CN101134678B - 耐高温的复合材料 - Google Patents

耐高温的复合材料 Download PDF

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CN101134678B
CN101134678B CN2007101464501A CN200710146450A CN101134678B CN 101134678 B CN101134678 B CN 101134678B CN 2007101464501 A CN2007101464501 A CN 2007101464501A CN 200710146450 A CN200710146450 A CN 200710146450A CN 101134678 B CN101134678 B CN 101134678B
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graphite
adhesive
layer
carbonization
carbon
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CN101134678A (zh
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K·兴斯特
M·克里斯特
E·埃贝尔
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SGL Carbon SE
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Abstract

本发明涉及耐高温的复合材料，包括至少两个耐高温的碳或石墨基的材料的层。并且所述层通过含有各向异性的扁平石墨颗粒的碳化胶粘剂相互粘合。

Description

耐高温的复合材料
本发明内容是耐高温的复合材料，适用于热绝缘、加热护板、炉内插入件等中。
用于高温炉和高温反应器的结构材料必须是热绝缘的而且还要耐受高温并且相对于炉或反应器内的反应性或释放的物质呈现惰性。由于其很高的耐热性，因此对于高温应用，即在高于800℃甚或高于1000℃的温度下并且在非氧化性气氛中通常使用基于碳或石墨的结构材料。
通过热辐射(主要是在高于1000℃的温度下)以及通过热传导和对流(主要是在低于1000℃的温度下)，可以实现通过绝热而避免热损失。致密的反射性材料一方面适于抑制热辐射和热对流，但另一方面也会随着密度的增加而提高导热性。较小密度的材料也一方面适于抑制热传导，但另一方面又不太合适抑制对流。
因此，优选要由层状复合材料构成绝热体，其含有至少一种用以绝缘热传导的且导热性相对较小的耐高温性材料(例如由碳纤维构成的毡)和第二种用以绝缘热辐射和对流的致密反射性材料(例如石墨箔片)。较为致密的材料还有利于复合材料的机械稳定性。
石墨箔片特别适于作为用于热绝缘的复合材料的成分，因为其是可弯曲和柔韧的，也适用于对于炉和反应器所典型的圆形。另外，石墨箔片的特点也在于其导热性的各向异性。因为在箔片平面内存在优选的热传导，所以可以避免在绝缘体内发生温度平衡和局部过热(热点)的现象。其他优点是有着很小的液体渗透性和石墨箔片的反射性表面。石墨箔片一般具有0.3至1.5cm范围内的厚度和0.4至1.6g/cm3范围内的密度。
已知，通过压缩由热冲击处理膨胀的石墨(膨胀石墨)，可获得石墨箔片。
在WO2004/063612的专利申请中记载了一种绝热复合体，其包括由较高压实的膨胀石墨(密度至少0.4g/cm3，优选0.5至1.6g/cm3)构成的至少一层和由压实不是很高的膨胀石墨(密度小于0.4g/cm3，优选0.05至0.3g/cm3)构成的至少一层，其通过碳化粘结剂(碳化酚醛树脂，沥青或类似物)而相互粘合而成。将由压实较高的膨胀石墨构成的层设置得较薄，能允许机械稳定性和不渗透性方面的要求(一般为0.3至1.5mm)；而由压实不是很高的膨胀石墨构成的层设置得较厚，使得能满足热绝缘的需求(一般在5至20mm之间)。可以将结构构造成夹层形式，并且其中由较高压实的膨胀石墨构成的两个层包围一个由压实不是很高的膨胀石墨构成的层。如此可以抑制颗粒从压实不是很高的层体中析出。
根据WO2004/063612，复合体的制备包括以下几个基本步骤：
·由膨胀石墨制备至少一个压实不是很高和至少一个压实较高的层
·相互粘结各层体，其中
·以可碳化的粘结剂涂覆压实不是很高的层，
·从粘结剂中蒸发可能存在的溶剂，
·将压实较高的层置于涂覆有粘结剂的压实不是很高的层之上和
·通过在非氧化性气氛中和在至少符合所要制备的绝缘材料的使用温度的温度下(一般在800至1000℃之间)热处理，碳化粘结剂。
