CN106661766A - 用于3d打印设备中的能烧结的进料 - Google Patents

用于3d打印设备中的能烧结的进料 Download PDF

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CN106661766A
CN106661766A CN201480080491.3A CN201480080491A CN106661766A CN 106661766 A CN106661766 A CN 106661766A CN 201480080491 A CN201480080491 A CN 201480080491A CN 106661766 A CN106661766 A CN 106661766A
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filamentous
plasticizer
ester
mixture
green compact
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P·多特
M·杰克尔
J·沃德曼
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Emery Oleochemicals GmbH
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Abstract

本发明涉及适用于3D打印设备中的丝状体，其中丝状体包含金属和/或陶瓷粉末、热塑性粘合剂和添加剂。本发明也涉及一种制备成型体的方法，包括使用根据本发明的丝状体打印生坯成型体的步骤。也提供根据本发明的丝状体用于3D打印设备中的用途，以及可通过混合金属和/或陶瓷粉末和热塑性粘合剂生产的生坯。本发明也涉及本发明的粘合剂用于生产在3D打印设备中使用的丝状体的用途。

Description

用于3D打印设备中的能烧结的进料
本发明涉及适用于3D打印设备中的丝状体(filament)，其中丝状体包含金属和/或陶瓷粉末、热塑性粘合剂和添加剂。本发明也涉及一种制备成型体的方法，包括使用本发明的丝状体打印生坯成型体(shaped green body)的步骤。也提供根据本发明的丝状体用于3D打印设备中的用途，以及可通过混合金属和/或陶瓷粉末和热塑性粘合剂生产的生坯。本发明也涉及本发明的粘合剂用于生产在3D打印设备中使用的丝状体的用途。
发明背景
在80年代后期，开发了粉末注塑方法，包括金属注塑(MIM)和陶瓷注塑(CIM)。在这些方法中，细粉状的金属或陶瓷材料与可检测量的粘合剂材料混合以形成“进料”，其能通过塑料加工设备按照公知的注塑成型工艺处理。成型方法允许在单个操作中以高体积成型复杂的部件。这些方法的最终产物是用于各种工业和应用中的常规组分物品。
在这些方法中，成型步骤涉及使用注塑机，并形成所谓的生坯。这种生坯进行进一步的步骤，其中通常在生坯被加热到金属或陶瓷组分的烧结温度之前至少部分地除去粘合剂。
许多用于形成原型例如3D打印机的现代方法也需要使用进料。但是，在这些方面中，已经发现用于3D打印设备的进料需要不同的性能，如下所述。
形成用于3D打印设备的进料并不是简单的，这是因为需要调节许多参数。最终的进料产物必须特别满足成功进行3D打印所需的柔性、劲度、粘附性和粘度。
在3D打印领域中，熔融沉积成型(FDM)方法日益增加地用于生产消费品，保证改进3D印刷产品的质量。
熔融沉积成型是一种常用于模制、原型设计和制造应用的添加剂生产技术。FDM是快速原型设计技术，这是机械制造技术之一，其中涉及挤出进料材料的挤出方法。通常，FDM通过将材料按照层铺展来操作。
已经知道体积流量误差会损害印刷产品的质量。热塑性丝状体本身对于FDM挤出机流量的可变性方面有显著影响。换句话说，根据其材料，进料丝状体对体积流量误差做出贡献。
另外，不希望受限于任何理论，认为在机械设计方面，发现丝状体直径的尺寸和公差在确定挤出机的流动特性方面有十分重要的影响。
