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CN105848812B - 在增材制造工艺中使用低温固化来从多孔基质生产单块体 - Google Patents

在增材制造工艺中使用低温固化来从多孔基质生产单块体 Download PDF

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CN105848812B
CN105848812B CN201480065497.3A CN201480065497A CN105848812B CN 105848812 B CN105848812 B CN 105848812B CN 201480065497 A CN201480065497 A CN 201480065497A CN 105848812 B CN105848812 B CN 105848812B
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理查德·E·里曼
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Rutgers State University of New Jersey
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Abstract

一种从多孔基质生产单块体的方法，其包含在增材制造工艺中使用低温固化。

Description

在增材制造工艺中使用低温固化来从多孔基质生产单块体
相关申请案
本申请案主张2013年11月6日申请的第61/900,774号美国临时专利申请案的优先权，所述美国临时专利申请案以全文引用的方式并入本文中。
技术领域
本发明大体上涉及增材制造工艺，且特定来说，涉及在增材制造中使用低温固化。
背景技术
增材制造(AM)是指一种工艺，借助所述工艺使用数字3D设计数据通过沉积材料分层构建组件。增材制造包含3D打印及下文将更详细描述的其它工艺。AM是可与需要材料移除的常规制造方法区分开的一种制造技术。代替从固体块研磨工件，举例来说，增材制造使用可以精细粉末形式提供的材料逐层构建组件。可在本文所论述的多种增材制造工艺中使用一系列不同金属、塑料及复合材料。
发明内容
一个实施例涉及一种从多孔基质生产单块体的方法，所述方法包含在增材制造工艺中使用低温固化。
另一实施例涉及一种从多孔基质生产单块体的方法，所述方法包含：提供具有填隙空间且包括至少第一反应物的一层多孔基质；使所述多孔基质的所述层与承载至少第二反应物的渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述层的所述填隙空间的至少一部分以提供至少第一产物；允许所述至少第一产物形成且填充所述多孔基质的所述层的所述填隙空间的至少一部分；以及重复以上步骤以生产单块体。
另一实施例涉及一种从多孔基质生产单块体的方法，所述方法包含：提供具有填隙空间且包括至少第一反应物的多孔基质的多个连续层；使所述多孔基质的所述多个连续层与承载至少第二反应物的渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述层的所述填隙空间的至少一部分以提供至少第一产物；以及允许所述至少第一产物形成且填充所述多孔基质的所述层的所述填隙空间的至少一部分以形成所述单块体。
另一实施例涉及一种从多孔基质生产单块体的方法，所述方法包含：提供具有填隙空间且包含至少第一反应物的多孔基质的第一层；使所述多孔基质的所述第一层与承载至少第二反应物的渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述第一层的填隙空间的至少一部分以提供至少第一产物；允许所述至少第一产物形成且填充所述多孔基质的所述第一层的所述填隙空间的至少一部分；在所述多孔基质的所述第一层之上提供所述多孔基质的多个连续层；使所述多孔基质的所述多个连续层与所述渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述连续层的所述填隙空间的至少一部分以提供至少第一产物；以及允许所述至少第一产物形成且填充所述多孔基质的所述第一层的所述填隙空间的至少一部分，由此生产单块体。
