CN1646448A - 碳化硅和无粘结剂碳的复合体及其制造方法 - Google Patents
碳化硅和无粘结剂碳的复合体及其制造方法 Download PDFInfo
- Publication number
- CN1646448A CN1646448A CNA038082519A CN03808251A CN1646448A CN 1646448 A CN1646448 A CN 1646448A CN A038082519 A CNA038082519 A CN A038082519A CN 03808251 A CN03808251 A CN 03808251A CN 1646448 A CN1646448 A CN 1646448A
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- Prior art keywords
- silicon carbide
- carbon
- binderless
- precursor
- producing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 163
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 137
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 89
- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 239000002245 particle Substances 0.000 claims abstract description 49
- 239000002243 precursor Substances 0.000 claims abstract description 47
- 239000008187 granular material Substances 0.000 claims abstract 3
- 229910002804 graphite Inorganic materials 0.000 claims description 42
- 239000010439 graphite Substances 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 42
- 238000005245 sintering Methods 0.000 claims description 36
- 239000002002 slurry Substances 0.000 claims description 30
- 239000011159 matrix material Substances 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- 239000005011 phenolic resin Substances 0.000 claims description 13
- 229920001568 phenolic resin Polymers 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical group [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 230000001050 lubricating effect Effects 0.000 claims description 10
- 229910021417 amorphous silicon Inorganic materials 0.000 claims description 9
- 238000000465 moulding Methods 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 5
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- 229910052790 beryllium Inorganic materials 0.000 claims description 5
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 5
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 4
- 229920000178 Acrylic resin Polymers 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 229910003481 amorphous carbon Inorganic materials 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 238000001694 spray drying Methods 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
