CN115867520A - 使用包括路易斯酸或路易斯络合物的粘附促进剂制造由复合材料制成的部件的方法 - Google Patents
使用包括路易斯酸或路易斯络合物的粘附促进剂制造由复合材料制成的部件的方法 Download PDFInfo
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- CN115867520A CN115867520A CN202180040895.XA CN202180040895A CN115867520A CN 115867520 A CN115867520 A CN 115867520A CN 202180040895 A CN202180040895 A CN 202180040895A CN 115867520 A CN115867520 A CN 115867520A
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Abstract
本发明涉及一种制造由复合材料制成的部件的方法，其中粘附促进剂被接枝到存在于纤维表面上的涂层以及陶瓷前体树脂上。然后，通过聚合树脂(40)的热解，在纤维预制件的孔隙中形成陶瓷基质相。
Description
技术领域
本发明涉及一种制造由复合材料制成的部件的方法，该复合材料具有至少部分陶瓷基质，具有更好的机械性能。
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。
根据这种技术，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隙中。然后将如此引入的组合物聚合，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。特别地，可以使用聚硅氮烷聚合物以获得SiCN基质，使用聚碳硅烷聚合物以获得SiC基质，或使用聚硅氧烷聚合物以获得SiCO基质。
通常连续几次重复这些渗透和热解循环，以获得致密化部件所需的孔隙率水平，因为通过热解转化为陶瓷涉及体积收缩。
具有通过PIP技术获得的基质的部件的机械性能的限制之一，是由于PIP基质的中间相上存在粘附问题。
此外，申请WO 2018/229428是已知的，它披露了使用硅烷粘附促进剂，以改善纤维增强件和陶瓷基质之间的粘附性。
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机械性能，复合材料的基质至少有一部分是通过PIP技术形成的。还希望能改善由PIP技术形成的基质的耐热性，特别是在1500℃左右的温度下。
发明内容
根据第一方面，本发明涉及一种制造由复合材料制成的部件的方法，至少包括以下步骤：
a)将粘附促进剂引入由表面具有-OH基团的涂层涂覆的纱线形成的纤维预制件的孔隙中，所述粘附促进剂是路易斯络合物或路易斯酸，所述路易斯络合物粘附促进剂包含式B1-X-H的反应性结构S1，其中B1是路易斯碱，所述路易斯酸粘附促进剂包含式X-H的反应性结构S2，其中原子X具有空轨道，在这两种选择中，X表示硼或铝，
b)通过在原子X上添加–OH基团，将粘附促进剂接枝到涂层表面，
c)在接枝粘附促进剂的步骤之后，将陶瓷前体树脂引入纤维预制件的孔隙中，
d)聚合引入的树脂，并通过这两种化合物在接枝促进剂的X-H键处的化学反应将接枝的粘附促进剂结合到树脂上，这种聚合和这种结合是通过加热已引入树脂的纤维预制件来进行的，以及
e)通过聚合树脂的热解在纤维预制件的孔隙中形成陶瓷基质相。
具有通过PIP技术获得的基质的部件的机械性能的限制之一，是由于PIP基质的中间相存在粘附问题。事实上，发明人已经观察到聚合状态的陶瓷前体与预先在纱线上形成的涂层之间的脱粘(见图1)。在与图1相关的测试中，涂层是覆盖纱线的热解碳(PyC)中间相层。图2反过来证明了在前体热解后获得的基质相与纱线上预先形成的碳化硅(SiC)涂层之间存在脱粘。由于基质和纤维增强件之间电荷转移的限制，这种脱粘的存在导致所获得部件的机械性能不理想。本发明是为了解决这个问题而开发的，它使用了一种粘附促进剂，该促进剂可以提高PIP基质相与预先形成在纱线上的涂层之间的粘附性。该先前形成的涂层可以是各种类型的，如下所述。
当粘附促进剂是路易斯酸时，它在原子X处包含空轨道，该空轨道旨在由存在于底层涂层表面的悬挂-OH基团的氧的电子填充。因此，在接枝过程中，-OH基团的氧原子和X原子之间形成共价键。应注意，将涂层暴露于环境空气后，–OH基团自然存在。一旦进行了接枝，促进剂的X-H键就能够与树脂发生化学反应。该反应可以将促进剂共价键合到陶瓷前体树脂上。
