CN1251083A - 纤维增强复合陶瓷及其生产方法 - Google Patents
纤维增强复合陶瓷及其生产方法 Download PDFInfo
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Abstract
本发明提供一种含有耐高温纤维,尤其是基于Si/C/B/N的纤维的纤维增强的复合陶瓷,所述纤维和以Si为基的基体反应结合。所述复合陶瓷的生产过程为:用一种适于热解的粘合剂浸渍由Si/C/B/N纤维组成的纤维束并使粘合剂固化,如果需要,随后用一种适于热解的抗硅化层,例如酚醛树脂或者聚碳硅烷处理所述纤维束,然后,制备一种纤维束,填料如SiC和形式为石墨或炭黑的炭以及粘合剂的混合物,将所述混合物压制成型成坯体,之后,在减压或保护性气氛中,热解坯体,从而获得一种多孔性成型体,然后,优选在减压条件下,用硅熔体对所述成型体进行渗入处理。这样,有可能以一种适于大量生产的有效方式,生产与传统的复合陶瓷相比,性能得到明显改善,而且尤其适合用于高性能制动系统的纤维增强复合陶瓷。
Description
本发明涉及一种含有基于Si/C/B/N的耐高温纤维的纤维增强复合陶瓷,所述纤维和以Si为基的基体反应结合。
DE-A-4438455中对这样一种方法和复合陶瓷进行了公开。
碳纤维增强的碳(C-C,也称作CFRC或在德语中,称为CFC)是迄今得到成功应用的复合陶瓷材料之一。
然而,例如用于赛车上的新近开发的,以具有专门研制的摩擦衬片的CFRC制动盘为基础的高性能制动系统的生产,需要采用大量的浸渍或者碳化和石墨化周期,因此,这种生产方法极其费时,能耗大且费用高,可能需花费几周或数月的时间。而且,用于在通常条件下运行的车辆中的CFRC制动盘,其在潮湿环境和低温条件下的制动性能完全不能令人满意。这尤其表现在作为运行温度和衬片表面的函数的摩擦系数极其不稳定,从而使得控制系统如迄今惯用的4通道ABS系统对车辆的控制极其困难成甚至是不可能的。基于这一背景,目前正在尝试发展例如可以用在汽车或火车中的高性能制动系统的制动盘的改进的纤维增强复合陶瓷材料。此外,这种纤维增强复合陶瓷材料对于众多的其它应用场合,例如作为汽轮机材料或滑动轴承材料也很价值。
尽管自六十年代,含有质量分数为2-15%自由硅的硅渗入反应结合的碳化硅(SiSiC)就已为人所知,并且,在热工程领域的某些场合也得到工业应用,但SiSiC材料的生产仍然非常复杂和昂贵。
上述的DE-A-4-438455公开了一种生产纤维增强的C-SiC复合陶瓷的方法,其中的坯体由浸渍树脂的纤维织物构成。这种方法的一个缺点是由并不真正便宜的这种前体来构造或形成复杂结构的过程非常麻烦,而且会产生大量的废料。因此,这一已知方法不适于用在诸如制动盘的部件的大规模生产中。这种层状结构又会导致以这种方法生产的结构体的各种性能具有强各向异性,这尤其对于制动盘的散热有不利影响。另外,这种制动盘在某些条件下如磨损有发生层离的倾向,因而特别危险。
因此,本发明的一个目的是提供一种含有耐高温纤维的改进的纤维增强复合陶瓷以及生产这种复合材料的方法,从而有可能实现大量生产的部件如制动盘的简便且便宜的生产而且能够使性能得以改善。
根据本发明,采用一种生产含有耐高温纤维,尤其是基于Si/C/B/N的纤维的纤维增强复合陶瓷的方法,上述目的得以实现。其中,所述纤维和以Si为基的基体反应结合。所述方法包括下列步骤:
-用一种适合于发生热解的粘合剂浸渍纤维束,尤其是Si/C/B/N纤维构成的纤维束,并使该粘合剂固化。
-制备一种纤维束、填料和粘合剂的混合物;
-将所述混合物压制成一坯体;
-在减压或保护性气体的条件下,热解所述坯体,以获得多孔的成型体;
-用硅熔体对所述成型体进行渗透处理。
通过一种含有耐高温纤维,尤其是基于Si/C/B/N的纤维的纤维增强复合陶瓷,也可以实现这一目的。所述纤维反应结合到以Si为基的基体上,其中,将随机分布的短纤维束包埋在所述基体中,所述短纤维束包含基本保留单独纤维丝状态的成束单个纤维丝,而且,至少在所述短纤维束表面区域内,短纤维束被一层炭覆层所包围,所述炭已完全或部分地与金属或半金属基体材料进行了反应。
根据本发明,已认识到,将短纤维束用于增强所述复合材料会很大程度上简化纤维的生产,因为这有可能预先混合各种独立组元并将其压制成坯体,而随后只需对所述坯体进行热解和熔体渗入处理即可,从而有可能提供一个相当简化的适于大量生产的生产方法。
