氧化锆陶瓷扫描光固化成形与脱脂烧结工艺研究

doi:10.15541/jim20210569

无机材料学报 ›› 2022, Vol. 37 ›› Issue (3): 303-309.DOI: 10.15541/jim20210569

氧化锆陶瓷扫描光固化成形与脱脂烧结工艺研究

王亚宁¹(), 张玉琪¹, 宋索成², 陈若梦¹^,³, 刘亚雄⁴(), 段玉岗¹

1.西安交通大学机械制造系统工程国家重点实验室, 西安 710049
2.西安交通大学高端制造装备协同创新中心, 西安 710054
3.唐山学院机电工程系, 唐山 063000
4.季华实验室, 佛山 528200

收稿日期:2021-09-15 修回日期:2021-10-12 出版日期:2022-03-20 网络出版日期:2021-12-24
通讯作者: 刘亚雄, 教授. E-mail: yaxiongliu@163.com
作者简介:王亚宁(1989-), 男, 博士研究生. E-mail: 905488248@qq.com
基金资助:
国家自然科学基金(52075421);广东省基础与应用基础研究基金(2020B1515130002);季华实验室项目(X200031TM200)

Laser Stereolithography for Zirconia Ceramic Fabrication and Its Debinding and Sintering Process

WANG Yaning¹(), ZHANG Yuqi¹, SONG Suocheng², CHEN Ruomeng¹^,³, LIU Yaxiong⁴(), DUAN Yugang¹

1. State Key Laboratory for Manufacturing Systems Engineering, Xi'an Jiaotong University, Xi’an 710049, China
2. Collaborative Innovation Center of High-end Manufacturing Equipment, Xi'an Jiaotong University, Xi'an 710054, China
3. Department of Electromechanical Engineering, Tangshan University, Tangshan 063000, China
4. Ji Hua Laboratory, Foshan 528200, China

Received:2021-09-15 Revised:2021-10-12 Published:2022-03-20 Online:2021-12-24
Contact: LIU Yaxiong, professor. E-mail: yaxiongliu@163.com
About author:WANG Yaning (1989-), male, PhD candidate. E-mail: 905488248@qq.com
Supported by:
National Natural Science Foundation of China(52075421);Guangdong Basic and Applied Basic Resesrch Foundation(2020B1515130002);Jihua Laboratory Foundation(X200031TM200)

摘要/Abstract

摘要：

氧化锆陶瓷具有良好的力学性能、生物相容性以及耐腐蚀性, 在牙科修复领域得到了广泛应用。目前的氧化锆陶瓷光固化成形技术存在成形精度低, 烧结效率低, 收缩率高以及收缩各向异性明显等缺点。为解决以上问题, 本工作利用不同官能度单体配置了混杂体系树脂, 并利用混杂体系树脂配置了体积分数55%固相含量的陶瓷浆料, 离散了有机物热解区间, 有效避免素坯开裂, 提高脱脂效率。研究了激光功率和扫描速度对固化单元形状的影响, 并在兼顾成形精度和效率的前提下, 选择的最佳激光功率和扫描速度分别为670 mW和2500 mm/s。分别研究了扫描间距和线宽补偿对平面成形精度的影响以及分层厚度对堆积方向成形精度的影响, 选择的最佳扫描间距、线宽补偿和分层厚度分别为0.08、0.10和0.03 mm。在氮气气氛下对素坯进行脱脂, 降低了有机物热解速度, 进一步避免素坯开裂, 提高脱脂效率。脱脂件烧结后的平面收缩率为(18.26±0.10)%, 堆积方向收缩率为(19.20±0.13)%, 在收缩率降低的同时, 收缩各向异性也明显得到控制, 为其在牙科修复领域的应用奠定了基础。

关键词: 氧化锆陶瓷, 扫描光固化, 精度, 脱脂, 烧结

Abstract:

