CN1130956C - 具有电极保护的场致发光元件 - Google Patents
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Abstract
一种具有阳极(4)和阴极(10),并在阳极(4)和阴极(10)之间安排光发射层(8)的场致发光元件的生产方法,还包含阳极保护层(6),它保护阳极(10)不受初始聚合物转换为半导体共轭聚合物的影响,其中该转换构成了光发射层(8)。已经发现这样增加了装置的亮度和半衰期。
Description
本发明涉及一种有机场致发光(EL)装置。
有机场致发光元件由一种材料制成,当在设置在这种材料两侧之一上的电极间施加适当的电压时,这种材料会发光。一类这样的材料是共轭聚合物,这在我们早些的第5,247,190号美国专利中有描述,其内容在这里通过引用而加以结合。例如,聚(p-亚苯基-亚乙烯基)[PPV],当通过在两个合适的电极之间施加电压使正的和负的载流子通过材料时,将发光。这些装置的场致发光效率一方面依赖于电子和空穴的平衡,所述电子和空穴被注入到装置中,并相遇而形成电子/空穴对,另一方面也依赖于这些电子/空穴对结合起来发生光的效率,即,光致发光(例如见N.C.Greenham和R.H.Friend,固体物理,49,1,1995)。因此,对一个有效率的装置来说,具有足够高的光致发光效率是非常重要的。
有好几种处理共轭聚合物的方法。一种方法使用初始聚合物,它是可溶的,因而可易于通过标准溶解基的处理技术进行涂敷(例如,旋涂和刮涂)。然后初始聚合物应当地通过适当的热处理转换,以给出共轭的和不能溶解的聚合物。另一种方法使用直接可溶解的共轭聚合物,这不需要后面的转换阶段。根据特定的应用,一种或另一种方法是是合适的。初始聚合物在后面的处理可导致聚合物薄膜的破坏(如果它直接可溶)的情况下尤其重要,这种处理有,例如:涂敷下一层的聚合物薄膜(例如不同颜色的传送层或发射层),或顶部电极的印刷。转换的初始薄膜还具有更好的热稳定性,这在装置的制造、库存以及高温下操作都是非常重要的。
当初始聚合物由溶解组的消除或改变而转换为其最终形式时,这些转换过程的副产品从薄膜上除去是重要的。在这个处理中它们不和基片相互影响也是重要的,例如如果这引起有害的杂质从基片进入薄膜中,因此影响场致发光元件的性能(包含发光效率和使用寿命)。我们已经发现,例如,当初始PPV聚合物在诸如氧化铟锡之类的导电氧化物基片上转换时,场致发光的淬熄。我们相信,这可能是由铟化合物由于转换副产品中的一种(例如卤化氢)和氧化铟锡的反应而释放到PPV中引起。
除了发现由于来自副产品和氧化铟锡在转换中反应引起杂质的出现而淬熄外,我们还发现由某种PPV共聚合物的增强转换引起的有害的效果。这些共聚合物和均聚合物相比,常常具有有限的共轭长度。这一般将导致游子约束,于是有高光致发光效率和场致发光效率。在这种情况下,我们相信,某些PPV共聚合物薄膜中的铟化合物,当在氧化铟场上转换时,会催化一些组的消失,这些组是我们为了完成转换过程而设计的。
本发明提供了一种克服了这种问题的场致发光元件的结构和生产的方法。
根据本发明的一个方面,提供了一种生产场致发光元件的方法,这种方法包含以下步骤:
形成正载流子注入材料的阳极;
在所述阳极上形成阳极保护层,其中所述阳极保护层由从聚吡咯和其衍生物、聚噻吩及其衍生物、聚乙烯咔唑(PVK)、聚苯乙烯、聚(乙烯吡啶)、介质材料、碳、无定形硅、不含铟导电氧化物,包含氧化锡、氧化锌、氧化矾、氧化钼和氧化镍、以及升华有机半导体的组合中选出的材料制成;
通过将初始物转换为半导体共轭聚合物的聚合物而形成光发射层;及
形成负载流子注入材料的阴极。
已经发现当光发射层从初始聚合物转换到共轭聚合物过程中,释放酸性副产品(例如卤化氢)时,阳极保护层特别有价值。
本发明的另一个方面提供了一种场致发光元件,它包含:
由正载流子注入材料制成的阳极;
在所述阳极上形成阳极保护层,其中所述阳极保护层由从聚吡咯和其衍生物、聚噻吩及其衍生物、聚乙烯咔唑(PVK)、聚苯乙烯、聚(乙烯吡啶)、介质材料、碳、元定形硅、不含铟导电氧化物,包含氧化锡、氧化锌、氧化矾、氧化钼和氧化镍、以及升华有机半导体的组合中选出的材料制成;