也认识到,原则上可以通过纤维增强获得的有利性能如伪塑性,只有在使用由适当的粘合剂固定一起并加以保护防止硅熔体侵害的纤维束来用作纤维增强时,则通过硅熔体渗入在生产中可以获得。根据本发明,通过将纤维束用适于热解的粘合剂浸并使粘合剂随后固化,就可以达到这一目的。这一浸渍步骤确保纤维束中单个的纤维牢固地结合一起并确保纤维束具有足够的机械稳定性,从而在很大程度上防止在后来的为获得坯体所进行的与其它组元的混合过程中,敏感的单个纤维丝发生机械损坏。
在所获得的复合陶瓷中,保护纤维束不受硅熔体侵害的作用通过至少在纤维束的表面区域使纤维束包围一层已经完全或者部分地与基体材料(即硅或硅的化合物)发生反应的碳涂层来展现。
因此总的来说,有可能以一种相对简单且便宜的方式生产一种纤维增强的复合陶瓷,所述陶瓷与传统的复合陶瓷相比,具有明显改善的性能,而且,尤其适合用来作为汽车或铁路车辆高性能制动系统中的制动体或制动盘。
对本发明而言,术语“硅熔体”不仅包括纯硅熔体,而且也包括含有通常的杂质或者可能添加有合金元素的工业硅熔体。
对于纤维增强,优选使用C纤维,或者,如果需要,也优选使用SiC纤维,尽管其它的以Si/C/B/N为基础的耐高温纤维,其中一些正处于开发之中,原则上也可以使用,而且,依据所使用的纤维性能,它们甚至还具有进一步的优点。对于特别便宜的产品,使用铝的氧化物纤维也是可能的。
在本发明的一个优选实施方案中,通过用胶水将单个的纤维丝粘合一起,来获得纤维束。
用胶水所进行的粘合一般由纤维束的制造者在完成单个纤维丝的生产之后,立即采用喷丝头进行的。随后,通常马上将所述纤维束切割成所要求的长度。
在本发明的另一个优选的实施方案中,纤维束在完成粘合剂的浸渍和固化之后,还要用适于热解的抗硅化层进行处理。
采用适于热解的保护层对纤维束进行的这一附加涂覆使纤维束在其外层边界上获得有利的附加保护层,这首先降低了在生产坯体的混合和压制过程中,纤维束受到机械损坏的危险,其次确保甚至在所获得的最终产品中,仍基本保留单根纤维丝状态。当使用C纤维时,液态硅熔体会与之反应,生成SiC,从而产生化学侵害,这种化学侵害很大程度上可为所述的碳保护层或者热解期间可能形成的陶瓷保护层所抑制,这样,至多只会有处于纤维束外层的少量单个的纤维丝仍然与硅反应,形成碳化硅。
在本发明又一个优选的实施方案中,所述纤维束用一种热解期间形成固态碳的富碳聚合物材料进行处理,优选用选自含有酚醛树脂的树脂或树脂混合物浸渍处理。这样就获得了非常有效的抗硅化层。
在本发明的再一个实施方案中,采用一种经过稀释或者溶解的粘合剂进行浸渍处理,优选在一种混合或搅拌装置中进行,以使通过蒸发或干燥形成未聚集一起的纤维棒,而单个的纤维束中的纤维间的粘合仍得以保持。
这一措施的优点是:纤维束可以采用一种简单的方式进行处理,来获得未聚集一起的纤维棒,这样,纤维棒保持自由流动,这有利于后续的混合处理并且具有相当大的工业价值。
在本发明的又一个优选的实施方案中,使用一种热解时形成固态碳的材料,优选沥青或者热塑性材料,进行浸渍处理。
特别是,这种浸渍方式与随后采用树脂或类似物质进行的处理相结合,可进一步改善所述复合陶瓷的耐破坏性。然而,开始例如用树脂浸渍,随后再用沥青处理,原则上也是可能的。
根据本发明的又一个实施方案,使用热解时形成碳化硅并优选选自于有机硅聚合物,特别是聚碳硅烷(polycarbosilane)的材料作为抗硅化层。
这就有可能实现在渗透期间,对所述纤维束进行有效保护,使其不受硅熔体侵害,因为热解期间所形成的SiC阻止所述纤维与硅进一步反应。
根据本发明的又一个实施方式,使用热解时发生陶瓷化的Si-B-C-N基的材料,优选选自于有机硅-硼聚合物,尤其是聚硼硅氮烷(polyborosilazanes),作为抗硅化层,同样能够获得改善的保护作用,从而免于受到硅熔体的化学侵害。
在本发明的又一个实施方案中所使用的纤维束包含1000-14000根的单个纤维,其中每根纤维的平均直径为约5-10μm,长度约1-30mm,并优选约3-16mm。
以这种方式,就有可能使用市售的粗纱(例如,12k的纤维束),这将更易于实现生产的低成本。
在本发明的一个优选的实施方案中,使用体积分数约20-50%,优选约30-40%的纤维束来制备所述混合物。
现已发现,这种体积比能够实现机械和热性能的显著优化。
在本发明的又一个优选的实施方案中,含碳填料,优选炭黑或石墨被添加至所述混合物中,以生产所述坯体。
这种填料有助于坯体在其生产和随后的热解中保持结合为整体状态,使热解过程加速并减小热解期间组元的体积变化。