当粘附促进剂是路易斯络合物时，路易斯碱B1构成在接枝过程中离开的基团。因此，-OH基团的氧原子和X原子之间形成共价键。然后，促进剂的X-H键能够与树脂发生化学反应，就像路易斯酸的情况一样。
因此，粘附促进剂构成了树脂(也就是说，最终是PIP基质)和底层涂层之间的粘合媒介，从而提高了该基质相与该涂层的粘附性。因此，本发明提出的粘附促进剂的使用有助于改善所获得的复合材料部件的机械性能。此外，粘附促进剂与陶瓷前体树脂的反应增加了其交联度和密度，从而增加了该树脂的质量产率并减少了其体积收缩。
在示例性实施例中，X是硼。
这样的特征是有利的，因为它使得可以在热解后在陶瓷基质相中获得硼，从而提高基质的耐热性。特别是，可以获得在1500℃下热稳定的陶瓷基质，例如SiBCN型。
或者，X可以是铝。
为了提高所形成的基质的抗氧化性，这种特征是有利的。
在示例性实施例中，粘附促进剂是通式B1-BH3或B1-AlH3的路易斯络合物。B1可以是例如具有1至12个碳原子，例如1至4个碳原子的脂族或芳族烃链。B1可以是具有1至12个碳原子，例如1至4个碳原子的直链或支链烃链。粘附促进剂可以是路易斯络合物，路易斯碱B1可以具有式*-S-R2或*-N-R3，其中*-表示与原子X的键，并且在这些式中的每一个中，R基团相同或不同，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。
R基团可以特别选自：甲基或乙基。
粘附促进剂可以特别是具有下式的硼烷二甲基硫醚：
【化学式1】
粘附促进剂可以特别是具有下式的铝烷N-N二甲胺：
【化学式2】
或者，粘附促进剂是通式R’2-BH或R’2-AlH的路易斯酸，在这些通式中，R’基团相同或不同，并且是氢原子、含有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，R’基团任选地一起定义同一的环状烃链。在这种情况下，粘附促进剂可以特别是具有下式的9-硼双环[3.3.1]壬烷：
【化学式3】
在一个示例性实施例中，陶瓷前体树脂包含至少一种与步骤d)期间接枝的粘附促进剂的X-H键反应的反应性官能团，其选自：碳-碳双键、N-H基团、Si-H基团和-OH基团。
特别地，反应性官能团可以是烯丙基或乙烯基。
在示例性实施例中，该方法还包括在引入促进剂之前，通过化学气相沉积或化学气相渗透(CVD或CVI)在纱线上形成涂层的步骤。
在这种情况下，涂层可以是中间相或初步基质相。在本实施例中，使用粘附促进剂提高了直接在该涂层上形成的PIP基质相的粘附性。
或者，该方法还包括在引入促进剂之前，通过将前体化合物引入预制件的孔隙中并热解该前体化合物，在纱线上形成涂层的步骤。
在这种情况下，涂层构成初步的PIP基质相，并且使用粘附促进剂提高了两个连续形成的PIP基质块之间的粘附性。应当注意，当基质由多个PIP基质块形成时，可以实施上述方法以改善这些块中的每一个之间的粘附性。
在示例性实施例中，形成涂层表面的材料选自：碳、硼掺杂碳、碳化硅、氮化硼、掺杂硅或氮化硅的氮化硼。
在一个示例性实施例中，树脂选自：聚硅氧烷树脂、聚硅氮烷树脂、聚碳硅氧烷树脂、聚硅烷树脂、聚碳硅氮烷树脂和这些树脂的混合物。
附图说明
图1是显示聚合状态的陶瓷前体与纱线上形成的PyC涂层(不构成本发明的一部分)之间存在脱粘的照片。
图2是显示PIP基质相和纱线上形成的SiC涂层(不构成本发明的一部分)之间存在脱粘的照片。
图3示意性地示出了根据本发明的第一示例性方法的步骤。
图4示意性地示出了根据本发明的第一示例性方法的步骤。
图5示意性地示出了根据本发明的第一示例性方法的步骤。
图6示意性地示出了根据本发明的第一示例性方法的步骤。
图7示意性地示出了根据本发明的第二示例性方法的步骤。
图8示意性地示出了根据本发明的第二示例性方法的步骤。
图9示意性地示出了根据本发明的第二示例性方法的步骤。
图10示意性地示出了根据本发明的第二示例性方法的步骤。
具体实施方式
首先，形成由耐火纱线(例如陶瓷或碳纱线)形成的纤维预制件。
例如，预制件可以由日本NGS公司提供的碳化硅纱线制成，参考号为“Nicalon”、“Hi-Nicalon”或“Hi-Nicalon Type S”。可用于形成该预制件的碳纱线例如由Toray以名称Torayca T300 3K提供。
纤维预制件由至少一次纺织操作获得。纤维预制件旨在形成待获得部件的纤维增强件。纤维预制件可特别通过多层或三维编织获得。
术语“三维编织”或“3D编织”应理解为一种编织方法，通过该方法，至少一些经线在多个纬纱层上连接纬纱。在本说明书中，经纱和纬纱之间的角色颠倒是可能的，并且也应当被认为是权利要求所涵盖的。
