数字光处理制备金刚石结构多孔氮化硅陶瓷的孔径调控与力学性能

Aperture regulation and mechanical properties of diamond-structured porous silicon nitride ceramics fabricated by digital light processing

  • 摘要: 背景 氮化硅(silicon nitride,Si3N4)是前景广阔的牙科生物陶瓷材料,数字光处理(digital light processing,DLP)是高精度先进3D打印技术,目前尚缺乏DLP成型Diamond 型三周期极小曲面(triply periodic minimal surfaces,TPMS)多孔氮化硅牙科种植体的相关研究。目的 通过数字光处理技术制备300 ~ 600 μm孔径梯度的Diamond(金刚石)型TPMS结构多孔氮化硅陶瓷,分析其微观结构与力学性能,筛选适配牙科种植体的最优孔径参数。方法 基于Diamond 型TPMS拓扑结构特征,固定单元晶胞尺寸,设计四组不同孔径(300、400、500、600 μm)的三维模型,将各组总孔隙率波动严格控制在5%以内,构建以孔径为唯一变量的单因素实验体系;通过DLP技术打印坯体并经高温烧结制备样品,每组设置5 ~ 6 个平行样本。采用X射线衍射仪(X-ray diffractometer,XRD)、扫描电子显微镜(scanning electron microscope,SEM)表征材料物相组成与微观形貌,通过阿基米德排水法测定总孔隙率,依据ISO 14704-2016、GB/T 10700-2006 标准,借助万能力学试验机测试样品的抗弯强度与弹性模量,采用单因素方差分析(one-way ANOVA)进行组间数据统计学比较。结果 所制备样品的主晶相为β-Si3N4,宏观结构完整,孔隙呈三维连通状态。随设计孔径增大,样品总孔隙率从45.04%呈梯度升高至50.06%,抗弯强度从110.69 ± 1.25 MPa单调降至74.47 ± 1.05 MPa,弹性模量呈阶梯式非线性升高,变化过程中存在小幅波动趋势,所有核心力学指标组间差异均具有极显著统计学意义(P<0.001)。其中300 μm孔径组展现出最优的力学性能组合,抗弯强度达到最高值(110.69 ± 1.25 MPa),同时弹性模量低至13.45 ± 0.20 GPa,与人体颌骨皮质骨的力学参数范围高度匹配。结论 调控Diamond 型TPMS结构的孔径参数,可有效协同调控多孔氮化硅陶瓷的孔隙特征与力学响应特性。300 μm孔径结构实现了高强度与低模量的最佳平衡,具备优异的骨组织力学适配性,为高性能“致密核心——多孔表层”梯度氮化硅口腔种植体的多孔表层结构优化设计提供了实验依据与数据支撑。

     

    Abstract: Background Silicon nitride (Si3N4) is a promising bioceramic material for dental applications, and digital light processing (DLP) is an advanced 3D printing (additive manufacturing) technology with high fabrication precision. However, there is a paucity of systematic investigations on DLP-fabricated porous Si3N4 dental implants with Diamond-type triply periodic minimal surfaces (TPMS) architecture.Objective The aim of this study was to fabricate porous Si3N4 ceramics with Diamond-type TPMS architecture and a pore size gradient ranging from 300 to 600 μm via DLP technology, to characterize their microstructure and mechanical properties, and to identify the optimal pore size parameters suitable for dental implant applications. Methods Based on the topological characteristics of Diamond-type TPMS structure, three-dimensional models with four different pore sizes (300, 400, 500, and 600 μm) were designed with a fixed unit cell size. The fluctuation of total porosity among each group was strictly controlled within 5% to establish a single-factor experimental system with pore size as the sole variable. Green bodies were printed via DLP technology and sintered at high temperature to prepare specimens, with 5 - 6 replicate specimens set for each group. The phase composition and microstructure of the materials were characterized by X-ray diffractometer (XRD) and scanning electron microscope (SEM). Total porosity was measured by the Archimedes method. The flexural strength and elastic modulus of the specimens were tested using a universal mechanical testing machine in accordance with ISO 14704-2016 and GB/T 10700-2006 standards. One-way analysis of variance (ANOVA) was used for statistical comparison of data among groups.Results  The main crystalline phase of the as-prepared samples was β -Si3N4, with an intact macrostructure and a three-dimensionally interconnected pore network. As the designed pore size increased, the total porosity of the samples increased in a gradient manner from 45.04% to 50.06%, the flexural strength decreased monotonically from 110.69 ± 1.25 MPa to 74.47 ± 1.05 MPa, and the elastic modulus exhibited a stepwise non-linear increase accompanied by minor fluctuations throughout the variation. There were extremely significant statistical differences in all core mechanical parameters among the groups (P<0.001). Notably, the group with a designed pore size of 300 μm presented the optimal combination of mechanical properties, with the highest flexural strength (110.69 ± 1.25 MPa) and a low elastic modulus of 13.45 ± 0.20 GPa, which was highly consistent with the mechanical parameter range of human mandibular cortical bone. Conclusion Tailoring the pore size parameters of Diamond-type TPMS structure can effectively and synergistically regulate the pore characteristics and mechanical response properties of porous Si3N4 ceramics. The 300 μm pore size structure achieves the optimal balance between high strength and low modulus, with excellent mechanical compatibility with bone tissue. It provides core experimental basis and data support for the optimal design of the porous surface structure of highperformance "dense core-porous surface" gradient Si3N4 dental implants.

     

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