CN105408288A - 通过低熔点浸渍制造复合部件的方法 - Google Patents

通过低熔点浸渍制造复合部件的方法 Download PDF

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Publication number
CN105408288A
CN105408288A CN201480041907.0A CN201480041907A CN105408288A CN 105408288 A CN105408288 A CN 105408288A CN 201480041907 A CN201480041907 A CN 201480041907A CN 105408288 A CN105408288 A CN 105408288A
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fiber
carbon
preformed member
silicon
boron
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埃里克·菲利普
埃里克·布永
埃米莉·科尔科特
塞巴斯蒂安·希门尼斯
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Safran Ceramics SA
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SNPE Materiaux Energetiques SA
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Abstract

本发明提供一种制造复合部件的方法，该方法包括以下步骤：·制造加强的纤维预成型件，所述预成型件的纤维是碳或陶瓷纤维，并且被涂覆有界面；·获得加强的和部分致密的纤维预成型件，部分致密化包括在所述界面上形成通过化学气相渗透所获得的第一基质相；和·通过渗入渗透组合物继续致密所述纤维预成型件，所述渗透组合物包含至少硅和至少一种其他适于降低该渗透组合物的熔融温度至低于或等于1150℃的元素。

Description

通过低熔点浸渍制造复合部件的方法
背景技术
本发明涉及当制造具有陶瓷基质或至少部分为陶瓷的基质的复合材料部件时，以及当制造由碳/碳(C/C)复合材料制成的部件时两种情形所用渗透组合物，该具有陶瓷基质或至少部分为陶瓷的基质的复合材料以下称为陶瓷基质复合(CMC)材料。
本发明的应用领域涉及制造曝露在高温下作业的部件，特别是航空航天领域，特别是用于航空发动机的热部件，可以理解为，本发明可以被应用到其他领域，如工业燃气涡轮机领域。
CMC和C/C复合材料具有良好的热结构性能，即：使得所述材料适于构成结构部件的强机械性能，以及在高温下保存那些性能的能力。
使用代替金属的CMC或C/C材料制造在高温下作业的部件，已经因此被推荐，尤其因为CMC和C/C材料比它们所代替的金属材料具有明显更低的密度。
制造CMC材料部件的公知方法包括自碳纤维或碳化硅(SiC)纤维的纤维层制造预成型件，以及用基于熔融硅的组合物渗透该预成型件，以形成陶瓷基质。这样的致密化过程被称为熔渗(MI)。例如，可以参考下述文献：US4889686，US4944904或US5015540。该渗透组合物主要以硅为基础，因为该元素具有与所述预成型件的纤维接近的热膨胀系数。该渗透组合物可以对应于硅本身或硅合金，硅合金通常包含少量的一种或多种其他元素，如钛、钼、硼、铁、铌等。
