CN1871662A - 溅射沉积中硒化银膜化学计量比和形态控制 - Google Patents
溅射沉积中硒化银膜化学计量比和形态控制 Download PDFInfo
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Abstract
一种溅射沉积硒化银并控制溅射沉积硒化银膜的化学计量比、结节缺陷形成和晶体结构的方法。该方法包括在约0.3-约10mTorr的压力下,使用溅射沉积方法沉积硒化银。根据本发明的一个方面,优选在约2-约3mTorr的压力下使用RF溅射沉积方法。根据本发明的另一个方面,优选在约4-约5mTorr的压力下使用脉冲DC溅射沉积方法。根据本发明的另一个方面,可以在约10mTorr的压力和小于约250W的溅射功率下溅射沉积含α-和β-硒化银的硒化银膜。
Description
发明领域
本发明涉及使用硫属玻璃形成的电阻可变存储器件领域,特别涉及一种将硒化银膜沉积在硫属玻璃上的改进方法。
发明背景
与目前使用的存储技术相比,由于在开关特性、不挥发性、存储速度、可靠性、热特性和耐用性方面有潜在的优点,所以将硫属化物材料用于电阻可变存储器件在目前引起极大的关注。在下面的论文中报道了此领域中的研究“High Speed Memory Behavior and Reliabilityof an Amorphous As2S3 Film doped with Ag”,Hirose等人,Phys.Stat.Sol.(1980),第K187-K190页;“Polarity-dependent memoryswitching and behavior of Ag dendrite in Ag-photodoped amorphousAs2S3 films”,Hirose等人,Journal of applied Physics,第47卷,No.6(1976),第2767-2772页;和“Dual Chemical Role of Ag as anAdditive in Chalcogenide Glasses”,Mitkova等人,Physical ReviewLetters,第83卷,No.19(1999),第3848-3851页,本文中引入其内容作为参考。
在许多使用硫属化物材料的存储元件设计中,将硒化银(As2S)的膜与硫属化物材料层结合。硒化银膜对电气性能是重要的。因此,硒化银沉积是制造电阻可变存储器件的一个重要方面。最可利用的对硒化银沉积的研究有限,通常选择蒸发沉积来形成硒化银膜。
蒸发沉积的硒化银具有伴随的问题,因为硒化银的分解性使得不可能获得硒化银的精密化学计量比。我们认为,在蒸发法中,当银开始向低浓度扩散时,它开始聚集。由于银被束缚在簇或聚集体中,所以在蒸发过程的开始,硒更容易蒸发。因此,在蒸发法的过程中,硒更迅速地蒸发,造成沉积靶变为富银的。接近蒸发过程的结束,很少乃至没有硒因为沉积而留在基质上,而因为沉积主要留下银。因此,大量的硒沉积在基质上,随后主要是银沉积。因此,蒸发法没有均匀沉积硒化银,并且控制蒸发硒化银的化学计量比和表面形态是困难的。
而且,蒸发沉积无助于工业应用。溅射沉积更容易用于工艺过程,而且与蒸发沉积法相比,溅射沉积具有许多优点。例如,溅射沉积提供更好的膜厚度和质量控制。
通常,通过将基质放在抽真空或加压至所需压力的沉积室中进行溅射沉积或溅射。然后,在该室内产生通常由靶产生的膜材料的粒子流,该颗粒冷凝到基质上而出现沉积。在另一种常常称为离子束轰击溅射的溅射法中,高能的离子源束射向靶。轰击离子的力将足够的能量传给靶的原子以使活化的原子离开靶子并形成粒子流。在基质上得到的沉积物形成薄膜。
