核用陶瓷光固化3D打印工艺及抗热震性能研究

Study on Digital Light Processing 3D Printing Process and Thermal Shock Resistance of Ceramic Materials for Nuclear Application

  • 摘要: 为提高精密铸造效率,缩短陶瓷模具制造周期,本文采用基于面曝光的光固化(DLP)3D打印技术制备了适用于铸造特种材料部件的Al2O3、ZrO2和MgO模具。光敏树脂与纳米级陶瓷粉体混合成的陶瓷浆料通过紫外光固化后形成陶瓷生坯,经过干燥、脱脂和烧结处理得到所需陶瓷样件。利用SEM对烧结前后的陶瓷进行了微观组织表征,并对光固化3D打印陶瓷样件进行了力学性能(压缩和弯曲)和抗热震性能测试。结果表明,陶瓷生坯经过适当温度烧结后,组织由多孔结构变致密。光固化3D打印陶瓷的压缩和弯曲强度均可达到等静压工艺水平。通过抗热震性能测试,光固化3D打印陶瓷展现出良好的抗热震性能,其中ZrO2陶瓷在800 ℃和1 300 ℃条件下的性能最优。光固化3D打印技术在制备结构功能复杂的陶瓷部件方面展现出巨大优势,可大幅减少制造周期与成本,为核能领域高精尖产品制造提供重要的技术支撑。

     

    Abstract: In order to improve the efficiency of precision casting and shorten the manufacturing cycle of ceramic molds, Al2O3, ZrO2 and MgO molds suitable for casting special material parts were prepared by digital light processing (DLP) 3D printing technology based on surface exposure. The ceramic slurry mixed with photosensitive resin and nano-scale ceramic powder was cured by ultraviolet light to form a ceramic green body. After drying, degreasing and sintering, the required ceramic sample was obtained. The process of DLP 3D printing ceramics includes ceramic slurry preparation, 3D modeling, model slicing, 3D printing green body, green body degreasing and sintering. The DLP ceramic slurry is composed of nano-ceramic powder and organic resin, in which the organic resin is composed of monomer, oligomer, photoinitiator, dispersant and defoaming agent. The monomer is 1,6-hexanediol diacrylate (HDDA), and the additive amount is 47.5% of the powder mass. The oligomer is aliphatic polyacrylate (E8210), the additive amount is 47.5% of the powder mass, the photoinitiator is TPO, and the dispersant is BYK11. The microstructure of the ceramics before and after sintering was characterized by SEM, and the mechanical properties (compression and bending) and thermal shock resistance of the 3D printing ceramic samples were tested. Al2O3, ZrO2 and MgO ceramic bodies were prepared by using 50% (volume fraction) ceramic slurry with light intensity of 25-32 mW/cm2, exposure time of 2-10 s and layer thickness of 30 μm. The microstructure of Al2O3, ZrO2 and MgO ceramic bodies is changed from porous to dense by heating in stages. Compared with the printed green bodies, the shrinkage rate of ceramic sintered body in three directions is in the range of 20%-23%. The compression strength and bending strength of photocured 3D printing ceramics can reach the level of isostatic pressing process, among which 3D printing ZrO2 ceramics have the highest strength. After the thermal shock resistance test, the three kinds of photocured 3D printing ceramics have more than 15 thermal shocks at 800 ℃, among which ZrO2 ceramics have the best thermal shock resistance at 800 ℃ and 1 300 ℃. The results show that the microstructure of the ceramic green body becomes densified from porous structure after sintering at appropriate temperature. Through the thermal shock resistance test, DLP 3D printing ceramics show good thermal shock resistance. DLP 3D printing technology shows great advantages in the preparation of ceramic components with complex structures and functions, which can greatly reduce the manufacturing cycle and cost, and provide important technical support for the manufacture of high-precision products in the field of nuclear energy.

     

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