纤维预制件可以具有例如多缎纹编织物，换言之，它可以是通过具有多个纬纱层的三维编织而获得的织物，对于这些纬纱层，每层的基本织法相当于传统的缎面织法，但有某些织法点将多层纬纱结合在一起。或者，纤维预制件可以具有互锁编织物。术语“互锁编织物或织物”应理解为指三维编织，其中每层经纱将多层纬纱连接起来，同一经纱列的所有纱线在编织平面中具有相同的运动。文献WO 2006/136755中描述了可用于形成纤维预制件的各种多层编织方法。
还可以首先形成纤维织构，例如二维织物或单向片材，并通过将这种纤维织构覆盖在模板(form)上获得纤维预制件。这些织构可以可选地结合在一起，例如通过缝合或植入纱线以形成纤维预制件。
然后在预制件的纱线上形成涂层。该涂层可以是中间相或包括一个或多个部分致密化纤维预制件的基质相。涂层可由碳、特别是PyC、硼掺杂碳(BC，硼的原子比例在5％和20％之间，其余部分为碳)制成，或由陶瓷材料制成，例如碳化硅、氮化硼(BN)、硅掺杂氮化硼(Si)，硅的质量比例在5％到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，中间相的表面表现出–OH基团，旨在实现粘附促进剂的接枝。该中间相可包括至少一层热解碳、氮化硼、硅掺杂氮化硼或硼掺杂碳。
这里，中间相具有复合材料的去脆化功能，其促进在基质中传播后到达中间相的可能裂纹的转移，防止或延迟纱线因这种裂纹而断裂。
中间相的厚度可以在10nm和1000nm之间，例如在10nm与100nm之间。中间相可以通过CVI在预制件的纱线上形成。
或者，可以在形成预制件之前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，涂层可包含至少一个初步基质相和任选地插入所述至少一个基本基质相与纱线之间的中间相。在这种情况下，外部初步基质相，即离预制件纱线最远的一个，其表面上具有–OH基团，旨在实现粘附促进剂的接枝。
初步外基质相可以通过各种已知的方法形成，例如CVI、硅熔体渗透或通过PIP技术。因此应注意，在后一种情况下，粘附促进剂改善了两个连续PIP基质块之间的粘附。初步外基质相可以是陶瓷或由碳制成。初步外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，以允许形成通过粘附促进剂结合到涂层的PIP陶瓷基质相。现在将借助于图3至图6所示的根据本发明的第一示例性方法来描述这一方面。
在纤维上形成涂层1后，将粘附促进剂10引入纤维预制件的残余孔隙中(见图3)。粘附促进剂10可以以液体状态引入纤维预制件的孔隙中。粘附促进剂10可以注射到纤维预制件的孔隙中。所引入的包括粘附促进剂10的液体介质可以填充纤维预制件的所有可进入的孔隙。引入的粘附促进剂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，即离形成预制件的纱线最远的表面。在所示实施例中，粘附促进剂10是通式B1-BH3的硼基路易斯络合物，其中B1表示路易斯碱。上面已经指出了路易斯络合物的其他可能的例子。为了简洁起见，图中仅显示了硼粘附促进剂，但当促进剂为铝基时，相同的原理仍然适用。
粘附促进剂特别包括式B1-B-H的反应性结构S1。B1-B(硼-路易斯碱键)部分旨在与–OH基团的氧反应，而B-H(硼-氢键)部分旨在和陶瓷前体树脂反应。
可以进行第一次加热，以将促进剂10接枝到涂层1的表面S上。然而，这种加热不是强制性的；将它们在环境温度(20℃)或较低温度下接触可能足以将促进剂接枝到纤维涂层上。接枝过程中施加的温度可以在-50℃和+60℃之间，例如-20℃和+30℃。将促进剂10和–OH基团接触足够长的时间以进行接枝。该持续时间取决于所选促进剂的化学性质。例如，为了进行接枝，可以使促进剂10和-OH基团接触大于或等于2小时，例如大于或等于3小时。粘附促进剂10的引入和接枝可以在惰性气氛或真空下进行。在接枝过程中，硼被添加到–OH基团的氧上，路易斯碱B1离开。接枝促进剂20通过–OH基团的氧和硼之间的共价键结合到涂层1的表面S(见图4)。
接枝后，接枝促进剂20总是具有至少一个悬挂硼氢键(B-H)，用于与陶瓷前体树脂反应(见图4)。
一旦粘附促进剂20被接枝，陶瓷前体树脂4被引入纤维预制件的孔隙中(见图5)。引入的树脂4与接枝促进剂20接触。树脂4可以以液态引入纤维预制件的孔隙中。树脂4可以被注射到纤维预制件的孔隙中。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、聚碳硅氮烷树脂和这些树脂的混合物。
一旦树脂4被引入，它将与接枝促进剂20共价键合。这种结合是由B-H键和树脂4携带的反应性功能之间的化学反应产生的。例如，树脂的反应功能可以是N-H基团，其可以通过脱氢偶联反应与促进剂的B-H键反应以形成B-N键。例如，当树脂是聚硅氮烷树脂时，如Merck公司以参考号“Durazane 1800”销售的树脂。根据另一个实施例，可以使用包含碳-碳双键作为反应功能的树脂，其能够通过硼氢化反应和随后的脱氢偶联与促进剂的B-H键反应以形成B-C键。例如，当树脂是聚碳硅烷树脂时，如
