CN107108213B - 含有碳复合材料的制品及其制造方法 - Google Patents

含有碳复合材料的制品及其制造方法 Download PDF

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CN107108213B
CN107108213B CN201580053083.3A CN201580053083A CN107108213B CN 107108213 B CN107108213 B CN 107108213B CN 201580053083 A CN201580053083 A CN 201580053083A CN 107108213 B CN107108213 B CN 107108213B
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carbon
binder
microstructures
metal
carbon composite
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CN107108213A (zh
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徐志跃
赵磊
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Baker Hughes Holdings LLC
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Baker Hughes Inc
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    • E21B33/12—Packers; Plugs
    • E21B33/1208—Packers; Plugs characterised by the construction of the sealing or packing means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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Abstract

公开了包括碳复合材料的制品。碳复合材料含有其间具有间隙空间的碳微结构，以及设置在至少一些间隙空间中的粘结剂；其中该碳微结构包括该碳微结构内未填充的空隙。或者，碳复合材料含有至少两个碳微结构；以及设置在该至少两个碳微结构之间的粘结相；其中该粘结相包括以下各者中的一者或多者：SiO2、Si、B、B2O3、金属、或该金属的合金，且其中该金属是以下各者中的至少一者：铝、铜、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅、镉或硒。

Description

含有碳复合材料的制品及其制造方法
相关申请的交叉引用
本申请要求于2014年10月15日提交的美国专利申请No.14/514510的权益，其全部内容通过引用并入本文。
背景技术
石墨是碳的同素异形体，具有层状平面结构。每一层中，碳原子通过共价键排列成六边形阵列或网络。但是，不同的碳层仅通过弱范德华力结合在一起。
由于石墨具有优异的导热性和导电性、质量轻、摩擦系数低以及高耐热性和耐腐蚀性，其已经用于各种应用中，包括电子、原子能、热金属加工、涂层、航空航天等应用。但是，石墨没有弹性，强度低，这可能限制其进一步的应用。因此，行业总是很愿意接受弹性和机械强度都提高的新石墨材料。如果这种材料的耐高温腐蚀性也提高，那么这将是另一个优势。
发明内容
在一个实施例中，一种碳复合材料以及一种包括该碳复合材料的制品克服了现有技术中的上述和其他缺点。在一个实施例中，该制品包括碳复合材料，该碳复合材料含有：碳微结构，这些碳微结构间具有间隙空间；以及设置在至少一些间隙空间中的粘结剂；其中该碳微结构包括碳微结构内未填充的空隙。
在另一个实施例中，该制品包括碳复合材料，该碳复合材料包含：至少两个碳微结构；以及设置在该至少两个碳微结构之间的粘结相；其中该粘结相包括粘结剂，该粘结剂包括以下各者中的一者或多者：SiO2、Si、B、B2O3、金属或该金属的合金，且其中该金属是以下至少一种：铝、铜、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅、镉或硒。
