CN100465135C - 包含分散于其中的金属碳化物颗粒的碳复合材料及其制备方法 - Google Patents
包含分散于其中的金属碳化物颗粒的碳复合材料及其制备方法 Download PDFInfo
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- CN100465135C CN100465135C CNB2005800126808A CN200580012680A CN100465135C CN 100465135 C CN100465135 C CN 100465135C CN B2005800126808 A CNB2005800126808 A CN B2005800126808A CN 200580012680 A CN200580012680 A CN 200580012680A CN 100465135 C CN100465135 C CN 100465135C
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Abstract
本发明涉及碳复合材料,所述碳复合材料包含分散在碳、碳纤维或碳/碳纤维基体中的金属碳化物颗粒且不含游离金属颗粒,其中金属碳化物颗粒在至少颗粒表面或整个颗粒为金属碳化物,由金属源(即选自金属颗粒、金属氧化物颗粒或复合金属氧化物颗粒中的至少一种)和碳源(即热固性树脂)在原位合成。本发明还提供了制备这种碳复合材料的方法,制得的碳复合材料摩擦系数大、热稳定性高并且耐磨损。
Description
技术领域
本发明涉及摩擦系数大、热稳定性高并且耐磨的碳复合材料。本发明还涉及这种碳复合材料的制备方法。
背景技术
碳材料与碳纤维结合可制备复合材料。已知此种方法能有效地改善碳材料的性能。例如,包含高强度碳纤维的碳纤维/碳复合材料被称为CC复合材料。与传统的金属材料相比,这种复合材料具有优异的比强度(即,强度/密度),因而其在各个领域中的应用日益广泛。例如,这样的CC复合材料被用于车辆和飞行器的制动垫片。
已经尝试了各种通过在碳材料中分散第二相颗粒来制备增强碳复合材料的技术。尽管分散颗粒的添加改善了复合材料的耐磨性,但是添加的颗粒有时会成为材料中的断裂源,并且不利地使材料的强度降低。因此,为了通过加入第二相颗粒以使碳材料的强度和耐磨性均得到改善,必须能以所需量添加精细的第二相颗粒,而不降低材料的强度。为了达到令人满意的强度,必须添加平均粒径为1μm或更小的精细的第二相颗粒。因而具有碳基体的第二相颗粒是合适的。这样的颗粒的例子包括高纯度金属碳化物,诸如碳化钨、碳化钛和碳化硅,它们在制备指定的元件的工艺中保持稳定而不变性。
然而,以低成本的方式来制备高纯度金属碳化物的精细颗粒具有很大的技术难度。随着金属氧化物颗粒的直径越来越小,团聚和其他行为导致颗粒在具有碳基体相的材料中的分散变得越来越难。因此,在技术上难以将这样的颗粒均匀地结合到具有碳基体相的材料中。在制备具有很大比表面积的精细颗粒的制备工艺过程中,这样的颗粒的表面容易被氧化。因此,实际上不可能制备由碳材料和高纯度金属碳化物精细颗粒组成的复合材料。
日本专利公开特开平No.11-130537公开了制备包含分散于其中的平均粒径为1μm或更小的增强金属碳化物颗粒的碳复合材料的方法,其中,具有碳基体相的起始粉末材料预先与至少一种金属氧化物混合,该混合物被成型然后煅烧,用沥青浸渍煅烧产物,之后再次煅烧。该方法旨在以高效和低成本的方式来制备包含分散于其中的增强、高纯、精细的金属碳化物的颗粒的碳复合材料。
