CN108439955A - 一种3d打印用陶瓷粉末材料的制备方法 - Google Patents

一种3d打印用陶瓷粉末材料的制备方法 Download PDF

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CN108439955A
CN108439955A CN201810279851.2A CN201810279851A CN108439955A CN 108439955 A CN108439955 A CN 108439955A CN 201810279851 A CN201810279851 A CN 201810279851A CN 108439955 A CN108439955 A CN 108439955A
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ceramic powder
preparation
slurry
powder material
printing
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黄文明
张坤
徐军
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Anhui Hongtai Precision Machinery Technology Co Ltd
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Abstract

本发明公开了一种3D打印用陶瓷粉末材料的制备方法，涉及3D打印使用材料技术领域；本发明3D打印用陶瓷粉末材料的制备方法为：浆料制备、粉料制备、氢化处理、气流磨粉、等静压提高密度、烧制、烧结；本发明方法制备的3D打印用陶瓷粉末材料成分控制精、致密度高、球形度好、颗粒尺寸小且粒度分布范围窄、分散性好、流动性好等特性；且原料安全无毒，添加分散剂更有利于陶瓷粉末材料分散性，使打印出的产品表面更光洁、细腻。

Description

一种3D打印用陶瓷粉末材料的制备方法
技术领域：
本发明涉及3D打印使用材料相关技术领域，具体涉及一种3D打印用陶瓷粉末材料的制备方法。
背景技术：
3D打印(3DP)即快速成型技术的一种，它是一种以数字模型文件为基础，运用粉末状金属或塑料等可粘合材料，通过逐层打印的方式来构造物体的技术。3D打印技术出现在20世纪90年代中期，实际上是利用光固化和纸层叠等技术的最新快速成型装置。它与普通打印工作原理基本相同，打印机内装有液体或粉末等“打印材料”，与电脑连接后，通过电脑控制把“打印材料”一层层叠加起来，最终把计算机上的蓝图变成实物。
所谓的3D打印机与普通打印机工作原理基本相同，只是打印材料有些不同，普通打印机的打印材料是墨水和纸张，而3D打印机内装有金属、陶瓷、塑料、砂等不同的“打印材料”，是实实在在的原材料，打印机与电脑连接后，通过电脑控制可以把“打印材料”一层层叠加起来，最终把计算机上的蓝图变成实物。通俗地说，3D打印机是可以“打印”出真实的3D物体的一种设备，比如打印一个机器人、打印玩具车，打印各种模型，甚至是食物等等。之所以通俗地称其为“打印机”是参照了普通打印机的技术原理，因为分层加工的过程与喷墨打印十分相似。
虽然高端工业印刷可以实现塑料、某些金属或者陶瓷打印，但实现打印的材料都是比较昂贵和稀缺的。另外，打印机也还没有达到成熟的水平，无法支持日常生活中所接触到的各种各样的材料。研究者们在多材料打印上已经取得了一定的进展，但除非这些进展达到成熟并有效，否则材料依然会是3D打印的一大障碍。
发明内容：
本发明针对上述3D打印中使用存在问题，所用陶瓷粉末材料具有成分控制精、致密度高、球形度好、颗粒尺寸小且粒度分布范围窄、分散性好、流动性好等特性。本发明提供一种3D打印用陶瓷粉末材料。