一种形成制品的方法包括：成形碳复合材料或机械加工碳复合材料中的至少一者。
在另一个实施例中，一种形成包括碳复合材料的制品的方法包括：在约350℃至约1200℃的温度和约500psi至约30,000psi的压力下压制含有碳和粘结剂的组合物，以形成制品；其中该粘结剂包括以下各者中的一者或多者：SiO2、Si、B、B2O3、金属或该金属的合金，且其中该金属是以下各者中的至少一者：铝、铜、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅、镉或硒。
在又另一个实施例中，一种形成包括碳复合材料的制品的方法包括：通过压制包括碳和粘结剂的组合物形成压坯；并且加热该压坯以形成制品；其中该粘结剂包括以下各者中的一者或多者：SiO2、Si、B、B2O3、金属或该金属的合金，且其中该金属是以下各者中的至少一者：铝、铜、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅、镉或硒。
一种从环境温度大于750°F的地下位置生产烃的方法包括：采用所述制品中的一者或多者。
一种隔离或封上井筒的方法包括：在井筒中部署包括一个或多个制品的设备。
附图说明
以下说明不应被认为以任何方式限制。参考附图，相同的元件附图标记也相同：
图1是含有在室温和大气压下共混的膨胀石墨和微米或纳米级粘结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由膨胀石墨和微米或纳米级粘结剂在高压和高温条件下形成的碳复合材料的SEM图像。
图3是根据本发明另一个实施例的碳微结构的SEM图像。
图4是根据本发明的一个实施例的碳复合材料的示意图。
图5示出了(A)天然石墨的应力-应变曲线；(B)膨胀石墨的应力-应变曲线；(C)膨胀石墨和微米或纳米级粘结剂的混合物的应力-应变曲线，其中该样品在室温和高压下压制而得；(D)由膨胀石墨和微米或纳米级粘结剂的混合物在高温和低压下压制而得的根据本发明的一个实施例的碳复合材料(也称为“软复合材料”)的应力-应变曲线；以及(E)由膨胀石墨和微米或纳米级粘结剂在高压和高温条件下形成的根据本公开另一个实施例的碳复合材料(也称为“硬复合材料”)的应力-应变曲线。
图6示出了不同负载下碳复合材料的环路试验结果。
图7示出了在室温和500°F下分别进行的碳复合材料的滞后试验的结果。
图8对500℃下暴露于空气5天之前和之后的碳复合材料进行比较。
图9(A)是热冲击后碳复合材料的照片；图9(B)示出了热冲击的条件。
图10A-C对在200°F下暴露于自来水20小时之前(图10A)和之后(图10B)的碳复合材料样品，或者在200°F下暴露于自来水3天之前(图10A)和之后(图10C)的碳复合材料样品进行比较。
图11A-C对在200°F下暴露于15％HCl溶液和抑制剂20小时之前(图11A)和之后(图1B)的碳复合材料样品，或者对在200°F下暴露于15％HCl溶液3天之前(图11A)和之后(图11C)的碳复合材料样品进行比较。
图12示出了碳复合材料在600°F下的密封力松弛试验结果。
具体实施方式
本发明人已经发现，与只含有石墨相比、或与由相同石墨但不同粘结剂形成的组合物相比、或与在室温和大气压或高压下共混的相同石墨和相同粘结剂的混合物相比，由石墨和微米或纳米级粘结剂在高温下形成的碳复合材料的平衡性能提高。新的碳复合材料具有优异的弹性。此外，该碳复合材料在高温下具有优异的机械强度、耐热性和耐化学性。在另一个有益的特征中，复合材料保持了石墨的各种优异性能，例如导热性、导电性、润滑性等等。
在不受理论约束的情况下，普遍认为通过设置在碳微结构中的粘结相实现机械强度的提高。因为碳微结构之间没有力或仅存在微弱的范德华力，所以石墨松散材料只有弱的机械强度。在高温下，微米或纳米级粘结剂液化和/或软化，使得其均匀地分散在碳微结构中。冷却时，粘结剂固化并形成通过机械联锁使碳纳米结构粘结在一起的粘结相。
此外在不受理论约束的情况下，对于机械强度和弹性都提高的复合材料，普遍认为碳微结构本身是堆叠层之间具有空间的层状结构。粘结剂仅在微结构的边界处选择性地锁住它们，而不穿透微结构。因此，微结构内的未粘结层提供弹性，而设置在碳微结构中的粘结相提供机械强度。
