CN110944963A - 一种制造复合部件的方法 - Google Patents

一种制造复合部件的方法 Download PDF

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Publication number
CN110944963A
CN110944963A CN201880048801.1A CN201880048801A CN110944963A CN 110944963 A CN110944963 A CN 110944963A CN 201880048801 A CN201880048801 A CN 201880048801A CN 110944963 A CN110944963 A CN 110944963A
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carbon
adhesion promoter
resin
group
coating
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CN110944963B (zh
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尼古拉斯·埃伯林-福克斯
埃里克·布永
盖伊·雅各布
埃迪·古利安
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Safran Ceramics SA
ArianeGroup SAS
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Safran Ceramics SA
ArianeGroup SAS
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Abstract

本发明涉及一种制造复合部件的方法，该方法包括至少以下步骤：将粘合促进剂(10)引入纤维预成型件的孔中，纤维预成型件由在其表面上覆盖具有‑OH基团的涂层(1)的纤维形成，所述粘合促进剂包含根据取代或亲核加成反应而与‑OH基团反应的吸电子基团G1和反应基团G2，所述反应基团G2选自：羟基官能团、环氧化物、卤素原子、胺基官能团、羰基官能团、碳‑碳双键或碳‑碳三键；通过基团G1与‑OH基团的取代或亲核加成反应，将所述粘合促进剂接枝到所述涂层表面，通过第一次加热已引入所述粘合促进剂的所述纤维预成型件进行该接枝；在接枝粘合促进剂的步骤之后，将陶瓷前体树脂(4)引入到所述纤维预成型件的孔中；使引入的树脂聚合，使接枝的粘合促进剂(20)与树脂通过这两种化合物在所述基团G2水平的化学反应结合，通过第二次加热已引入树脂的所述纤维预成型件来进行所述聚合和所述结合，以及通过聚合树脂(40)的热解而在所述纤维预成型件的孔中形成陶瓷基体相。

Description

一种制造复合部件的方法
技术领域
本发明涉及一种制造具有至少部分地为陶瓷的基体的复合部件的方法，其中该复合部件具有改善的机械性能。
背景技术
具有至少部分地为陶瓷的基体的复合部件可以通过聚合物浸渍和热解(PIP)的技术常规地获得。
在该技术中，将陶瓷前体聚合物的液体组合物引入到纤维预成型件的孔中。如此引入的组合物被聚合并热解以形成陶瓷基体相。依据所使用的前体的选择，可以通过该方法形成各种类型的陶瓷基体。具体地，聚硅氮烷聚合物可用于获得SiCN基体，聚碳硅烷聚合物用于获得SiC基体，或聚硅氧烷聚合物用于获得SiCO基体。
