CN111226057B - 复合材料摩擦部件的制造方法 - Google Patents

复合材料摩擦部件的制造方法 Download PDF

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CN111226057B
CN111226057B CN201880067714.0A CN201880067714A CN111226057B CN 111226057 B CN111226057 B CN 111226057B CN 201880067714 A CN201880067714 A CN 201880067714A CN 111226057 B CN111226057 B CN 111226057B
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precursor
phase
zro
carbon
matrix
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CN111226057A (zh
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埃里克·布永
阿诺·德勒胡兹
阿曼丁·洛里奥
劳伦斯·梅勒
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Centre National de la Recherche Scientifique CNRS
Safran Ceramics SA
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Abstract

本发明涉及复合材料摩擦部件的制造方法，至少包括以下步骤：用至少包含热解碳和至少一个ZrOxCy相的基体使碳纱的纤维预制件致密化，其中，1≤x≤2且0≤y≤1，基体通过至少由热解碳的第一气相前体和包含锆的第二气相前体进行化学气相渗透形成，所述第二前体是通过将至少一个醇官能团的氧原子连接至通式为‑Zr‑R3基团的改性的一元醇或C1到C6多元醇，取代基R相同或不同，取代基R选自：‑H、C1到C5碳链和卤素原子。

Description

复合材料摩擦部件的制造方法
本发明涉及基于碳/碳(C/C)复合材料的摩擦部件的制造，例如飞行器制动盘。
背景技术
申请文件EP2253604中提出了获得由碳/碳(C/C)复合材料制备的包含陶瓷相的摩擦部件的方法。该摩擦部件磨损量小，具有适于制动应用的摩擦系数并且稳定，尤其是在高能制动时。
该申请中公开的方法包括制备碳纱预制件，用碳基体使预制件致密化并在制造过程中引入分散在部件内的陶瓷晶粒或颗粒。更准确地说，申请文件EP2253604公开了在致密化处理完成之前，用可以分散一种或多种锆化合物的溶胶-凝胶型溶液和/或胶体悬浮液进行浸渍的方法。然后，在最终部件中获ZrOxCy型氧化物至少是主要成分的晶粒或微晶，其中，1≤x≤2且0≤y≤1。
通过申请文件EP2253604中描述的方法所获得的摩擦部件具有良好的性能。另一方面，该方法相较生产全C/C盘的标准工艺更为复杂。事实上，在那份申请文件中，锆基化合物的***是在液相步骤期间进行的，该液相步骤与通过气体致密化(CVI)生产热解碳的步骤完全分离。
具体地，在申请文件EP2253604中公开了在通过CVI用热解碳进行第一步的致密化后，进行锆的***。然后，部件从CVI炉中取出并浸入氧化锆前体土壤中，干燥并进行热处理。然后将该部件重新放入CVI炉中完成热解碳基体的致密化。锆的这种***，与化学气相渗透过程完全分离，导致制造工艺复杂且漫长。
因此，希望能够简化由C/C复合材料制备的包含锆陶瓷相的摩擦部件的制造方法。
发明内容
本发明涉及用复合材料制备摩擦部件的制造工艺，至少包括以下步骤：
-通过至少包括热解碳(PyC)和至少一个ZrOxCy相的基体使碳纱的纤维预制件致密化，其中，1≤x≤2且0≤y≤1，所述基体至少由热解碳的第一气相前体和包含锆的第二气相前体，通过化学气相渗透(CVI)形成，所述第二前体是通过将至少一个醇官能团的氧原子连接至通式为Zr-R3的基团的改性的一元醇或C1-C6多元醇，取代基R相同或不同，且R选自-H，C1到C 5碳链和卤素原子。
一元醇应当被理解为是具有单个醇官能团的化合物。多元醇是指具有多个醇官能团的化合物。
这里使用的第二前体是官能化的一元醇或C1到C6多元醇，该一元醇或C1到C6多元醇的至少一个醇官能团的氧原子被键合有三个取代基R的锆Zr所形成的基团官能化。该前体具有以下通式：CH-O-Zr-R3，其中CH代表一元醇或多元醇的C1到C6碳链，O代表与锆键合的醇官能团的氧原子。