附图说明
图1是根据实施例的可在制造单块体的方法中使用的设备的示意性说明。
图2是根据实施例的可在制造单块体的方法中使用的另一设备的照片。
图3是根据所述方法的实施例所制造的锥形单块体的照片。
具体实施方式
可使用增材制造方法(例如3D打印、立体光刻、熔融沉积成型、电子束无模制造、直接金属激光烧结、电子束熔化、选择性激光熔化、选择性热烧结、选择性激光烧结、基于石膏的3D打印、分层实体制造、数字光处理、聚合材料喷射(polyjet)及粉末层喷墨打印)制造单块体。下文在表1及2中更详细描述这些方法，表1和2分别从2013年七月/八月光学及光子学新闻(Optics&Photonics News)第22页的蒂姆·海耶斯(Tim Hayes)所著的“3D打印的未来(The future of 3D printing)”及11/6/13所访问的维基百科(Wikipedia)3D打印网页复制。然而，这些方法中的若干方法仅适用于使用金属制造，而其它方法仅适用于使用聚合物制造。发明者已发现，在增材制造中使用低温固化过程导致能够制造任何类型的材料(包含金属、陶瓷、陶瓷金属、聚合物或其复合物)的单块体的方法。
表1
表2
在低温固化或热液液相致密化过程中，使包含第一反应物(即，能够经受化学反应的材料)的多孔基质与包含第二反应物的渗透介质接触。第一及第二反应物起反应以形成填充多孔基质中的孔的产物。在实施例中，含有第一反应物的多孔基质呈粉末形式。在实施例中，多孔基质还包含粘结剂(例如聚合物粘结剂)以使粉末结块。替代地，可省略粘结剂。在另一实施例中，多孔基质包含流体，例如水、酒精或其组合。替代地，可使用其它非水流体。任何适合的基质及渗透材料，例如，作为附件附加到本文且特此以全文引用方式并入的美国专利8,313,802中所揭示的基质及渗透材料。使用术语低温固化作为用于8,313,802专利中所描述的热液液相烧结方法的同义词。
所述方法的实施例包含在增材制造工艺中使用低温固化来从多孔基质生产单块体。低温可为小于通常与金属及陶瓷的烧结相关联的温度的任何温度。通常，温度可小于约500℃，例如小于约250℃，例如室温到200℃(包含80到180℃)。反应压力可小于100,000psi，例如1到3个大气压。
另一实施例包含一种从多孔基质生产单块体的方法，所述方法包含：提供具有填隙空间且包括至少第一反应物的一层多孔基质；使所述多孔基质的所述层与承载至少第二反应物的渗透介质接触；允许渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述层的所述填隙空间的至少一部分以提供至少第一产物；允许所述至少第一产物形成且填充所述多孔基质的所述层的所述填隙空间的至少一部分；以及重复以上步骤以生产单块体。
又一实施例涉及一种从多孔基质生产单块体的方法，所述方法包含：提供具有填隙空间且包括至少第一反应物的多孔基质的多个连续层；使所述多孔基质的所述多个连续层与承载至少第二反应物的渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述层的所述填隙空间的至少一部分以提供至少第一产物；以及允许所述至少第一产物形成且填充所述多孔基质的所述层的所述填隙空间的至少一部分以形成所述单块体。
另一实施例涉及一种从多孔基质生产单块体的方法，所述方法：提供具有填隙空间且包括至少第一反应物的多孔基质的第一层；使所述多孔基质的所述第一层与承载至少第二反应物的渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述第一层的所述填隙空间的至少一部分以提供至少第一产物；允许所述至少第一产物形成且填充所述多孔基质的所述第一层的所述填隙空间的至少一部分；在所述多孔基质的所述第一层之上提供所述多孔基质的多个连续层；使所述多孔基质的所述多个连续层与所述渗透介质接触；允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述连续层的所述填隙空间的至少一部分以提供第一产物；以及允许所述至少第一产物形成且填充所述多孔基质的所述第一层的所述填隙空间的至少一部分，由此生产单块体。
