CN115697941B - 使用杂化交联共聚物制造复合材料部件的方法 - Google Patents

使用杂化交联共聚物制造复合材料部件的方法 Download PDF

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CN115697941B
CN115697941B CN202180041738.0A CN202180041738A CN115697941B CN 115697941 B CN115697941 B CN 115697941B CN 202180041738 A CN202180041738 A CN 202180041738A CN 115697941 B CN115697941 B CN 115697941B
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CN115697941A (zh
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M·F·H·施密特
S·J-C·伯纳德
N·易柏灵福克斯
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French National Academy Of Sciences
Universite de Montpellier I
Ecole Nationale Superieure de Chimie de Montpellier ENSCM
Universite de Bordeaux
Safran Ceramics SA
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French National Academy Of Sciences
Universite de Montpellier I
Ecole Nationale Superieure de Chimie de Montpellier ENSCM
Universite de Bordeaux
Safran Ceramics SA
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Abstract

本发明涉及制造由复合材料制备的部件，其基质至少部分地通过杂化交联共聚物热解而形成，所述杂化交联共聚物产生具有低游离碳含量和改进的性质的基质。

Description

使用杂化交联共聚物制造复合材料部件的方法
技术领域
本发明涉及制造由具有至少部分陶瓷基质的复合材料制备的部件的方法，所述部件具有改进的机械性能。
背景技术
由具有至少部分陶瓷基质的复合材料制成的部件通常可以通过聚合物浸渍和热解(PIP)技术获得。
根据该技术，将包含陶瓷前体聚合物的液体组合物引入纤维预制件的孔中。然后使如此引入的组合物进行聚合，然后热解，以形成陶瓷基质相。根据所用前体的选择，可以通过该方法形成各种类型的陶瓷基质。具体来说，可以使用聚硅氮烷聚合物以获得碳氮化硅基质(SiCN)、使用聚碳硅烷聚合物以获得碳化硅基质(SiC)或使用聚硅氧烷聚合物以获得碳氧化硅基质(SiCO)。
通常连续几次重复这些渗透和热解循环，以获得致密化部件的所需孔隙率水平，因为通过热解转化为陶瓷涉及体积收缩。
通过热解市售前体获得的基于碳化硅或碳氮化硅的基质可以显示出游离碳。游离碳的存在会影响陶瓷基质的抗氧化性，并且游离碳会与任选存在的氮化硅反应，导致氮的损失，引起材料的质量损失和孔隙产生，从而在高于1450℃的温度下改变基质的性质。
因此，希望有新的解决方案来改善由复合材料制成的部件所表现出的性能，所述复合材料的基质已经通过PIP技术至少部分形成。还需要改进由PIP技术在氧化介质中和/或高于1450℃的温度下所形成的基质的性能。
发明内容
本发明的第一方面涉及一种用于制造由复合材料制成的部件的方法，所述方法至少包括：
