CN107073877B - 增强复合材料、制造方法及其制品 - Google Patents

增强复合材料、制造方法及其制品 Download PDF

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Publication number
CN107073877B
CN107073877B CN201580058342.1A CN201580058342A CN107073877B CN 107073877 B CN107073877 B CN 107073877B CN 201580058342 A CN201580058342 A CN 201580058342A CN 107073877 B CN107073877 B CN 107073877B
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carbon
composite material
enhancing
adhesive
metal
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CN107073877A (zh
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赵磊
徐志跃
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Baker Hughes Holdings LLC
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Baker Hughes Inc
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Abstract

本发明提供一种增强复合材料，其包括含有以下中的一种或多种：基于碳纤维的增强材料；基于玻璃纤维的增强材料；或基于金属的增强材料；或基于陶瓷的增强材料；碳复合材料；其中碳复合材料包括碳和粘合剂，粘合剂含有以下中的一种或多种：二氧化硅；硅；硼；三氧化二硼；金属；或金属合金；且其中，金属是以下中的一种或多种：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；镉；或硒。

Description

增强复合材料、制造方法及其制品
相关申请的交叉引用
本申请要求享有2014年11月13日提交的美国专利申请第14/540177号的优先权，该申请的全部内容通过引用并入本文中。
背景技术
石墨是碳的同素异形体，具有分层平面结构。在每一层中，碳原子通过共价键以六边形阵列或网状形式排列。然而，不同的碳层仅通过弱的范德华力而结合在一起。
由于石墨具有极佳的导热性和导电性、明亮度、低摩擦、以及高耐热性和耐腐蚀性，因此已经用于包括电子设备、原子能量、热金属加工、涂料、航空等在内的各种应用中。然而，石墨本质上是一种脆性材料，具有较差的耐受性和抗冲击性。石墨的低强度限制了其在具有较大或复杂负载要求的机械零件中的应用。因此，本行业一直都在接纳具有改善的机械性能的新型石墨材料。如果这种材料还具有改善的耐高温腐蚀性，那将会更加有利。
发明内容
在一个实施例中，通过一种增强复合材料来克服本领域中的上述和其它缺陷，这种增强复合材料包括一种增强材料，其包含有以下中的一种或多种：基于碳纤维的增强材料；基于金属的增强材料；基于玻璃纤维的增强材料或基于陶瓷的增强材料；以及碳复合材料；其中碳复合材料包括碳和粘合剂，该粘合剂含有以下中的一种或多种：二氧化硅；硅；硼；三氧化二硼；金属；或金属合金；且其中，该金属是以下中的一种或多种：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；镉；或硒。还公开了一种含有增强复合材料的制品。
一种用于制造增强复合材料的方法，其包括：将增强材料以及含有碳和粘合剂的组合物交替地布置于模具中，以提供增强组合物；并在约350℃到约1400℃的温度、以及约500psi到约30000psi的压力下对增强组合物进行压缩，以形成增强复合材料。
在另一个实施例中，一种用于制造增强复合材料的方法包括：将增强层叠压到碳复合材料上，以提供增强组合物；并在约350℃到约1400℃的温度、以及约500psi到约30000psi的压力下对增强组合物进行压缩，以形成增强复合材料。
