CN106431357A - 用于3d打印成型的陶瓷膏体、膏体的制备方法及其应用 - Google Patents

用于3d打印成型的陶瓷膏体、膏体的制备方法及其应用 Download PDF

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CN106431357A
CN106431357A CN201610791225.2A CN201610791225A CN106431357A CN 106431357 A CN106431357 A CN 106431357A CN 201610791225 A CN201610791225 A CN 201610791225A CN 106431357 A CN106431357 A CN 106431357A
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ceramic paste
ceramic
printing
paste
printing molding
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尹长霞
孙华君
胡帅
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Why Zibo Ceramics Science And Technology Ltd Co
Zibo Advanced High Tech Industrial Development Zone Advanced Ceramics Research Institute
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Why Zibo Ceramics Science And Technology Ltd Co
Zibo Advanced High Tech Industrial Development Zone Advanced Ceramics Research Institute
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Abstract

本发明具体涉及一种用于3D打印成型的陶瓷膏体、膏体的制备方法及其应用，原料组成如下：颗粒级配的陶瓷粉体60％‑80％、分散剂1.5％‑3.5％、粘结剂3％‑7％、润滑剂0.5％‑1.5％，其余为溶剂。为了克服上述现有技术的不足，本发明提供了一种用于3D打印成型的陶瓷膏体、膏体的制备方法及其应用，此方法工艺简单、3D打印设备成本低，无需加热和支撑材料，膏体在打印挤出过程中可减小陶瓷粉末颗粒之间的间距，坯体致密度高，陶瓷膏体可制备各种形状复杂的陶瓷制品。

