CN107076310A - 功能分级制品以及制造方法 - Google Patents

功能分级制品以及制造方法 Download PDF

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Publication number
CN107076310A
CN107076310A CN201580060091.0A CN201580060091A CN107076310A CN 107076310 A CN107076310 A CN 107076310A CN 201580060091 A CN201580060091 A CN 201580060091A CN 107076310 A CN107076310 A CN 107076310A
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component
carbon
product
adhesive
mixture
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CN107076310B (zh
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赵磊
徐志跃
邓桂俊
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Baker Hughes Holdings LLC
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Baker Hughes Inc
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    • B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
    • B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
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    • F16J15/10—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing
    • F16J15/102—Sealings between relatively-stationary surfaces with solid packing compressed between sealing surfaces with non-metallic packing characterised by material
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
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Abstract

本发明提供一种制品，所述制品包括第一构件，所述第一构件包含第一碳复合材料；以及第二构件，所述第二构件安置在所述第一构件上并且包含第二碳复合材料和增强剂，其中所述第二构件在所述第二碳复合材料与所述增强剂的重量比方面具有梯度，并且其中所述第一构件具有不同于所述第二构件的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。

Description

功能分级制品以及制造方法
相关申请的交叉引用
本申请要求于2014年11月25日提交的美国申请号14/552832的权益，所述申请以引用的方式整体并入本文。
发明背景
各种工具中已使用密封件来用于广泛范围的应用。由于所述密封件尤其是在高压和高温应用中或在其他恶劣环境中的广泛使用，希望提供具有高热稳定性和高化学稳定性的密封件。还希望提供具有高耐侵蚀性的密封件。
弹性体是相对柔软的且可变形的材料，并且已经用在密封件中。然而，弹性体在苛刻的条件下容易分解，因而它们的应用存在很多限制。作为替代方案，由于金属的高耐侵蚀性以及优异的高压和高温耐性，已使用金属对金属密封件。然而，金属具有低弹性和低顺应性。因此，在密封粗糙的外壳表面中，金属不如弹性体有效。
因此，该行业总是善于接受同时具有提高的弹性和耐侵蚀性的新材料。将更有利的是，这类材料还具有提高的热稳定性和化学稳定性。
发明内容
