CN116113534A - 用于生产结构的增材制造工艺 - Google Patents
用于生产结构的增材制造工艺 Download PDFInfo
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- CN116113534A CN116113534A CN202180056868.1A CN202180056868A CN116113534A CN 116113534 A CN116113534 A CN 116113534A CN 202180056868 A CN202180056868 A CN 202180056868A CN 116113534 A CN116113534 A CN 116113534A
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Abstract
本发明涉及一种用于通过增材制造技术来制造结构的方法,该增材制造技术实施由聚焦的能量辐射所辅助的化学气相沉积,该方法包括形成增强件,该增强件包括多个互连的陶瓷或碳的增强元件,这些增强元件一起限定间隙体积,该间隙体积具有沿所述沉积轴线的曲折形状。
Description
技术领域
本发明涉及增强件的制造,该增强件特别地用于通过增材制造技术,并且更具体地通过由聚焦的能量辐射所辅助的化学气相沉积,由陶瓷基质复合材料(CMC材料)制造的部件。
背景技术
已知由CMC材料制成的部件具有允许它们用于结构元件的良好机械特性以及在高温下保持这些特性的能力。CMC部件包括由耐火纤维(通常地,碳或陶瓷)制成的纤维增强件,其通过例如由碳化硅(SiC)制成的陶瓷基质致密。目前,陶瓷基质复合材料技术基本上基于编织的纤维增强件的使用。除了耐火纤维的高成本之外,编织操作也是昂贵的,并且在部件的几何形状方面可能存在限制,特别地对于具有小尺寸和复杂几何形状的部件,与编织的织物节距的不足有关。
增材制造技术也是已知的,这些技术允许制造金属或聚合物材料的部件,但这些技术目前对于耐火材料(如陶瓷)的沉积没有给出完全地令人满意的结果。
因此,期望具有允许制造具有复杂几何形状的结构,并且适于沉积多种耐火材料的方法。
发明内容
本发明涉及一种用于通过增材制造来制造结构的方法,该方法至少包括:
-通过由聚焦的能量辐射所辅助的化学气相沉积,形成增强件,所述增强件沿着沉积轴线沉积,并且包括由陶瓷或碳制成的多个互连的增强元件,所述多个互连的增强元件在它们之间限定间隙体积,所述间隙体积沿着所述沉积轴线具有曲折形状。
本发明提出一种增材制造方法,其中结构逐渐地被构建,并且包括至少一个增强件和可能的基质和界面,所述基质和界面随着增强件的形成而形成,如下文详述。增强件以及基质和界面(当存在时)各自由聚焦的能量辐射所辅助的化学气相沉积形成。所提出的增材制造技术一方面实施了化学气相沉积,其中,在由聚焦的能量辐射产生的局部和点状加热的作用下,存在一种或多种前体的转化,该聚焦的能量辐射允许根据前体的选择,沉积多种材料。另一方面,通过仅在期望材料沉积的区域的水平聚焦能量辐射,进行这种(这些)前体的局部加热,这允许接近增强件的复杂几何形状,并且特别地增强元件之间的间隙体积。因此,获得具有复杂形状的增强件,该增强件具有间隙体积,该间隙体积至少沿着沉积轴线具有曲折形状,也就是说,当沿着这个轴线移动时具有蜿蜒的和非直线的形状。增强件的复杂形状允许替换编织的织物,并且导致优化的增强特性。根据本发明的方法在不实施纤维编织操作以制造增强件的情况下和通过克服与这种技术相关联的限制,提供了可触及的形式的很大的多样性。
在一个示范性实施方式中,增强件为4D增强件。然而,本发明在增强件的几何形状方面不受限制。
根据一个变体,有可能对增强件提供另一种形状,例如,诸如蜂巢形状,该增强件的形状被适配成所期望的应用。
在一个示范性实施方式中,该方法包括通过由聚焦的能量辐射所辅助的化学气相沉积,增强件层沉积和基质沉积之间的交替,基质存在于所获得的增强件的间隙体积中。
在这种情况下,在形成增强件时沉积基质。由此,直接地获得由复合材料制成的部件,其具有致密增强元件之间的间隙体积的基质。
在一个示范性实施方式中,该方法至少包括:
-沉积增强件的第一层,
-将基质沉积在增强件的第一层的间隙体积中,以获得致密的增强件的第一层,以及
-将增强件的第二层沉积在致密的增强件的第一层上。
在这种情况下,基质沉积在预先沉积的增强件的层的间隙体积中。然而,在首先沉积基质,并且在先前沉积的基质周围沉积增强层的相反情况下,不脱离本发明的范围。