使用本发明所要解决的技术问题采用以下技术方案来实现：
一种3D打印用陶瓷粉末材料，所述3D打印用陶瓷粉末材料的制备方法，包括以下步骤：
(1)将钠石、氧化锌、祁门高岭土、氧化锌、改性方解石混合磨碎成细粉，将细粉混入拌料并置于玻璃器皿中密封，然后将玻璃器皿置于阳光下曝晒；
(2)取出玻璃器皿中物料并干燥，然后与石棉粉、有机铋抗氧剂、二硼化锆、马铃薯淀粉醚、玄武岩纤维、分散剂混合并磨碎成混合料，然后加入混合料重量35.5％-40.5％的水将混合料拌匀成浆料；
(3)将步骤2制成的浆料中加入石膏晶须、硅酮胶、聚羟基烷酸酯、环氧乙烯基酯树脂、膨润土、碳酸锶，加热50-80℃搅拌均匀，后进行氢化处理：装料、抽真空、吸氢、氢碎、脱氢、冷却出炉；得到0.5mm以下粉料；
(4)将步骤3制成的粉料加入到气流磨，进行制粉加工，得到2～3um的粉料；
(5)将步骤4制成的粉料经装模、充磁、加压得到坯料，再经等静压提高密度；
(6)将步骤5等静压后浆料投入炉内烧制，此时烧制温度为200-400℃，烧制10分钟后将浆料取出置于密闭容器内并用200℃二氧化碳气体对密闭容器内加压至1.2-1.6MPa，然后保压10分钟，继续将浆料放入炉内烧制，此时烧制温度为300-500℃，30分钟后取出浆料再继续烧制1小时，此时烧制温度为500-600℃，取出浆料送入风冷机内在2h内将浆料风冷至常温；
(7)将步骤6烧结的浆料进行装匣钵：先在匣钵底部洒上高熔点金属粉末钼，将坯料放入匣钵内，在用高熔点金属粉末将坯料掩埋，然后放入真空烧结炉中，进行真空烧结炉内：烧结工艺、抽真空、加热到180～300℃保温、保温60～240分钟、放气、再加热到180～300℃保温、保温1～10小时、充氩气风冷，即制备成3D打印用陶瓷粉末材料。
所述3D打印用陶瓷粉末材料的制备方法的步骤1中，曝晒选择太阳光强度为6万～10万LX，照射4-6h，照射5-7天。
所述3D打印用陶瓷粉末材料的制备方法的步骤3中，氢化处理氢气浓度为50-80L/m3。
所述3D打印用陶瓷粉末材料的制备方法的步骤4中，所述气流磨，使用气流为压缩空气，空气速度为800-1000s/m。
所述陶瓷粉末材料包括如下份数组分：石膏晶须0.5-0.7份、分散剂1-4份、硅酮胶17-24份、聚羟基烷酸酯5-20份、环氧乙烯基酯树脂20-34份、石棉粉5-13份、有机铋抗氧剂2-16份、钠石12-18份、祁门高岭土22-26份、二硼化锆3-5份、氧化锌3-5份、马铃薯淀粉醚1-1.5份、玄武岩纤维2-4份、膨润土3-6份、改性二氧化硅4-6份、氧化锌4-6份、五氧化二钒2-3份、碳酸钡2-3份。
所述分散剂由下列重量份的原料制成：纳米硅粉5-10份、活性炭4-6份、铝粉0.8-1.5份、茶多酚5-8份、烷基葡萄糖苷2-3份、硼酸2-3份、琥珀酸2-3份、釉果1-2份、三聚磷酸钠1-2份；其制备方法是，将各原料混合磨碎成细粉，然后将细粉用60-100KHz超声波处理10分钟，再向细粉混入其重量份30％-40％的鲸蜡醇搅拌均匀成浆料，然后将浆料送入烘干机内烘干，烘干后继续磨碎成细粉即为分散剂。
所述改性方解石制备方法是：将方解石用-50℃低温氮气冷冻10分钟，然后再用60-100℃苹果醋、枸缘酸、棕榈酸、水按1:1:1:100比例混合液浸泡保温处理30分钟，再用去离子水洗净方解石，然后磨碎成粉，再向粉末中加入香蒲绒纤维素3-5份，羧甲基纤维素0.6-1.0份，丁基硫醇锡0.3-0.5份，麦冬总皂苷0.5-3份、四甲基氢氧化铵0.2-2份、水12-21份搅拌并加热50-70℃直至完全溶解混合均匀，后投入乳化机中70-80℃乳化反应2-4h，后取出立刻放入-50-100℃的环境中迅速冷冻2-6h，后取出放至室温恢复至室温后即得改性方解石。
本发明3D打印用陶瓷粉末材料优点和有益效果是：
