织构化多孔Al2O3-SiO2复合陶瓷片-球混合浆料特性及光强分布仿真

doi:10.15541/jim20230553

无机材料学报 ›› 2024, Vol. 39 ›› Issue (7): 769-778.DOI: 10.15541/jim20230553

织构化多孔Al₂O₃-SiO₂复合陶瓷片-球混合浆料特性及光强分布仿真

武向权¹^,²(), 滕家琛¹, 季祥旭¹, 郝禹博¹, 张忠明¹^,², 徐春杰¹^,²()

1.西安理工大学材料科学与工程学院, 西安 710048
2.西安理工大学谢赫特曼诺奖新材料研究院, 西安 710048

收稿日期:2023-12-04 修回日期:2024-02-06 出版日期:2024-02-22 网络出版日期:2024-02-22
通讯作者: 武向权, 讲师. E-mail: xqwu@xaut.edu.cn;
徐春杰, 教授. E-mail: xuchunjie@xaut.edu.cn
作者简介:武向权(1989-), 男, 讲师. E-mail: xqwu@xaut.edu.cn
基金资助:
陕西省重点研发计划一般项目(2024GX-YBXM-225);西安市科技计划项目(22GXFW0072);中国博士后面上基金(2021MD703876);陕西省国际科技合作计划重点项目(2023-GHZD-50)

Textured Porous Al₂O₃-SiO₂ Composite Ceramic Platelet-sphere Slurry: Characteristics and Simulation of Light Intensity Distribution

WU Xiangquan¹^,²(), TENG Jiachen¹, JI Xiangxu¹, HAO Yubo¹, ZHANG Zhongming¹^,², XU Chunjie¹^,²()

1. School of Materials Science and Engineering, Xi’an University of Technology, Xi’an 710048, China
2. Xi’an Shechtman Nobel Prize New Materials Institute, Xi'an University of Technology, Xi’an 710048, China

Received:2023-12-04 Revised:2024-02-06 Published:2024-02-22 Online:2024-02-22
Contact: WU Xiangquan, lecturer. E-mail: xqwu@xaut.edu.cn;
XU Chunjie, professor. E-mail: xuchunjie@xaut.edu.cn
About author:WU Xiangquan (1989-), male, lecturer. E-mail: xqwu@xaut.edu.cn
Supported by:
General Project of Shaanxi Key Research and Development Plan(2024GX-YBXM-225);Xi’an Bureau of Science and Technology(22GXFW0072);The Project funded by China Postdoctoral Science Foundation(2021MD703876);International Science and Technology Cooperation Program of Shaanxi Province(2023-GHZD-50)

摘要/Abstract

摘要：

陶瓷光固化技术在制备Al₂O₃-SiO₂复合陶瓷方面具有广阔前景, 织构化的Al₂O₃-SiO₂复合陶瓷在陶瓷光固化增材制备方面亟待研究。本工作研究了添加片状氧化铝、等轴氧化铝、球形二氧化硅的片-球混合陶瓷光固化浆料的特性。针对不同固相配比, 研究了浆料的黏度、沉降性、固化特性和固化精度, 并针对所研究的片-球混合浆料开发了一种紫外光强分布模拟算法, 对浆料在曝光中的光强分布进行了理论模拟分析, 最终成功制备了具有片状氧化铝定向特征的织构化多孔Al₂O₃-SiO₂复合陶瓷。研究结果表明, 片状氧化铝与球状粉体组合可以使浆料在高固相含量(总固相体积分数40%~45%, 片状氧化铝体积分数占50%~60%)下保持低黏度和剪切稀释性。在相同总固相含量下, 增大片状氧化铝或球形二氧化硅的含量能够减小浆料的黏度, 从而提高浆料的沉降率。片状氧化铝相比于等轴氧化铝可以减少浆料对紫外光的阻挡和散射作用。在相同曝光能量条件下, 降低等轴氧化铝、增加球形二氧化硅的含量可以增加的浆料固化厚度; 而增加片状氧化铝和球形二氧化硅的含量会扩大尺寸误差。理论模拟结果表明, 接近水平分布的片状氧化铝对光的阻挡和偏转作用弱, 接近垂直分布的片状氧化铝对紫外光具有引导作用。模型上边界紫外光强平均值的变化与固化厚度测量值的变化接近, 所建立的模型可以为浆料固化厚度的实验测试结果提供理论支持。