在本发明的再一个优选的实施方案中,形式为硅或者难熔金属的碳化物、氮化物或硼化物,优选碳化硅、碳化钛或硼化钛的填料以粉末形式混入到生产坯体所需的混合物中或者混入到用于浸渍或处理纤维束的材料中。
这种硬填料的添加改善了所述复合陶瓷的耐磨性。
在添加有可热固化粘合剂的捏和机或混合机中,制备各种单个组元的混合物,随后在模具中将其压制成型并固化,从而形成坯体。
在热解之前或者之后,可先将所述坯体加工成所需形状,然后再用硅熔体进行渗入处理。
以这种方式,则可显著降低机械加工的难度,因为所述坯体耐磨性很低,因而即使热解之后也能轻而易举地加以机械加工。
在本发明的又一个优选实施方案中,通过选择组元材料及其比例来调整所述混合物,以使坯体热解时所形成的成型体的孔隙率为约20-50%。
因为孔隙率很容易受到所选择的添加剂的类型及数量的影响,所以,有可能在熔融的渗入金属与复合材料的其它组元,即纤维束、填料和C前体间确定一个最佳体积比,以便获得最佳的机械和热性能。
在本发明的又一个优选的实施方案中,优选具有有利的热解动力学特性的粘合剂,例如PVA或甲基纤维素代替热塑性或热固性物质添加至所述混合物中,这更容易实现热解和硅化的进行。
因此,一个加速热解步骤的方法可将这一步骤与熔体的渗入结合在一起,从而显著改善经济效益。
对本领域的技术人员不言而喻的是,上述的特点以及下面仍将说明的特点不仅在上述每种情形中所指出的结合方式中存在,而且也包含在其它的结合方式或单独情形中,而未超出本发明的范围。
下面结合附图通过优选的说明性实施方案的描述,可了解本发明的进一步的特性和优点。附图中:
图1示出的是加工顺序(从左至右):一个作为CFRC体的压制成型的坯体,一个坯体加工后的制动盘和一个最终加工而成的C/Si-SiC制动盘;
图2示出的是经热解并用液态硅熔融渗入后,复合材料基体的一抛光后剖面的光学显微照片,其放大倍数为200x;
图3是经熔体渗入处理后的纤维束的横截面,其中,可以看到,由于双层涂覆,纤维束实际上完全得以保留;以及
图4是纤维-基体间界面的扫描电子显微镜照片,从中可以看到,由于纤维的拔出作用,所述复合体已具有伪塑性。
图1是生产制动盘的第一个说明性实施例;在约150℃的高温下压制成型的尺寸稳定的CFRC坯体示于左边,之后进行钻孔和热解处理(中间),热解后再次进行机械加工(右边的图),只有在此之后,才用工业硅熔体进行渗入处理。
熔体渗入之后所获得的显微结构见图2。
实施例1
将长为3mm但束强度未确定的碳纤维束用一种沥青溶液浸渍并随后加以干燥。之后,通过用酚醛树脂溶液浸渍并随后进行干燥来进行处理。采用这种方式涂覆处理的纤维就构成了生产压制成型的组成物的基础,所述组成物通过在捏和机中添加碳粉和酚醛树脂来制备。捏和过程中,连续添加平均颗粒尺寸d50分别为3μm和5.5μm的粉末形式的TiC和B4C混合物。将如此获得的组成物用一个形状与最终形状接近的压制模具进行压制,其中,所述组成物在至少150℃的温度下,以最终形状进行固化,以获得尺寸稳定的CFRC盘。之后,在热解炉内,于保护性气氛中,约800℃的温度下热解处理。
在这一阶段,可以采用传统的方法如车削非常简单且便宜的进行任何获得最终形状所必须的机加工(参见图1)。
在这一机加工之后,在高于Si的熔点(即约1600℃)的温度,减压条件下,用液态硅熔体对材料进行渗入处理。
随后将所获产品冷至室温。
正如由示于图3的抛光截面中所看到的单个碳纤维束那样,由于酚醛树脂和沥青的双层涂覆,实际上,碳纤维束在整个生产过程中得以完全保留,而且,其表面受到充分保护,从而免于受到硅熔体的反应性侵害。
从图4中所示的纤维-基体间界面的扫描电子照片,可看到,由于纤维的拔出作用,所生产的复合体已具有伪塑性。
Claims (19)
1.生产含有耐高温纤维,特别是基于Si/C/B/N的纤维的纤维增强复合陶瓷的方法,其中所述纤维与以Si为基的基体反应结合,所述方法包括下列步骤:
-用一种适于热解的粘合剂浸渍纤维束,尤其是Si/C/B/N纤维构成的纤维束并使该粘合剂固化;
-制备纤维束、填料和粘合剂的混合物;
-压制成型所获得的混合物,以制备坯体;
-在减压条件下或保护性气氛中热解所述坯体,以制备多孔成型体;
-用硅熔体对该成型体进行渗入处理。
2.根据权利要求1的方法,其中所使用的纤维是C纤维或SiC纤维。
3.根据权利要求1或2的方法,其中,通过用胶水将单个的纤维丝束集一起,来获得所述的纤维束。
4.根据权利要求1、2或3的方法,其中,在浸渍之后,通过采用一种适于热解的抗硅化层涂覆纤维束,来对其进行附加的处理。
5.根据前述权利要求中任一项的方法,其中,一种热解时形成固态碳的材料,优选为沥青,用来进行所述浸渍。