1、本发明3D打印用陶瓷粉末材料的制备方法经过后续的抽真空、吸氢、氢碎、脱氢、气流磨粉、等静压提高密度、烧结工艺而制备的3D打印用陶瓷粉末材料性能更稳定，耐久性好，经处理后的陶瓷粉末材料粗细分布均匀，使打印出的产品表面更光洁、细腻；
2、本发明方法制备的3D打印用陶瓷粉末材料，成分控制精、致密度高、球形度好、颗粒尺寸小且粒度分布范围窄、分散性好、流动性好等特性；且原料安全无毒，添加分散剂更有利于陶瓷粉末材料分散性。
具体实施方式：
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例，进一步阐述本发明。
实施例1：
本发明所要解决的技术问题采用以下技术方案来实现：
一种3D打印用陶瓷粉末材料，所述3D打印用陶瓷粉末材料的制备方法，包括以下步骤：
(1)将钠石、氧化锌、祁门高岭土、氧化锌、改性方解石混合磨碎成细粉，将细粉混入拌料并置于玻璃器皿中密封，然后将玻璃器皿置于阳光下曝晒；
(2)取出玻璃器皿中物料并干燥，然后与石棉粉、有机铋抗氧剂、二硼化锆、马铃薯淀粉醚、玄武岩纤维、分散剂混合并磨碎成混合料，然后加入混合料重量36.5％的水将混合料拌匀成浆料；
(3)将步骤2制成的浆料中加入石膏晶须、硅酮胶、聚羟基烷酸酯、环氧乙烯基酯树脂、膨润土、碳酸锶，加热80℃搅拌均匀，后进行氢化处理：装料、抽真空、吸氢、氢碎、脱氢、冷却出炉；得到0.5mm以下粉料；
(4)将步骤3制成的粉料加入到气流磨，进行制粉加工，得到2～3um的粉料；
(5)将步骤4制成的粉料经装模、充磁、加压得到坯料，再经等静压提高密度；
(6)将步骤5等静压后浆料投入炉内烧制，此时烧制温度为250℃，烧制10分钟后将浆料取出置于密闭容器内并用200℃二氧化碳气体对密闭容器内加压至1.5MPa，然后保压10分钟，继续将浆料放入炉内烧制，此时烧制温度为350℃，30分钟后取出浆料再继续烧制1小时，此时烧制温度为550℃，取出浆料送入风冷机内在2h内将浆料风冷至常温；
(7)将步骤6烧结的浆料进行装匣钵：先在匣钵底部洒上高熔点金属粉末钼，将坯料放入匣钵内，在用高熔点金属粉末将坯料掩埋，然后放入真空烧结炉中，进行真空烧结炉内：烧结工艺、抽真空、加热到180℃保温、保温200分钟、放气、再加热到2200℃保温、保温4小时、充氩气风冷，即制备成3D打印用陶瓷粉末材料。
所述3D打印用陶瓷粉末材料的制备方法的步骤1中，曝晒选择太阳光强度为6万～10万LX，照射5h，照射5天。
所述3D打印用陶瓷粉末材料的制备方法的步骤3中，氢化处理氢气浓度为60L/m3。
所述3D打印用陶瓷粉末材料的制备方法的步骤4中，气流磨，使用气流为压缩空气，空气速度为800s/m。
所述陶瓷粉末材料包括如下份数组分：石膏晶须0.5份、分散剂2份、硅酮胶17份、聚羟基烷酸酯13份、环氧乙烯基酯树脂20份、石棉粉11份、有机铋抗氧剂6份、钠石12份、祁门高岭土22份、二硼化锆3份、氧化锌3.5份、马铃薯淀粉醚1.5份、玄武岩纤维2份、膨润土3份、改性二氧化硅4份、氧化锌4.5份、五氧化二钒2.5份、碳酸钡2份。
所述分散剂由下列重量份的原料制成：纳米硅粉5份、活性炭4份、铝粉0.8份、茶多酚5份、烷基葡萄糖苷3份、硼酸2份、琥珀酸2.5份、釉果1.5份、三聚磷酸钠2份；其制备方法是，将各原料混合磨碎成细粉，然后将细粉用90KHz超声波处理10分钟，再向细粉混入其重量份30％的鲸蜡醇搅拌均匀成浆料，然后将浆料送入烘干机内烘干，烘干后继续磨碎成细粉即为分散剂。
所述改性方解石制备方法是：将方解石用-50℃低温氮气冷冻10分钟，然后再用80℃苹果醋、枸缘酸、棕榈酸、水按1:1:1:100比例混合液浸泡保温处理30分钟，再用去离子水洗净方解石，然后磨碎成粉，再向粉末中加入香蒲绒纤维素3份，羧甲基纤维素0.6份，丁基硫醇锡0.3份，麦冬总皂苷0.7份、四甲基氢氧化铵1.5份、水15份搅拌并加热50℃直至完全溶解混合均匀，后投入乳化机中80℃乳化反应3h，后取出立刻放入-60℃的环境中迅速冷冻4h，后取出放至室温恢复至室温后即得改性方解石。