该改性的第二前体一元醇或多元醇有利于通过使用化学气相渗透工艺获得ZrOxCy相。与商用的锆基前体相比，第二前体的优点是其分解温度与传统上应用CVI形成PyC的温度相匹配，从而简化了致密化过程。此外，第二前体成本较低，相较商用锆基前体具有良好的化学稳定性。在特殊情况下，如果在气相中添加氧化剂来氧化第二前体的碳原子的话，上述通式中的y可以是0。这类氧化剂可以是氧气O2或NOX。还可以减少碳输入来降低CVI处理温度，从而使碳不裂化并保留在气相中。
本发明可以通过比现有技术更简单的方式，获得具有理想的摩擦和耐磨损性能的摩擦部件。特别地，可以省去在现有技术中由于只由CVI形成基体而需要在炉中进行卸料和重新填料的步骤。
另外，锆接枝到的一元醇或多元醇是一种可广泛获得的化合物，其可以从再生资源中获得，由此而使得上述第二前体比商业锆前体更容易获得。
在示例性的具体实施例中，致密化包括：
-第一致密化周期，在此期间，由第一前体形成第一热解碳基体相；
-第二致密化周期，在第一周期之后进行，在此期间，至少由第二前体形成包含ZrOxCy相的第二基体相，以及，
-第三致密化周期，在第二周期之后实施，在此期间由第三气相热解碳前体形成与第一前体相同或不同的第三热解碳基体相。
在示例性的具体实施例中，致密化包括至少由气相热解碳前体和第二前体的气相混合物形成热解碳和ZrOxCy相的共沉积。
在示例性的具体实施例中，R选自：-H、C1到C3碳链和卤素原子。
在示例性的具体实施例中，至少一个取代基R是C1到C5或C1到C3碳链或卤素原子。换言之，在此情形下，并非所有连接到锆上的取代基R均为-H。
在示例性的具体实施例中，该方法还包括使形成的ZrOxCy相脱氧的热处理。
在示例性的具体实施例中，ZrOxCy相，可以是脱氧的，在最终部件中的质量含量为0.5％～25％之间，例如，含量为2％～10％。
在具体实施例中，摩擦部件是制动盘。
附图说明
本发明的其他特征和优点将通过以下参照附图的非限制性说明给出，其中：
-图1示出了本发明的第一示例性的方法的不同步骤的流程图；
-图2示出了本发明的第二示例性的方法的不同步骤的流程图。
具体实施方式
以下说明更具体的考虑了基于C/C复合材料的飞行器制动盘的制造，然而，本发明也适用于基于C/C复合材料的其他摩擦部件的生产，例如用于陆地车辆，特别是汽车的制动盘，以及非盘类的摩擦部件，特别是衬垫。
本发明的方法的第一示例性具体实施例由图1示出。
第一步包括：制备用于刹车盘的碳纱预制件(步骤E10)。例如，这样的预制件可以通过在碳前体纱中叠置从纤维织构中切割出的层，用缝针将多个层连接在一起，并通过热处理将前体转化成碳而制备。
可替代地，也可以将碳前体纱的螺旋织物缠绕成叠置的线匝，用缝针将多个线匝连接在一起并通过热处理转化前体。参见例如US 5792715、US 6009605和US 6363593。
可替代地，预制件可以直接地由叠置和结合在一起，例如通过缝针结合在一起的纤维织构的碳纱层制备。
然后进行CVI致密化处理，以通过基体来致密预制件。
为实现该目的，将要致密的纤维预制件放置在CVI反应容器中。可以使用已知的适于形成PyC的反应容器。
在与图1中流程相关联的示例中，致密化包括第一致密化周期，在此期间，由第一前体形成第一PyC基体相(步骤E20)。第一PyC相可以直接地在形成预制件的纱上形成。
在第一致密化周期之后，并且在第二致密化周期开始之前，获得被第一PyC基体相部分致密的预制件。第一PyC基体相可以占据纤维预制件5％到60％的初始孔隙，例如可以占10％到30％。
然后，进行第二致密化周期，在此期间，至少由第二前体形成包含ZrOxCy相的第二基体相(步骤E30)。第二基体相可以直接地在第一PyC基体相上形成。在该示例中，在从第一致密化周期到第二致密化周期的过渡期间，开始向反应容器中引入第二气相前体。
在示例中，第二前体可以是在第二致密化周期期间引入到反应容器中的唯一反应气体(在此情形下未引入PyC前体)。在此情形下，在该第二周期期间仅形成ZrOxCy相。
可替代地，PyC前体和第二前体的混合物可以在第二致密化周期期间引入反应容器。在此情形下，获得共沉积的ZrOxCy相和PyC相。在后一种情况下，PyC前体可以是第一或第三前体，或也可以是不同于第一和第三前提的PyC前体。第二基体相可以占据预制件初始孔隙的1％到10％之间，例如2％到7％之间。
如果需要，可以进行脱氧热处理(可选步骤E40)，以便去除所得的ZrOxCy相中锆和氧之间的至少部分现有键。该处理使得可以调节该相的化学计量。特别地，在脱氧后，ZrOxCy相可以转化成ZrC相。在所示示例中，脱氧热处理在第二致密化周期之后，并且在第三致密化周期开始之前进行。
