²^,³

1.北京工业大学材料与制造学部, 北京 100124
2.北京市数字化医疗3D打印工程技术研究中心, 北京 100124
3.跨尺度激光成型制造技术教育部重点实验室, 北京 100124

收稿日期:2021-10-12 修回日期:2021-10-25 出版日期:2022-03-20 网络出版日期:2021-11-01
作者简介:曾勇(1987-), 男, 副教授. E-mail: zengyong@bjut.edu.cn
基金资助:
北京市教委科研计划(KM2020100050003)

Atmosphere Debinding Heat Treatment of 3D Printed Alumina Ceramics

ZENG Yong¹^,²^,³(), ZHANG Zijia¹^,²^,³, SUN Lijun¹^,²^,³, YAO Haihua¹^,²^,³, CHEN Jiming¹^,²^,³

1. Faculty of Materials and Manufacturing, Beijing University of Technology, Beijing 100124, China
2. Beijing Engineering Research Center of 3D Printing for Digital Medical Health, Beijing 100124, China
3. Key Laboratory of Trans-scale Laser Manufacturing Technology, Ministry of Education, Beijing 100124, China

Received:2021-10-12 Revised:2021-10-25 Published:2022-03-20 Online:2021-11-01
About author:ZENG Yong (1987-), male, associate professor. E-mail: zengyong@bjut.edu.cn
Supported by:
Scientific Research Project of Beijing Education Committee(KM2020100050003)

摘要/Abstract

摘要：

脱脂热处理工艺对于3D打印陶瓷的成形质量具有重要的影响。目前光固化3D打印制备得到的氧化铝生坯经过在空气中的脱脂热处理工艺后烧结最终得到的氧化铝陶瓷存在的微观裂纹等缺陷, 将导致其力学性能较差。本工作研究了基于数字光处理(Digital light processing, DLP)技术的氧化铝陶瓷打印热处理工艺, 将3D打印制备得到的氧化铝陶瓷生坯分别在空气与氩气中脱脂后比较其宏观形貌, 发现在空气下脱脂的氧化铝生坯存在微观裂纹。再将脱脂后的生坯在空气下烧结得到氧化铝陶瓷, 并对其微观形貌和宏观性能进行表征, 发现在氩气下脱脂的氧化铝陶瓷平均晶粒尺寸要比直接在空气中脱脂得到的氧化铝陶瓷平均晶粒尺寸大, 而且晶粒结构致密, 无明显气孔和杂相, 而且具有更高的抗压强度。这说明在氩气中脱脂后烧结得到的氧化铝陶瓷性能更好。在氩气中脱脂的氧化铝致密度最高可达到96.72%, 抗压强度可达到761.7 MPa, 相比于只在空气中脱脂的氧化铝陶瓷性能得到显著提升。

关键词: 数字光处理技术(DLP), 氧化铝, 氩气脱脂, 空气脱脂

Abstract:

Debinding heat treatment process play an important role in forming quality of 3D printing ceramics. At present, the alumina green body prepared by light curing 3D printing is sintered after debinding in air. The final alumina ceramics may have defects such as micro cracks, resulting in poor mechanical properties. Direct heating and debinding in air may lead to cracks caused by reaction between resin and oxygen in green body. To avoid this situation, this work studies the printing heat treatment process of alumina ceramics based on digital light processing (DLP) technology. The alumina ceramic green body prepared by 3D printing was degreased either in air or in argon, and their macro morphologies were compared with each other. It is found that there are micro cracks in the alumina green body debinding in air. After being sintered in air, the alumina ceramics was obtained and their micro morphology and macro properties were characterized. Average grain size of alumina ceramics debinding in argon was larger than that directly debinding in air, while the grain structure was dense without obvious pore and impurity. Moreover, in terms of mechanical properties, alumina ceramics debinding in air have higher compressive strength. The highest density of alumina debinding in argon reaches 96.72%, and the compressive strength reaches 761.7 MPa, significantly improved as compared with the one debinding in air.

Key words: digital light processing (DLP), alumina, argon debinding, air debinding

中图分类号:

TQ174

曾勇, 张子佳, 孙立君, 姚海华, 陈继民. 3D打印氧化铝陶瓷的气氛脱脂热处理工艺研究[J]. 无机材料学报, 2022, 37(3): 333-337.

ZENG Yong, ZHANG Zijia, SUN Lijun, YAO Haihua, CHEN Jiming. Atmosphere Debinding Heat Treatment of 3D Printed Alumina Ceramics[J]. Journal of Inorganic Materials, 2022, 37(3): 333-337.

图/表 6

图1 氩气脱脂后在空气中烧结工艺曲线

Fig. 1 Sintering process curve in air after debinding in argon

图2 氧化铝生坯在不同气氛中脱脂得到的样品照片

Fig. 2 Photos of alumina green body obtained after debinding in different atmospheres (a) In air; (b) In argon

图3 氧化铝粉末和不同气氛下脱脂后烧结氧化铝陶瓷的SEM 照片

Fig. 3 SEM images of surface modified alumina powder and sintered alumina ceramics after debinding in different atmospheres (a) Surface modified alumina powder; (b) Sintered alumina ceramics after debinding in air; (c) Sintered alumina ceramics after debinding in argon

图4 氧化铝粉末和不同气氛脱脂后烧结氧化铝陶瓷的XRD图谱

Fig. 4 XRD patterns of alumina powders and sintered alumina ceramics after debinding in different atmospheres

表1 不同脱脂后烧结样品的收缩率和致密度

Table 1 Shrinkage and density of sintered samples after debinding in different atmospheres

Atmosphere	Shrinkage/%			Densification/%
Atmosphere	X	Y	Z	Densification/%
Air	4.81	4.55	9.23	95.39
Ar	5.62	5.48	11.54	96.72

图5 不同气氛下脱脂后烧结氧化铝陶瓷的应力-应变曲线

Fig. 5 Stress-strain curves of sintered alumina ceramics after debinding in different atmospheres

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3D打印氧化铝陶瓷的气氛脱脂热处理工艺研究

Atmosphere Debinding Heat Treatment of 3D Printed Alumina Ceramics

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