CN114213107A - 一种基于陶瓷材料的3d打印成型方法 - Google Patents
一种基于陶瓷材料的3d打印成型方法 Download PDFInfo
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Abstract
本发明涉及陶瓷3D打印技术领域，具体涉及一种基于陶瓷材料的3D打印成型方法，包括如下步骤：将各种原料按比例混炼配置成预混液；向预混液中加陶瓷粉体及分散剂，并继续混炼得到混料；将得到的混料挤出、冷却、造粒以制得陶瓷喂料；将得到的陶瓷喂料进行挤出、拉丝并冷却以制得3D打印用陶瓷线材；以得到的陶瓷线材为原材料，利用3D打印加工成型，制得陶瓷生坯；将制得的陶瓷生坯经脱脂烧结制得最终的陶瓷器件。本发明所涉及的基于陶瓷材料的3D打印成型方法适用所有陶瓷粉体的加工成型，是一种适用范围及广的陶瓷增材制造技术，解决了光固化等3D打印技术仅适用于少部分陶瓷粉体的缺点。
Description
技术领域
本发明涉及陶瓷3D打印技术领域，具体涉及一种基于陶瓷材料的3D打印成型方法。
背景技术
3D打印技术(3D printing)，又称增材制造技术(Additive manufacturing)，是一种新兴的材料加工成型技术，适用于各种复杂形状器件的成型加工，具有无需模具、设计自由、节省原料、高效环保等优势。陶瓷材料性能优异，在航空航天、车辆制造、零件加工、微纳制造等领域应用广泛。然而，陶瓷材料自身硬且脆的特点带来了加工成型的困难。因此，将3D打印技术应用于陶瓷材料的加工成型，能够解决复杂结构陶瓷器件加工成型的困难，能够在各种应用需求中更好地发挥陶瓷材料性能的优势。
目前，主流的3D打印技术包括选区激光烧结技术(Selective laser sintering)、选区激光熔融技术(Selective laser melting)、光固化技术(Stereolithography)、墨水直写技术(Direct ink writing)、熔融沉积技术(Fused deposition manufacturing)等。其中，应用于复杂形状陶瓷器件加工成型的主要包括光固化3D打印技术和选区激光烧结技术。然而，陶瓷光固化3D打印技术对陶瓷粉体原料要求较高，难以加工氮化硅、碳化硅等高折射率粉体，且加工成本较高，不适合大体积陶瓷器件的加工成型；陶瓷选区激光烧结技术由于其成型特征，所制备陶瓷器件性能较差，通常需要热等静压、溶渗等后处理工艺，步骤繁琐，限制了其应用发展。
综上，目前陶瓷3D打印技术均具有一定局限性，难以满足各种陶瓷材料复杂器件的成型加工，尤其是大尺寸陶瓷异形件的加工成型，一定程度上阻碍了陶瓷3D打印技术的应用推广。
如中国发明专利《一种用于光固化3D打印的陶瓷材料、陶瓷件及其制备方法》(CN201710283233.0)中要求光固化3D打印所选用陶瓷粉体为Al2O3、ZrO2和HAP粉，所选用陶瓷粉体均为折射率较低的粉体，陶瓷光固化3D打印能够成型加工的陶瓷粉体种类受到极大的限制；文献《3D printing of dense structural ceramic microcomponents with lowcost:Tailoring the sintering kinetics and the microstructure evolution》(J.Am.Ceram.Soc,5(102)(2019)2257-2262.)中利用光固化3D打印技术制备的氧化铝陶瓷和氧化锆陶瓷异形件尺寸均在1cm以下，光固化3D打印技术难以制备大尺寸陶瓷异形件。如中国发明专利《基于増材制造的连续纤维增强SiC零件制备方法及产品》(CN201910684009.1)中利用选区激光烧结技术制备SiC陶瓷，需采用先驱体浸渍裂解法提升其力学性能，工艺较为复杂；文献《Research on selective laser sintering ofKaolin-epoxy resin ceramic powders combined with cold isostatic pressing andsintering》(Ceram Int,9(103)(2016)10711-10718)中采用选区激光烧结和冷等静压结合的方式制备高岭石质陶瓷。上述制备陶瓷器件的3D打印方法均存在可加工陶瓷粉体种类受限、制备陶瓷器件尺寸偏小、加工成本高、后处理工艺复杂等问题。
