Process optimization of zirconia ceramics via photocuring 3D printing

doi:10.3969/j.issn.1001-1935.2026.01.005

Abstract

Abstract: To address the poor dispersibility of sub-micron zirconia powder and the severe warpage that occurs during photocuring,zirconia ceramics were fabricated via photocuring 3D printing,using high-purity sub-micron zirconia powder (4Y-TZP) as the raw material,a blend of trimethylolpropane triacrylate (TMPTA),1,6-hexanediol diacrylate (HDDA) and polyethylene glycol diacrylate (PEG400DA) as the composite photosensitive resin system,bis(2,4,6-trimethylbenzoyl)phenylphosphine oxide as the photoinitiator,and 3-glycidoxypropyltrimethoxysilane (KH560),castor oil,and polymeric phosphate anionic dispersant (BYK-111) as dispersants,respectively.The effects of the photosensitive resin formulation,dispersant type,solid content,and photocuring molding process parameters on the rheological properties and suspension stability of the zirconia ceramic slurry,as well as the quality of green bodies were investigated systematically.The results indicate that:(1)when the dispersant KH560 addition is 0.5% of the zirconia powder mass,TMPTA accounts for 36% of the total addition of the composite photosensitive resin,and the solid content is 36 vol%,the prepared zirconia ceramic slurry exhibits excellent rheological properties and suspension stability;(2)under the printing parameters of exposure power of 1 230 mW·cm^-2,scanning speed of 2 000 mm·s^-1,and curing times of 2,the monolayer curing depth can reach 0.095 mm with high forming precision;after debinding at 600 ℃ in a nitrogen atmosphere and subsequent sintering at 1 550 ℃,dense zirconia ceramics can be obtained,with the apparent density of 5.80 g·cm^-3 and flexural strength of 641 MPa.

Key words: zirconia, photocuring, rheological properties, 3D printing

摘要： 针对亚微米氧化锆粉体分散性差、光固化成型过程中易发生翘曲等问题,以高纯亚微米氧化锆粉体(4Y-TZP)为原料,以三羟甲基丙烷三丙烯酸酯(TMPTA)、1,6-己二醇二丙烯酸酯(HDDA)和聚乙二醇二丙烯酸酯(PEG400DA)为复合光敏树脂体系,以双(2,4,6-三甲基苯甲酰基)苯基氧化膦作为光引发剂,分别以3-缩水甘油醚氧基丙基三甲氧基硅烷(KH560)、蓖麻油、聚合磷酸酯类阴离子分散剂(BYK-111)作为分散剂,光固化3D打印制备氧化锆陶瓷。探究了光敏树脂配比、分散剂、固含量、光固化成型工艺参数等对氧化锆陶瓷浆料流变性能、悬浮稳定性及生坯质量的影响。结果表明:1)分散剂KH560添加量为氧化锆粉体质量的0.5%、TMPTA占复合光敏树脂总质量的36%、固相体积分数为36%的氧化锆陶瓷浆料具备良好的流变性能与悬浮稳定性;2)在曝光功率为1 230 mW·cm^-2、扫描速度为2 000 mm·s^-1、固化次数为2的打印参数下,浆料的单层固化深度可达0.095 mm,且成形精度较高,坯体在氮气气氛下经600 ℃脱脂后再经1 550 ℃烧结,可获得致密氧化锆陶瓷,表观密度为5.80 g·cm^-3,抗弯强度达641 MPa。

关键词: 氧化锆, 光固化, 流变性能, 3D打印

CLC Number:

TQ175

Shi Yingtong, Zheng Wenwen, Xie Hehan, Liu Peng, Liu Ziyu, Yang Xianfeng. Process optimization of zirconia ceramics via photocuring 3D printing[J]. Refractories, 2026, 60(1): 25-30.

施英统, 郑雯雯, 谢呵瀚, 刘鹏, 刘子玉, 杨现锋. 光固化3D打印制备氧化锆陶瓷的工艺优化[J]. 耐火材料, 2026, 60(1): 25-30.

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