CN110342930A - 一种用于dlp快速成型的3d打印氧化锆陶瓷的光固化树脂 - Google Patents

一种用于dlp快速成型的3d打印氧化锆陶瓷的光固化树脂 Download PDF

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CN110342930A
CN110342930A CN201910634335.1A CN201910634335A CN110342930A CN 110342930 A CN110342930 A CN 110342930A CN 201910634335 A CN201910634335 A CN 201910634335A CN 110342930 A CN110342930 A CN 110342930A
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cured resin
zirconia ceramics
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覃春林
覃芫
林玲
田序元
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Weihai Jihe Materials Engineering Research Institute
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Abstract

本发明提出一种用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，按重量百分比计，所述光固化树脂包括15‑20%的第一预聚物，15‑20%的第二预聚物，5‑15%的韧化剂，0.5‑4%的光引发剂，50‑64.5%的氧化锆粉体。上述光固化树脂采用具有较高官能度的第一预聚物和第二预聚物使得该光固化树脂具有较高反应活性，因而能提高上述光固化树脂固化后形成的薄层的交联密度，从而提升可见光波段的固化性；将各组分的用量限定在上述范围内有利于同时提高该树脂经光固化后形成的薄层的耐沾污性与耐磨性；本发明所涉及的树脂可用普通白色光源光固化，实现氧化锆陶瓷的3D打印效果。