日本专利公开特开平No.11-217267公开了制备二维纤维增强碳化硅-碳复合陶瓷的方法,该方法包括:使包含硅粉末、作为碳源的树脂和二维纤维增强材料的成形产物形成期望的形状;在惰性气氛中在900℃至1300℃下碳化该成形产物;用树脂浸渍所得产物,在惰性气氛中在900℃至1300℃下对已浸渍的材料进行再烧结;重复上述树脂浸渍和烧结步骤;最后在惰性气氛中在约1350℃至1500℃下烧结该材料。该方法旨在通过用树脂浸渍陶瓷以及反应烧结法来容易地制备尽管孔隙率高但是具有高强度和复杂形状的二维纤维增强碳化硅-碳复合陶瓷。
发明内容
根据日本专利公开特开平No.11-130537中公开的方法,粉状金属氧化物与粉状碳混合,并且生成的金属氧化物的分散能力不足。因此,在金属氧化物附近提供的碳量不够,并且金属氧化物与碳之间的反应进行得不充分。
根据日本专利公开特开平No.11-217267中公开的方法,SiC是通过金属硅与碳之间的直接反应而生成的。因而不利地残留未反应的金属硅作为游离的金属硅。
本发明的目的是提供摩擦系数大、热稳定性高并且耐磨的碳复合材料,并且提供制备这样的碳复合材料的方法。
本发明人发现,上述目的可通过将给定的金属源与碳源结合并在原位生成金属碳化物的颗粒来实现。这导致了本发明的完成。
具体地,本发明的第一方面涉及包含碳复合材料的摩擦材料,所述碳复合材料包含分散在碳、碳纤维或碳/碳纤维基体中的金属碳化物颗粒且不含游离金属颗粒,其中金属碳化物颗粒在至少颗粒表面上或整个颗粒中为金属碳化物,由金属源(即选自金属颗粒、金属氧化物颗粒和复合金属氧化物颗粒中的至少一种)和碳源(即热固性树脂)在原位合成。
碳复合材料中原位合成的金属碳化物颗粒、金属氧化物或复合金属氧化物的平均粒径并无具体限制。例如,可为2μm至5μm。金属碳化物颗粒、金属氧化物或复合金属氧化物的形状并无具体限制。例如,这样的颗粒的形状可为近似球形或非球形。
优选地,金属源选自例如Si、Ti、Zr、Al、W、Cr和Zn的金属颗粒中的至少一种。这些金属颗粒可以被氧化以得到SiO2、TiO2、ZrO2、Al2O3、WO3、CrO3和ZnO颗粒,选自其中的至少一种金属氧化物颗粒或复合金属氧化物颗粒也优选用作金属源。
更具体地,优选地,作为金属源的金属氧化物颗粒为SiO2颗粒,并且由此生成的金属碳化物颗粒为SiC颗粒。SiO2颗粒的优选例子包括通过金属硅与氧之间的反应得到的球形二氧化硅颗粒、通过熔解破碎的二氧化硅而得到的球形二氧化硅颗粒、以及破碎的二氧化硅颗粒。而且,优选地,作为金属源的复合金属氧化物颗粒为SiO2/ZrO2复合金属氧化物,并且由此生成的金属碳化物颗粒为SiC/ZrC复合碳化物颗粒。
本发明的第二方面涉及制备包括包含分散于其中的金属碳化物颗粒的碳复合材料的的摩擦材料的方法,其中金属颗粒、金属氧化物颗粒和复合金属氧化物颗粒中的至少一种被分散在热固性树脂中,以得到浆液混合物,用该浆液混合物浸渍碳纤维,并且进行碳化以碳化热固性树脂,然后进一步进行煅烧以原位合成金属碳化物(至少颗粒表面或整个颗粒为金属碳化物)。
图1示出了制备包含分散于其中的金属碳化物颗粒的碳复合材料的一个实施例的流程图。
如同本发明的第一方面,例如,优选使用至少一个选自Si、Ti、Zr、Al、W、Cr和Zn的金属颗粒的金属源。而且,这些金属颗粒可以被氧化以得到SiO2、TiO2、ZrO2、Al2O3、WO3、CrO3和ZnO颗粒,选自其中的至少一种金属氧化物颗粒或复合金属氧化物颗粒也优选用作金属源。
更具体地,优选地,作为金属源的金属氧化物颗粒为SiO2颗粒,并且由此生成的金属碳化物颗粒为SiC颗粒。优选地,SiO2颗粒的例子包括通过金属硅与氧之间的反应得到的球形二氧化硅颗粒、通过熔解破碎的二氧化硅而得到的球形二氧化硅颗粒、以及破碎的二氧化硅颗粒。
对作为碳源的热固性树脂并无具体限制。例如,可以使用的热固性树脂例如为酚醛树脂、三聚氰胺树脂、脲醛树脂、环氧树脂、不饱和聚酯树脂、醇酸树脂、硅酮树脂、邻苯二甲酸二烯丙酯树脂、聚酰胺-双马来酰亚胺树脂、丙烯酸树脂、呋喃树脂、聚氨酯树脂、苯胺树脂或聚双酰胺***树脂,或由这些树脂中的两种或多种组成的热固性树脂。特别优选具有高碳含量的酚醛树脂。