现有技术中的以上和其他缺陷通过以下制品克服：在实施方案中，所述制品包括第一构件，所述第一构件包含第一碳复合材料；以及第二构件，所述第二构件安置在第一构件上并且包含第二碳复合材料和增强剂，其中第二构件在第二碳复合材料与增强剂的重量比方面具有梯度，并且其中第一构件具有不同于第二构件的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。
在另一个实施方案中，制品包括：第一构件，所述第一构件包含第一碳复合材料；以及第二构件，所述第二构件安置在第一构件上并且包含第二碳复合材料，所述第二碳复合材料包括第二碳和第二粘合剂，其中第二构件在第二碳与第二粘合剂的重量比方面具有梯度，并且其中第一构件具有不同于第二构件的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。
制造制品的方法包括将第一粉末混合物安置在模具中；第一粉末混合物包含第一碳和第一粘合剂；将第二粉末混合物安置在第一粉末混合物上以提供合并的组合物；第二粉末混合物包含第二碳、第二粘合剂和增强剂；并且第二粉末混合物在第二碳和第二粘合剂的重量总和相对于增强剂的重量的比率方面具有梯度；以及在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩合并的组合物来形成制品。
在另一个实施方案中，制造制品的方法包括：形成包含第一碳复合材料的第一构件；以及将第二构件安置在第一构件上，所述第二构件包含第二碳复合材料和增强剂，并且第二构件在第二碳复合材料与增强剂的重量比方面具有梯度，其中第一构件具有不同于第二构件的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。
制造制品的方法也可以包括将第一构件安置在模具中；第一构件包含第一碳复合材料；将粉末混合物安置在第一构件上；粉末混合物包含第二碳、第二粘合剂和增强剂；并且第二粉末混合物在第二碳和第二粘合剂的重量总和相对于增强剂的重量的比率方面具有梯度；以及在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩粉末组合物来形成制品。
在又另一个实施方案中，制造制品的方法包括将第一粉末混合物安置在模具中；第一粉末混合物包含第一碳和第一粘合剂；将第二粉末混合物安置在第一粉末混合物上以提供合并的组合物；第二粉末混合物包含第二碳和第二粘合剂；并且第二粉末混合物在第二碳与第二粘合剂的重量比方面具有梯度；以及在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩合并的组合物来形成制品。
附图简述
以下描述不应被视为以任何方式进行限制。参考附图，相同元件的编号相同：
图1示出根据本公开的实施方案的制品的截面；
图2示出具有梯度石墨/粘合剂比的第二构件的截面，其中具有最高石墨/粘合剂比的区域具有最浅的灰度值，而具有最低石墨/粘合剂比的区域由最暗的灰度值指示；
图3示出图2所示的第二构件的区域A的微结构；
图4示出图2所示的制品的区域B的微结构；并且
图5示出图2所示的制品的区域C的微结构。
具体实施方式
发明人已发现由碳复合材料制成的制品可以是功能分级的，使得制品的一部分能够具有不同于所述制品的另一个部分的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。所述发现允许制造同时具有高弹性和高耐侵蚀性/耐磨性的制品。与弹性体密封件相比较，本文的制品具有提高的耐侵蚀性/耐磨性和提高的热稳定性，因此可以用在需要高耐侵蚀性/耐磨性的应用中或用在高温和高压环境中。与常规的耐侵蚀的金属对金属密封件相比较，本文的制品大幅提高弹性和顺应性以实现密封率更高且可靠性更大的密封。
此外，制品可以在低温(例如，制冷温度)与高温(例如，略小于制品的分解温度的温度)之间重复地热循环，并且制品将维持其化学、物理和机械特性，而不会出现实质性的偏差。另外，即使是在低温或高温下浸渍较长时间，例如，超过3个月、具体地是超过6个月、更具体地是超过1年以及还更具体地是超过2年之后，所述制品也将维持其化学、物理和机械特性，而不会出现实质性的偏差。作为另外的有利特征，所述制品具有优异的机械强度。
在实施方案中，制品包括：第一构件，所述第一构件包含第一碳复合材料；以及第二构件，所述第二构件安置在第一构件上并且包含第二碳复合材料和增强剂，其中第二构件在第二碳复合材料与增强剂的重量比方面具有梯度，并且其中第一构件具有不同于第二构件的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。
