CN112789128A - 从预制件开始通过加压烧结制造复杂形状的部件的方法 - Google Patents

从预制件开始通过加压烧结制造复杂形状的部件的方法 Download PDF

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CN112789128A
CN112789128A CN201980064433.4A CN201980064433A CN112789128A CN 112789128 A CN112789128 A CN 112789128A CN 201980064433 A CN201980064433 A CN 201980064433A CN 112789128 A CN112789128 A CN 112789128A
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mould
preform
manufacturing
porous
sintering
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CN112789128B (zh
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亚尼克·贝内特
罗曼·埃费尔
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Norimat SAS
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Abstract

本发明涉及一种通过根据3D增材打印和加压烧结技术连续沉积层来制造复杂形状的部件(3)的方法，包括以下步骤：从基于金属合金、陶瓷、复合材料及损耗材料的多孔或粉末状材料中选择的一材料，通过根据数字控制的3D增材打印技术形成连续的沉积层来生产一模型(1)的一初始步骤，接着将由多孔或粉末状的待致密化材料所制成、从所述模型(1)所导出的一预制件(1)引入至一模具(2)中的步骤，所述模具(2)除了所述预制件(1)外还填充有牺牲多孔或粉末状的材料(13)，然后对所述模具(2)施加单轴致密加压烧结(10)从而形成所述部件(3)，所述部件(3)最终是从所述模具(2)中所提取出。