WO2004/092628公开了一种绝热材料，其含有至少一层石墨箔片或由多层石墨箔片构成的层合体，以及至少一个由在导热性方面各向同性的绝热的碳纤维增强碳材料构成的层。石墨箔片构成的层合体厚度优选为不超过2cm，各向同性的绝缘层厚度为1至10cm而密度优选为0.1至0.5g/cm3。由石墨箔片构成的较内层(即朝向热源的层)能起到反射作用并且抑制局部过热。较外层则由于其密度很小而会减小通过热传导引起的热损失。
将相互之间所要层合的石墨箔片交替地与一层两面都涂覆以可碳化胶粘剂(例如酚醛树脂)的、且在加热时会分解而留下碳残留物的材料(例如牛皮纸)堆叠起来。在中间层分解时所形成的孔隙，允许在胶粘剂固化和碳化过程中释放出的气体排出。利用可碳化的接合剂可以实现将石墨箔片构成的层合体与各向同性的碳纤维增强的碳构成的层相结合。优选所述接合剂除了溶剂和可聚合的单体外还含有所谓的碳颗粒填料，且其体积份数为20至60％。作为合适的碳颗粒，推荐使用粒径小于20μm的碳黑、沥青或研磨的焦炭。在建立石墨箔片层合体与碳纤维增强的碳层之间的结合时，首先要在250℃至300℃的温度下活化接合剂，并接着进一步加热到800℃进行碳化。
对于这种层状复合材料可靠的功能来说关键因素即是由不同材料组成的层间的结合。这种结合必须要保证可靠的连接，但另一方面不允许在所要连接的层间起到显著的热传导作用。
另一问题是由于不同材料的不同热膨胀性而产生了应力。
根据现有技术，都是借助于其中任选还含有碳颗粒作为所谓填料的可碳化胶粘剂来实现材料层之间的连接，并接着进行碳化。
现已发现，如果向可碳化胶粘剂中添加由在其晶体结构和热传导性方面具有很高各向同性的石墨，例如天然石墨或压实的膨胀石墨构成的平面状颗粒，则就能改善不同石墨或碳基结构材料的层之间的连接状况。
本发明的其他一些细节、方案和优点都可以由以下详述的说明内容、附图和实施例给出。
图1所示为圆柱形部件的横截面图，其包括一个卷绕的内层和一个由经压实的膨胀石墨形成的各段接合而成的外层。
与传统诸如经研磨的焦炭的填料不同，根据本发明向可碳化胶粘剂中添加入的颗粒是平面状的，即其平面内的维度尺寸(直径)实质上要大于其厚度。
适于本发明的填料例如是其颗粒呈片状的天然石墨。另一替代品是通过粉碎(切割、研磨、切碎或破碎)由压实为平面结构(例如石墨箔片)的膨胀石墨获得的颗粒。优选为此使用在制备石墨箔片的密封件或其他物件时必然产生的切屑。如此获得的颗粒是小片状的。
根据本发明向可碳化胶粘剂中添加入的颗粒的平均直径在1至250μm之间，优选具有5至55μm平均直径的颗粒。
在本发明加入到可碳化胶粘剂中去的颗粒的两个方案中，即在天然石墨片以及通过石墨箔片的粉碎而获得的小片状颗粒中，存在着典型的能起到适于石墨特点的热传导能力较高各向同性作用的石墨层面结构。沿着层平面，也即在颗粒平面延伸方向内的热传导能力比垂直于层平面方向的高至少10个数量级，优选至少20个数量级。对于石墨箔片，垂直于箔片平面的热传导能力例如只是为约3至5W/K*m，而平行于箔片平面的热传导能力则可以达到约100W/K*m(密度为0.6g/cm3时)至约260W/K*m(密度为1.5g/cm3)之间的值。
因为胶粘剂层中的平面状各向异性的颗粒方向平行于所邻接的材料层，所以越过不同材料之间界面的热传导能力表现得很小。若使用经研磨的焦炭作为填料，则由于焦炭有着更为各向同性的导热性，因此材料层之间的热传导性被抑制得更小。
胶粘剂层中石墨构成的扁平颗粒的又一有益作用是，含有这种颗粒的胶粘剂层可起到应力滑动层的作用，也即减小各种经由胶粘剂层相互粘合起来的材料之间的机械应力。可以假设，这种效应归因于众所周知的石墨的润滑效应，但是本发明不受这种解释的束缚。
颗粒的质量为所用胶粘剂质量的至少5％。特别合适的是颗粒质量为胶粘剂质量的10至30％，但本发明对于颗粒与胶粘剂之间的质量比并不限制在该数值范围内。
作为可碳化的胶粘剂，可以使用现有技术中已知的胶粘剂，如酚醛树脂、呋喃树脂、环氧树脂、沥青或类似物。以本领域普通技术人员公知的方式和方法进行胶粘剂在层状复合材料中的固化、碳化和任选的石墨化过程。固化过程可以例如以已知的真空袋法进行。碳化或石墨化过程以已知方法在800至2000℃的温度下进行。
含有各向异性的扁平石墨颗粒的可碳化胶粘剂适于制备由各种常用于高温应用的碳或石墨材料或其前体构成的层状复合材料，例如由压实的各种密度的膨胀石墨构成的层(包括石墨箔片)、碳纤维-硬质毡、碳纤维-软质毡、碳纤维增强的材料、织物预浸渍体。本发明的复合材料包括至少两个由基于碳或石墨的耐高温材料构成的层。
根据使用目的的不同，本领域普通技术人员可根据其已知的特殊优点而选择合适的材料，并且根据本发明通过含有各向异性的扁平石墨颗粒的可碳化胶粘剂而将其粘结成具有理想层序的层状复合材料，并接着碳化胶粘剂。