在另一个实施方案中，特性的变化通过改变碳/粘合剂重量比来实现。例如，第二构件包含碳复合材料，所述碳复合材料含有碳和粘合剂；并且第二构件在碳与粘合剂的重量比方面具有梯度。任选地，第二构件还包含增强剂。增强剂可以均匀地分布在第二构件中。可替代地，第二构件在碳与增强剂的重量比方面具有梯度。
第二构件可以具有任何合适的形式。在一个实施方案中，第二构件包括安置在第一构件上的层。第二构件可以具有执行与所述制品相关联的一个或多个井筒操作所需的任何合适的厚度。在示例性实施方案中，第二构件具有约50μm至约10mm或约500μm至约5mm的厚度。
在某些实施方案中，第一构件可以完全或部分被第二构件包围，诸如第二构件包括完全或部分包围第一构件的外层的实例。在其他实施方案中，可以仅将第二构件施加至第一构件的一个或多个部分。
第二构件中的增强剂包括以下一项或多项：氧化物、氮化物、碳化物、金属间化合物、金属、金属合金、碳纤维；碳黑；云母；粘土；玻璃纤维；或陶瓷材料。金属包括Ni；Ta；Co；Cr；Ti；Mo；Zr；Fe；或W。还可以使用这些金属的合金、氧化物、氮化物、碳化物或金属间化合物。陶瓷材料包括SiC、Si3N4、SiO2、BN等等。可以使用增强剂的组合。在实施方案中，在第一构件的碳组合物或第二构件中的碳复合材料中，增强剂与粘合剂是不同的。
第二碳复合材料与增强剂的重量比可以为约1:100至约100:1、约1:50至约50:1、或约1:20至约20:1。有利的是，第二构件在第二碳复合材料与增强剂的重量比方面具有梯度。梯度从接近第一构件的内部部分朝向远离第一构件的外部部分延伸。梯度可以包括第二碳复合材料与增强剂的从第二构件的内部部分到第二构件的外部部分的递减的重量比。例如，第二碳复合材料与增强剂的重量比可以从第二构件的内部部分的约50:1、约20:1或约10:1到第二构件的外部部分处的约1:50、约1:20或约1:10变化。在实施方案中，梯度从第二构件的内部部分到第二构件的外部部分连续地变化。在另一个实施方案中，梯度从第二构件的内部部分到第二构件的外部部分以离散的步长变化。
在第二构件在碳与粘合剂的重量比方面具有梯度的情况下，重量比可以为约1:100至约1:1或约1:10至约1:2。梯度从接近第一构件的内部部分朝向远离第一构件的外部部分延伸。梯度可以包括碳与粘合剂的从第二构件的内部部分到第二构件的外部部分的递减的重量比。例如，碳与粘合剂的重量比可以从第二构件的内部部分的约1:1或约1:2到第二构件的外部部分处的约1:100或约1:10变化。在实施方案中，梯度从第二构件的内部部分到第二构件的外部部分连续地变化。在另一个实施方案中，梯度从第二构件的内部部分到第二构件的外部部分以离散的步长变化。
第一构件和第二构件独立地包含含有碳诸如石墨和粘合剂的碳复合材料。第一构件和第二构件中的碳复合材料可以是相同的或不同的。在实施方案中，第一构件中的碳复合材料与第二构件中的碳复合材料是相同的。在另一个实施方案中，第二构件中的粘合剂具有高于第一构件中的粘合剂的耐腐蚀性/耐磨性。
如本文所使用，石墨包括以下一项或多项：天然石墨；合成石墨；可膨胀石墨；或膨胀石墨。天然石墨是大自然形成的石墨。所述天然石墨可以被分类为“片状”石墨、“脉”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。可膨胀石墨指代天然石墨或合成石墨的各层之间插入了嵌插材料的石墨。已经使用各种各样的化学材料来对石墨材料进行嵌插。这些化学材料包括酸、氧化剂、卤化物等等。示例性嵌插材料包括硫酸、硝酸、铬酸、硼酸、SO3或卤化物，诸如FeCl3、ZnCl2和SbCl5。在加热时，嵌插物从液态或固态转变为气相。气体形成产生了压力，所述压力推动邻近的碳层分开，从而产生膨胀石墨。膨胀石墨颗粒在外观上呈蠕虫状，并且因此通常被称为蠕虫。
有利的是，石墨包括膨胀石墨。与其他形式的石墨相比较，膨胀石墨具有高柔性、高压缩回复性和较大的各向异性。除了所需的机械强度之外，由本文公开的膨胀石墨和粘合剂形成的碳复合材料因此还可以具有优异的弹性。
碳复合材料可以包括石墨相和粘合剂相。粘合相包括通过机械互锁而粘合石墨团、石墨颗粒、石墨片、石墨晶体或石墨微结构的粘合剂。在实施方案中，碳复合材料包括碳微结构，所述碳微结构在所述碳微结构当中具有间隙空间；其中粘合剂安置在间隙空间中的至少一些中；并且其中碳微结构包括碳微结构内的未填充的空隙。