6.根据前述权利要求中任一项的方法,其中,采用热解时形成碳的富碳聚合物材料作为抗硅化层对纤维束进行处理,优选采用选自于酚醛树脂的一种树脂或树脂混合物进行处理。
7.根据前述权利要求中任一项的方法,其中,所使用的抗硅化层是一种热解时形成碳化硅的材料,该材料优选选自于有机硅聚合物,尤其是聚碳硅烷。
8.根据权利要求1-6中任一项的方法,其中,所使用的抗硅化层是一种基于Si-B-C-N的、热解时发生陶瓷化的材料,该材料优选选自于有机硅-硼的聚合物,尤其是聚硼硅氮烷。
9.根据前述权利要求中任一项的方法,其中,使用一种稀释的或者溶解的粘合剂进行浸渍处理,并优选在混合或搅拌装置中进行,这样,蒸发或干燥后形成未聚集一起的纤维棒,而单个纤维束中纤维间的粘合仍得以保持。
10.根据前述权利要求中任一项的方法,其中,所使用的纤维束包含约1000-14000根、平均直径约5-10μm的单个纤维。
11.根据前述权利要求中任一项的方法,其中,所使用的纤维束的长度约1-30mm,优选约3-16mm。
12.根据前述权利要求中任一项的方法,其中用体积分数约为20-50%,优选约30-40%的纤维束来制备所述混合物。
13.根据前述权利要求中任一项的方法,其中含碳的填料,优选碳黑或石墨,被添加到所述混合物中,以制备坯体。
14.根据前述权利要求中任一项的方法,其中形式为硅或难熔金属的碳化物、氮化物或硼化物,优选碳化硅、碳化钛或硼化钛的填料,以粉末形式混合至所述混合物中,以生产所述坯体,或者混合至进行纤维束的浸渍或处理所使用的材料中。
15.根据前述权利要求中任一项的方法,其中在捏和机或混合机中,添加可热固化的粘合剂制备所述混合物,随后在一模具中将其压制成型并固化形成坯体。
16.根据前述权利要求中任一项的方法,其中在热解所述坯体之前或之后,将其加工成所要求的形状,之后,用硅熔体进行渗入处理。
17.根据前述权利要求中任一项的方法,其中通过选择组元材料及其比例来调整所述混合物,以使坯体热解时所形成的成型体中的孔隙率为约20-50%。
18.根据前述权利要求中任一项的方法,其中将具有有利的热解动力学特性的粘合剂,优选PVA或者甲基纤维素,添加至所述混合物中,以共同促进热解和硅化过程的进行。
19.含有耐高温纤维,尤其是基于Si/C/B/N的纤维的纤维增强复合陶瓷,所述纤维和以Si为基的基体反应结合,其中,包含成束的单个纤维丝且该纤维丝基本保持单根纤维丝状态的短纤维束以随机分布方式包埋在所述基体中,而且,至少在该短纤维束的表面区域,其围绕有一层已完全或者部分地与所述基体材料反应的碳覆层。
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JPH02205640A (ja) * | 1989-02-06 | 1990-08-15 | Mitsubishi Kasei Corp | 繊維強化金属複合材用の予備成形体 |
DE3933039A1 (de) * | 1989-10-04 | 1991-04-18 | Sintec Keramik Gmbh | Verfahren zur herstellung von oxidationsgeschuetzten cfc-formkoerpern |
JPH03177384A (ja) * | 1989-12-06 | 1991-08-01 | Toshiro Yamashina | 耐酸化性材料及びその製造法 |
JPH04358031A (ja) * | 1991-06-04 | 1992-12-11 | Hitachi Chem Co Ltd | セラミック繊維織布強化複合材料及びその製造法 |
DE4136880C2 (de) * | 1991-11-09 | 1994-02-17 | Sintec Keramik Gmbh | Verfahren zur Herstellung eines oxidationsbeständigen Bauteils auf CFC-Basis und dessen Anwendung |
DE9422458U1 (de) * | 1994-10-26 | 2003-08-28 | Deutsches Zentrum für Luft- und Raumfahrt e.V., 51147 Köln | Reibeinheit |
DE4438456C2 (de) * | 1994-10-28 | 2002-07-11 | Deutsch Zentr Luft & Raumfahrt | Reibeinheit |