发明内容
本发明的目的在于提供基于陶瓷材料的3D打印成型方法，具有适用所有陶瓷粉体、适合大体积陶瓷器件成型、加工成本低、无需后处理等优势。
本发明实现目的所采用的方案是：一种基于陶瓷材料的3D打印成型方法，包括如下步骤：
1)将各种原料按比例混炼配置成预混液；
2)向步骤1)得到的预混液中加陶瓷粉体及分散剂，并继续混炼得到混料；
3)将步骤2)得到的混料挤出、冷却、造粒以制得陶瓷喂料；
4)将步骤3)得到的陶瓷喂料进行挤出、拉丝并冷却以制得3D打印用陶瓷线材；
5)以步骤4)得到的陶瓷线材为原材料，利用3D打印加工成型，制得陶瓷生坯；
6)将步骤5)制得的陶瓷生坯经脱脂烧结制得最终的陶瓷器件。
优选地，所述步骤1)中，粘接剂的主要成分为50vol％-70vol％的高密聚乙烯和低密聚乙烯的混合物，辅料为30vol％-50vol％的石蜡和无定型聚烯烃混合物。
优选地，所述高密聚乙烯和低密聚乙烯的体积比为7:3-5:5；所述石蜡和无定型聚烯烃的体积比为6:4-4:6。
优选地，所述步骤1)和步骤2)中，混炼温度均为160-180℃。
优选地，所述步骤2)中，陶瓷粉体可为氧化铝、氧化锆、氮化硅、碳化硅、碳化硼、莫来石、红柱石、氧化硅中的至少一种。
优选地，所述步骤2)中，分散剂为硬脂酸和/或油酸，所述分散剂的添加量为陶瓷粉体的2wt％-5wt％。
优选地，所述步骤4)中，拉丝直径在0.5-2.5mm。
优选地，所述步骤5)中，采用FDM陶瓷3D打印机加工成型。
优选地，所述步骤6)中，脱脂工艺采用两步脱脂，先采用溶剂脱脂，再采用热脱脂。
优选地，所述溶剂为环己烷和乙醇的混合物。
本发明具有以下优点和有益效果：
1、本发明所涉及的基于陶瓷材料的3D打印成型方法适用所有陶瓷粉体的加工成型，是一种适用范围及广的陶瓷增材制造技术，解决了光固化等3D打印技术仅适用于少部分陶瓷粉体的缺点；
2、本发明所涉及的基于陶瓷材料的3D打印成型方法适合各类大尺寸陶瓷器件的加工成型，更加符合实际生产需求，能够极大拓宽陶瓷3D打印技术的应用范围，解决了光固化等3D打印技术仅能够制备小尺寸陶瓷异形件的缺点，能够将成型尺寸100*100mm最大拓宽至1000*1000mm；
3、本发明所设计的基于陶瓷材料的3D打印成型方法制备各类陶瓷异形件，加工成型过程较为简单，较传统陶瓷注模成型等方式相比，成本降低80％以上，效率提高70％以上，无需复杂的后处理工艺，适合大规模推广使用，解决了选区激光烧结等3D打印技术制备陶瓷工艺过程繁琐的难题。
具体实施方式
为更好的理解本发明，下面的实施例是对本发明的进一步说明，但本发明的内容不仅仅局限于下面的实施例。
实施例1：
1)将氧化铝陶瓷粉体烘干后经研磨粉碎并过筛；
2)将高密聚乙烯、低密聚乙烯、石蜡、无定型聚烯烃加入高温混炼机中在180℃下混炼配置成预混液，预混液中，高密聚乙烯和低密聚乙烯的总体积占60％，二者体积比为5:5石蜡和无定型聚烯烃的总体积占40％，二者体积比为5:5；
3)向上述预混液中加入步骤1)得到的陶瓷粉体及占陶瓷粉体2wt％的分散剂硬脂酸，并继续在180℃混炼1h得到混料；
4)将步骤3)得到的混料挤出、冷却、造粒以制得陶瓷喂料；
5)将步骤4)得到的陶瓷喂料放入单螺杆挤出机中进行挤出、拉丝并冷却以制得3D打印用0.5mm陶瓷线材；
6)陶瓷3D打印：以步骤5)得到的陶瓷线材为原材料，利用FDM陶瓷3D打印机加工成型各种复杂形状的陶瓷器件。
7)脱脂烧结：将步骤6)中制得陶瓷生坯，经环己烷和乙醇溶剂脱脂，再采用热脱脂制得氧化铝陶瓷异形件。
实施例2：
1)将氮化硅陶瓷粉体烘干后经研磨粉碎并过筛；
2)将高密聚乙烯、低密聚乙烯、石蜡、无定型聚烯烃加入高温混炼机中在170℃下混炼配置成预混液，预混液中，高密聚乙烯和低密聚乙烯的总体积占70％，二者体积比为7:3石蜡和无定型聚烯烃的总体积占30％，二者体积比为6:4；
3)向上述预混液中加入步骤1)得到的陶瓷粉体及分散剂2.5wt％油酸，并继续在170℃混炼1h得到混料；
4)将步骤3)得到的高温混料挤出、冷却、造粒以制得陶瓷喂料；
5)拉丝：将步骤4)得到的陶瓷喂料放入单螺杆挤出机中进行挤出、拉丝并冷却以制得3D打印用1.5mm陶瓷线材；
6)陶瓷3D打印：以步骤5)得到的陶瓷线材为原材料，利用FDM陶瓷3D打印机加工成型各种复杂形状的陶瓷器件。
