CN109467387A - 一种低孔隙率3d打印陶瓷制品及其制备方法 - Google Patents

一种低孔隙率3d打印陶瓷制品及其制备方法 Download PDF

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CN109467387A
CN109467387A CN201810037271.2A CN201810037271A CN109467387A CN 109467387 A CN109467387 A CN 109467387A CN 201810037271 A CN201810037271 A CN 201810037271A CN 109467387 A CN109467387 A CN 109467387A
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王欣雨
李博
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Hangzhou Chong Yi Electromechanical Technology Co Ltd
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Abstract

本发明涉及3D打印陶瓷制品，公开了一种低孔隙率3D打印陶瓷制品及其制备方法。该陶瓷制品陶瓷坯体和陶瓷釉面组成，坯体的浆料配方采用两种光固化体系，通过二步光固化法进行固化，所得陶瓷制品孔隙率较低，孔隙分布均匀，陶瓷生坯上釉后，可形成釉面形态可控的陶瓷制品。该制备方法操作简单，成本较低，制备效率高，有效降低了时间成本和人力成本，所得产品陶瓷颗粒分散均匀、表面光洁度好，提高了陶瓷产品的可靠性，是一种适于实际生产3D打印陶瓷制品的制备方法。

Description

一种低孔隙率3D打印陶瓷制品及其制备方法
技术领域
本发明涉及3D打印陶瓷制品，尤其涉及一种低孔隙率3D打印陶瓷制品及其制备方法。
背景技术
陶瓷制品，有着悠久且成熟的传统制备工艺，新的3D打印成型技术的出现使得陶瓷生产和制造紧跟着科技的发展而创新，给陶瓷的制备提供了一种新的成型思路，使得制备过程由原来的减材制作变成了增材制作，改变了陶瓷生产制备需要模具和机加工等切削设备来生产的传统成型工艺。
申请号为201610749393.5的中国专利公开了一种直接成型3D陶瓷打印用粘土泥料及其制备方法和应用，该泥料按质量比组成为：陶瓷骨料粉体∶瓜尔豆胶粉体∶分散剂∶增稠剂∶去离子水＝180～185∶0 .4～0 .6∶1 .0～1 .5∶0 .2～0 .6∶40～70。粘土泥料固含量高、剪稀性能良好，适宜于直接成型法3D打印陶瓷器件的制备，于室温条件下在3D打印过程中即可逐渐干燥、固化，从而获得既定的结构而不会塌陷，打印精度高，能够很好地满足3D打印直接成型的需求。但是在后续烧结过程中，由于采用了瓜尔豆胶粉体，在高温下瓜尔豆胶会溶解或碳化，在陶瓷内部形成大量孔隙，影响陶瓷产品的质量。
申请号为201510590675.0的中国专利公开了一种光固化成型的高致密陶瓷的制备方法，通过优化浆料的组分及配比，采用液态干燥方式干燥，采用真空/气氛保护排胶与空气排胶的二步脱脂法进行排胶，陶瓷相对密度在90%以上，但是该方法采用大量溶剂和一步光固化，虽然排胶彻底，相对密度高，但是光固化过程中固化树脂收缩率较高，难以避免会导致陶瓷内部出现梯度密度，影响后续上釉和烧结。
发明内容
为了解决上述技术问题，本发明提供了一种低孔隙率3D打印陶瓷制品及其制备方法，通过优化浆料配方，采用二步光固化法进行固化，所得陶瓷制品孔隙率较低，孔隙分布均匀可调。
本发明的具体技术方案为：该陶瓷制品陶瓷坯体和陶瓷釉面组成；其中陶瓷坯体由以下组分及重量份组成：木岱瓷土30-40份、高岭土10-20份、氧化铝19-23份、氧化锆13-17份、乙烯基酯树脂7-9份、酚醛环氧树脂3-5份、TPO0.2-0.4份、二苯基碘鎓盐0.1-0.2份、分散剂2-3份、消泡剂0.2-0.5份；陶瓷釉面由以下组分及重量份组成：黏土18-20份，长石20-25份，碳酸钡4-6份，碳酸锂8-10份，石英6-8份。
作为优选，所述分散剂为乙烯基化合物。
光固化树脂的黏度一般较大，加入乙烯基化合物一方面能够降低浆料黏度，帮助不同成分混溶，另一方面能够调节固化速率，不会导致成型件局部密度差异。
作为优选，所述消泡剂为GPES型消泡剂。
GPES型消泡剂两端是疏水链，中间隔有亲水链的嵌段共聚物，这种结构的分子易于平卧状聚集在气液界面，因而表面活性强，消泡效率高，适用于泥浆类体系消泡。
该陶瓷制品的制备方法为：
1）将乙烯基酯树脂、酚醛环氧树脂、TPO、二苯基碘鎓盐、分散剂和消泡剂按配方混合搅拌成均匀溶液，再按配方加入木岱瓷土、高岭土、氧化铝、氧化锆，机械搅拌，制成浆料；按配方将黏土，长石，碳酸钡，碳酸锂，石英混合均匀，制成陶瓷釉；
2）将浆料装入3D打印机进行打印，采用高压汞灯对材料进行第一次光固化，第一次固化结束5-10min后，采用低压汞灯对材料进行第二次光固化，得到陶瓷生坯；
3）将陶瓷生坯进行预排树脂后，上陶瓷釉；
4）干燥后，再进行烧结，得到陶瓷制品。