理想的是，所用丝状体的直径可以最小化，并且可以更严谨的直径公差生产丝状体以减少体积流量误差。
而且，在开发新进料方面，需要选择复合材料以具有合理优良的机械和热性能，以及它们的混合能力和与粘合剂的表面粘合性。
考虑到上述方面，需要新的用于3D打印设备的进料，其可以成型为具有恒定直径的丝状体，并且也满足其他材料要求，例如足够的硬度，合适的粘度，优良的挤出性能，以及在印刷线料之间的优良粘合性。
粘附性是至少一种性能，通过此性能，适用于3D打印设备的进料区别于常规用于粉末注塑(PIM)或粉末挤出模塑(PEM)方法中的那些进料。适用于3D打印的进料需要在各个线料之间的优良粘合能力，从而以高分辨率和优良的重现性生产3D结构。但是，进料的这种性能不能有利地用于粉末模塑(PIM)或粉末挤出模塑(PEM)，特别是如果这些应用涉及光滑的压延机、狭缝式口型或相似的装置时。实际上，在PIM或PEM应用中，这种粘附性不是所需要的，并且通常通过制备不具有此性能的特定进料来避免，例如通过包含抗粘附性的添加剂。
本发明的目的是提供新的适用于3D打印设备的进料材料，其能满足上述标准。
发明概述
为了解决上述问题，本发明提供适用于3D打印设备中的丝状体，其中丝状体包含以下组分或由以下组分组成：
(a)金属(例如铝或钢)和/或陶瓷粉末；
(b)热塑性粘合剂，其包含热塑性聚合物和至少一种增塑剂；和
(c)基于丝状体总重量计的0-10重量％的添加剂。
本发明的另一方面涉及制备成型体的方法，此方法包括以下步骤：
(i)使用根据本发明的丝状体和3D打印设备打印生坯成型体；
(ii)从生坯成型体除去至少一部分的增塑剂；和
(iii)烧结从步骤(ii)得到的生坯成型体以得到所述成型体。
也提供根据本发明的丝状体用于3D打印设备中的用途。
在另一个方面，本发明也涉及生坯，其可以通过混合根据本发明的金属和/或陶瓷粉末和根据本发明的热塑性粘合剂制备。
另一方面也提供根据本发明定义的粘合剂用于生产在3D打印设备中使用的丝状体的用途。
发明详述
在详细描述本发明之前，应当理解的是，本发明不限于这里所述的特定的方法、原型设计和试剂，这里描述的这些可以变化。也应当理解的是，这里使用的术语仅仅为了描述具体实施方案的目的，并不限制本发明的范围，本发明范围将仅仅由所附权利要求限定。除非另有说明，这里使用的所有技术和科学术语是与本领域技术人员常规理解的含义相同的。
在以文中更详细地说明本发明的不同方面。除非另有说明，每个所述方面可以与任何其它一个或多个方面组合。特别是，任何优选或有利的特征可以与任何其它所述的一个或多个优选或有利特征组合。
在本申请中引用一些文献。这里引用的每个文献(包括所有专利、专利申请、科学出版物、产品说明书、指南、DIN命名等)，不论是在上文或下文中，都全部引入本文以供参考。它们都不理解为使得这些公开内容先于之前披露的发明。
下文提供一些化学术语的定义。这些术语将在说明书的其余部分中各自使用情况下分别具有所限定的意义和优选的含义。
术语"烷基"表示饱和的直链或支化碳链。优选，这里使用的烷基是C1-C22烷基，更优选是C1-C10烷基，即具有1、2、3、4、5、6、7、8、9或10个碳原子，例如选自甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基、戊基、己基、庚基、辛基、壬基和癸基。烷基是任选被取代的。
术语"醇"表示具有一个或多个羟基的化合物。例如C8-C36烷基醇是被一个或多个羟基取代的C8-C36烷基。这里使用的脂肪醇表示直链脂族伯醇。
本发明提供适用于3D打印设备中的新型丝状体，例如熔融沉积成型设备。出人意料地发现，这些丝状体显示粘度和硬度性能以及在打印时足够粘合性的理想组合。
因此，在第一方面中，本发明提供适用于3D打印设备中的丝状体，其中丝状体包含以下组分或由以下组分组成：
(a)金属(例如铝或钢)和/或陶瓷粉末；
(b)热塑性粘合剂，其包含热塑性聚合物和至少一种增塑剂；和
(c)基于丝状体总重量计的0-10重量％的添加剂。