通过渗溶过程进行的致密化比通过化学气相渗透(CVI)进行的致密化具有更快更容易实施的优点。尽管如此，所使用的硅基渗透组合物能够呈现出比所述预成型件的纤维的热稳定性温度更高的熔点或温度(热稳定性)。在这种情况下，当熔融组合物被渗入到所述预成型件中，所述纤维可能会经受降解，这样会明显降低所述纤维的机械性能。
发明内容
本发明的一个特别目的在于提供一种没有上述缺陷的、制造复合材料部件的方法。
此目的通过包括以下步骤的制造复合材料部件的方法得以实现：
·制造加强的纤维预成型件，所述预成型件的纤维是碳或陶瓷纤维和被涂覆有界面；
·获得加强的和部分致密的纤维预成型件，部分致密化包括使用化学气相渗透在所述界面上形成第一基质相；和
·通过渗入渗透组合物继续致密所述纤维预成型件，所述渗透组合物包含至少硅和至少一种其他适于降低该渗透组合物的熔融温度至低于或等于1150℃的元素。
具体地，通过向硅中添加使得得到具有低于或等于1150℃熔点的渗透组合物成为可能的元素，而获得渗透组合物，其保持在大部分纤维尤其是用于制作CMC材料的纤维加强件的陶瓷纤维的热稳定性温度范围之中。所以，本发明所述的通过使用MI类致密化过程制造复合材料部件的方法，能够实施而没有损害所述预成型件的纤维的风险。
在本发明所述方法的第一方面，所述渗透组合物包含镍，镍在所述组合物中所占重量百分比在50％～75％范围。除了硅以外，镍的含量在50％～75％的范围，熔点低于或等于1150℃的渗透组合物被获得。
在本发明所述方法的第二方面，所述渗透组合物包含锗，锗在所述组合物中所占重量百分比在89％～98％范围。除了硅以外，有了至少89％的锗，熔点低于或等于1150℃的渗透组合物被获得。
在本发明所述方法的第三方面，所述渗透组合物包含，除所述的适于降低渗透组合物的熔融温度至低于或等于1150℃的元素外，少于10％(重量百分比)的下列元素中的至少一种：铝和硼。添加这些组分中的至少一种使得改善位于待处理的基质上渗透组合物的去氧化性和润湿性成为可能，并且还赋予处理过的材料以特殊性能，例如更好的耐氧化和耐腐蚀的能力。
在本发明所述方法的第四方面，所述纤维预成型件由碳纤维或碳化硅(SiC)纤维制成。
在本发明所述方法的第五方面，所述纤维预成型件由三维或多层编织或从多个二维纤维层形成被制作为单件的纤维结构。
在本发明所述方法的第六方面，所述界面由至少一层下列材料中的任何一种形成：热解碳(PyC)，掺硼碳(BC)，和氮化硼(BN)。
本实施例中所述的PyC，BC或BN界面，具有因PyC，BC或BN的片状结构而为所述复合材料提供脆性减轻的常规功能，其有助于使通过基质已经扩展后达到所述界面的裂纹偏转，如此，防止这样的裂纹使纤维破裂，或者至少延缓任何所述破裂。
术语“掺硼碳”或者BC用于表示包含5原子百分比(at％)到20at％的硼，其余为碳。这样的组合物具有乱层结构，即：在堆叠的片状结构中方向错乱，这有利于脆性减轻功能。
在本发明所述方法的第七方面，所述第一基质相包含至少一层选自下列材料中的至少一种的材料：自愈材料，氮化硅(Si3N4)和碳化硅(SiC)。所述自愈材料选自三元的硅-硼-碳系统和碳化硼(B4C)。
所述基质的第一层包括多层自愈材料，该自愈材料与选自热解碳(PyC)，掺硼碳(BC)和不含硼的陶瓷材料的一层或多层材料交替。
在本方法的一个实施方式中，所述第一基质相由自愈材料的单层或者自愈材料的多层形成，并且包括至少一层不含碳的陶瓷材料，该层形成于自愈材料的所述单层上或最后一层上。
所述不含硼的陶瓷材料层可以有不少于500nm的厚度。
所述不含硼的陶瓷材料层可以由碳化硅(SiC)或实际上氮化硅(Si3N4)制成。
