浆料固相含量对数字光处理成形Si3N4陶瓷性能的影响

doi:10.15541/jim20210609

无机材料学报 ›› 2022, Vol. 37 ›› Issue (3): 310-316.DOI: 10.15541/jim20210609

浆料固相含量对数字光处理成形Si₃N₄陶瓷性能的影响

李萌¹^,²(), 黄海露¹^,², 吴甲民¹^,²(), 刘春磊¹^,², 吴亚茹¹^,², 张景贤³, 史玉升¹^,²

1.华中科技大学材料科学与工程学院, 材料成形与模具技术国家重点实验室, 武汉430074
2.增材制造陶瓷材料教育部工程研究中心, 武汉430074
3.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

收稿日期:2021-10-02 修回日期:2021-12-08 出版日期:2022-03-20 网络出版日期:2021-12-24
通讯作者: 吴甲民, 副教授. E-mail: jiaminwu@hust.edu.cn
作者简介:李萌(1996-), 女, 硕士研究生. E-mail: 819448243@qq.com
基金资助:
国家自然科学基金(51975230);湖北省技术创新专项重大项目(2019AAA002);高性能陶瓷和超微结构国家重点实验室开放课题(SKL201903SIC)

Effect of Solid Loading of Slurry on Properties of Si₃N₄ Ceramics Formed by Digital Light Processing

LI Meng¹^,²(), HUANG Hailu¹^,², WU Jiamin¹^,²(), LIU Chunlei¹^,², WU Yaru¹^,², ZHANG Jingxian³, SHI Yusheng¹^,²

1. State Key Laboratory of Materials Processing and Die & Mould Technology, School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430074, China
2. Engineering Research Center of Ceramic Materials for Additive Manufacturing, Ministry of Education, Wuhan 430074, China
3. State Key Laboratory of High Performance Ceramics and Superfine Microstructure, Shanghai Institute of Ceramics, Chinese Academy of Sciences, Shanghai 200050, China

Received:2021-10-02 Revised:2021-12-08 Published:2022-03-20 Online:2021-12-24
Contact: WU Jiamin, associate professor. E-mail: jiaminwu@hust.edu.cn
About author:LI Meng (1996-), female, Master candidate. E-mail: 819448243@qq.com
Supported by:
National Natural Science Foundation of China(51975230);Major Special Projects of Technological Innovation in Hubei Province(2019AAA002);Opening Project of State Key Laboratory of High Performance Ceramics and Superfine Microstructures(SKL201903SIC)

摘要/Abstract

摘要：

随着科技的不断发展, Si₃N₄陶瓷在航空、机械、生物医疗等高新领域发挥着越来越重要的作用。本工作采用包覆助烧剂Al₂O₃-Y₂O₃后的Si₃N₄粉体为原材料, 利用数字光处理(Digital light processing, DLP)技术成功制备出Si₃N₄陶瓷, 并系统研究了浆料固相含量对Si₃N₄陶瓷浆料、DLP成形Si₃N₄陶瓷素坯和陶瓷性能的影响。研究表明, 浆料固相含量低于40.0% (体积分数)时, 浆料在30 s^-1剪切速率下的粘度均小于2 Pa·s, 可用于DLP成形。在这种情况下, 浆料的单层固化深度随浆料固相含量的增加而减小。随着浆料固相含量的增大, DLP成形Si₃N₄陶瓷的相对密度和抗弯强度先升高后降低。固相含量为37.5% (体积分数)的样品获得最大的相对密度和抗弯强度, 分别为89.8%和162.5 MPa, 较固相含量为32.5% (体积分数)的样品分别提升了10%和16%。本研究通过对陶瓷浆料性能的优化, 提升了DLP成形Si₃N₄陶瓷的性能, 为Si₃N₄等非氧化物陶瓷光固化成形奠定了实验基础。

关键词: 氮化硅, 数字光处理, 固相含量, 相对密度, 抗弯强度

Abstract:

With the continuous development of science and technology, Si₃N₄ ceramics are playing an increasingly important role in high-tech fields such as aviation machinery, biology and medical treatment. In this work, Si₃N₄ ceramics were successfully prepared by digital light processing (DLP) technology using Si₃N₄ powder coated with Al₂O₃-Y₂O₃ as raw material. Effects of solid loading of slurry on the performance of Si₃N₄ ceramic slurry, Si₃N₄ ceramic green parts and Si₃N₄ceramics were systematically studied. The results showed that when the solid loading of slurry was less than 40.0% (in volume), its viscosity was less than 2 Pa·s at shear rate of 30 s^-1, which can be used for DLP forming. In that case, the single curing depth of the slurry decreased with the increase of solid loading of the slurry, while the relative density and flexural strength of Si₃N₄ ceramics formed by DLP increased firstly and then decreased. The relative density and flexural strength reached the maximum of 89.8% and 162.5 MPa at solid loading of 37.5% (in volume), which were 10% and 16% higher than those with solid loading of 32.5% (in volume), respectively. In this work, the properties of Si₃N₄ ceramics formed by DLP were optimized by determining the best solid loading, which laid the experimental foundation for the photocuring of non-oxide ceramics such as Si₃N₄.