Description

用于3D打印成型的陶瓷膏体、膏体的制备方法及其应用
技术领域
本发明涉及陶瓷材料技术领域，具体涉及一种用于3D打印成型的陶瓷膏体、膏体的制备方法及其应用。
背景技术
陶瓷材料作为一种重要的结构材料，具有高强度、高硬度、耐高温、耐腐蚀等优点，无论在传统工业领域还是新兴的高新技术领域都有广泛的应用。陶瓷成型是生产过程的一个重要步骤，目前主要成型方法有：挤压成型、干压成型、注浆成型、凝胶注模成型等，上述成型方法在制备陶瓷的过程中，首先根据陶瓷产品的要求制备相应的模具，若设计或构件结构发生变化，需重新制备模具，生产周期长，研发成本高；制造产品的形状种类有限；多种异形件无法用传统成型方法制备；制造产品时产生的副产品比较多，浪费原料和增大资源消耗。随着工业的快速发展，这些传统的成型方法已不能满足某些领域的要求，3D打印成型是近年来快速发展的一种新型成型工艺，该工艺是一种以数字模型文件为基础，运用粉末状金属、塑料、陶瓷粉末等可粘合材料，通过逐层打印的方式来构造物体的技术。相比于传统陶瓷成型方式，3D打印成型具有以下先进性：(1)制造精度高；(2)生产周期短；(3)可以实现个性化异形制造；(4)制造成本低。
目前用于陶瓷3D打印的技术主要有分层实体制造(LOM)、熔化沉积造型(FDM)、形状沉积成型(SDM)、喷墨打印法(IJM)、立体光刻(SLA)、选区激光烧结(SLS)。
分层实体制造技术对陶瓷基片要求高、多余部分材料去除困难；熔化沉积造型精度低，难以构建结构复杂的零件，垂直方向强度小，成形速度较慢，原材料价格昂贵；形状沉积成型，需要制作支撑，原型的部分复杂和细微结构的支撑很难去除；喷墨打印法和选区激光烧结制备陶瓷材料存在陶瓷粉末颗粒之间间距大，坯体密度低，在高温烧结过程中无法致密化，陶瓷性能低的问题；立体光刻制备陶瓷材料由于所用的液态光敏树脂成本高、可选择范围小、树脂有一定毒性、设备价格高等无法得到广泛应用。
发明内容
为了克服上述现有技术的不足，本发明提供了一种用于3D打印成型的陶瓷膏体、膏体的制备方法及其应用，此方法工艺简单、3D打印设备成本低，无需加热和支撑材料，膏体在打印挤出过程中可减小陶瓷粉末颗粒之间的间距，坯体致密度高，陶瓷膏体可制备各种形状复杂的陶瓷制品。
本发明所述的一种用于3D打印成型的陶瓷膏体，原料组成如下：
颗粒级配的陶瓷粉体60％-80％、分散剂1.5％-3.5％、粘结剂3％-7％、润滑剂0.5％-1.5％，其余为溶剂。
陶瓷粉体为氧化铝、碳化硅、氮化硅或氧化锆中的一种。
颗粒级配的陶瓷粉体粗细粉之比为2:3；颗粒级配的粗粉体粒度D50在30-100μm，颗粒级配的细粉体粒度D50在1-10μm。
分散剂为聚丙烯酸铵、柠檬酸铵、聚乙二醇、甲基纤维素、三乙醇胺或聚甲基丙烯酸铵中的一种或几种。
粘结剂为聚乙烯醇、聚乙二醇、甲基纤维素、羧甲基纤维素、聚丙基纤维素或石蜡中的一种或几种。
润滑剂为丙三醇、硬脂酸酰胺或硬脂酸锌中的一种或几种。
溶剂为去离子水和乙醇。
所述的用于3D打印成型的陶瓷膏体的制备方法，将原料混合1-3h，制备成陶瓷膏体。
所述的用于3D打印成型的陶瓷膏体的应用，采用3D打印成型的陶瓷膏体制备目标零件，包括以下步骤：
(1)将原料混合1-3h，制备成陶瓷膏体；
(2)将配置好的陶瓷膏体装入3D打印机的料筒中，按照预先导入3D打印机中的切片gcode文件打印；
(3)打印过程中使用1mm或2mm喷头，在gcode制造程序的控制下，调节打印速度和出丝量，通过层层堆积，制得3D打印成型的坯体；
(4)坯体经烘干、烧结制得目标零件。
陶瓷膏体的出丝为30-150％，挤出速度为6-100mm/s。
本发明中陶瓷粉体优选微米级别。
与现有技术相比，本发明的有益效果是：
本发明不需要专门的设备，膏体配制简单易行，成本低，此方法工艺简单、3D打印过程中无需激光及其它方式加热、无需支撑材料或其它高成本操作，在3D打印挤出过程中通过调节膏体的黏度、固相含量、打印速度和出丝量等参数，可减少陶瓷料浆中粉末颗粒的间距，得到坯体致密度高且不受形状的限制，适合制备各种复杂形状的陶瓷制品，为陶瓷零件的快速成型提供了一种新的途径。
附图说明
图1为实施例1配制的陶瓷膏体3D打印成型烧结后产品的SEM图。
具体实施方式
下面结合实施例对本发明做进一步的说明。
实施例1
(1)取161g颗粒级配的氧化铝微米级粉体(占总质量的70wt％)，颗粒级配粉体粗粉与细粉之比为2:3，粗粉粒度D50在80μm，细粉粒度D505μm，形状为近球形，3.94g聚乙二醇、6.9g聚乙烯醇溶液(溶液浓度为10wt％)和3.1g石蜡的混合物、3.45g丙三醇、21.48g去离子水和9.20g酒精，16.45g滑石粉和4.48g碳酸钙的混合物，装入小型真空练泥机中混合2h，制备成氧化铝陶瓷膏体；
(2)将配置好的陶瓷膏体装入陶泥3D打印机的料筒中，按照预先导入3D打印机中的切片gcode文件打印；
(3)打印过程中使用1mm喷头，在gcode制造程序的控制下，氧化铝陶瓷膏体的出丝为70％，陶瓷膏体的挤出速度为90mm/s；
(4)坯体经烘箱中60℃下干燥1h，素坯完全干燥；
(5)常压烧结。
烧结曲线为：从室温以2℃/min升温至500℃，然后升温至800℃，接着升温至900℃，速率不变，最后以1℃/min升温至1580℃保温3h即可，烧结密度达到3.80g/cm3以上。
以上百分数均为质量分数。
实施例2
本实施例与实施例1制备步骤相同，不同的是，步骤(1)中采用的陶瓷粉末为碳化硅，取60wt％碳化硅颗粒级配微米粉体，粗粉粒度D50在40μm，细粉粒度D5010μm，碳化硅粉中炭粉与碳化硅质量之比为1:4，分散剂为2.8％柠檬酸铵和0.7％甲基纤维素混合物；粘结剂为7％甲基纤维素，润滑剂为1％硬脂酸锌，19.95％去离子水和8.55％酒精；在步骤(5)中为真空反应烧结，素坯周围加入Si粒，烧结曲线：从室温升温至600℃，然后升温至1000℃，接着升温至1600℃保温2h，烧结密度到3.02g/cm3以上。
以上百分数均为质量分数。
实施例3
本实施例与实施例1制备步骤相同，不同的是，步骤(1)中采用的陶瓷粉末为氧化锆，取80wt％氧化锆颗粒级配粉体，粗粉粒度D50在100μm，细粉粒度D502μm，分散剂为2％的三乙醇胺；粘结剂为3.5％的聚丙基纤维素，润滑剂为0.5％丙三醇，其余为9.8％去离子水和4.2％酒精；步骤(3)中，打印过程中使用2mm喷头，在步骤(5)中烧结曲线：从室温以2℃/min升温至500℃，然后升温至800℃，速率不变，最后以1℃/min升温至1500℃保温3h即可，烧结密度达到5.30g/cm3以上。
以上百分数均为质量分数。

