CN112795044B - 一种复合透明膜，其制备方法及基于其的连续光固化3d打印陶瓷方法 - Google Patents

一种复合透明膜，其制备方法及基于其的连续光固化3d打印陶瓷方法 Download PDF

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CN112795044B
CN112795044B CN202110011236.5A CN202110011236A CN112795044B CN 112795044 B CN112795044 B CN 112795044B CN 202110011236 A CN202110011236 A CN 202110011236A CN 112795044 B CN112795044 B CN 112795044B
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printing
ceramic
transparent film
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composite
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张广明
蒋进
兰红波
王飞
宋道森
黄辉
李汶海
于尊
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Qingdao University of Technology
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Abstract

本发明公开了一种复合透明膜，其制备方法及基于其的连续光固化3D打印陶瓷方法，选用二氧化硅微球和PDMS混合制膜，在此膜上利用二氧化硅制作形成疏水层，结合特定优化的参数，使其更适合连续光固化3D打印陶瓷，实现了陶瓷浆料的连续打印，解决了现有陶瓷3D打印方法得到的打印件分层问题，提高了打印精度，降低了打印成本。

Description

一种复合透明膜，其制备方法及基于其的连续光固化3D打印 陶瓷方法
技术领域
本发明涉及3D打印领域，尤其涉及一种复合透明膜，其制备方法及基于其的连续光固化3D打印陶瓷方法。
背景技术
陶瓷材料具有高强度、高硬度、耐高温、耐氧化、耐腐蚀、化学性能稳定和轻质等突出优点，在航空航天、生物医疗、汽车、电、能源、国防等诸多领域有着广泛的应用。然而传统的陶瓷成型技术面临加工困难(尤其是复杂形状结构成型更为困难)、制造周期长、生产成本高等不足和局限性，制约着陶瓷零件更为广泛的应用。相比于传统的陶瓷成型工艺，陶瓷3D打印技术具有以下显著的优势：(1)无需原坯和模具，生产周期短，制造成本低；(2)制造精度高；(3)可实现几乎任意形状复杂结构成型，突破了传统工艺制造几何形状的约束；(4)适合个性化定制和单件小批量生产；(5)成型材料种类广泛，如氧化锆、氧化铝、磷酸三钙、碳化硅、碳硅化钛、陶瓷前驱体、陶瓷基复合材料等。此外，在微小零件3D打印、陶瓷/金属复合材料和功能梯度材料方面，以及材料-结构-功能一体化打印方面还具有独特的优势。
陶瓷3D打印技术根据使用陶瓷材料的不同和使用用途的不同，目前已有十几种陶瓷3D成型工艺。陶瓷3D打印技术主要分为：立体光固化成型；选择性激光烧结；喷墨打印成型；三维打印成型(3DP)；直写自由成型；熔融沉积成型；叠层实体制造。其中，光固化成型技术主要有逐点扫描式光固化和面曝光固化，但是都面临打印分层的问题，这不仅影响成型件的表面质量，而且也导致成型件存在各向异性等问题。再者光固化3D打印技术的打印材料主要为液态材料，都存在液态材料对于固化区域填充的问题。尤其是面曝光光固化技术，对于粘度过高的打印材料，必须加入刮板装置，这增加了零件的成型时间和打印装置的复杂程度，因此大大延长整体的打印时间。因此，现有的各种光固化陶瓷3D打印技术仍然面临以下挑战性难题：打印效率低；逐层打印致使成型零件存在各项异性，导致后续烧结过程中易于出现裂纹、变形等缺陷，严重影响打印件的质量和精度。迫切需要开发新的工艺和技术。
申请号为201910090004.6的专利中公开了一种连续面曝光陶瓷3D打印装置及其工作方法，其使用了一种复合富氧膜在陶瓷浆料中形成死区，但是这种复合富氧膜所使用的PET多孔膜中的微米孔会严重影响透光率，因此导致光源穿透性下降，影响打印质量。
因此，亟需一种复合透明膜来改善上述问题，实现陶瓷的连续3D打印。
发明内容