碳微结构是将石墨压缩成高凝状态后形成的石墨的微观结构。它们包括沿压制方向堆叠在一起的石墨基面。如本文所用的，碳基面是指基本上扁平、平行的碳原子片或层，其中每片或每层都具有单原子厚度。石墨基面也称为碳层。碳微结构通常是扁平和薄的。它们可以具有不同的形状，并且也可以称为微片，微盘等等。在一个实施例中，碳微结构基本上彼此平行。
在碳复合材料中有两种类型的空隙，即碳微结构中的空隙或间隙空间以及每个单独的碳微结构内的空隙。碳微结构中的间隙空间的尺寸为约0.1至约100微米，具体地约1至约20微米，而碳微结构内的空隙则小得多，通常在约20纳米至约1微米之间，具体地约200纳米至约1微米。空隙或间隙空间的形状没有特别限制。如本文所使用的，空隙或间隙空间的尺寸是指空隙或间隙空间的最大尺寸，并且可以通过高分辨率电子或原子力显微镜技术来确定。
碳微结构中的间隙空间填充有微米或纳米级粘结剂。例如，粘结剂可以占碳微结构中的间隙空间的约10％至约90％。但是，粘结剂不渗各个碳微结构，碳微结构中的空隙没有填充，即没有填充任何粘结剂。因此碳微结构中的碳层没有通过粘结剂锁在一起。通过这种机制，可以保留碳复合材料，特别是含有膨胀石墨微结构的碳复合材料的柔韧性。
碳微结构的厚度为约1微米至约200微米，约1微米至约150微米，约1微米至约100微米，约1微米至约50微米，或约10微米至约20微米。碳微结构的直径或最大尺寸为约5微米至约500微米，或者约10微米至约500微米。碳微结构的长宽比可以为约10至约500，约20至约400或约25至约350。在一个实施例中，碳微结构中碳层之间的距离为约0.3纳米至约1微米。碳微结构的密度可以为约0.5g/cm3至约g/cm3，或约0.1g/cm3至约2g/cm3。
如本文所使用的，石墨包括以下一种或多种：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。它可以分为“片状”石墨、“纹理”石墨和“无定形”石墨。合成石墨是由碳材料制成的制成品。热解石墨是合成石墨的一种形式。可膨胀石墨是指具有插层剂材料的石墨，插层剂材料插入天然石墨或合成石墨的各个层之间。已经使用多种化学品来插入石墨材料。这些化学品包括酸、氧化剂，卤化物等等。示例性插层剂材料包括硫酸，硝酸，铬酸，硼酸，SO3或卤化物(例如FeCl3、ZnCl2和SbCl5)。加热时，插层剂从液态或固态转化为气相。气体生成产生压力，压力推动相邻的碳层分开，从而产生膨胀石墨。膨胀石墨颗粒在外观上呈蠕虫状，因此通常被称为蠕虫。
碳复合材料包括膨胀石墨微结构是有益的。与其他形式的石墨相比，膨胀石墨具有高柔韧性，高压缩回复性和较大的各向异性。因此，由膨胀石墨和微米或纳米级粘结剂在高压和高温条件下形成的复合材料除了具有所需的机械强度外还具有优异的弹性。
在碳复合材料中，碳微结构通过粘结相结合在一起。粘结相包括通过机械联锁使碳微结构结合的粘结剂。任选地，粘结剂和碳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。存在化学键，固溶体或其组合时，它们可以增强碳微结构的联锁作用。应当理解的是，碳微结构可以通过机械联锁和化学键合结合在一起。例如，可以在一些碳微结构和粘结剂之间形成化学键合，固溶体或其组合，或者仅在碳微结构表面上的一部分碳和粘结剂之间形成特定的碳微结构。对于没有形成化学键，固溶体或其组合的碳微结构或碳微结构的一部分，碳微结构可以通过机械联锁来绑定。粘结相的厚度为约0.1微米至约100微米，或约1微米至约20微米。粘结相可以形成使碳微结构结合在一起的连续或不连续的网络。
示例性粘结剂包括非金属，金属，合金或包括前述中的至少一种的组合。非金属是以下一种或多种：SiO2、Si、B或B2O3。金属可以是以下至少一种：铝、铜、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅、镉或硒。合金包括以下一种或多种：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，粘结剂包括以下一种或多种：铜、镍、铬、铁、钛、铜的合金、镍的合金、铬的合金、铁的合金或钛的合金。示例性合金包括钢、镍铬基合金(例如Inconel*)以及镍铜基合金(例如Monel合金)。镍铬基合金可以含有约40-75％的Ni和约10-35％的Cr。镍-铬基合金还可以包含约1至约15％的铁。镍铬基合金中还可以包括少量的Mo、Nb、Co、Mn、Cu、Al、Ti、Si、C、S、P、B或包括前述至少一种的组合。镍铜基合金主要由镍(高达约67％)和铜组成。镍-铜基合金还可以含有少量铁、锰、碳和硅。这些材料可以是不同的形状，例如颗粒，纤维和线材。可以使用这些材料的组合。