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- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
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- 239000011295 pitch Substances 0.000 claims description 3
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- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
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- 125000000623 heterocyclic group Chemical group 0.000 claims description 2
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- 238000010000 carbonizing Methods 0.000 claims 5
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- 150000002894 organic compounds Chemical class 0.000 claims 3
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- 229930195733 hydrocarbon Natural products 0.000 claims 2
- 150000002430 hydrocarbons Chemical class 0.000 claims 2
- 239000007767 bonding agent Substances 0.000 claims 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052710 silicon Inorganic materials 0.000 abstract description 13
- 239000010703 silicon Substances 0.000 abstract description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 2
- 239000000843 powder Substances 0.000 description 21
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 229910052580 B4C Inorganic materials 0.000 description 7
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 7
- 239000000654 additive Substances 0.000 description 6
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
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- 229910001873 dinitrogen Inorganic materials 0.000 description 3
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- 238000003801 milling Methods 0.000 description 3
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- 230000007847 structural defect Effects 0.000 description 3
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 229910021418 black silicon Inorganic materials 0.000 description 2
- -1 graphite Chemical compound 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
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- 238000001272 pressureless sintering Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910021431 alpha silicon carbide Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
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- 239000010419 fine particle Substances 0.000 description 1
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- 238000005552 hardfacing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
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- 235000012054 meals Nutrition 0.000 description 1
- 239000011331 needle coke Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 235000019809 paraffin wax Nutrition 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
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- 239000012260 resinous material Substances 0.000 description 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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Abstract
制备了一种其中遍布着无粘结剂的同素异形碳颗粒的碳化硅复合体。这种无粘结剂同素异形碳颗粒的名义尺寸在5-500微米的范围。无粘结剂同素异形碳颗粒的含量可在1.0-35.0%的重量百分比内变化。制备这种复合体的方法是将碳化硅和无粘结剂的产碳前体颗粒一起烧结。这种复合体用在摩擦学应用中。这种致密的,不透水的碳化硅-无粘结剂碳复合体,当用作一种机械面密封,滑动轴承配置,或者其它一些磨损部件时,呈现出优异的物理和摩擦学特性。
Description
发明领域
本发明涉及碳化硅和无粘结剂的同素异形碳的复合体以及制造这种复合体的方法。更具体的,本发明涉及这样的复合体,其用于摩擦学应用中,比如机械密封,轴承以及其它的滑动或者磨损部件,其需要在低于理想润滑条件下有好的耐用性和磨损性能。
发明背景
材料科学一直以来是为具有或者可能具有彼此滑动接触的表面的部件选择材料的依据。例如,在机械面密封领域中,通常所知,由碳或者类碳材料制成的主环(primary ring),以及由另一种材料比如碳化硅,碳化钨,氧化铝,不锈钢等制成的接合环。然而,在暴露在高摩蚀流体中的机械面密封中,主环需要用比碳抗磨损更强的材料来制造。此种情况下,一种特殊的碳化硅会与一种硬质材料比如另一种碳化硅相对运动。为了提高这些硬面材料的摩擦相容性,特别是在较高的压力下,已经发展了特制的碳化硅等级。由于碳化硅的润滑性相对较差,许多发明者已经开发出在基体中结合使用石墨。
1985年8月20日授权的Kennedy等的US专利No.4536449描述了用反应键合的方法将石墨加入到碳化硅中。遗憾的是,由于通常存在2-20%的高活性自由硅,难以控制石墨的尺寸和含量。
Boecker等在1985年6月25日授权的US专利No.4525461中描述了通过无压烧结制成的含石墨的碳化硅。这种方法利用的是加入平均尺寸不超过8微米的小石墨颗粒。然而,由于与直接烧结工艺相伴的固有的高收缩,所加入的石墨颗粒的数量和尺寸受到这种方法的限制。
Okuno等在1987年10月20日授权的US专利No.4701426和1987年9月1日授权的US专利4690909中描述了碳化硅-石墨复合材料。依据这些专利,石墨或者碳黑加入到碳化硅中,形成一种复合材料,其中石墨具有的平均晶粒尺寸不超过3微米,并沿着所有碳化硅晶粒的晶界均匀分散形成第二相。
Moehle等在1990年7月17日授权的US专利No.4942145中描述了一种含石墨的碳化硅。这种方法建立在使用一种有机硅粘结剂的基础上,比如聚硅氮烷,碳化硅和石墨填料。将含有石墨的碳化硅与溶解在有机溶剂中的聚硅氮烷相混和,干燥,成型,并在1300℃左右热解。在一个实施例中,发现这种含石墨的碳化硅样品具有2.18gM/CM3的密度和15.9]~g/MM2(22600psi)的抗弯强度。
Talbert等在1996年8月6日授权的US专利No.5543368和1996年1月23日授权的US专利No.5486496中描述了一种含石墨的碳化硅。依据这些专利,首先将碳化硅粉末与粘结剂比如聚乙二醇和其它添加剂相混和,以促进石墨在浆料中的均匀分散。所公开的石墨的尺寸在3-4微米的范围。然后将含有石墨的浆料喷雾干燥成具有所希望的尺寸分布的石墨团聚体。依据这些专利,所报导的优选的平均球状石墨团聚体的尺寸在100微米左右。另外,通过相似的喷雾干燥技术,用亚微米的碳化硅和适当的添加剂制得碳化硅成型粉末。接下来,将所希望数量的石墨团聚体加入到喷雾干燥的碳化硅成型粉末中并与之混和。最后,依据1977年8月9日授权的Prochazka的US专利No.4041117中的教导加工成所希望的含石墨的碳化硅复合部件。使用松散结合的石墨团聚体代替固体石墨颗粒的结果,解决了往固有高收缩的自烧结碳化硅中加入石墨的问题。然而,这样一种方法会反过来影响材料摩擦性能的可重复性。