Systems公司以参考号“SMP-10”销售的树脂。无论考虑何种实施例，引入的树脂和接枝的粘附促进剂之间的化学反应可包括脱氢偶联反应，任选地在硼氢化反应之前。
树脂4与接枝促进剂20的结合通过进行第二次加热来进行。第二次加热能够使树脂4聚合并激活其与接枝促进剂20的键的反应。根据本领域技术人员的常识，已知根据所使用的树脂和接枝促进剂20来确定第二次加热期间施加的温度值。在第二次加热期间通常可以施加90℃和250℃之间的温度。
图6显示了聚合树脂40与接枝促进剂30的结合。接枝促进剂30形成聚合树脂40和涂层1之间的键的一个臂。然后将聚合树脂40热解，以便在纤维预制件的孔隙中形成陶瓷基质相。
应注意的是，部件的基质的形成可涉及用于引入和热解陶瓷前体树脂的多个PIP循环的性能。在这种情况下，在每次新引入陶瓷前体树脂之前，可以将粘附促进剂接枝到通过PIP获得的基质块上。在这种情况下，粘附促进剂结合各种PIP基质块，以提高这些块彼此的粘附性。
图7至图10类似于图3至图6，并涉及粘附促进剂100为路易斯酸(此处为BH3)的情况。粘附促进剂100包括式B-H的反应性结构S2，其中B具有由图7中的空矩形示意性表示的空轨道。–OH基团的氧用于填充该空轨道，B-H部分用于与陶瓷前体树脂反应。由此获得促进剂20，将其接枝到涂层1的表面(图8)。图9和图10所示的接枝促进剂20与树脂4的相互作用和反应以与前述相同的方式进行。
一旦获得，由此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或工业涡轮机的燃气轮机的热部件。该部件可以是涡轮发动机部件。该部件可构成分配器的至少一部分、喷嘴的至少一部、或热保护涂层、燃烧室的壁、涡轮机的环形部分或涡轮发动机叶片。
实施例
在浸渍方法期间，纤维预制件在惰性气氛下保持在密封模具中。纤维预制件由涂覆有通过CVI获得的SiC基质的SiC纤维(Hi-Nicalon S)制成。在加入聚合物之前，用受控量的硼烷二甲基硫醚(2M，在甲苯中，Sigma-Aldrich)浸渍纤维预制件。硼烷二甲基硫醚在20℃下与涂层纤维接触12小时，然后将组件置于动态真空下，以去除溶剂，即甲苯，该溶剂在浸入液氮的捕集器中冷凝。在溶剂蒸发后，将模具置于静态真空下，以便用陶瓷前体聚合物(Durazane 1800)浸渍纤维预制件。用聚合物浸渍后，将组件保持在动态真空下，然后置于氩气下，以便在冷却之前进行高达130℃(聚合物固化温度)的热处理，以便将浸渍了聚合物的纤维预制件脱模。
“在......和......之间”的表述应理解为包括边界。
Claims (9)
1.一种制造由复合材料制成的部件的方法，至少包括以下步骤：
a)将粘附促进剂(10；100)引入由表面(S)具有-OH基团的涂层(1)涂覆的纱线形成的纤维预制件的孔隙中，所述粘附促进剂是路易斯络合物或路易斯酸，所述路易斯络合物粘附促进剂(10)包含式B1-X-H的反应性结构S1，其中B1是路易斯碱，所述路易斯酸粘附促进剂(100)包含式X-H的反应性结构S2，其中原子X具有空轨道，在这两种选择中，X表示硼或铝，
b)通过在原子X上添加–OH基，将粘附促进剂接枝到涂层表面，
c)在接枝粘附促进剂的步骤之后，将陶瓷前体树脂(4)引入纤维预制件的孔隙中，
d)聚合引入的树脂，并通过这两种化合物在接枝促进剂的X-H键处的化学反应将接枝的粘附促进剂结合到树脂上，这种聚合和这种结合是通过加热已引入树脂的纤维预制件来进行的，
e)通过聚合树脂(40)的热解在纤维预制件的孔隙中形成陶瓷基质相。
2.根据权利要求1所述的方法，其中X是硼。
3.根据权利要求1或2所述的方法，其中所述粘附促进剂是通式B1-BH3或B1-AlH3的路易斯络合物。
4.根据权利要求1至3中任一项所述的方法，其中所述粘附促进剂(10)是路易斯络合物，其中路易斯碱B1为式*-S-R2或*-N-R3，其中*-表示与原子X结合的键，并且在这些式中的每一个中，R基团相同或不同，是含有1至12个碳原子的饱和或不饱和烃链。
5.根据权利要求1至3中任一项所述的方法，其中所述粘附促进剂(100)是通式R’2-BH或R’2-AlH的路易斯酸，在这些通式中，R’基团相同或不同，并且是氢原子、含有1至12个碳原子的饱和或不饱和烃链，R’基团任选地一起定义同一的环状烃链。
6.根据权利要求1至5中任一项所述的方法，其中所述陶瓷前体树脂(4)包含至少一种与步骤d)期间接枝的粘附促进剂的X-H键反应的反应性官能团，其选自：碳-碳双键、N-H基团、Si-H基团或-OH基团。