在又一个实施例中，一种用于制造增强复合材料的方法包括：在约350℃到约1400℃的温度、以及约500psi到约30000psi的压力下对包含碳复合材料和增强材料的增强组合物进行压缩，以形成增强复合材料。
附图说明
以下描述无论如何都不应被视为限制。参照附图，相似的元件被相似地标记：
图1是含有在室温和大气压下混合的膨胀石墨和微米或纳米尺寸的粘合剂的组合物的扫描电子显微镜(“SEM”)图像；
图2是根据本发明的一个实施例的由膨胀石墨和微米或纳米尺寸的粘合剂在高压和高温条件下形成的一种碳复合材料的SEM图像；
图3是根据本发明的另一个实施例的碳显微结构的SEM图像；
图4是根据本发明的一个实施例的一种碳复合材料的示意图；
图5示出了根据本发明的一个实施例的增强复合材料的一种制作工艺，其中图5(a)示出了含有波形碳纤维以及石墨和粘合剂组合的增强组合物；图5(b)示出了一种具有交替的碳复合材料层和波形碳纤维层的叠压结构；以及图5(c)示出了一种增强复合材料；以及
图6示出了根据本发明的另一个实施例的用于制造增强复合材料的一种工艺，其中图6(a)示出了一种碳复合材料实心件；图6(b)示出了由图6(a)的实心件铣削而成的颗粒；图6(c)示出了图6(b)的颗粒和碳纤维的组合物；以及图6(d)示出了一种增强复合材料。
具体实施方式
本发明人已经发现，增强复合材料可以由石墨、粘合剂和增强材料形成。增强复合材料具有极佳的耐热性和耐化学性。与传统的石墨材料相比，增强复合材料具有显著提高的结构强度和韧性。进一步，增强复合材料可以被修整以具有各向异性或各向同性机械性能，用于单轴加载或多轴加载应用中。在进一步的有利特征中，增强复合材料保持石墨的各种优异性能，比如明亮度、低热膨胀系数、极佳的耐热冲击性、良好的导热性、耐高温性、润滑性等。
增强复合材料中的碳纤维没有特别的限制，且包含碳纤维丝；碳纤维粗纱；碳纤维纱线；碳纤维丝束；碳纤维带；碳纤维丝带；碳纤维织网；碳纤维管；碳纤维膜；碳纤维编带；织造碳纤维；非织造碳纤维；或碳纤维衬垫。可以使用碳纤维的组合。
高阶纤维形式(比如织造和非织造碳纤维、碳纤维板层、以及碳纤维织网)可以由低阶碳纤维(比如碳丝和碳纤维丝束)形成。在一个实施例中，碳纤维包括具有至少一种高阶纤维形式的碳。在另一个实施例中，碳纤维包括网孔尺寸为约14到约400、约18到约200或约18到约40的织造碳织物。在不受理论束缚的情况下，据信当织造碳纤维织物具有的网孔尺寸在这些范围之内时，用于碳复合材料的粘合剂可以浸润到织造碳纤维中，从而使碳纤维与碳复合材料结合在一起。
碳纤维可以由诸如人造丝、聚丙烯腈(PAN)和沥青等前体形成。人造丝前体是纤维素材料。由人造丝前体形成的碳纤维具有相对较低的碳含量，约为20％，且倾向于具有低强度和刚度。相反，PAN前体提供的碳纤维具有约55％的碳含量，且由于表面缺陷最少，因此具有极佳的抗拉强度。基于石油沥青、煤焦油和聚氯乙烯的沥青前体还可以用于制造碳纤维。在一个实施例中，增强复合材料中的碳纤维由PAN前体形成。
玻璃纤维中所用的最常见类型的玻璃纤维是E型玻璃，其是硼硅酸铝玻璃，具有小于1％重量百分比的碱性氧化物，主要用于玻璃增强塑料。所用的其它类型的玻璃是A型玻璃(碱钙玻璃，含有很少的或不含氧化硼)、E-CR型玻璃(耐电子/化学性；硅酸铝-钙具有小于1％重量百分比的碱性氧化物，具有高耐酸性)、C型玻璃(具有高氧化硼含量的碱钙玻璃，用于玻璃短纤维和绝缘层)、D型玻璃(硼硅酸盐玻璃，因具有低介电常数而命名)、R型玻璃(硅酸铝玻璃，无氧化镁和氧化钙，具有增强所需的高机械要求)、以及S型玻璃(硅酸铝玻璃，无氧化钙，但具有高氧化镁含量，具有高拉伸强度)。在一个实施例中，玻璃纤维包括玻璃纤维织物。
金属纤维是由金属、塑料涂层的金属、金属涂层的塑料、或完全被金属覆盖的芯组成的制造纤维。金属纤维包含铝、青铜、钢、锌、铜、镍、金、银等的纤维。金属纤维还可以由金属丝(钢丝棉)盘绕而成、由较大直径的金属丝捆束拉拔而成、由熔化金属铸造而成、或在晶粒(通常为碳)周围生长而成。基于金属的增强材料可以是纤维、纱线、织网；织物等形式。
基于陶瓷纤维的增强材料包含陶瓷纤维棉，比如碱土硅酸铝棉、铝硅酸棉、以及多晶棉；耐火陶瓷纤维；以及陶瓷纺织物。
根据期望的机械强度，增强复合材料可以包含约0.5到约50wt.％、约0.5到约40wt.％、约1到约40wt.％、或约0.5到约10wt.％、或约1到约8wt.％的碳纤维(基于增强复合材料的总重量)。