在本发明所述方法的第八方面，在所述纤维预成型件部分致密化之后以及通过渗透组合物的渗入使所述纤维预成型件致密化之前，该方法包括修改纤维预成型件之中的孔的阵列的步骤，该修改通过下列处理方法中的任何一种方法实施：
·在所述预成型件之中分散下列材料中的至少一种的粉末：碳化硅(SiC)；氮化硅(Si3N4)；碳(C)；硼(B)；碳化硼(B4C)；和碳化钛(TiC)；
·通过用聚合物浸渍所述预成型件并热解该聚合物，在所述预成型件中引入陶瓷或碳相；或者
·在所述预成型件中引入碳或陶瓷泡沫，通过用聚合物浸渍所述预成型件并热解该聚合物。
附图说明
通过阅读下面参考唯一的附图而做出的非限制性描述可以更好地理解本发明，附图给出了在本发明的实施方式中制造CMC材料部件的方法的连续步骤。
具体实施方式
本发明建议一种制造部件的方法，该部件由复合材料制成，尤其是热结构陶瓷基质复合(CMC)材料，即通过由碳或陶瓷纤维制成的加强件形成并且被至少部分为陶瓷的基质致密的材料制成；同时还可以由热结构碳/碳(C/C)复合材料，即通过被碳基质致密的碳纤维加强件形成的材料制成。
本发明的制造方法显著之处在于它使用一种渗透组合物，其具有比常用于致密纤维预成型件的硅基渗透组合物更低的熔融温度。更具体地，本发明所使用的渗透组合物使得用熔融组合物在比所述纤维的热稳定性温度更低的温度下渗入纤维预成型件成为可能(热稳定性)，即温度足够低以避免渗透过程中所述预成型件的纤维的机械性能的任何降解，特别适用于第一代碳化硅纤维。根据本发明，所述纤维预成型件由在低于或等于1150℃时熔融的渗透组合物渗入。
为了这个目的，除了硅以外，所述渗透组合物包含至少一种其他元素，该元素适于降低所述组合物的熔点或温度至低于或等于1150℃的温度。所述渗透组合物的熔点的这种降低尤其可以通过向硅中添加镍(Ni)或锗(Ge)获得。更确切地，当添加镍时，所述渗透组合物包含50％-75％(重量百分比)的镍，则使得获得范围在1000℃(渗透组合物包含50％硅和50％镍)-1150℃(渗透组合物包含25％硅和75％镍)之间的熔点成为可能。当添加锗时，所述渗透组合物包含89％-98％的锗，则使得获得范围在1000℃(渗透组合物包含2％硅和98％锗)-1150℃(渗透组合物包含11％硅和89％锗)之间的熔点成为可能。因此，通过向硅中添加含量范围在50％-75％之间的镍或者至少89％的锗，可以获得具有低于或等于1150℃的熔融温度的硅合金，该温度低于由碳化硅(SiC)制成的纤维(下称碳化硅纤维)，例如第一代Tyranno或者Tyranno型碳化硅纤维的热稳定性温度。
除了低熔点，所述渗透组合物具有能够使得良好质量的复合材料被制造所要求的其他全部性能。具体地，所述渗透组合物与所述预成型件中用于渗入的元素在化学上相容。所述渗透组合物还呈现出对氧化或腐蚀环境的良好抵抗性以及卓越的长期特性。
所述渗透组合物还可以包含少于10％(重量百分比)的下列元素中的至少一种：铝和硼。添加这些组分中的至少一种用于改善位于待处理的基质上渗透组合物的去氧化性和润湿性，并且还赋予处理过的材料特殊性能，例如更好的耐氧化和腐蚀的能力。
参考唯一的附图，根据本发明所述制造CMC材料的方法的第一实施方式，如下文所述。
第一步骤10包括制造纤维结构，形状与待制造的部件的形状接近的纤维预成型件由该纤维结构制成。这样的纤维结构可以通过使用纱线或丝束进行多层或三维编织获得。还可以从二维纤维织构，如编织的纺织物或者纱线或丝束片开始以形成层，这些层随后被覆盖在模套上并且可能结合在一起，如通过缝合或植入纱线。
