CN1271467A - 挠性的石墨复合材料 - Google Patents

挠性的石墨复合材料 Download PDF

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CN1271467A
CN1271467A CN98809551A CN98809551A CN1271467A CN 1271467 A CN1271467 A CN 1271467A CN 98809551 A CN98809551 A CN 98809551A CN 98809551 A CN98809551 A CN 98809551A CN 1271467 A CN1271467 A CN 1271467A
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R·A·默库里
J·P·卡普
J·J·高夫
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Abstract

一种挠性石墨片,其内嵌埋的陶瓷纤维从其表面延伸到片内而增强了这种对树脂的渗入性,此石墨片经机械变形成带有沟槽,可用作燃料电池的流场板极。

Description

挠性的石墨复合材料
发明领域
本发明涉及能用于制造密封垫和燃料电池用流场板极的挠性石墨和针状陶瓷粒的复合材料。
发明背景
本说明书中所用的词“挠性石墨”表示的是天然石墨粒经快速加热的分层反应产物，这种天然石墨粒通过对其晶体结构中进行试剂的夹杂处理，使得经此夹杂处理的石墨粒在垂直于上述晶体结构的碳层方向至少膨胀80倍或更多倍。挠性石墨及其制造方法已在Shane等人的美国专利No.3404061中予以描述，膨胀的即分层的石墨可以压成薄片(以后称之为挠性石墨“箔”)，而其密度接近理论密度，虽然约10～85磅/英尺3(lb/ft3)的密度但可适用于多种情形，压成的形状包括可用于发动机排气装置中的密封圈形状和其他用途的形状。
制造可膨胀的石墨粒的一般方法已由Shane等于美国专利No.3404061中说明，其中所公开的内容已综合于此供参考。这一方法的典型过程是，将天然石墨小片分散到含有例如硝酸和硫酸混合物的氧化剂溶液中以对其进行夹杂处理。这种夹杂溶液含有本项技术中周知的氧化剂和其它夹杂剂。夹杂溶液的例子包括那些含有氧化剂和氧化混合物的，如含有硝酸、氯酸钾、铬酸、高猛酸钾、铬酸钾、重铬酸钾、高氯酸等的溶液；或是含有例如浓硝酸与氯酸盐、铬酸与磷酸、硫酸与硝酸等混合物的溶液，或者是含有强有机酸如三氟醋酸和可溶于此有机酸的强氧化剂两者的混合物的溶液。最佳的夹层剂是这样的混合物的溶液，此混合物包括硫酸或硫酸与磷酸以及氧化剂，这里的氧化剂即硝酸、高氯酸、铬酸、高猛酸钾、过氧化氢、碘酸或高碘酸，等等。尽管不是理想的情形，这种夹杂溶液还可以包含金属卤化物如氯化铁以及氯化铁与硫酸的混合物，或是卤化物如作为溴与硫酸溶液的溴或是有机溶剂中的溴。在石墨小片经夹杂处理后，即从这种小片中排出过剩的溶液，再用水洗涤，然后将这种夹杂的石墨小片干燥，于火焰下暴露仅仅几秒钟使其膨胀。下面将如此处理过的石墨粒称作为“夹杂的石墨粒”。在暴露于高温下时，夹杂的石墨粒沿C方向即沿垂直于组份石墨粒的晶面的方向，依手风琴方式相对其原始体积于尺寸上膨胀80～1000倍或更多的倍数。这种分层的石墨粒的外观呈蠕虫状，因而一般称作虫形件。虫形件可以在压合到一起成为挠性片，后者与原始的石墨小片不同，可以形成和切割成各种形状。
挠性石墨箔是有凝聚力的，有良好的处理强度，可以使其绕成卷并能卷绕到金属固定件如心轴上，同时具有理想的传热性质，因而特别适合高温用途，例如用作发动机排气装置的密封圈。为了增强挠性石墨片或箔的密封性能，已提出过用树脂浸渍。但是挠性石墨片或箔的表面层由于分层的石墨粒的准直性和原子的组分层平行于此挠性片或箔的表面，当这种片或箔浸于液体树脂中时会阻碍树脂的浸渍。然而由于挠性石墨周知的各向异性，要是首先能让树脂渗入挠性石墨片或箔中树脂就会沿平行于这种片或箔的两个相对于平行平面的方向以及平行于这种片或箔的组分石墨粒的平面即横切石墨粒的“C轴”方向，迅速地流入挠性石墨片内。
附图的简要描述
图1以放大的横剖图概示出本发明的含陶瓷纤维的挠性石墨片(原始厚度为0.01英寸)；