Description

一种用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂
技术领域
本发明涉及3D打印技术领域，尤其涉及一种用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，具体而言，涉及一种利用可见光波段进行光固化的树脂，其可用于氧化锆陶瓷的快速成型。
背景技术
先进陶瓷的设计和开发最早从汽车领域开始，并逐渐向高性能领域发展。现阶段先进陶瓷在航空航天、国土防御、能源及生物医学领域都得到了发展与应用。陶瓷制品需经过原料粉体处理、坯体制备成型、固体制品烧结和最终加工处理四个主要环节。其中，陶瓷制品的成型是一个耗时且较为昂贵的过程。节约制备材料、缩短加工周期、降低制造成本及实现制品量产化是先进陶瓷所面临的问题。为解决先进陶瓷面临的问题，无模陶瓷成型制造技术应运而生。其中DLP光固化快速成型技术可用于陶瓷的立体成型，具有高效率、无模化和可复杂化等优势，相对于其他3D打印成型技术，基于DLP(数字光处理)光固化快速成型技术合成的陶瓷件在烧结后具有最接近传统烧结陶瓷的强度，在牙科和骨愈合应用的医学、微机电系统(MEMS)、传感器、压电元件和光子晶体的制备上，具有很高的实用性和性价比。
由于氧化锆陶瓷具有强度高、熔点高、化学性质稳定、抗腐蚀性优良以及导热系数低等特点，被广泛应用于成形工具、整形模、拉丝模、切削刀具、高温挤出模具、剪刀、高尔夫球棍头、发动机推杆、连杆、轴承、汽缸内衬、活塞帽、耐火材料、浇铸口、熔炼铂和锗的坩埚以及齿科牙冠、基台、种植体、骨科关节球头和椎间融合器等，具有很大的市场空间。
利用光固化3D打印的方法来成型氧化锆陶瓷的报道已经有不少，如专利申请号为201710051795.2的发明专利申请公开了一种基于光固化成型的3D打印制备氧化锆陶瓷的方法，专利申请号为201710036077.8的发明专利申请公开了一种氧化锆增强3D打印陶瓷浆料及其制备方法，专利申请号为201810615646.9的发明专利申请公开了一种3D打印义齿陶瓷材料及制备方法。但是这些现有技术中使用UV光来实现氧化锆陶瓷的3D打印，由于使用UV光机或紫外激光器做为光源，成本较高，导致了目前陶瓷3D打印机价格昂贵不利于推广，因此，开发出使用可见光波段固化的树脂，提高光敏反应的速度成为解决这个问题的关键。
发明内容
为了解决现有技术中存在的问题，本发明提出了一种用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，以便克服现有技术中3D打印需采用UV固化陶瓷浆料的不足，实现普通DLP白光源或手机液晶屏即可做光源的3D打印。
为了实现上述目的，本发明提出了一种用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，按重量百分比计，所述光固化树脂包括15-20％的第一预聚物，15-20％的第二预聚物，5-15％的韧化剂，0.5-4％的光引发剂，50-64.5％的氧化锆粉体。
优选的是，所述第一预聚物为官能度9-10的脂肪族聚氨酯丙烯酸预聚物。
优选的是，所述第二预聚物为乙氧化三羟甲基丙烷三丙烯酸酯。
优选的是，所述韧化剂为丙烯酰吗啉。
优选的是，所述光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，其中二者的质量百分比为：(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐：2-重氮-1-萘酚-5-磺酰氯＝3:1-1:4。
优选的是，所述氧化锆粉体采用晶粒度为50-2000nm的氧化锆陶瓷粉。
本发明的该方案的有益效果在于上述用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂采用的光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，使树脂固化波长在200-480nm，避免了使用365nm或405nm的UV光来进行光固化的问题，使普通DLP投影机或手机光源作为3D打印机光源成为可能。所述光固化树脂使用具有较高官能度的第一预聚物和第二预聚物使得该光固化树脂具有较高反应活性，因而能够提高上述光固化树脂固化后形成的薄层的交联密度，从而提升可见光波段的固化性；所述丙烯酰吗啉与脂肪族聚氨酯丙烯酸预聚物具有较高的反应活性和粘合力，因而该组分的加入有利于增强固化后树脂的柔韧性、耐磨性和使用寿命；此外，将各组分的用量限定在上述范围内有利于同时提高该树脂经光固化后形成的薄层的耐沾污性与耐磨性。综合以上因素使得本发明所涉及的树脂不同于其他已报道的树脂，本发明所涉及的树脂可用普通白光光源光固化，实现氧化锆陶瓷的3D打印效果。
具体实施方式
下面结合实施例对本发明的具体实施方式作进一步的说明。
本发明的主要目的是解决目前光固化氧化锆陶瓷的3D打印中，使用365nm或405nm的UV光来进行光固化的问题，上述光固化方式导致了目前陶瓷3D打印机价格昂贵不利于推广。本发明所涉及的光固化树脂使用可见光波段进行固化，固化波长在200-480nm，提高光敏反应的速度，使普通DLP投影机或手机光源作为3D打印机光源成为可能。
实施例1
本发明所涉及的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，按重量百分比计，包括15％的第一预聚物，15％的第二预聚物，6％的韧化剂，4％的光引发剂，60％的氧化锆粉体。
其中所述第一预聚物为官能度9-10的脂肪族聚氨酯丙烯酸预聚物；所述第二预聚物为乙氧化三羟甲基丙烷三丙烯酸酯；所述韧化剂为丙烯酰吗啉；所述光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，其中二者的质量百分比为：(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐：2-重氮-1-萘酚-5-磺酰氯＝3:7；所述氧化锆粉体采用晶粒度为600nm的氧化锆陶瓷粉。