在本发明中,对于制备浆液混合物的方法并无具体限制,所述浆液混合物包含至少一种分散在作为碳源的热固性树脂中的选自金属颗粒、金属氧化物颗粒和复合金属氧化物颗粒的金属源。为了得到具有良好分散条件的稳定的浆液混合物,优选向浆液混合物中添加分散稳定剂,或者优选用表面活性剂处理作为金属源的颗粒。
由于浆液混合物是包含金属氧化物颗粒和并入酚醛树脂溶液的分散剂的溶液,分散剂的使用可使金属氧化物均匀分散在酚醛树脂中。金属氧化物的均匀分散可使碳以反应所需的量存在,从而实现有效反应。
在本发明中,在浸渍步骤之后、碳化步骤之前,通过层压浸渍产物来进行热压结合步骤。因而,可以得到具有给定厚度和强度的碳复合材料。
在本发明中,出于制备高密度的金属碳化物的考虑,优选进行两次或更多次的用浆液混合物来浸渍碳纤维材料的步骤,所述浆液混合物包含分散在作为碳源的热固性树脂中的作为金属源的颗粒。例如,在通过煅烧工艺来原位制备金属碳化物颗粒之前,作为金属源的颗粒被分散在热固性树脂中以得到浆液混合物,并且用该浆液混合物浸渍碳纤维以使其碳化。此过程进行两次或多次。或者,在通过煅烧工艺原位制备金属碳化物颗粒之后,作为金属源的颗粒被分散在热固性树脂中以得到浆液混合物,并且用该浆液混合物浸渍碳纤维以使其碳化。此过程被重复一次或多次。
通过在煅烧过程中使二氧化硅与碳反应来生成碳化硅的反应是固-气反应。由于一氧化硅与碳在气相中反应,因此为了制备碳化硅颗粒,使二氧化硅颗粒被碳完全覆盖而不留下任何间隙是重要的。在复合材料成型之后,通过在500℃或更高的温度下加热,将酚醛树脂碳化,并且使其收缩。因而,形成了间隙。一氧化硅气体从该间隙泄漏,形成碳化硅颗粒的可能性减小。在煅烧步骤之前,用液态酚醛树脂浸渍成形产物,然后再进行煅烧,二氧化硅颗粒完全被碳覆盖而不留下任何间隙。因此,生成了碳化硅颗粒。
在本发明中,碳化在惰性气氛中,在200℃至1600℃、优选杂500℃至1000℃下进行。煅烧是在热固性树脂在惰性气氛中热分解并且成为碳源的温度下进行的,例如1650℃或更高。
本发明的第三方面涉及包含前述碳复合材料的摩擦材料。利用碳复合材料的特性(诸如高摩擦系数、高热稳定性和耐磨性),这样的摩擦材料可用于各类应用。这种材料的特别有效的应用是例如车辆和飞行器的制动盘和/或制动垫材料。
本发明的碳复合材料具有诸如摩擦系数大、热稳定性高、耐磨损和重量轻的特性。
附图说明
图1示出了制备本发明的碳复合材料的工艺的流程图;
图2示出了根据本发明成型的测试样品的次级电子图像;
图3示出了经历成型、碳化、然后立即煅烧的碳化硅的次级电子图像;
图4示出了经历成型、碳化、用酚醛树脂再浸渍、再次碳化以及煅烧的经处理的测试样品中的颗粒形态;
图5示出了包含原位合成的SiC的样品的TEM图像;
图6示出了包含与其混合的SiC的样品的TEM图像;
图7示出了与图5相同的包含原位合成的SiC的样品的TEM图像;
图8示出了图7中的A和B位置处的EDX定性分析结果;
图9示出了图7中的C和D位置处的EDX定性分析结果;
图10示出了与图6相同的包含与其混合的SiC的样品的TEM图像;
图11示出了图10中的A到C位置处的EDX定性分析结果。
具体实施方式
以下参照包含氧化硅(即二氧化硅:SiO2)作为金属源的碳复合材料的实施例对本发明进行描述。
传统技术是以金属(Si)与碳(C)的直接反应为基础。然而在本发明中,通过下列分步反应(1)和(2)反应来生成气相SiO,然后SiO与碳(C)反应以生成SiC。
SiO2+C→SiO↑+CO↑ (1)
SiO+2C→SiC+CO↑ (2)
二氧化硅与碳反应生成碳化硅的反应是固-气反应,用碳完全覆盖二氧化硅颗粒而不留下任何间隙对于生产碳化硅颗粒来说是十分关键的。
合并式(1)所示的反应与式(2)所示的反应,得到式(3)所示的反应:
SiO2+3C→SiC+2CO↑ (3)
因此,使用金属氧化物(SiO2)原位生成了金属碳化物SiC。
有利的是,这样的反应不涉及游离金属,并且不存在游离金属。因此,呈现出高摩擦系数和高热稳定性。通过调节SiO2的量和形态,可以对生成的SiC的量、形态、粒径等进行随意的调节。使用Admatechs有限公司出售的球形SiO2,可以在碳-碳纤维复合材料(CC复合材料)中原位合成球形SiC。
本发明包括使用包含单分散在热固性树脂前体(诸如酚醛树脂)溶液中而不团聚的SiO2颗粒的均相分散体系。因此,通过进行涂层来覆盖由热固性树脂前体生成的SiO2颗粒的表面。这可以防止增强材料(即碳纤维)与SiO2之间的反应。因此,材料的强度不会由于碳纤维受损而降低,并且本发明的复合材料在强度方面优于传统的复合材料。
更具体地,本发明的特点总结如下:
(1)使用包含单分散在热固性树脂前体溶液中的SiO2颗粒的稳定浆液;
(2)使用热固性树脂前体、SiO2和碳纤维作为起始物料;
(3)选择性地在原位进行SiO2与由热固性树脂前体生成的碳的反应,并且防止SiO2与碳纤维的反应;
(4)通过形成扩散反应相使SiC与碳基体相牢固结合;
(5)所生成的SiC颗粒的均匀分散;
(6)不含游离Si颗粒的SiC/碳/碳纤维复合材料。
以下通过电子显微图像来描述本发明的碳复合材料。
图2示出了根据本发明成型的测试样品的次级电子图像。在图2中,颗粒物质是生成的金属碳化物。在使金属氧化物与碳反应以生成金属碳化物的工艺中,重要的是将足够量的碳置于金属氧化物颗粒附近而不引起金属氧化物团聚。根据传统技术,当金属氧化物和碳均为粉末时,有些金属氧化物发生团聚是不可避免的。然而根据本发明,通过在酚醛树脂溶液中加入金属氧化物颗粒和分散剂,实现了金属氧化物在碳中的均匀分散。
二氧化硅颗粒与碳反应生成碳化硅的反应是固-气反应。为了生成碳化硅颗粒,二氧化硅颗粒周围必须用碳完全覆盖而不留下任何间隙。图3示出了碳化硅的次级电子图像,其中碳化硅是通过如下方法制备:将金属氧化物颗粒分散于酚醛树脂溶液中,然后进行成型和碳化,之后立即进行煅烧。经过用酚醛树脂浸渍和碳化的单次操作,生成的碳化硅具有1μm或更小的粒径。
图4示出了经处理的测试样品中的颗粒形态,其中测试样品通过如下方法来制备:将类似于图3的溶液成型、碳化、用酚醛树脂再次浸渍、再次碳化以在二氧化硅颗粒周围提供足够量的碳、然后煅烧。从图4可看出,通过在煅烧之前用酚醛树脂对测试样品进行浸渍和碳化两次,所生成的球形碳化硅颗粒具有2μm至5μm的直径。
本发明所用的金属氧化物可以根据例如与碳材料的反应性或碳复合材料的应用来选择,并无具体限制。金属氧化物的例子包括氧化钛、氧化铬、氧化钨、氧化铌、氧化硅、氧化锆、氧化铪、氧化钽、氧化钼和氧化钒。
可以使用通过氧化金属粉末所得的金属氧化物颗粒和复合金属氧化物颗粒。例如,优选使用硅、铝、锆、多铝红柱石、尖晶石和氧化锌中的任意一种。特别优选使用的是:通过金属硅与氧反应得到的球形二氧化硅颗粒;通过熔解破碎的二氧化硅而得到的球形二氧化硅颗粒;选自破碎的二氧化硅产物的二氧化硅颗粒;通过金属铝与氧反应得到的球形氧化铝颗粒;通过熔解破碎的氧化铝而得到的球形氧化铝颗粒;以及选自破碎的氧化铝产物的氧化铝颗粒。
以下述方式来制备由烧结金属得到的金属氧化物颗粒:在含有载气和氧的气氛中形成化学火焰;将金属粉末混合物(例如,诸如硅、铝、镁、锆或钛的金属粉末、在多铝红柱石组合物中混合的铝和硅粉末、在尖晶石组合物中混合的镁和铝粉末、以及在堇青石组合物中混合的铝、镁和硅粉末)引入所述化学火焰;然后在所述化学火焰中生成所需的金属氧化物或复合金属氧化物(诸如二氧化硅(SiO2)、氧化铝(Al2O3)、二氧化钛(TiO2)或氧化锆(ZrO2))的精细颗粒。这样的金属氧化物颗粒由Admatechs有限公司制造并出售。
