CN112142455A - 基于光固化的3d打印深色陶瓷浆料及陶瓷产品制备方法 - Google Patents
基于光固化的3d打印深色陶瓷浆料及陶瓷产品制备方法 Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 78
- 238000000016 photochemical curing Methods 0.000 title claims abstract description 50
- 238000010146 3D printing Methods 0.000 title claims abstract description 47
- 239000002002 slurry Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000000843 powder Substances 0.000 claims abstract description 51
- 239000002994 raw material Substances 0.000 claims abstract description 30
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000001678 irradiating effect Effects 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 14
- 235000015895 biscuits Nutrition 0.000 claims description 14
- 239000003054 catalyst Substances 0.000 claims description 14
- 239000002270 dispersing agent Substances 0.000 claims description 14
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 9
- 238000005238 degreasing Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000005995 Aluminium silicate Substances 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 7
- 235000012211 aluminium silicate Nutrition 0.000 claims description 7
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 7
- 239000002518 antifoaming agent Substances 0.000 claims description 7
- 239000010433 feldspar Substances 0.000 claims description 7
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 7
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- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 7
- 229910052708 sodium Inorganic materials 0.000 claims description 7
- 239000011734 sodium Substances 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 7
- 229910052736 halogen Inorganic materials 0.000 claims description 6
- 150000002367 halogens Chemical class 0.000 claims description 6
- XEHUIDSUOAGHBW-UHFFFAOYSA-N chromium;pentane-2,4-dione Chemical compound [Cr].CC(=O)CC(C)=O.CC(=O)CC(C)=O.CC(=O)CC(C)=O XEHUIDSUOAGHBW-UHFFFAOYSA-N 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
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Abstract