在上文实施例中的任何者中，可在提供下一连续层之前使多个连续层中的每一层与渗透介质接触。替代地，可首先提供单块体的所有层，且接着使其与渗透介质接触。此外，在上文实施例中的任何者中，使用渗透介质完全或部分渗透整个多孔基质。在实施例中，多孔基质可包含粘结剂材料。在实施例中，渗透介质可与粘结剂起反应，从而导致粘结剂从多孔基质移除。
在实施例中，允许至少第一产物形成且填充多孔基质的层的填隙空间的至少一部分包含加热多孔基质的层。可经由传导、感应、对流或辐射施加热量。在实施例中，多孔基质包含用于金属、陶瓷、陶瓷金属、聚合物或其复合物的前体。
在实施例中，多孔基质是生坯。即，沉积态多孔基质尚未与渗透介质起反应以形成最终产物相(即，单块体，例如陶瓷、金属、陶瓷金属、聚合物或其复合物体)。
在实施例中，渗透介质可包含气体，例如CO2。在实施例中，多孔基质是浆液。浆液包含水或酒精或其组合，例如0到20％酒精。在实施例中，使用打印头提供多孔基质的层(例如，形成于支撑件上)，如下文更详细论述。在实施例中，使用打印头提供渗透介质，如下文更详细论述。
在实施例中，在增材制造工艺中使用低温固化以固化生坯或从所述生坯移除粘结剂。在实施例中，生坯包括从打印头沉积的基于粉末的陶瓷、金属或陶瓷金属材料或其前体。在实施例中，低温固化包含将碱性液体(例如，pH>7)提供到生坯且将所述生坯加热到低于250℃的温度以从所述生坯移除粘结剂。在另一实施例中，低温固化包含将流体提供到生坯且将其加热到低于250℃的温度以将所述生坯固化成单块固体。在实施例中，使用低温固化同时固化生坯且从所述生坯移除粘结剂。在此步骤中，所述方法包含将碱性液体提供到生坯且将所述生坯加热到低于250℃的温度以从所述生坯移除粘结剂，且接着在与粘结剂移除步骤相同的步骤期间或在使用相同或使用不同(例如，中性或酸性)流体的随后步骤期间将所述生坯固化成单块固体。
在实施例中，单块固体具有在生坯大小的大小的2％范围以内的大小。因此，生坯多孔基质的低温固化导致多孔基质的层基本上不收缩。即，最后单块体具有与原始生坯基本上相同的大小。举例来说，收缩率可小于2％，例如小于1％。这被认为是归因于在低温固化过程中缺少粉粒朝向彼此的移动。相比之下，在常规高温烧结期间，生坯中的粉粒朝向彼此移动从而产生收缩。此外，可在增材制造期间使用低温固化的组合形成不能耐高温烧结或高温增材制造的材料。
在另一实施例中，渗透流体在经部分渗透低温固化中包含气体及液体，或所述流体在经完全渗透低温固化中包含液体。实施例还包含由任何上文所论述的方法所制造的产物。
图1说明设备100的实施例，可使用设备100实践上文所论述的实施例的方法。在此实施例中，设备100包含粉末井/贮集器102，在其中存储用于制造多孔基质的粉末材料。设备100还包含：打印托盘104，在其上将生产单块体110；以及打印头106，其可用于递送渗透介质(例如流体)及/或粉末。可将渗透介质存储于流体地连接到打印头106的贮集器108。在实施例中，打印头106经配置以在X及Y方向上移动，而打印托盘104经配置以在Z方向上移动。以此方式，随着由打印头106沉积单块体的每一连续层，打印托盘104降低。在设备100的替代实施例中，打印头106经配置以在X、Y及Z方向上移动，而打印托盘104保持静止。替代地，可将打印头106保持为静止，且打印托盘106可经配置以在X、Y及Z方向上移动。
实例
实例1：CACO3-SiO2-键合硅灰石(CaSiO3)体的形成
3D打印机油墨浆液的制备
在第一实例中，将220g的硅灰石(CaSiO3)粉末分散于210mL的去离子水中且在轧制罐中使用钇稳定氧化锆球介质研磨其6小时。将所述球介质与所得悬浮液分离。使用额外的100mL水将粘到球介质的粉末洗涤回到所述悬浮液中。然后，将1.1g的Darvan811TM分散剂添加到所述悬浮液，且将氢氧化铵(NH4OH)逐滴添加到所述悬浮液以将所述悬浮液的pH调整到9。接着将所述悬浮液压滤成具有45％固相体积分数的浆液。接着，将1mL的正辛醇及1.2g的羟丙甲纤维素添加到所述浆液，在此之后，使用油漆搅拌器搅拌所述浆液30分钟。然后，将0.5g的聚乙烯亚胺(PEI)水基溶液(按重量计算，～50％的PEI)添加到所述浆液，在此之后，由油漆搅拌器搅拌所述浆液至少1小时。此过程产生大约175mL的油墨浆液。