脱氧热处理本身是一种已知的处理方法。根据将要获得的所需材料的不同，确定在该脱氧处理过程中使用的时间和温度是本领域技术人员的常识的一部分。
在脱氧处理期间施加的温度可高于在基体形成期间遇到的最高温度。
然后进行第三致密化周期，在此期间，由与第一前体相同或不同的第三气相PyC前体形成第三PyC基体相(步骤E50)。第三基体相可以直接在第二基体相上形成，可选地脱氧。在该示例中，在第二致密化周期结束时停止向反应容器中引入第二前体，并且在第三致密化周期中不恢复。
第一和第三前体可以彼此独立地，选自：天然气、甲烷、丙烷、乙醇或这些化合物的混合物。
第二前体可以通过实施已为技术人员所知的有机化学反应，对一元醇或C1到C6多元醇改性，从而将醇官能团的氧原子共价键键合到–Zr-R3基团而获得。这种键合可以通过在锆上对醇官能团的氧原子进行亲核取代来实现。
作为第二种可用前体的示例，可以使用通过将Schwartz试剂(C5H5)2ZrHCl接枝到醇的氧中而改性的一元醇或C1到C6多元醇。该接枝可以通过将醇官能团的氧连接到锆，并从Schwartz试剂中引发氯而发生亲核取代反应来进行。
对于每一种情况，R基可以相同或不同地为：-H、C1到C5碳链，例如，C1到C5烷基或卤素原子。
更具体地，对于每一种情况，R可以相同或不同地为：-H、C1到C3碳链，例如，C1到C3烷基或卤素原子。
更具体地，对于每一种情况，R可以相同或不同地为：-H、甲基或卤素原子。
在示例性的具体实施例中，一元醇或多元醇是C2到C4一元醇或多元醇。该一元醇或多元醇可以具有直链、支链或环链。
在示例性的具体实施方式中，一元醇或多元醇(在经锆键改性前)选自：甲醇，乙醇，乙二醇，丙醇，甘油，丁醇，戊醇，己醇，环丙醇，环丁醇，环戊醇，环己醇或苯酚。特别地，一元醇是乙醇。
在示例中，前体是一种改性的多元醇，每个醇官能团的氧原子可以连接至相同或不同的–Zr-R3基团，其中R如前所述。可替代地，仅某些醇官能团可以被–Zr-R3基团官能化。
本发明可以在已知的适于对PyC进行致密化的CVI装置中实施，该装置包括允许将第二气相前体注入到反应容器中的附加导管。第二前体可以通过已知的在CVI中广泛应用的引入气相前体的方法而引入到反应容器中。
致密化可以在1000℃左右的温度和最好低于5kPa的压力下，在反应容器中进行。这些条件对应于通常使用CVI形成PyC的温度条件和压力条件。
在刚刚结合图1描述的示例中，顺序形成第一PyC基体相、然后是包含ZrOxCy相的第二基体相、然后是第三PyC基体相。因此获得了包括至少第一和第三PyC层和***在第一和第三层之间的包含ZrOxCy相的第二层的顺序化基体。在未示出的变型方法示例中，可以省去该第三基体相的形成。在此情况下，首先形成如上所述的第一PyC基体相，然后形成如上所述的第二ZrOxCy相。因此，预制件的致密化可以通过形成该第二基体相而完成。
下面将结合图2描述本发明的方法的一个变型示例。
在图2的示例中，方法包括：首先形成纤维预制件(步骤E60)，然后致密化该预制件，其至少包括形成PyC和ZrOxCy相的共沉积(E70)。
特别地，可以获得分布在整个基体体积的ZrOxCy夹杂物。这些ZrOxCy夹杂物分散在热解碳基体中。
由第一和第二前体形成的基体可以占据纤维预制件的至少50％或者甚至至少75％的初始孔隙。整个基体可以通过PyC和ZrOxCy相的共沉积来形成。因此，预制件可以通过该共沉积而完全致密化。可替代地，只有基体的一部分可以通过PyC和ZrOxCy相的共沉积来形成，基体的其余部分具有不同的组分。
PyC和ZrOxCy相的共沉积可以具有一致的组分(共沉积相具有均匀的组分)。在此情形下，PyC前体气体和第二锆基前体之间的相对比例在共沉积过程中保持恒定。
可替代地，PyC共沉积和ZrOxCy相的组分可变化。在此情形下，PyC前体气体和第二锆基前体之间的相对比例在共沉积期间发生改变。这种沉积期间相对比例的变化使得可以部分地控制在基体中形成的ZrOxCy相的比例。
如果需要，可以以与上述方式类似的方式，在共沉积之后进行脱氧热处理(步骤E80)。在该脱氧热处理E80之后，可选地，可以进行附加基体相的致密化E90。附加基体相可以是，例如PyC。
上述有关纤维预制件、PyC和ZrOxCy前体以及CVI操作条件的详细信息仍然适用于图2的示例。
注入的PyC前体和第二注入的ZrOxCy前体之间的相对比例决定了最终部件中所得到的ZrOxCy相的质量含量。具体地，ZrOxCy相在最终部件中的含量可以为0.5％到25％之间，或者甚至为2％到10％之间，该相可以经过或可以不经过上述脱氧处理。
应当理解，用语“…到…之间”包括边界。

