CN107382327B - 陶瓷3d打印浆料的制备及应用 - Google Patents

陶瓷3d打印浆料的制备及应用 Download PDF

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CN107382327B
CN107382327B CN201710849400.3A CN201710849400A CN107382327B CN 107382327 B CN107382327 B CN 107382327B CN 201710849400 A CN201710849400 A CN 201710849400A CN 107382327 B CN107382327 B CN 107382327B
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周宏志
邢占文
戴宪光
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SUZHOU JIANGNAN JIAJIE ELECTROMECHANICAL TECHNOLOGY RESEARCH INSTITUTE Co Ltd
Suzhou Zhong Rui Zhi Chuang 3d Polytron Technologies Inc
Suzhou Academy of Xian Jiaotong University
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SUZHOU JIANGNAN JIAJIE ELECTROMECHANICAL TECHNOLOGY RESEARCH INSTITUTE Co Ltd
Suzhou Zhong Rui Zhi Chuang 3d Polytron Technologies Inc
Suzhou Academy of Xian Jiaotong University
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Abstract

本发明涉及增材制造技术领域，本发明公开了一种陶瓷3D打印浆料的制备及应用，首先，将质量百分比为单体的1.5～3%光引发剂加入到丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；其次，将质量百分比为陶瓷粉末的0.3～2%分散剂加入到预混液1后，将质量百分比含量70～85%的陶瓷粉末加入，球磨1～3小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；最后，将质量百分比0.5～2%的触变剂加入预混液2,磁力搅拌0.5～2小时,静置2～4小时，得到陶瓷浆料。本发明能够实现陶瓷浆料的输送、刮平，并最终实现致密度高的陶瓷制品制备。

Description

陶瓷3D打印浆料的制备及应用
技术领域
本发明涉及增材制造技术领域，具体涉及一种陶瓷3D打印浆料的制备及应用。
背景技术
陶瓷材料具有强度高、耐磨、耐腐蚀等优异性能，在航空航天、石油化工、生物医用等领域应用广泛。传统的成形工艺是开模后将陶瓷浆料干燥成为坯体，再进行高温烧结得到陶瓷制品。这种成形方法受开模限制，制约陶瓷制品复杂化的发展。
近年来发展的各种3D打印成形技术使陶瓷成形实现了无模化生产。其中，1990年代中期法国利摩日大学开发了针对陶瓷坯体的光固化3D打印成形工艺，将单体、光引发剂、分散剂、陶瓷粉末配置成粘度较低、固含量较高的浆料，基于光固化成形设备利用紫外光引发单体发生聚合反应，固化形成陶瓷坯体，再经过后续脱脂和烧结获得最终的陶瓷制品。该成形工艺能够获得致密度高、结构复杂的陶瓷制品，成为陶瓷3D打印成形的代表性工作。
国内对于陶瓷工件光固化3D打印所用陶瓷浆料方面，西安交通大学的李涤尘等人开发了亚甲基双丙烯酸胺、分散剂、光引发剂制备的水基光固化陶瓷浆料，并借助振镜驱动的激光束完成每个陶瓷样品切面的快速成形。结合其设备的成形能力，该类浆料粘度较小，固含量较低。而较低的固含量将对最终陶瓷工件的致密度和强度带来影响，因此该类浆料不能满足高质量陶瓷坯体的制造需求。
当提高陶瓷浆料固含量之后，其粘度较大，在3D打印过程中容易造成局部缺损或模型发生损坏。因此，如何获得固含量相对较高、流动性较好的陶瓷浆料，成为提高光固化3D打印陶瓷制品质量、拓展其应用领域的关键。
发明内容
为解决上述技术问题，我们提出了一种陶瓷3D打印浆料的制备及应用，通过在浆料中添加一定量的触变剂，将高固含量陶瓷浆料的粘度调节至合适范围，以利于进行光固化成形，同时保证最终烧结致密度和强度要求。
为达到上述目的，本发明的技术方案如下：
陶瓷3D打印浆料的制备，其包括如下步骤：
首先，将质量百分比为单体的1.5～3%光引发剂加入到丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；其次，将质量百分比为陶瓷粉末的0.3～2%分散剂加入到预混液1后，将质量百分比含量70～85%的陶瓷粉末分成多等份逐次加入，每次球磨1～3小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；最后，将质量百分比0.5～2%的触变剂加入预混液2,磁力搅拌0.5～2小时,静置2～4小时，得到陶瓷浆料。
优选的，所述陶瓷粉末是Al2O3、ZrO2、HAP、TCP中一种。
优选的，所述光引发剂是光引发剂184和光引发剂651中任一个。
优选的，所述分散剂是分散剂655和分散剂670中任一个。
优选的，所述触变剂是触变剂BYK410。
为了实现上述目的，本发明还提出了一种陶瓷3D打印浆料的制备应用，其具体包括如下：
1)将CAD三维陶瓷部件模型导入陶瓷3D打印机进行分层处理，并将上述陶瓷浆料置于料槽中，采用光固化成形方法制备陶瓷坯体；
2)将上述制备陶瓷坯体脱脂、烧结：其中脱脂要求温度为450～600度，保温1.5～3小时；其中烧结要求温度为1250～1650度，保温1.5～3小时，制得陶瓷制品。
通过上述技术方案，本发明以弥补现有陶瓷3D打印浆料的不足为目的，通过添加合适比例的触变剂，使高固含量的浆料具备恰当触变性，使之在光固化成形过程中能够实现陶瓷浆料的输送、刮平，并最终实现致密度高的陶瓷制品制备。
附图说明
为了更清楚地说明本发明实施例的技术方案，下面将对实施例描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明实施例所公开的一种陶瓷3D打印浆料的制备及应用的流程图。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
下面结合示意图对本发明的具体实施方式作进一步详细的说明。
参照图1，陶瓷3D打印浆料的制备及应用的流程图
1）制备陶瓷浆料：首先，将质量百分比为单体的1.5～3%光引发剂加入到丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；其次，将质量百分比为陶瓷粉末的0.3～2%分散剂加入到预混液1后，将质量百分比含量70～85%的陶瓷粉末分成多等份逐次加入，每次球磨1～3小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；最后，将质量百分比0.5～2%的触变剂加入预混液2,磁力搅拌0.5～2小时,静置2～4小时，得到陶瓷浆料；
2)将CAD三维陶瓷部件模型导入陶瓷3D打印机进行分层处理，并将上述陶瓷浆料置于料槽中，采用光固化成形方法制备陶瓷坯体；
3)将上述制备陶瓷坯体脱脂、烧结：其中脱脂要求温度为450～600度，保温1.5～3小时；其中烧结要求温度为1250～1650度，保温1.5～3小时，制得陶瓷制品。
实施例1
陶瓷3D打印浆料的制备及应用按以下步骤进行：
（1）制备陶瓷浆料
将1g光引发剂184加入到50g丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；
其次，将2.4g分散剂655加入到预混液1后，将260g Al2O3陶瓷粉末分成多等份，逐次加入，每次球磨1小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；
最后，将3.1g触变剂BYK410加入预混液2,磁力搅拌1小时,静置2小时得到陶瓷浆料。
（2）将CAD三维陶瓷部件模型导入陶瓷3D打印机进行分层处理，并将上述陶瓷浆料置于料槽中，采用光固化成形方法制备陶瓷坯体；
（3）脱脂：温度为550度，保温1.5小时；
（4）烧结：温度为1650度，保温1.5小时，制得陶瓷制品。
实施例2
陶瓷3D打印浆料的制备及应用按以下步骤进行：
（1）制备陶瓷浆料
将0.75g光引发剂651加入到50g丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；
其次，将2g分散剂670加入到预混液1后，将200g ZrO2陶瓷粉末分成多等份，逐次加入，每次球磨2小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；
最后，将1.25g触变剂BYK410加入预混液2,磁力搅拌1.5小时,静置2小时，得到陶瓷浆料。
（2）将CAD三维陶瓷部件模型导入陶瓷3D打印机进行分层处理，并将上述陶瓷浆料置于料槽中，采用光固化成形方法制备陶瓷坯体；
（3）脱脂：温度为550度，保温2小时；
（4）烧结：温度为1450度，保温2小时，制得陶瓷制品。
实施例3
陶瓷3D打印浆料的制备及应用按以下步骤进行：
（1）制备陶瓷浆料
将1.4g光引发剂651加入到70g丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；
其次，将6.3g分散剂670加入到预混液1后，将210g HAP或TCP陶瓷粉末分成多等份，逐次加入，每次球磨2小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；
最后，将4.9g触变剂BYK410加入预混液2,磁力搅拌2小时,静置2小时，得到陶瓷浆料。
（2）将CAD三维陶瓷部件模型导入陶瓷3D打印机进行分层处理，并将上述陶瓷浆料置于料槽中，采用光固化成形方法制备陶瓷坯体；
（3）脱脂：温度为600度，保温3小时；
（4）烧结：温度为1450度，保温3小时，制得陶瓷制品。
以上所述的仅是本发明的优选实施方式，应当指出，对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。