图2～6是本发明的含陶瓷纤维的挠性石墨片的平表面的一部分，在增大电子束强度的电压(2.5KV～40KV)下的电子显微照片图(原图放大100X)；
图7、7A示明本发明的含陶瓷纤维的挠性石墨片的一部分，此石墨片已由机械方法变形或用作燃料电池中流场板极的沟槽板；
图8、8A是本发明的用作如燃料电池的元件的流场板极的顶视图和局部侧视(剖面)图；以及
图9概示先有技术的电化学燃料电池。
发明概要
本发明涉及含树脂的挠性石墨片的复合材料，此片状复合材料具有相对的平行的平整外表面且在挠性片中埋置有针状的陶瓷纤维粒，而这种陶瓷纤维从此挠性片的内部延伸到其至少一个平整外表面。本发明的挠性石墨片能够形成为电化学燃料电池的流场板极。
详细说明
在实施本发明的具体实施例时，将夹杂的天然石墨小片以约1.5～30％重量百分比的长0.15～1.5mm的针状陶瓷纤维粒混合，同时混和。这种纤维粒的宽度应当是从0.04到0.004mm。这种陶瓷纤维粒是不反应的且不粘附到石墨上，并能在高达2000°F的温度，理想时高达2500°F的温度下稳定。适用的陶瓷纤维粒是由下述纤维料形成：浸渍过的石英玻璃纤维；碳纤维与石墨纤维；氧化锆、氮化硼、碳化硅与氧化镁纤维；天然存在的矿物纤维如偏硅酸钙纤维、钙铝硅酸盐纤维、氧化铝纤维，等等。
夹杂的天然石墨小片和针状陶瓷纤维粒的混合物中的天然石墨小片和陶瓷纤维粒一般是准确的。将这种混合物暴露于温度高达2500°F的温度下分层，也即使得此夹杂的石墨小片膨胀成展开的石墨粒，成为未膨胀的夹杂天然石墨片的体积的80～1000倍，包围和裹绕着针状陶瓷纤维粒。膨胀的结果，陶瓷纤维粒不再与石墨粒基本准直，而是无规地位于分层的石墨和陶瓷纤维的混合物中。此分层的石墨粒和无规取向的针状陶瓷纤维粒的混合物压平成通常厚0.1～3.5mm的片或箔。这样形成的片或箔的特征是，它所具有的针状陶瓷纤维粒从挠性石墨片的内部延伸到并通过其两相对平表面的至少一个。由于这种针状陶瓷纤维粒是不反应的且不附着于挠性石墨片上，可在此挠性石墨片中设置许多围绕各针状陶瓷纤维粒的环形通道，它们从石墨片的相对表面延伸到石墨片的本体内。当石墨片浸于液体树脂中时，这些通道便接纳树脂，而树脂便在平行于挠性石墨片的平表面的较易渗透方向渗透入石墨片，此树脂受到其间埋入有针状陶瓷纤维粒所形成的通道的支持而浸渍形成此种片的受压的分层石墨粒，但不穿透此挠性石墨片的平行平表面。在此加工处理的所有步骤中，陶瓷纤维粒保持稳定，使得所述通道不会为熔化的纤维或纤维分解产物堵塞。在树脂于石墨片中固化后，由于从该片形成了密封垫而提高了这种挠性石墨片的密封性能。在最佳实施例中，此含树脂的片是在压力辊之间经辊压压制成的。
图1是根据对0.01英寸厚的挠性石墨片的显微镜观察结果绘成的示意图。此图以横剖图概示出挠性石墨片10具有相对的平行平面22、24。嵌埋入的陶瓷纤维粒以标号30表明。石墨片40为陶瓷纤维30的穿透情形示明于40处。
例I
将保持在50目网上过筛的80％重量百分比的天然石墨小片于90％重量百分比的硫酸和10％重量百分比的硝酸的混合溶液中处理。用水冲洗这样处理过的夹杂石墨小片，再干燥至含约1％重量百分比的水。以1磅这样的夹层小片，混合以0.15磅市售的规格绝大多数为15∶1的长度与直径比的偏硅酸钙针状陶瓷纤维。把此夹杂石墨与偏硅石钙纤维的混合物引入2500°F的加热炉内，获得使夹杂的石墨小片快速膨胀成弯曲蠕虫形的粒料，其体积约为未膨胀的夹杂石墨小片的约325倍。此膨胀的蠕虫形料包围着混合的偏硅酸钙纤维，并将此混合物辊压成0.01英寸厚和24英寸宽的挠性石墨片，其中所混合的偏硅酸钙纤维从此片的表面延伸到此片的体内，而此片则含有约12％重量百分比的偏硅酸钙纤维。
图2的电子显微图(100X，100μ分度)表明陶瓷纤维100的上都穿透挠性石墨片的平表面22。图3～6在增大的电压下表明“较深地”观察到挠性石墨片内，且同时表明陶瓷纤维100穿入到挠性石墨片内。嵌埋入挠性石墨片在表面72下的陶瓷纤维示明于标号140、160处。
例II
将宽8英寸的例1中石墨片的试样浸没于10％的酚醛树脂以丙酮稀释的溶液中，并以10英寸/分的速率从此溶液中拉过。经浸没及干燥后，此试样的重量增加了18.7％。
