CN1259111A - 可变形的石墨复合材料 - Google Patents

可变形的石墨复合材料 Download PDF

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CN1259111A
CN1259111A CN98805838A CN98805838A CN1259111A CN 1259111 A CN1259111 A CN 1259111A CN 98805838 A CN98805838 A CN 98805838A CN 98805838 A CN98805838 A CN 98805838A CN 1259111 A CN1259111 A CN 1259111A
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graphite
particle
deformable
resin
ceramic fiber
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R·A·默库里
J·P·卡普
J·J·高夫
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Graftech Technology LLC
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Ucar Carbon Technology Corp
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Abstract

有包裹陶瓷纤维的可变形石墨片,其陶瓷纤维从片表面延伸到片中,以提高片对树脂的渗透性。

Description

可变形的石墨复合材料
                      发明领域
本发明涉及可变形石墨的复合材料与可以用于生产密封填料的针形陶瓷颗粒。
                      发明背景
本文使用的术语“可变形石墨”表示曾用试剂处理过的快速加热天然石墨颗粒的层离反应产物，这种试剂嵌入石墨晶体-结构中，使嵌入的颗粒在晶体结构中沿着与碳层垂直的方向膨胀至少80倍或80倍以上。在Shane等人的US3 404 061中描述了可变形石墨及其制品。膨胀石墨，即层离石墨，可以压制成薄片(下面称之可变形石墨“薄片”)，其密度接近理论密度，尽管密度约50-85磅/英尺3适合大多数应用，其中包括压制成适合作引擎排气管密封环的形状，和其他应用。
Shane等人在US3 404 061中描述的一种通常生产可膨胀石墨颗粒的方法，其公开内容作物参考文献列于本文。在典型的实施该方法时，天然石墨絮片是通过将其絮片分散到含有如硝酸和硫酸混合物之类的氧化剂的溶液中嵌入的。这种嵌入溶液含有在现有技术中已知的氧化剂和其他嵌入剂。实例包括含有氧化剂和氧化混合物的那些实例，如含有下述物质的溶液：硝酸、氯酸钾、铬酸、高锰酸钾、铬酸钾、重铬酸钾、高氯酸等，或混合物，例如像浓硝酸和氯酸盐、铬酸和磷酸、硫酸和硝酸，或强有机酸混合物，例如三氟乙酸，以及可溶于有机酸的强氧化剂。优选的嵌入剂是硫酸，或硫酸和磷酸，以及如硝酸、高氯酸、铬酸、高锰酸钾、过氧化氢、碘酸或高碘酸等之类氧化剂的混合物溶液。尽管不是优选的，嵌入溶液可以含有金属卤化物，如氯化铁，以及与硫酸混合的氯化铁，或卤化物，例如像溴和硫酸溶液中的溴或溴在有机溶剂中的溶液的溴。在嵌入絮片之后，从絮片中排出过量的溶液，再用水洗涤后，嵌入的石墨絮片经干燥，并接触火仅几秒钟就是可膨胀的。如此处理的石墨颗粒在后面称之“嵌入石墨颗粒”。在接触高温时，嵌入石墨颗粒的膨胀尺寸为原体积的80-1000倍或1000倍以上，在c-方向，即与构成石墨颗粒的晶体平面垂直的方向呈褶状。层离的石墨颗粒在外观上是蠕虫状的，因此通常称之蠕虫。其蠕虫可被压缩成可变形的片，它与原来的石墨絮片不同，可以成型并切成各种各样的形状。
可变形石墨薄片是黏合在一起的，具有良好的操作强度，可变形石墨薄片可以缠绕成轧辊，也可以绕在如心轴之类的金属固定物上，具有所要求的传热性质，因此在高温应用方面，如发动机排气装置密封环的应用是特别有用的。曾提出用树脂浸透可变形石墨片或薄片来增加它的密封性。但是，由于层离石墨颗粒排列和由平行于变形石墨片或薄片表面的组成的原子层，当变形石墨片或薄片浸在液体树脂中时，变形石墨片或薄片的表面层阻止树脂浸透变形石墨片或薄片。然而，由于熟知的变形石墨的各向异性，如果可能首先渗入进变形石墨薄片，树脂会很容易地沿着平行于变形石墨片或薄片对置平行的平的表面和片的构成石墨颗粒平面的方向，即对于石墨颗粒“c-轴”方向为横向，流入变形石墨薄片中。