碳微结构是在将石墨压缩成高度浓缩状态之后形成的石墨的微观结构。所述碳微结构包括沿压缩方向堆叠在一起的石墨基面。如本文所使用，碳基面指代基本上平坦的平行碳原子片或层，其中每个片或层具有单一原子厚度。石墨基面还被称为碳层。碳微结构通常是薄而平的。所述碳微结构可以具有不同的形状并且也可以被称为微片、微盘等等。在实施方案中，碳微结构彼此基本平行。
碳复合材料中存在两种类型的空隙-碳微结构当中的空隙或间隙空间以及每个单独碳微结构内的空隙。碳微结构当中的间隙空间的大小为约0.1至约100μm、具体地为约1至约20μm，而碳微结构内的空隙要小得多并且通常是介于约20纳米至约1μm、具体地为约200纳米至约1μm之间。空隙或间隙空间的形状并无特别限制。如本文所使用，空隙或间隙空间的大小指代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。
碳微结构当中的间隙空间填充有μm或纳米级粘合剂。例如，粘合剂在碳微结构当中会占用约10％至约90％的间隙空间。在实施方案中，粘合剂并不渗透个别碳微结构，并且碳微结构内的空隙未充填(即，未填充)任何粘合剂。因此，碳微结构内的碳层并不通过粘合剂来锁定在一起。通过此机制，可以保持制品，尤其是包含膨胀石墨的制品的柔性。
任选地，界面层形成在粘合剂与石墨之间。界面层可以包含化学键、固体溶液或其组合。当存在时，化学键、固体溶液或其组合可以增强石墨的互锁。应了解到，石墨可以通过机械互锁和化学键合两者来保持在一起。粘合相的厚度为约0.1至约100μm或约1至约20μm。粘合相可以形成将石墨粘合在一起的连续或不连续网络。
示例性粘合剂包括非金属、金属、合金、或包括以上至少一项的组合。非金属是以下一项或多项：SiO2；Si；B；或B2O3。金属可以是以下至少一项：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；镉；或硒。合金包括以下一项或多项：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。在实施方案中，粘合剂包括以下一项或多项：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、镍铬基合金诸如Inconel*和镍铜基合金诸如Monel合金。镍铬基合金可以含有约40％-75％的Ni和约10％-35％的Cr。镍铬基合金还可以含有约1％至约15％的铁。镍铬基合金中也可以包括少量Mo、Nb、Co、Mn、Cu、Al、Ti、Si、C、S、P、B或包括以上至少一项的组合。镍铜基合金主要由镍(高达约67％)和铜构成。镍铜基合金还可以含有少量铁、锰、碳以及硅。这些材料可以处于不同的形状，诸如颗粒、纤维和丝线。可以使用所述材料的组合。
耐侵蚀/耐磨粘合剂包括以下一项或多项：Ni；Ta；Co、Cr、Ti、Mo；Zr、Fe、W；以及其合金。应了解到，耐侵蚀/耐磨粘合剂同样应是相对可延展的，使得制品能够充分适应于密封粗糙表面。考虑到其高韧性，耐侵蚀粘合剂在使用时可以限于制品表面附近的区域。在制品的其他部分中，诸如在第一构件中可以使用延展性更高的粘合剂。以此方式，制品可以是耐侵蚀/耐磨的，并且同时在有限的调节力下充分地变形。在实施方案中，第二构件的碳组合物中的第二粘合剂包括耐侵蚀/耐磨粘合剂。
用于制造制品的粘合剂是μm或纳米级的。在实施方案中，粘合剂具有以下平均粒度：约0.05至约250μm、约0.05至约50μm、约0.05至约10μm、具体地为约0.5至约5μm、更具体地为约0.1至约3μm。不希望受理论束缚，相信在粘合剂的大小处于这些范围内时，所述粘合剂可均匀地分散在石墨中。
当存在界面层时，粘合相包括包含粘合剂的粘合剂层以及将石墨结合至粘合剂层的界面层。界面层包括以下一项或多项：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。所述键由粘合剂和在石墨表面上的碳形成。
在实施方案中，界面层包含粘合剂的碳化物。碳化物包括以下一项或多项：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。这些碳化物通过使对应的金属或金属合金粘合剂与碳微结构的碳原子反应来形成。粘合相还可以包含SiC，其通过使SiO2或Si与碳微结构的碳反应来形成；或B4C，其通过使B或B2O3与碳微结构的碳反应来形成。当使用粘合剂材料的组合时，界面层可以包含这些碳化物的组合。碳化物可以是盐类碳化物，诸如碳化铝、共价碳化物诸如SiC和B4C、间隙碳化物诸如第4、5和6族过渡金属的碳化物、或中间过渡金属碳化物，例如Cr、Mn、Fe、Co和Ni的碳化物。
