CN112608136A - 一种高气孔率陶瓷型芯的光固化3d打印制造方法 - Google Patents

一种高气孔率陶瓷型芯的光固化3d打印制造方法 Download PDF

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CN112608136A
CN112608136A CN202011511034.9A CN202011511034A CN112608136A CN 112608136 A CN112608136 A CN 112608136A CN 202011511034 A CN202011511034 A CN 202011511034A CN 112608136 A CN112608136 A CN 112608136A
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ceramic core
photocuring
graphene
ceramic
alumina
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刘永胜
李鹤
刘岩松
曾庆丰
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Northwestern Polytechnical University
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Abstract

本发明涉及一种高气孔率陶瓷型芯的光固化3D打印制造方法，将石墨烯加入到以氧化铝为主体的无机粉体中并混合均匀，将上述混合物加入到光敏树脂中，得到陶瓷浆料；将陶瓷浆料倒入光固化3D打印机中并在紫外灯固化条件下打印得到陶瓷型芯素坯；将陶瓷型芯素坯置于管式炉中，在氩气气氛中以一定升温速率、温度、保温时间条件下完成脱脂过程；再转移至马弗炉中，在空气气氛中以一定升温速率、温度、保温时间条件下完成石墨烯的脱除及烧结过程。本发明通过在陶瓷浆料中引入石墨烯，并在热处理过程将其中除去，提高了陶瓷型芯的气孔率，降低了脱除难度，利于陶瓷型芯的脱除过程。可应用于氧化铝基陶瓷型芯的生产领域。

Description

一种高气孔率陶瓷型芯的光固化3D打印制造方法
技术领域
本发明属于增材制造技术领域，涉及一种高气孔率陶瓷型芯的光固化3D打印制造方法。
背景技术
氧化铝基陶瓷型芯因结构复杂、高温化学稳定性良好，而用于成型空心叶片内腔的精密结构。
3D打印技术为陶瓷型芯的制造提供了高效快速的成型方法，然而由于氧化铝难以与碱液反应脱除，限制了其在工业上的应用。提高陶瓷型芯的气孔率可以为碱液提供更多的接触空间，有利于陶瓷型芯的去除。
中科院金属研究所(中国专利，专利号CN102266906A)提出了添加纳米碳管制备陶瓷型芯的制备方法，通过纳米碳管烧结后形成的空间管道连接型芯中的空隙，加快型芯与化学试剂的反应速率，从而加快的型芯脱除过程。辽宁航安特铸材料有限公司(中国专利，专利号CN108326239A)提出了引入球形石墨制备陶瓷型芯的方法，由于石墨在烧结过程中的氧化脱除，导致型芯内部疏松多孔，从而易于陶瓷型芯的脱除过程。然而这些制备方法使用的陶瓷型芯的成型技术过于繁琐，限制了其在工业上的应用。
制备陶瓷型芯仍存在成型过程繁琐复杂、气孔率较低难以脱除等难题，阻碍了该技术在工业生产中的应用。
发明内容
要解决的技术问题
为了避免现有技术的不足之处，本发明提出一种高气孔率陶瓷型芯的光固化3D打印制造方法，适用于高气孔率陶瓷型芯的制造。
技术方案
一种高气孔率陶瓷型芯的光固化3D打印制造方法，其特征在于步骤如下：
步骤1：将石墨烯加入到以氧化铝为主体的无机粉体中并混合均匀，将上述混合物加入到光敏树脂丙烯酸树脂中，得到陶瓷浆料；
所述石墨烯占总粉体的质量百分含量为0.05％～15％，以氧化铝为主体的无机粉体占总粉体的质量百分含量为85％～99.95％；
所述陶瓷浆料中粉体所占的质量百分含量为50％～90％，光敏树脂所占的质量百分含量为10％～50％；
步骤2：将陶瓷浆料倒入光固化3D打印机中并在紫外灯固化条件下打印得到陶瓷型芯素坯；
步骤3：将陶瓷型芯素坯置于管式炉中，在氩气气氛中，以升温速率为0.2-5℃/min、温度为350-650℃、保温时间为0.5-6h条件下完成脱脂过程；
步骤4：再转移至马弗炉中，在空气气氛中以升温速率为0.1-10℃/min、温度为550-1550℃、保温时间为0.1-10h完成石墨烯的脱除及烧结过程。
所述以氧化铝为主体的无机粉体包含氧化铝与氧化硅、氧化铜、氧化锆、氧化钛、氧化钇、氧化钙、氧化镁中的一种或者多种组成的混合物。
所述以氧化铝为主体的无机粉体中氧化铝与其他物质的比例为：6～6.3︰1～0.7。
所述氩气气氛为高纯氩，其纯度大于99.999％。
有益效果
本发明提出的一种高气孔率陶瓷型芯的光固化3D打印制造方法，(1)将石墨烯加入到以氧化铝为主体的无机粉体中并混合均匀，将上述混合物加入到光敏树脂中，得到陶瓷浆料；(2)将上述陶瓷浆料倒入光固化3D打印机中并在特定条件下打印得到陶瓷型芯素坯；(3)将上步得到的陶瓷型芯素坯置于管式炉中，在氩气气氛中以一定升温速率、温度、保温时间条件下完成脱脂过程；(4)将上步得到的样品转移至马弗炉中，在空气气氛中以一定升温速率、温度、保温时间条件下完成石墨烯的脱除及烧结过程。本发明通过在陶瓷浆料中引入石墨烯，并在热处理过程将其中除去，提高了陶瓷型芯的气孔率，降低了脱除难度，利于陶瓷型芯的脱除过程。可应用于氧化铝基陶瓷型芯的生产领域。
本发明的有益效果：
通过在陶瓷浆料中引入石墨烯，并在热处理过程将其中除去，提高了陶瓷型芯的气孔率，降低了脱除难度，利于陶瓷型芯的脱除过程。可应用于氧化铝基陶瓷型芯的生产领域。解决了现有技术中制备陶瓷型芯仍存在成型过程繁琐复杂、气孔率较低难以脱除等难题，使得该技术在工业生产中的应用。
由于在组分中引入的石墨烯可在高温下(800～1550℃)除去，使得打印所得素坯中含有更多可除去的成分，进而引入了气孔，从而提高了陶瓷型芯的气孔率，降低了脱除难度，利于陶瓷型芯的脱除过程。脱脂后样品的微观结构如图1所示。其中大颗粒为氧化铝，氧化铝颗粒间填充物为石墨烯，即起到提高气孔率的有效成分。且本发明的配方及组份不是简单的能够确定的。本发明的高气孔率陶瓷型芯的光固化3D打印制造方法的素坯成型过程操作简洁，流程简易，极大的缩短了陶瓷型芯的周期，提高了生产效率。
附图说明
图1：脱脂后样品的微观结构图
图2：高气孔率陶瓷型芯的光固化3D打印制造流程图
具体实施方式
现结合实施例、附图对本发明作进一步描述：
实施例1
将由石墨烯(10g)、氧化铝粉(600g)和氧化硅粉(90g)混合均匀组成的700g无机粉体加入到300g光敏树脂中，得到陶瓷浆料；然后将得到的陶瓷浆料通过光固化3D打印机打印得到陶瓷型芯素坯；将得到的陶瓷型芯素坯置于管式炉中，在氩气气氛中以1℃/min的升温速率升至500℃并保温2h；然后将其转移至马弗炉中，以1℃/min的升温速率升至550℃并保温2h，然后以5℃/min的升温速率升至1400℃并保温2h，即得到具有高气孔率的陶瓷型芯。
实施例2
将由石墨烯(50g)、氧化铝粉(600g)和氧化锆粉(100g)混合均匀组成的750g无机粉体加入到250g光敏树脂中，得到陶瓷浆料；然后将得到的陶瓷浆料通过光固化3D打印机得到陶瓷型芯素坯；将得到的陶瓷型芯素坯置于管式炉中，在氩气气氛中以2℃/min的升温速率升至550℃并保温1h；然后将其转移至马弗炉中，以2℃/min的升温速率升至650℃并保温1h，然后以7℃/min的升温速率升至1450℃并保温2h，即得到具有高气孔率的陶瓷型芯。
实施例3
将由石墨烯(10g)、氧化铝粉(63g)和氧化钇粉(7g)混合均匀组成的80g无机粉体加入到20g光敏树脂中，得到陶瓷浆料；然后将得到的陶瓷浆料通过光固化3D打印机得到陶瓷型芯素坯；将得到的陶瓷型芯素坯置于管式炉中，在氩气气氛中以5℃/min的升温速率升至600℃并保温3h；然后将其转移至马弗炉中，以5℃/min的升温速率升至600℃并保温3h，然后以10℃/min的升温速率升至1350℃并保温3h，即得到具有高气孔率的陶瓷型芯。