因此，本发明的目的是提供一种变形石墨片或薄片，它具有增加的渗透性，以便能够提高树脂的浸透性。
                     附图简要描述
图1以放大的截面表示本发明含有陶瓷纤维的变形石墨薄片骨架(原厚度为0.01英寸)；
图2至图6是本发明含有陶瓷纤维的变形石墨薄片的一部分平的表面，在不断增加的电子束强度电压(2.5KV至40KV)下的电子显微镜视图(原始的放大倍数100X)。
                         本发明简要说明
本发明涉及具有对置平行的平的外表面的可变形石墨片与针形陶瓷纤维颗粒的复合材料，颗粒被包裹在可变形石墨中，并从可变形片内延伸到可变形石墨片的至少一个平的外表面。
                            详细说明
在实施本发明特定的实施方案中，嵌入的天然石墨絮片经混合，再与约1.5-30％(重量)其长度0.15-1.5毫米的针形陶瓷纤维颗粒掺混。颗粒宽度应是0.04-0.004毫米。陶瓷纤维颗粒与石墨无反应性，也无粘附性，在温度高达2000°F，优选地是2500°F是稳定的。合适的陶瓷纤维颗粒是由浸软的石英玻璃纤维、炭和石墨纤维、二氧化锆、氮化硼、碳化硅和氧化镁纤维，天然存在的矿物纤维，例如硅酸钙纤维、硅酸铝钙纤维、氧化铝纤维等构成的。
嵌入的天然石墨絮片和针形陶瓷纤维颗粒的混合物，其中石墨絮片和陶瓷纤维颗粒一般地是排列成行的，接触到温度高达2500°F的火焰而层离，即嵌入石墨絮片膨胀成已膨胀的石墨颗粒，其体积为未膨胀的嵌入天然石墨絮片的80-1000倍，而这种絮片围绕与包裹针形陶瓷纤维颗粒。由于这种膨胀，陶瓷纤维颗粒基本上不再是与石墨颗粒排列成行的，而在层离石墨和陶瓷纤维混合物中是随机定位的。层离石墨颗粒和随机定向的针形陶瓷纤维颗粒的混合物辊压成片或薄片，其典型厚度为0.1-3.5毫米。所得到的片或薄片的特征在于具有针形颗粒，它们从可变形石墨片内延伸到并穿过至少一个可变形石墨片的对置的平的表面。因为针形陶瓷纤维颗粒对可变形片中的石墨是非反应性的，也是非粘附性的，所以在可变形石墨片中提供了围绕各个针形颗粒的多个环形通道，从片的对置表面延伸到片体内。在液体树脂中浸渍的可变形石墨片的这些通道接纳这种树脂，而这种树脂然后以平行于可变形石墨片的平的表面的较易渗透的方向穿过可变形石墨片和形成片的压制剥离石墨颗粒，借助于由包裹在其间但是不渗入可变形石墨片的平的平行表面的针形陶瓷纤维颗粒构成的通道形成片。陶瓷纤维颗粒在所有加工处理步骤中仍是稳定的，因此这些通道不被熔化纤维或纤维分解产物堵塞。在树脂固化之后，在石墨片内，提高了由可变形石墨片制成的密封填料的可密封性。在优选的实施方案中，含有树脂的片经在压力辊之间辊压而砑光。
图1是基于厚度为0.01英寸的可变形石墨片显微镜观察结果的简图，该图示出了可变形石墨片10截面图，与平行的对置的平的表面22，24。30表示了包裹的陶瓷纤维颗粒。40说明了陶瓷纤维30对片10的穿透。
                          实施例I
在90％(重量)硫酸和10％(重量)硝酸混合物中处理天然石墨絮片，其80％(重量)絮片为50目。如此处理的嵌入石墨絮片用水洗涤并干燥到约1％(重量)水。一磅嵌入石墨絮片与0.15磅市售硅酸钙针形陶瓷纤维混合，其硅酸钙的长度直径比大部分为15-25％。将嵌入石墨和硅酸钙纤维混合物放入炉温为2500°F的炉中，可达到嵌入石墨絮片快速膨胀成蠕虫状的颗粒，其体积是未膨胀嵌入絮片的约325倍。膨胀的蠕虫状颗粒围绕着混入的硅酸钙纤维，其混合物辊压成可变形石墨片，其厚度为0.01英寸，宽度为24英寸，在该片中混合的硅酸钙从片表面延伸到片体内，其片含有约12％(重量)硅酸钙纤维。
图2电子显微镜图(100X-可见100微米大小)显示出陶瓷纤维100上部分，这部分穿透到可变形石墨片的平面表面22。图3至6，电压不断增加，看来“更深”入可变形石墨片，表明陶瓷纤维100穿透到可变形石墨片中。在140、160示出了在表面72以下的包裹在可变形石墨片中的陶瓷纤维。
                        实施例II
将宽度为8英寸的实施例I片样品浸没在10％用丙酮稀释的酚醛树脂的溶液中，并以每分钟10英尺速度拉过其溶液。在浸没与干燥之后，该样品表明重量增加18.7％。
该样品加热到235℃进行进一步处理，以便使树脂稳定，让片在压辊之间砑光达到密度为1.5克/厘米3。砑光片浸泡在油中和水中而没有影响。未加任何陶瓷纤维或树脂添加剂的对照片，接触到同样的试验条件，则重量增加约35％，厚度增加约8％。
含有5％、15％与25％(重量)硅酸钙纤维添加剂的样品片，以每分钟10英尺速度拉过树脂，树脂饱和量达到约17-19％(重量)。未加任何陶瓷纤维的对照样品以每分钟10英尺速度同样拉过时仅保留5％(重量)树脂。