由于银的高扩散性能,硒的低熔点以及硒化银的记忆性能,在溅射沉积的过程中控制硒化银膜的化学计量比和形态是困难的。例如,硒化银块材是导电的,但其电导率(约几千ohm-1cm-1)较大多数金属的电导率相对低。并且,银浓度对器件的电气性能是关健的,因此必须使银浓度保持在接近于约66.7原子%(本文中,后面表示为“%”)。随着银浓度高于约67.5%,在硒化银膜中和/或硒化银膜上许多结节缺陷。这些缺陷的尺寸可以为约1/10微米,这对亚微米器件制造有严重的负面影响。尽管还不知道形成这些缺陷的准确机理,但我们认为这些缺陷是由超过硒化银膜中所需化学计量比的银浓度要求的过量银造成的。
常规的溅射方法还导致其结构几乎仅仅由β-硒化银组成的沉积硒化银膜。然而,对于最佳的器件性能来说,理想的是制造含α-和β-硒化银的硒化银膜。
理想的是具有一种改进的沉积硒化银膜的方法。对于溅射沉积来说,具有一种控制硒化银的化学计量比和形态的方法也是理想的。具有一种形成含α-和β-硒化银的溅射沉积硒化银的方法也是理想的。
发明概述
本发明一个示范性的实施方案包括将硒化银膜沉积在基质上的方法。该方法包括使用低压溅射沉积方法。优选的溅射沉积方法包括RF溅射或脉冲DC溅射。优选地,该溅射沉积将在约0.3-约10mTorr的压力范围内进行。本发明特别用于沉积具有较好化学计量比精度的硒化银膜。本发明也特别用于溅射沉积硒化银膜,同时避免在整个硒化银膜内和在该硒化银膜的表面上形成结节缺陷。最后,在约10mTorr的溅射压力和小于约250W的溅射功率下,本发明也用于沉积包含α-和β-硒化银的硒化银膜。
根据以下结合附图提供的详细说明将会更好地理解本发明的这些及其它特点和优点。
附图简述
图1(a)是使用20mTorr压力沉积的脉冲DC溅射沉积硒化银膜的SEM图。
图1(b)是使用10mTorr压力沉积的脉冲DC溅射沉积硒化银膜的SEM图。
图1(c)是使用3mTorr压力沉积的脉冲DC溅射沉积硒化银膜的SEM图。
图2说明在不同溅射压力和功率下溅射的沉积硒化银膜的两个X-射线衍射图。
发明详述
在下面的详细说明中,涉及到本发明各种具体结构的实施方案和方法的实施方案。用足够的细节描述这些实施方案以使本领域普通技术人员能够实施本发明。应该理解的是,可以使用其它实施方案,并且可以进行各种结构上的、逻辑上的和电气上的改变而不背离本发明的精神或范围。
术语“硒化银”意在包括各类硒化银,包括具有稍过量或缺乏银的种类,例如Ag2Se、Ag2+xSe和Ag2-xSe。
术语“硫属玻璃”意在包括基于只选自VIA族中的元素(S、Se、Te、Po、O)或选自其与IV族(Si、Ge)和/或V族(P、As、Sb、Bi)中元素组合的各种组合物结构。
本发明涉及一种沉积硒化银的方法。根据本发明,使用例如0.3-约10mTorr的低压来溅射沉积硒化银。并且,根据本发明,优选使用RF溅射方法或脉冲DC溅射方法沉积硒化银。
硒化银本身具有电存储性能,即电导率,而溅射沉积方法通常包括强电流、电压和离子轰击。因此,溅射沉积方法中的电和热效应都会影响硒化银溅射靶和沉积的硒化银膜。出于上述原因,溅射沉积需要考虑怎样将电能施加到硒化银靶上。
因为硒化银的电导率较大多数金属的电导率相对低,所以D.C.溅射不起作用。规则的DC磁控管溅射试验没有效,主要是因为等离子体不容易引燃。
取决于靶年龄,在较高压力,例如约20mTorr或更高压力下溅射沉积导致银浓度低于或高于所需约66.7%的化学计量比银浓度的膜。已经观察到,使用RF或脉冲DC磁控管溅射沉积的相对新靶的高压沉积,例如约20mTorr或更高,产生银浓度只有约60%的硒化银膜,这比所需66.7%的化学计量比银浓度低得多。也已观察到,使用RF或脉冲DC磁控管溅射沉积的相对老靶的高压沉积,例如约20mTorr或更高,产生银浓度高于约67.5%的硒化银膜。