用于制备碳复合材料的粘结剂是微米或纳米级的。在一个实施例中，粘结剂的平均粒径为约0.050微米至约10微米，具体地为约0.50微米至约5微米，更具体地为约0.1微米至约3微米。在不受受理论约束的情况下，普遍认为当粘结剂的粒径大小在这些范围内，它均匀地分散在碳微结构中。
当存在界面层时，粘结相包括粘结剂层，该粘结剂层包括粘结剂以及使至少两个碳微结构中的其中之一结合到粘结剂层的界面层。在一个实施例中，粘结相包括粘结剂层，使至少两个碳微结构中的一个结合到粘结剂层的第一界面层，以及使至少两个碳微结构中的另一个结合到粘结剂层的第二界面层。第一界面层和第二界面层可以具有相同或不同的组成。
界面层包括以下一种或多种：C-金属键、C-B键、C-Si键、C-O-Si键、C-O-金属键或金属碳溶液。这些键由碳微结构表面上的碳和粘结剂形成。
在一个实施例中，界面层包括粘结剂的碳化物。碳化物包括以下一种或多种：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。这些碳化物是通过使相应的金属或金属合金粘结剂与碳微结构的碳原子反应而形成。粘结相还可以包括通过使SiO2或Si与碳微结构的碳反应而形成的SiC，或通过使B或B2O3与碳微结构的碳反应而形成的B4C。当使用粘结剂材料的组合时，界面层可以包括这些碳化物的组合。碳化物可以是盐状碳化物(例如碳化铝)，共价碳化物(例如SiC和B4C)，间隙式碳化物(例如第4、5和6族过渡金属的碳化物)或者中间过渡金属碳化物，例如，Cr、Mn、Fe、Co和Ni的碳化物。
在另一个实施例中，界面层包括碳的固溶体，例如石墨和粘结剂。碳在某些金属基质中或在某些温度范围下具有溶解性，这可以促进金属相润湿和结合到碳微结构上。通过热处理，可以在低温下保持碳在金属中的高溶解度。这些金属包括以下一种或多种：Co、Fe、La、Mn、Ni或Cu。粘结剂层还可以包括固溶体和碳化物的组合。
碳复合材料包括，以复合材料的总重量计，约20wt.％至约95wt.％，约20wt.％至约80wt.％，或约50wt.％至约80wt.％的碳。粘结剂的量，以复合材料的总重量计，为约5wt.％至约75wt.％，或约20wt.％至约50wt.％。在碳复合材料中，碳相对于粘结剂的重量比为约1∶4至约20∶1，或约1∶4至约4∶1，或约1∶1至约4∶1。
图1是含有在室温和大气压下共混的膨胀石墨和微米或纳米级粘结剂的组合物的SEM图像。如图1所示，粘结剂(白色区域)仅沉积在一些膨胀石墨蠕虫的表面上。
图2是由膨胀石墨和微米或纳米级粘结剂在高压和高温条件下形成的碳复合材料的SEM图像。如图2所示，粘结相(光区域)均匀分布在膨胀石墨微结构(暗区域)中。
图3示出了碳石墨微结构的SEM图像。图4示出了碳复合材料的一个实施例。如图4所示，复合材料包括碳微结构1以及锁住碳微结构的粘结相2。粘结相2包括粘结剂层3以及任选的设置在粘结剂层3和碳微结构1之间的界面层4。碳复合材料含有碳微结构1之间的间隙空间5。在碳微结构中，存在未填充的空隙6。
碳复合材料可任选地包括填充剂。示例性填充剂包括以下一种或多种：碳纤维、碳黑、云母、粘土、玻璃纤维、陶瓷纤维或陶瓷中空结构。陶瓷材料包括SiC、Si3N4、SiO2、BN等等。填充剂的量可以为约0.5wt.％至约10wt.％或约1wt.％至约8％。
复合材料可以具有任何所需的形状，包括棒，块，片，管，圆柱形坯，圆环，粉末，丸粒或可以机械加工，成形或以其他方式用于形成有用制造品的其他形式。这些形式的大小或尺寸没有特别限制。举例而言，片的厚度为约10微米至约10厘米，宽度为约10毫米至约2微米。粉末包括平均粒径为约10微米至约1厘米的颗粒。丸粒包括平均粒径为约1厘米至约5厘米的颗粒。
形成碳复合材料的一种方式是压制包括碳和微米或纳米级粘结剂的组合，以通过冷压制提供生坯；压制并加热生坯，从而形成碳复合材料。在另一个实施例中，可以在室温下压制该组合以形成压坯，然后在大气压下加热该压坯以形成碳复合材料。这些过程可以称为两步法。或者，可以被压制并直接加热包括碳和微米或纳米级粘结剂的组合，以形成碳复合材料。该过程可以称为一步法。