本发明涉及3D打印陶瓷制品技术领域，尤其涉及一种基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料65～80份、光固化辅料12～25份、助剂6～12份；所述光固化辅料由以下重量份的原料组成：环氧丙烯酸酯38～46份、聚醚丙烯酸酯18～24份、聚酯丙烯酸酯10～15份、聚氨酯丙烯酸酯10～15份、丙烯酸树脂0～10份、光引发剂0.2～1.0份、活性稀释剂20～30份。本发明采用复配光固化树脂，并采用逐层上料、逐层固化的方式堆叠成型，可解决深色陶瓷固化深度不足的问题，在堆叠成型的过程中，每层材料先经长波灯照射深层固化，再经短波灯表层固化，提高了陶瓷产品的可靠度。
Description
技术领域
本发明涉及3D打印陶瓷制品技术领域，尤其涉及一种基于光固化的3D打印深色陶瓷浆料及陶瓷产品制备方法。
背景技术
3D打印成型技术的出现使得陶瓷生产和制造发生了创新性的改变，使得制备过程由原来的减材制作变成了增材制作。3D打印制备陶瓷制品的成型方法主要有加热固化、氧化固化和光固化，其中光固化成型固化速度快，能量利用率高，有机挥发分少，是一种节能环保高效的固化成型方法。
光固化3D打印陶瓷的固化深度受陶瓷颜色深度的影响，在同种光固化灯相同时间相同功率的照射下，陶瓷颜色越深，其固化深度越浅，因此深色陶瓷在加工的过程中容易出现固化不完全的问题，在烧结的过程中产品容易变形，并且影响陶瓷产品的强度。
因此，我们提出了一种基于光固化的3D打印深色陶瓷浆料及陶瓷产品制备方法用于解决上述问题。
发明内容
本发明的目的是为了解决现有技术中存在的缺点，而提出的基于光固化的3D打印深色陶瓷浆料及陶瓷产品制备方法。
基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料65～80份、光固化辅料12～25份、助剂6～12份；所述陶瓷粉料由以下重量份的原料组成：钾长石粉12～18份、钠长石粉15～22份、高岭土粉10～15份、叶腊石粉5～10份、氧化铝3～8份、硅酸锆6～15份、烧氧化锌3～10份；所述光固化辅料由以下重量份的原料组成：环氧丙烯酸酯38～46份、聚醚丙烯酸酯18～24份、聚酯丙烯酸酯10～15份、聚氨酯丙烯酸酯10～15份、丙烯酸树脂0～10份、光引发剂0.2～1.0份、活性稀释剂20～30份；所述助剂包括以下重量份的原料：分散剂1～4份、消泡剂0.5～1.5份、催化剂0.1～3份。
优选的，所述陶瓷粉料的粒度为0.5μm～2μm。
优选的，所述光引发剂的型号为784、819、ITX、TPO和TPO-L中的一种或多种。
优选的，所述分散剂为PMAA-NH4。
优选的，所述催化剂为三苯基膦、乙酰丙酮铬和月桂酸二丁基锡中的一种或多种。
基于光固化的3D打印深色陶瓷产品制备方法，包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌20min～40min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度1.1mm～2mm,每层上料完毕后，先通过波长460nm～480nm的长波灯照射7s～10s，再通过波长400nm～420nm的短波灯照射2s～5s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、经脱脂、烧结，制得深色陶瓷产品。
优选的，所述长波灯的功率为1000mW/cm2～1500mW/cm2，所述长波灯为LED灯或卤素灯中的一种。
优选的，所述短波灯的功率为1500mW/cm2～2000mW/cm2，所述短波灯为LED灯或卤素灯中的一种。
本发明的有益效果是：
1、本发明采用复配光固化树脂，不同种树脂性能互补，并采用逐层上料、逐层固化的方式堆叠成型，可解决深色陶瓷固化深度不足的问题，提高陶瓷产品的强度。
2、在堆叠成型的过程中，每层材料先经长波灯照射深层固化，使得陶瓷粉体不坍塌变形，再经短波灯表层固化，降低内应力，提高了陶瓷产品的可靠度。
具体实施方式
下面结合具体实施例对本发明作进一步解说。
实施例一：
基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料65份、光固化辅料25份、助剂10份；
陶瓷粉料由以下重量份的原料组成：钾长石粉13份、钠长石粉18份、高岭土粉12份、叶腊石粉8份、氧化铝5份、硅酸锆12份、烧氧化锌5份；
光固化辅料由以下重量份的原料组成：环氧丙烯酸酯42份、聚醚丙烯酸酯20份、聚酯丙烯酸酯13份、聚氨酯丙烯酸酯13份、丙烯酸树脂5份、光引发剂0.5份、活性稀释剂22份；
助剂包括以下重量份的原料：分散剂3份、消泡剂1份、催化剂0.5份。
本实施例中，陶瓷粉料的粒度为1μm，光引发剂选用重量比为1:1的784和819，分散剂为PMAA-NH4，催化剂为三苯基膦。
基于光固化的3D打印深色陶瓷产品制备方法,包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌30min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度1.1mm,每层上料完毕后，先通过波长470nm的长波灯照射7s，再通过波长410nm的短波灯照射3s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、对素坯进行缓慢加热至650℃，加热时间1.5h，进行脱脂，再在1300℃进行烧结2h，制得深色陶瓷产品。