本发明的丝状体优选包含至多8重量％、6重量％、4重量％、2重量％或至多1重量％的添加剂，基于丝状体总重量计。本发明丝状体成分的优选用量列在下表中，其中所列成分的总和是100重量％，基于丝状体的总重量计：
根据应用，可以有利地包含粘度改进剂或润滑剂作为添加剂。如果包含粘度改进剂，则其优选选自：苯乙烯-丁二烯的氢化共聚物，乙烯-丙烯共聚物，聚异丁烯，氢化苯乙烯-异戊二烯聚合物，氢化异戊二烯聚合物，聚甲基丙烯酸酯，聚丙烯酸酯，聚烷基苯乙烯，链烯基芳基共轭二烯共聚物，聚烯烃，酯，官能化聚烯烃，被马来酸酐和胺的反应产物官能化的乙烯-丙烯共聚物，被胺官能化的聚甲基丙烯酸酯，与胺反应的苯乙烯-马来酸酐共聚物，聚甲基丙烯酸酯聚合物，酯化聚合物，乙烯基芳族单体和不饱和羧酸或其衍生物的酯化聚合物，烯烃共聚物，乙烯-丙烯共聚物，聚异丁烯或它们的混合物。如果要包含润滑剂作为添加剂，则硬脂酸可以用于此目的。
在其它应用中，添加剂不是必要的。因此，最优选的是，本发明的丝状体不包含添加剂。这将使得在丝状体中包含最大量的金属和/或陶瓷粉末，这是有利的，因为这将减少打印的原型在烧结时的体积变化。如果丝状体不包含添加剂，则优选的是丝状体可以包含杂质，它们通常存在于金属或陶瓷粉末中或本发明的热塑性粘合剂中。最优选的是，这些杂质的量不超过本发明丝状体总质量的0.8重量％。优选的是，本发明的丝状体不包含任何抗粘合的添加剂。
优选的是，在一个实施方案中，所述丝状体包含5-25重量％的粘合剂，基于丝状体的总重量计。
优选，丝状体在20℃下的肖氏A硬度是至少85。
在根据本发明的丝状体中，金属和/或陶瓷粉末优选是能烧结的。这意味着在打印成型体中包含的金属或陶瓷粉末将在加热时形成粘附性物质，且不会熔融。
优选的是本发明的丝状体，其中所述热塑性聚合物是选自聚氨酯，聚酰胺，聚乙烯基吡咯烷酮，聚丙烯酸酯，聚烯烃，和它们的混合物。优选，所述热塑性聚合物是聚酰胺，其选自共聚酰胺、聚酰胺11、聚酰胺12、聚醚-嵌段酰胺和它们的混合物。共聚酰胺可以在一个实施方案中可溶于醇，是优选从C4-C8内酰胺和C10-C18内酰胺制备的。最优选，所述共聚酰胺是从己内酰胺和月桂内酰胺制备的。
也优选的是，所述增塑剂可以至少部分地从丝状体除去，这通过使用有机溶剂在至少20℃、优选20-80℃的温度下提取来进行。
至少一种增塑剂可以优选是取代或未取代的芳族或杂芳族的羧酸酯或它们的混合物。优选，所述至少一种增塑剂是羟基苯甲酸酯的混合物。如果在丝状体中使用羟基苯甲酸酯的混合物作为增塑剂，则羟基苯甲酸酯优选是羟基苯甲酸和支化或直链醇形成的酯，其中醇是选自支化或直链C8-C22醇和它们的混合物，和其中醇是优选选自2-丙基庚基醇，异癸基醇，1-二十二醇，1-十八醇，1-十二醇，2-乙基己基醇和它们的混合物。在另一个优选实施方案中，增塑剂包含羟基苯甲酸和直链C8-C22伯醇形成的酯。
在本发明丝状体的另一个优选实施方案中，羟基苯甲酸酯优选是对-羟基苯甲酸酯。在丝状体的一个更优选的实施方案中，所述至少一种增塑剂是从对-羟基苯甲酸和醇混合物制得的酯混合物，其中醇混合物优选包含2-丙基庚基醇、异癸基醇、1-二十二醇、1-十八醇、1-十二醇和/或2-乙基己基醇。
在本发明丝状体的一个优选实施方案中，所述至少一种增塑剂是酯的混合物，其中酯混合物包含在20℃下为固体的酯和在20℃下为液体的酯，或仅仅包含在20℃下为固体的酯。出人意料地发现，在增塑剂中包含这种混合物允许本发明的丝状体、特别是基于陶瓷粉末的丝状体能长期保持弹性，同时提供足够的在打印时的粘合能力(参见以下实施例3)。
在丝状体的另一个优选实施方案中，热塑性粘合剂包含40-70重量％的增塑剂，基于粘合剂的总重量计。优选，所述热塑性粘合剂具有100-190℃的熔融温度。
也优选的是，在一个实施方案中，本发明的丝状体是弹性的，并具有0.5-5mm的直径，更优选1-3mm。优选，丝状体具有足够的弹性，使得其可以卷在线轴上。在优选实施方案中，本发明的丝状体被卷在线轴上，其中线轴具有400mm的直径。也优选的是，本发明的丝状体具有至少1米的长度，更优选至少10cm。在另一个实施方案中，本发明的丝状体是线性的，并适合于储存在分配器中。