增强复合材料中的碳复合材料包括碳和粘合剂。碳可以是石墨。如本文中所用的，石墨包含以下中的一种或多种：天然石墨；合成石墨；可膨胀石墨；或膨胀石墨。天然石墨是天然形成的石墨。其可以分为“鳞片”石墨、“纹理”石墨、以及“无定形”石墨。合成石墨是由碳材料制成的制造品。热解石墨是合成石墨的一种形式。可膨胀石墨是指将插入剂材料插入到天然石墨层或合成石墨层之间的石墨。许多化学品已经被用于插入石墨材料。这些包含酸、氧化剂、卤化物等。示例性的插入剂材料包含硫酸、硝酸、铬酸、硼酸、三氧化硫、或卤化物(比如氯化铁、氯化锌和五氯化锑)。加热时，插入剂由液态或固态转化为气相。气体的形成产生了压力，其将相邻的碳层推开，形成膨胀石墨。膨胀石墨颗粒在外观上呈蠕虫状，因而通常被称为蠕虫。
有利地，碳复合材料包括膨胀石墨。与其它形式的石墨相比，膨胀石墨具有高柔韧性、高压缩恢复性和较大的各向异性。因此，由膨胀石墨和粘合剂形成的复合材料除了具有期望的机械强度以外，还可以具有极佳的弹性。
在一个实施例中，碳复合材料包括碳显微结构，在碳显微结构之间具有间隙；其中，粘合剂布置在至少一些间隙内；以及其中碳显微结构包括碳显微结构内未填充的空隙。
碳显微结构是将石墨压缩到高度凝聚状态后形成的石墨的显微结构。其包括沿压缩方向层叠在一起的石墨基面。如本文中所用的，碳基面是指基本上平坦且平行的碳原子片或层，其中每个片或层具有单一的原子厚度。石墨基面也被称为碳层。碳显微结构通常平坦且薄。其可以具有不同的形状，且可以被称为微薄片、微圆片等。在一个实施例中，碳显微结构基本上彼此平行。
碳复合材料中有两种类型的空隙——碳显微结构之间的空隙或间隙，以及每个单独的碳显微结构内的空隙。碳显微结构之间的间隙的大小为约0.1到约100微米，具体地为约1到约20微米，而碳显微结构内的空隙更小，通常在约20纳米到约1微米之间，具体地为约200纳米到约1微米。空隙或间隙的形状并无特别限制。如本文中所用的，空隙或间隙的大小是指空隙或间隙的最大尺寸，可以通过高分辨率电子或原子力显微镜技术进行确定。
碳显微结构之间的间隙填充有微米或纳米尺寸的粘合剂。例如，粘合剂可以占据碳显微结构之间的间隙的约10％到约90％。在一个实施例中，粘合剂不穿透各个碳显微结构，且碳显微结构内的空隙未填充即不填充任何粘合剂。因此，碳显微结构内的碳层并未被粘合剂锁定在一起。通过这种机制，可以保持碳复合材料尤其是膨胀碳复合材料的柔韧性。在另一个实施例中，为了实现高强度，碳显微结构内的空隙填充有粘合剂。对碳显微结构内的空隙进行填充的方法包含气相沉积。
碳显微结构具有的厚度为约1到约200微米、约1到约150微米、约1到约100微米、约1到约50微米、或约10到约20微米。碳显微结构的直径或最大尺寸为约5到约500微米，或约10到约500微米。碳显微结构的长径比可以为约10到约500、约20到约400、或约25到约350。在一个实施例中，碳显微结构中的碳层之间的距离为约0.3纳米到约1微米。碳显微结构可以具有约0.5到约3g/cm3、或约0.1到约2g/cm3的密度。
在碳复合材料中，碳显微结构通过粘合相保持在一起。粘合相包括通过机械互锁将碳显微结构进行结合的粘合剂。可选地，在粘合剂和碳显微结构之间形成界面层。界面层可以包括化学键、固溶体或其组合。当存在化学键、固溶体或其组合时，可以增强碳显微结构的互锁。应该理解，碳显微结构可以通过机械互锁和化学粘合而保持在一起。例如，化学键、固溶体或其组合可以形成于一些碳显微结构和粘合剂之间，对于特殊的碳显微结构，仅形成于碳显微结构的表面上的一部分碳和粘合剂之间。对于未形成化学键、固溶体或其组合的碳显微结构或碳显微结构的部分，碳显微结构可以通过机械互锁进行粘合。粘合相的厚度为约0.1到约100微米，或约1到约20微米。粘合相可以形成连续的或不连续的网络，其将碳显微结构粘合在一起。
示例性的粘合剂包含非金属、金属、合金、或含有上述至少一种的组合。非金属是以下中的一种或多种：二氧化硅；硅；硼；或三氧化二硼。金属可以是以下中的至少一种：铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；镉；或硒。合金包含以下中的一种或多种：铝合金；铜合金；钛合金；镍合金；钨合金；铬合金；铁合金；锰合金；锆合金；铪合金；钒合金；铌合金；钼合金；锡合金；铋合金；锑合金；铅合金；镉合金；或硒合金。在一个实施例中，粘合剂包括以下中的一种或多种：铜；镍；铬；铁；钛；铜合金；镍合金；铬合金；铁合金；或钛合金。示例性的合金包含钢、镍铬基合金(比如Inconel*合金)以及镍铜基合金(比如蒙乃尔合金)。镍铬基合金可以含有约40-75％的镍和约10-35％的铬。镍铬基合金还可以含有约1到约15％的铁。镍铬基合金中还可以包含少量的钼、铌、钴、锰、铜、铝、钛、硅、碳、硫、磷、硼，或含有上述至少一种物质的组合。镍铜基合金主要由镍(高达约67％)和铜构成。镍铜合金还可以含有少量的铁、锰、碳和硅。这些材料可以是不同的形状，比如颗粒、纤维和丝状。可以使用材料的组合。