本实施例中，长波灯的功率为1300mW/cm2，长波灯为LED灯，短波灯的功率为1800mW/cm2，短波灯为LED灯，通过在长波灯和短波灯上加装滤光片来取得特定波长。
实施例二：
基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料70份、光固化辅料20份、助剂10份；
陶瓷粉料由以下重量份的原料组成：钾长石粉13份、钠长石粉18份、高岭土粉12份、叶腊石粉8份、氧化铝5份、硅酸锆12份、烧氧化锌5份；
光固化辅料由以下重量份的原料组成：环氧丙烯酸酯42份、聚醚丙烯酸酯20份、聚酯丙烯酸酯13份、聚氨酯丙烯酸酯13份、丙烯酸树脂5份、光引发剂0.5份、活性稀释剂22份；
助剂包括以下重量份的原料：分散剂3份、消泡剂1份、催化剂0.5份。
本实施例中，陶瓷粉料的粒度为1μm，光引发剂选用重量比为1:1的784和819，分散剂为PMAA-NH4，催化剂为三苯基膦。
基于光固化的3D打印深色陶瓷产品制备方法，包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌30min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度2mm,每层上料完毕后，先通过波长470nm的长波灯照射7s，再通过波长410nm的短波灯照射3s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、对素坯进行缓慢加热至650℃，加热时间1.5h，进行脱脂，再在1300℃进行烧结2h，制得深色陶瓷产品。
本实施例中，长波灯的功率为1300mW/cm2，长波灯为LED灯，短波灯的功率为1800mW/cm2，短波灯为LED灯，通过在长波灯和短波灯上加装滤光片来取得特定波长。
实施例三：
基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料70份、光固化辅料20份、助剂10份；
陶瓷粉料由以下重量份的原料组成：钾长石粉13份、钠长石粉18份、高岭土粉12份、叶腊石粉8份、氧化铝5份、硅酸锆12份、烧氧化锌5份；
光固化辅料由以下重量份的原料组成：环氧丙烯酸酯42份、聚醚丙烯酸酯20份、聚酯丙烯酸酯13份、聚氨酯丙烯酸酯13份、丙烯酸树脂5份、光引发剂0.5份、活性稀释剂22份；
助剂包括以下重量份的原料：分散剂3份、消泡剂1份、催化剂0.5份。
本实施例中，陶瓷粉料的粒度为1μm，光引发剂选用重量比为1:1的784和ITX，分散剂为PMAA-NH4，催化剂为三苯基膦。
基于光固化的3D打印深色陶瓷产品制备方法，包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌30min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度2mm,每层上料完毕后，先通过波长470nm的长波灯照射10s，再通过波长410nm的短波灯照射5s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、对素坯进行缓慢加热至650℃，加热时间1.5h，进行脱脂，再在1300℃进行烧结2h，制得深色陶瓷产品。
本实施例中，长波灯的功率为1500mW/cm2，长波灯为LED灯，短波灯的功率为1500mW/cm2，短波灯为LED灯，通过在长波灯和短波灯上加装滤光片来取得特定波长。
实施例四：
基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料75份、光固化辅料17份、助剂8份；
陶瓷粉料由以下重量份的原料组成：钾长石粉15份、钠长石粉16份、高岭土粉12份、叶腊石粉6份、氧化铝5份、硅酸锆15份、烧氧化锌3份；
光固化辅料由以下重量份的原料组成：环氧丙烯酸酯45份、聚醚丙烯酸酯20份、聚酯丙烯酸酯12份、聚氨酯丙烯酸酯10份、丙烯酸树脂6份、光引发剂0.6份、活性稀释剂25份；
助剂包括以下重量份的原料：分散剂3.5份、消泡剂0.8份、催化剂0.8份。
本实施例中，陶瓷粉料的粒度为1.2μm，光引发剂选用重量比为1:1的784和TPO，分散剂为PMAA-NH4，催化剂为乙酰丙酮铬。
基于光固化的3D打印深色陶瓷产品制备方法，包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌30min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度1.5mm,每层上料完毕后，先通过波长470nm的长波灯照射7s，再通过波长410nm的短波灯照射3s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、对素坯进行缓慢加热至650℃，加热时间1.5h，进行脱脂，再在1300℃进行烧结2h，制得深色陶瓷产品。
本实施例中，长波灯的功率为1300mW/cm2，长波灯为LED灯，短波灯的功率为1800mW/cm2，短波灯为LED灯，通过在长波灯和短波灯上加装滤光片来取得特定波长。
实施例五：