特别地,该方法还可以包括在沉积基质之前,在增强件的第一层的增强元件上形成界面,通过聚焦的能量辐射所辅助的化学气相沉积能够形成界面。
在这种情况下,当形成增强件和基质时,也执行界面的形成。
在一个示范性实施方式中,在位于必须执行沉积的区域附近的固体部分上,存在能量辐射的聚焦。
在这种情况下,能量辐射的焦点不在气相中,而是在固体部分上,该固体部分可以对应于在其上形成结构的基体或者对应于在其上旨在进行沉积的结构本身的一部分,也就是说对应于先前沉积的结构的一部分。在这种情况下,固体部分的加热将能量局部地传输到气态前体,以便转化它,并且获得沉积。与气相的直接加热相比,这样的特征允许改善对沉积位置的控制。这种特征进一步允许在冷壁反应器中工作,该冷壁反应器允许对气体压力和沉积温度具有更大的灵活性,同时避免在均相中成核的任何风险。这允许更容易地调节沉积动力学。
应该注意,在结构的形成期间,可以使用能量辐射在固体部分上和在气相中的聚焦的组合。作为变体,可以将能量辐射仅聚焦于固体部分上或仅聚焦于气相中。
在一个示范性实施方式中,聚焦的能量辐射是聚焦的激光束。
特别地,聚焦的激光束的波长可以包括在1,058nm与1,068nm之间,例如基本上等于1,063nm。
近红外中的这些波长值允许在将激光束聚焦于其上时,通过固体部分获得最大能量吸收。例如,在激光束聚焦在气相中的情况下,波长可以在UV或可见光区更低。
然而,本发明不限于使用激光作为能量辐射。作为变体,因此,可能使用聚焦的电子束。
因此,可能使用相同的气态前体,以形成整个增强件,或者当沉积增强件时改变气态前体。可以进一步改变在增强件的沉积与基质和可能的界面的沉积之间的气态前体。形成基质和可能的界面的材料可以不同于增强件的材料。例如,有可能在间隙体积中沉积碳化硅增强、高温碳或氮化硼界面和碳化硅基质。
举例而言,结构可以包括以下材料中的至少一种:碳化物陶瓷(例如碳化硅)、氮化物陶瓷、碳氮化物陶瓷、氧化物陶瓷(例如氧化铝)或共晶组份的陶瓷。特别地,增强件、基质和可能的界面可以彼此独立地包括选自上述列表的材料。
在一个示范性实施方式中,增强件是涡轮机部件的增强件。特别地,增强件可以构成涡轮机叶片、喷管或涡轮环扇段的增强件。增强件可构成飞行器涡轮机部件的增强件。
附图说明
图1示意性地和部分地表示在根据本发明的方法的实施例的框架内增强件的第一层的沉积。
图2示意性地和部分地表示基质在图1的增强件的第一层的间隙体积中的沉积。
图3示意性地和部分地表示在由图2的基质致密的第一层上增强件的第二层的沉积。
图4示意性地和部分地表示基质在图3的增强件的第二层的间隙体积中的沉积。
图5表示通过实施根据本发明的方法的实施例而获得的4D增强件。
图6表示通过实施根据本发明的方法的实施例而获得的涡轮机部件。
具体实施方式
关于图1至4,将描述通过由聚焦的能量辐射所辅助的化学气相沉积,逐层地沉积结构的可能实施例。出于可读性的原因,在图中已经放大了层的尺寸。在图示的实施例中,所制造的结构包括增强件和基质,该基质致密在其沉积时所形成的增强件。根据该实施例,通过在增强件层的沉积与基质的沉积之间交替,形成结构。根据未示出的一个变体,并且根据相同的原理,在增强件层的沉积之后,并且在基质的沉积之前,还可以在增强元件上形成界面。通过增材制造形成逐层的结构,结构的层对应于其沿着沉积轴线的区段,并且在所考虑的实施例中包括增强件、基质和可能存在的界面。
图1示出了通过由来自气态前体G11的聚焦的能量辐射所辅助的化学气相沉积,增强件的第一层10的形成。第一层10沉积在密封反应室C中存在的支撑件S上,例如与该支撑件S接触。
在开始沉积之前,清除反应室C中痕量的水和二氧。为此,可以进行气体(如氩气)的泵送和膨胀的多个循环。通过气体引入通道15,将气态前体G11引入反应室C中。本领域的技术人员知道如何根据待沉积的所期望的材料,从常规的化学气相沉积中已知的气态前体中选择气态前体。用于监测气态前体的注入和泵送的技术也是常识的一部分,并且不需要在此详述。例如,甲基三氯硅烷(CH3SiCl3或MTS)或单甲基硅烷(MMS)可以用于沉积碳化硅。丙烷和/或甲烷可以用于沉积碳。以类似于常规化学气相沉积技术中可实施的方式,可以在互补中性或反应气体中稀释气态前体。因此,有可能将氢和/或氮添加到前体中。