实施例2：
本发明所要解决的技术问题采用以下技术方案来实现：
一种3D打印用陶瓷粉末材料，所述3D打印用陶瓷粉末材料的制备方法，包括以下步骤：
(1)将钠石、氧化锌、祁门高岭土、氧化锌、改性方解石混合磨碎成细粉，将细粉混入拌料并置于玻璃器皿中密封，然后将玻璃器皿置于阳光下曝晒；
(2)取出玻璃器皿中物料并干燥，然后与石棉粉、有机铋抗氧剂、二硼化锆、马铃薯淀粉醚、玄武岩纤维、分散剂混合并磨碎成混合料，然后加入混合料重量38.5％的水将混合料拌匀成浆料；
(3)将步骤2制成的浆料中加入石膏晶须、硅酮胶、聚羟基烷酸酯、环氧乙烯基酯树脂、膨润土、碳酸锶，加热60℃搅拌均匀，后进行氢化处理：装料、抽真空、吸氢、氢碎、脱氢、冷却出炉；得到0.5mm以下粉料；
(4)将步骤3制成的粉料加入到气流磨，进行制粉加工，得到2～3um的粉料；
(5)将步骤4制成的粉料经装模、充磁、加压得到坯料，再经等静压提高密度；
(6)将步骤5等静压后浆料投入炉内烧制，此时烧制温度为230℃，烧制10分钟后将浆料取出置于密闭容器内并用200℃二氧化碳气体对密闭容器内加压至1.4MPa，然后保压10分钟，继续将浆料放入炉内烧制，此时烧制温度为350℃，30分钟后取出浆料再继续烧制1小时，此时烧制温度为500℃，取出浆料送入风冷机内在2h内将浆料风冷至常温；
(7)将步骤6烧结的浆料进行装匣钵：先在匣钵底部洒上高熔点金属粉末钼，将坯料放入匣钵内，在用高熔点金属粉末将坯料掩埋，然后放入真空烧结炉中，进行真空烧结炉内：烧结工艺、抽真空、加热到180℃保温、保温120分钟、放气、再加热到250℃保温、保温4小时、充氩气风冷，即制备成3D打印用陶瓷粉末材料。
所述3D打印用陶瓷粉末材料的制备方法的步骤1中，曝晒选择太阳光强度为6万～10万LX，照射4h，照射7天。
所述3D打印用陶瓷粉末材料的制备方法的步骤3中，氢化处理氢气浓度为65L/m3。
所述3D打印用陶瓷粉末材料的制备方法的步骤4中，气流磨，使用气流为压缩空气，空气速度为1000s/m。
所述陶瓷粉末材料包括如下份数组分：石膏晶须0.7份、分散剂4份、硅酮胶18份、聚羟基烷酸酯16份、环氧乙烯基酯树脂20份、石棉粉13份、有机铋抗氧剂6份、钠石12份、祁门高岭土22份、二硼化锆5份、氧化锌3.5份、马铃薯淀粉醚1份、玄武岩纤维2.5份、膨润土3份、改性二氧化硅4份、氧化锌5份、五氧化二钒2份、碳酸钡2.5份。
所述分散剂由下列重量份的原料制成：纳米硅粉5份、活性炭4份、铝粉0.8份、茶多酚5份、烷基葡萄糖苷2份、硼酸2.5份、琥珀酸2份、釉果1.5份、三聚磷酸钠1份；其制备方法是，将各原料混合磨碎成细粉，然后将细粉用80KHz超声波处理10分钟，再向细粉混入其重量份30％的鲸蜡醇搅拌均匀成浆料，然后将浆料送入烘干机内烘干，烘干后继续磨碎成细粉即为分散剂。
所述改性方解石制备方法是：将方解石用-50℃低温氮气冷冻10分钟，然后再用60-100℃苹果醋、枸缘酸、棕榈酸、水按1:1:1:100比例混合液浸泡保温处理30分钟，再用去离子水洗净方解石，然后磨碎成粉，再向粉末中加入香蒲绒纤维素4份，羧甲基纤维素0.6份，丁基硫醇锡0.5份，麦冬总皂苷0.5份、四甲基氢氧化铵1.2份、水12份搅拌并加热60℃直至完全溶解混合均匀，后投入乳化机中80℃乳化反应4h，后取出立刻放入-50℃的环境中迅速冷冻4h，后取出放至室温恢复至室温后即得改性方解石。
对本发明提供的实施例中分别进行试验考察，实施例1和实施例2制备的3D打印用陶瓷粉末材料进行考察，以普通3D打印材料为对照，其结果如表1所示；
表1 考察结果
由以上结果显示：