-通过交联共聚物陶瓷前体的热解，在纤维预制件的孔中形成陶瓷基质相，所述交联共聚物包含具有游离碳的第一陶瓷的第一前体大分子链和具有游离硅的第二陶瓷的第二前体大分子链，所述第一大分子链通过包含式*1-X-*2的结合结构的交联桥结合至所述第二大分子链；在该式中，X表示硼或铝，-*1表示与第一大分子链的键，-*2表示与第二大分子链的键。
本发明提出通过使杂化共聚物热解来形成陶瓷基质相，所述杂化(hybrid)共聚物包括旨在形成呈现游离碳的第一陶瓷的第一大分子链和旨在形成呈现游离硅的第二陶瓷的第二大分子链的组合。第一大分子链和第二大分子链各自对应于本身已知的树脂。本发明提出将其组合，以通过与第二陶瓷的游离硅反应来消耗第一陶瓷的游离碳，从而改进部件的性能，特别是抗氧化性。此外，与单独使用第一大分子链和第二大分子链相比，交联共聚物的使用使得有可能提高热解后的陶瓷产率。在本发明中，第一大分子链和第二大分子链通过包含原子X的交联桥成键，原子X的掺入使得有可能进一步改进陶瓷基质相性质，这将在下文中进行描述。
在示例性实施方式中，X是硼。
在热解后获得的陶瓷基质相中掺入硼使得可以通过形成热稳定无定形陶瓷进一步提高基质在高于1450℃温度下的耐热性。
或者，X是铝。
在热解后获得的陶瓷基质相中掺入铝使得可以进一步改进所获得陶瓷基质相的耐氧化性和耐腐蚀性。
在一个实施方式中，交联共聚物的形成包括：通过第一大分子链与第二大分子链所携带的反应性官能团与包含X-H键的路易斯络合物或路易斯酸交联剂反应使这些链交联，该反应在原子X处发生。
在该情况下，在链已经处于大分子状态且已经聚合时，进行交联。
或者，交联共聚物的形成包括：包含X-H键的路易斯络合物或路易斯酸交联剂与旨在形成第一大分子链和第二大分子链的单体或低聚物所携带的反应性官能团反应，该反应在原子X处发生；以及所述单体或低聚物聚合。
在该情况下，在链是不完全聚合时，进行交联。
无论考虑哪个示例，路易斯络合物或酸包含X-H键，所述X-H键能够与反应性官能团发生化学反应。在这些反应之后，原子X共价结合至大分子链，并在这些链之间形成交联桥，如上文所述。
具体来说，交联剂可以与至少一种第一反应性官能团和至少一种第二反应性官能团反应，所述第一反应性官能团选自下组：碳碳双键、CH3基团或C-OH基团，第二反应性官能团选自下组：N-H基团、Si-H基团或Si-OH基团。
第一反应性官能团可以属于第一大分子链或旨在形成该第一链的单体或低聚物，第二反应性官能团可以属于第二大分子链或旨在形成该第二链的单体或低聚物。
具体来说，第一反应性官能团是碳碳双键，例如，属于烯丙基或乙烯基，并且第二反应性官能团是N-H基团或Si-H基团。
在一个实施方式中，交联剂是包含式B1-XH2的反应性结构的路易斯络合物，其中，B1是路易斯碱。
具体来说，交联剂可以是通式为B1-BH3或B1-AlH3的路易斯络合物。
路易斯碱B1可以具有式*-S-R2或*-N-R3，并且*-表示与原子X的键，并且在这些式的每一个中，R基团是相同或不同的，并且是具有1至12个碳原子(例如，1至4个碳原子)的饱和或不饱和烃链，或者B1可以是具有1至12个碳原子(例如，1至4个碳原子)的脂肪族或芳香族烃链。R基团可以具体选自：甲基基团或乙基基团。B1可以是具有1至12个碳原子、例如1至4个碳原子的线性或支化烃链。
具体来说，交联剂可以是具有下式的硼烷二甲硫醚：
[式1]
具体来说，交联剂可以是具有下式的N,N-二甲基乙基醛烷胺络合物(Alane N-Ndimethylamine)：
[式2]
具体地，交联剂是通式为R’-BH2或R’-AlH2的路易斯酸，在这些式的每一个中，R’基团是氢原子或具有1至12个碳原子(例如1至4个碳原子)的饱和或不饱和烃链。
在一个实施方式中，第一大分子链和第二大分子链彼此独立地选自：聚硅氧烷、聚硅氮烷、聚碳硅氧烷、聚碳硅烷、聚碳硅氮烷或这些树脂的混合物。
附图说明
[图1]图1示意性显示了在本发明范围内可以实施的形成交联共聚物的步骤。
[图2]图2示意性显示了在本发明范围内可以实施的形成交联共聚物的步骤。
[图3]图3示意性显示了在本发明范围内可以实施的形成交联共聚物的步骤。