通过聚焦的能量辐射E11,气态前体G11经受局部加热,以便沉积具有期望几何形状的增强件的第一层10。沉积的第一层10包括多个互连的增强元件22,这些增强元件在它们之间限定了具有预定的和监测的形状的间隙体积V,以下将关于图5,详述增强件的几何形状的实施例。为了实现所期望的几何形状,能量辐射E11被连续地聚焦在期望沉积的区域中,以便局部地提供热量,并且局部地转化气态前体G11。如上所述,能量辐射E11的焦点可以位于固体部分的水平,例如支撑件S的水平或先前进行的沉积的部分的水平,以便引起其加热,并且引起附近的前体G11的转化,并且因此进行材料的沉积。根据非优选的变体,能量辐射E11的焦点可以直接地位于气态前体G11中。
在所示出的实施例中,能量辐射E11来自激光器。根据该实施例所示出的系统包括辐射装置D,该辐射装置包括激光源30、准直器33、允许在该方法期间对激光束进行定向的光学扫描仪35以及聚焦装置34(如透镜),该聚焦装置使之有可能在必须进行沉积的区域中聚焦激光束。激光源可以是具有包括在1,058nm与1,068nm之间的波长的红外线源,例如可纤维化光电二极管Yb类型的源。作为变体,激光的波长在紫外线或在可见光内,特别是在气相的直接加热的情况下。激光源30可以优选地以连续模式操作,或者如果期望避免提供太多表面功率,则以不连续模式操作。然而,如果使用除了激光之外的能量源,诸如电子束,则不脱离本发明的范围。在所设想的不同情况下,以本领域技术人员已知的方式,通过使用光学或电磁聚焦装置进行热源的聚焦。无论所使用的能量辐射的性质如何,聚焦的能量辐射的功率可以包括在1mW与100W之间、优选地在20mW与5W之间。
可以移动聚焦的能量辐射E11,以便通过修改光学扫描仪35的位置和/或倾斜度,进行具有所期望的几何形状的第一增强件层10的沉积。用于监测辐射的装置(未示出)允许监测能量辐射E11的运动。因此,这允许通过聚焦的能量辐射E11在必须进行第一层10的构成材料的沉积的预定区域中进行扫描。用于移动聚焦的能量辐射的装置类似于选择性激光成型(SLM)技术中所使用的装置。将注意的是,除了或代替移动聚焦的能量辐射E11,可以在沉积期间移动和/或倾斜支撑件S。支撑件监测装置(未示出)允许实现这种移动或这种倾斜。因此,支撑件S可以在空间中沿着至少一个方向移动,例如并且优选地,沿着垂直方向Z移动,或者甚至在空间中沿着三个方向移动。作为变体或组合,支撑件S可以围绕空间中的至少一个方向倾斜,或者甚至围绕每个方向倾斜。然而,如果支撑件S保持固定,并且仅通过在多个预定区域中移动聚焦的能量辐射E11,获得第一层10的沉积,则不脱离本发明的范围。
作为指示,在结构的形成期间反应室C中的压力可以包括在5mbar与3bar之间,例如在5mbar与15mbar之间,或者在1bar与3bar之间。反应室C可包括压力传感器(未示出)以及泵送装置P,以便在沉积结构时分别地测量和调节反应室C中的压力。反应室C包括气体出口通道17,残留的气态前体GR11和反应副产物通过该气体出口通道17被泵出反应室。如果期望,有可能使用分离器装置(如色谱系统),将前体分离,并且再注入到室C中和排除副产物。本领域的技术人员根据所使用的前体的性质,确定反应室C中的压力和所实施的能量辐射的表面功率,以便适配沉积动力学。反应室C可以进一步包括热传感器(未示出),例如热相机,以便测量在能量辐射的焦点处的局部温度,以及调节装置,该调节装置允许根据来自热传感器的测量,修改聚焦的能量辐射的功率,以便施加所期望的预定功率来转化前体和进行沉积。
刚刚关于图1已经描述了增强件的第一层10的沉积。在所考虑的实施例中,增强件的沉积被暂时中断,以便在先前形成的第一层10的间隙体积中形成基质M,如现在将关于图2描述的。
一旦已经沉积增强件的第一层10,就中断由聚焦的能量辐射E11的辐射,并且清洗反应室C。然后,将气态前体G12引入反应室C中,该气态前体旨在通过由聚焦的能量辐射所辅助的化学气相沉积,在第一层10的间隙体积中形成基质M。前体G12可以不同于前体G11,并且导致由与增强件的第一层10的材料不同的材料形成的基质M的沉积。为了在期望的区域中进行基质M的沉积,以与以上已经刚刚针对第一层10描述的方式类似的方式,驱动能量辐射E12和/或支撑体S。能量辐射E12的表面功率可以通过适配于前体G12而不同于能量辐射E11的表面功率。反应室中压力的监测以及残留的基质前体GR12和副产物的混合物的处理可以如上述沉积第一层10的情况。
基质M可以包括或主要由碳化物、氮化物或氧化物陶瓷的质量组成。例如,基质可以包括碳化硅或者主要地由碳化硅的质量构成。