用于制造碳复合材料的粘合剂可以是微米或纳米尺寸。在一个实施例中，粘合剂具有的平均粒度为约0.05到约50微米，约1微米到约40微米，具体地为约0.5到约5微米，更具体地为约0.1到约3微米。在不希望受理论束缚的情况下，据信当粘合剂具有这些范围内的尺寸时，其均匀地分散在碳显微结构之间。
当存在界面层的情况下，粘合相包括含有粘合剂的粘合剂层，以及将至少两个碳显微结构中的一个粘合到粘合剂层的界面层。在一个实施例中，粘合相包括粘合剂层、将碳显微结构中的一个粘合到粘合剂层的第一界面层、以及将碳显微结构中的另一个粘合到粘合剂层的第二界面层。第一界面层和第二界面层可以具有相同或不同的组合物。
界面层包括以下中的一种或多种：碳金属键；碳硼键；碳硅键；碳氧硅键；碳氧金属键；或金属碳溶体。这些键由碳显微结构的表面上的碳和粘合剂形成。
在一个实施例中，界面层包括粘合剂的碳化物。碳化物包含以下中的一种或多种：铝的碳化物；钛的碳化物；镍的碳化物；钨的碳化物；铬的碳化物；铁的碳化物；锰的碳化物；锆的碳化物；铪的碳化物；钒的碳化物；铌的碳化物；或钼的碳化物。这些碳化物由对应的金属或金属合金粘合剂与碳显微结构的碳原子发生反应而形成。粘合相还可以包括由二氧化硅或硅与碳显微结构的碳发生反应形成的碳化硅，或由硼或三氧化二硼与碳显微结构的碳发生反应形成的碳化硼。当使用粘合剂材料的组合时，界面层可以包括这些碳化物的组合。碳化物可以是盐类碳化物(比如碳化铝)、共价碳化物(比如碳化硅和碳化硼)、间质碳化物(比如4、5和6组过渡金属的碳化物)、或中间过渡金属碳化物(比如，铬、锰、铁、钴和镍的碳化物)。
在另一个实施例中，界面层包括碳(比如石墨)和粘合剂的固溶体。碳在某些金属基质或在某些温度范围内具有溶解性，这样可以有利于碳显微结构上的金属相的润湿和粘合。通过热处理，可以在低温下保持碳在金属中的高溶解度。这些金属包含以下中的一种或多种：钴；铁；镧；锰；镍；或铜。粘合剂层还可以包括固溶体和碳化物的组合。
基于碳复合材料的总重量，碳复合材料包括约20到约95wt.％、约20到约80wt.％、或约50到约80wt.％的碳。基于碳复合材料的总重量，粘合剂的含量为约5wt.％到约75wt.％、或约20wt.％到约50wt.％。在碳复合材料中，碳相对于粘合剂的重量比率为约1∶4到约20∶1，或约1∶4到约4∶1，或约1∶1到约4∶1。
图1是含有在室温和大气压下混合的膨胀石墨和粘合剂的组合物的SEM图像。如图1中所示，粘合剂(白色区域)仅沉积在一些膨胀石墨蠕虫的表面上。
图2是由膨胀石墨和粘合剂在高压和高温条件下形成的一种碳复合材料的SEM图像。如图2中所示，粘合相(亮区)均匀分布在膨胀石墨显微结构(暗区)之间。
图3中示出了碳石墨显微结构的SEM图像。图4中示出了碳复合材料的一个实施例。如图4中所示，复合材料包括碳显微结构1和将碳显微结构进行锁定的粘合相2。粘合相2包括粘合剂层3和可选的界面层4，界面层4布置在粘合剂层和碳显微结构之间。碳复合材料在碳显微结构之间含有间隙5。碳显微结构内具有未填充的空隙6。可选地，空隙可以被填充。
碳复合材料可以可选地包括填充剂。示例性的填充剂包含炭黑、云母、粘土、玻璃纤维、陶瓷纤维、以及陶瓷空心结构。陶瓷材料包含碳化硅、氮化硅、二氧化硅、氮化硼等。填充剂的含量可以为约0.5到约50wt.％、约0.5到约40wt.％、约1到约40wt.％、或约0.5到约10wt.％、或约1到约8％。
基于增强复合材料的总重量，增强复合材料包含约20wt.％到约99.5wt.％、约30wt.％到约99wt.％、约40wt.％到约99wt.％、约50wt.％到约99wt.％、或约92％到约99wt.％的碳复合材料。
增强复合材料的形式没有特别的限制。在一个实施例中，增强复合材料具有分层结构，并包括第一层(增强层)和布置在第一层上的第二层(碳复合材料层)，其中第一层含有本文所公开的增强材料，第二层包括本文所公开的碳复合材料。应该了解，增强复合材料可以具有一个以上的增强层和一个以上的碳复合材料层。例如，增强复合材料可以包含交替的增强层和碳复合材料层。当采用单轴力制造时，分层的增强复合材料可以具有各向异性特征。