在该组合中，诸如石墨等碳的量，以复合材料的总重量计，为约20wt.％至约95wt.％，约20wt.％至约80wt.％，或约50wt.％至约80wt.％。粘结剂的量，以复合材料的总重量计，为约5wt.％至约75wt.％，或约20wt.％至约50wt.％。该组合中的石墨可以是碎片，粉末，小片，薄片等形式。在一个实施例中，石墨是薄片形式，碎片的直径为约50微米至约5,000微米，优选地约100至约300微米。石墨薄片的厚度可以为约1微米至约5微米。该组合的密度为约0.01g/cm3至约0.05g/cm3，约0.01g/cm3至约0.04g/cm3，约0.01g/cm3至约0.03g/cm3或约0.026g/cm3。该组合可以通过本领域已知的任何合适的方法使石墨与微米或纳米级粘结剂共混而形成。合适方法的示例包括球磨混合，声混合，带式共混，垂直螺杆混合和V-共混。
参照二步法，冷压意味着包括石墨和微米或纳米级粘结剂组合在常温或高温下压制，只要粘结剂不与石墨微结构明显结合即可。在一个实施例中，在生压坯中，大于约80wt.％，大于约85wt.％，大于约90wt.％，大于约95wt.％，或大于约99wt.％的微结构没有结合。形成生压坯的压力可以为约500psi至约10psi，温度可以为约20℃至约200℃。这个阶段的压缩比，即生坯体积相对于组合体积的体积为约40％至约80％。生压坯的密度为约0.1g/cm3至约5g/cm3、约0.5g/cm3至约3g/cm3、或约0.5g/cm3至约2g/cm3。
生压坯可以在约350℃至约1200℃，具体地约800℃至约1200℃的温度下加热，以形成碳复合材料。在一个实施例中，温度为粘结剂熔点的约±20℃至约±100℃，或粘结剂熔点的约±20℃至约±50℃。在另一个实施例中，温度高于粘结剂的熔点，例如比粘结剂的熔点高约20℃至约100℃或约20℃至约50℃。当温度较高时，粘结剂变得不粘了且流动性更好，使粘结剂均匀地分布在碳微结构中的空隙中所需的压力较少。但是，如果温度太高，可能对仪器造成不良影响。
可以根据预定的温度计划或升温速率来设置温度。加热方式没有特别限制。示例性加热方法包括直流(DC)加热，感应加热，微波加热和放电等离子体烧结(SPS)。在一个实施例中，通过DC加热进行加热。例如，包括石墨和微米或纳米级粘结剂的组合可以用电流充电，电流流过该组合，非常快速地产生热量。任选地，也可以在惰性气氛下进行加热，例如在氩气或氮气气氛下进行加热。在一个实施例中，在有空气存在的情况下加热压坯。
加热可以在约500psi至约30,000psi，或约1000psi至约5000psi的压力下进行加热。压力可以是超大气压或低大气压。在不受理论约束的情况下，普遍认为当向组合施加超大气压时，微米或纳米级粘结剂通过渗透作用被迫进入碳微结构中的空隙。当向组合施加低大气压时，微米或纳米级粘结剂也通过毛细作用被迫进入碳微结构中的空隙。
在一个实施例中，形成碳复合材料所需的压力并非一次性全部施加。加载生压坯后，先在室温或低温下向组合物施加低压，以封闭组合物中的大孔。否则，熔融的粘结剂可能流到模具的表面。一旦温度达到预定的最高温度，就可以施加制造碳复合材料所需的压力。温度和压力可以保持在预定最高温度和预定最大压力下约5分钟至约120分钟。在一个实施例中，预定最高温度为粘结剂熔点的约±20℃至约±100℃，或粘结剂熔点的约±20℃至约±50℃。
这个阶段的压缩比，即碳复合材料体积相对于生压坯体积为约10％至约70％或约20％至约40％。碳复合材料的密度可以通过控制压制程度来改变。碳复合材料的密度为约0.5g/cm3至约10g/cm3，约1g/cm3至约8g/cm3，约1g/cm3至约6g/cm3，约2g/cm3至约5g/cm3，约3g/cm3至约5g/cm3，或约2g/cm3至约4g/cm3。
或者，还参照两步法，首先可以在室温和约500psi至30,000psi压力下压制该组合，以形成压坯；压坯可以进一步在约350℃至约1200℃，具体地约800℃至约1200℃的温度下加热，以制备碳复合材料。在一个实施例中，温度为粘结剂熔点的约±20℃至约±100℃，或粘结剂熔点的约±20℃至约±50℃。在另一个实施例中，温度可以比粘结剂的熔点高约20℃至约100℃或约20℃至约50℃。可以在存在或不存在惰性气氛的情况下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结剂的组合制成，无需制备生压坯。压制和加热可以同时进行。合适的压力和温度可以与本文针对两步法的第二步骤所述的压力和温度相同。