另一方面，本发明提供一种制备成型体的方法，此方法包括以下步骤：
(i)使用根据本发明的丝状体和3D打印设备打印生坯成型体；
(ii)从生坯成型体除去至少一部分的增塑剂；和
(iii)烧结从步骤(ii)得到的生坯成型体以得到所述成型体。
优选，在本发明方法的步骤(ii)中，增塑剂是通过使生坯与能提取增塑剂的有机溶剂接触而提取的，其中所述提取不会改变生坯成型体的形状。不同的有机溶剂可以用于步骤(ii)中，例如包括丙酮。
另一方面，本发明提供本发明的任何丝状体用于3D打印设备中的用途，即用于使用这种打印设备打印3D形状。
本发明的另一方面是一种生坯，其可以通过混合根据本发明的金属和/或陶瓷粉末和所述热塑性粘合剂来生产。在一个优选实施方案中，所述生坯是选自植入物、填充物、牙冠和在烧结后用于牙齿修复中的牙桥。也提供本发明的粘合剂用于生产在3D打印设备中使用的丝状体的用途。
在不偏离本发明范围的情况下，本领域技术人员可以显然对本发明进行各种改进和变化。虽然已经结合具体的优选实施方案描述了本发明，但是应当理解的是，本发明应当不限于这些具体实施方案。
以下实施例仅仅用于说明本发明，并不以任何方式限制由所附权利要求定义的本发明范围。
实施例
实施例1:生产基于钢的丝状体
将平均粒径为约15微米的雾化不锈钢粉末在捏合机中于130℃与以下粘合剂组分混合，并均化1小时以得到塑性状态的组合物：
表1
将上表列出的组合物进一步研磨成具有约1-3mm颗粒的颗粒形式。
使用单螺杆挤出机将这些颗粒挤出成直径为2.5mm的线料，其中机筒温度为120℃，恒定喷嘴温度为80℃。然后将丝状体卷到直径为400mm的线轴上。
实施例2:生产基于铝的丝状体
将平均粒径为约1微米的氧化铝粉末在捏合机中于130℃与以下粘合剂组分混合，并均化1小时以得到塑性状态的组合物：
将上表列出的组合物进一步研磨成具有约1-3mm颗粒的颗粒形式。
使用单螺杆挤出机将这些颗粒挤出成直径为2.5mm的线料，其中机筒温度为130℃，恒定喷嘴温度为75℃。然后将丝状体卷到直径为400mm的线轴上。
实施例3:检测粘合性能
为了检测丝状体彼此之间的粘合能力，经挤出的丝状体彼此层压。在120℃的温度下，丝状体熔融并彼此表面粘合一起，且不需要施加任何压力。以此方式制备的样品在丙酮中于40℃提取12小时，干燥，并在合适的条件下烧结(基于钢的材料于1360℃在氢气气氛中进行，基于氧化铝的材料于1620℃在空气中进行)。烧结密度是大于理论值的95％。
在120-170℃的温度下，丝状体的粘合性能显示彼此之间的优化的粘附性，从而允许丝状体粘合和随后除去增塑剂，且不会损失粘合的丝状体的结构稳定性。所以优选的是，在本发明的丝状体中，本发明热塑性粘合剂的熔融温度是120-170℃。
实施例4：检测肖氏A硬度：
如果在丝状体中的粘合剂过软，则典型3D打印机的输送设备将不能用足够的功率有效地将丝状体输送到打印头。相反，如果粘合剂过硬，则这将引起丝状体、特别是具有非常细陶瓷粒子的基于陶瓷的丝状体过脆，这不便于处理，也可能导致丝状体在打印期间断裂。
所以，这里所述的丝状体的组成也在肖氏A硬度方面得到优化。在这方面，在实施例1和2所示表格中的本发明粘合剂组合物的肖氏A硬度是使用HPE II硬度检测仪按照标准DIN ISO 7619-1检测的。
此检测在20℃下进行，测得在实施例1中所示的粘合剂具有94.5的肖氏A硬度，在实施例2中所示的粘合剂具有89.7的肖氏A硬度。因此，对于在本发明丝状体中所含的粘合剂而言优选的肖氏A硬度值是在85-95的范围内。出人意料的是，选择在此范围内的肖氏A硬度显示最终的丝状体具有在软度和弹性之间的优化平衡。
具有在此范围之外的肖氏A硬度的丝状体组合物将是不利的，因为丝状体将是过脆的或不够致密，这引起在烧结时的收缩问题。
实施例5：检测丝状体的熔体流动指数(MFI)值