[图4]图4是对在本发明范围内可实施的交联共聚物的陶瓷产率与构成交联共聚物的各大分子链热解后获得的陶瓷产率进行比较的测试结果。
[图5]图5是对在本发明范围内可实施的由交联共聚物获得的陶瓷的热稳定性与构成交联共聚物的各大分子链热解后获得的陶瓷的热稳定性进行比较的测试结果。
具体实施方式
形成待获得部件的纤维增强件的纤维预制件可由耐火纱线(例如陶瓷或碳纱线)制成。例如，预制件可以由如下物质形成：由日本供应商NGS提供的名称为“Nicalon”、“Hi-Nicalon”或“Hi-Nicalon S型”的碳化硅纱线。可用于形成该预制件的碳纱线例如由日本东丽株式会社(Toray)以名称Torayca T300 3K提供。
纤维预制件由至少一种纺织操作获得。纤维预制件可以具体通过多层或三维编织来获得。术语“三维编织”或“3D编织”应理解为是指至少一些经纱在多个纬纱层上将纬纱连接在一起的编织方法。经线和纬线的角色在本说明书中可以互换，并且同样应当视为被权利要求所涵盖。
例如，纤维预制件可以具有多缎纹编织，换言之，其可以是通过用多层纬线三维编织获得的织物，其中，各层的基础编织等同于常规缎纹型编织，但是编织的某些点与纬线层结合在一起。或者，纤维预制件可以具有互锁编织。术语“互锁编织或织物”应理解为是指三维编织，其中，经纱的各层与多层纬纱连接，其中，相同经列中的所有纱线在编织平面中同样地移动。可以用于形成纤维预制件的各种多层编织方法见述于文件WO 2006/136755。
还可以首先形成纤维织构，例如二维织物或单向片(即，由基本沿相同方向延伸的纱线形成)，并通过在成形器上覆盖这种纤维织构来获得纤维预制件。这些织构可以任选地结合在一起，例如，通过缝纫或植入纱线结合在一起，从而形成纤维预制件。
然后可以在预制件的纱线上形成涂层。该涂层可以是中间相和/或包括使纤维预制件部分致密化的一个或多个基质相。涂层可以由碳制成，特别是由PyC、硼掺杂的碳(BC，硼的原子比例为5％至20％，余量为碳)制成，或者由陶瓷材料制成，例如，碳化硅、氮化硼(BN)、硅掺杂的氮化硼(BN(Si)，硅的质量比例为5％至40％，余量为氮化硼)或氮化硅(Si3N4)。
涂层可以包括单层或多层中间相。该中间相可以包括至少一层热解碳、氮化硼、硅掺杂的氮化硼或硼掺杂的碳。
此处，中间相对复合材料具有去脆(de-embrittlement)功能，促进在基质中传播后到达中间相的可能裂纹偏转，防止或延迟由于该裂纹导致的纱线断裂。
中间相的厚度可以为10nm至1000nm，例如，10nm至100nm。中间相可以通过在预制件纱线上进行化学气相渗透来形成。
或者，在形成预制件之前，可以通过化学气相沉积在纱线上形成中间相，然后由以这种方式涂覆的纱线形成该预制件。
或者，涂层可以包含至少一个初步基质相和任选地插入所述至少一个初步基质相和纱线之间的中间相。初步基质相可以通过各种已知方法形成，例如，化学气相渗透、硅熔体渗透或PIP技术。初步基质相可以是陶瓷的或由碳制成。初步基质相可以由碳制成，或者甚至由PyC制成、由碳化硅、氮化硼或氮化硅制成。
当然，纤维预制件在涂层形成后保持多孔，以允许通过交联共聚物的热解形成陶瓷基质相，如上文所述。现在将结合图1至图3描述可在本发明范围内使用的交联共聚物的形成示例。
构成第一大分子链和第二大分子链的树脂(在图1至3中表示为C1和C2)可以在液体状态下进行混合。然后可以将交联剂10添加到该混合物中。图1至3涉及包含硼的交联剂的情况，但是相同的原理适用于该交联剂包含铝的情况。
交联剂10与第一反应性官能团R1反应，此处其包括由第一大分子链C1携带的碳碳双键，如图1所示。根据该示例，第一链C1具有反应性烯丙基；具有碳碳双键的反应性基团的其它示例也是可行的，例如乙烯基基团。第一大分子链C1在热解后产生具有游离碳的第一陶瓷，例如原子含量大于或等于5％，例如5％至20％。第一陶瓷可以是碳化硅、碳氮化硅或氮化硅。第一大分子链C1可以包含硅和碳，并且Si/C的原子比小于1，换言之，碳的原子含量大于硅的原子含量。