US5955391A (en) * | 1996-03-29 | 1999-09-21 | Kabushiki Kaisha Toshiba | Ceramic matrix composite and method of manufacturing the same |
US6024898A (en) * | 1996-12-30 | 2000-02-15 | General Electric Company | Article and method for making complex shaped preform and silicon carbide composite by melt infiltration |
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1997
- 1997-03-21 DE DE19711829A patent/DE19711829C1/de not_active Expired - Lifetime
-
1998
- 1998-02-24 CN CNB988035758A patent/CN1155539C/zh not_active Expired - Fee Related
- 1998-02-24 ES ES98912381T patent/ES2162431T3/es not_active Expired - Lifetime
- 1998-02-24 WO PCT/EP1998/001044 patent/WO1998042635A1/de active IP Right Grant
- 1998-02-24 CZ CZ0333599A patent/CZ299421B6/cs not_active IP Right Cessation
- 1998-02-24 CA CA002284617A patent/CA2284617C/en not_active Expired - Lifetime
- 1998-02-24 KR KR1019997008146A patent/KR100346256B1/ko not_active IP Right Cessation
- 1998-02-24 JP JP54206698A patent/JP3502395B2/ja not_active Expired - Lifetime
- 1998-02-24 EP EP98912381A patent/EP0968150B1/de not_active Expired - Lifetime
- 1998-02-24 DE DE59801312T patent/DE59801312D1/de not_active Expired - Lifetime
- 1998-02-24 PL PL335684A patent/PL191605B1/pl unknown
- 1998-02-24 US US09/381,465 patent/US6261981B1/en not_active Expired - Lifetime
- 1998-02-24 RU RU99122165/03A patent/RU2184715C2/ru active
- 1998-02-24 BR BR9808032-6A patent/BR9808032A/pt not_active Application Discontinuation
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CN1955144B (zh) * | 2005-10-25 | 2011-10-19 | 通用电气公司 | 生产一种陶瓷基体复合材料制品的方法和由此形成的制品 |
CN102239129A (zh) * | 2008-12-04 | 2011-11-09 | 斯奈克玛动力部件公司 | 用于使由cmc材料制备的部件的表面平滑的方法 |
CN101885618B (zh) * | 2010-08-19 | 2013-03-06 | 哈尔滨工业大学 | 反应烧结碳化硅陶瓷件的连接方法 |
CN101885618A (zh) * | 2010-08-19 | 2010-11-17 | 哈尔滨工业大学 | 反应烧结碳化硅陶瓷件的连接方法 |
CN103770195A (zh) * | 2012-10-17 | 2014-05-07 | 上海久牵实业有限公司 | 纤维陶瓷粉末压制成型工艺 |