在另一个实施方案中，界面层包括碳诸如石墨和粘合剂的固体溶液。碳在某些金属基质中或在某些温度范围下具有溶解度，这可以有助于金属相的润湿并且将其粘合到碳微结构上。通过热处理，可以在低温下维持碳在金属中的高溶解度。这些金属包括以下一项或多项：Co；Fe；La；Mn；Ni；或Cu。粘合剂层还可以包含固体溶液和碳化物的组合。
基于碳复合材料的总重，碳复合材料包含约20重量％至约95重量％、约20重量％至约80重量％或约50重量％至约80重量％的石墨。基于碳复合材料的总重，粘合剂以约5重量％至约75重量％或约20重量％至约50重量％的量存在。
参考图1，在示例性实施方案中，制品10包括包含第一碳复合材料的第一构件1。制品10还包括第二构件2，所述第二构件2安置在第一构件1上并且包含第二碳复合材料和增强剂，其中第二构件2在第二碳复合材料3与增强剂4的重量比方面具有梯度。
图2示出具有梯度石墨/粘合剂比的第二构件5的截面。在图2中，具有最高石墨/粘合剂比的区域具有最浅的灰度值，而具有最低石墨/粘合剂比的区域由最暗的灰度值指示。如图2所示，石墨/粘合剂比从第二构件的顶部到第二构件的底部逐渐增大。
图3-5中分别示出了第二构件的区域A-C的微结构。如图3所示，在制品暴露于磨料的第二构件的顶部附近，粘合剂7与其中作为润滑剂分散的石墨颗粒6起主导作用，以减小磨料与制品表面之间的摩擦。图4示出在第二构件的中间，粘合剂形成将石墨9粘合在一起的粘合相8，以提高制品的结构完整性和耐热性。如图5所示，在第二构件的底部处，石墨相9起主导作用，从而实现较高弹性，进而实现更有效和可靠的密封。
形成功能分级制品的一种方式包括：将第一粉末混合物安置在模具中；第一粉末混合物包含第一碳和第一粘合剂；将第二粉末混合物安置在第一组合物上以提供合并的组合物；第二粉末混合物包含第二碳、第二粘合剂和增强剂；并且第二粉末混合物在第二碳和第二粘合剂的重量总和相对于增强剂的重量的比率方面具有梯度；以及在约350℃至约1200℃的温度和约500psi至约30,000psi的压力下压缩合并的组合物来形成制品。
在第二构件在碳与粘合剂的重量比方面具有梯度的情况下，所述方法包括：将第一粉末混合物安置在模具中；第一粉末混合物包含第一碳和第一粘合剂；将第二粉末混合物安置在第一粉末混合物上以提供合并的组合物；第二粉末混合物包含第二碳和第二粘合剂；并且第二粉末混合物在第二碳与第二粘合剂的重量比方面具有梯度；以及在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩合并的组合物来形成制品。
在实施方案中，分多个部分安置第二粉末混合物以便于在第二碳和第二粘合剂的重量总和相对于增强剂的重量的比率(又称为原材料重量比)方面建立梯度。例如，第二粉末混合物的第一部分可以具有90:10的原材料重量比。第二粉末混合物的第二部分可以具有80:20的原材料重量比。第二粉末混合物的第三部分可以具有70:30的原材料重量比。另外，第二粉末混合物的最后部分可以具有10:90的原材料重量比。一旦第一粉末混合物被安置在模具中，就将第二粉末混合物的第一部分安置在第一粉末混合物上，将第二部分安置在第一部分上，并且将第三部分安置在第二部分上直到最后部分被安置在模具中为止。部分的数目并无特别限制。在实施方案中，梯度通过以约3至约100个部分、约3至约50个部分、约3至约20个部分、约5至约15个部分、或约5至10个部分连续安置第二粉末混合物来建立，其中连续部分具有递减的原材料重量比。为了在第二碳与第二粘合剂的重量比方面建立梯度，可以相似的方式安置第二粉末混合物。
粉末混合物可以通过经由本领域已知的任何合适的方法将石墨和μm或纳米级粘合剂以及增强剂(如果存在的话)共混在一起来形成。合适的方法的实例包括球混、声学混合、带式共混、立式螺杆混合以及V式共混。
制品可以经由一步法或两步法来形成。在两步法中，通过冷压来压缩合并的组合物以提供生压坯；并且之后压缩和加热生压坯，从而形成制品。在另一个实施方案中，可以在室温下压制合并的组合物来形成压坯，并且之后在大气压下加热所述压坯来形成制品。这些方法可以被称为两步法。可替代地，可以直接压缩和加热合并的组合物来形成制品。所述方法可以被称为一步法。
石墨可以是呈碎片、粉末、小片、薄片等等的形式。在实施方案中，石墨是呈具有约50μm至约5,000μm、优选地为约100至约300μm的直径的薄片的形式。石墨片可以具有约1至约5μm的厚度。