Chen等在1995年6月6日授权的US专利No.5422322和1997年8月12日授权的US专利No.5656563中描述了一种含石墨的碳化硅。在1999年11月2日授权的US专利No.5976429中描述了制造含石墨的碳化硅的方法。依据这些专利,首先将尺寸为45微米的石墨与溶解在有机溶剂比如丙酮中的酚醛树脂相混和。然后,将该混和物干燥,把溶剂蒸发掉,并进行粉碎,过200目筛。接下来,将所希望数量的树脂结合的石墨加入到由亚微米碳化硅和相应的添加剂组成的浆料中。将此浆料喷雾干燥,制成平均尺寸小于500微米的球状颗粒。将喷雾干燥的成型化合物压制成所希望的形状,碳化到850T,并在优选的2000-2200℃下于惰性气氛比如氦或者氩中烧结。烧结后的碳化硅-石墨复合物中含有2-30%重量百分比的碳结合的石墨。这种复合物,特别是在较高的碳结合石墨浓度时,含有在此专利中所说的微裂纹的结构缺陷。并且,碳结合石墨颗粒的形状是不规则的,这使得在该烧结的复合材料中应力浓度最大化。而且,树脂包覆的石墨的大并且不可控的颗粒尺寸分布影响碳化硅基体的固有的高收缩的可重复性。
用与现有技术不同的方法制造的含石墨的碳化硅,似乎是一种具有满足高要求的摩擦学应用的工艺特性的坚硬材料。
发明内容
这里所公开并要求保护的发明包括一种遍布着无粘结剂的同素异形碳的碳化硅复合体,一种制造这种复合体的方法,以及一种利用这样的复合体制造的用于摩擦学应用中的部件。制造这种复合体的步骤包括制备碳化硅和无粘结剂的产生同素异形碳的前体颗粒的混和物,然后,将该混和物成型加热成所希望的复合体。依据本发明制造的部件可以制成各种形状以用于摩擦学应用中,比如机械面密封。
附图简述
图1是依据本发明制造碳化硅-无粘结剂碳复合体的方法示意图。
图2是这种复合体的抛光环的表面形貌,该复合体用喷雾干燥的碳化硅粉末和生焦炭(green coke)的混和物制成。
图3是这种复合体的抛光环的表面形貌,该复合体用喷雾干燥的碳化硅粉末和喷雾干燥的酚醛树脂的混和物制成。
图4是这种复合体的抛光环的表面形貌,该复合体用喷雾干燥的碳化硅粉末和球状中间相微珠的混和物制成。
优选实施方案详述
依据本发明,已经发现,通过往自烧结碳化硅基体中加入无粘结剂的产碳前体颗粒,比如未煅烧的生焦炭,酚醛树脂,球状中间相碳,煤焦油沥青,石油沥青,产碳树脂,沥青,烟煤,石油焦炭,灯黑,炭黑或者其它的含碳颗粒,用于磨损应用,比如机械面密封,轴承等中的自烧结碳化硅的性能特性会有预想不到的提高。依据本发明制造的部件可以制备成各种形状,例如杆状,管状,板状等,以用在密封,轴承,叶片,活塞,阀门座等中。
依据本发明制成的碳化硅复合体可以依据大量的标准的无压自烧结碳化硅的制造工艺中的任何一种制造。制造这种碳化硅-无粘结剂碳复合体的工艺示意图如图1中所示。
对于本发明,优选的原料是用Acheson工艺制造的alpha相碳化硅。Alpha碳化硅包含多种不同的晶体结构,六方和菱方多型体是最主要的。Acheson工艺制造的碳化硅依赖于杂质的种类和数量可以是绿色的或者黑色的。绿色的碳化硅比黑色的含杂质少。黑色碳化硅晶粒中的主要杂质是铝,碳和自由硅。本发明优选的碳化硅是绿色的。然而,更丰富的黑色碳化硅也可以使用。也可以采用Beta相碳化硅,无定形碳化硅,alpha相碳化硅以及它们的混和物。碳化硅可以是球状的,椭球状的或者无规则形状的。
用于自烧结工艺的碳化硅必须具有精细的颗粒尺寸,主要在亚微米范围。碳化硅粉末的表面积优选的用B.E.T.方法测定在5-15平方米每克。可以通过标准的球磨技术,利用碳化硅研磨介质,将粗碳化硅磨到所希望的颗粒尺寸范围。然而,这可能需要进一步化学提纯,以去除阻碍烧结工艺的杂质。初始的碳化硅原料应该小于100微米,以得到经济的研磨处理量。尽管所希望颗粒尺寸的碳化硅可以从许多提供商得到,但研磨工艺是优选方法,因为进行研磨的同时可以和所希望数量的烧结助剂相混和,比如碳化硼,这是无压自烧结工艺所需要的。也可以用元素硼,铝,铍,碳或者它们的结合来催化碳化硅的致密化工艺。优选的碳化硼的浓度为大约0.5-2.0%的重量百分比。同样,亚微米的碳化硼也可以从许多提供商获得。
具有所希望的颗粒尺寸分布的碳化硅含有相当数量的表面氧化物。为了有助于烧结,通过未结合的碳与粉末按下式的反应,将这些表面氧化物去除:
优选的,这种未结合的碳均匀分布在碳化硅颗粒表面上。这可以通过往碳化硅粉末中加入液态的含碳前体来得到。尽管可以使用任何的水或者溶剂可溶的含碳前体,优选的材料是水溶性的酚醛树脂,基于原料中碳化硅的含量,其在2-8%重量百分比的范围。
为了有助于形成结实的生坯,需要加入的另一种添加剂优选的是具有低的焦炭产量的水溶性有机树脂材料。这些可接受的暂时的挥发性粘结剂的例子包括可溶的聚乙烯醇,丙烯酸的水溶性树脂,酚醛树脂,煤焦油沥青以及其它含碳材料。
为了有助于粉末的致密化工艺,必须往原料中加入有机润滑化合物,比如聚乙烯醇,油酸,丙烯酸,湿润剂,硬脂酸,石蜡或者脂肪酸。这种添加剂的浓度基于碳化硅的含量在0.5-3.0%重量百分比的范围,或者占总混和物的0.1-15.0%的重量百分比。