由半导体共轭聚合物制成的光发射层;及
由负载流子注入材料制成的阴极。
本发明在阳极由氧化铟锡(ITO)制成时特别有用。但是,其他的材料也是适当的,诸如氧化锡。
在一个实施例中,沉积在玻璃或塑料上的透明导电材料层形成装置的阳极。适当的阳极的例子包含氧化锡和氧化铟锡。典型的层的厚度为500-2000A,而片电阻是10-100Ohm/square,最好<30Ohm/square。转换的初始聚合物可以是例如聚(p-亚苯基-亚乙烯基)[PPV]或均合物或PPV衍生的共聚物。该层的厚度可以在100-3000A的范围中,最好是500-2000A,更好的是1000-2000A。转换前初始层的厚度对旋转涂敷层来说可在100-6000A范围中,对刮涂最多200μm。阳极保护层选为用作对付初始聚合物转换副产品的障碍,但还应不成为空穴从阳极注入发射层的障碍,在那里它们和从阴极注入的电子结合,发射光。导电聚合物是结合处理方便、能保护下面的电极和适合空穴传送以及注入性质,而成为好的候选的一大类材料。可以使用10-2000A之间,最好是10-500A的薄层,因此薄层的透明度可以较高。这些薄层典型的片电阻为100-1000Ohm/square,但也可以高达1010Ω/squ。例子包含被掺杂的共轭聚合物,包含聚噻吩、聚苯胺、聚吡咯和它们的衍生物。阴极电极设置在转换的初始材料的另一侧上,以完成该装置的结构。另外,当在当地发生掺杂时,通过在装置制造过程中和转换副产品反应,还可以使用如上列出的不掺杂的共轭聚合物。
本发明还提供了在有机光发射装置的制造方法中,电极保护层的使用,以保护有机光发射装置不受初始聚合物转换为光发射半导体共轭聚合物的影响,其中有机光发射装置包含第一和第二电极,其中光发射聚合物位于它们中间。
因此,在另一个实施例中,在阴极上沉积电极保护层和初始聚合物,典型地是诸如铝或具有较低的逸出功元素的铝合金,或任何低逸出功元素,或合金之类的材料。在这种情况下,保护层需要传输电子,但可以,以可不必为透明的。导电聚合物再次是阴极保护层合适的候选者。阳极设置在转换的初始材料的另一侧,以完成装置的结构。
在另一个实施例中,提供如上所述的阳极或阴极的保护层,但是保护层是不掺杂的共轭聚合物,对空穴或电子具有充分的注入特性和传输移动性,这依赖于它是否分别保护阳极或阴极。这种保护层的一个例子是可溶PPV衍生材料或可选的初始PPV或PPV衍生材料。在后一种情况下,如果保护层比场效应发光层薄得多,则转换处理的副产品更容易被移去,并且因此减小了在转换过程中和电极的任何反应。
在另一个实施例中,提供如上所述的阳极和阴极的保护层,但是保护层是蒸发或溅射或反应溅射薄膜,它对空穴或电子具有充分注入特性和传输移动性。这依赖于它是否分别保护阳极或阴极。这种保护层的例子可以是溅射或蒸发的碳薄层、无定形硅或不含铟导电氧化物(包含氧化锡、氧化锌、氧化矾、氧化钼和氧化镍)的溅射层或者升华有机半导体层。
在另一个实施例中,设置用于上述阴极和阳极的保护层,但是保护层是不掺杂和不共轭的聚合物,但具有充分注入特性以及对空穴或电子的透明移动性(依赖于它是否分别保护阳极和阴极)。一个例子可以是聚乙烯咔唑,这是良好的空穴传输材料,但不是共轭聚合物。或者非常薄的聚合物材料薄层,它具有相对较差的空穴和电子移动性,这可以用作良好的电极保护层,而不损害电子和空穴载流子的平衡。例子可以是聚苯乙烯和聚(乙烯吡啶)。
在本发明的另一个实施例中,设置用于保护上述阴极和阳极的保护层,但是保护层是非常薄的无机介质,它提供了对初始的转换的副产品的障碍,但是它足够薄,从而空穴可以由隧道通过它(当它接触并保护阳极时),以及电极可以由隧道通过它(当它接触并保护阴极时)。
本发明还提供了场致发光元件的生产方法,包含步骤:
形成由负载流子注入材料制成的阳极;
在所述阳极上形成牺阳极保护层;
在牺牲层上将初始物沉积到半导体共轭聚合物上;
将初始物转换为半导体共轭聚合物,以形成光发射层,在所述转换步骤过程中所述阳极保护层保护所述阳极不受转换的影响,并且自消耗;及
形成由负载流子注入材料制成的阴极。