Description

从预制件开始通过加压烧结制造复杂形状的部件的方法
技术领域
本发明涉及一种从通过增材技术所生产的预制件开始通过加压烧结制造复杂形状的部件的方法。
本发明涉及通过致密化多孔或粉末状材料来制造部件，特别是工业机械部件的领域。本领域涵盖通过在单轴或多轴的等静负载(isostatic load)下的烧结(例如，热的、特别是等静的、加压的、高压火花烧结(称为火花等离子体烧结(spark plasma sintering，SPS))、或是选择性激光烧结)的各种致密化技术。
更具体地说，SPS烧结技术包括将一定体积的陶瓷、聚合物或金属粉末固结(consolidating)在导电模具中，从而快速获得微观结构良好的致密材料。这种固结是通过同时施加一个载荷(在施加在模具上的高单轴压力下，例如100MPa的压力和由模具中的高强度脉冲直流电提供的500至10000A的加热来实现的，粉末的完全烧结只需几分钟完成。
这种SPS烧结技术的主要优点是，考虑到高温下的高升温速率和相对较短的停留时间，材料的致密化不会伴随或伴随很少的晶体生长。
背景技术
SPS烧结技术施加的单轴加压具有导致致密化异质性(heterogeneity)的缺点，特别是针对在厚度上有很大差异的复杂形状的部件，其导致了相对于有限的空间和时间在不同厚度的区域之间去除材料的不均匀性。一般来说，复杂形状是指具有或不具有厚度变化的可变曲率、或是具有或不具有曲率变化且具有较大的厚度变化、及/或具有几何断裂的形状。
为了克服致密化不均匀(inhomogeneity)的缺点，专利文件FR 3042992提供在粉末状(或多孔)材料以及用于生产部件所定制的模具的反模板(counterform)面之间添加可变形的界面层。
然而，烧结技术也存在一个问题，当部件具有复杂形状时，模具或模具反模板的使用不容易使部件从模具中移走，特别是形成难以接近的咬边，因此，锥形很难在不部分地破坏部件下从模具中移开。
反模板可以是通过压制由粘合剂聚集(agglomerated)的陶瓷粉末层或通过将陶瓷粉末粘合在聚合物预制件上所获得的印刷件，惰性(inert)界面覆盖于反模板。由于复杂形状的咬边问题以及需要界面覆盖的这些反模板的表面状态问题，这些技术在可接近的几何形状方面有很大的局限性。
为了生产与可从模具上移除的咬边相兼容的反模板，有必要倍增反模板的数量，以便避免从模具上移开的问题。然后，为每个反模板所定制的工具需要被制造，导致了额外的设计和加工步骤。这许多反模板的组装也是缺陷的一个来源(最终部件的不匹配几何形状、初始裂纹、材料损失等)。
为了通过致密化材料来生产复杂形状的部件，使用多轴等静加载技术(称为热等静压(hot isostatic pressing，HIP)也是众所周知的做法。此技术例如在文件WO 2016/189312中说明，所述文件提供了使用填充有完全围绕目标的外皮的压力传递材料且通过增材打印技术所预制的致密化炉，以便具有不同密度的外皮和内部体积。这种方法实现了大尺寸、复杂和耗时的手段，特别是在HIP技术的背景下。
替代地，文件WO 2016/030654的模具涉及通过HIP技术来生产组件，所述模具使用陶瓷围绕组件的牺牲模型来生产。模型被移开而形成空腔，在陶瓷上涂上金属层以构成模具，所述模具中填充有金属粉末，然后放入HIP技术容器中。这个解决方案仍然很复杂，并且实施HIP技术。
发明内容
本发明旨在克服此问题，为此，本发明提供了使用通过数字控制的增材技术结合单轴致密化的方式所生产的部件的预制件。
更具体地说，本发明的主旨是根据3D增材打印和加压烧结技术，通过连续沉积层来制造复杂形状的部件的方法，所述方法包括以下步骤：从基于金属合金、陶瓷、复合材料及损耗材料的多孔或粉末状材料中选择的材料，通过根据数字控制的三维(3D)增材打印技术形成连续的沉积层来生产模型的初始步骤，接着将由多孔或粉末状的待致密化材料所制成、从所述模型所导出的预制件引入至模具中的步骤，所述模具除了所述预制件外还填充有牺牲多孔或粉末状的材料，然后对所述模具施加单轴致密加压烧结从而形成所述部件，所述部件最终是从所述模具中所提取。
特别地，所述3D增材打印技术选自立体光刻(stereolithography)、粘合剂喷射(binder jetting)、可控挤出(controlled extrusion)、熔融沉积成型(fused filamentfabrication)、喷墨打印(inkjet printing)以及气溶胶喷射打印(aerosol jetprinting)。
此外，单轴致密化允许相对于HIP类型的三维等静压致密化简化的致密化，同时能够获得物理化学均匀性(physico-chemical homogeneity)和零件尺寸精度的特征。
根据一些有利特征：
-牺牲材料是选自陶瓷、二氧化硅、金属硅酸盐和复合材料的材料；
-陶瓷可选自粉末化的钇稳定氧化锆(yttria-stabilized zirconia，YSZ)、氧化铝增韧氧化锆(alumina-toughened zirconia，ATZ)、氧化锆增韧氧化铝(zirconia-toughened alumina，ZTA)和氧化铝，所述陶瓷表现出40％到80％的致密化程度。
-在预制件被包括在模具中之前，可以在预制件的至少一个表面上设置界面层，以便防止预制件和牺牲材料之间的任何相互作用；
-在烧结开始温度和结束温度下，预制件、界面层和牺牲材料的材料表现出相同的致密化行为。
从预制件上去除粘合剂的步骤可以有利地在3D增材打印输出时通过在200与600℃温度之间及以介于0.1与1℃/分之间的升温速率的热处理来执行。此步骤可以去除在反模板生产期间所引入至材料中的有机化合物。
此外，去除粘合剂的步骤可随后进行预烧结的步骤，所述步骤包括在更高温度下(介于600℃与1500℃之间，取决于反模板的材料)对反模板进行热处理，此步骤可使反模板得以开始致密化，赋予它机械强度并且促进界面的施加。