由于通过热解转化为陶瓷涉及体积收缩，通常要连续多次重复这些渗透和热解循环，以便获得致密的部件所需的孔隙度。
改善具有至少部分已通过PIP技术形成的基体的复合部件所呈现的机械性能是值得期望的。
发明内容
根据第一方面，本发明涉及一种制造复合部件的方法，该方法包括至少以下步骤：
-将粘合促进剂引入纤维预成型件的孔中，纤维预成型件由在其表面上覆盖具有-OH基团的涂层的纤维形成，所述粘合促进剂包含根据取代或亲核加成反应，而与-OH基反应的吸电子基团G1和反应基团G2，该反应基团G2选自：羟基官能团、环氧化物、卤素原子、胺基官能团、羰基官能团、碳-碳双键或碳-碳三键，
-通过基团G1与-OH基团的取代或亲核加成反应，将粘合促进剂接枝到涂层表面，通过第一次加热已引入粘合促进剂的纤维预成型件，进行该接枝，
-在接枝粘合促进剂的步骤之后，将陶瓷前体树脂引入到纤维预成型件的孔中，
-使引入的树脂聚合，使接枝的粘合促进剂与树脂通过这两种化合物在基团G2水平的化学反应结合，所述聚合和所述结合通过第二次加热已引入树脂的纤维预成型件来进行，以及
-通过聚合树脂的热解而在纤维预成型件的孔中形成陶瓷基体相。
发明人已经对具有通过PIP技术获得的基体的部件进行了研究。这些研究可以确定这些部件的机械性能的缺陷是由于在PIP基体界面处的粘合问题引起的。实际上，发明人已经发现了处于聚合状态的陶瓷前体与预先在纤维上形成的涂层之间的内聚力损失(参见图1)。在与图1相关的测试中，涂层是覆盖纤维的一层热解碳(PyC)中间相。就其本身而言，图2显示了在前体热解后获得的基体相与预先在纤维上形成的碳化硅(SiC)涂层之间存在内聚力损失。这些内聚力损失的存在反映在所获得部件的次优机械性能上。
本发明被开发以解决该问题，并因此施用粘合促进剂以改善PIP基体相与预先在纤维上形成的涂层之间的粘合性。如下面将描述的，该先前形成的涂层可以是各种类型的。由于基团G1，粘合促进剂能够被共价接枝至下面的涂层。粘合促进剂被接枝在涂层表面上存在的侧基-OH基团水平，该-OH基团在将涂层暴露于环境空气后自然存在。此外，由于基团G2，粘合促进剂能够与树脂进行化学反应。该反应使促进剂与陶瓷前体树脂共价结合。因此，粘合促进剂构成了树脂(即最终的PIP基体相)与下面的涂层之间的结合中间物，从而可以改善该基体相对该涂层的粘合性。因此，本发明提出的粘合促进剂的使用有助于改善所得复合部件的机械性能。
在一个实施例中，该方法还包括在引入促进剂之前，通过化学气相沉积或渗透(CVD或CVI)在纤维上形成涂层的步骤。
在这种情况中，涂层可以是中间相或初始基体相。在该实施例中，粘合促进剂的使用改善了在该涂层上直接形成的PIP基体相的粘合性。
作为变型，该方法还包括在引入促进剂之前，通过将前体化合物引入到预成型件的孔中并对该前体化合物进行热解而在纤维上形成涂层的步骤。
在这种情况中，该涂层构成了初始的PIP基体相，并且粘合促进剂的使用改善了相继形成的两块PIP基体之间的粘合性。应当注意，当基体由多块PIP基体形成时，可以施用上述方法以改善这些块中的各自间的粘合性。
在一个实施例中，形成涂层表面的材料选自：碳，具体为热解碳、掺有硼的碳、碳化硅、氮化硼、掺有硅的氮化硼或氮化硅。
在一个实施例中，基团G1选自：环氧化物、羧基官能团、卤素原子、碳-碳双键或碳-碳三键。
在一个实施例中，基团G2选自：羟基官能团、胺基官能团或碳-碳双键。
在一个实施例中，单体状态下的粘合促进剂具有以下通式：G1-E-G2，其中E表示包含1至10个之间的碳原子的碳链或包含1至10个之间的硅原子的硅烷链、硅氧烷链、硅氮烷链或碳硅烷链。
例如，E可以是脂肪族或芳族碳链。E可以是直链或支链。单体状态下的促进剂可以具有单个基团G2或多个基团G2。