在未示出的一个变体中,脆化释放界面相似地在形成基质之前,通过由聚焦的能量辐射所辅助的化学气相沉积而沉积在增强件的第一层的增强元件上。界面可以是单层的或多层的。该界面可包括例如,碳化硅、氮化硼、掺杂有硅或高温碳PyC的氮化硼BN(Si)。界面具有复合材料的脆化释放的功能,其促进已经在基质中传播之后到达界面的任何裂纹的偏转,防止或延迟增强件的破裂。
在基质M在增强件的第一层10的间隙体积中沉积之后,通过在由基质M致密的第一层10上沉积陶瓷或碳增强件的第二层20,再继续增强件的沉积,如图3所示。
中断由聚焦的能量辐射E12进行的辐射,并且清洗反应室C。然后,将气态前体G21引入到反应室C中,该气态前体G21旨在通过由聚焦的能量辐射所辅助的化学气相沉积,形成增强件的第二层20。施加聚焦的能量辐射E21,以便在第一层10上以期望的几何形状沉积增强件的第二层20,类似于上文所述。上述用于沉积第一层10的特性保持适用于沉积第二层20。应注意,前体G21可以与前体G11相同或不同。增强件的第二层20的材料可以与增强件的第一层10的材料相同或不同。优选地,增强件的第二层20的材料与增强件的第一层10的材料相同。能量辐射E21的表面功率可以与能量辐射E11的表面功率相同或不同。可以如以上对第一层10的沉积的情况所描述的,监测反应室中的压力以及处理残留的前体GR21和副产物的混合物。
在第二层20的沉积期间,能量辐射E21可以扫描一组区域,该一组区域相对于在第一层10的沉积期间由能量辐射E11所扫描的一组区域所限定的模式,限定不同的模式。在此,第二层20沿着由垂直方向Z所实现的沉积轴线,叠置在第一层10上。第二层20可以与第一层10接触沉积。第二层20可以基本上覆盖整个第一层10,或者仅覆盖其一部分。第二层20包括由陶瓷或碳制成的多个互连的增强元件,这些增强元件在它们之间限定间隙体积,该间隙体积具有与第一层10的增强元件之间的间隙体积的形状不同的形状,以便沿着沉积轴线Z为增强件1的间隙体积提供曲折的形状。第二层20的间隙体积的形状可以基本上不同于第一层10的间隙体积的形状,以便对应于增强件的期望定向。
一旦已经沉积增强件的第二层20,则中断由聚焦的能量辐射E21进行的辐射,并且清洗反应室C。然后,将气态前体G22引入到反应室C中,该气态前体G22旨在通过聚焦的能量辐射所辅助的化学气相沉积,在第二层20的间隙体积中形成基质M(图4)。然后如上所述,继续该方法,以通过驱动聚焦的能量辐射E22和/或支撑体S,将基质M沉积在该第二层20的间隙体积中,而将基质M沉积在所期望的区域中。可以如上所述,处理残留的前体GR22和副产物的混合物。如上所述,界面可以在基质M沉积之前,沉积在第二层20的增强元件上。
然后,获得复合材料结构100,其包括增强件1和致密增强件的基质M。该结构中的增强件体积比可以包括在15%与55%之间,例如在25%与35%之间。该增强件是受控的,并且该增强件根据待获得的部件的负载方向在空间中被定向。
所示例的实施例示出了结构100的制造,在该结构中沉积了增强件的两个层10和20。当然,该方法可以通过以类似的方式在第二层20上沉积增强件的第三层来继续。每个沉积层的间隙体积可具有不同的形状,以使增强件的间隙体积具有曲折形状。
刚刚描述了实施例,其中存在在形成增强件时形成基质的结构的形成。然而,该基质的形成是可选的,增强件能够简单地逐层地形成,而不以伴随的方式形成基质,或者简单地通过在形成增强件时形成界面。根据变体,可以在通过已知技术形成增强件之后形成基质和/或界面。
现在将关于图5描述可以通过实施本发明获得的增强件1的几何形状的实施例。图5所示的增强件1对应于4D增强件。增强件1包括多个增强元件22,所述多个增强元件22沿由立方体的对角线给出的四个方向定向,并且在其间限定间隙体积V,所述间隙体积V具有沿沉积的垂直方向Z的曲折形状。增强元件22可具有各种形状,诸如平行六面体、具有例如圆形、椭圆形、正方形或矩形截面的梁、球体、椭圆体等。增强元件22可以是实心的或空心的。增强元件22的直径可以小于或等于100μm。增强元件22可进一步布置成网络,以形成增强件。无论所考虑的实施方式如何,增强件1具有连接的间隙体积,也就是说,存在允许从增强元件22之间的一个空间移动到另一个空间而不穿过增强元件的材料的路径。间隙体积由陶瓷或碳材料的内表面界定。当连接间隙体积时,陶瓷或碳材料的该内表面在结构中是连续的。本领域技术人员将毫无困难地认识到除了4D增强结构之外的结构是可能的。
图6示例了可以通过实施根据本发明的方法获得的部件的实施例。本发明可以允许形成涡轮机部件,例如航空涡轮机部件。如图6所示,有可能形成涡轮机叶片40。其他实施例是可能的,例如,诸如涡轮环区段或涡轮喷管区段。
