CN108046779A - 采用激光选区烧结制备复杂结构空心球陶瓷零件的方法 - Google Patents

采用激光选区烧结制备复杂结构空心球陶瓷零件的方法 Download PDF

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CN108046779A
CN108046779A CN201711375281.9A CN201711375281A CN108046779A CN 108046779 A CN108046779 A CN 108046779A CN 201711375281 A CN201711375281 A CN 201711375281A CN 108046779 A CN108046779 A CN 108046779A
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hollow ball
ceramic
labyrinth
sls
sintering
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吴甲民
刘珊珊
史玉升
文世峰
陈敬炎
陈安南
李晨辉
陈芬
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Huazhong University of Science and Technology
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Abstract

本发明属于快速成型技术领域，并公开了采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，包括如下步骤：(1)根据实际需求设计出复杂结构空心球陶瓷零件的三维模型；(2)将由陶瓷空心球组成的原材料粉体进行预烧；(3)将粘结剂和原材料粉体进行混合，以获得SLS用复合陶瓷空心球成型粉体；(4)将步骤(3)中所得SLS用复合陶瓷空心球成型粉体在SLS设备上进行成型，通过调整SLS成型工艺参数得到满足要求的空心球陶瓷素坯；(5)将步骤(4)中所得空心球陶瓷素坯依次进行脱脂和烧结，得到所需的复杂结构空心球陶瓷零件。本发明将SLS技术和陶瓷空心球材料相结合，可以直接制备出更高孔隙率的多孔复杂结构空心球陶瓷零件。

Description

采用激光选区烧结制备复杂结构空心球陶瓷零件的方法
技术领域
本发明属于快速成型技术领域，更具体地，涉及一种采用激光选区烧结制备复杂结构空心球陶瓷零件的方法。
背景技术
多孔陶瓷将陶瓷材料自身的优异性能和气孔特性有效结合，具有良好的化学稳定性、孔隙率高等优异的性能，作为过滤材料、催化剂载体、保温隔热材料、生物功能材料等，已经广泛应用于化工、能源、生物医药、环境保护和航空航天等诸多领域。目前广泛应用的多孔陶瓷大部分由挤压成型、模板法、发泡法、冷冻干燥法、添加造孔剂等传统方法制备。但是这些传统制备方法难以成型复杂结构的多孔陶瓷，而且制备的多孔陶瓷性能和孔隙可控性不强，急需寻找一种新型的多孔陶瓷制备方法。
增材制造(Additive Manufacturing，AM)技术是一种由零件三维数据驱动直接制造零件的方法，在制备复杂形状的零件方面具有其他工艺不可比拟的优势。而其中的激光选区烧结(Selective laser sintering，SLS)技术由于使用的成型材料十分广泛，非常适用于陶瓷粉体材料的成型，所以广泛用于成型复杂结构陶瓷零件。SLS成型陶瓷的原理决定了该工艺更加适用于成型多孔陶瓷零件，由于粘结剂的存在，在烧结后，陶瓷零件内部可以形成大量微观孔隙结构。但是，目前用SLS技术直接成型的多孔陶瓷零件普遍强度较低，并且无法有效调控多孔陶瓷的综合性能。粉末性能对SLS成型陶瓷零件性能有很大影响，要求用于SLS成型的原材料粉末具有良好的流动性和适宜的粒径分布(一般要求10-150μm)，但是传统成型过程中，制备适合于SLS成型的粉体不仅流程复杂，成本也较高。