然后将此试样进行再处理加热到235℃，固化并稳定此酚醛树脂，然后将此石墨片在压力辊之间延压至密度为1.5g/cc。此延压成的片浸泡于油和水中未受影响，即不会为油和水透过。将未添加任何陶瓷纤维或树脂添加剂的对比石墨片暴露于与上述相同的试验条件下，结果重量增加了约35％，而厚度增加了约8％。
将按重量计添加5％、15％和25％偏硅酸钙纤维的试样石墨片，将添加剂按10英尺/分钟的速率从树脂溶液中拉过，试样为按重约17～19％重量百分比的树脂所浸润。未添加任何陶瓷纤维的对比试样在按10英尺/分钟的相同速率从树脂溶液中拉过时，则只含有5％重量百分比的树脂。
例III
将含有5％重量百分比偏硅酸钙纤维(100mm×100mm)的例1中所述这种延压的挠性石墨片用机械方法变形。冲压成图7、7A的顶视图和侧视图所示的适用作燃料电池的流场板极的形状。板极100上有许多为壁120分开的许多沟槽110。沟槽110通常为1.5mm深和1～1.5mm宽，并延伸到覆盖燃料电池的电极。壁120通常厚为1-1.5mm。机械变形前的密度约0.1～0.3gm/cc，经冲压后的密度一般超过1.1g/cc。
图7、7A中的板极100用例II中的树脂在约15psi的压力下用树脂浸渍，经加热到235℃固化后，在此板中提供约20％重量百分比的树脂。与先有技术的具有铣削的沟槽的石墨板相比，这种由树脂浸渍的板在其用作燃料电池的流场板极时增加了挠曲强度，改进了热耗散，同时降低了其在整个厚度上的电压降。
例IV
将含有5％重量百分比的例1中所述类型的纤维的1平方英寸的石墨片试样浸于例1中的稀释树脂溶液中15秒，使此片试样含有均匀分布的15％重量百分比的树脂。干燥此片料至无粘性状态(100℃)，并用机械方法变形，冲压成图7、7A的顶视图和侧视图所示的适用作燃料电池中的流场板极的形状。此板极100具有为壁120所分开的许多沟槽。沟槽110通常为1.5mm深和1～1.5mm宽，延伸到复盖燃料电池的电极。壁120通常为1～1.5mm厚。此试样片在机械变形前的密度约为0.1～0.3gm/cc，经冲压后的密度通常超过1.1g/cc。然后将图7、7A中的板极100徐缓地热至235℃以实现例III中的性质改进。
图9概示了燃料电池的基本元件，它的更完全的细节公开于美国专利No.4988583和No.5300370以及PCT WO 95/16287(1995年6月15日)中。
参看图9，以标记500概括指出的燃料电池包括取塑料形式的电解质，例如固体聚合物膜电解质550。碳纤维电极600于电极-薄膜界面601、603处以催化剂600例如铂涂层。流场板极1000、1100贴靠着催化剂层600，燃料例如氢气则循环通过氧化剂流场板极1100的沟槽1400。工作中，此燃料流场板极1000成为阳极，而氧化剂流场板极1100则成为阴极，结果便在燃料流场板极1000和氧化极场板极1100之间产生了电势即电压。上述的电化学燃料电池与燃料电池堆的其他部件结合，可提供上述美国专利No.5300370所述的合乎要求的电功率。
Watkms的美国专利No.4988583中所述的那种型式具有连续试剂流通道的流场板极1000’示明于图8和8A中。这种板极是含树脂的挠性石墨片，其中含有12％重量百分比的例III中所述的那种偏硅酸钙纤维。板极1000’的表面经冲压或模制成单一的连续流体流通道1200’，后者具有流体入口1600和流体出口1800。流体入口1600在阳极流场板极情形连接燃料源(未示明)，或在阴板流场极情形连接氧化剂源(未示明)。通道1200’多次地通过板极1000’的主要中央区，后者对应于图8A所示组装好情形中与其相邻的阳极或阴极的电催化的激活区。当组装成燃料电池堆时，各流场板极便起到电流集电器的作用。

Claims (1)

1.一种由树脂浸渍的挠性石墨片单一形式的、用作燃料电池的流场板极，此石墨片具有相对的平的外表面，且所述挠性石墨片于其中埋设有许多分散的针状陶瓷纤维粒，这些陶瓷纤维粒不与该挠性石墨片起反应，并在高达2000°F的温度下稳定，从至少一个所述针状陶瓷纤维粒的平的外表面延伸到所述石墨片之内而形成包含所述树脂的通道，同时所述平的外表面之一在其中形成有连续的流体流动通道，可用来接纳和排出流体燃料或氧化剂。
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