构成纤维结构的纤维优选地为陶瓷纤维，如本质上由碳化硅(SiC)制成的纤维(下称SiC纤维)，或者由氮化硅(Si3N4)制成的纤维。还可以使用日本供应商UbeIndustries,Limited销售的名为"TyrannoZMI","TyrannoLox-M",和"TyrannoSA3"SiC纤维，或者日本供应商NipponCarbon销售的"Nicalon","Hi-Nicalon",和"Hi-Nicalon(S)"碳化硅纤维。作为上述方法的变形，还可使用碳纤维。
在已知方法中，使用陶瓷纤维特别是SiC纤维，优选地，在形成界面涂覆之前在纤维上实施表面处理(步骤20)，以消除浆纱和表面氧化层，如呈现在纤维上的二氧化硅SiO2。
步骤30包括利用工具使纤维结构成型，以获得形状与待制造部件的形状接近的预成型件。
使所述预成型件保持在其成型工具例如由石墨制成的工具中，在所述预成型件的纤维上通过CVI形成脆性减轻界面，该界面特别地由热解碳(PyC)或氮化硼(BN)或掺硼碳(BC)构成，具有5at％-20at％的硼，平衡为碳(步骤40)。热解碳(PyC)或掺硼碳(BC)界面的厚度优选为在10nm-1000nm的范围中。
此后(步骤50)，所述第一基质相由CVI形成，该基质可能包含至少一层自愈材料。选择包含碳的自愈材料是可能的，如三元的硅-硼-碳系统或碳化硼(B4C)，由于氧气的存在，其能够形成具有自愈性能的硼硅酸盐型玻璃。所述第一基质相的厚度不少于500nm，并且优选地在1μm-30μm的范围之间。
所述第一基质相可以包括自愈材料的单层或者不同自愈材料的多层。还可以由与热解碳(PyC)或者掺硼碳(BC)或者不含硼的陶瓷材料层，如SiC或者Si3N4层交替的多层自愈材料形成第一基质层。
当所述第一基质相只包括一层自愈材料时，不含硼的陶瓷材料层，如碳化硅SiC或者氮化硅Si3N4层形成于自愈材料层上，或者当所述第一基质相包括多层自愈材料时，不含硼的陶瓷材料层，如SiC或者Si3N4层形成于自愈材料的最后一层上，旨在自愈材料和随后引入的熔融硅或硅基液态组合物之间形成反应屏障。
形成反应屏障的陶瓷材料层的厚度可以是至少500nm，典型地，在1μm至几个μm的范围之间。除了SiC或Si3N4以外的不含硼的陶瓷材料，可被用于形成所述反应屏障，例如：耐火碳化物，如ZrC或HfC。
所述界面连同第一基质相的总厚度被选定为足够加强纤维预成型件，即将预成型件的纤维充分结合在一起，为了在保存所述预成型件的形状时，没有支持工具的辅助而能够对预成型件进行处理。该厚度可以是至少500nm。经过加强，所述预成型件保持多孔的，例如，其最初的孔仅被所述界面和第一基质相在很小的程度上填充。
使用CVI沉积PyC,BC,B4C,Si-B-C,Si3N4,BN和SiC是公知的。可以特别参考下列文献：US5246736,US5738951,US5965266,US6068930和US6284358。
可以观察到所述界面可通过CVI在纤维结构定型前形成于该纤维结构的纤维上，只要所述界面足够薄以避免影响期望的所述纤维结构发生变形的能力。
将多孔的加强的预成型件自其成型工具移除，以便通过包括修改孔的阵列和使用渗透组合物渗入预成型件的MI型过程继续致密化。
所述纤维预成型件中的孔的阵列通过下列处理方法之一修改(步骤60)：
·分散所述预成型件之中的下列材料中的至少一种的粉末：碳化硅(SiC)；氮化硅(Si3N4)；碳(C)；硼(B)；碳化硼(B4C)；和碳化钛(TiC)；
·通过用聚合物浸渍所述预成型件并热解该聚合物，在所述预成型件中引入陶瓷或碳相；或者
·通过用聚合物浸渍所述预成型件并热解该聚合物，在所述预成型件中引入碳或陶瓷泡沫。
在当前描述的实施例中，所述预成型件中的孔的阵列通过使用浸渍组合物分散粉末而被修改。所述浸渍组合物可以是包含了悬浮在液态媒介例如水中的粉末的浆料。该粉末可以通过过滤或沉降，可能还在吸力的帮助下，保留在预成型件中。优选地，使用由具有小于5μm的平均粒径的粒子制成的粉末。