Key words: Si₃N₄, digital light processing, solid loading, relative density, flexural strength

中图分类号:

TQ174

李萌, 黄海露, 吴甲民, 刘春磊, 吴亚茹, 张景贤, 史玉升. 浆料固相含量对数字光处理成形Si₃N₄陶瓷性能的影响[J]. 无机材料学报, 2022, 37(3): 310-316.

LI Meng, HUANG Hailu, WU Jiamin, LIU Chunlei, WU Yaru, ZHANG Jingxian, SHI Yusheng. Effect of Solid Loading of Slurry on Properties of Si₃N₄ Ceramics Formed by Digital Light Processing[J]. Journal of Inorganic Materials, 2022, 37(3): 310-316.

图/表 8

图1 Si3N4原粉和包覆后的Si3N4粉体的微观形貌、粒径分布图以及能谱图

Fig. 1 Microstructures, particle size distributions, and EDX mappings of Si3N4 raw powder and Si3N4 powder after being coated (a) Microstructure of Si3N4 raw powder; (b) Particle size distribution of Si3N4 raw powder; (c) Microstructure of Si3N4 powder after being coated; (d) Particle size distribution of Si3N4 powder after being coated; (e) EDX mappings of Si3N4 powder after being coated

图2 不同固相含量(体积分数)的Si3N4浆料在不同剪切速率下的粘度(a)和在剪切速率为30 s-1下的粘度(b)

Fig. 2 Viscosities at different shear rates (a) and at the shear rate of 30 s-1 (b) of Si3N4 slurries with different solid loadings (in volume)

图3 不同固相含量(体积分数)的Si3N4陶瓷浆料在激光能量密度为800 mJ/cm2下的单层固化深度

Fig. 3 Cure depth of Si3N4 slurries at the energy dose of 800 mJ/cm2 with different solid loadings (in volume)

图4 不同固相含量(体积分数)的Si3N4陶瓷素坯侧面的光学显微照片

Fig. 4 Optical micrographs of Si3N4 ceramic green parts with different solid loadings (in volume) (a) 32.5%; (b) 35.0%; (c) 37.5%; (d) 40.0%

图5 不同固相含量(体积分数)的Si3N4陶瓷的物相组成

Fig. 5 Phase compositions of Si3N4 ceramics with different solid loadings (in volume)

图6 不同固相含量(体积分数)的Si3N4陶瓷表面的SEM照片

Fig. 6 SEM micrographs of the surfaces of Si3N4 ceramics with different solid loadings (in volume) (a) 32.5%; (b) 35.0%; (c) 37.5%; (d) 40.0%

图7 不同固相含量(体积分数)的Si3N4陶瓷断面的SEM照片

Fig. 7 Cross-sectional SEM micrographs of Si3N4 ceramics with different solid loadings (in volume) (a) 32.5%; (b) 35.0%; (c) 37.5%; (d) 40.0%

图8 不同固相含量(体积分数)的Si3N4陶瓷的收缩率(a)和抗弯强度以及相对密度(b)

Fig. 8 Shrinkage (a), flexural strength and relative density (b) of Si3N4 ceramics with different solid loadings (in volume)