具体地，E表示包含1至5个之间的碳原子的碳链。作为变型，E表示包含1至5个之间的硅原子的硅烷链、硅氧烷链、硅氮烷链或碳硅烷链。
具体地，粘合促进剂是卤代硅烷。
在一个实施例中，树脂选自：聚硅氧烷树脂、聚硅氮烷树脂、聚碳硅氧烷树脂、聚碳硅烷树脂以及所述树脂的混合物。
附图说明
通过以下非限制性的描述并参考附图，本发明的其他特征和优点将变得更加清楚，其中：
图1是显示处于聚合状态的陶瓷前体与在纤维上形成的PyC涂层之间存在内聚力损失的照片(未根据本发明)，
图2是示出在PIP基体相与在纤维上形成的SiC涂层之间存在内聚力损失的照片(未根据本发明)，
图3A至3D示意性地示出根据本发明的方法的实施例的不同步骤，
图4示出了在根据本发明的方法的第一实施例的背景下，在接枝粘合促进剂之后进行的通过X射线光电子能谱法分析的测量结果，
图5A至5C是在根据本发明的方法的第一实施例中获得的复合材料的照片，和
图6A至6C是在根据本发明的方法的第二实施例中获得的复合材料的照片。
具体实施方式
首先，形成由诸如，陶瓷或碳纤维的耐火纤维形成的纤维预成型件。
预成型件可以由例如，日本NGS公司提供的商品名为“Nicalon”、“Hi-Nicalon”或“Hi-Nicalon Type S”的碳化硅的纤维形成。可用于形成该预成型件的碳纤维由例如，Toray公司供应，其商品名为Torayca T300 3K。
纤维预成型件是由至少一种纺织操作获得。纤维预成型件用于构成要获得的部件的纤维增强。纤维预成型件可具体通过多层或三维编织来获得。
“三维编织”或“3D编织”应被理解为编织的方式，其中某些至少一些经纱在数个纬纱层上连接纬纱。在本文中，经纱和纬纱之间的作用可以颠倒，并且也应被权利要求书所涵盖。
纤维预成型件例如，可以具有多缎纹编织，即，是通过用数层纬纱进行三维编织而获得的织物，其中每层的基本编织等同于常规缎纹类型的编织，但是编织的某些点将纬纱层连接在一起。作为变型，纤维预成型件可具有互锁编织。“互锁编织物或织物”应理解为3D编织中的一种编织，其中每层经纱连接几层纬纱，相同经纱柱的所有纱线在编织物平面内的运动相同。可用于形成纤维预成型件的各种类型的多层编织描述在文献WO 2006/136755中。
还可以首先形成纤维结构，诸如二维织物或单向层，并通过在模具上覆盖形成所述纤维纹理来获得纤维预成型件。这些结构可以任选地例如，通过缝合或植入纤维而连接在一起以形成纤维预成型件。
然后在预成型件的纤维上形成涂层。该涂层可以是中间相，或者可以包含一个或多个部分地使纤维预成型件致密的基体相。涂层可以是碳，特别是PyC、掺有硼的碳(BC，硼的原子比例为5％至20％之间，其余为碳)或陶瓷材料，诸如碳化硅、氮化硼(BN)、掺有硅的氮化硼(BN(Si)，硅的重量比在5％至40％之间，其余为氮化硼)或氮化硅(Si3N4)。
因此，涂层可以通过单层或多层中间相形成。在这种情况下，中间相的表面具有-OH基团，该基团用于使粘合促进剂接枝。该中间相可以包括至少一层热解碳、氮化硼、掺有硅的氮化硼或掺有硼的碳。
在此，中间相具有减轻复合材料的脆化的功能，这促进了在基体中传播之后到达中间相的任何裂纹的偏离，防止或延迟了由所述裂纹引起的纤维的断裂。
中间相的厚度可以在10nm至1000nm之间，例如在10nm至100nm之间。中间相可以通过CVI在预成型件的纤维上形成。
作为变型，中间相可以在形成预成型件之前，通过化学气相沉积在纤维上形成，然后从如此涂层的纤维开始形成该预成型件。
作为变型，涂层可以包括至少一个初始基体相和任选地置于所述至少一个初始基体相和纤维之间的中间相。在那种情况下，外部初始基体相，即离预成型件的纤维最远的相，在其表面上具有用于使粘合促进剂接枝的-OH基团。