在包含碳碳双键的第一反应性官能团R1的情况下，其可以产生交联剂10的B-H键和C-C双键之间的自由基加成反应，以及路易斯碱B1的损失。B1可以如上文所述。因此，在大分子链C1和交联剂10之间获得共价键B-C。构成具有碳碳双键形式的反应性官能团的第一大分子链C1的树脂的示例包括：聚碳硅烷树脂，例如Systems以名称“SMP-10”销售的树脂；或聚硅氮烷树脂，例如默克公司(Merck)以名称“Durazane 1800”或以名称“HTT1800”销售的树脂。
已与第一反应性官能团R1反应的交联剂20具有能够与由第二大分子链C2携带的第二反应性官能团R2反应以与其结合的至少一个其它B-H键(参见图2)。根据该示例，第二链C2具有反应性官能团R2，Si-H，其可以替代地或额外地具有反应性官能团N-H。第二大分子链C2在热解后产生具有游离硅的第二陶瓷，例如原子含量大于或等于5％，例如5％至20％。第二陶瓷可以是碳化硅或氮化硅。第二大分子链C2可以包含硅和碳，并且Si/C的原子比大于1，换言之，硅的原子含量大于碳的原子含量。
反应性官能团R2可以通过脱氢偶联反应与交联剂的B-H键反应，以在反应性官能团为Si-H的情况下形成B-Si键，或者在反应性官能团为N-H的情况下形成B-N键。构成第二大分子链C2的树脂的示例包括聚硅氮烷树脂全氢聚硅氮烷(PHPS)，其包含反应性官能团N-H和Si-H两者。
在交联剂10与反应性官能团R1和R2反应后，在大分子链C1和C2之间获得交联桥P，其具有式*1-B-*2的结合结构S，在图3中用虚线框出。结合结构S在大分子链C1和C2之间形成键臂(bond arm)。
例如，相对于第一大分子链C1的摩尔当量，可以使用2至3摩尔当量的第二大分子链C2。通常，相对于第一大分子链的量，交联剂可以0.1至1.2摩尔当量的比例存在于混合物中。
交联可以在环境温度(20℃)下进行。根据一个示例，交联可以包括在-50℃至60℃、如-20℃至30℃的温度下的至少一个步骤，以使交联剂附着至反应性官能团R1和R2中的至少一个。该第一步骤之后可以是在较高温度下(例如大于或等于90℃，例如，90℃至250℃)的第二步，以便终结交联。该交联的持续时间可以大于或等于30分钟，例如30分钟至3天，例如30分钟至5小时。
恰好结合图1至图3描述交联剂10在一个链C1上然后在另一个链C2上的顺序结合，本领域技术人员将认识到这些结合可以同时产生。此外，所示示例涉及已经形成的大分子链C1和C2交联的情况，但如上所述，当在单体或低聚物状态下进行交联时，并未超出本发明的范围。相同的原理也可以应用于路易斯酸形式的交联剂。
该方法可通过如下进行：将交联共聚物注入待获得部件的纤维预制件的孔中，然后使引入预制件中的共聚物热解。获得游离碳原子含量低的陶瓷基质相，该含量例如小于或等于5％，例如小于或等于3％。热解后，可以获得陶瓷基质相Si-B-C-N，其是在1500℃下热稳定的陶瓷。
应注意，也可以在交联结束之前将混合物注入纤维预制件的孔中，并在预制件的孔中在原位进行交联，以获得交联共聚物。其他方法也是可行的，例如，使用混合物或交联共聚物的预浸渍纤维层，然后使这些层覆盖在待获得部件的形式上。无论考虑哪种实施方式，交联共聚物可以基本填充纤维预制件的所有可进入孔。
混合物的形成、交联、将交联共聚物任选注入纤维预制件的孔中以及其热解可以在惰性气氛下进行。
应注意，部件基质的形成可涉及引入混合物或共聚物以及共聚物热解的多个循环的执行。
一旦获得，由此制造的部件可以是用于航空或航天应用的部件。该部件可以是航空或航天发动机或工业涡轮机中的燃气涡轮机的热部件。该部件可以是涡轮机部件。该部件可以构成分配器的至少一部分、喷嘴的至少一部分、或热保护涂层、燃烧室的壁、涡轮环扇区或涡轮机叶片。
实施例
在惰性气氛下由两种市售聚硅氮烷(Durazane 1800，含游离碳的Si-C-N陶瓷前体；以及PHPS，含游离硅的Si3N4陶瓷前体，均由默克公司销售)和硼基交联剂：硼烷二甲基硫醚(BDMS，由西格玛奥德里奇公司(Sigma Aldrich)销售；甲苯中2M)制备混合物。对于1当量Durazane，加入2当量PHPS。首先混合聚合物，然后在添加前以甲苯稀释，然后使用滴液漏斗在℃下进行搅拌时逐滴添加受控量的硼烷二甲基硫醚。对于1当量Durazane，加入0.1当量硼烷二甲基硫醚。