参考文献 30

[1]	BOCANEGRA-BERNAL M H, MATOVIC B. Mechanical properties of silicon nitride-based ceramics and its use in structural applications at high temperatures. Materials Science and Engineering: A, 2010, 527(6): 1314-1338. DOI URL
[2]	DANTE R C, KAJDAS C K. A review and a fundamental theory of silicon nitride tribochemistry. Wear, 2012, 288(3): 27-38. DOI URL
[3]	SUN Y G, HE S L, LIU R A, et al. Preparation and application of silicon nitride ceramics. China Ceramic Industry, 2016, 23(5): 31-34.
[4]	RILEY F L. Silicon nitride and related materials. Journal of the American Ceramic Society, 2000, 83(2): 245-265. DOI URL
[5]	KLEMM H. Silicon nitride for high-temperature applications. Journal of the American Ceramic Society, 2010, 93(6): 1501-1522. DOI URL
[6]	KRSTIC Z, KRSTIC V D. Silicon nitride: the engineering material of the future. Journal of Materials Science, 2012, 47(2): 535-552. DOI URL
[7]	WANG B M. State of the art of advanced ceramic material. Progress in Chemistry, 2000, 12(3): 357-359.
[8]	NISHIMURA T, MITOMO M, SUEMATSU H. High temperature strength of silicon nitride ceramics with ytterbium silicon oxynitride. Journal of Materials Research, 1997, 12(1): 203-209. DOI URL
[9]	CHEN A N, WU J M, HAN L X, et al. Preparation of Si₃N₄ foams by DCC method via dispersant reaction combined with protein-gelling. Journal of Alloys and Compounds, 2018, 745(1): 262-270. DOI URL
[10]	XIE G R, ZHANG X G, CEN X D. Study and application of silicon nitride ceramic cutting tool. Tool Engineering, 2007, 41(2): 78-80.
[11]	PYZIK A J, BEAMAN D R. Microstructure and properties of self-reinforced silicon nitride. Journal of the American Ceramic Society, 1993, 76(11): 2737-2744. DOI URL
[12]	NEUMANN A, RESKE T, HELD M, et al. Comparative investigation of the biocompatibility of various silicon nitride ceramic qualities in vitro. Journal of Materials Science: Materials in Medicine, 2004, 15(10): 1135-1140. DOI URL
[13]	ORTH J, LUDWIG M, PIENING W, et al. Biocompatibility of Silicon Carbide and Silicon Nitride Ceramics. Results of an Animal Experiment. Bioceramics and the Human Body. Berlin: Springer, 1992, 28(12): 372-377.
[14]	KANDI K K, THALLAPALLI N, CHILAKALAPALLI S P R. Development of silicon nitride-based ceramic radomes-a review. International Journal of Applied Ceramic Technology, 2015, 12(5): 909-920. DOI URL
[15]	WU W J, LIU J, ZHANG J, et al. Preparation and application status of porous Si₃N₄ ceramic. China Ceramics, 2016, 52(7): 10-13.
[16]	HE J H, WU J M, CHEN A N, et al. Ceramic materials for additive manufacturing and their forming technologies. Materials China, 2020, 39(5): 337-348.
[17]	CHEN Z W, LI Z Y, LI J J, et al. 3D printing of ceramics: a review. Journal of European Ceramic Society, 2019, 39(4): 661-687. DOI URL
[18]	LIU S S, LI M, WU J M, et al. Preparation of high-porosity Al₂O₃ ceramic foams via selective laser sintering of Al₂O₃ poly-hollow microspheres. Ceramics International, 2020, 46(4): 4240-4247. DOI URL
[19]	WONG K V, HERNANDEZ A. A review of additive manufacturing. ISRN Mechanical Engineering, 2012, 34(15): 30-38.
[20]	CHEN F, ZHU H, WU J M, et al. Preparation and biological evaluation of ZrO₂ all-ceramic teeth by DLP technology. Ceramics International, 2020, 46(8): 11268-11274. DOI URL
[21]	DMITRII A K, PETR S S, ANASTASIYA D E, et al. Rheological and curing behavior of acrylate-based suspensions for the DLP 3D printing of complex zirconia parts. Materials, 2018, 11(12): 2350-2362 DOI URL
[22]	LI S, DUAN W, ZHAO T, et al. The fabrication of SiBCN ceramic components from preceramic polymers by digital light processing (DLP) 3D printing technology. Journal of the European Ceramic Society, 2018, 38(14): 4597-4603. DOI URL
[23]	WU J M, YANG Y Q, WANG C, et al. Photopolymerization technologies for ceramics and their applications. Journal of Mechanical Engineering, 2020, 56(19): 221-238.
[24]	SHUAI X, ZENG Y, LI P, et al. Fabrication of fine and complex lattice structure Al₂O₃ ceramic by digital light processing 3D printing technology. Journal of Materials Science, 2020, 55(3): 6771-6782. DOI URL
[25]	HE R, LIU W, WU Z, et al. Fabrication of complex-shaped zirconia ceramic parts via a DLP-stereolithography-based 3D printing method. Ceramics International, 2018, 44(3): 3412-3416. DOI URL
[26]	HUA S B, ZHU H, WU J M, et al. Performance of lattice structure scaffold prepared via digital light processing manufacture by DLP technology. Journal of Chinese Ceramic Society, 2021, 49(4): 608-617.
[27]	GRIFFITH M L, HALLORAN J W. Ultraviolet Curing of Highly Loaded Ceramic Suspensions for Stereolithography of Ceramics. Proc. Solid Freeform Fabr. Symp., 1994: 396-403.
[28]	WU X Q, XU C J, ZHANG Z M. Preparation and optimization of Si₃N₄ ceramic slurry for low-cast LCD mask stereolithography. Ceramics International, 2021, 47(7): 9400-9408. DOI URL
[29]	DING G J, HE R J, ZHANG K Q, et al. Stereolithography-based additive manufacturing of gray-colored SiC ceramic green body. Journal of the American Ceramic Society, 2019, 102(12): 7198-7209. DOI URL
[30]	HUANG R J, JIANG Q G, WU H D, et al. Fabrication of complex shaped ceramic parts with surface-oxidized Si₃N₄ powder via digital light processing based stereolithography method. Ceramics International, 2019, 45(4): 5158-5162. DOI URL