本发明采用了两种光固化体系，3D打印后分两步分别固化成型，首先采用长波固化，穿透力强，适于有色厚膜层快速固化，支撑打印出的陶瓷填料不坍塌，但自由基聚合固化，树脂收缩率高，有氧气抑制作用，因此长波固化后，内部支撑作用良好，内部浆料和表面仍具有一定流动性，能够填充收缩造成的空隙，表面流平，并且能够降低内应力，再短波固化，适于表面固化，收缩率低，没有氧气抑制作用，产品表面平滑，有利于后期排胶烧结。本发明还可以通过调整浆料中树脂的含量和比例来调整陶瓷生坯的收缩率，不同收缩率的陶瓷生坯上釉后，可形成光滑的釉面或不同形态的釉面开片，给陶瓷制品增添了生机。
作为优选，所述步骤1）中机械搅拌转速为400-800r/min，搅拌时间20-60min。
作为优选，所述步骤2）中高压汞灯采用340nm滤光片。
虽然高压汞灯的主要光源为365nm的紫外光，但是仍然会有一些其他波长的光漏出，采用滤光片能够有效拦截340nm以下波长的光，防止阳离子聚合光引发剂被提前引发。
作为优选，所述步骤3）中预排树脂温度为700℃以上，时间为1-2h。
作为优选，所述步骤4）中烧结温度为1350-1400℃，时间为4-8h。
作为优选，所述步骤3）中上陶瓷釉为分步上釉。
作为优选，所述步骤1）中木岱瓷土、高岭土、氧化铝和氧化锆为风干球磨至400目以下的粉末。
瓷土粒径减小能够提高浆料的流动性，降低孔隙率。
与现有技术对比，本发明的有益效果是：本发明通过优化坯体的浆料配方，采用了两种光固化体系，二步光固化法进行固化，所得陶瓷制品孔隙率较低，孔隙分布均匀，还可以通过调整浆料中树脂的含量和比例来调整陶瓷生坯的收缩率，陶瓷生坯上釉后，可形成釉面形态可控的陶瓷制品。该制备方法操作简单，成本较低，制备效率高，有效降低了时间成本和人力成本，所得产品陶瓷颗粒分散均匀、表面光洁度好，提高了陶瓷产品的可靠性，是一种适于实际生产3D打印陶瓷制品的制备方法。
具体实施方式
下面结合实施例对本发明作进一步的描述。
实施例1
将9份乙烯基酯树脂、3份酚醛环氧树脂、0.4份TPO、0.1份二苯基碘鎓盐、3份乙烯基化合物和0.2份GPES型消泡剂混合搅拌成均匀溶液，再按配方加入风干球磨至400目以下的40份木岱瓷土、10份高岭土、20份氧化铝和13份氧化锆，400r/min搅拌60min，制成浆料；将黏土19份，长石23份，碳酸钡4份，碳酸锂9份，石英7份，混合均匀，制成陶瓷釉；将浆料装入3D打印机进行打印，采用装配340nm滤光片的高压汞灯对材料进行第一次光固化，第一次固化结束8min后，采用低压汞灯对材料进行第二次光固化，得到陶瓷生坯；将陶瓷生坯进行700℃预排树脂2h后，上陶瓷釉；干燥后，再进行烧结，温度1400℃，时间为4h，得到陶瓷制品。
所得陶瓷制品相对密度为98%，维氏硬度17.1GPa，烧结后坯体形变量小，釉面平滑无开裂。
实施例2
将7份乙烯基酯树脂、5份酚醛环氧树脂、0.2份TPO、0.2份二苯基碘鎓盐、2份乙烯基化合物和0.5份GPES型消泡剂混合搅拌成均匀溶液，再按配方加入风干球磨至400目以下的30份木岱瓷土、20份高岭土、19份氧化铝和17份氧化锆，500r/min搅拌40min，制成浆料；将黏土20份，长石20份，碳酸钡6份，碳酸锂10份，石英8份，混合均匀，制成陶瓷釉；将浆料装入3D打印机进行打印，采用装配340nm滤光片的高压汞灯对材料进行第一次光固化，第一次固化结束10min后，采用低压汞灯对材料进行第二次光固化，得到陶瓷生坯；将陶瓷生坯进行700℃预排树脂1h后，上陶瓷釉；干燥后，再进行烧结，温度1350℃，时间为8h，得到陶瓷制品。
所得陶瓷制品相对密度为96%，维氏硬度15.2GPa，烧结后坯体形变量与釉面不同，釉面有开片。
实施例3
将8份乙烯基酯树脂、4份酚醛环氧树脂、0.3份TPO、0.2份二苯基碘鎓盐、3份乙烯基化合物和0.4份GPES型消泡剂混合搅拌成均匀溶液，再按配方加入风干球磨至400目以下的35份木岱瓷土、15份高岭土、23份氧化铝和15份氧化锆，800r/min搅拌20min，制成浆料；将黏土18份，长石25份，碳酸钡5份，碳酸锂8份，石英6份，混合均匀，制成陶瓷釉；将浆料装入3D打印机进行打印，采用装配340nm滤光片的高压汞灯对材料进行第一次光固化，第一次固化结束5min后，采用低压汞灯对材料进行第二次光固化，得到陶瓷生坯；将陶瓷生坯进行700℃预排树脂1.5h后，上陶瓷釉；干燥后，再进行烧结，温度1370℃，时间为6h，得到陶瓷制品。
所得陶瓷制品相对密度为95%，维氏硬度14.9GPa，烧结后釉面有开片。
对比例1
除光固化步骤改为用高压汞灯和低压汞灯同时照射固化外，其余配方和制备方法与实施例1相同。
所得陶瓷制品相对密度为90%，维氏硬度12.9GPa，但是坯体形变量大，不符合要求。
对比例2
除光固化步骤改为用高压汞灯和低压汞灯同时照射固化外，其余配方和制备方法与实施例3相同。
所得陶瓷制品坯体有裂缝，不符合要求。
本发明中所用原料、设备，若无特别说明，均为本领域的常用原料、设备；本发明中所用方法，若无特别说明，均为本领域的常规方法。
以上所述，仅是本发明的较佳实施例，并非对本发明作任何限制，凡是根据本发明技术实质对以上实施例所作的任何简单修改、变更以及等效变换，均仍属于本发明技术方案的保护范围。