制造自润滑碳化硅-碳复合物的关键成分是无粘结剂的产碳前体颗粒。在无压烧结过程中,所生产的该人工制品的线性收缩可以达到17%。这种收缩的结果,使得加入无收缩的碳比如石墨将要么阻碍致密化工艺,要么产生结构缺陷。为了将石墨加入到致密的碳化硅基体中,石墨的颗粒尺寸和浓度必须小而低。在现有技术中,已经有报导采用含碳的粘结剂石墨复合物颗粒来代替石墨。
依据本发明,通过采用无粘结剂的产碳前体颗粒,比如未煅烧的生焦炭,酚醛树脂,球状中间相碳以及其它含碳颗粒,可以将高浓度的自由石墨或者碳加入到碳化硅基体中,而不产生结构缺陷。该生料粉末的典型组成为93.5%的碳,4.5%的氢,1.0%的氮和1.0%的氧。可用的该生料粉末的平均颗粒尺寸在1-80微米的范围。在碳化硅基体中的中间相微珠的浓度在2-30%重量百分比的范围。平均颗粒尺寸在25-80微米的范围。
烧结温度超过2100℃的结果,高取向的芳香族前体将收缩并转变成石墨。采用球状颗粒也会生成的碳化硅-碳复合物,与由不规则形状的碳制成的复合物相比,还具有较低的内部应力。不过,在制造碳化硅-石墨复合物时,仍可使用高取向的生的针状焦炭。
总之,可以依据需要,对这种碳化硅-碳复合物进行定制制造。可以通过采用一种产石墨的高取向的芳香族前体或者一种产生无定形碳的,低取向的杂环含碳前体,来控制碳化硅-碳基体的摩擦学性能。
如图1中所示,制造自烧结碳化硅-碳复合物的方法从制造精细碳化硅粉末的碳化硅水浆料开始。接下来,将所希望数量的亚微米的碳化硼,或者其它烧结助剂,加入到这种浆料中。由于超细碳化硅中含有相当数量的表面氧化物,必须往浆料中加入含碳前体,比如水溶性的酚醛树脂。树脂的优选用量在占碳化硅粉末的2-8%重量百分比的范围。接下来,将暂时的粘结剂,优选的是水溶性的丙烯酸树脂,加入到碳化硅浆料中。这种暂时的粘结剂的优选用量在占碳化硅粉末的2-8%的重量百分比的范围。基于浆料中碳化硅的含量,还要往浆料中加入0.5-3.0%重量百分比的有机润滑化合物,比如硬脂酸。然而,加入这种成分的优选方法是将其与喷雾干燥的碳化硅浆料干混。
将包含所有上述成分的浆料按照标准的喷雾干燥技术喷雾干燥。然后,将喷雾干燥的颗粒与所希望数量的产碳前体颗粒相混和。接下来,将此混和物压制成所希望的形状,固化,并如果需要的话,进行生坯加工。由于该人工制品中的含碳组分必须在大气条件下作加热处理,以得到所希望数量的碳含量,并且烧结工艺优选的在减压下进行,因此焦化和烧结工艺在不同的设备中分开进行。首先,在惰性气氛中,将该人工制品加热到大约600℃。这种热处理的结果,使该人工制品可以在减压下烧结,以有助于碳表面氧化物的反应。烧结首先在可达1800℃的真空下进行,然后是在氩或者氦中,于300-500torr的绝对压力下进行。峰值烧结温度在2100-2200℃的范围。
已经详细描述了优选的实施方案。作为结果,本领域技术人员可对本发明进行大量的更改。下面,通过实施例对本发明作更加详细的描述。这些实施例的目的仅仅是为了说明,而不想限制本发明的范围。
实施例1
制备如下组成的原料:
组分
重量百分比
碳化硅 85.4
碳化硼 0.6
酚醛树脂 7.0
丙烯酸树脂 5.0
聚乙烯醇 1.0
油酸 1.0
该亚微米碳化硅的B.E.T.表面积为15m2/g。中值颗粒尺寸为0.6微米。所用的是商业可获的碳化硼,其B.E.T.表面积为15-20m2/g,中值颗粒尺寸为0.5微米。液态的水基酚醛树脂具有70%的固体含量。水乳液丙烯酸树脂具有45%的固体含量。聚乙烯醇具有21%的固体含量。在这种配方中采用的是蒸馏动物脂基油酸。
用上述组分制成40%重量百分比的水基浆料。首先,将碳化硅粉末加入到所希望数量的蒸馏水中。在碳化硅加入过程中将水持续搅拌。接下来,将所希望数量的碳化硼加入到浆料中。最后将少量的有机成分加入到持续搅拌的浆料中。在混和1小时之后,依据本领域技术人员熟知的标准的成熟的方法将该浆料进行喷雾干燥。将喷雾干燥后的粉末用100目筛过筛,除去大的不想要的颗粒。然后将这种自由流动的成型粉末按如下实施例中所描述的进行处理。
实施例2
将可挥发性含量为14%的生焦炭研磨,并用100目筛过筛,制得颗粒尺寸小于150微米的粉末。将这种粉末与实施例1中所述的碳化硅成型粉末干混。制得如下配方的混和物:
组分
重量百分比
喷雾干燥的碳化硅成型粉末 95.0
生焦炭 5.0
将上述混合物在一个装有增强杆的V-形混和器中混和5分钟。用这种粉末在17000psi的压力下等静压成型管件。将这些成型管件在175℃下固化,并进行生坯加工成所希望的环状。将这些环在真空中于2100℃烧结。这些烧结部件的密度在大约3.02g/cm3。图2给出了这些抛光环的表面形貌。这些环用100psig的氮气检测表明是不透气的。发现这些环中没有微裂纹。
实施例3
将喷雾干燥的酚醛树脂过筛,去除所有大于150微米的颗粒。将这种粉末与碳化硅成型粉末按照下面的配方干混:
组分
重量百分比
喷雾干燥的碳化硅成型粉末 95.0
喷雾干燥的酚醛树脂 5.0