热压是同时施加温度和压力的过程。它在一步法和两步法制备碳复合材料中均可使用。
可以在模具中通过一步法或两步法制备碳复合材料。得到的碳复合材料可以进一步机械加工或成形，以形成棒，块，管，圆柱形坯或圆环。机械加工包括使用例如铣床、锯、车床、铣床、放电加工机床等进行切割、锯切、烧蚀、铣削、面铣、车削、钻孔等。或者，可以通过选择具有所需形状的模具将碳复合材料直接成型为可用的形状。
也可以通过热轧制成诸如网、纸、条、带、箔、垫等片材。在一个实施例中，通过热轧制备的碳复合片材可以进一步加热，以使粘结剂有效地将碳微结构结合在一起。
可通过挤出成型制备碳复合丸粒。例如，首先可以将石墨和微米或纳米级粘结剂的组合装到容器中。然后通过活塞将该组合推入挤出机。挤出温度可以为约350℃至约1200℃或约800℃至约1200℃。在一个实施例中，温度为粘结剂熔点的约±20℃至约±100℃，或粘结剂熔点的约±20℃至约±50℃。在另一个实施例中，挤出温度高于粘结剂的熔点，例如比粘结剂的熔点高约20℃至约50℃。在一个实施例中，通过挤出得到线材，线材可以被切割以形成丸粒。在另一个实施例中，丸粒直接从挤出机得到。任选地，可以对丸粒进行后处理工艺。例如，可以在超过粘结剂熔融温度的炉中加热丸粒，这样如果挤出期间碳微结构没有结合或没有充分结合，那么粘结剂可以将碳微结构结合在一起。
可以通过剪切力(切削力)研磨碳复合材料(例如实心体)来制备碳复合粉末。应注意的是，碳复合材料不应被粉碎。否则，碳微结构中的空隙可能被破坏，因而碳复合材料失去弹性。
碳复合材料具有许多有益性能，可用于多种应用。在一个特别有益的特征中，通过形成碳复合材料，碳(例如石墨)的机械强度和弹性性能都得到提高。
为了说明碳复合材料的弹性能得到提高，图5示出了以下样品的应力-应变曲线：(A)天然石墨，(B)膨胀石墨，(C)膨胀石墨和微米或纳米级粘结剂在室温和大气压下形成的混合物，(D)膨胀石墨和微米或纳米级粘结剂在高温和低压下形成的混合物(“软碳复合材料”)；以及(E)由膨胀石墨和微米或纳米级粘结剂在高压和高温条件下形成的碳复合材料。对于天然石墨，通过在钢模中高压下压制天然石墨来制备样品。膨胀石墨样品(B)也以类似的方式制备。
如图5所示，天然石墨(A)具有非常低的弹性能(应力-应变曲线下的面积)，并且非常脆。膨胀石墨(B)的弹性能和膨胀石墨与微米或纳米级粘结剂在室温和高压下压制形成的混合物的弹性能(C)高于天然石墨(A)的弹性能。相反，与单独使用天然石墨(A)，单独使用膨胀石墨(B)以及膨胀石墨和粘结剂在室温和高压下压制形成的混合物(C)相比，本发明的硬碳复合材料和软碳复合材料物(E和D)表现出明显提高的弹性能。在一个实施例中，本发明的碳复合材料的弹性伸长率大于约4％，大于约6％，或约4％至约40％之间。
图6和图7进一步示出了碳复合材料的弹性。图6示出了不同负载下碳复合材料的环路试验结果。图7分别示出了碳复合材料在室温和500°F下的滞后试验结果。如图7所示，碳复合材料的弹性保持在500°F。
除了机械强度和弹性提高之外，碳复合材料还可以在高温下具有优异的热稳定性。图8对500℃下暴露于空气5天之前和之后的碳复合材料进行比较。图9(A)是热冲击8小时后碳复合材料样品的照片。图9(B)示出了热冲击的条件。如图8和图9(A)所示，在500℃暴露于空气5天后或热冲击后，碳复合材料样品没有任何变化。碳复合材料可具有高耐热性，其工作温度范围从约-65°F高至约1200°F，具体地高至约1100°F，更具体地约1000°F。
碳复合材料在高温下还可以具有优异的耐化学性。在一个实施例中，复合材料对水，油，盐水和酸有化学耐受性，耐受等级从良好至优异。在一个实施例中，碳复合材料可以在包括碱性和酸性条件的湿条件下，在高温和高压下连续使用，温度例如约68°F至约1200°F，或约68°F至约1000°F，或约68°F至约750°F。因此，当暴露于化学试剂(例如水，盐水，烃，诸如HCl等酸，诸如甲苯等溶剂)时，甚至在高达200°F的高温和高压(大于大气压)下，碳复合材料都能耐受膨胀和性能劣化很长时间。在图10A-10C和图11A-11C示出了碳复合材料的耐化学性。图10A-10C对在200°F下暴露于自来水20小时之前和之后的碳复合材料样品，或者在200°F下暴露于自来水3天之前和之后的碳复合材料样品进行比较。如图10所示，样品没有任何变化。图11A-11C对在200°F下暴露于15％HCl溶液和抑制剂20小时之前和之后的碳复合材料样品，或者对在200°F下暴露于15％HCl溶液3天之前和之后的碳复合材料样品进行比较。同样，碳复合材料样品没有任何变化。