CaSiO3体的打印及碳化
接着，将基于CaSiO3的浆液加载到经改性的熔融长丝制造(FFF)三角形形态的3D打印机中。图2是FFF打印机100的照片。使打印机100位于能够使用可加热打印床维持加压大气的腔室(未展示)中。通过以1mm/s的速率将浆液挤压成具有0.7mm的直径的连续长丝来打印不同形状的若干对象。在图3中展示通过FFF工艺打印且通过气辅热液液相致密化(g-rHLPD)过程所固化的单块体110、锥形CaCO3/SiO2键合CaSiO3对象的一个实例。在打印及随后进行的90℃下的干燥之后的单块体110的重量是2.38g，且其总体积是如使用阿基米德方法所测量的1.28cm3。将所打印且干燥的CaSiO3单块体碳化于相同腔室中，其中通过在90℃下在具有2.36atm CO2气体及0.69atm蒸汽的大气中持续20小时打印其。由外部储槽提供CO2，而通过加热所述腔室内部的贮水器提供蒸汽。在g-rHLPD过程之后，再次干燥所述单块体。在碳化及干燥之后重量为3.00g的锥形物等同于样本中的～70mol％的碳化反应完成率。所述过程使样本的相对密度从～64％有效地增加到～85％。
实例2：CaCO3-SiO2-键合硅灰石(CaSiO3)体的逐层及逐体元3D打印
制备CaSiO3油墨浆液且将其加载到类似于上文实例1中所描述的3D打印机的3D打印机中。然而，连同经加热沉积床及长丝挤压机一起，所述打印机具有：第二喷嘴，其用于使用去离子水洗涤；及第三头，其含有红外光束发射器以对光点进行直接局部加热。在一种情况中，逐层打印锥形物。首先，长丝挤压机(打印头)沉积呈锥形物的底层图案的2mm厚的浆液层。在打印腔室中在90℃下干燥此层15分钟，且接着使用前述条件通过g-rHLPD碳化此层另外30分钟。所获得的所述反应产率是80mol％，等同于增重30％且相对密度从64％增加到88％。在碳化之后，沉积下一个2mm层且重复所述干燥/碳化循环。所述整个过程被重复9次以通过逐层打印获取所述锥形物。
在另一实例中，逐体元地打印具有20mm的长度、10mm的宽度及10mm的高度的立方体。首先，将浆液挤压成5mm长、5mm宽及2mm厚的拐角体元图案。执行上文所描述的干燥/g-rHLPD碳化循环。所实现的反应产率是95mol％，等同于增重36％且相对密度从64％增加到92％。随后通过打印所述浆液沉积下一体元。所述循环被重复39次以获得所述立方体。
实例3：钛酸锶(SrTiO3)-固化锐钛矿体的形成
使用类似于实例1中的程序的程序制备基于锐钛矿(TiO2)的浆液且将其打印成对象。在属于打印部件的所述构建基地的一部分的较小压力容器内，在88mL水中使用14.20g的八水氢氧化锶(Sr(OH)2-8H2O)的溶液渗透具有30mm的直径、2mm的厚度及3.30g的干重的圆柱形TiO2单块体。将所述压力容器加热到95℃持续144小时以将所述对象中的TiO2转化成SrTiO3，由此通过反应物热液液相致密化(rHLPD)过程固化所述对象。接着，将经固化的单块体从所述容器移除以进行洗涤及干燥。样本事实上维持与其在rHLPD处理之前相同的维度，但重量为6.09g。增重等同于65.5mol％的反应完成率且相对密度从60％增加到88％。
实例4：钛酸锶(SrTiO3)-固化锐钛矿体的逐层及逐体元3D打印
制备基于锐钛矿(TiO2)的浆液且将其加载到类似于实例2中所描述的3D打印机的3D打印机中。然而，此打印机包含额外打印头，其具有喷嘴及外壳以保持经加热反应溶液。全部四个打印头可独立于彼此而移动。
首先，长丝挤压机沉积呈经打印对象的第一层图案的2mm厚的浆液层。在90℃下加热打印机床以迅速干燥所述经打印材料持续15分钟。接着第二喷嘴以500μL/min的速率将水中的15mL的Sr(OH)2-8H2O的1摩尔溶液沉积到经打印层上。所述溶液渗透所沉积材料的多孔基质。将外壳及打印床(打印托盘)两者中的溶液加热到95℃以允许所述溶液与所沉积层易于起反应以便使其固化。此固化步骤执行持续30分钟。反应完成率是70mol％，且相对密度从60％增加到91％。然后，通过DI水喷嘴清洗掉经密化层中的未反应锶及盐基离子，且接着在90℃下干燥其15分钟。在此之后，接着在上文过程之后沉积2mm的对象层。在另一实例中，在下一层沉积之前使用水中的1摩尔Sr(OH)2-8H2O溶液的额外循环进一步密化所述层。整个过程被重复59次以生产锥形单块体。