本发明人发现,在约0.3-约10mTorr的低压下,可以使用RF或脉冲DC磁控管溅射沉积方法来沉积更精密化学计量比的硒化银膜,同时避免在该膜中形成结节缺陷。还已发现,硒化银靶组成随靶的寿命而改变,而使用低压溅射沉积方法用老的和新的硒化银靶都可以获得精密化学计量比沉积物。
图1说明具有氮化硅薄膜的、由工业等级硅片形成的基质的SEM图,所述氮化硅膜具有约500埃厚的脉冲DC溅射沉积的硒化银膜。使用200kHz、脉冲宽度1056ns、恒定动力供应150W的DentonVacuum Discovery24脉冲DC溅射沉积图1中所示的硒化银膜。使用具有约66.7%的化学计量比银浓度的硒化银靶来沉积硒化银膜。比较各种压力下脉冲DC溅射沉积硒化银膜的SEM图表明,约0.3-约10mTorr的低压溅射沉积降低并消除结节缺陷形成。观察到,使用高压,即约20mTorr沉积的硒化银膜具有高于约67.5%的银浓度,并且如图1(a)所示,在该膜的表面上和整个膜内形成结节缺陷;如图1(b)所示,使用10mTorr低压形成的沉积硒化银膜具有相对少的结节缺陷;如图1(c)所示,使用3mTorr的更低压力的沉积膜具有无结节缺陷的光滑表面。
根据本发明的第一个实施方案,在约0.3-约10mTorr,更优选约2-约3mTorr的低压下,使用RF溅射沉积方法溅射沉积硒化银靶,从而提供这样的硒化银膜,该膜具有很少,甚至没有结节缺陷,银浓度约等于用于溅射沉积该硒化银膜的硒化银靶的银浓度。例如,在RF溅射沉积方法中使用银浓度约为66.7%的硒化银靶的情况下,沉积的硒化银膜的银浓度小于约67.5%,优选约67%,更优选约66.7%。根据本发明第一个实施方案的方法可以用于任何年龄的硒化银靶,同时还提供这样一种溅射沉积硒化银膜,所述硒化银膜的银浓度约等于用于沉积该硒化银膜的硒化银靶的银浓度。
在根据本发明第一个实施方案的溅射方法中,溅射沉积通常发生在室中。首先建立初始基础真空压力(initial base vacuum pressure)。该初始基础真空压力可以是任何合适的压力,包括高于约10mTorr的压力,这可以帮助引燃等离子体。在溅射方法的过程中,应该将工艺气体维持在约0.3-约10mTorr,优选约2-约3mTorr的压力下。工艺气体可以是任何合适的溅射工艺气体,例如氪、氙、氦、氖、氩或它们的组合。优选的工艺气体是氩。尽管不希望受到任何特定功率的限制,但在溅射方法的过程中施加的功率优选为,例如,约100-约500瓦,最优选为约150瓦。能量密度和能量需要可以改变,这取决于选择的系统或靶的尺寸。例如,4英寸或更大的靶需要更大的功率。优选的RF频率为约100kHz-约20MHz,优选为13.5MHz。示范性的溅射沉积系统是Denton Vacuum Discovery24。
根据本发明的第二个实施方案,在约0.3-约10mTorr的低压下,使用脉冲DC溅射沉积方法溅射沉积硒化银,从而提供这样的硒化银膜,该膜具有的银浓度约等于用于溅射沉积该硒化银膜的硒化银靶的银浓度。例如,在脉冲DC溅射沉积方法中使用银浓度约为66.7%的硒化银靶的情况下,沉积的硒化银膜的银浓度小于约67.5%,优选约67%,更优选约66.7%。约4-约5mTorr的低压是优选的。RF溅射沉积与脉冲DC溅射沉积之间的差异在于,对于脉冲DC溅射,约4-约5mTorr的沉积压力制造银浓度基本上等于硒化银靶银浓度,例如66.7%的沉积硒化银膜。然而,通常,低压沉积提供具有更精密硒化银化学计量比的更光滑溅射沉积硒化银膜。使用的优选低压可以依靶的状况,例如靶的年龄而改变。