可选地，增强层进一步包括粘合剂，其含有以下中的一种或多种：二氧化硅；硅；硼；三氧化二硼；金属；或金属合金；且其中，该金属是以下中的一种或多种：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；镉；或硒。在不希望受理论约束的情况下，据信在制造过程中，碳复合材料的粘合剂可以渗透到增强层内，从而将增强层与碳复合材料层结合在一起。
增强层和碳复合材料层的厚度没有特别的限制。在一个实施例中，增强层的厚度相对于碳复合材料层的厚度为约10∶1到约1∶10、或约5∶1到约1∶5、或约2∶1到约1∶2。
在另一个实施例中，增强复合材料包括碳复合材料基质以及在基质中分散的增强材料。本实施例的增强复合材料可以由多种随意取向的碳复合材料颗粒制成。因此，这些复合材料可以具有各向同性特征。碳复合材料基质的重量相对于增强材料的重量为约50∶1到约1∶50、约35∶1到约1∶35、约20∶1到约1∶20、或约10∶1到约1∶10。
增强复合材料可以具有任何期望的形状，包括杆状、块状、薄片状、管状、圆柱形坯料状、圆环状、粉末状、珠粒状，或可以加工、形成或以其它方式用于形成有用的制造品的其它形式。这些形式的大小或尺寸没有特别的限制。作为示例，薄片具有的厚度为约10μm到约10cm，宽度为约10mm到约2m。粉末包括平均粒度为约10μm到约1cm的颗粒。珠粒包括的颗粒的平均粒度为约1cm到约5cm。
增强复合材料可以由碳(比如石墨)、粘合剂和增强材料直接制造而成。或者，增强复合材料可以由碳复合材料和增强材料制造而成。
在一个实施例中，在模具内交替地装载增强材料以及含有碳(比如石墨)和粘合剂的组合物，以提供增强组合物。然后，在约350℃到约1400℃的温度、以及约500psi到约30000psi的压力下对增强组合物进行压缩，以形成增强复合材料。图5示出了一种示例性的工艺。如图5中所示，碳纤维织物8以及含有碳(比如石墨)和粘合剂的组合物7被交替地装载到模具(未示出)中，以提供增强组合物，然后对其进行热压，以形成增强复合材料10。
在该组合物中，基于组合物的总重量，碳(比如石墨)的含量为约20wt.％到约95wt.％、约20wt.％到约80wt.％、或约50wt.％到约80wt.％。基于组合物的总重量，粘合剂的含量为约5wt.％到约75wt.％、或约20wt.％到约50wt.％。组合物中的石墨可以是晶片状、粉末状、薄片状、鳞片状等。在一个实施例中，石墨是鳞片的形式，鳞片的直径为约50微米到约5000微米，优选地为约100到约300微米。石墨鳞片可以具有约1到约5微米的厚度。组合物的密度为约0.01到约0.05g/cm3、约0.01到约0.04g/cm3、约0.01到约0.03g/cm3或约0.026g/cm3。可以通过将石墨和微米或纳米尺寸的粘合剂经由本领域已知的任何合适的方法进行混合而形成该组合物。合适的方法的实例包含球磨混合、声混合、螺条混合、立式螺杆混合、以及V型混合。在另一个实施例中，该组合物通过气相沉积制得。“气相沉积”工艺是指通过气相法将材料沉积在基底上的工艺。气相沉积工艺包含物理气相沉积、化学气相沉积、原子层沉积、激光气相沉积、以及等离子体辅助气相沉积。粘合剂前体的实例包含三乙基铝和羰基镍。可以使用物理沉积、化学沉积、以及等离子体辅助气相沉积的不同变型。示例性的沉积工艺可以包含等离子体辅助的化学气相沉积、溅射、离子束沉积、激光烧蚀、或热蒸发。通过气相沉积工艺，粘合剂可以至少部分地填充碳显微结构中的空隙。
在另一个实施例中，一种用于制造增强复合材料的方法包括：将增强层叠压到碳复合材料上，以提供增强组合物；在约350℃到约1400℃的温度、以及约500psi到约30000psi的压力下对增强组合物进行压缩，以形成增强复合材料。当增强复合材料含有一个以上的增强层或者一个以上的碳复合材料层时，该叠压包括对增强层和碳复合材料层的多个交替层进行叠压，以形成增强组合物。图5示出了一种示例性的工艺。如图5中所示，对碳纤维织物9和碳复合材料层8的多个交替层进行叠压，以形成增强组合物，然后对其进行热压或烧结，以形成增强复合材料10。