基于光固化的3D打印深色陶瓷浆料，由以下重量份的原料组成：陶瓷粉料75份、光固化辅料17份、助剂8份；
陶瓷粉料由以下重量份的原料组成：钾长石粉15份、钠长石粉16份、高岭土粉12份、叶腊石粉6份、氧化铝5份、硅酸锆15份、烧氧化锌3份；
光固化辅料由以下重量份的原料组成：环氧丙烯酸酯45份、聚醚丙烯酸酯20份、聚酯丙烯酸酯12份、聚氨酯丙烯酸酯10份、丙烯酸树脂6份、光引发剂0.6份、活性稀释剂25份；
助剂包括以下重量份的原料：分散剂3.5份、消泡剂0.8份、催化剂0.8份。
本实施例中，陶瓷粉料的粒度为1.2μm，光引发剂选用重量比为1:1的784和TPO-L，分散剂为PMAA-NH4，催化剂为乙酰丙酮铬。
基于光固化的3D打印深色陶瓷产品制备方法，包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌30min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度2mm,每层上料完毕后，先通过波长470nm的长波灯照射10s，再通过波长410nm的短波灯照射5s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、对素坯进行缓慢加热至650℃，加热时间1.5h，进行脱脂，再在1300℃进行烧结2h，制得深色陶瓷产品。
本实施例中，长波灯的功率为1500mW/cm2，长波灯为LED灯，短波灯的功率为2000mW/cm2，短波灯为LED灯，通过在长波灯和短波灯上加装滤光片来取得特定波长。
对比例：
使用实施例五中的陶瓷浆料进行3D打印,步骤如下：
S1、将浆料置入真空搅拌机中抽真空并搅拌30min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行3D打印，一次完成上料通过波长410nm的卤素灯照射5s，卤素灯功率1800mW/cm2，制得素坯；
S3、对素坯进行缓慢加热至650℃，加热时间1.5h，进行脱脂，再在1300℃进行烧结2h，制得深色陶瓷产品。
对实施例一至实施例五以及对比例中的陶瓷产品进行相对密度和抗压强度检测(相对密度为素坯的密度与烧结后的产品的密度之比)，实验结果如下：
| 序号 | 相对密度 | 抗压强度(MPa) |
| 实施例一 | 97.8％ | 71.8 |
| 实施例二 | 98.1％ | 68.2 |
| 实施例三 | 97.2％ | 71.5 |
| 实施例四 | 98.5％ | 65.5 |
| 实施例五 | 98.2％ | 62.3 |
| 对比例 | 95.5％ | 47.2 |
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。
Claims (8)
1.基于光固化的3D打印深色陶瓷浆料，其特征在于，由以下重量份的原料组成：陶瓷粉料65～80份、光固化辅料12～25份、助剂6～12份；
所述陶瓷粉料由以下重量份的原料组成：钾长石粉12～18份、钠长石粉15～22份、高岭土粉10～15份、叶腊石粉5～10份、氧化铝3～8份、硅酸锆6～15份、烧氧化锌3～10份；
所述光固化辅料由以下重量份的原料组成：环氧丙烯酸酯38～46份、聚醚丙烯酸酯18～24份、聚酯丙烯酸酯10～15份、聚氨酯丙烯酸酯10～15份、丙烯酸树脂0～10份、光引发剂0.2～1.0份、活性稀释剂20～30份；
所述助剂包括以下重量份的原料：分散剂1～4份、消泡剂0.5～1.5份、催化剂0.1～3份。
2.根据权利要求1所述的基于光固化的3D打印深色陶瓷浆料，其特征在于，所述陶瓷粉料的粒度为0.5μm～2μm。
3.根据权利要求1所述的基于光固化的3D打印深色陶瓷浆料，其特征在于，所述光引发剂的型号为784、819、ITX、TPO和TPO-L中的一种或多种。
4.根据权利要求1所述的基于光固化的3D打印深色陶瓷浆料，其特征在于，所述分散剂为PMAA-NH4。
5.根据权利要求1所述的基于光固化的3D打印深色陶瓷浆料，其特征在于，所述催化剂为三苯基膦、乙酰丙酮铬和月桂酸二丁基锡中的一种或多种。
6.基于光固化的3D打印深色陶瓷产品制备方法，其特征在于,包括以下步骤：
S1、将浆料置入真空搅拌机中抽真空并搅拌20min～40min，加入光固化3D打印机中；
S2、设定3D打印机程序，进行逐层3D打印，每层厚度1.1mm～2mm,每层上料完毕后，先通过波长460nm～480nm的长波灯照射7s～10s，再通过波长400nm～420nm的短波灯照射2s～5s；
S3、重复逐层上料和长、短波灯照射的过程，直到3D打印完成，制得素坯；
S4、经脱脂、烧结，制得深色陶瓷产品。
7.根据权利要求6所述的基于光固化的3D打印深色陶瓷产品制备方法，其特征在于，所述长波灯的功率为1000mW/cm2～1500mW/cm2，所述长波灯为LED灯或卤素灯中的一种。
8.根据权利要求6所述的基于光固化的3D打印深色陶瓷产品制备方法，其特征在于，所述短波灯的功率为1500mW/cm2～2000mW/cm2，所述短波灯为LED灯或卤素灯中的一种。
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