为了解决上述问题，本发明提供了一种复合透明膜，其制备方法及基于其的连续光固化3D打印陶瓷方法，①增强复合透明膜的强度，适应更大质量的浆料的打印；②延长复合膜的使用寿命，从而可以针对多种类型陶瓷粉进行大尺寸、任意形状成形件低成本、高效连续打印。
为实现上述发明目的，本发明采用下述技术方案予以实现：
在本申请的一些实施例中，一种连续光固化3D打印陶瓷用复合透明膜的制备方法，
操作步骤如下：
⑤取粒径为200nm左右的球状SiO2颗粒与道康宁PDMS预混液，SiO2质量占比为10％-40％，以200r/min-300r/min搅拌2-5min；
②将上述混合溶液放入超声波清洗机中混合15-20min；
③静置冷却后加入PDMS固化剂，固化剂与PDMS预混液质量比为1/10-1/8，以200r/min-300r/min搅拌3-5min；
③在0-8℃温度中静置12-24h，直至完全没有气泡；
④利用数控雕刻机，以80-100℃的底板加热、30-50Kpa的气压、320-400mm/s将混合溶液打印成膜；
⑤将打印所得膜置于干燥箱中干燥；
⑥将完全固化的SiO2/PDMS混合膜浸入装满SiO2悬浮液的容器中，其中悬浮液中SiO2粒径为2-5μm，利用提拉机器以1-8mm/s匀速竖直向上提拉；
⑧将上述复合膜置于200-250℃中加热60-80h；
⑨用旋涂机将光刻胶SU-8基环氧树脂旋涂在复合膜表面SiO2缝隙中，转速2500-3500r/min、旋涂时间30-60s，再用有机溶剂清洗表面残留的光刻胶；
⑩用紫外固化灯对表面的光刻胶进行固化，时间1-3min；
Figure BDA0002884282780000031
将上述复合膜置于氢氟酸溶液中蚀刻5-15min去除表面SiO2，用酒精彻底清洗，干燥箱干燥。
在本申请的一些实施例中，所述步骤
Figure BDA0002884282780000032
中氢氟酸溶液的浓度2-5vol％
在本申请的一些实施例中，所述步骤⑥中干燥的温度为80-100℃，干燥时间为2-3h；所述步骤
Figure BDA0002884282780000033
中干燥箱干燥温度60-80℃，干燥时间2-5h。
在本申请的一些实施例中，最终所得的复合透明膜厚度50-100μm，并且氧气透过效率在50barrer以上，紫外光透过率不低于80％，强度不低于20kPa。
在本申请的一些实施例中，所述数控雕刻机为晶研CNC3040数控雕刻机；所述超声波清洗机为歌能DL-3150超声波清洗机。
在本申请的一些实施例中，基于该复合透明膜的连续光固化3D打印陶瓷装置，包括工作台和底座，工作台自上而下包括打印平台、储料盒、复合透明膜、供氧冷却模块、数字光模块。
在本申请的一些实施例中，一种基于该复合透明膜的连续光固化3D打印陶瓷方法，包括以下步骤：
⑦在储料槽中倒入配制好的陶瓷浆料；
⑥控制打印平台的底部停在复合透明膜的上方20-30μm，浆料没过平台底部；
⑦通入冷却氧气；
⑧打开光源，使得事先处理好的图像投影在复合透明膜上；
⑤10-15s后控制打印平台以不超过400mm/h匀速向上移动，同时，投影图像作相应变换；
⑥打印结束后依次关闭光源、暂停打印平台、停止冷却氧气的流通；
⑦取下打印陶瓷素胚件，清洗掉微固化的浆料残余；
⑧使用紫外固化灯对打印件进行二次固化，最终得到所需陶瓷打印素胚件；
⑨按照相应的烧结工序烧结后即可得到所需陶瓷件。
在本申请的一些实施例中，陶瓷种类选用氧化锆、氧化铝、氮化硅、氧化镁、氧化钇中的一种或多种组合，粒径平均尺寸为0.5-5μm，粉末形状为多边形或球形。
在本申请的一些实施例中，将选择好的陶瓷原料与光敏树脂混合，以200-300r/min手动搅拌2-5min后，倒入球磨机中，以300-450r/min转速混合6-8h，球磨结束将混料置于干燥箱中常温干燥60-90min后得到所需陶瓷浆料。
与现有技术相比，本公开的有益效果是：
①发明人综合对所需复合膜的强度、透光性、透氧性、使用寿命等性能的考量，创造性地选用二氧化硅微球和PDMS混合制膜，在此膜上利用二氧化硅制作形成疏水层，结合特定的优化的参数，使其更适合连续光固化3D打印陶瓷。
②实现了陶瓷浆料的连续打印，解决了现有陶瓷3D打印方法得到的打印件分层问题，提高了打印精度。
③将SiO2混入PDMS中，首先可以改善原先PDMS膜的富氧性能，并且不会降低原先PDMS膜的透光性，其次可以改善原先PDMS膜的力学性能，可以配合较大的打印窗口进行大体积产品的打印；
④研究发现复合膜的富氧性能随着SiO2添加量的增加而增加，这样便可以对打印时产生的“死区”厚度进行一定范围的调控，最终可以在匹配打印浆料的粘稠性上产生一定效果。
⑤打印时，上部为复合透明膜，下部为供氧冷却气体，形成气-固接触面；供氧冷却模块可以降低打印光束照射区域温度，使得复合膜老化速度降低，降低了成本、提高了效率，并且可以为打印提供充足的氧气。