所谓碳纤维应理解为是不取决于原材料的各种碳纤维，且其中最为常用的原材料是聚丙烯腈纤维、沥青纤维和纤维素纤维。在碳纤维增强的碳材料中，碳纤维可以例如以单纤维、短切纤维、纤维束、纤维垫、毡、织物或铺置物(Gelege)形式存在，也可以是上述纤维结构的多种的组合。织物可以由长纤维或者由被撕成条又重新纺成的碳纤维(所谓的短切纤维)组成。
由碳纤维构成或以碳纤维增强的材料有益于复合材料的刚性和强度。具有与石墨箔片相比只是压实到密度为0.02至0.3g/cm3的很小密度值的层，例如由碳纤维毡或由膨胀石墨构成的层，会由于其很小的热导性而起到特别的绝热作用。另一个优点是其很小的重量。
将石墨箔片用于绝热等类似用途的特别优点已有描述。
除了石墨箔片外，含有短切纤维的材料也适用于直接界定构成炉、反应器等类似物的内腔的层。由于经过撕条(Streckreiβ)处理，所以这些纤维几乎不会形成可能会污染炉或反应器内腔的粉尘。在例如WO2004/063612中指出了由于使用传统碳纤维增强的热绝缘体构成的细小纤维而会形成粉尘的问题，会导致待绝缘的炉或反应器内腔受到污染。
已知，要以卷绕技术特别构成弯曲的碳纤维增强的层，为此可参见欧洲专利EP1157809。该过程中，将适当时还以可碳化胶粘剂浸渍过的、由碳纤维构成的长的(线、纱、粗纱、带等类似物)和/或平面的纺织结构体(织物、铺置物、毡)卷绕在一个成形的绕卷心轴上。
通过卷绕石墨箔片的幅面可以制得石墨箔片的弯曲层。
在不同材料层之间涂覆一个由含各向异性的扁平石墨颗粒的可碳化胶粘剂构成的层。由于含各向异性的扁平石墨颗粒的胶粘剂有着20000至30000mPa范围内的高粘度，因此其也可以毫无问题地涂覆(例如刷涂)在非水平的平面上，例如涂覆在诸如对于炉、反应器和管典型的并且例如以缠绕技术制得的弯曲表面上。
在对于机械稳定性有着很高要求的部件中，层状复合材料含有优选至少一个设置成交叉缠绕形式的层。对此可理解为，经卷绕的层含有相互之间以相反角度缠绕的层，例如+/-45℃。这些层可以通过卷绕长的纤维结构体，如线、纱、粗纱或带而得到，其中所述的纤维结构体可以用可碳化的胶粘剂浸渍。在接着的碳化或石墨化过程中，碳化或石墨化可能含于经卷绕的纤维结构体中的胶粘剂，从而得到一种碳纤维增强的碳材料(CFC)。
证明有利的是使相互待粘合的表面或至少其上涂覆有胶粘剂的表面粗糙化。
利用含有各向异性的扁平石墨颗粒如天然石墨薄片或者压实的膨胀石墨小片的可碳化胶粘剂，也可以将各个部件，例如耐高温的碳或石墨基结构材料构成的管或片相互粘合成为复杂的部件。
本发明的一个特殊方案涉及的是弯曲部件，例如用于炉或反应器的圆柱形绝热体。优选使用缠绕技术制备它们。但是一些可以考虑的材料，例如压实到密度为0.02至0.3g/cm3的膨胀石墨，并不能灵活地足以通过卷绕相应的材料幅面且并不折断地制得相应材料的层。因此，本发明推荐，将由各个相应材料段构成的弯曲层接合起来。这些片段利用常规的成形技术制得，例如将膨胀石墨在相应于所要制备的片段形状的模具中压制，或者从压制的膨胀石墨块中切割出这些片段。
通过使用其中添加各向异性的扁平石墨颗粒的可碳化胶粘剂，可以如各层之间的连接一样，实现层内的片段之间的连接，接着将胶粘剂固化并碳化。
图1所示为圆柱形部件1的横截面，其包括例如通过缠绕一层石墨箔片到一个绕卷心轴上得到的卷绕内层2，和由压制的膨胀石墨构成的各段3a，3b，3c...接合而成的外层3。在层2和层3之间的界面上以及在备段3a，3b，3c之间的界面上都施涂一层其中添加有各向异性的扁平石墨颗粒的可碳化的胶粘剂。
很明显的，在由片段3a，3b，3c...组合而成的层3上还可涂覆其他层，例如由碳纤维构成的稳定性卷绕体。
实施例
以下推荐一些材料组合体，它们借助于含各向异性的扁平石墨颗粒的可碳化胶粘剂而粘合成为适用于绝热体、加热护板或类似物的层状复合材料。
例举的本发明的第一复合材料包括由石墨箔片构成的热反射内层(朝向炉或反应器的内腔)，由其中膨胀石墨的压实没有石墨箔片高的膨胀石墨构成的抑制热传导的层和由碳纤维增强的碳(CFC)构成的稳定外层。通过碳纤维纱线、纱或粗纱的织物或通过其交叉、例如以角度+/-45°卷绕的层，构成CFC的纤维增强。
例举的本发明的第二复合材料包括由压实的膨胀石墨构成的层和由CFC构成的层。
例举的本发明的第三复合材料包括由两层包围了一层压实不甚高的膨胀石墨层的石墨箔片构成的夹层结构。
表1 中列出了各个材料的典型的厚度和密度。
  材料   厚度/[mm]   密度/[g/cm3]
  石墨箔片   0.25-3   0.4-1.6
  压缩不高的膨胀石墨   2-40   0.02-0.3
  CFC   0.2-0.75   1.15