实施例
使用1)平均粒径为3μm的二氧化硅颗粒和2)液体酚醛树脂作为起始物料。二氧化硅颗粒连同分散剂一起被引入液体酚醛树脂,以将其浓度调节为至少3:1的C:Si比(摩尔比)。在此实施例中,二氧化硅颗粒在9:1的C:Si摩尔比下被混合。
用上文所述的浆液浸渍碳板,然后通过加热而成型。成型之后,在电子显微镜下观察二氧化硅颗粒的分散状态,得到如图2所示的图像。
在1000℃下在惰性气氛中对成型产物进行碳化。
在真空容器中用酚醛树脂再次浸渍碳板,然后再次碳化。然后,在1650℃下在惰性气氛中对成型产物进行煅烧。在电子显微镜下观察所得的测试样品的颗粒形状。同时对测试样品进行X射线衍射分析并确认其为碳化硅。图4示出了电子显微图像。
原位合成SiC与简单添加SiC的比较
在本发明中,碳复合材料中所含的SiC颗粒是在煅烧期间通过二氧化硅颗粒与碳之间的原位反应来合成的。将原位生成的SiC与碳的界面与通过简单混合SiC而制备的SiC/C/C复合材料进行比较,从而评价原位反应的作用。
TEM图像比较
通过将球形二氧化硅颗粒(平均粒径:3μm)与酚醛树脂混合、固化该混合物以防止起泡然后在1750℃下煅烧该固化产物2小时,得到包含由原位反应生成的SiC的样品。通过将SiC颗粒(平均粒径:2至3μm)与酚醛树脂混合、固化该混合物以防止起泡然后在1750℃下煅烧该固化产物2小时,得到经由简单混合而包含SiC的样品。
用TEM观察这两种样品的SiC/C界面。图5示出了包含原位合成的SiC的样品的TEM图像照片。图6示出了包含混合于其中的SiC的样品的TEM图像照片。在图5所示的照片中,在SiC/C界面处生成了中间层,并且没有观察到间隙,但是在图6所示的照片中观察到了一些间隙。这表明,通过原位反应来生成SiC,SiC与碳之间的粘附得以改善。
EDX定性分析比较
图5所示的包含原位合成的SiC的样品的TEM图像被再次示于图7。图8和图9示出了图7所示的位置A至D的EDX定性分析结果。从结果可以看出,位置A表示生成的SiC,位置D表示碳。如EDX定性分析结果图所示,随着观察位置从位置A向位置D靠近,Si峰强度变小,并且位置B和C是由原位反应得到的中间层。而且,在SiC/C界面处没有间隙,并且SiC颗粒与碳相粘附。
图6所示的包含混合于其中的SiC的样品的TEM图像被再次示于图10。图11示出了图10所示的位置A至C的EDX定性分析结果。从结果可以看出,位置A表示碳,位置B和C均表示混合在样品中的SiC。在SiC/C界面处存在间隙,并且SiC颗粒并未与碳相粘附。
在原位生成的SiC与碳的界面处没有间隙,但是在混合在样品中的SiC与碳的界面处存在间隙。这表明,通过原位反应生成SiC可以实现更好的SiC颗粒与碳之间的粘附。
工业适用性
本发明的碳复合材料具有诸如大摩擦系数、高热稳定性、耐磨损以及重量轻的特性。因此,利用上述特性,这种材料可作为摩擦材料用于各种应用。而且,这种碳复合材料的生产成本低,因而具有实用性。
Claims (17)
1.一种摩擦材料,其包含分散在碳、碳纤维或碳/碳纤维基体中的金属碳化物颗粒且不含游离金属颗粒,其中所述金属碳化物颗粒至少在颗粒表面或整个颗粒为金属碳化物,所述金属碳化物由选自金属颗粒、金属氧化物颗粒或复合金属氧化物颗粒中的至少一种的金属源和热固性树脂的碳源在原位合成。
2.如权利要求1的摩擦材料,其中所述金属氧化物颗粒或复合金属氧化物颗粒是通过氧化金属粉末而得到的SiO2、TiO2、ZrO2、Al2O3、WO3、CrO3或ZnO中的至少一种。
3.如权利要求2的摩擦材料,其中所述金属氧化物颗粒为SiO2颗粒,并且所述金属碳化物颗粒为SiC颗粒。
4.如权利要求2的摩擦材料,其中所述复合金属氧化物颗粒为SiO2/ZrO2复合金属氧化物颗粒,并且所述金属碳化物颗粒为SiC/ZrC复合碳化物颗粒。