Claims (7)

1.陶瓷3D打印浆料的制备，其特征在于，其包括如下步骤：首先，将质量百分比为单体的1.5～3%光引发剂加入到丙烯酸酯单体中，磁力搅拌分散使其完全溶解得到预混液1；其次，将质量百分比为陶瓷粉末的0.3～2%分散剂加入到预混液1后， 将质量百分比含量70～85%的陶瓷粉末分成多等份，逐次加入，每次球磨1～3小时，全部粉末加入后球磨6小时，使各组分混合均匀，获得预混液2；最后，将质量百分比0.5～2%的触变剂加入预混液2,磁力搅拌0.5～2小时,静置2～4小时，得到陶瓷浆料。
2.根据权利要求1所述的陶瓷3D打印浆料的制备，其特征在于，所述陶瓷粉末为Al2O3、ZrO2、HAP、TCP中一种。
3.根据权利要求1所述的陶瓷3D打印浆料的制备，其特征在于，所述光引发剂是光引发剂184、光引发剂651中一种。
4.根据权利要求1所述的陶瓷3D打印浆料的制备，其特征在于，所述分散剂是分散剂655、分散剂670中一种。
5.根据权利要求1所述的陶瓷3D打印浆料的制备，其特征在于，所述触变剂是触变剂BYK410。
6.根据权利要求1-5所述的陶瓷3D打印浆料的应用，其应用于3D打印机上制备陶瓷制品，其特征在于，其包括如下步骤：
将CAD三维陶瓷部件模型导入3D打印机进行分层处理，并将上述陶瓷浆料置于料槽中，采用光固化成形方法制备陶瓷坯体；
将上述制备陶瓷胚体脱脂、烧结：其中脱脂要求温度为450～600度，保温1.5～3小时；其中烧结要求温度为1250～1650度，保温1.5～3小时，制得陶瓷制品。
7.根据权利要求6所述的陶瓷3D打印浆料的应用，其特征在于，所述3D打印机是陶瓷3D打印机。
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