或者，增强复合材料还可以由碳复合材料和增强材料形成。该方法包含在约350℃到约1400℃的温度、以及约500psi到约30000psi的压力下对增强组合物进行压缩，以形成增强复合材料。用于制造增强复合材料的碳复合材料可以是粉末或珠粒的形式。图6示出了一种示例性的工艺。如图6中所示，碳复合材料固体件11经铣削以形成碳复合材料粉末或颗粒12，其可以与碳纤维13结合，以形成增强组合物。增强组合物可以热压或烧结以形成增强复合材料14。
制造增强复合材料的工艺温度为约350℃到约1200℃，具体地为约800℃到约1200℃。在一个实施例中，该温度为粘合剂的熔点的约±20℃到约±100℃，或者为粘合剂的熔点的约±20℃到约±50℃。在另一个实施例中，该温度高于粘合剂的熔点，比如比粘合剂的熔点高出约20℃到约100℃，或约20℃到约50℃。
可以根据预定的温度安排或升降速率来应用该温度。加热的方式没有特别的限制。示例性的加热方法包含直流(DC)加热、感应加热、微波加热、以及放电等离子体烧结(SPS)。在一个实施例中，经由直流加热进行该加热。可选地，也可以在惰性气体环境中(比如在氩气或氮气中)进行加热。在一个实施例中，增强组合物在含有空气的环境中进行加热。
可以在约500psi到约30000psi、或约1000psi到约5000psi的压力下进行加热。该压力可以是超大气压或接近真空的负压。
所得的增强复合材料可以进一步加工或成形，以形成条状、块状、管状、圆柱形坯料状或螺环状。该加工可以包含使用例如铣床、锯条、车床、修边机、放电加工机床等进行的切割、锯切、烧蚀、铣削、刨削、车削、钻孔等。或者，通过选择具有期望形状的模具，可以将增强复合材料直接模制成可用的形状。
可以经由热轧制造出诸如织物、纸制品、条带、带材、箔、薄毡等薄片材料。在一个实施例中，通过热轧形成的增强碳复合材料薄片可以进一步加热，以使粘合剂与碳显微结构有效地粘合在一起。
可以通过剪切力(切割力)，通过将增强复合材料(例如固体件)进行铣削而制成增强复合材料粉末。注意，增强复合材料不要粉碎。否则，可能破坏碳显微结构中的空隙，从而使碳复合材料失去弹性。
专利申请第14/499397号描述了碳复合材料的制造工艺，其全部内容通过引用而包括于此。
形成碳复合材料的一种方式是对含有碳和微米或纳米尺寸的粘合剂的组合物进行压缩，以通过冷压提供生坯；并对生坯进行压缩和加热，从而形成碳复合材料。在另一个实施例中，可以在常温下对该组合物进行加压，以形成坯块，然后在大气压力下对该坯块进行加热，以形成碳复合材料。这些工艺可以被称为两步法。或者，含有碳和微米或纳米尺寸的粘合剂的组合物可以直接压缩和加热，以形成碳复合材料。该工艺可以被称为一步法。一步法和两步法中所用的组合物可以与制造增强复合材料所用的组合物相同。
参照两步法，冷压意味着在室温或在升温下压缩含有石墨和微米尺寸或纳米尺寸的粘合剂的组合物，只要粘合剂不与石墨显微结构明显粘合。在一个实施例中，生坯中超过约80wt.％、超过约85wt.％、超过约90wt.％、超过约95wt.％、或超过约99wt.％的显微结构未粘合。形成生坯的压力可以为约500psi到约10ksi，温度可以为约20℃到约200℃。这一阶段的减少比率(即生坯的体积相对于组合物的体积)为约40％到约80％。生坯的密度为约0.1到约5g/cm3，约0.5到约3g/cm3，或约0.5到约2g/cm3。
可以在约350℃到约1200℃，具体地在约800℃到约1200℃的温度下加热生坯，以形成碳复合材料。在一个实施例中，该温度为粘合剂的熔点的约±20℃到约±100℃，或者为粘合剂的熔点的约±20℃到约±50℃。在另一个实施例中，该温度高于粘合剂的熔点，比如比粘合剂的熔点高出约20℃到约100℃，或约20℃到约50℃。当温度较高时，粘合剂变得不太粘合，且更易流动，可能需要很小的压力便可将粘合剂均匀地分布到碳显微结构之间的空隙内。然而，如果温度过高，则可能对仪器有不良影响。
可以在约500psi到约30000psi、或约1000psi到约5000psi的压力下进行加热。压力可以是超大气压或接近真空的负压。在不希望受理论约束的情况下，据信当超大气压施加到该组合物时，微米或纳米尺寸的粘合剂通过渗透被迫进入碳显微结构之间的空隙内。当接近真空的负压施加到该组合物时，微米或纳米尺寸的粘合剂通过毛细作用力也可以被迫进入碳显微结构之间的空隙内。