5.如权利要求3的摩擦材料,其中所述SiO2颗粒选自通过金属硅与氧之间的反应得到的球形二氧化硅颗粒、通过熔解破碎的二氧化硅而得到的球形二氧化硅颗粒、以及破碎的二氧化硅颗粒。
6.制备包含分散于其中的金属碳化物颗粒的摩擦材料的方法,其中,金属颗粒、金属氧化物颗粒和复合金属氧化物颗粒中的至少一种被分散在热固性树脂中以得到浆液混合物,用所述浆液混合物浸渍碳纤维,并且进行碳化和煅烧来碳化热固性树脂以原位合成金属碳化物,至少颗粒表面或整个颗粒为金属碳化物。
7.如权利要求6的制备摩擦材料的方法,其中所述金属氧化物颗粒或复合金属氧化物颗粒是通过氧化金属粉末而得到的SiO2、TiO2、ZrO2、Al2O3、WO3、CrO3和ZnO中的至少一种。
8.如权利要求7的制备摩擦材料的方法,其中所述金属氧化物颗粒为SiO2颗粒,并且所述金属碳化物颗粒为SiC颗粒。
9.如权利要求7的制备摩擦材料的方法,其中所述复合金属氧化物颗粒为SiO2/ZrO2复合金属氧化物颗粒,并且所述金属碳化物颗粒为SiC/ZrC复合碳化物颗粒。
10.如权利要求8的制备摩擦材料的方法,其中所述SiO2颗粒选自通过金属硅与氧之间的反应得到的球形二氧化硅颗粒、通过熔解破碎的二氧化硅而得到的球形二氧化硅颗粒、以及破碎的二氧化硅颗粒。
11.如权利要求6至10中任何一项的制备摩擦材料的方法,其中所述热固性树脂选自酚醛树脂、环氧树脂、不饱和聚酯树脂、丙烯酸树脂、脲醛树脂、呋喃树脂、邻苯二甲酸二烯丙酯树脂、三聚氰胺树脂、聚氨酯树脂和苯胺树脂中的至少一种。
12.如权利要求6至10中任何一项的制备摩擦材料的方法,其中在所述浸渍步骤之后、所述碳化步骤之前,通过层压浸渍产物来进行热压结合步骤。
13.如权利要求6至10中任何一项的制备摩擦材料的方法,其中,在通过所述煅烧工艺原位制备金属碳化物颗粒之前,进行两次或多次用包含至少一种分散在热固性树脂中的金属氧化物颗粒的浆液混合物来浸渍所述碳纤维材料并进行碳化处理的步骤。
14.如权利要求6至10中任何一项的制备摩擦材料的方法,其中,在通过所述煅烧工艺原位制备金属碳化物颗粒之后,重复一次或多次用包含至少一种分散在热固性树脂中的金属氧化物颗粒的浆液混合物来浸渍所述碳纤维材料并进行碳化处理的步骤。
15.如权利要求6至10中任何一项的制备摩擦材料的方法,其中碳化是在200℃至1600℃温度下在惰性气氛中进行的。
16.如权利要求6至10中任何一项的制备摩擦材料的方法,其中煅烧是在1650℃或更高温度下在惰性气氛中进行的。
17.如权利要求1至5中任何一项的摩擦材料,其中所述摩擦材料为制动盘和/或制动垫材料。
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KR100818577B1 (ko) | 2008-04-02 |
EP2216310A1 (en) | 2010-08-11 |
US20100292069A1 (en) | 2010-11-18 |
JP2005306688A (ja) | 2005-11-04 |
EP1748036B1 (en) | 2017-07-19 |
CN1946655A (zh) | 2007-04-11 |
JP5113982B2 (ja) | 2013-01-09 |
WO2005102961A1 (ja) | 2005-11-03 |
US20070166546A1 (en) | 2007-07-19 |
EP1748036A1 (en) | 2007-01-31 |
US8058197B2 (en) | 2011-11-15 |
KR20070012494A (ko) | 2007-01-25 |
EP1748036A4 (en) | 2008-03-12 |
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