熔体流动指数(MFI)是衡量热塑性材料熔体的流动容易性的手段。这定义为在10分钟内在预定温度下在经由预定重力砝码施加的压力下从具有特定直径和长度的毛细管流过的材料的质量克数。
根据实施例1和实施例2制备的丝状体的MFI值是使用MFlow检测设备按照标准ISO1133检测的。
结果显示在下面的图1和2中。测定的流动值表明本发明的丝状体尤其适合用于3D打印设备。
实施例6：结果
在实施例1和2中所述的新型复合材料已经成功地用作在熔融沉积成型快速原型设计方法中的丝状体进料。成功地制备了本发明的柔性丝状体。它们可以卷绕到线轴上，并能在合适的温度下很好地粘合，例如120℃。已经表征了新型丝状体的材料。进料材料的力学实验值和MFI值的分析显示此进料适合用于3D打印体系中，例如FDM体系。此外，它们显示优异的在各层之间的粘合，所以也具有优良的构建平台粘合性能。

Claims (19)

1.一种适用于3D打印设备中的丝状体，其中丝状体包含以下组分或由以下组分组成：
(a)金属和/或陶瓷粉末；
(b)热塑性粘合剂，其包含热塑性聚合物和至少一种增塑剂；和
(c)基于丝状体总重量计的0-10重量％的添加剂。
2.根据权利要求1的丝状体，其中金属和/或陶瓷粉末是能烧结的。
3.根据权利要求1或2的丝状体，其中热塑性聚合物是选自聚氨酯，聚酰胺，聚乙烯基吡咯烷酮，聚丙烯酸酯，聚烯烃，和它们的混合物。
4.根据权利要求3的丝状体，其中聚酰胺是选自共聚酰胺、聚酰胺11、聚酰胺12、聚醚-嵌段酰胺，和它们的混合物。
5.根据权利要求1-4中任一项的丝状体，其中增塑剂能通过在至少20℃下使用有机溶剂提取而至少部分地从丝状体除去。
6.根据权利要求1-5中任一项的丝状体，其中至少一种增塑剂是取代的或未取代的芳族或杂芳族羧酸酯或它们的混合物。
7.根据权利要求1-6中任一项的丝状体，其中所述至少一种增塑剂是羟基苯甲酸酯的混合物。
8.根据权利要求7的丝状体，其中羟基苯甲酸酯是羟基苯甲酸与支化或直链醇形成的酯，其中醇是选自支化或直链的C8-C22醇和它们的混合物，优选选自2-丙基庚基醇、异癸基醇、1-二十二醇、1-十八醇、1-十二醇、2-乙基己基醇和它们的混合物。
9.根据权利要求7或8的丝状体，其中羟基苯甲酸酯是对-羟基苯甲酸酯。
10.根据权利要求1-9中任一项的丝状体，其中至少一种增塑剂是酯的混合物，和其中酯的混合物包含在20℃下为固体的酯和在20℃下为液体的酯，或仅仅包含在20℃下为固体的酯。
11.根据权利要求1-10中任一项的丝状体，其中热塑性粘合剂包含40-70重量％的增塑剂，基于粘合剂的总重量计。
12.根据权利要求1-11中任一项的丝状体，其中热塑性粘合剂具有100-190℃的熔融温度。
13.根据权利要求1-12中任一项的丝状体，其中丝状体是弹性的，并具有0.5-5mm的直径和至少10cm的长度。
14.根据权利要求1-13中任一项的丝状体，其中在以下表格中对于实施方案(A)至(F)给出以下化合物(a)、(b)和(c)的用量，前提是所示的基于丝状体总重量计的重量百分比的总和是100重量％：
(a)金属和/或陶瓷粉末，
(b)热塑性粘合剂，其包含热塑性聚合物和增塑剂，和
(c)添加剂，
15.一种制备成型体的方法，此方法包括以下步骤：
(i)使用根据权利要求1-14中任一项的丝状体和3D打印设备打印生坯成型体；
(ii)从生坯成型体除去至少一部分的增塑剂；和
(iii)烧结从步骤(ii)得到的生坯成型体以得到所述成型体。
16.根据权利要求15的方法，其中在步骤(ii)中，增塑剂是通过生坯与能提取增塑剂的有机溶剂接触而提取的，其中所述提取不会改变生坯成型体的形状。
17.根据权利要求1-14中任一项的丝状体用于3D打印设备中的用途。
18.生坯，其可以通过混合如权利要求1-14任一项中定义的金属和/或陶瓷粉末和如权利要求1-14任一项中定义的热塑性粘合剂制备。
19.如权利要求1-14任一项中定义的粘合剂用于生产在3D打印设备中使用的丝状体的用途。
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