将上述混和物在一个装有增强杆的V-形混和器中混和5分钟。用上述粉末混和物在17000psi的压力下等静压成型管件。将这些成型管件在175℃下固化,并进行生坯加工成所希望的环状。将这些加工后的环首先在氮气氛中于600℃碳化,然后在真空中于2100℃烧结。这些烧结部件的测量密度在大约2.95g/cm3。图3给出了这些抛光环的表面形貌。必须看到,依据上述方法制备的这些环中没有微裂纹以及/或者互连孔。这些环还用100psig的氮气检测表明是不透气的。
实施例4
用从煤焦油沥青中制得的球状的生中间相含碳粉末作为碳化硅成型粉末的添加剂。这种中间相微珠的平均尺寸为大约25微米。采用如下配方:
组分
重量百分比
喷雾干燥的碳化硅成型粉末 97.5
球状的生的中间相微珠 2.5
将上述混和物在一个装有增强杆的V-形混和器中混和5分钟。用上述粉末混和物在17000psi的压力下等静压成型管件。将这些成型管件在1750℃下固化,并进行生坯加工成所希望的环状。将这些加工后的环首先在氮气氛中于600℃碳化,然后在真空中于2100℃烧结。这些烧结部件的测量密度在大约3.10g/cm3。图4给出了这些抛光环的表面形貌。这些环还用100psig的氮气检测表明是不透气的。发现这些环中不含微裂纹。
在上面所引的实施例中,并结合具体的实施方案对本发明进行了详细描述。所进行的这些描述的目的是为了说明,而不会彻底覆盖或者限制本发明。只要不脱离下面权利要求中本发明的范围和主旨,可以根据本发明的教导对所制器件进行各种改变和完善。
Claims (98)
1.一种碳化硅复合体,包括:
a.用无压自烧结方法制备的烧结碳化硅基体;以及
b.遍布于碳化硅基体中的无粘结剂的同素异形碳颗粒。
2.权利要求1中的碳化硅复合体,其中的无粘结剂的同素异形碳颗粒均匀分布在整个碳化硅基体中。
3.权利要求1中的碳化硅复合体,其中,无粘结剂的同素异形碳颗粒构成该复合体的1.0-35.0%的重量百分比。
4.权利要求1中的碳化硅复合体,其中,无粘结剂的碳颗粒具有石墨结构。
5.权利要求1中的碳化硅复合体,其中,无粘结剂的碳颗粒具有无定形碳结构。
6.权利要求1中的碳化硅复合体,其中,无粘结剂的碳颗粒含有内部空隙。
7.权利要求1中的碳化硅复合体,其中,碳化硅基体具有球状形貌。
8.权利要求1中的碳化硅复合体,其中,碳化硅基体具有椭球状形貌。
9.权利要求1中的碳化硅复合体,其中,碳化硅基体具有不规则形貌。
10.权利要求1中的碳化硅复合体,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
11.权利要求7中的碳化硅复合体,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
12.权利要求8中的碳化硅复合体,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
13.权利要求9中的碳化硅复合体,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
14.权利要求1中的碳化硅复合体,其中,碳化硅是alpha相的碳化硅。
15.权利要求1中的碳化硅复合体,其中,碳化硅是beta相的碳化硅。
16.权利要求1中的碳化硅复合体,其中,碳化硅是无定形的碳化硅。
17.权利要求1中的碳化硅复合体,其中,碳化硅是如下两种或者多种的混和物:alpha相的碳化硅,beta相的碳化硅和无定形的碳化硅。
18.一种制造碳化硅复合体的方法,包括步骤:
a.制备包括如下组分的混和物:
i.碳化硅,
ii.烧结助剂,以及
iii.无粘结剂的,产碳前体颗粒,不含无收缩的碳;
b.将该混和物成型;以及
c.将成型后的混和物烧结。
19.权利要求18中的方法,其中,碳化硅是alpha相的碳化硅。
20.权利要求18中的方法,其中,碳化硅是beta相的碳化硅。
21.权利要求18中的方法,其中,碳化硅是无定形的碳化硅。
22.权利要求18中的方法,其中,碳化硅是如下两种或者多种的混和物:alpha相的碳化硅,beta相的碳化硅和无定形的碳化硅。
23.权利要求18中的方法,其中,无粘结剂的产碳前体是产生石墨的、高取向的芳香族前体。
24.权利要求18中的方法,其中,无粘结剂的产碳前体是产生无定形碳的低取向的杂环含碳前体。
25.权利要求18中的方法,其中,无粘结剂的产碳前体是未煅烧的生焦炭。
26.权利要求18中的方法,其中,无粘结剂的产碳前体是酚醛树脂。
27.权利要求18中的方法,其中,无粘结剂的产碳前体是球状中间相碳。
28.权利要求18中的方法,其中,无粘结剂的产碳前体是含碳的颗粒。
29.权利要求18中的方法,其中,无粘结剂的产碳前体是产碳树脂。
30.权利要求18中的方法,其中,无粘结剂的产碳前体是煤焦油沥青。
31.权利要求18中的方法,其中,无粘结剂的产碳前体是石油沥青。
32.权利要求18中的方法,其中,无粘结剂的产碳前体是沥青。
33.权利要求18中的方法,其中,无粘结剂的产碳前体是烟煤。
34.权利要求18中的方法,其中,无粘结剂的产碳前体是石油焦炭。
35.权利要求18中的方法,其中,无粘结剂的产碳前体是灯黑。
36.权利要求18中的方法,其中,无粘结剂的产碳前体是炭黑。
37.权利要求18中的方法,其中,无粘结剂的产碳前体的量占总混和物的1.0-35.0%的重量百分比。
38.权利要求18中的方法,其中,烧结助剂是硼。
39.权利要求18中的方法,其中,烧结助剂是铝。