添加后，使温度自然升高至环境温度(20℃)，并且组件在该温度下搅拌3天。然后溶剂在30℃(大部分残余硼烷二甲基硫醚消失)至60℃(大部分甲苯消失)进行提取，在动态真空下保持该温度1小时，以获得交联共聚物。
然后共聚物在氮气下热解，同时使温度升高至1000℃，以转化为Si-B-C-N陶瓷。由于其在热解期间与来自PHPS的游离硅反应，所获得的陶瓷具有约5原子％的低游离碳原子含量。
图4比较了所获得的共聚物(曲线“A”)的陶瓷产率与单独使用PHPS(曲线“B”)和Durazane 1800(曲线“C”)的陶瓷产率。观察到共聚物的陶瓷产率远高于单独使用(而不是组合使用)两种其它聚合物的陶瓷产率。
此外，图5显示了与仅Durazane 1800热解后获得的陶瓷相比，共聚物热解后获得的陶瓷具有改进的热稳定性。共聚物热解后获得的陶瓷在高达1700℃时也不会呈现出任何质量损失效应。
术语“……至……”应理解为包括端值。

Claims (11)

1.一种用于制造由复合材料制成的部件的方法，所述方法至少包括：
-通过交联共聚物陶瓷前体的热解，在纤维预制件的孔中形成陶瓷基质相，所述交联共聚物包含具有游离碳的第一陶瓷的第一前体大分子链(C1)和具有游离硅的第二陶瓷的第二前体大分子链(C2)，所述第一前体大分子链通过包含式*1-X-*2的结合结构(S)的交联桥(P)结合至所述第二前体大分子链；在该式中，X表示硼或铝，-*1表示与第一前体大分子链的键，-*2表示与第二前体大分子链的键。
2.如权利要求1所述的方法，其中，X是硼。
3.如权利要求1或2所述的方法，其中，交联共聚物的形成包括：通过第一前体大分子链(C1)与第二前体大分子链(C2)所携带的反应性官能团(R1；R2)与包含X-H键的路易斯络合物或路易斯酸交联剂(10)反应使这些链交联，该反应在原子X处发生。
4.如权利要求1或2所述的方法，其中，交联共聚物的形成包括：包含X-H键的路易斯络合物或路易斯酸交联剂(10)与旨在形成第一前体大分子链(C1)和第二前体大分子链(C2)的单体或低聚物所携带的反应性官能团反应，该反应在原子X处发生；以及所述单体或低聚物聚合。
5.如权利要求3或4所述的方法，其中，交联剂(10)与至少一种第一反应性官能团(R1)和至少一种第二反应性官能团(R2)反应，所述第一反应性官能团(R1)选自下组：碳碳双键、CH3基团、C-OH基团，第二反应性官能团(R2)选自下组：N-H基团、Si-H基团或Si-OH基团。
6.如权利要求5所述的方法，其中，第一反应性官能团(R1)是碳碳双键，并且第二反应性官能团(R2)是N-H基团或Si-H基团。
7.如权利要求3至6中任一项所述的方法，其中，交联剂(10)是包含式为B1-XH2的反应性结构的路易斯络合物，其中B1是路易斯碱。
8.如权利要求7所述的方法，其中，交联剂(10)是通式为B1-BH3或B1-AlH3的路易斯络合物。
9.如权利要求7或8中任一项所述的方法，其中，路易斯碱B1具有式*-S-R2或*-N-R3，并且*-表示与原子X的键，并且在这些式的每一个中，R基团是相同或不同的，并且是具有1至12个碳原子的饱和或不饱和烃链，或者其中B1是具有1至12个碳原子的脂肪族或芳香族烃链。
10.如权利要求3至6中任一项所述的方法，其中，交联剂是通式为R’-BH2或R’-AlH2的路易斯酸，在这些式的每一个中，R’基团是氢原子或具有1至12个碳原子的饱和或不饱和烃链。
11.如权利要求1至10中任一项所述的方法，其中，第一前体大分子链(C1)和第二前体大分子链(C2)彼此独立地选自：聚硅氧烷、聚硅氮烷、聚碳硅氧烷、聚碳硅烷、聚碳硅氮烷或这些树脂的混合物。
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