Claims (10)

1.一种用于3D打印成型的陶瓷膏体，其特征在于，原料组成如下：
颗粒级配的陶瓷粉体60％-80％、分散剂1.5％-3.5％、粘结剂3％-7％、润滑剂0.5％-1.5％，其余为溶剂。
2.根据权利要求1所述的用于3D打印成型的陶瓷膏体，其特征在于，陶瓷粉体为氧化铝、碳化硅、氮化硅或氧化锆中的一种。
3.根据权利要求1所述的用于3D打印成型的陶瓷膏体，其特征在于，颗粒级配的陶瓷粉体粗细粉之比为2:3；颗粒级配的粗粉体粒度D50在30-100μm，颗粒级配的细粉体粒度D50在1-10μm。
4.根据权利要求1所述的用于3D打印成型的陶瓷膏体，其特征在于，分散剂为聚丙烯酸铵、柠檬酸铵、聚乙二醇、甲基纤维素、三乙醇胺或聚甲基丙烯酸铵中的一种或几种。
5.根据权利要求1所述的用于3D打印成型的陶瓷膏体，其特征在于，粘结剂为聚乙烯醇、聚乙二醇、甲基纤维素、羧甲基纤维素、聚丙基纤维素或石蜡中的一种或几种。
6.根据权利要求1所述的用于3D打印成型的陶瓷膏体，其特征在于，润滑剂为丙三醇、硬脂酸酰胺或硬脂酸锌中的一种或几种。
7.根据权利要求1所述的用于3D打印成型的陶瓷膏体，其特征在于，溶剂为去离子水和乙醇。
8.一种权利要求1所述的用于3D打印成型的陶瓷膏体的制备方法，其特征在于，将原料混合1-3h，制备成陶瓷膏体。
9.一种权利要求1所述的用于3D打印成型的陶瓷膏体的应用，其特征在于，采用3D打印成型的陶瓷膏体制备目标零件，包括以下步骤：
(1)将原料混合1-3h，制备成陶瓷膏体；
(2)将配置好的陶瓷膏体装入3D打印机的料筒中，按照预先导入3D打印机中的切片gcode文件打印；
(3)打印过程中使用1mm或2mm喷头，在gcode制造程序的控制下，调节打印速度和出丝量，通过层层堆积，制得3D打印成型的坯体；
(4)坯体经烘干、烧结制得目标零件。
10.根据权利要求9所述的用于3D打印成型的陶瓷膏体的应用，其特征在于，陶瓷膏体的出丝为30-150％，挤出速度为6-100mm/s。
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