40.权利要求18中的方法,其中,烧结助剂是铍。
41.权利要求18中的方法,其中,烧结助剂是碳。
42.权利要求18中的方法,其中,烧结助剂是含有如下一种或者多种的化合物:硼,铝,铍和碳。
43.权利要求18中的方法,其中,烧结助剂的含量占总混和物的0.1-15.0%的重量百分比。
44.一种制备碳化硅复合体的方法,包括步骤:
a.制备一种混和物,包括:
i.液态介质,
ii.碳化硅,
iii.烧结助剂,
iv.湿润剂,
v.抗絮凝剂,
vi.产碳有机化合物,
vii.暂时的粘结剂,
viii.有机润滑剂,以及
ix.无粘结剂的产碳前体颗粒,不含无收缩碳;
b.将此混和物压制成固结体;
c.将此固结体固化;
d.将此固结体碳化;以及
e.将此固结体烧结。
45.权利要求44中制备碳化硅复合体的方法,其中制备混和物的步骤包括:
a.将碳化硅与烧结助剂在液体介质中研磨,制成浆料;
b.往浆料中加入湿润剂和抗絮凝剂;
c.往浆料中加入无粘结剂的产碳前体颗粒,该前体颗粒不含无收缩碳;
d.往浆料中加入产碳的有机化合物;
e.往浆料中加入暂时的粘结剂;
f.往浆料中加入润滑剂;以及
g.将此浆料喷雾干燥;
46.权利要求44中制备碳化硅复合体的方法,其中制备混和物的步骤包括:
a.将碳化硅与烧结助剂在液体介质中研磨,制成一种浆料;
b.往浆料中加入湿润剂和抗絮凝剂;
c.往浆料中加入产碳的有机化合物;
d.往浆料中加入暂时的粘结剂;
e.往浆料中加入润滑剂;
f.将此浆料喷雾干燥;并
g.将不含无收缩碳的无粘结剂的产碳前体颗粒与喷雾干燥的浆料干混。
47.权利要求44中制备碳化硅复合体的方法,其中对此混和物进行压制,固化,碳化和烧结的步骤包括:
a.将此混和物等静压制成固结体;
b.将此固结体固化,使树脂聚合;
c.对此固结体进行生坯加工;
d.将此固结体碳化;并
e.将此固结体烧结。
48.权利要求44中制备碳化硅复合体的方法,其中对此混和物进行压制,固化,碳化和烧结的步骤包括:
a.将此混和物模压制成固结体;
b.将此固结体固化,使树脂聚合;
c.将此固结体碳化;并
d.将此固结体烧结。
49.权利要求44中的方法,其中,碳化硅是alpha相的碳化硅。
50.权利要求4 4中的方法,其中,碳化硅是beta相的碳化硅。
51.权利要求44中的方法,其中,碳化硅是无定形的碳化硅。
52.权利要求44中的方法,其中,碳化硅是如下两种或者多种的混和物:alpha相的碳化硅,beta相的碳化硅和无定形的碳化硅。
53.权利要求44中的方法,其中,无粘结剂的产碳前体是未煅烧的生焦炭。
54.权利要求44中的方法,其中,无粘结剂的产碳前体是酚醛树脂。
55.权利要求44中的方法,其中,无粘结剂的产碳前体是球状中间相碳。
56.权利要求44中的方法,其中,无粘结剂的产碳前体是含碳的颗粒。
57.权利要求44中的方法,其中,无粘结剂的产碳前体是产碳树脂。
58.权利要求44中的方法,其中,无粘结剂的产碳前体是煤焦油沥青。
59.权利要求44中的方法,其中,无粘结剂的产碳前体是石油沥青。
60.权利要求44中的方法,其中,无粘结剂的产碳前体是沥青。
61.权利要求44中的方法,其中,无粘结剂的产碳前体是烟煤。
62.权利要求44中的方法,其中,无粘结剂的产碳前体是石油焦炭。
63.权利要求44中的方法,其中,无粘结剂的产碳前体是灯黑。
64.权利要求44中的方法,其中,无粘结剂的产碳前体是碳黑。
65.权利要求44中的方法,其中,无粘结剂的产碳前体的含量占总混和物的1.0-35.0%的重量百分比。
66.权利要求44中的方法,其中,烧结助剂是硼。
67.权利要求44中的方法,其中,烧结助剂是铝。
68.权利要求44中的方法,其中,烧结助剂是铍。
69.权利要求44中的方法,其中,烧结助剂是碳。
70.权利要求44中的方法,其中,烧结助剂是含有如下一种或者多种的化合物:硼,铝,铍和碳。
71.权利要求44中的方法,其中,烧结助剂的含量占总混和物的0.1-15.0%的重量百分比。
72.权利要求4 4中的方法,其中,有机润滑化合物是聚乙烯醇。
73.权利要求44中的方法,其中,有机润滑化合物是油酸。
74.权利要求44中的方法,其中,有机润滑化合物是丙烯酸树脂。
75.权利要求44中的方法,其中,有机润滑化合物是湿润剂。
76.权利要求44中的方法,其中,有机润滑化合物是硬脂酸。
77.权利要求44中的方法,其中,有机润滑化合物是石蜡。
78.权利要求44中的方法,其中,有机润滑化合物是脂肪酸。
79.权利要求44中的方法,其中,有机润滑化合物的含量占总混和物的1.0-20.0%的重量百分比。
80.权利要求44中的方法,其中,混和物中包括另外的来自原料中的无机杂质组分。
81.一种由碳化硅复合体制成的用于摩擦学应用中的制品,包括:
a.用无压自烧结方法制备的烧结碳化硅基体;以及
b.遍布在碳化硅基体中的无粘结剂的同素异形碳颗粒。
82.权利要求81中的制品,其中的无粘结剂的同素异形碳颗粒均匀的遍布在碳化硅基体中。
83.权利要求81中的制品,其中,碳化硅复合体是一种机械面密封部件。
84.权利要求81中的制品,其中,无粘结剂的同素异形碳颗粒构成该复合体的1.0-35.0%的重量百分比。
85.权利要求81中的制品,其中,无粘结剂的碳颗粒具有石墨结构。