⑥复合膜上的疏水层使得浆料在复合膜上的流动性加强，即打印过程中的浆料填充速度加快。
⑦组装成本低。所有装置采用都是低成本耗材，大大降低了打印装置的装机成本。
附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例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是本申请的打印装置立体图；
图2是本申请的打印装置主视图；
图3是本申请的复合透明膜及供氧冷却模块示意图；
图4是本申请的复合透明膜的结构示意图；
图5是本申请实施例2制备所得陶瓷素胚件与烧结件。
其中，1、工作台；2、打印平台；3、储料盒；4、复合透明膜及供氧冷却模块；5、底座；6、光源；401、PDMS/SiO2复合膜；402、复合气体腔；403、进气口；404、出气口；405、刻蚀掉SiO2的PDMS膜；406、PDMS/SiO2膜。
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做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。在本发明的描述中，需要理解的是，术语“中心”、“上”、“下”、“前”、“后”、“左”、“右”、“竖直”、“水平”、“顶”、“底”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。
在本发明的描述中，需要说明的是，除非另有明确的规定和限定，术语“安装”、“相连”、“连接”应做广义理解，例如，可以是固定连接，也可以是可拆卸连接，或一体地连接。对于本领域的普通技术人员而言，可以具体情况理解上述术语在本发明中的具体含义。在上述实施方式的描述中，具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。术语“第一”、“第二”仅用于描述目的，而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此，限定有“第一”、“第二”的特征可以明示或者隐含地包括一个或者更多个该特征。在本发明的描述中，除非另有说明，“多个”的含义是两个或两个以上。
实施例1
①取粒径为200nm的球状SiO2颗粒与道康宁PDMS预混液，SiO2质量占比为20％，以200r/min手动搅拌2min；
②将上述混合溶液放入歌能DL-3150超声波清洗机中混合15min；
③静置冷却后加入PDMS固化剂，固化剂与PDMS预混液质量比为1/10，以200r/min手动搅拌3min；
④在4℃温度中静置24h，直至完全没有气泡；
⑤利用晶研CNC3040数控雕刻机，以90℃的底板加热、35Kpa的气压、320km/h将混合溶液打印成膜；
⑥将打印所得膜置于干燥箱中以90℃加热2h；
⑦将完全固化的SiO2/PDMS混合膜浸入装满SiO2悬浮液的容器中，其中SiO2粒径为3μm，利用提拉机器以2mm/s匀速竖直向上提拉；
⑧将上述复合膜置于220℃中加热72h；
⑨用旋涂机将光刻胶SU-8基环氧树脂旋涂在复合膜表面SiO2缝隙中，转速3000r/min、旋涂时间为60s，再用乙酸乙酯清洗表面残留的光刻胶；
⑩用紫外固化灯对表面的光刻胶进行固化，时间2min；
Figure BDA0002884282780000081
将上述复合膜置于2.5vol％的氢氟酸溶液中蚀刻10min去除表面SiO2，用酒精彻底清洗，干燥箱中65℃中加热3h。
最终得到厚度为55μm的复合透明膜，其紫外光透过率为85％，且100cm2上可以支撑100ml ZrO2陶瓷浆料基本不变形。
实施例2
①在储料槽中倒入30vol％的ZrO2陶瓷浆料；
②控制打印平台的底部停在复合膜的上方20μm；
③通入冷却氧气；
④打开光源，使得事先处理好的图像投影在复合膜上；
⑤10s后控制打印平台以200mm/h匀速向上移动，同时，投影图像作相应变换；
⑥打印结束后依次关闭光源、暂停打印平台、停止冷却氧气的流通；
⑦取下打印陶瓷素胚件，用酒精清洗掉微固化的浆料残余；
⑧使用紫外固化灯对打印件进行二次固化，最终得到所需陶瓷打印素胚件；
⑨按照相应的烧结工序烧结后即可得到所需陶瓷件。
以上实施例仅用以说明本发明的技术方案，而非对其进行限制；尽管参照前述实施例对本发明进行了详细的说明，对于本领域的普通技术人员来说，依然可以对前述实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或替换，并不使相应技术方案的本质脱离本发明所要求保护的技术方案的精神和范围。