根据第一实现方式，模型在致密化之前直接提供预制件，并且在引入预制件之前和之后模具用粉末状或多孔的牺牲材料填充模具。
根据另一个实现方式，所述方法提供了通过增材打印的方式从损耗材料(例如从具有低熔点的蜡或树脂)生产模型，然后在所述模型周围形成由多孔或粉末状材料所制成的反模板。去除损耗材料，然后用待致密化的材料填充反模板，所述待致密化的材料构成与模型相对应的预制件，然后将反模板引入至加压烧结模具中，将牺牲材料添加到模具中。施加加压烧结后，部件从反模板中提取出。
在附图中，相同的组件由相同的参考符号所标识，所述参考符号指的是叙述内容中的一个或多个段落所提及的。
附图说明
通过阅读以下参考附图给出的非限制性描述，本发明的进一步信息、特征和优点将变得显而易见，附图分别示出：
-图1，根据从预制件制造复杂形状部件的第一实施例的方法的一个示例性实现方式的主要步骤(1A到1F)的透视图；以及
-图2，根据从预制件制造复杂形状部件的第二实施例的方法的一个简化示例性实现方式的主要步骤(2A到2G)的截面示意图。
具体实施方式
根据本发明的用于制造复杂形状部件的方法的一个示例的主要步骤1A到1f在图1中通过截面视图所示出。在步骤1A中，将待制造的部件的多孔金属模型1通过根据3D增材打印技术(在本示例中为粘合剂喷射(binder jetting))在连续层中喷射而形成。所述模型复制了预先存储在喷射系统(未示出)的控制单元中的一配置，并构成烧结后待获得的部件的预制件。此预制件定义了根据本发明的制造方法中待制造的部件的形状的几何形状。
部件的材料最初是基于金属合金的粉末状或多孔材料的形式，在所示出的示例中，特别是基于钛合金、钛铝合金，例如不锈钢或是René族的镍基超合金(nickel-basedsuperalloy)。
有利的是，从以模型1的形式的预制件中去除粘合剂是通过在200与600℃之间(在示例中为400℃)的温度下以介于0.1与1℃/分之间(在示例中为0.5℃/分)的升温速率的热处理来实现。此步骤使得在用于生产反模板(counterform)部分的3D打印期间可能引入至陶瓷粉末中的有机化合物得以去除。
优选地，在去除粘合剂之后还进行了预烧结。此预烧结包括在更高的温度下处理预制件1，例如在600℃和1500℃之间，取决于所用材料，在示例中为1200℃。此热处理使得反模板部分的致密化得以开始，以便赋予它们机械强度并从而促进一个或多个界面层的施加，如下所述。
在步骤1B中，石墨界面层11通过喷涂有利地均匀沉积在预制件1的外表面1e(参见步骤1C)或内表面1i(参见步骤1A)上。或者，石墨层被喷涂在预制件1的两面1i、1e上。石墨层11能够防止在模型1以及牺牲粉末材料(示例中为陶瓷)之间的任何相互作用，所述牺牲粉末材料将在稍后沉积以便于最终从模具中去除。
参照步骤1C，覆盖有石墨层11的预制件1被引入SPS加压烧结模具2中且位于预先被引入的陶瓷粉末的牺牲材料层上(不可见)。接下来，牺牲粉末13还被引入至模具2中，使得此模具2填充有待致密化的材料的组件(步骤1C)。牺牲粉末能够补偿随后烧结过程中致密化的差异。
然后，对模具2施加SPS烧结(50MPa的负载10，3000A的直流强度，这导致此模具2中所包含的材料组件的致密化(步骤1E)。然后，通过拆模并移除围绕部件3的牺牲材料13的部分将致密化的部件3从模具2中移开(步骤1F)。
根据另一个实施例，如图2步骤2A到2G的示意图所示，脱蜡(lost-wax)模型4首先通过立体光刻(步骤2A)进行打印。示例中的模型是锥形的。
然后，以示例所示的滑动(slip)形式在蜡4周围施加锥形反模板5(步骤2B)。交替地，形成反模板的多孔材料可以是陶瓷、二氧化硅、金属硅酸盐、复合材料等。
然后，蜡4通过使蜡液化的适当加热方式从反模板5上去除。液体通过一个开口51逸出(箭头F1)，所述开口51形成在反模板锥5的底部，因此被完全排空(步骤2C)。
有利的是，反模板5在其内表面5i上覆盖有石墨界面层7，以便于从模具中去除以及防止反模板与待致密材料之间的任何相互作用。或者，石墨层被喷涂在反模板5的至少一个面5i、5e上。
参照步骤2D，对反模板5填充待致密化的粉末状材料，所述待致密化的粉末状材料构成了待制造部件的预制件6并对应于蜡模型。然后，反模板5的内表面5i的石墨层7覆盖预制件6。
然后，有利地，在上述的温度和升温速率条件下实施去除粘合剂和预烧结的步骤。
然后，反模板5和预制件6被引入SPS烧结模具2中(步骤2E)，且牺牲材料9被附加地引入模具2中。在所示的示例中，牺牲材料是从选自陶瓷、二氧化硅、金属硅酸盐、复合材料等的材料。
通过施加负载10和3000A的直流电来实现SPS致密化(步骤2F)。牺牲粉末能够补偿烧结过程中致密化的差异。
然后，通过脱模、移除牺牲材料9和反模板5(步骤2G)从模具2中取出部件8。
本发明不限于所描述和示出的示例。因此，界面层可由除了石墨以外的多孔或粉末状材料所形成，尤其是氧化钇、氮化硼等。
第一种实现方式特别适用于具有相对凸面和凹面的中空部件，第二种实现方式适用于实心双凸部件。
无论哪种实现方式，牺牲材料、反模板、预制件以及界面层的材料在烧结开始温度和结束温度方面表现出相似的行为。所使用的陶瓷是以钇稳定氧化锆(yttria-stabilizedzirconia，YSZ)、氧化铝增韧氧化锆(alumina-toughened zirconia，ATZ)、氧化锆增韧氧化铝(zirconia-toughened alumina，ZTA)和氧化铝为基础的粉末形式，所述陶瓷表现出40％到80％的致密化程度。
此外，界面层可采用以下形式施加：喷雾、通过与粉末相对应的粘合剂(水溶液、
Figure BDA0002998970280000071
溶液等)结合的粉末沉积、适当形状的片材等。
此外，在第一实施例中，预制件直接是所述示例中的模型。一般来说，预制件也可以通过另一种3D增材打印技术及/或通过使用另一种材料从基础模型所导出，这使得可以根据待制造的部件的材料的选择来改变打印技术和打印材料。