因此,在另一个实施例中,提供用于如上所述的阳极或阴极保护层,但是保护层是牺牲层。在转换处理过程中,牺牲层由转换副产品腐蚀掉,相互作用的后续产物选择得使它们不影响转换的初始共轭聚合物的光致发光或场致发光效率。这种保护层的例子可以包含非化学计量氧化物薄膜,诸如氧化硅和氧化铝,层厚由在转换处理中的相互作用程度确定。
本发明还提供了一种有机光发射装置,包含:
电极;
由转换的有机初始聚合物制成的有机光发射层;及
形成在所述电极和所述光发射层之间的电极保护层,从而在有机初始聚合物转换过程中保护电极。
本发明还提供了一种有机光发射装置的生产方法,其特征在于包含步骤:
沉积电极;
在所述电极上沉积电极保护层;
为发射材料沉积有机初始聚合物层;及
将有机初始聚合物转换为光发射材料;
其中,电极保护层在有机初始聚合物的转换过程中保护电极。
图1A到1C是结合了阳极保护层的场致发光元件的示意图;
图2描述了初始聚合物到PPV的两种转换途径;
图3A和3B是描述UV-PPV均合物光谱的图表,分别是在石英、氧化铟锡和阳极保护层上转换的。
图4是描述UV-PPV共聚物的图表,它们在分别在石英、氧化铟锡和阳极保护层上转换;及
图5是描述醋酸盐基共聚物的IR光谱的示图,它在硅、具有铟层的硅、具有铟层和保护层的硅上转换。
为了更好地理解本发明,并显示怎样实现相同的情况,现在将通过例子对上述附图进行解释。
较佳实施例的描述
图1A描述了场致发光元件的结构。由透明玻璃或塑料材料制成的基片2用构成装置的阳极4的材料覆盖。阳极保护层6位于阳极4和光发射层8之间。阴极条10设置得和装置的阳极光发射区域一致。装置发射光的工作(没有阳极保护层)在我们前面参照的第5,247,190号美国专利中讨论,这里除了受到本发明的影响的范围,不在进一步描述。
实施例I
现在描述第一实施例。用DC或RF溅射技术将构成阳极4的氧化铟锡沉积到抛光的玻璃基片2上。这种基片可以买到。可以使用纳钙玻璃,它具有薄的硅阻挡层和氧化铟锡层(电阻率为30Ohm/square,透明度为大约85%,厚度1500)。将聚噻吩基的导电聚合物系统用作阳极保护层6。聚乙烯二氧噻吩/聚苯乙烯磺酸盐(PEDT/PSS@1∶1.2摩尔浓度),它可以从Bayer AG,Leverkusen,Germany作为试验品AI4071买到。导电聚合物的100薄膜旋涂在基片上。EL层8由旋涂初始聚合物(诸如均聚体PPV)形成。由这种初始聚合物,溶解组(它在150℃下在氮中转换4小时的过程中被去掉)为四氢噻吩,而到噻吩盐的逆流离子是溴化物。另一个副产品于是为溴化氢,它易于攻击ITO,并可以引起有害产品释放到薄膜中,使场致发光淬灭。PPV基初始物的转换副产品在图2中指出,其中a=0,a’=0。
没有阳极保护层,在热转换处理之后,PPV材料的PL效率的初始测量从大约13%降低到最好是大约0.7%。进一步的测量确定PL效率可以在10%下到大约2-3%的范围内。有阳极保护层的初始量测指出PL效率为大约3%。以后的工作显示这可以增加到大约5%。在转换之后,一种适合的阴极材料(比如钙)沉积在共轭聚合体8上,并进行印刷以形成带10。此后,在手套式操作箱中马上进行接线,并用环氧基树脂/玻璃进行封装。典型地,和没有保护层6的装置相比,有保护层制成的装置具有显著改善的场致发光效应。
实施例II
现在描述另一个具体实施例。前面的步骤和实施例I相同,直到EL层的形成。在这个实施例中,沉积醋酸盐基PPV共聚物的初始为。这种材料具有非常高的场致发光(PL)效率,其中溶解组(它在转换中被去掉)是四氢噻吩,到噻吩盐的逆流离子是溴化物。另一个副产品是溴化氢,它易于攻击ITO,并可以使有害的产品释放到薄膜中,这使场致发光淬灭,并引起更强的转换。没有阳极保护层6,则在热转换处理(如上所述,在150℃下,在氮中处理4小时)后,PPV材料的PL效率令人注目地从大约50-60%降低到最好大约7%。但是,有保护层,在转换后得到为大约22%的PL效率。图2示出转换体系,其中a≠0,a’≠0。在转换后,一种适当的阴极材料(比如钙)沉积在共轭聚合物上。