表述“包括在……与……之间”必须被理解为包括界限。
Claims (10)
1.一种用于通过增材制造来制造结构(100)的方法,该方法至少包括:
-通过由聚焦的能量辐射所辅助的化学气相沉积,形成增强件(1),所述增强件沿着沉积轴线(Z)沉积,并且包括由陶瓷或碳制成的多个互连的增强元件(22),所述增强元件在它们之间限定间隙体积(V),所述间隙体积沿着所述沉积轴线具有曲折形状。
2.根据权利要求1所述的方法,其中,所述增强件(1)为4D增强件。
3.根据权利要求1或2所述的方法,其中,所述方法包括通过由聚焦的能量辐射所辅助的化学气相沉积,在所述增强件的层沉积与基质(M)沉积之间的交替,所述基质存在于所获得的增强件的间隙体积中。
4.根据权利要求3所述的方法,其中所述方法至少包括:
-沉积增强件的第一层(10),
-在增强件的第一层的间隙体积(V)中沉积基质(M),以获得致密的增强件的第一层,以及
-将增强件的第二层(20)沉积在致密的增强件的第一层上。
5.根据权利要求4所述的方法,其中,所述方法还包括在沉积基质(M)之前,在增强件的第一层(10)的增强元件(22)上形成界面,由聚焦的能量辐射所辅助的化学气相沉积形成所述界面。
6.根据权利要求1至5中任一项所述的方法,其中,在位于必须执行沉积的区域附近的固体部分(S;10;20)上,存在能量辐射(E11;E12;E21;E22)。
7.根据权利要求1至6中任一项所述的方法,其中,所述聚焦的能量辐射(E11;E12;E21;E22)是聚焦的激光束。
8.根据权利要求7所述的方法,其中,所述聚焦的激光束的波长包括在1,058nm与1,068nm之间。
9.根据权利要求1至8中任一项所述的方法,其中所述结构(100)包括以下材料中的至少一种:碳化物陶瓷、氮化物陶瓷、碳氮化物陶瓷、氧化物陶瓷或共晶组份的陶瓷。
10.根据权利要求1至9中任一项所述的方法,其中,所述增强件(1)是涡轮机部件(40)的增强件。
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US20060223312A1 (en) * | 2005-03-31 | 2006-10-05 | Battelle Memorial Institute | Method and apparatus for selective deposition of materials to surfaces and substrates |
US20140328964A1 (en) * | 2013-03-22 | 2014-11-06 | Markforged, Inc. | Three dimensional printing |
CN106390198A (zh) * | 2016-09-19 | 2017-02-15 | 西安交通大学 | 一种选区激光成形及电解还原制备个性化多孔植入物方法 |
CN106862563A (zh) * | 2015-12-10 | 2017-06-20 | 佳能株式会社 | 用于产生粉末的方法和装置以及用于制造成形物体的方法 |
US20170361600A1 (en) * | 2016-06-21 | 2017-12-21 | Washington State University | Additive manufacturing of composite materials with composition gradient |
FR3057864A1 (fr) * | 2016-10-25 | 2018-04-27 | Safran Ceram | Procede d'infiltration ou de depot chimique en phase vapeur mettant en oeuvre le precurseur ci2bnh2 pour former du nitrure de bore |
US20180148864A1 (en) * | 2016-11-29 | 2018-05-31 | Free Form Fibers, Llc | Fiber with elemental additive(s) and method of making |
CN108698126A (zh) * | 2015-12-10 | 2018-10-23 | 维洛3D公司 | 精湛的三维打印 |