CN105531493A (zh) * | 2013-04-26 | 2016-04-27 | 派特欧赛拉米克斯股份公司 | 以纤维增强材料制造制动盘的方法和该方法制造的制动盘 |
CN105531493B (zh) * | 2013-04-26 | 2018-11-02 | 派特欧赛拉米克斯股份公司 | 以纤维增强材料制造制动盘的方法和该方法制造的制动盘 |
US10591007B2 (en) | 2013-04-26 | 2020-03-17 | Petroceramics S.P.A. | Method for making brake discs in fiber reinforced material and brake disc made with such method |
CN106396713A (zh) * | 2015-07-30 | 2017-02-15 | 通用电气公司 | 改进cmc材料中的纤维间隔的均匀性 |
CN106830967B (zh) * | 2016-12-30 | 2020-08-14 | 烟台凯泊复合材料科技有限公司 | 一种耐热高强度炭/陶材料的紧固件及其制备方法 |
CN106830967A (zh) * | 2016-12-30 | 2017-06-13 | 烟台凯泊复合材料科技有限公司 | 一种耐热高强度炭/陶材料的紧固件及其制备方法 |
CN110998127B (zh) * | 2017-08-03 | 2021-07-09 | 福乐尼·乐姆宝公开有限公司 | 用于制作制动系统部件的预成型件 |
CN108315837A (zh) * | 2018-03-19 | 2018-07-24 | 武汉科技大学 | 一种硼掺杂碳化硅纤维及其制备方法 |
CN108315837B (zh) * | 2018-03-19 | 2020-07-10 | 武汉科技大学 | 一种硼掺杂碳化硅纤维及其制备方法 |
CN110407597B (zh) * | 2018-04-28 | 2021-05-25 | 中国科学院上海硅酸盐研究所 | 一种稀土氧化物改性碳化硅陶瓷基复合材料及其制备方法 |
CN110407597A (zh) * | 2018-04-28 | 2019-11-05 | 中国科学院上海硅酸盐研究所 | 一种稀土氧化物改性碳化硅陶瓷基复合材料及其制备方法 |
CN114938637A (zh) * | 2019-08-20 | 2022-08-23 | Bkrz有限公司 | 再循环隔绝棉的方法,加工隔绝棉、纤维增强泡沫、耐火木质材料的设备以及生产耐火木质材料的方法 |
Also Published As
Publication number | Publication date |
---|---|
EP0968150B1 (de) | 2001-08-29 |
JP3502395B2 (ja) | 2004-03-02 |
CZ333599A3 (cs) | 2000-08-16 |
PL191605B1 (pl) | 2006-06-30 |
US6261981B1 (en) | 2001-07-17 |
CN1155539C (zh) | 2004-06-30 |
CA2284617C (en) | 2002-11-05 |
EP0968150A1 (de) | 2000-01-05 |
WO1998042635A1 (de) | 1998-10-01 |
KR20000076058A (ko) | 2000-12-26 |
PL335684A1 (en) | 2000-05-08 |
JP2000512257A (ja) | 2000-09-19 |
BR9808032A (pt) | 2000-03-08 |
DE19711829C1 (de) | 1998-09-03 |
ES2162431T3 (es) | 2001-12-16 |
RU2184715C2 (ru) | 2002-07-10 |
KR100346256B1 (ko) | 2002-07-26 |
CZ299421B6 (cs) | 2008-07-23 |
CA2284617A1 (en) | 1998-10-01 |
DE59801312D1 (de) | 2001-10-04 |
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