关键词: 陶瓷光固化, Al₂O_3-SiO₂复合陶瓷, 片状氧化铝, 光强分布模拟, 浆料特性

Abstract:

Ceramic stereolithography has a broad prospect in preparation of Al₂O₃-SiO₂ composite ceramics through which the prepared textured Al₂O₃-SiO₂ composite still faces challenges in improving their slurry quality and light intensity distribution. Here, characteristics of a novel ceramic slurry with addition of alumina platelet, equiaxed alumina, and spherical silica were investigated. Comparative analysis on viscosity, sedimentation, curing characteristics, and curing accuracy of the slurry with different solid content was carried out. Simulation algorithm of ultraviolet (UV) light intensity distribution was developed, and theoretical simulation analysis of light intensity distribution in the slurry during light exposure was carried out. Results of the prepared textured porous Al₂O₃-SiO₂composite with the characteristics of oriented alumina platelet showed that combination of alumina platelet with spherical powders endowed the slurry with low viscosity and shear shinning behavior at high solid content in volume (40%-45%) of which alumina platelet took 50%-60%. Under the same content of the total solid, increasing either amount of alumina platelet or amount of spherical silica could reduce the viscosity, leading to the increase of the slurry total sedimentation. Alumina platelet in the slurry could reduce blocking and scattering of UV light better than equiaxed alumina. Under the same exposure conditions, both decreasing content of the equiaxed alumina and increasing content of the spherical silica could increase curing thickness of the slurry, while increasing content of alumina platelet and spherical silica could adversely increase error in dimension. Numerical simulation results showed that alumina platelet with approximately horizontal distribution showed week effect on UV light blocking and deflection, while that with approximately vertical distribution showed indeed guiding effect on UV light. The variation of the mean UV intensity at the upper boundary of the model was close to that of the curing thickness. Therefore, the established model can provide theoretical support for the experimental value of curing thickness.

Key words: ceramic stereolithography, Al₂O₃-SiO₂ composite ceramic, alumina platelet, light intensity distribution simulation, slurry characterization

中图分类号:

TB321

武向权, 滕家琛, 季祥旭, 郝禹博, 张忠明, 徐春杰. 织构化多孔Al₂O₃-SiO₂复合陶瓷片-球混合浆料特性及光强分布仿真[J]. 无机材料学报, 2024, 39(7): 769-778.

WU Xiangquan, TENG Jiachen, JI Xiangxu, HAO Yubo, ZHANG Zhongming, XU Chunjie. Textured Porous Al₂O₃-SiO₂ Composite Ceramic Platelet-sphere Slurry: Characteristics and Simulation of Light Intensity Distribution[J]. Journal of Inorganic Materials, 2024, 39(7): 769-778.

图/表 14

表1 配制的浆料固相成分和固相含量

Table 1 Solid-phase compositions and contents of the as-prepared slurries

Slurry No.	Total solid content/ %(in vol)	Al₂O₃-PL /%(in vol)	Al₂O₃-NP /%(in vol)	SiO₂/%(in vol)
1	40	50	30	20
2	45	50	30	20
3	45	60	20	20
4	45	60	10	30

图1 片状、球形颗粒混合浆料的光强分布模拟模型建模算法流程图

Fig. 1 Flowchart of modeling algorithm for light intensity distribution simulation model of slurry containing platelets and spherical particles

图2 光强分布分析模型及其边界条件

Fig. 2 Model of light intensity distribution and its boundary conditions

图3 粉体的扫描电镜照片

Fig. 3 SEM images of the powders (a) Al2O3-PL; (b) Frequency counts of Al2O3-PL thickness; (c) Spherical silica; (d) Al2O3-NP