在一个实施例中，形成碳复合材料所期望的压力并非一次全部使用。在装载生坯后，一开始在室温或低温下将第压力施加到组合物，以封闭组合物中的大空隙。否则，熔化后的粘合剂可能流到模具的表面。一旦温度达到预定的最高温度，则可以施加制造碳复合材料所需的期望压力。可以将温度和压力保持在预定的最高温度和预定的最大压力约5分钟到约120分钟。在一个实施例中，预定的最高温度为粘合剂的熔点的约±20℃到约±100℃，或者为粘合剂的熔点的约±20℃到约±50℃。
这一阶段的减少比率(即碳复合材料的体积相对于生坯的体积)为约10％到约70％、或约20到约40％。通过控制压缩程度可以改变碳复合材料的密度。碳复合材料具有的密度为约0.5到约10g/cm3、约1到约8g/cm3、约1到约6g/cm3、约2到约5g/cm3、约3到约5g/cm3、或约2到约4g/cm3。
或者，依然参照两步法，可以首先在室温和约500psi到30000psi的压力下对组合物进行加压，以形成坯块；可以在约350℃到约1200℃，具体地在约800℃到约1200℃的温度下对坯块进一步进行加热，以制造碳复合材料。在一个实施例中，该温度为粘合剂的熔点的约±20℃到约±100℃，或者为粘合剂的熔点的约±20℃到约±50℃。在另一个实施例中，该温度可以比粘合剂的熔点高出约20℃到约100℃、或约20℃到约50℃。可以在大气压下进行加热。
在另一个实施例中，碳复合材料可以直接由石墨和粘合剂的组合物制成，无需制造生坯。加压和加热可以同时进行。合适的压力和温度可以与本文中所述的两步法的第二步的压力和温度相同，以制造碳复合材料。
热压是同时施加温度和压力的工艺。在一步法和两步法中均可用其来制造碳复合材料。热压还可以用于制造增强复合材料的工艺中。
增强复合材料具有许多有利的性能，适用于多种应用。在一个特别有利的特征中，通过形成碳复合材料，碳(比如石墨)的机械强度大大提高。
除了机械强度和弹性外，增强复合材料在高温下还可以具有极佳的热稳定性。增强复合材料可以具有高耐热性，工作温度范围为从约-65°F直至约1200°F，具体地为直至约1100°F，更具体地为直至约1000°F。
增强复合材料在高温下还可以具有极佳的耐化学性。在一个实施例中，增强复合材料化学地耐受水、油、卤水和酸，耐受率从良好到极佳。在一个实施例中，在湿润条件下，包括在碱性和酸性条件下，增强复合材料可以在高温和高压(比如约68°F到约1200°F、或约68°F到约1000°F、或约68°F到约750°F)下连续使用。因此，当增强复合材料长时间暴露于化学药剂(比如水、卤水、烃、酸(比如盐酸)、溶剂(比如甲苯)等)、甚至在高达200°F的高温以及高压(高于大气压)时，其具有耐溶胀和耐降解性能。
增强复合材料为中硬到超硬，其硬度从肖氏A硬度中的约50直至肖氏D硬度中的约75。
增强复合材料用于制备多种应用的制品，包括但不限于电子、原子能量、热金属加工、涂层、航空、汽车、石油及天然气、以及航海应用。因此，在一个实施例中，制品包括增强复合材料。碳复合材料可以用于形成制品的全部或一部分。
制品可以是承重元件。示例性的制品包含轴承；轴承座；衬套；活塞；或垫环。
制品可以是井下元件。示例性的制品包含密封件、密封孔保护器、刷涂元件保护器、压裂插接件部件、桥塞、压缩衬垫元件(初级密封件)、膨胀衬垫元件(ARC密封件)、O形环、粘结密封件、子弹形密封件、井下安全阀(SSSV)动态密封件、井下安全阀挡板密封件、V形环、垫圈、钻头密封件、或ESP密封件。在一个实施例中，制品是封隔器、密封件或O形环。
本文中公开的所有范围均包括端点，且端点可以彼此独立地组合。本文中所用的后缀“(复数形式)”意指包含所修饰术语的单数和复数形式，因而包含至少一个该术语(比如着色剂(复数形式)包括至少一种着色剂)。“或者”是指“和/或”。“可选的”或“可选地”是指随后描述的事件或情形可发生或可不发生，并且该描述包含事件发生的情形也包括事件不发生情形。本文所使用“组合物”包括共混物、混合物、合金、反应产物等。“及其组合”是指“含有所列项目的一种或一种以上以及可选地含有未列的相似项目”。所有参考通过引用并入本文。
用于描述本发明(尤其是以下权利要求书)的术语“一”、“一个”和“该”以及类似的指代词被解释为包括单数和复数，除非另外指明或上下文中明显矛盾。此外，应该进一步指出，本发明中的术语“第一”、“第二”等不指代任何顺序、数量或重要性，而是用于元素彼此之间的区分。与数量结合使用的修饰语“约”包括所述的数值，并具有上下文所示的含义(例如，它包含与具体的数量的测量值相关的误差程度)。