Claims (16)

1.耐高温复合材料，包括至少两个耐高温的碳或石墨基的材料的层，所述层通过碳化的胶粘剂相互粘合，其特征在于，胶粘剂含有各向异性的扁平石墨颗粒。
2.如权利要求1所述的复合材料，其特征在于，所述至少两个相互粘合的层分别由以下材料之一构成：石墨箔片，压实到密度为0.02至0.3g/cm3的膨胀石墨，碳纤维硬质毡，碳纤维软质毡，碳纤维增强的碳。
3.如权利要求1所述的复合材料，其特征在于，复合材料含有至少一个由压实到密度为0.02至0.3g/cm3的膨胀石墨构成的弯曲层(3)，且弯曲层(3)是由各片段(3a，3b，3c)通过含有各向异性的扁平石墨颗粒的碳化胶粘剂相互粘合而组合成。
4.如权利要求1或3所述的复合材料，其特征在于，各向异性的扁平颗粒是天然石墨的薄片或通过粉碎压实成为扁平结构体的膨胀石墨而得到的颗粒。
5.如权利要求1或3所述的复合材料，其特征在于，各向异性的扁平石墨颗粒的平均直径在1至250μm之间。
6.如权利要求1或3所述的复合材料，其特征在于，各向异性的扁平石墨颗粒内沿着石墨层平面的热传导性要比垂直于石墨层平面的至少高10个数量级。
7.如权利要求1至6任一项所述的复合材料的应用，用于加热护板、热绝缘体、炉内插入件中。
8.耐高温的碳或石墨基材料层或部件的粘合方法，包括以下步骤，
·将其中添加有各向异性的扁平石墨颗粒的可碳化胶粘剂涂覆于应要与第二层或第二部件相粘合的第一层或第一部件的表面上，
·在涂覆有胶粘剂的第一层或第一部件的表面上施加第二层或第二部件，
·固化胶粘剂，
·碳化和/或石墨化胶粘剂。
9.如权利要求8所述的方法，其特征在于，所述至少两个相互粘合的层分别由以下材料之一组成：石墨箔片，压实到密度为0.02至0.3g/cm3的膨胀石墨，硬质毡，软质毡，碳纤维增强的碳。
10.如权利要求9所述的方法，其特征在于，至少一所述层通过卷绕碳纤维的织物结构体或石墨箔片幅面而制得。
11.如权利要求9所述的方法，其特征在于，至少一个要相互粘合的层是由压实到密度为0.02至0.3g/cm3的膨胀石墨构成的弯曲层(3)，且其是由如下步骤构成的：
·制备各片段(3a，3b，3c)，它们组合而成层(3)，
·通过含有各向异性的扁平石墨颗粒的可碳化胶粘剂粘结各片段，
·固化胶粘剂，
·碳化和/或石墨化胶粘剂。
12.如权利要求8所述的方法，其特征在于，要相互粘合的部件是由碳或石墨基材料构成的管或板。
13.如权利要求8或11所述的方法，其特征在于，各向异性的扁平颗粒是天然石墨的薄片或通过粉碎压实成为扁平结构体的膨胀石墨而得到的颗粒。
14.如权利要求8或11所述的方法，其特征在于，各向异性的扁平石墨颗粒的平均直径在1至250μm之间。
15.如权利要求8或11所述的方法，其特征在于，添加到胶粘剂中去的各向异性的扁平石墨颗粒的质量为胶粘剂质量的至少5％。
16.如权利要求8或11所述的方法，其特征在于，各向异性的扁平石墨颗粒内沿着石墨层平面的热传导性要比垂直于石墨层平面的至少高10个数量级。
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