参考两步法，冷压意指在室温下或在高温下压缩合并的组合物，只要粘合剂没有明显结合石墨即可。在实施方案中，生压坯中并未结合大于约80重量％、大于约85重量％、大于约90重量％、大于约95重量％、或大于约99重量％的石墨。用于形成生压坯的压力可以为约500psi至约10ksi，并且温度可以为约20℃至约200℃。这个阶段的缩减比(即，生压坯的体积相对于合并的组合物的体积之比)为约40％至约80％。生压坯的密度为约0.1至约5g/cm3、约0.5至约3g/cm3、或约0.5至约2g/cm3。
可以在约350℃至约1400℃、具体地为约800℃至约1400℃的温度下加热生压坯来形成制品。在实施方案中，温度是粘合剂的熔点的约±20℃至约±100℃，或粘合剂的熔点的约±20℃至约±50℃。在另一个实施方案中，温度高于粘合剂的熔点，例如，比粘合剂的熔点高约20℃至约100℃或约20℃至约50℃。当温度更高时，粘合剂的粘性变小并且流动性变好，为了将粘合剂与石墨均匀地共混在一起，可能需要更小的压力。然而，如果温度过高，那么可能会对仪器产生不利影响。
温度可以根据预定温度进度表或斜升率来施加。加热的手段并无特别限制。示例性加热方法包括直流(DC)加热、感应加热、微波加热以及火花等离子体烧结(SPS)。在实施方案中，加热经由DC加热来进行。例如，可以用电流对合并的组合物进行充电，所述电流流过组合物，很快产生热量。任选地，还可以在惰性气氛下，例如在氩气或氮气下进行加热。在实施方案中，在存在空气下加热生压坯。
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于大气压的压力。在实施方案中，用于形成制品的希望压力不是一次性施加的。在装载生压坯之后，最初在室温下或在低温下将低压施加至组合物以封闭组合物中的大孔隙。否则的话，可以使熔融的粘合剂流动至压模的表面。一旦温度达到预定最大温度，就可以施加制造制品所需的希望压力。可以将温度和压力保持处于预定最大温度和预定最大压力，持续约5分钟至约120分钟。在实施方案中，预定最大温度为粘合剂的熔点的约±20℃至约±100℃，或粘合剂的熔点的约±20℃至约±50℃。
这个阶段的缩减比(即，制品的体积相对于生压坯的体积之比)为约10％至约70％或约20％至约40％。制品的密度可以通过控制压缩程度来改变。制品可以具有约0.5至约10g/cm3、约1至约8g/cm3、约1至约6g/cm3、约2至约5g/cm3、约3至约5g/cm3或约2至约4g/cm3的密度。
可替代地，又称为两步法，可以首先在室温和约500psi至30,000psi的压力下压制合并的组合物来形成压坯；并且可以进一步在约350℃至约1400℃、具体地为约800℃至约1400℃的温度下加热压坯来制造制品。在实施方案中，温度是粘合剂的熔点的约±20℃至约±100℃，或粘合剂的熔点的约±20℃至约±50℃。在另一个实施方案中，温度可以比粘合剂的熔点高约20℃至约100℃或约20℃至约50℃。可以在存在或不存在惰性气氛下在大气压下进行加热。
在另一个实施方案中，无需制造生压坯就可以直接从合并的组合物制造制品。可以同时执行压制和加热。合适的压力和温度可以与本文针对两步法的第二步骤所论述相同。
热压是同时施加温度和压力的工艺。所述热压可以用在一步法和两步法两者中来制造功能分级制品。
在另一个实施方案中，单独地形成第一构件和第二构件。之后将第一构件安置在第二构件上。例如，可以向模具装载第一粉末混合物，所述第一粉末混合物根据如本文所公开的一步法或两步法来处理以从合并的组合物制造制品。类似地，可以向模具装载第二粉末混合物，所述第二粉末混合物根据如本文所公开的一步法或两步法来处理以从合并的组合物制造制品，其中第二构件在第二碳复合材料与增强剂的重量比方面具有梯度或在第二碳与第二粘合剂的重量比方面具有梯度。
用于将第一构件安置在第二构件上的方法并无特别限制。在实施方案中，通过将局部热量施加至第一构件的表面和/或第二构件的表面来将第一构件层压至第二构件。其他示例性方法包括等静压、扩散结合、热模制、焊接、钎焊等等。
在另一个实施方案中，在形成第一构件之后，将所述第一构件安置在模具中。接着，将如本文所述的第二粉末混合物安置在第一构件的表面上。之后，将第二粉末混合物和第一构件模制在一起，从而形成功能分级制品。
本文的功能分级制品可以许多不同形状形成，诸如环形、管状、圆管状、杆状、圆环、球形、多边形、锥形、圆柱形、其截头形状等等。这种形状可以由模制工艺、挤出等等产生。另外，模制形状还可以经受各种成型工艺，包括切割、锯削、消融以及其他材料去除方法。