在又一实例中，以类似于实例2中所描述的过程的过程逐体元地打印具有20mm的长度、10mm的宽度及10mm的高度的立方体。将所述浆液挤压成具有5mm长x 5mm宽x2mm厚的拐角体元图案。加热打印机床以干燥经打印材料持续15分钟，在此之后，第二喷嘴以200μL/min的速率沉积3mL的前述Sr(OH)2-8H2O。在此实例中，在上文所描述的条件下允许所沉积的材料与所述溶液起反应持续15分钟，在此之后，清洗及干燥所沉积的材料持续另外15分钟。反应完成率为83mol％，且相对密度从60％增加到96％。挤压下一体元且所述循环重复39次以产生完全固化的立方体。
尽管前述内容涉及特定优选实施例，但应理解，本发明并非如此受限。所属领域中的一般技术人员将设想出，可对所揭示的实施例作出多种修改且此类修改意图在本发明的范围内。本文所列举的所有公开案、专利申请案及专利案以全文引用方式并入本文中。

Claims (23)

1.一种从多孔基质生产单块体的方法，其包括：
提供具有填隙空间且包括至少第一反应物的多孔基质的第一层；
使所述多孔基质的所述第一层与承载至少第二反应物的渗透介质接触；
允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述第一层的所述填隙空间的至少一部分以提供至少第一产物；
允许所述至少第一产物形成且填充所述多孔基质的所述第一层的所述填隙空间的至少一部分；
在所述多孔基质的所述第一层之上提供所述多孔基质的多个连续层；
使所述多孔基质的所述多个连续层与所述渗透介质接触；
允许所述渗透介质在促进所述至少第一反应物与所述至少第二反应物之间的反应的条件下渗透所述多孔基质的所述连续层的所述填隙空间的至少一部分以提供至少第一产物；以及
允许所述至少第一产物形成且填充所述多孔基质的所述第一层的所述填隙空间的至少一部分，由此生产单块体。
2.根据权利要求1所述的方法，其中使用所述渗透介质完全渗透整个所述多孔基质。
3.根据权利要求1所述的方法，其中所述多孔基质包括粘结剂材料。
4.根据权利要求1所述的方法，其中所述渗透介质与粘结剂起反应，从而导致所述粘结剂从所述多孔基质移除。
5.根据权利要求1所述的方法，其中所述方法包括增材制造工艺。
6.根据权利要求5所述的方法，其中所述增材制造工艺包括3D打印、立体光刻、熔融沉积成型、电子束无模制造、直接金属激光烧结、电子束熔化、选择性激光熔化、选择性热烧结、选择性激光烧结、分层实体制造及数字光处理、聚合材料喷射及粉末层喷墨打印。
7.根据权利要求5所述的方法，其中所述增材制造工艺包括基于石膏的3D打印。
8.根据权利要求1所述的方法，其中允许所述至少第一产物形成且填充所述多孔基质的所述层的所述填隙空间的至少一部分包括加热所述多孔基质的所述层。
9.根据权利要求8所述的方法，其中经由对流或辐射施加热量。
10.根据权利要求1所述的方法，其中所述多孔基质包括用于金属、陶瓷、陶瓷金属、聚合物或其复合物的前体。
11.根据权利要求1所述的方法，其中所述多孔基质是生坯。
12.根据权利要求1所述的方法，其中允许所述至少第一产物形成且填充所述多孔基质的所述层的所述填隙空间的至少一部分导致多孔基质的所述层基本上不收缩。
13.根据权利要求12所述的方法，其中所述收缩率小于2％。
14.根据权利要求13所述的方法，其中所述收缩率小于1％。
15.根据权利要求1所述的方法，其中所述多孔基质及所述渗透介质在低于500℃的温度下起反应。
16.根据权利要求15所述的方法，其中所述多孔基质及所述渗透介质在低于250℃的温度下起反应。
17.根据权利要求1所述的方法，其中所述渗透介质包括气体。
18.根据权利要求17所述的方法，其中所述气体包括CO2。
19.根据权利要求1所述的方法，其中所述多孔基质包括浆液。
20.根据权利要求19所述的方法，其中所述浆液包括水及/或酒精。
21.根据权利要求1所述的方法，其中使用打印头提供所述多孔基质的所述层。
22.根据权利要求1所述的方法，其中使用打印头提供所述渗透介质。
23.一种根据权利要求1到22中任一权利要求制成的产物。
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