86.权利要求81中的制品,其中,无粘结剂的碳颗粒具有无定形碳结构。
87.权利要求81中的制品,其中,无粘结剂的碳颗粒含有内部空隙。
88.权利要求81中的制品,其中,碳化硅基体具有球状形貌。
89.权利要求81中的制品,其中,碳化硅基体具有椭球状形貌。
90.权利要求81中的制品,其中,碳化硅基体具有不规则形貌。
91.权利要求81中的制品,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
92.权利要求88中的制品,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
93.权利要求89中的制品,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
94.权利要求90中的制品,其中,无粘结剂的同素异形碳颗粒的尺寸在5-500微米之间。
95.权利要求81中的制品,其中,碳化硅是alpha相的碳化硅。
96.权利要求81中的制品,其中,碳化硅是beta相的碳化硅。
97.权利要求81中的制品,其中,碳化硅是无定形的碳化硅。
98.权利要求81中的制品,其中,碳化硅是如下两种或者多种的混和物:alpha相的碳化硅,beta相的碳化硅和无定形的碳化硅。
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US10/122,293 US6716800B2 (en) | 2002-04-12 | 2002-04-12 | Composite body of silicon carbide and binderless carbon, process for producing such composite body, and article of manufacturing utilizing such composite body for tribological applications |
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2003
- 2003-04-10 BR BR0309201-1A patent/BR0309201A/pt not_active Application Discontinuation
- 2003-04-10 EP EP03723985A patent/EP1499572A4/en not_active Withdrawn
- 2003-04-10 MX MXPA04009915A patent/MXPA04009915A/es active IP Right Grant
- 2003-04-10 CN CNB038082519A patent/CN100337983C/zh not_active Expired - Fee Related
- 2003-04-10 WO PCT/US2003/011206 patent/WO2003087013A1/en active Application Filing
- 2003-04-10 JP JP2003583972A patent/JP2005523225A/ja active Pending
- 2003-04-10 AU AU2003230879A patent/AU2003230879B2/en not_active Ceased
- 2003-04-10 KR KR10-2004-7016097A patent/KR20050003355A/ko not_active Application Discontinuation
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Publication number | Publication date |
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MXPA04009915A (es) | 2004-12-07 |
EP1499572A4 (en) | 2009-12-30 |
JP2005523225A (ja) | 2005-08-04 |
US20030195122A1 (en) | 2003-10-16 |
WO2003087013A1 (en) | 2003-10-23 |
AU2003230879A1 (en) | 2003-10-27 |
CA2480156C (en) | 2008-12-23 |
KR20050003355A (ko) | 2005-01-10 |
US6716800B2 (en) | 2004-04-06 |
BR0309201A (pt) | 2005-02-01 |
AU2003230879B2 (en) | 2008-04-17 |
EP1499572A1 (en) | 2005-01-26 |
CN100337983C (zh) | 2007-09-19 |
CA2480156A1 (en) | 2003-10-23 |
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