功能分级制品具有多种有利特性并且可以用在各种各样的应用中。制品可以用于制造工具或工具的部件。说明性工具包括密封件、高压珠粒状压裂筛网塞、筛网基管塞、压缩填充元件、O形环、结合密封件、子弹密封件、地下安全阀密封件、地下安全阀挡板密封件、动态密封件、支承环、钻头密封件、衬套端口塞、碎屑屏障、钻入激励衬套塞、流入控制装置塞、挡板、球座、气举阀塞、防滤失挡板、电潜泵密封件、切口塞、挡板阀、气举阀以及套管。其他说明性制品包括核反应堆压力容器密封件；核致动器密封件；核电站中的泵密封件；泄压密封件；旋转密封件；滑阀密封件；制动活塞密封件；轴密封件；轴承密封件；或小齿轮密封件。在实施方案中，制品是井下元件。
制品具有操作温度范围从约-65℉直至约1200℉的高耐热性。在特别有利的特征中，通过形成功能分级制品，提高了耐侵蚀性/耐腐蚀性和弹性两者。所述制品特别适合于用作遭受侵蚀/腐蚀破坏的密封件，例如用在安全阀或阻挡阀应用中的挡板或旋转球阀密封件。制品或包括制品的工具可以用于各种应用。在实施方案中，制品或包括制品的工具可以用于抑制流动。
本文公开的所有范围都包括端点，并且端点可独立地相互组合。如本文所使用的后缀“(s)”旨在包括其所修饰的术语的单数和复数形式两者，因而包括至少一个所述术语(例如，着色剂(一种或多种)包括至少一种着色剂)。“或者”意指“和/或”。“任选的”或“任选地”意指随后描述的事件或情况可能发生或不发生，并且所述描述包括事件发生的情况和事件不发生的情况。如本文所使用，“组合物”包括共混物、混合物、合金、反应产物等等。“其组合”意指“包括所列项目中的一项或多项以及任选地未列出的类似项目的组合”。所有参考文献都以引用的方式并入本文。
除非本文另外指明或明显与上下文抵触，否则术语“一个”和“一种”以及“所述”和类似术语在描述本发明的上下文中(尤其是在以上权利要求书的上下文中)的使用应被视为覆盖单数和复数形式两者。另外，应进一步注意到，本文中的术语“第一”、“第二”等等并不表示任何次序、数量或重要性，而是用于区分各个元件。与数量结合使用的修饰词“约”包括所指出的值，并且具有上下文中指定的含义(例如，它包括与具体数量的测量相关联的误差程度)。
虽然已出于说明目的阐述了典型的实施方案，但是前文描述不应被视为是对本文的范围的限制。因此，在不脱离本文的精神和范围的情况下，本领域技术人员可以想到各种修改、调整和替换。

Claims (15)

1.一种制品(10)，所述制品(10)包括：
第一构件(1)，所述第一构件(1)包含第一碳复合材料；以及
第二构件(2)，所述第二构件(2)安置在所述第一构件(1)上并且包含第二碳复合材料(3)和增强剂(4)，
其中所述第二构件(2)在所述第二碳复合材料(3)与所述增强剂(4)的重量比方面具有梯度，并且
其中所述第一构件(1)具有不同于所述第二构件(2)的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。
2.一种制品(10)，所述制品(10)包括：
第一构件(1)，所述第一构件(1)包含第一碳复合材料；以及
第二构件(2)，所述第二构件(2)安置在所述第一构件(1)上并且包含第二碳复合材料(3)，所述第二碳复合材料(3)包含第二碳和第二粘合剂，
其中所述第二构件(2)在所述第二碳与所述第二粘合剂的重量比方面具有梯度，并且
其中所述第一构件(1)具有不同于所述第二构件(2)的以下特性中的一项或多项：弹性；耐腐蚀性；耐侵蚀性；或硬度。
3.如权利要求1或权利要求2所述的制品(10)，其中所述梯度从接近所述第一构件(1)的内部部分朝向远离所述第一构件(1)的外部部分延伸；并且
其中所述梯度从所述第二构件(2)的内部部分到所述第二构件(2)的外部部分包括所述第二碳复合材料(3)与所述增强剂(4)的递减的重量比，或所述第二碳与所述第二粘合剂的递减的重量比。
4.如权利要求2或权利要求3所述的制品(10)，其中所述梯度从所述第二构件(2)的内部部分到所述第二构件(2)的外部部分连续地变化，或者所述梯度从所述第二构件(2)的内部部分到所述第二构件(2)的外部部分以离散的步长变化。
5.如权利要求1至4中任一项所述的制品(10)，其中所述第一碳复合材料和所述第二碳复合材料(3)中的每一者独立地包含碳和粘合剂(7)，所述粘合剂(7)含有以下一项或多项：SiO2；Si；B；B2O3；金属；或所述金属的合金；并且其中所述金属是以下一项或多项：铝；铜；钛；镍；钨；铬；铁；锰；锆；铪；钒；铌；钼；锡；铋；锑；铅；镉；或硒；并且其中所述第一碳复合材料中的所述碳和所述第二碳复合材料(3)中的所述碳独立地包括以下一项或多项：膨胀石墨；可膨胀石墨；天然石墨；或合成石墨。