Claims (15)

1.一种根据3D增材打印和加压烧结的技术通过连续沉积层来制造复杂形状的一部件(3；8)的方法，其特征在于，所述方法包括以下步骤：从基于金属合金、陶瓷、复合材料及损耗材料的多孔或粉末状材料中选择的一材料，通过根据数字控制的3D增材打印技术形成连续的沉积层来生产一模型(1；4)的一初始步骤，接着将由多孔或粉末状的材料所制成、从所述模型(1；4)所导出且待致密化的一预制件(1；6)引入至一模具(2)中的步骤，所述模具(2)除了所述预制件(1；6)外还填充有牺牲多孔或粉末状的材料(13；9)，然后对所述模具(2)施加单轴致密加压烧结(10)从而形成所述部件(3；8)，所述部件(3；8)最终是从所述模具(2)中所提取出。
2.如权利要求1所述的制造方法，其特征在于，所述3D增材打印技术选自立体光刻、粘合剂喷射、可控挤出、熔融沉积成型、喷墨打印以及气溶胶喷射打印。
3.如前述任一权利要求所述的制造方法，其特征在于，在所述预制件被包括在所述模具(2)中之前，在所述预制件的至少一个面(1i、1e；5i、5e)上设置一界面层(11；7)。
4.如前一权利要求所述的制造方法，其特征在于，所述预制件、所述界面层以及所述牺牲材料的材料在烧结开始温度和结束温度下表现出相同的致密化行为。
5.如前述任一权利要求所述的制造方法，其特征在于，所述牺牲材料(13；9)是选自陶瓷、二氧化硅、金属硅酸盐以及复合材料的材料。
6.如前一权利要求所述的制造方法，其特征在于，所述陶瓷选自YSZ、ATZ、ZTA以及氧化铝粉末，所述陶瓷表现出的致密程度可在40％到80％之间。
7.如权利要求3和4中任一权利要求所述的制造方法，其特征在于，所述界面由选自石墨、氧化钇和氮化硼的一材料层所形成。
8.如权利要求3和4中任一权利要求所述的的制造方法，其特征在于，所述界面层(11；7)是以选自喷雾、粉末沉积以及适当形状的片材的一形式所施加。
9.如前述任一权利要求所述的制造方法，其特征在于，待制造的所述部件的所述金属合金是选自钛合金、不锈钢以及René族中的镍基超合金。
10.如前述任一权利要求所述的制造方法，其特征在于，在3D增材打印输出时通过在200与600℃温度之间及以介于0.1与1℃/分之间的升温速率的热处理执行从所述预制件(1；6)中去除粘合剂的一步骤。
11.如前一权利要求所述的制造方法，其特征在于，在去除粘合剂的步骤之后，接着通过对所述预制件(1；6)进行在600与1500℃之间的热处理的预烧结的一步骤。
12.如前述任一权利要求所述的制造方法，其特征在于，由多孔或粉末状的材料所制成的所述模型(1)在致密化之前构成所述预制件，并且其特征在于，在引入所述预制件(1)之前和之后，所述模具(2)填充有粉末状或多孔的牺牲材料(13)。
13.如权利要求1至11中任一权利要求所述的制造方法，其特征在于，所述模型(4)是通过增材打印从损耗材料中所生产的，并且在所述模型(4)周围形成由多孔或粉末状的材料所制成的一反模板(5)，其特征在于，所述损耗材料被去除后，在引入所述反模板(5)至所述加压烧结模具(2)之前，用构成相对应所述模型(4)的所述预制件(6)的待致密材料填充所述反模板(5)，其特征在于，所述牺牲材料(9)被添加至所述模具(2)，以及其特征在于，在施加加压烧结(10)后，从所述反模板(5)中提取所述部件(8)。
14.如前一权利要求所述的制造方法，其特征在于，反模板(5)的材料选自陶瓷、二氧化硅、金属硅酸盐以及复合材料，同时在烧结开始温度和结束温度下表现出与所述预制件(1；6)、所述牺牲材料(13；9)以及所述界面层(7)的材料相同的致密化行为。
15.如前一权利要求所述的制造方法，其特征在于，所述陶瓷选自粉末化的YSZ、ATZ、ZTA以及氧化铝，所述陶瓷表现出的致密程度可在40％至80％之间。
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