外部初始基体相本身可以通过各种已知方法，诸如CVI、熔融态硅的渗透(“熔体渗透”方法)或通过PIP技术形成。因此，应注意的是，在后一种情况下，粘合促进剂可以改善连续两块PIP基体之间的粘合性。外部初始基体相可以是陶瓷或碳。外部初始基体相可以是碳、或PyC、碳化硅、氮化硼或氮化硅。
当然，在形成涂层之后，纤维预成型件保持多孔，以允许形成通过粘合促进剂连接到涂层的PIP陶瓷基体相。现在将利用图3A至3D所示的根据本发明的方法的实施例来描述这方面。
在形成涂层之后，将粘合促进剂10引入到纤维预成型件的剩余孔中(参见图3A)。液态的粘合促进剂10可以引入到纤维预成型件的孔中。粘合促进剂10可注入到纤维预成型件的孔中。引入的粘合促进剂10与带有-OH基团的涂层1的表面S接触。该表面S对应于涂层1的外表面，即距形成预成型件的纤维最远的表面。
在所示的实施例中，单体状态下的促进剂10具有以下通式：G1-E-G2。在此，基团G1为氯原子，E链为具有一个硅原子的碳硅烷链。在此，粘合促进剂10是氯硅烷。如上所述，对于基团G1和G2以及对于E链，可能有数种变型。
在所示的实施例中，单体状态的促进剂10被引入。然而，当引入寡聚状态的促进剂10时，其仍在本发明的范围内。
基团G1允许将促进剂10接枝到涂层1。基团G2允许将促进剂连接到陶瓷前体树脂，并因此最终连接到热解后获得的陶瓷基体相。
进行第一次加热以将促进剂10接枝到涂层1的表面S上。该第一次加热可以激活基团G1与表面S的-OH基团的取代或亲核加成反应，从而实现了促进剂10的接枝。在所示的实施例中，接枝通过亲核取代反应实现。接枝后，我们通过在-OH基团的氧与上述E链之间形成共价键来获得接枝到涂层1表面S的促进剂20(参见图3B)。
在第一次加热期间中可施加大约恒定的温度(±2℃)。基于公知常识，本领域技术人员将能够根据粘合促进剂，确定在第一次加热期间施加的温度值。在第一次加热期间施加的温度通常可以在30℃至60℃之间。
接枝后，接枝过的促进剂20仍然具有至少一个用于与陶瓷前体树脂反应的侧基团G2(参见图3B)。
一旦粘合促进剂20已被接枝，就将陶瓷前体树脂4引入到纤维预成型件的孔中(参见图3C)。引入的树脂4与接枝过的促进剂20接触。液态的树脂4可引入纤维预成型件的孔中。树脂4可注入到纤维预成型件的孔中。该树脂4本身是已知的，并且可以选自：聚硅氧烷树脂、聚硅氮烷树脂、聚碳硅氧烷树脂、聚碳硅烷树脂以及所述树脂的混合物。
一旦引入树脂4，它将共价结合到接枝过的促进剂20。该键通过接枝过的促进剂20的基团G2与树脂4所携带的反应性官能团之间的化学反应产生。例如，树脂4的反应性官能团可以选自以下基团：-OH、Si-H或碳-碳双键。
有利地，基团G2选自：-OH、-NH2或碳-碳双键。所述基团G2的选择允许进一步改善树脂4与接枝过的促进剂20的粘合性。当树脂为聚硅氧烷树脂时，G2为-OH是有利的。当树脂为聚硅氮烷树脂时，G2为-NH2是有利的。当树脂是聚硅氧烷、聚硅氮烷或聚碳硅烷树脂时，G2是碳-碳双键是有利的。
例如，可以使用
Figure BDA0002375212320000061
Systems出售的商品名为“SMP-10”的聚碳硅烷树脂。该树脂具有能够与基团G2反应的Si-H官能团和碳-碳双键。
例如，可以使用科莱恩(Clariant)出售的商品名为“HTT1800”或“PSZ 20”的聚硅氮烷树脂。该树脂具有能够与基团G2反应的Si-H官能团和碳-碳双键。
例如，可以使用Wacker出售的商品名为“H62C”的聚硅氧烷树脂。该树脂具有能够与基团G2反应的Si-H官能团和碳-碳双键。
