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氧化铝陶瓷DLP增材制造光固化成形与烧结质量控制

Forming Process and Sintering Quality Control of DLP Additive Manufacturing for Alumina Ceramic

作者:钱楚楚
  • 学号
    2016******
  • 学位
    博士
  • 电子邮箱
    qcc******.cn
  • 答辩日期
    2023.03.23
  • 导师
    李培杰
  • 学科名
    机械工程
  • 页码
    175
  • 保密级别
    公开
  • 培养单位
    012 机械系
  • 中文关键词
    氧化铝,DLP光固化增材制造,光固化成形机理,烧结性能,粒度级配
  • 英文关键词
    alumina ceramic, digital light processing, stereolithography forming mechanism, sintering properties of additive manufacturing, particle size grading

摘要

本文基于氧化铝陶瓷DLP光固化增材制造技术,围绕成形工艺及其烧结性能与组织演变规律进行了系统研究,总结了不同颗粒粒度级配对陶瓷浆料光固化特性及成形质量的影响规律,揭示了颗粒粒度级配、烧结方式以及烧结助剂对DLP光固化增材制造氧化铝陶瓷烧结性能的影响机制。研究成果对高精度陶瓷增材制造技术发展和复杂氧化铝陶瓷制造具有指导意义,主要研究内容包括:(1)基于Mie散射模型提出了一种包含粒度分布、随机位置定义的多颗粒光散射分析方法,描述不同颗粒粒度的陶瓷浆料在特定光入射条件下的浆料内光场分布固化轮廓,分析了入射光强、陶瓷光学特性等参数的影响规律与机制。(2)采用激光反射法、红外光谱法、红外热像仪动态原位分别测定氧化铝陶瓷浆料在DLP光固化过程中的实时收缩率、实时转化率和全幅面温度变化。分析了碳碳双键浓度、单体比例、光引发剂和入射光强等参数对固化收缩率、单体转化率的影响。建立了反应过程热扩散模型,仿真和实验结果表明增加曝光图案边界长度可降低热集中,图案不连续化可减缓最高温升、提高温度分布均匀性。提出了光固化增材制造成形精度调控指导公式。(3)研究了颗粒粒度级配对烧结过程中物理、化学变化的影响,对增材制造件层间的颗粒烧结行为进行模拟仿真。实验发现,烧结件的高度与宽度收缩率比值随粉料粒度变化,指出与边缘树脂层的存在有关,据此提出了烧结收缩修正公式。通过剪切强度对层间结合强度进行定量表征,分析颗粒粒度级配对其影响规律。采用元胞自动机计算方法模拟层间颗粒烧结过程,结果表明颗粒粒度越小,烧结温度越高,对层间间隙敏感性越强。(4)探究微波烧结和烧结助剂(CaO、TiO2、La2O3、ZrO2)对光固化增材制造氧化铝陶瓷烧结性能的影响。研究发现,微波烧结会加速层间烧结进程、提高层间结合强度,增大烧结收缩各向异性。在烧结助剂的研究中,发现3% CaO增加层间微裂纹沿内孔扩展可能性,降低抗弯强度;0.5% TiO2在烧结温度1650℃时可提高抗弯强度90 MPa;La2O3基本无细化晶粒作用;1% ZrO2在1450℃烧结时可提高15%显孔隙率和88%层间剪切强度,同时降低30%烧结收缩率。综合采用优化后工艺参数,打印了涡流器用芯-壳一体化陶瓷铸型,湿坯尺寸误差、表面粗糙度小于±0.2 mm、5 μm。氧化铝材料(粒度10 μm/ 2 μm,固含量55%,1% ZrO2,烧结温度1450℃)烧结性能满足陶瓷型芯的使用性能指标要求。

Based on the Digital Light Processing additive manufacturing technology of alumina ceramics, this paper systematically studies the forming process, sintering properties and the evolution of the microstructure. The influence mechanism of particle size distribution, sintering method and additives on the sintering performance of DLP additive manufacturing ceramics was revealed. The research results have guiding significance for the development of high-precision ceramic additive manufacturing technology and the manufacture of complex alumina ceramic cores. The main research contents are as follows:Based on the Mie scattering model, a multi-particle light scattering analysis method with particle size distribution and random positions was proposed to describe the light field distribution and edge curing of ceramic pastes with different particle sizes under specific incident conditions. The influence laws and mechanisms of parameters such as incident light intensity and ceramic optical properties were studied and analyzed.The real-time shrinkage rate, real-time conversion rate and full-width temperature change of alumina ceramic slurry during DLP photocuring were measured by laser reflection method, infrared spectroscopy method and infrared thermal imaging camera. The effects of parameters such as carbon-carbon double bond concentration, monomer ratio, photoinitiator and incident light intensity on curing shrinkage and monomer conversion were analyzed. The thermal diffusion simulation model of the reaction process was established. The simulation and experimental results showed that increasing the length of the boundary of the exposure pattern reduced the heat concentration, and optimizing it as a discontinuous pattern slowed down the maximum temperature rise and improved the uniformity of temperature distribution. Based on the above research, a guiding formula for the regulation and control of the forming accuracy of DLP additive manufacturing was proposed.The effect of particle size grading on physical and chemical changes during sintering was studied, and the sintering behavior of microscopic interlayer particles was simulated. Experiments found that the ratio of height to width sintering shrinkage varied with particle size. Combined with the sample and particle size ratio, the phenomenon was explained through the edge resin layer, and a revised calculation formula for sintering shrinkage was proposed. The shear strength was used to quantitatively characterize the interlayer bonding strength, and analysis of the influence of particle size classification on it. The cellular automata calculation method was used to simulate the sintering process of interlayer particles. The results showed that when particle size became smaller, the sintering temperature grew higher, and the sensitivity to the interlayer gap became stronger, which was consistent with the light scattering research conclusion and the sintering experiment law.The effects of microwave sintering and additives (CaO, TiO2, La2O3, ZrO2) on the sintering properties of alumina ceramics were further explored. The study found that microwave sintering accelerated the process of interlayer sintering, improved the bonding strength between layers, and increased the anisotropy of sintering shrinkage. In the research of additives, it was found that 3% CaO increased the possibility of interlayer microcracks expanding along the inner hole and reduced the flexural strength; 0.5% TiO2 increased the flexural strength by 90MPa when the sintering temperature was 1650 ℃; La2O3 basically had no refinement Grain effect; 1% ZrO2 sintered at 1450℃ increased the apparent porosity by 15% and the interlaminar shear strength by 88%, and reduced the sintering shrinkage by 30%.By comprehensively adopting the above optimized process parameters, the core-shell integrated ceramic casting of the eddy current parts was printed, the green part precision was better than ±0.2 mm, and the surface roughness was better than 5 μm. The sintering performance of the selected alumina material (10 μm/ 2 μm, 55% solid content, 1% ZrO2, sintering temperature 1450°C) met the performance requirements of the ceramic core.