6.如权利要求1至5中任一项所述的制品(10)，其中所述第一碳复合材料和所述第二碳复合材料(3)包括碳微结构，所述碳微结构在所述碳微结构当中具有间隙空间；其中所述粘合剂(7)安置在所述间隙空间中的至少一些中；并且其中所述碳微结构包括所述碳微结构内的未填充的空隙。
7.如权利要求1至5中任一项所述的制品(10)，其中所述第一碳复合材料和所述第二碳复合材料(3)包括至少两个碳微结构和粘合相(8)，所述粘合相(8)安置在所述至少两个碳微结构之间；并且其中所述粘合相(8)包括粘合剂层和界面层，所述界面层将所述至少两个碳微结构中的一个键合至所述粘合剂层；并且其中所述界面层包括以下一项或多项：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。
8.如权利要求1至7中任一项所述的制品(10)，其中所述增强剂(4)包括以下一项或多项：氧化物、氮化物、碳化物、金属间化合物、金属、金属合金、碳纤维；碳黑；云母；粘土；玻璃纤维；或陶瓷材料。
9.如权利要求1至8中任一项所述的制品(10)，其中所述制品(10)是核反应堆压力容器密封件；核致动器密封件；核电站中的泵密封件；泄压密封件；旋转密封件；滑阀密封件；制动活塞密封件；轴密封件；轴承密封件；小齿轮密封件；或选自以下的井下制品(10)：密封件；密封座；密封组件；高压珠粒状压裂筛网塞；筛网基管塞；旋转球阀密封件、压缩填充元件；O形环；结合密封件；子弹密封件；地下安全阀密封件；地下安全阀挡板密封件；动态密封件；支承环；钻头密封件；衬套端口塞；碎片阻挡件；钻入激励衬套塞；流入控制装置塞；挡板；球座；气举阀塞；防滤失挡板；电潜泵密封件；切口塞；挡板阀；气举阀；或套管。
10.一种制造制品(10)的方法，所述方法包括：
将第一粉末混合物安置在模具中；所述第一粉末混合物包含第一碳和第一粘合剂；
将第二粉末混合物安置在所述第一粉末混合物上以提供合并的组合物；所述第二粉末混合物包含第二碳、第二粘合剂和增强剂(4)；并且所述第二粉末混合物在所述第二碳和所述第二粘合剂的重量总和相对于所述增强剂(4)的重量的比率方面具有梯度；以及
在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩所述合并的组合物来形成所述制品(10)。
11.一种制造制品(10)的方法，所述方法包括：
将第一粉末混合物安置在模具中；所述第一粉末混合物包含第一碳和第一粘合剂；
将第二粉末混合物安置在所述第一粉末混合物上以提供合并的组合物；所述第二粉末混合物包含第二碳和第二粘合剂；并且所述第二粉末混合物在所述第二碳与所述第二粘合剂的重量比方面具有梯度；以及
在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩所述合并的组合物来形成所述制品(10)。
12.如权利要求10或权利要求11所述的方法，其中分多个部分安置所述第二粉末混合物以在所述第二碳和所述第二粘合剂的重量总和相对于所述增强剂(4)的重量的比率方面建立所述梯度，或在所述第二碳与所述第二粘合剂的所述重量比方面建立所述梯度。
13.一种制造如权利要求1所述的制品(10)的方法，所述方法包括：
形成包含第一碳复合材料的第一构件(1)；以及
将第二构件(2)安置在所述第一构件(1)上，所述第二构件(2)包含第二碳复合材料(3)和增强剂(4)，并且所述第二构件(2)在所述第二碳复合材料(3)与所述增强剂(4)的重量比方面具有梯度，
其中所述第一构件(1)具有不同于所述第二构件(2)的以下特性中的一项或多项：弹性、耐腐蚀性、耐侵蚀性或硬度。
14.一种制造如权利要求1所述的制品(10)的方法，所述方法包括：
将第一构件(1)安置在模具中；所述第一构件(1)包含第一碳复合材料；
将粉末混合物安置在所述第一构件(1)上；所述粉末混合物包含第二碳、第二粘合剂和增强剂(4)；并且所述第二粉末混合物在所述第二碳和所述第二粘合剂的重量总和相对于所述增强剂(4)的重量的比率方面具有梯度；以及
在约350℃至约1400℃的温度和约500psi至约30,000psi的压力下压缩所述粉末混合物来形成所述制品(10)。
15.一种抑制流动的方法，所述方法包括采用如权利要求1至9中任一项所述的制品(10)中的一种或多种。
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