7)脱脂烧结：将步骤6)中制得陶瓷生坯，经环己烷和乙醇溶剂脱脂，再采用氮气下热脱脂烧结制得氮化硅陶瓷异形件。
实施例3：
1)将氧化锆陶瓷粉体烘干后经研磨粉碎并过筛；
2)将高密聚乙烯、低密聚乙烯、石蜡、无定型聚烯烃加入高温混炼机中在160℃下混炼配置成预混液，预混液中，高密聚乙烯和低密聚乙烯的总体积占50％，二者体积比为6:4石蜡和无定型聚烯烃的总体积占50％，二者体积比为4:6；
3)向上述预混液中加入步骤1)得到的陶瓷粉体及分散剂5wt％油酸和硬脂酸按照质量比1:1混合的分散剂，并继续在160℃混炼1.5h得到混料；
4)将步骤3)得到的高温混料挤出、冷却、造粒以制得陶瓷喂料；
5)拉丝：将步骤4)得到的陶瓷喂料放入单螺杆挤出机中进行挤出、拉丝并冷却以制得3D打印用2.5mm陶瓷线材；
6)陶瓷3D打印：以步骤5)得到的陶瓷线材为原材料，利用FDM陶瓷3D打印机加工成型各种复杂形状的陶瓷器件。
7)脱脂烧结：将步骤6)中制得陶瓷生坯，经环己烷和乙醇溶剂脱脂，再采用热脱脂制得氧化锆陶瓷异形件。
经测试，本发明利用的陶瓷3D打印方法适用于各种陶瓷材料的加工成型，且加工工艺简单，无需复杂的后处理工艺，实施例1所制备氧化铝陶瓷抗折强度达250MPa，实施例3所制备的氧化锆陶瓷抗折强度达500MPa，实施例2所制备的氮化硅陶瓷抗折强度达500MPa，较传统陶瓷成型方法制备陶瓷器件性能相当。
以上所述是本发明的优选实施方式而已，当然不能以此来限定本发明之权利范围，应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和变动，这些改进和变动也视为本发明的保护范围。
Claims (10)
1.一种基于陶瓷材料的3D打印成型方法，其特征在于，包括如下步骤：
1)将各种原料按比例混炼配置成预混液；
2)向步骤1)得到的预混液中加陶瓷粉体及分散剂，并继续混炼得到混料；
3)将步骤2)得到的混料挤出、冷却、造粒以制得陶瓷喂料；
4)将步骤3)得到的陶瓷喂料进行挤出、拉丝并冷却以制得3D打印用陶瓷线材；
5)以步骤4)得到的陶瓷线材为原材料，利用3D打印加工成型，制得陶瓷生坯；
6)将步骤5)制得的陶瓷生坯经脱脂烧结制得最终的陶瓷器件。
2.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤1)中，粘接剂的主要成分为50vol％-70vol％的高密聚乙烯和低密聚乙烯的混合物，辅料为30vol％-50vol％的石蜡和无定型聚烯烃混合物。
3.根据权利要求2所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述高密聚乙烯和低密聚乙烯的体积比为7:3-5:5；所述石蜡和无定型聚烯烃的体积比为6:4-4:6。
4.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤1)和步骤2)中，混炼温度均为160-180℃。
5.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤2)中，陶瓷粉体可为氧化铝、氧化锆、氮化硅、碳化硅、碳化硼、莫来石、红柱石、氧化硅中的至少一种。
6.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤2)中，分散剂为硬脂酸和/或油酸，所述分散剂的添加量为陶瓷粉体的2wt％-5wt％。
7.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤4)中，拉丝直径在0.5-2.5mm。
8.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤5)中，采用FDM陶瓷3D打印机加工成型。
9.根据权利要求1所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述步骤6)中，脱脂工艺采用两步脱脂，先采用溶剂脱脂，再采用热脱脂。
10.根据权利要求9所述的基于陶瓷材料的3D打印成型方法，其特征在于：所述溶剂为环己烷和乙醇的混合物。
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