浆料固相含量对数字光处理成形Si₃N₄陶瓷性能的影响

Effect of Solid Loading of Slurry on Properties of Si₃N₄ Ceramics Formed by Digital Light Processing

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

图/表 8

参考文献 30

相关文章 15

编辑推荐

Metrics

本文评价

[1]	付师, 杨增朝, 李宏华, 王良, 李江涛. 复合烧结助剂对Si₃N₄陶瓷力学性能和热导率的影响[J]. 无机材料学报, 2022, 37(9): 947-953.
[2]	张叶, 曾宇平. 自蔓延高温合成氮化硅多孔陶瓷的研究进展[J]. 无机材料学报, 2022, 37(8): 853-864.
[3]	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.
[4]	王为得, 陈寰贝, 李世帅, 姚冬旭, 左开慧, 曾宇平. 以YbH₂-MgO体系为烧结助剂制备高热导率高强度氮化硅陶瓷[J]. 无机材料学报, 2021, 36(9): 959-966.
[5]	梁汉琴, 尹金伟, 左开慧, 夏咏锋, 姚冬旭, 曾宇平. 添加BaTiO₃的热压烧结Si₃N₄陶瓷的力学和介电性能[J]. 无机材料学报, 2021, 36(5): 535-540.
[6]	刘洋, 陆有军, 李彦瑞, 林立群, 袁振侠, 黄振坤. Hf-Si-La-O-N体系中HfN的形成及相关系[J]. 无机材料学报, 2021, 36(4): 443-448.
[7]	雷超, 魏飞. 单晶α-Si₃N₄纳米线宏量制备研究[J]. 无机材料学报, 2019, 34(6): 667-672.
[8]	廖春景, 董绍明, 靳喜海, 胡建宝, 张翔宇, 吴惠霞. 沉积温度及热处理对低压化学气相沉积氮化硅涂层的影响[J]. 无机材料学报, 2019, 34(11): 1231-1237.
[9]	邢媛媛, 吴海波, 刘学建, 黄政仁. 颗粒级配对固相烧结碳化硅陶瓷的影响[J]. 无机材料学报, 2018, 33(11): 1167-1172.
[10]	段于森, 张景贤, 李晓光, 黄鸣鸣, 施鹰, 谢建军, 江东亮. 稀土氧化物对常压烧结氮化硅陶瓷性能的影响[J]. 无机材料学报, 2017, 32(12): 1275-1279.
[11]	邓健, 姚冬旭, 夏咏锋, 左开慧, 尹金伟, 曾宇平. 注浆成型结合真空发泡法制备梯度多孔氮化硅陶瓷[J]. 无机材料学报, 2016, 31(8): 865-868.
[12]	梁灵江, 李凯, 颜冬, 马奔, 杨佳军, 蒲健, 池波, 李箭. 固体氧化物燃料电池力学性能和形变行为研究[J]. 无机材料学报, 2015, 30(6): 633-638.
[13]	杨治刚, 余建波, 李传军, 玄伟东, 张振强, 邓康, 任忠鸣. 热固性硅树脂压注法制备多孔硅基陶瓷型芯研究[J]. 无机材料学报, 2015, 30(2): 147-152.
[14]	胡海龙, 曾宇平, 左开慧, 夏咏锋,姚冬旭. 烧结助剂种类对Si₃N₄/SiC陶瓷力学与摩擦性能的影响[J]. 无机材料学报, 2014, 29(8): 885-890.
[15]	张俊禧, 徐照芸, 王波, 秦毅, 杨建锋, 赵中坚, 胡伟, 施志伟. 氮气压力对多孔氮化硅陶瓷显微组织和力学性能的影响[J]. 无机材料学报, 2014, 29(7): 701-705.