本发明3D打印用陶瓷粉末材料，由以上检测结果可以看出：经本发明制备方法抽真空、吸氢、氢碎、脱氢、气流磨粉、等静压提高密度、烧结工艺而制备的3D打印用陶瓷粉末材料性能更稳定，耐久性好，经处理后的陶瓷粉末材料粗细分布均匀，使打印出的产品表面更光洁、细腻；且制备的3D打印用陶瓷粉末材料，成分控制精、致密度高、球形度好、颗粒尺寸小且粒度分布范围窄、分散性好、流动性好等特性；且原料安全无毒，添加分散剂更有利于陶瓷粉末材料分散性。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (4)

1.一种3D打印用陶瓷粉末材料的制备方法，其特征在于：所述3D打印用陶瓷粉末材料的制备方法，包括以下步骤：
(1)将钠石、氧化锌、祁门高岭土、氧化锌、改性方解石混合磨碎成细粉，将细粉混入拌料并置于玻璃器皿中密封，然后将玻璃器皿置于阳光下曝晒；
(2)取出玻璃器皿中物料并干燥，然后与石棉粉、有机铋抗氧剂、二硼化锆、马铃薯淀粉醚、玄武岩纤维、分散剂混合并磨碎成混合料，然后加入混合料重量35.5％-40.5％的水将混合料拌匀成浆料；
(3)将步骤2制成的浆料中加入石膏晶须、硅酮胶、聚羟基烷酸酯、环氧乙烯基酯树脂、膨润土、碳酸锶，加热50-80℃搅拌均匀，后进行氢化处理：装料、抽真空、吸氢、氢碎、脱氢、冷却出炉；得到0.5mm以下粉料；
(4)将步骤3制成的粉料加入到气流磨，进行制粉加工，得到2～3um的粉料；
(5)将步骤4制成的粉料经装模、充磁、加压得到坯料，再经等静压提高密度；
(6)将步骤5等静压后浆料投入炉内烧制，此时烧制温度为200-400℃，烧制10分钟后将浆料取出置于密闭容器内并用200℃二氧化碳气体对密闭容器内加压至1.2-1.6MPa，然后保压10分钟，继续将浆料放入炉内烧制，此时烧制温度为300-500℃，30分钟后取出浆料再继续烧制1小时，此时烧制温度为500-600℃，取出浆料送入风冷机内在2h内将浆料风冷至常温；
(7)将步骤6烧结的浆料进行装匣钵：先在匣钵底部洒上高熔点金属粉末钼，将坯料放入匣钵内，在用高熔点金属粉末将坯料掩埋，然后放入真空烧结炉中，进行真空烧结炉内：烧结工艺、抽真空、加热到180～300℃保温、保温60～240分钟、放气、再加热到180～300℃保温、保温1～10小时、充氩气风冷，即制备成3D打印用陶瓷粉末材料。
2.根据权利要求1所述的3D打印用陶瓷粉末材料的制备方法，其特征在于：所述3D打印用陶瓷粉末材料的制备方法的步骤1中，曝晒选择太阳光强度为6万～10万LX，照射4-6h，照射5-7天。
3.根据权利要求1所述的3D打印用陶瓷粉末材料的制备方法，其特征在于：所述3D打印用陶瓷粉末材料的制备方法的步骤3中，氢化处理氢气浓度为50-80L/m3。
4.根据权利要求1所述的3D打印用陶瓷粉末材料的制备方法，其特征在于：所述气流磨，使用气流为压缩空气，空气速度为800-1000s/m。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111718177A (zh) * 2020-05-17 2020-09-29 陕西励峰德精密陶瓷科技有限公司 一种陶瓷后盖3d打印材料制备方法
WO2022088703A1 (zh) * 2020-10-30 2022-05-05 嘉思特华剑医疗器材(天津)有限公司 含氧化层锆铌合金分区骨小梁单间室胫骨平台及制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111718177A (zh) * 2020-05-17 2020-09-29 陕西励峰德精密陶瓷科技有限公司 一种陶瓷后盖3d打印材料制备方法
WO2022088703A1 (zh) * 2020-10-30 2022-05-05 嘉思特华剑医疗器材(天津)有限公司 含氧化层锆铌合金分区骨小梁单间室胫骨平台及制备方法

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