例如，可以使用Wacker出售的商品名为“MK”或“MS100”的聚硅氧烷树脂。该树脂具有能够与基团G2反应的Si-H官能团和-OH基团。
例如，可以使用
Figure BDA0002375212320000062
Systems出售的商品名为“SPR212”或“SPR036”的聚碳硅氧烷树脂。该树脂具有能够与基团G2反应的Si-H官能团和碳-碳双键。
依据基团G2的性质和树脂4所带的反应性官能团，接枝过的粘合促进剂20与树脂4的结合可以通过各种化学反应来进行。
例如，当树脂具有Si-H官能团并且基团G2是碳-碳双键时，反应可以是形成Si-C-C键的氢化硅烷化。
例如，当树脂具有Si-H官能团且基团G2为-OH时，反应可以是形成Si-O-Si键的缩合反应。
例如，当树脂具有Si-H官能团且基团G2为-NH2时，该反应可以是形成Si-N-Si键的缩合(氨基转移)。
例如，当树脂带有碳-碳双键并且基团G2是碳-碳双键时，该反应可以是形成C-C-C-C键的加成。
通过进行第二次加热，进行树脂4与接枝的促进剂20结合。第二次加热可以使树脂4聚合并激活树脂4与接枝的促进剂20的结合反应。基于公知常识，本领域技术人员将能够根据所使用的树脂和接枝的促进剂20来确定第二次加热期间要施加的温度值。在第二次加热期间，通常可施加90℃至250℃之间的温度。
图3D示出了聚合的树脂40与接枝的促进剂30的结合。在这种构造中，促进剂30形成聚合的树脂40和涂层1之间的连接。然后将聚合的树脂40热解以形成纤维预成型件的孔中的陶瓷基体相。
应当指出，部件基体的形成可涉及陶瓷前体树脂的引入和热解的数个PIP循环的执行。在那种情况下，可以在每次新引入陶瓷前体树脂之前，将粘合促进剂接枝到通过PIP获得的基体块。在这种情况下，粘合促进剂将多块PIP基体连接在一起，以提高这些块之间的粘合性。
一旦获得，这样制造的部件可以是航空或航天应用的部件。该部件可以是航空或航天发动机的燃气轮机或工业涡轮的热部分的部件。该部件可以是涡轮发动机的一部分。该部件可以构成分配器的至少一部分、喷嘴或热保护涂层的至少一部分、燃烧室的壁、涡轮环的扇区或涡轮发动机的叶片。
实施例
实施例1
将粘合促进剂引入用SiC初始基体相预致密的SiC纤维的纤维预成型件的孔中。使用的粘合促进剂是乙酰氧乙基二甲基氯硅烷。
通过进行第一次加热，将由此引入的粘合促进剂接枝到SiC初始基体相的表面。相应的化学反应在环己烷中在热控反应器中进行24小时，在第一次加热期间将温度设定为40℃。在该反应期间，将氮气流速设定为0.6L/h。
通过X射线光电子谱法分析(“XPS”分析)来验证粘合促进剂的接枝。所得结果示于图4中，并显示了在SiC初始基体相的表面上存在对应于接枝的促进剂的有机硅物质。
一旦促进剂已接枝，就将由Wacker出售的商品名为“MK”的聚硅氧烷树脂引入到纤维预成型件的孔中。
然后在250℃下进行第二次加热，以使引入的树脂聚合并将其结合到接枝的粘合促进剂。图5A是在聚硅氧烷树脂聚合之后和其热解之前获得的材料的照片。发现存在裂纹“F”，其优先在聚合物基体内而不是在聚合物基体与SiC初始基体相之间的界面处传播。这证明了该聚合物基体与SiC初始基体以及因此与纤维增强之间存在强的粘合性。这种强的粘合性是由于在第二次加热期间在树脂和接枝的促进剂之间形成了键。
然后陶瓷基体相通过在900℃下施行热处理，通过聚硅氧烷树脂的热解获得。图5B和5C是在该热解后获得的材料的照片。再次发现，裂纹“F”优先存在于通过热解获得的基体中而不是在初始基体相与通过热解获得的基体相之间的界面处。这证实了通过热解获得的基体相对涂层和下面的纤维增强的良好粘合性。
实施例2