Due to good mechanical properties, biocompatibility and corrosion resistance, zirconia ceramic has been widely used in dental repairing. However, the present technologies for zirconia ceramic fabrication based on stereolithography have some drawbacks, such as low fabrication accuracy, low debinding efficiency, high shrinkage, and shrinkage anisotropy. In order to solve these problems, a kind of hybrid resin was prepared by using different monomers with different functionalities, and then zirconia ceramic slurry with solid content of 55% (volume percentage) was prepared by using this hybrid resin, which dispersed organic matter pyrolysis interva, promoting debinding efficiency and avoiding crack. Besides, effect of laser power and scanning speed to the curing unit shape were studied, the optimum laser power of 670 mW and scanning speed of 2500 mm/s were selected to meet requirments of fabrication accuracy and efficiency. In addition, effects of scanning line space and scanning line width compensation to horizontal dimension accuracy and slicing thickness to the stacking dimension accuracy were studied. Optimum process scanning line space of 0.08 mm, scanning line width compensation of 0.10 mm, and slicing thickness of 0.03 mm were determined. Meanwhile, the green part was debinded in nitrogen atmosphere, which reduced pyrolysis rate of organic matter, performed a further improvement of debinding efficiency and green part cracking. At last, the debinded part was sintered. The plane and stacking direction shrinkages of the sintered part are (18.26±0.10)% and (19.20±0.13)%, respectively. All these results demonstrated that the shrinkage is reduced and the shrinkage anisotropy is reduced obviously, which provides basis for application in dental repairing.

Key words: zirconia ceramic, stereolithography, accuracy, debinding, sintering

中图分类号:

TQ174

王亚宁, 张玉琪, 宋索成, 陈若梦, 刘亚雄, 段玉岗. 氧化锆陶瓷扫描光固化成形与脱脂烧结工艺研究[J]. 无机材料学报, 2022, 37(3): 303-309.

WANG Yaning, ZHANG Yuqi, SONG Suocheng, CHEN Ruomeng, LIU Yaxiong, DUAN Yugang. Laser Stereolithography for Zirconia Ceramic Fabrication and Its Debinding and Sintering Process[J]. Journal of Inorganic Materials, 2022, 37(3): 303-309.

图/表 7

表1 混杂体系树脂组分比例

Table 1 Component proportion of hybrid resin

Component	Mass percentage/%
Bifunctional monomer (HDDA, Curease, China)	38.0
Trifunctional monomer (TMPTA, Curease, China)	28.5
Hexafunctional monomer (DPHA, Curease, China)	28.5
Oligomer (NeoRadU Curease, China)	5.0

表2 陶瓷浆料组分比例

Table 2 Component proportion of ceramic slurry

Component	Proportion
Zirconia powder	Volume ratio to resin: 11 : 9
Resin	Volume ratio to ceramic: 9 : 11
Photoinitiator (819, Curease, China)	0.3% (mass percentage) of resin
Dispersant (TEGO685, TEG, China)	2% (mass percentage) of ceramic
Defoamer (TEGO900, TEG, China)	1% (mass percentage) of resin

图1 陶瓷固化单元截面

Fig. 1 Section of ceramic curing unit

图2 固化单元宽度(a)和厚度(b)与激光功率的关系曲线、固化单元宽度(c)和厚度(d)与扫描速度的关系曲线

Fig. 2 Curing unit width (a) and thickness (b) vs. laser power, and curing unit width (c) and thickness (d) vs. scanning speed

图3 扫描间距对平面尺寸误差的影响(a)、扫描策略示意图(b)、线宽补偿对平面尺寸误差的影响(c)和分层厚度对堆积方向尺寸误差的影响(d)

Fig. 3 Horizontal dimension error vs. scanning line space (a), schematic diagram of scanning strategy (b), horizontal dimension error vs. scanning line width compensation (c), and stacking dimension error vs. slicing thickness (d)

图4 不同树脂在不同气氛下的TG曲线和DTG曲线(a), 脱脂曲线(b), 氮气气氛(c)和空气气氛(d)下脱脂的长条制件照片, 素坯(e)和脱脂件(f) SEM照片

Fig. 4 TG and DTG curves of different resin in different atmosphere (a), debinding curve of green body (b), pictures of strip parts after debinding in nitrogen (c) and air (d) atmospheres, and SEM images of green part (e) and debinded part (f) Colorful figures are availuable on the website

图5 烧结曲线(a)、立方体素坯(b)、三单位牙桥素坯(c)、立方体烧结件(d)、三单位牙桥烧结件(e)的照片和烧结件SEM照片(f)

Fig. 5 Sintering curve (a), pictures of green parts of cube (b) and three units dental bridge (c), sintered parts of cube (d) and three units dental bridge (e), and SEM image of sintered part (f)

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氧化锆陶瓷扫描光固化成形与脱脂烧结工艺研究

Laser Stereolithography for Zirconia Ceramic Fabrication and Its Debinding and Sintering Process

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