7.根据权利要求6所述的方法，其中所述反应性官能团是烯丙基或乙烯基。
8.根据权利要求1至7中任一项所述的方法，其中形成所述涂层(1)的表面(S)的材料选自：碳、硼掺杂碳、碳化硅、氮化硼、掺杂硅或氮化硅的氮化硼。
9.根据权利要求1至8中任一项所述的方法，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、聚碳硅氮烷树脂和这些树脂的混合物。
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| FRFR2005989 | 2020-06-09 | ||
| FR2005989A FR3111136B1 (fr) | 2020-06-09 | 2020-06-09 | Procédé de fabrication d’une pièce en matériau composite à l’aide d’un promoteur d’adhésion comportant un complexe ou un acide de Lewis |
| PCT/FR2021/050998 WO2021250341A1 (fr) | 2020-06-09 | 2021-06-02 | Procede de fabrication d'une piece en materiau composite a l'aide d'un promoteur d'adhesion comportant un complexe ou un acide de lewis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5707471A (en) * | 1991-12-20 | 1998-01-13 | Dow Corning Corporation | Method for making ceramic matrix composites |
| CN101558104A (zh) * | 2006-12-11 | 2009-10-14 | 阿斯特里姆有限公司 | 碳纤维对于有机基质的粘合性的改善方法 |
| CN110944963A (zh) * | 2017-06-13 | 2020-03-31 | 赛峰集团陶瓷 | 一种制造复合部件的方法 |
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| FR2887601B1 (fr) | 2005-06-24 | 2007-10-05 | Snecma Moteurs Sa | Piece mecanique et procede de fabrication d'une telle piece |
| MX2018005793A (es) * | 2015-11-11 | 2018-08-15 | Gates Corp | Tratamiento adhesivo para fibra de reforzamiento de polimeros y productos reforzados. |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5707471A (en) * | 1991-12-20 | 1998-01-13 | Dow Corning Corporation | Method for making ceramic matrix composites |
| CN101558104A (zh) * | 2006-12-11 | 2009-10-14 | 阿斯特里姆有限公司 | 碳纤维对于有机基质的粘合性的改善方法 |
| CN110944963A (zh) * | 2017-06-13 | 2020-03-31 | 赛峰集团陶瓷 | 一种制造复合部件的方法 |
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| US20230192567A1 (en) | 2023-06-22 |
| US11746065B2 (en) | 2023-09-05 |
| EP4161885A1 (fr) | 2023-04-12 |
| FR3111136A1 (fr) | 2021-12-10 |
| WO2021250341A1 (fr) | 2021-12-16 |
| FR3111136B1 (fr) | 2022-06-17 |
| CN115867520B (zh) | 2023-12-26 |
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