表1的最后一栏描述了实施例I和II的场致发光效率。表1的第一和第二栏描述在初始层被分别旋涂在石英和铟锡氧化物上,不使用阳极保护层情况下场致发光效率的值。表1A为我们认为从更好的统计基础和更精确的测量而得的相当数字。
在这种情况下指的共聚物最初测量为含大约20mol%的醋酸盐功能。后来的测量(被认为更加精确)指出醋酸盐含量为大约40摩尔%。共聚物醋酸盐值的改变导致当由PEDT/PSS保护层在ITO上转换时,场致发光效率为大约30%。
图3到5示出PPV共聚物的保护也使有ITO保护层的增强的转换最小化。图3A描述了取自具有不同层厚的结构的测量。图3B示出使用共同层厚的情况。图3B表示了论使用的基层如何,均匀聚合物中的UV对光谱变化都很小。但是,图4示出当在ITO上转换醋酸盐基共聚物时有增强的红移。另外,在IR光谱中在1737cm-1处有一吸收波峰,它属于醋酸盐羰基的吸收。其相对的强度可和光谱中的其他峰值比较,诸如在1517cm-1处的吸收,它起源于聚合物的芳香族成份。由此得到的两个峰值的强度比给出醋酸盐功能的相对量的测量。表2示出了当在具有铟层的硅上进行转换时,该比例(醋酸盐∶芳香族)被显著减小。我们将这些结果解释为醋酸盐基共聚物通过来自有铟层的硅基片的铟化合物所增强的转换,这一过程由保护层的出现而减小。相对场致发光效率在表1A和B中详细描述。包含保护层的系统的装置性能可以概括为100cd/m2起始亮度,效率为0.2-0.6lm/W到2lm/W,亮度的半衰期(在恒流或恒压驱动)为10-100小时,至2000小时。
实施例III
现在描述另一个具体实施例。在这个实施例中,生产步骤和实施例2系统,除了聚乙烯二氧噻吩/聚苯乙烯磺酸盐(用作阳极保护层)被优化,以通过最佳PSS含量,给出有益的寿命性能。因此,现在材料具有1∶5摩尔比PRDT/PSS。这些系统的装置的性能可以概括为100cd/m2起始亮度;效率为0.3-1.2lm/W,直到2lm/W,半衰期为大约500小时,到2000小时。
实施例IV
在实施例III的情况下,我们已经发现在PEDT/PSS保护层(@1∶5摩尔比)与PPV初始溶体之间有有害的相互作用。我们相信,这是因为在PPV初始溶体中PEDT/PSS层的溶解作用,并且这可导致最后装置中的不均匀发射。例如,如果在装置的过程中将PPV旋涂在PEDT/PSS薄膜上,则在转换后,在PEDT/PSS-PPV处发现环状的不均匀。我们已经通过在施加PPV初始溶体之前,在PEDT/PSS层上旋涂薄的poly(vinyl pyridine)(PVP)薄膜(图1B-参数7)克服这个问题。如已经知道的,可买到的PVP包含聚苯乙烯成分(典型地为10%)以致使其可溶。因此,如上所述沉积100薄膜,接着自0.1%w/v的甲醇溶体中旋涂薄的PVP薄膜。剩下的装置以常规的方法制造,并得到上面指出的特点(即,100cd/m2初始亮度、0.3-1.2lm/W效率,半衰期为大约500小时)。但是,发射均匀性大大改善。由于PVP作为PEDT/PSS系统和PPV之间的障碍,该方法也可以用于印刷这个ITO保护层。
实施例V
现在描述另一个具体实施例,并联系列这种装置的制造。取ITO敷层玻璃的板,并进行清洁。ITO敷层玻璃的尺寸可以从12*12mm到比80*80mm还大许多。PEDT/PSS ITO保护层然后旋涂在基片上,厚度为大约100。在这个PPV初始溶体刮涂到PEDT/PSS湿薄膜层上,该层厚度为100μm,初始溶体浓度为0.4-0.5%固体含量。在这种情况下,装置的均匀性优于PPV初始层由施涂得到的装置。或者,可以如此刮涂双层PPV装置,从而每一层都是大约500-700厚,并且在第二层沉积之前进行短时间转换(在150℃下大约20秒)(参看图1C的1)。在转换了最后的转换后,所得到的PPV薄膜为大约1000-1400厚。在这种情况下,对于装置效率和总体的均匀性,发现有益的效果。然后沉积适当的阴极,装置被连接起来。
实施例VI
在另一个实施例中,玻璃基片以上述的方式敷有氧化铟锡。然后,PVP溶化在甲醇中,浓度为0.1%,预过滤为1微米孔隙尺寸,并涂敷在氧化铟锡中,厚度大约100。然后,参照实施例I,上述的PPV初始层旋涂在上面,并在150℃下在氮中转换4小时,以使PPV层厚度为大约1000。然后,在由铝/锂合金制成的阴极溅射在上面之前,装置被储存在干燥器中48小时。