Claims (3)

1、一种具有对置平的外表面的可变形石墨片，有多种针形陶瓷纤维颗粒分散体包裹在其中，这些颗粒与可变形石墨无反应性，在温度高达2000°F下是稳定的，所述的针形颗粒从至少一个所述的平的外表面延伸到所述的石墨片中，以便增加石墨片对液体树脂溶液的渗透性。
2、生产具有对置平的外表面的可变形石墨片的方法，其表面是可渗透液体树脂溶液的，该方法包括：
(1)用嵌入溶液处理天然石墨絮片，得到可热膨胀的嵌入石墨絮片颗粒；
(2)让1.5-30％(重量)针形陶瓷纤维颗粒与所述的嵌入石墨絮片颗粒混合，得到掺混混合物，所述的针形陶瓷纤维颗粒与可变形石墨无反应性，并在温度高达2500°F下是稳定的；
(3)让所述的嵌入的天然石墨絮片颗粒与针形陶瓷纤维颗粒的掺混混合物通过火焰，引起所述的嵌入天然石墨颗粒快速层离，得到一种所述的针形陶瓷纤维颗粒与已层离石墨颗粒的混合物；以及
(4)让所述的针形颗粒与已层离的石墨颗粒的混合物通过压力辊，生成一种可变形石墨的压制片，有许多针形颗粒的分散体包裹在其中，颗粒从至少一个所述的平的外表面延伸到片中。
3、根据权利要求2所述的方法，其中(1)步骤(4)的片浸没在树脂中，而树脂渗透片；(2)采用加热方法使树脂稳定；以及(3)让含有树脂的片在压力辊之间通过而使含有树脂的片砑光。
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US5902762A (en) 1999-05-11
TW397776B (en) 2000-07-11
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