碳复合材料具有中等硬度至特强硬度，硬度从约50肖氏A标准至约75肖氏D标准。
作为另一个有益的特征，碳复合材料在高温下具有稳定的密封力。恒定压缩应变下的部件应力衰减被称为压缩应力松弛。压缩应力松弛试验也称为密封力松弛试验，用来测量在两个板之间的压缩作用下密封件或O形密封环所施加的密封力。通过测量作为时间，温度和环境的函数的样品密封力衰减，它提供了用于预测材料使用寿命的确定信息。图12示出了碳复合材料在600°F下的密封力松弛试验结果。如图12所示，碳复合材料的密封力在高温下稳定。在一个实施例中，复合材料样品的密封力在15％应变和600°F下保持约5800psi而没有松弛至少20分钟。
碳复合材料可用来制备用于各种应用的制品，包括但不限于电子，原子能，热金属加工，涂层，航空航天，汽车，石油和天然气以及船舶应用。碳复合材料可用于形成制品的全部或一部分。因此，提供了包括碳复合材料的制品。这些制品包括密封元件，散热或换热元件，或减摩元件。
例示性密封元件包括例如静密封件或动态密封件等密封件、密封座，封隔密封件(例如可回收固井封隔器、抛光孔座封隔器、电缆封隔器)，封隔器，接合片，密封垫，桥塞，填料(例如水泵填料、阀填料等)。可以在不同类型的密封元件中进行重叠。静态密封件是指两个稳定不可移动的部件之间的密封件，包括C形密封环，E形密封环，O形密封环，U形密封环，T形密封环，L形密封环，矩形密封环，方形密封环，X型截面密封环等等。动态密封件没有特别限制，包括在一对相对可移动的构件之间的任何密封件。密封垫是填充两个或两个以上匹配表面之间的空间的机械密封件。示例性密封垫包括耐受压力和热的高性能密封垫，例如，用于汽车的气缸密封垫和排气密封垫，和用于炼油的法兰垫圈。这些密封元件具有优异的弹性性能。因此，它们可以填充待密封表面中的间隙和凹陷，从而提供流体密封或气密密封。这些密封元件还可以具有高耐热性和耐久性，可以在大的温度范围内使用。
本发明的碳复合材料具有高导热性和各向异性，可用于制造散热元件或换热元件。散热元件通常用于快速释放由诸如计算机，CPU和功率晶体管等电子装置或部件产生的热量。换热元件将热量从一种介质传递到另一种介质，用于空间加热，制冷，空调发电厂，化工厂，石油化工厂，炼油厂，天然气处理，污水处理等。示例性散热或换热元件包括散热器，冷却系统，加热散热部件和换热器。在一个实施例中，散热元件是用于便携式电脑的散热器，其使便携式电脑冷却同时减少重量。
本发明的碳复合材料具有高强度，高硬度和优异的自润滑性能。因此，包括碳复合材料的制品可以是减摩元件，例如轴承，轴承座，涂层等。
这些制品可以是井下元件。示例性制品包括密封件、高压滚珠压裂筛塞、筛基管塞、用于阀球和阀座的涂层、压缩填料元件、可膨胀填料元件、O形密封环、结合密封件、子弹形密封件、地下安全阀密封件、地下安全阀挡板密封件、动态密封件、V形密封环、支撑环、钻头密封件、衬管端口塞、大气盘、大气室盘、碎屑屏障、钻进杆衬管塞、流入控制装置塞、挡板、阀座、球形座、直接连接盘、钻进线性盘、气举阀塞、失液控制挡板、电潜泵密封件、剪切塞、挡板阀、气举阀和套管。
碳复合材料具有高耐热性，工作温度范围为约-65°F至约1200°F。因此，诸如封隔器等井下制品可用于从环境温度大于750°F或大于1000°F的地下位置生产烃。在一个实施例中，本发明的制品在大于750°F的环境温度下连续耐受以下一种或多种情况超过30天：热裂解、热降解或热分解。如本文所使用的，“连续耐受”是指小于约10重量％，小于约5重量％，小于约2重量％或小于约1重量％的碳复合材料或含有碳复合材料的制品被热裂解，热降解和/或热分解。
井下制品还可以用于隔离或封上井筒。该方法包括将包括一个或多个井下制品的设备部署在井筒中。例如，制品可以是适于填充位于一个或多个生产管周围的钻孔内的环隙的类型。如本文所使用的，术语“生产管”的定义是包括例如用于完井的任何类型的管，例如但不限于生产管道，生产套管，中间套管和使烃流到地表的装置。在非限制性实施例中，这种制品的示例包括用于阻断非目标生产区或水区的环形隔离器等。