尽管为了说明的目的而阐述了典型的实施例，但前面的描述不应被认为是对本文的范围的限制。因此，在不背离本发明的精神和范围的情况下，本领域技术人员可以进行各种修改、调整和替换。

Claims (13)

1.一种增强复合材料(10)，其包括：
增强材料，其包括以下中的一种或多种：基于碳纤维的增强材料；基于玻璃纤维的增强材料；基于金属的增强材料；或基于陶瓷的增强材料；以及
碳复合材料；
其中所述碳复合材料包括碳和粘合剂，所述粘合剂含有以下中的一种或多种：二氧化硅；硅；硼；三氧化二硼；硒；金属；或金属合金；且其中，所述金属是以下中的一种或多种：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；或镉，
其中所述碳复合材料包括碳显微结构，其在所述碳显微结构之间具有间隙；其中，所述粘合剂布置在至少一些所述间隙内；且其中所述碳显微结构包括所述碳显微结构内的填充空隙(6)，且所述碳显微结构是将石墨压缩到高度凝聚状态后形成的石墨的显微结构，并且
其中所述增强复合材料包括第一层和第二层；其中所述第一层包括所述增强材料，所述第二层包括所述碳复合材料。
2.根据权利要求1所述的增强复合材料(10)，其中所述基于碳纤维的材料包括以下中的一种或多种：碳纤维丝；碳纤维纱线；碳纤维丝束；碳纤维带；碳纤维管；碳纤维膜；织造碳纤维；非织造碳纤维；或碳纤维衬垫；所述基于金属的增强材料包括以下中的一种或多种：金属纤维；金属纤维纱线；金属纤维网；或金属纤维织物；所述基于玻璃纤维的增强材料包括玻璃纤维织物；以及所述基于陶瓷的增强材料包括以下中的一种或多种：陶瓷织物；陶瓷纤维棉；或耐火陶瓷纤维。
3.根据权利要求1所述的增强复合材料(10)，其中所述基于碳纤维的材料包括以下中的一种或多种：碳纤维丝；碳纤维粗纱；碳纤维丝束；碳纤维丝带；碳纤维网；碳纤维管；碳纤维膜；碳纤维编带；非织造碳纤维；或碳纤维衬垫；所述基于金属的增强材料包括以下中的一种或多种：金属纤维；金属纤维纱线；金属纤维网；或金属纤维织物；所述基于玻璃纤维的增强材料包括玻璃纤维织物；以及所述基于陶瓷的增强材料包括以下中的一种或多种：陶瓷织物；陶瓷纤维棉；或耐火陶瓷纤维。
4.根据权利要求1至3中任一项所述的增强复合材料(10)，其中所述增强材料包括织造的碳纤维，其具有的筛目尺寸为10到400。
5.根据权利要求1至3中任一项所述的增强复合材料(10)，其中所述碳复合材料中的所述碳包括以下中的一种或多种：膨胀石墨；可膨胀石墨；天然石墨；或合成石墨。
6.根据权利要求1至3中任一项所述的增强复合材料(10)，其中所述碳复合材料包括至少两个碳显微结构以及布置在所述至少两个碳显微结构之间的粘合相(2)；且其中，所述粘合相(2)包括所述粘合剂。
7.根据权利要求6所述的增强复合材料(10)，其中所述粘合相(2)包括粘合剂层(3)和界面层(4)，所述界面层(4)将所述至少两个碳显微结构中的一个粘合到所述粘合剂层；且其中所述界面层(4)包括以下中的一种或多种：碳金属键；碳硼键；碳硅键；碳氧硅键；碳氧金属键；或金属碳溶体。
8.根据权利要求1所述的增强复合材料(10)，其中所述第一层进一步包括粘合剂，所述粘合剂含有以下中的一种或多种：二氧化硅；硅；硼；三氧化二硼；硒；金属；或金属合金；且其中，所述金属是以下中的一种或多种：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；或镉。
9.根据权利要求1所述的增强复合材料(10)，其中所述增强复合材料(10)包括交替的第一层和第二层。
10.一种包括权利要求1至9中的任一项所述的增强复合材料(10)的制品。
11.根据权利要求10所述的制品，其中所述制品是轴承；轴承座；衬套；活塞；或垫环。
12.一种制造权利要求1至9中的任一项所述的增强复合材料(10)的方法，所述方法包括：
将增强材料以及包括碳和粘合剂的组合物交替地布置于模具中，以提供增强组合物；以及
在350℃到1400℃的温度、以及500psi到30000psi的压力下对所述增强组合物进行压缩，以形成所述增强复合材料。
13.一种制造根据权利要求1至9中的任一项所述的增强复合材料(10)的方法，所述方法包括：
将增强层叠压到碳复合材料层(8)上，以提供增强组合物；以及
在350℃到1400℃的温度、以及500psi到30000psi的压力下对所述增强组合物进行压缩，以形成所述增强复合材料。
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