Claims (9)

1.制造复合材料摩擦部件的方法，至少包括以下步骤：
-用至少包含热解碳和至少一个ZrOxCy相两者的基体使碳纱的纤维预制件致密化，其中，1≤x≤2且0≤y≤1，基体通过至少从热解碳的第一气相前体和包含锆的第二气相前体进行化学气相渗透形成，所述第二前体是通过将至少一个醇官能团的氧原子连接至通式为-Zr-R3基团的改性的一元醇或C1到C6多元醇，取代基R相同或不同，取代基R选自：-H、C1到C5碳链和卤素原子。
2.根据权利要求1的方法，其中，致密化包括：
-第一致密化周期，在此期间，由第一前体形成第一热解碳基体相；
-第二致密化周期，在第一周期之后进行，在此期间，至少由第二前体形成包含ZrOxCy相的第二基体相；以及
-第三致密化周期，在第二周期之后进行，在此期间，由与第一前体相同或不同的第三气相热解碳前体形成第三热解碳基体相。
3.根据权利要求1的方法，其中，致密化至少包括由气相热解碳前体和第二前体的气相混合物形成热解碳相和ZrOxCy相的共沉积。
4.根据前述权利要求1的方法，其中，R选自：-H、C1到C3碳链和卤素原子。
5.根据权利要求1的方法，其中，至少一个取代基R是C1到C5碳链或C1到C3碳链或卤素原子。
6.根据权利要求1的方法，其中，方法进一步包括对形成的ZrOxCy相进行脱氧热处理。
7.根据权利要求1的方法，其中，可选地脱氧的ZrOxCy相在最终部件中质量含量在0.5％到25％之间。
8.根据权利要求7的方法，其中，可选地脱氧的ZrOxCy相在最终部件中质量含量在2％到10％之间。
9.根据权利要求1到8任一项的方法，其中，摩擦部件是制动盘。
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