干燥后，获得加强的预成型件，其孔中具有被分散的碳和/或陶瓷粉末。
通过使用渗透组合物渗入所述预成型件继续致密化(步骤70)，具体地，本实施例中渗透组合物包含46％(重量百分比)的硅和54％(重量百分比)的镍，该组合物在约1000℃的温度下被熔融。渗透在非氧化环境下实施，优选为减压环境下。
当在先引入的粉末由碳制成，或者如果该材料含有可接受的碳相，以及当用于浸渍所述加强的预成型件的树脂的残留碳出现，所述硅与其发生反应形成SiC。当在先引入的粉末由陶瓷制成，特别地，为碳化物、氮化物或硅化物，以及当用于浸渍所述加强的预成型件的树脂的残留陶瓷出现，部分由硅制成的、结合了陶瓷粉末的基质被获得。在所有情形下，大多数基质是陶瓷。

Claims (11)

1.一种制造复合材料部件的方法，该方法包括以下步骤：
·制造加强的纤维预成型件，所述预成型件的纤维是碳或陶瓷纤维，并且被涂覆有界面；
·获得加强的和部分致密的纤维预成型件，部分致密化包括使用化学气相渗透在所述界面上形成第一基质相；和
·通过渗入渗透组合物继续致密所述纤维预成型件，所述渗透组合物包含至少硅和至少一种其他适于降低该渗透组合物的熔融温度至低于或等于1150℃的元素。
2.根据权利要求1所述的方法，其特征在于：所述渗透组合物包含镍，镍在所述组合物中所占重量比例在50％～75％的范围。
3.根据权利要求1所述的方法，其特征在于：所述渗透组合物包含锗，锗在所述组合物中所占重量比例在89％～98％的范围。
4.根据权利要求2或3所述的方法，其特征在于：所述渗透组合物包含，除所述的适于降低渗透组合物的熔融温度至低于或等于1150℃的元素外，还包含重量少于10％的下列元素中的至少一种：铝和硼。
5.根据权利要求1-4中任一权利要求所述的方法，其特征在于：所述纤维预成型件由碳纤维或碳化硅(SiC)纤维制成。
6.根据权利要求1-5中任一权利要求所述的方法，其特征在于：所述纤维预成型件由三维或多层编织或从多个二维纤维层形成被制作为单件的纤维结构。
7.根据权利要求1-6中任一权利要求所述的方法，其特征在于：所述界面由至少一层下列材料中的任何一种形成：热解碳(PyC)，掺硼碳(BC)，和氮化硼(BN)。
8.根据权利要求7所述的方法，其特征在于：所述第一基质相包括至少一层选自下列材料中至少一种的材料：自愈材料，氮化硅(Si3N4)和碳化硅(SiC)。
9.根据权利要求8所述的方法，其特征在于：所述第一基质相包括至少一层选自三元的硅-硼-碳系统和碳化硼B4C的自愈材料。
10.根据权利要求1-9中任一权利要求所述的方法，其特征在于：所述第一基质相包括多层自愈材料，该自愈材料与选自热解碳(PyC)，掺硼碳(BC)和不含硼的陶瓷材料的一层或多层材料交替。
11.根据权利要求1-10中任一权利要求所述的方法，其特征在于：在所述纤维预成型件的部分致密化之后以及通过渗透组合物渗入使所述纤维预成型件致密化之前，该方法包括修改纤维预成型件之中的孔的阵列的步骤，该修改通过下列处理方法中的任何一种方法实施：
·在所述预成型件之中分散下列材料中的至少一种的粉末：碳化硅(SiC)；氮化硅(Si3N4)；碳(C)；硼(B)；碳化硼(B4C)；和碳化钛(TiC)；
·通过用聚合物浸渍所述预成型件并热解该聚合物，在所述预成型件中引入陶瓷或碳相；或者
·通过用聚合物浸渍所述预成型件并热解该聚合物，在所述预成型件中引入碳或陶瓷泡沫。
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