Claims (4)

1.一种高气孔率陶瓷型芯的光固化3D打印制造方法，其特征在于步骤如下：
步骤1：将石墨烯加入到以氧化铝为主体的无机粉体中并混合均匀，将上述混合物加入到光敏树脂丙烯酸树脂中，得到陶瓷浆料；
所述石墨烯占总粉体的质量百分含量为0.05％～15％，以氧化铝为主体的无机粉体占总粉体的质量百分含量为85％～99.95％；
所述陶瓷浆料中粉体所占的质量百分含量为50％～90％，光敏树脂所占的质量百分含量为10％～50％；
步骤2：将陶瓷浆料倒入光固化3D打印机中并在紫外灯固化条件下打印得到陶瓷型芯素坯；
步骤3：将陶瓷型芯素坯置于管式炉中，在氩气气氛中，以升温速率为0.2-5℃/min、温度为350-650℃、保温时间为0.5-6h条件下完成脱脂过程；
步骤4：再转移至马弗炉中，在空气气氛中以升温速率为0.1-10℃/min、温度为550-1550℃、保温时间为0.1-10h完成石墨烯的脱除及烧结过程。
2.根据权利要求1所述高气孔率陶瓷型芯的光固化3D打印制造方法，其特征在于：所述以氧化铝为主体的无机粉体包含氧化铝与氧化硅、氧化铜、氧化锆、氧化钛、氧化钇、氧化钙、氧化镁中的一种或者多种组成的混合物。
3.根据权利要求1或2所述高气孔率陶瓷型芯的光固化3D打印制造方法，其特征在于：所述以氧化铝为主体的无机粉体中氧化铝与其他物质的比例为：6～6.3︰1～0.7。
4.根据权利要求1所述高气孔率陶瓷型芯的光固化3D打印制造方法，其特征在于：所述氩气气氛为高纯氩，其纯度大于99.999％。
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