该光固化树脂可使用普通DLP投影作为光源的3D打印机固化成型，6s可实现100um的固化层厚，所得浆料均匀性好，放置120小时不发生沉降分层，打印所得产品为树脂/氧化锆陶瓷复合材料构件，打印表面粗糙度0.23um，密度2.2g/cm3，该光固化树脂3D打印的胚体具有固含量高，成型速度快，精度高的优点。
实施例2
本发明所涉及的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，按重量百分比计，包括18％的第一预聚物，18％的第二预聚物，10％的韧化剂，4％的光引发剂，50％的氧化锆粉体。
其中所述第一预聚物为官能度9-10的脂肪族聚氨酯丙烯酸预聚物；所述第二预聚物为乙氧化三羟甲基丙烷三丙烯酸酯；所述韧化剂为丙烯酰吗啉；所述光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，其中二者的质量百分比为：(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐：2-重氮-1-萘酚-5-磺酰氯＝1:1；所述氧化锆粉体采用晶粒度为1000nm的氧化锆陶瓷粉。
该光固化树脂可使用普通DLP投影作为光源的3D打印机固化成型，10s可实现120um的固化层厚，所得浆料均匀性好，放置100小时不发生沉降分层，打印所得产品为树脂/氧化锆陶瓷复合材料构件，打印表面粗糙度0.40um，密度2.0g/cm3，该光固化树脂3D打印的胚体具有成型速度快，精度高的优点。
实施例3
本发明所涉及的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，按重量百分比计，包括18％的第一预聚物，18％的第二预聚物，7％的韧化剂，2％的光引发剂，55％的氧化锆粉体。
其中所述第一预聚物为官能度9-10的脂肪族聚氨酯丙烯酸预聚物；所述第二预聚物为乙氧化三羟甲基丙烷三丙烯酸酯；所述韧化剂为丙烯酰吗啉；所述光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，其中二者的质量百分比为：(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐：2-重氮-1-萘酚-5-磺酰氯＝1:2；所述氧化锆粉体采用晶粒度为200nm的氧化锆陶瓷粉。
该光固化树脂可使用普通DLP投影作为光源的3D打印机固化成型，6s可实现50um的固化层厚，所得浆料均匀性好，放置120小时不发生沉降分层，打印所得产品为树脂/氧化锆陶瓷复合材料构件，打印表面粗糙度0.30um，密度2.1g/cm3，该光固化树脂3D打印的胚体具有固含量高，成型速度快，精度高的优点。
实施例4
本发明所涉及的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，按重量百分比计，包括15％的第一预聚物，15％的第二预聚物，5％的韧化剂，0.5％的光引发剂，64.5％的氧化锆粉体。
其中所述第一预聚物为官能度9-10的脂肪族聚氨酯丙烯酸预聚物；所述第二预聚物为乙氧化三羟甲基丙烷三丙烯酸酯；所述韧化剂为丙烯酰吗啉；所述光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，其中二者的质量百分比为：(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐：2-重氮-1-萘酚-5-磺酰氯＝1:4；所述氧化锆粉体采用晶粒度为800nm的氧化锆陶瓷粉。
该光固化树脂可使用普通DLP投影作为光源的3D打印机固化成型，10s可实现60um的固化层厚，所得浆料均匀性好，放置120小时不发生沉降分层，打印所得产品为树脂/氧化锆陶瓷复合材料构件，打印表面粗糙度0.25um，密度2.3g/cm3，该光固化树脂3D打印的胚体具有固含量高，精度高的优点。

Claims (6)

1.一种用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，其特征在于：按重量百分比计，所述光固化树脂包括15-20％的第一预聚物，15-20％的第二预聚物，5-15％的韧化剂，0.5-4％的光引发剂，50-64.5％的氧化锆粉体。
2.根据权利要求1所述的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，其特征在于：所述第一预聚物为官能度9-10的脂肪族聚氨酯丙烯酸预聚物。
3.根据权利要求1所述的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，其特征在于：所述第二预聚物为乙氧化三羟甲基丙烷三丙烯酸酯。
4.根据权利要求1所述的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，其特征在于：所述韧化剂为丙烯酰吗啉。
5.根据权利要求1所述的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，其特征在于：所述光引发剂为(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐和2-重氮-1-萘酚-5-磺酰氯的混合物，其中二者的质量百分比为：(4-羟基苯基)甲基苄基硫鎓六氟锑酸盐：2-重氮-1-萘酚-5-磺酰氯＝3:1-1:4。
6.根据权利要求1所述的用于DLP快速成型的3D打印氧化锆陶瓷的光固化树脂，其特征在于：所述氧化锆粉体采用晶粒度为50-2000nm的氧化锆陶瓷粉。
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