树脂包覆球形SiO2颗粒制备3D打印用陶瓷/树脂复合粉体

doi:10.15541/jim20180383

摘要/Abstract

摘要：

采用球形致密的SiO₂微米颗粒制备用于3D打印的陶瓷/树脂复合粉体, 并对粉体的固化和烧结性能进行了研究。结果显示, 随着温度升高或固体含量的增加, 包覆介质的粘度逐渐增大, 最佳树脂浓度为27wt%。均匀包覆的陶瓷/树脂复合粉体具有良好的分散性、流动性(25 (s/50 g))和较大的堆积密度(45.0%)。球形颗粒堆积形成的贯通孔道和球形颗粒表面均匀的吸附能对均匀包覆过程起到了至关重要的作用。包覆层的厚度(1.1~3.7 μm)可以通过调节抽滤过程的负压进行精确控制。由于颗粒之间形成了树脂颈部, 使制备的粉体具有很好的固化强度, 固化的陶瓷生胚经1250 ℃烧结后获得了性能优异的陶瓷: 压缩强度为10.2 MPa, 弯曲强度为2.7 MPa, 烧结收缩仅5%。上述结果表明, 复合粉体在3D打印产业上具有良好的应用前景。

关键词: 粉体技术, SiO₂球, 3D打印, 包覆层

Abstract:

Ceramic/resin composite powders used for 3D printing are synthesized by micro-sized SiO₂ dense spheres through a simple method, and their consolidation and sintering performances are fully characterized. The results show that the viscosity of coating media decreases gradually with the increasing temperature or decreasing the resin content and the most suitable resin content is 27wt%. The uniformly coated ceramic/resin composite spheres with well dispersity, fine fluidity (25 (s/50 g)) and larger packing density (45.0%) are successfully synthesized. The spherical shape of ceramic powders is revealed to be the vital factor for the achievement of uniform coating layers, because of the interconnected packed pores and the uniform cohesive energy of spheres. Meanwhile, the thickness (1.1-3.7 μm) of coating layer is controlled precisely through changing the pressure during the filtration process. Moreover, the synthesized powders show well consolidation performance for the favorite necks among spheres. After sintered at 1250 ℃, the ceramics with compressive strength of 10.2 MPa and bending strength of 2.7 MPa are obtained while the shrinkage is only 5%, which indicates the composite spheres have an advantage in improving the precision of 3D technology.

Key words: powder technology, SiO₂ spheres, 3D printing, coating layer

中图分类号:

TB332

孙志强, 杨小波, 王华栋, 李德里, 李淑琴, 吕毅. 树脂包覆球形SiO₂颗粒制备3D打印用陶瓷/树脂复合粉体[J]. 无机材料学报, 2019, 34(5): 567-572.

Zhi-Qiang SUN, Xiao-Bo YANG, Hua-Dong WANG, De-Li LI, Shu-Qin LI, Yi LÜ. Ceramic/Resin Composite Powders with Uniform Resin Layer Synthesized from SiO₂ Spheres for 3D Technology[J]. Journal of Inorganic Materials, 2019, 34(5): 567-572.

图/表 7

Fig. 1 Schematic of fabrication for ceramic/resin composite powders

Fig. 2 Effect of temperature and solid content on viscosity of resin slurry

Fig. 3 SEM images of SiO2 spheres (a), coated spheres (b), the cross section of coating layer (c), and particle size distribution before/after coating (d)

Fig. 4 SEM images of composite spheres and corresponding coating layer fabricated at different negative pressures (a) 0.1 MPa; (b) 0.3 MPa

Fig. 5 Photographs of (a) composite powders, (b) consolidated bulk and (c) polished bulk

Fig. 6 SEM image of microstructure of consolidated bulk

Fig. 7 shows the characterization of SiO2 ceramics synthesized by the composite spheres with layer thickness of 2 μm after consolidated and sintered at 1250 ℃ for 2 h. Fig. 7(a) is the SEM image of the fracture surface of ceramic, exhibiting that the uniformly arranged particles are sintered together and the sintered necks among spheres can be easily observed. The pores are mostly composed of the cell walls of spheres and no blockages derived from uneven shrinkage can be found. The narrow pore size distribution shown in Fig. 7(b) also indicates the ceramics are well structured without structural defects.

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树脂包覆球形SiO₂颗粒制备3D打印用陶瓷/树脂复合粉体

Ceramic/Resin Composite Powders with Uniform Resin Layer Synthesized from SiO₂ Spheres for 3D Technology

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