实施例VII
以和实施例VI相同的方式形成此实施例,除了阳极保护层由聚乙烯咔唑(PVK)(在THF中溶化)形成,浓度为0.1%。
实施例VIII
这一实施例以和实施例VI相同的方式形成,除了阳极保护层由在THF中溶解的聚苯乙烯制成,浓度为0.1%。
实施例IX
这个实施例以和实施例VI,VII和VIII相同的方式形成,除了阳极保护层由在甲醇溶解的poly(乙烯基吡啶)制成,浓度为0.1%。
实施例X
在另一个实施例中,装置根据实施例II制造,但是阴极由锂/铝合金代替钙制成。例如,锂/铝合金(最多含有10%重量百分比的锂)溅射在共轭聚合物的上面,厚度为10-1μm,最好是大约1200。Li/Al合金靶是可买到的,并且典型地可包含大约2.5%重量百分比的Li。也可以有诸如Zr、Mg、Cu之类的其他稳定元素。和没有保护层,并使用钙电极的装置相比,有保护层和锂基阴极的装置大大改善了场致发光效率。
因此,本发明的上述各种实施例都提供了一种多层场致发光元件,它结合了转换的初始聚合物,作为发射层,以及放置在转换的初始聚合物和下面的电极之间的电极保护层,它用作在初始转换处理中保护电极。至少还有一层,其中之一是第二电极。
上述的实施例是一种场致发光元件制造方法的说明,其中共轭聚合物材料的初始层被沉积在基片上,其上具有预先沉积的电极层和之后沉积的电极保护层。然后在之后的层或至少其中一层是第二电极的层沉积之前,初始层转换为最后共轭聚合物形式。
表1
典型的场致发光效率(%)测量
聚合体类型 | PL eff/Quartz | PL eff/ITO | PL eff/保护层/ITO |
均聚体 | 13.2 | 0.7 | 3 |
共聚体 | 56 | 6.8 | 22 |
表1A
改进的场致发光(%)测量
聚合体类型 | PL eff/Quartz | PL eff/ITO | PL eff/保护层/ITO |
均聚体 | 10 | 2-3 | 4-5 |
共聚体 | 50-60 | 7 | 20 |
表2
来自IR光谱的1737/1517cm-1比(醋酸基∶羰基)
基片 | 1737、1517cm-1比 |
惰性(Si) | 1.1 |
具有铟层保护的Si | 1 |
具有铟层的Si | 0.3 |
Claims (9)
1.一种有机场致发光元件,其特征在于包含:
由正载流子注入材料制成的阳极(4)
在所述阳极上的层(6),所述层由从无机介质材料、碳、无定形硅、不含铟导电氧化物,包含氧化锡、氧化锌、氧化矾、氧化钼和氧化镍的组合中选出的材料制成:
光发射层(8);及
由负载流子注入材料制成的阴极(10)。
2.如权利要求1所述的装置,其特征在于阳极上的层的厚度在10到500之间。
3.如权利要求1所述的装置,其特征在于所述阳极和所述光发射层的厚度都在500到2000之间。
4.如权利要求1所述的装置,其特征在于所述阳极由ITO制成。
5.如权利要求1所述的装置,其特征在于所述阴极由铝或铝合金制成。
6.一种场致发光元件,其特征在于,它包含:
由正载流子注入材料制成的阳极(4);
在阳极上的聚乙烯二氧噻吩(PEDT)/聚苯乙烯磺酸盐(PSS)层(6),PSS对PEDT的摩尔比大于1.2∶1;
由半导体共轭聚合物制成的光发射层(8);及
由负载流子注入材料制成的阴极(10)。
7.如权利要求6所述的元件,其特征在于,PSS对PEDT的摩尔比为5∶1或更大。
8.如权利要求6所述的元件,其特征在于,在所述PEDT:PSS层和所述光发射层之间沉积有另一层。
9.如权利要求8所述的元件,其特征在于,所述另一层包含聚(乙烯吡啶)PVP。
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GBGB9624707.7A GB9624707D0 (en) | 1996-07-29 | 1996-11-28 | High efficiency EL devices |