Claims (9)

1.一种连续光固化3D打印陶瓷用复合透明膜的制备方法，其特征在于，所述方法包括以下步骤：（1）取粒径为200nm的球状SiO2颗粒与道康宁PDMS预混液，SiO2质量占比为10％-40％，以200r/min-300r/min搅拌2-5min，得到混合溶液；（2）将步骤（1）得到的混合溶液放入超声波清洗机中混合15-20min；（3）静置冷却后加入PDMS固化剂，固化剂与PDMS预混液质量比为1/10-1/8，以200r/min-300r/min搅拌3-5min；（4）在0-8℃温度中静置12-24h，直至完全没有气泡；（5）利用数控雕刻机，以80-100℃的底板加热、30-50Kpa的气压、320-400mm/s将混合溶液打印成膜；（6）将打印所得膜置于干燥箱中干燥；（7）将完全固化的SiO2/PDMS混合膜浸入装满SiO2悬浮液的容器中，其中悬浮液中SiO2粒径为2-5μm，利用提拉机器以1-8mm/s匀速竖直向上提拉，得到复合膜；（8）将步骤（7）得到的复合膜置于200-250℃中加热60-80h；（9）用旋涂机将光刻胶SU-8基环氧树脂旋涂在复合膜表面SiO2缝隙中，转速2500-3500r/min、旋涂时间30-60s，再用有机溶剂清洗表面残留的光刻胶；（10）用紫外固化灯对表面的光刻胶进行固化，时间1-3min，得到固化后的复合膜；（11）将步骤（10）得到的复合膜置于氢氟酸溶液中蚀刻5-15min去除表面SiO2，用酒精彻底清洗，干燥箱干燥。
2.根据权利要求1所述的一种连续光固化3D打印陶瓷用复合透明膜的制备方法，其特征在于，所述步骤（11）中氢氟酸溶液的浓度为2-5vol％。
3.根据权利要求1所述的一种连续光固化3D打印陶瓷用复合透明膜的制备方法，其特征在于，所述步骤（6）中干燥的温度为80-100℃，干燥时间为2-3h；所述步骤（11）中干燥箱干燥温度60-80℃，干燥时间2-5h。
4.根据权利要求1-3任一项所述的一种连续光固化3D打印陶瓷用复合透明膜的制备方法制备得到的复合透明膜，其特征在于，最终所得的复合透明膜厚度50-100μm，并且氧气透过效率在50barrer以上，紫外光透过率不低于80％，强度不低于20kPa。
5.一种连续光固化3D打印陶瓷方法，其特征在于，使用权利要求4所述的复合透明膜，包括以下步骤：①在储料槽中倒入配制好的陶瓷浆料；②控制打印平台的底部停在复合透明膜的上方20-30μm，浆料没过平台底部；③通入冷却氧气；④打开光源，使得事先处理好的图像投影在复合透明膜上；⑤10-15s后控制打印平台以不超过400mm/h匀速向上移动，同时，投影图像作相应变换；⑥打印结束后依次关闭光源、暂停打印平台、停止冷却氧气的流通；⑦取下打印陶瓷素胚件，清洗掉微固化的浆料残余；⑧使用紫外固化灯对打印件进行二次固化，最终得到所需陶瓷打印素胚件；⑨按照相应的烧结工序烧结后即可得到所需陶瓷件。
6.根据权利要求5所述的一种连续光固化3D打印陶瓷方法，其特征在于，所述陶瓷种类选用氧化锆、氧化铝、氮化硅、氧化镁、氧化钇中的一种或多种组合。
7.根据权利要求6所述的一种连续光固化3D打印陶瓷方法，其特征在于，粒径平均尺寸为0.5-5μm，粉末形状为多边形或球形。
8.根据权利要求5所述的一种连续光固化3D打印陶瓷方法，其特征在于，将选择好的陶瓷原料与光敏树脂混合，以200-300r/min手动搅拌2-5min后，倒入球磨机中，以300-450r/min转速混合6-8h，球磨结束将混料置于干燥箱中常温干燥60-90min后得到所需陶瓷浆料。
9.根据权利要求5所述的一种连续光固化3D打印陶瓷方法，其特征在于，所述方法所用装置，包括工作台和底座，工作台自上而下包括打印平台、储料盒、复合透明膜、供氧冷却模块、数字光模块。
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