Claims (10)

1.一种低孔隙率3D打印陶瓷制品，其特征在于，该陶瓷制品陶瓷坯体和陶瓷釉面组成；其中陶瓷坯体由以下组分及重量份组成：木岱瓷土30-40份、高岭土10-20份、氧化铝19-23份、氧化锆13-17份、乙烯基酯树脂7-9份、酚醛环氧树脂3-5份、TPO0.2-0.4份、二苯基碘鎓盐0.1-0.2份、分散剂2-3份、消泡剂0.2-0.5份；陶瓷釉面由以下组分及重量份组成：黏土18-20份，长石20-25份，碳酸钡4-6份，碳酸锂8-10份，石英6-8份。
2.如权利要求1所述的低孔隙率3D打印陶瓷制品，其特征在于，所述分散剂为乙烯基化合物。
3.如权利要求1所述的低孔隙率3D打印陶瓷制品，其特征在于，所述消泡剂为GPES型消泡剂。
4.一种权利要求1所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，该制备方法为：
1）将乙烯基酯树脂、酚醛环氧树脂、TPO、二苯基碘鎓盐、分散剂和消泡剂按配方混合搅拌成均匀溶液，再按配方加入木岱瓷土、高岭土、氧化铝、氧化锆，机械搅拌，制成浆料；按配方将黏土，长石，碳酸钡，碳酸锂，石英混合均匀，制成陶瓷釉；
2）将浆料装入3D打印机进行打印，采用高压汞灯对材料进行第一次光固化，第一次固化结束5-10min后，采用低压汞灯对材料进行第二次光固化，得到陶瓷生坯；
3）将陶瓷生坯进行预排树脂后，上陶瓷釉；
4）干燥后，再进行烧结，得到陶瓷制品。
5.如权利要求4所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，所述步骤1）中机械搅拌转速为400-800r/min，搅拌时间20-60min。
6.如权利要求4所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，所述步骤2）中高压汞灯采用340nm滤光片。
7.如权利要求4所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，所述步骤3）中预排树脂温度为700℃以上，时间为1-2h。
8.如权利要求4所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，所述步骤4）中烧结温度为1350-1400℃，时间为4-8h。
9.如权利要求4所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，所述步骤3）中上陶瓷釉为分步上釉。
10.如权利要求4所述的低孔隙率3D打印陶瓷制品的制备方法，其特征在于，所述步骤1）中木岱瓷土、高岭土、氧化铝和氧化锆为风干球磨至400目以下的粉末。
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