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EP4034061A4 (en) * | 2019-09-25 | 2023-10-18 | Free Form Fibers, LLC | NON-WOVEN FABRICS IN MICRO-MATTS AND COMPOSITE OR HYBRID MATERIALS AND COMPOSITES REINFORCED THEREWITH |
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2020
- 2020-08-06 FR FR2008320A patent/FR3113286B1/fr active Active
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2021
- 2021-07-09 WO PCT/FR2021/051281 patent/WO2022029377A1/fr active Application Filing
- 2021-07-09 CN CN202180056868.1A patent/CN116113534A/zh active Pending
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Patent Citations (9)
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JPS63278835A (ja) * | 1987-05-11 | 1988-11-16 | Nippon Steel Corp | セラミックス積層体の製造方法 |
US20060223312A1 (en) * | 2005-03-31 | 2006-10-05 | Battelle Memorial Institute | Method and apparatus for selective deposition of materials to surfaces and substrates |
US20140328964A1 (en) * | 2013-03-22 | 2014-11-06 | Markforged, Inc. | Three dimensional printing |
CN106862563A (zh) * | 2015-12-10 | 2017-06-20 | 佳能株式会社 | 用于产生粉末的方法和装置以及用于制造成形物体的方法 |
CN108698126A (zh) * | 2015-12-10 | 2018-10-23 | 维洛3D公司 | 精湛的三维打印 |
US20170361600A1 (en) * | 2016-06-21 | 2017-12-21 | Washington State University | Additive manufacturing of composite materials with composition gradient |
CN106390198A (zh) * | 2016-09-19 | 2017-02-15 | 西安交通大学 | 一种选区激光成形及电解还原制备个性化多孔植入物方法 |
FR3057864A1 (fr) * | 2016-10-25 | 2018-04-27 | Safran Ceram | Procede d'infiltration ou de depot chimique en phase vapeur mettant en oeuvre le precurseur ci2bnh2 pour former du nitrure de bore |
US20180148864A1 (en) * | 2016-11-29 | 2018-05-31 | Free Form Fibers, Llc | Fiber with elemental additive(s) and method of making |
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EP4192690A1 (fr) | 2023-06-14 |
WO2022029377A1 (fr) | 2022-02-10 |
FR3113286B1 (fr) | 2023-02-10 |
FR3113286A1 (fr) | 2022-02-11 |
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