陶瓷空心球是一种尺寸微小形状为球形的新型空心无机非金属材料，具有尺寸稳定、抗冲击能力强、低导热、热稳定性好以及制备成本低等优点。陶瓷空心球本身具有气孔，在制备多孔陶瓷时，可以有效避免造孔剂等其他材料的加入，不会引入杂质和产生其他缺陷。陶瓷空心球的尺寸和成分可以通过调整空心球的制备工艺来进行设计，从而有效控制多孔陶瓷的孔径大小、气孔率和力学性能等。是一种制备多孔陶瓷的理想材料。但是现有的空心球陶瓷制备工艺大多采用干压法和胶态成型法，这些方法依赖于模具，导致产品开发周期长、加工成本高，不利于产品的更新换代，而且，所能成型的形状也受到了模具加工的限制，难以成型甚至无法成型复杂结构陶瓷坯体。
发明内容
针对现有技术的以上缺陷或改进需求，本发明提供了采用激光选区烧结制备复杂结构空心球陶瓷零件的方法。直接使用陶瓷空心球作为原材料通过SLS技术制备多孔陶瓷，不仅将SLS直接成型复杂结构陶瓷零件的特点和陶瓷空心球制备高性能多孔陶瓷的优点充分结合，还利用陶瓷空心球的特性解决了SLS原材料的问题，保证了零件的成型性能，并使最终成型的多孔陶瓷性能可控。同时，利用陶瓷空心球本身的气孔，加上SLS成型过程中形成的孔隙，可以制备更高孔隙率的多孔陶瓷。
为实现上述目的，按照本发明，提供了采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，包括如下步骤：
(1)根据实际需求设计出复杂结构空心球陶瓷零件的三维模型；
(2)将由陶瓷空心球组成的原材料粉体进行预烧，以增加陶瓷空心球的强度并保证其具备烧结活性；
(3)将粘结剂和步骤(2)中预烧后的原材料粉体进行混合，以获得SLS用复合陶瓷空心球成型粉体；
(4)将步骤(1)的三维模型导入SLS设备，然后将步骤(3)中所得SLS用复合陶瓷空心球成型粉体在SLS设备上进行成型，通过调整SLS成型工艺参数得到满足要求的空心球陶瓷素坯；
(5)将步骤(4)中所得空心球陶瓷素坯依次进行脱脂和烧结，得到所需的复杂结构空心球陶瓷零件。
优选地，步骤(2)中的陶瓷空心球的材料为氧化物、氮化物、碳化物和硅酸铝盐中的一种或多种，陶瓷空心球的内部为完全中空或者多孔；陶瓷空心球的预烧温度根据空心球具体材料来制定，以保证预烧后陶瓷空心球具有烧结活性和强度，从而保证陶瓷空心球能再次被烧结且成型过程中不易溃散，原材料粉体中陶瓷空心球的平均粒径为10μm-150μm。
优选地，步骤(3)中的混合方法为机械混合法、溶解沉淀法或溶剂蒸发法。
优选地，步骤(3)中的粘结剂为有机粘结剂，所述有机粘结剂为热固性聚合物和/或热塑性聚合物，其中热固性聚合物为环氧树脂和/或热固性酚醛树脂，热塑性聚合物为聚丙烯、聚甲基丙烯酸甲酯、硬脂酸、苯乙烯和尼龙中的一种或多种。
优选地，步骤(4)中的SLS成型工艺参数中，根据具体使用的粘结剂种类和SLS用复合陶瓷空心球成型粉体性质，SLS用复合陶瓷空心球成型粉体的预热温度为30℃～150℃，单层铺粉层厚为0.1mm～0.3mm，激光扫描间距为0.1mm～0.3mm，激光功率为5W～20W，扫描速度为1000mm/s～3000mm/s。
优选地，步骤(5)中的脱脂工艺的参数如下：脱脂温度为400℃～600℃，保温1h～3h，升温速率为0.3℃/min～2℃/min。
优选地，所述步骤(5)中的烧结工艺的参数如下：烧结温度为1450℃～1950℃，保温2h～3h。
总体而言，通过本发明所构思的以上技术方案与现有技术相比，能够取得下列有益效果：
1)制备工艺简单，不需要模具，可以直接制备出设计的复杂结构多孔陶瓷；
2)采用陶瓷空心球作为原材料，不仅避免造孔剂等杂质的引入和其他缺陷的产生，还能通过调整空心球的制备工艺来控制其尺寸和成分，从而有效调控空心球陶瓷的气孔大小、孔隙率等综合性能；