图4 4组浆料的黏度和沉降性对比

Fig. 4 Comparison of viscosities and sedimentation of the four slurries (a) Viscosity change of the four slurries at the shear rate from 0.16 to 6.42 s-1; (b) Viscosity of the four slurries at a shear rate of 1.28 s-1; (c) Sedimentation of the four slurries; (d) Photography of the slurries after sedimentation; (e) Photography of the newly prepared slurry

图5 4组浆料的固化特性拟合曲线

Fig. 5 Fitting curves of curing characteristics of the four slurries

表2 浆料的透射深度及临界曝光量

Table 2 Penetration depth and critical exposure energy of the slurries

Slurry No.	Penetration depth, D_p/μm	Critical exposure energy, E_c/(mJ·cm^-2)
1	80.3	6.4
2	87.5	7.5
3	67.7	3.4
4	66.6	2.7

图6 固化单层精度分析

Fig. 6 Monolayer curing accuracy analysis (a) Mask of the monolayer and test dimensions indicated by the yellow lines and arrows; (b-e) Optical micrographs of (b) slurry 1, (c) slurry 2, (d) slurry 3, and (e) slurry 4

图7 固化单层尺寸误差频率统计

Fig. 7 Dimensional error frequency statistics of cured monolayer (a) Slurry 1; (b) Slurry 2; (c) Slurry 3; (d) Slurry 4

图8 织构化多孔结构及打印的前牙贴面

Fig. 8 Textured porous structure and the printed front tooth veneer (a, b) SEM images of the cross-sectional sintering part printed by using slurry 2; (b1) Al element distribution; (b2) Si element distribution; (c, c1) complex front tooth veneer structure

表3 采用模型生成算法生成模型的固相含量

Table 3 Solid contents of the slurry models generated by the algorithm

Slurry No.	Model No.	Total solid content/ %(in vol)^a	Al₂O₃-PL/ %(in vol)^a	Al₂O₃-NP/ %(in vol)^a	SiO₂/ %(in vol)^a	Slurry No.	Model No.	Total solid content/ %(in vol)^a	Al₂O₃-PL/ %(in vol)^a	Al₂O₃-NP/ %(in vol)^a	SiO₂/ %(in vol)^a
1	1-1	40.5	20.4	12.1	8.0	3	3-1	45.6	27.6	9.2	9.2
	1-2	39.5	20.4	11.7	7.8		3-2	45.7	27.3	9.3	9.3
	1-3	39.8	20.4	11.6	7.8		3-3	45.0	27.5	8.8	8.8
2	2-1	44.9	22.5	13.4	8.9	4	4-1	45.6	27.6	4.5	13.5
	2-2	44.9	22.5	13.4	8.9		4-2	45.1	27.3	4.5	13.4
	2-3	44.5	22.4	13.2	8.8		4-3	45.6	27.5	4.5	13.6

图9 基于浆料光强分布模拟模型建模算法建立的浆料1的3个模型对比

Fig. 9 Comparison of three models for the slurry 1 based on modeling algorithm (a) Model 1-1; (b) Model 1-2; (c) Model 1-3

图10 4组浆料模型及对应的光强分布模拟结果

Fig. 10 Four slurry models and corresponding simulation results of light intensity distribution (a) Model 1-1, (b) model 2-2, (c) model 3-3, (d) model 4-1, and their corresponding (a1-d1) cloud and (a2-d2) streamline charts of light intensity distribution

图11 光强分布模拟模型的上边界、左边界和右边界的紫外光强线平均值对比

Fig. 11 Average values of the light intensity distribution in the upper, left and right boundaries

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织构化多孔Al₂O₃-SiO₂复合陶瓷片-球混合浆料特性及光强分布仿真

Textured Porous Al₂O₃-SiO₂ Composite Ceramic Platelet-sphere Slurry: Characteristics and Simulation of Light Intensity Distribution

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