通过选择具有所需形状的模具，可以通过一步法或两步法在与本文针对碳复合材料所述的相同条件下直接由含有碳(例如石墨)和粘结剂的组合物制备这些制品。或者，这些制品通过成形或机械加工或其组合由碳复合材料形成。成形包括成型，挤出，浇铸和层压。机械加工包括使用例如铣床、锯、车床、铣床、放电加工机床等进行切割、锯切、烧蚀、铣削、面铣、车削、钻孔等。用于制备制品的碳复合材料的形式没有特别限制，包括例如粉末、丸粒、片材、棒、块、管、圆柱形坯料、圆环等。
本文所公开的所有范围包括端点，并且端点可以彼此独立地组合。本文所使用的未明确为单个的术语旨在包括其修饰的术语的单数和复数，从而包括该术语中的至少一者(例如，着色剂包括至少一种着色剂)。“或者”是指“和/或”。“任选的”或“任选地”是指随后所述的事件或情况可以发生或可以不发生，并且该描述包括事件发生的情况和不发生的情况。如本文所使用的，“组合”包括共混物、混合物、合金、反应产物等。“其组合”是指“包括列出的项目中的一个或多个以及任选地未列出的类似项目的组合”。所有参考文献通过引用并入本文。
除非本文另有说明或与上下文明显矛盾，说明本发明的上下文中(特别是在所附权利要求的上下文中)所使用的术语“一”、“一个”和“该”以及类似指代旨在涵盖单数和复数。此外，应该进一步指出的是，本文中的术语“第一”、“第二”诸如此类不指代任何顺序、数量或重要性，而是用于将元素彼此区分。涉及数量的修饰语“约”包括所述值，并具有上下文所规定的含义(例如，其包括与具体数量的测量相关的误差程度)。
虽然为了说明的目的已经阐述了典型的实施例，但是前述不应当被认为是对本文范围的限制。因此，在不脱离本发明本质和范围的情况下，本领域技术人员可以作出各种修改、调整和替换。

Claims (6)

1.一种从环境温度大于750°F的地下位置生产烃的方法，其使用一个或多个包括碳复合材料的制品，所述碳复合材料包括至少两个碳微结构以及设置在所述至少两个碳微结构之间的粘结相；
其中所述碳微结构具有1至50微米的厚度和10至500的长宽比并且包含膨胀石墨微结构；且
所述粘结相包括粘结剂，所述粘结剂包括以下各者中的一者或多者：SiO2、Si、B、B2O3、硒、金属或所述金属的合金，且其中所述金属是以下各者中的一者或多者：铝、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅或镉，并且所述粘结剂占所述碳微结构中的间隙空间的10％至90％。
2.一种隔离或封上井筒的方法，其包括：在井筒中部署包括一个或多个制品的设备，所述制品包括碳复合材料，所述碳复合材料包括至少两个碳微结构以及设置在所述至少两个碳微结构之间的粘结相；
其中所述碳微结构具有1至50微米的厚度和10至500的长宽比并且包含膨胀石墨微结构；且
所述粘结相包括粘结剂，所述粘结剂包括以下各者中的一者或多者：SiO2、Si、B、B2O3、硒、金属或所述金属的合金，且其中所述金属是以下各者中的一者或多者：铝、钛、镍、钨、铬、铁、锰、锆、铪、钒、铌、钼、锡、铋、锑、铅或镉，并且所述粘结剂占所述碳微结构中的间隙空间的10％至90％。
3.根据权利要求1或2所述的方法，其中所述粘结相包括粘结剂层以及使所述至少两个碳微结构中的一者结合到所述粘结剂层的界面层，其中所述界面层包括以下各者中的至少一者：C-金属键、C-B键、C-Si键、C-O-Si键、C-O-金属键或金属碳溶体。
4.根据权利要求1或2所述的方法，其中所述制品是井下元件，所述井下元件包括密封件。
5.根据权利要求1或2所述的方法，其中所述制品是井下元件，所述井下元件包括高压滚珠压裂筛塞、筛基管塞、用于阀球和阀座的涂层、压缩填料元件、可膨胀填料元件、O形密封环、结合密封件、子弹形密封件、地下安全阀密封件、地下安全阀挡板密封件、动态密封件、V形密封环、支撑环、钻头密封件、衬管端口塞、大气盘、大气室盘、碎屑屏障、钻进杆衬管塞、流入控制装置塞、挡板、阀座、球形座、直接连接盘、钻进线性盘、气举阀塞、失液控制挡板、电潜泵密封件、剪切塞、挡板阀、气举阀或套管。
6.根据权利要求1或2所述的方法，其中所述制品在大于750°F的环境温度下连续耐受热裂解、热降解或热分解中的一者或多者超过30天。
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