3)将SLS技术和陶瓷空心球材料相结合，可以制备更高孔隙率的多孔复杂结构空心球陶瓷零件；
4)空心球球形度高从而流动性好，可控的粒径分布完全满足SLS成型要求，不仅解决了SLS成型原材料的问题，避免了传统SLS成型过程中高成本、复杂的粉体制备工艺，还保证了最终多孔空心球陶瓷的成型性能。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1：
首先根据实际需求优化设计出多孔陶瓷的三维模型。将平均直径为100μm的Al2O3陶瓷空心球在1200℃进行预烧，使其具有一定的机械强度，同时又具有烧结活性。然后采用机械混合法在预烧过的Al2O3陶瓷空心球中均匀混合粘结剂环氧树脂E12，得到Al2O3/E12复合陶瓷空心球粉体。将所得复合陶瓷空心球粉体在SLS设备上进行成型，预热温度为30℃，铺粉层厚为0.15mm，扫描间距为0.11mm，激光功率为7W，扫描速度为2000mm/s，得到多孔陶瓷素坯。最后对素坯进行脱脂等后处理和烧结得到Al2O3空心球陶瓷。素坯脱脂温度为600℃，保温1h，升温速率为0.3℃/min；烧结温度为1550℃，保温2h。所得Al2O3空心球陶瓷的孔隙率为70％，抗弯强度为21MPa。
实施例2
首先根据实际需求优化设计出多孔陶瓷的三维模型。将平均直径为10μm的SiO2-Al2O3陶瓷空心球在1150℃进行预烧，使其具有一定的机械强度，同时又具有烧结活性。然后采用溶解沉淀法在预烧过的SiO2-Al2O3陶瓷空心球上包覆粘结剂尼龙PA12，得到SiO2-Al2O3/PA12复合陶瓷空心球粉体。将所得复合陶瓷空心球粉体在SLS设备上进行成型，预热温度为150℃，铺粉层厚为0.1mm，扫描间距为0.1mm，激光功率为15W，扫描速度为1000mm/s，得到多孔陶瓷素坯。最后对素坯进行脱脂等后处理和烧结得到莫来石多孔陶瓷。素坯脱脂温度为500℃，保温3h，升温速率为1℃/min；烧结温度为1450℃，保温2.5h。所得莫来石多孔陶瓷的孔隙率为81％，抗压强度为6MPa。
实施例3
首先根据实际需求优化设计出多孔陶瓷的三维模型。将平均直径为150μm的Si3N4陶瓷空心球在1600℃进行预烧，使其具有一定的机械强度，同时又具有烧结活性。然后采用机械混合法在预烧过的Si3N4陶瓷空心球中均匀混合粘结剂环氧树脂E12，得到Si3N4/E12复合陶瓷空心球粉体。将所得复合陶瓷空心球粉体在SLS设备上进行成型，预热温度为50℃，铺粉层厚为0.3mm，扫描间距为0.3mm，激光功率为5W，扫描速度为1800mm/s，得到多孔陶瓷素坯。最后对素坯进行脱脂等后处理和烧结得到Si3N4空心球陶瓷。素坯脱脂温度为600℃，保温2h，升温速率为2℃/min；烧结温度为1750℃，保温2h。所得Si3N4空心球陶瓷的孔隙率为75％，抗压强度为34MPa。
实施例4
首先根据实际需求优化设计出多孔陶瓷的三维模型。将平均直径为50μm的SiC陶瓷空心球在1750℃进行预烧，使其具有一定的机械强度，同时又具有烧结活性。然后采用溶解沉淀法在预烧过的SiC陶瓷空心球上包覆粘结剂尼龙PA12，得到SiC/PA12复合陶瓷空心球粉体。将所得复合陶瓷空心球粉体在SLS设备上进行成型，预热温度为150℃，铺粉层厚为0.15mm，扫描间距为0.17mm，激光功率为20W，扫描速度为2200mm/s，得到多孔陶瓷素坯。最后对素坯进行脱脂等后处理和烧结得到SiC空心球陶瓷。素坯脱脂温度为500℃，保温2h，升温速率为0.5℃/min；烧结温度为1950℃，保温3h。所得SiC空心球陶瓷的孔隙率为76％，抗压强度为9MPa。
实施例5