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EP (1) | EP0947123B1 (zh) |
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-
1997
- 1997-07-29 DE DE69710781T patent/DE69710781T2/de not_active Expired - Lifetime
- 1997-07-29 CN CN97196867A patent/CN1130956C/zh not_active Expired - Lifetime
- 1997-07-29 JP JP50861698A patent/JP3724589B2/ja not_active Expired - Lifetime
- 1997-07-29 EP EP97933784A patent/EP0947123B1/en not_active Expired - Lifetime
- 1997-07-29 US US09/230,401 patent/US6605823B1/en not_active Expired - Lifetime
- 1997-07-29 WO PCT/GB1997/002039 patent/WO1998005187A1/en active IP Right Grant
- 1997-07-29 GB GB9901733A patent/GB2331400B/en not_active Expired - Fee Related
-
2003
- 2003-07-10 US US10/615,924 patent/US7151341B2/en not_active Expired - Fee Related
-
2006
- 2006-04-14 US US11/404,677 patent/US20060186794A1/en not_active Abandoned
-
2008
- 2008-08-28 US US12/200,442 patent/US8039041B2/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN100519691C (zh) * | 2006-09-29 | 2009-07-29 | 中国科学院长春应用化学研究所 | 近红外有机电致发光材料与器件及器件的制备方法 |
Also Published As
Publication number | Publication date |
---|---|
WO1998005187A1 (en) | 1998-02-05 |
JP2000516760A (ja) | 2000-12-12 |
GB2331400B (en) | 2001-01-17 |
US6605823B1 (en) | 2003-08-12 |
US7151341B2 (en) | 2006-12-19 |
DE69710781T2 (de) | 2002-10-31 |
EP0947123B1 (en) | 2002-02-27 |
US20050023961A1 (en) | 2005-02-03 |
DE69710781D1 (de) | 2002-04-04 |
CN1227040A (zh) | 1999-08-25 |
US20060186794A1 (en) | 2006-08-24 |
US20090017191A1 (en) | 2009-01-15 |
EP0947123A1 (en) | 1999-10-06 |
GB9901733D0 (en) | 1999-03-17 |
US8039041B2 (en) | 2011-10-18 |
GB2331400A (en) | 1999-05-19 |
JP3724589B2 (ja) | 2005-12-07 |
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