将粘合促进剂引入用SiC初始基体相预致密的SiC纤维的纤维预成型件的孔中。使用的粘合促进剂是烯丙基二甲基氯硅烷。
通过进行第一次加热，将由此引入的粘合促进剂接枝到SiC初始基体相的表面。相应的化学反应在环己烷中在热控反应器中进行24小时，在第一次加热期间将温度设定为40℃。在该反应期间，将氮气流速设定为0.6L/h。
以与实施例1相同的方式，通过X射线光电子谱法(“XPS”分析)证实了粘合促进剂的接枝。
一旦促进剂已接枝，就将由科莱恩出售的商品名为“PSZ 20”的聚硅氮烷树脂引入到纤维预成型件的孔中。
然后在250℃下进行第二次加热以使引入的树脂聚合并将其结合到接枝的粘合促进剂。图6A是在聚硅氮烷树脂聚合之后和在其热解之前获得的材料的照片。如实施例1，发现裂纹“F”优先存在于聚合物基体中，因此证明了该聚合物基体的良好粘合性。
然后陶瓷基体相通过在900℃下施行热处理，通过聚硅氮烷树脂的热解获得。图6B和6C是在该热解后获得的材料的照片。还发现裂纹“F”优选存在于通过热解获得的基体中。
表述“...至...之间”应理解为包括范围的极值。

Claims (10)

1.一种制造复合部件的方法，该方法包括至少以下步骤：
将粘合促进剂(10)引入纤维预成型件的孔中，纤维预成型件由在其表面上覆盖具有-OH基团的涂层(1)的纤维形成，所述粘合促进剂包含根据取代或亲核加成反应而与-OH基团反应的吸电子基团G1和反应基团G2，所述反应基团G2选自：羟基官能团、环氧化物、卤素原子、胺基官能团、羰基官能团、碳-碳双键或碳-碳三键，
通过基团G1与-OH基团的取代或亲核加成反应，将所述粘合促进剂接枝到所述涂层表面，通过第一次加热已引入所述粘合促进剂的所述纤维预成型件进行该接枝，
在接枝粘合促进剂的步骤之后，将陶瓷前体树脂(4)引入到所述纤维预成型件的孔中，
使引入的树脂聚合，使接枝的粘合促进剂(20)与树脂通过这两种化合物在所述基团G2水平的化学反应结合，通过第二次加热已引入树脂的所述纤维预成型件来进行所述聚合和所述结合，以及
通过聚合树脂(40)的热解而在所述纤维预成型件的孔中形成陶瓷基体相。
2.根据权利要求1所述的方法，其中所述方法进一步包括在引入促进剂之前，通过化学气相沉积或渗透在纤维上形成涂层(1)的步骤。
3.根据权利要求1所述的方法，其中所述方法进一步包括在引入促进剂之前，通过将前体化合物引入到预成型件的孔中并对所述前体化合物进行热解而在纤维上形成涂层(1)的步骤。
4.根据权利要求1至3任一项所述的方法，其中形成涂层(1)表面的材料选自：碳、掺有硼的碳、碳化硅、氮化硼、掺有硅的氮化硼或氮化硅。
5.根据权利要求1至4任一项所述的方法，其中所述基团G1选自：环氧化物、羧基官能团、卤素原子、碳-碳双键或碳-碳三键。
6.根据权利要求1至5任一项所述的方法，其中基团G2选自：羟基官能团、胺基官能团或碳-碳双键。
7.根据权利要求1至6任一项所述的方法，其中单体状态下的粘合促进剂(10)具有以下通式：G1-E-G2，其中E表示包含1至10个之间的碳原子的碳链或包含1至10个之间的硅原子的硅烷链、硅氧烷链、硅氮烷链或碳硅烷链。
8.根据权利要求7所述的方法，其中E表示包含1至5个之间的碳原子的碳链，或其中E表示包含1至5个之间的硅原子的硅烷链、硅氧烷链、硅氮烷链或碳硅烷链。
9.根据权利要求7或8所述的方法，其中所述粘合促进剂(10)是卤代硅烷。
10.根据权利要求1至9任一项所述的方法，其中所述树脂(4)选自：聚硅氧烷树脂、聚硅氮烷树脂、聚碳硅氧烷树脂、聚碳硅烷树脂以及这些树脂的混合物。
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