首先根据实际需求优化设计出多孔陶瓷的三维模型。将平均直径为85μm的Al2O3-ZrO2陶瓷空心球在1300℃进行预烧，使其具有一定的机械强度，同时又具有烧结活性。然后采用溶剂蒸发法在预烧过的Al2O3-ZrO2陶瓷空心球上包覆粘结剂硬脂酸，得到Al2O3-ZrO2/硬脂酸复合陶瓷空心球粉体。将所得复合陶瓷空心球粉体在SLS设备上进行成型，预热温度为69℃，铺粉层厚为0.2mm，扫描间距为0.13mm，激光功率为18W，扫描速度为3000mm/s，得到多孔陶瓷素坯。最后对素坯进行脱脂等后处理和烧结得到Al2O3-ZrO2空心球陶瓷。素坯脱脂温度为400℃，保温2h，升温速率为0.8℃/min；烧结温度为1600℃，保温3h。所得Al2O3-ZrO2空心球陶瓷的孔隙率为78％，抗压强度为12MPa。
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，包括如下步骤：
(1)根据实际需求设计出复杂结构空心球陶瓷零件的三维模型；
(2)将由陶瓷空心球组成的原材料粉体进行预烧，以增加陶瓷空心球的强度并保证其具备烧结活性；
(3)将粘结剂和步骤(2)中预烧后的原材料粉体进行混合，以获得SLS用复合陶瓷空心球成型粉体；
(4)将步骤(1)的三维模型导入SLS设备，然后将步骤(3)中所得SLS用复合陶瓷空心球成型粉体在SLS设备上进行成型，通过调整SLS成型工艺参数得到满足要求的空心球陶瓷素坯；
(5)将步骤(4)中所得空心球陶瓷素坯依次进行脱脂和烧结，得到所需的复杂结构空心球陶瓷零件。
2.根据权利要求1所述的采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，步骤(2)中的陶瓷空心球的材料为氧化物、氮化物、碳化物和硅酸铝盐中的一种或多种，陶瓷空心球的内部为完全中空或者多孔；陶瓷空心球的预烧温度根据空心球具体材料来制定，以保证预烧后陶瓷空心球具有烧结活性和强度，从而保证陶瓷空心球能再次被烧结且成型过程中不易溃散，原材料粉体中陶瓷空心球的平均粒径为10μm-150μm。
3.根据权利要求1所述的采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，步骤(3)中的混合方法为机械混合法、溶解沉淀法或溶剂蒸发法。
4.根据权利要求1所述的采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，步骤(3)中的粘结剂为有机粘结剂，所述有机粘结剂为热固性聚合物和/或热塑性聚合物，其中热固性聚合物为环氧树脂和/或热固性酚醛树脂，热塑性聚合物为聚丙烯、聚甲基丙烯酸甲酯、硬脂酸、苯乙烯和尼龙中的一种或多种。
5.根据权利要求1所述的采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，步骤(4)中的SLS成型工艺参数中，根据具体使用的粘结剂种类和SLS用复合陶瓷空心球成型粉体性质，SLS用复合陶瓷空心球成型粉体的预热温度为30℃～150℃，单层铺粉层厚为0.1mm～0.3mm，激光扫描间距为0.1mm～0.3mm，激光功率为5W～20W，扫描速度为1000mm/s～3000mm/s。
6.根据权利要求1所述的采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，步骤(5)中的脱脂工艺的参数如下：脱脂温度为400℃～600℃，保温1h～3h，升温速率为0.3℃/min～2℃/min。
7.根据权利要求1所述的采用激光选区烧结制备复杂结构空心球陶瓷零件的方法，其特征在于，所述步骤(5)中的烧结工艺的参数如下：烧结温度为1450℃～1950℃，保温2h～3h。
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Application publication date: 20180518