与上述根据本发明第一个实施方案的方法相似,根据第二个实施方案的溅射沉积也发生在室中,例如Denton Vacuum Discovery24中,其中首先建立合适的初始基础真空压力,并使用合适的工艺气体。然而,根据第二个实施方案,在溅射方法的过程中,应该将工艺气体维持在约0.3-约10mTorr,优选约4-约5mTorr的压力下。尽管不希望受到任何特定功率的限制,但在溅射方法的过程中施加的功率优选为,例如,约100-约500瓦,最优选为150瓦;优选的脉冲DC频率可以为,例如约100-约250kHz,优选为约200kHz。然而,能量密度和能量要求可以改变,并且t取决于选择的系统和/或靶的尺寸。例如,4英寸或更大的靶需要更大的功率。脉冲宽度应该为约1000-约1200ns,优选为约1056ns。
尽管还不知道解释实验观测值起点的准确机理,但溅射压力、离子动能、散射诱导能量降低和/或RF与脉冲DC等离子体电性质之间有联系。对于实际应用,发明人建议在较低压力下使用RF溅射沉积方法或脉冲DC溅射沉积方法来沉积较好精度化学计量比的硒化银膜,并避免在该膜上形成结节缺陷。因此,压力可以在约0.3-约10mTorr的低压范围内改变以微调硒化银膜的银浓度。也可以改变功率源。这在器件制造中非常重要,因为许多器件需要元素浓度稍微偏离(即,±2%浓度)约66.7%的优选值。因此,由于低压溅射沉积也可以用在相对老的靶上,同时仍然提供更精密的银化学计量比浓度,所以本发明延长了靶寿命,因此降低了工艺成本。
根据本发明,除了在溅射沉积的过程中控制硒化银的化学计量比和形态之外,理想的是也控制了沉积硒化银的晶体结构。
硒化银(例如Ag2Se)由于其406K(约130℃)的低温相转变点而众所周知。Ag2Se在低于406K的温度下形成称为“β相”的斜方结构。Ag2Se在高于406K(约133℃)的温度下经历结构改变,其中Se形成体心立方亚晶格,同时银经受熔化转变。在此所谓的“α相”或“超离子相(superionic phase)”中,Ag离子显示液体状分散。Se亚晶格在约1170K(897℃)下也将经受熔化转变。
根据本发明,理想的是由α-和β-硒化银相的混合物形成沉积的硒化银膜。这种混合物对由硒化银膜形成的某些器件的最佳性能来说是关健的。根据本发明,可以在相对低功率/相对高压力的条件下,通过溅射方法形成含α和β相的硒化银膜。
图2说明溅射沉积硒化银膜的两幅X-射线衍射(XRD)图200和220。图1说明在350W的溅射功率和50sccm的氩气溅射气体流速下溅射沉积的硒化银膜的XRD图200,该气体流速相应于约7mTorr的溅射气压。图2说明在350W的溅射功率和75sccm的氩气溅射气体流速下溅射沉积的硒化银膜的XRD图220,该气体流速相应于约10mTorr的溅射气压。图200和220表明,在后一种状况下,在粗略模式2θXRD图中,在约23和37度出现α和β峰。
虽然不受理论的限制,但基于XRD图200和220,好像在溅射过程中硒化银与基质的较低能量冲击在沉积膜中产生更多的α相硒化银。较低的溅射功率和较高的溅射压力降低赋予溅射硒化银分子的动能,因此导致硒化银与基质的较低能量冲击。而且,似乎将基质加热至高于室温(约25℃)的温度也提高沉积膜中的α相。
虽然硒化银的晶体结构(即α和β相的混合物)对于使用这种膜的器件的最佳性能来说是重要的,但是膜的化学计量比和组织(例如光滑性)也影响如上所述的器件性能。因此,一定程度上降低溅射功率或升高溅射压力导致显示具有粗糙表面或非所要求的化学计量比的膜,为了制造具有所需化学计量比并且结构显示α和β两相的光滑硒化物膜,必须平衡溅射功率和压力参数。然而,应该强调,与用于制造该膜的方法无关,理想的是在沉积的硒化银膜中存在有α相。
根据本发明的第三个示范性实施方案,在使所述硒化银膜的结构含α相和β相的溅射条件下溅射沉积硒化银膜。具体地说,使用小于约250W的溅射功率和至少约10mTorr的溅射压力溅射沉积硒化银。而且,在溅射功率小于约250W,溅射压力约为10mTorr的溅射条件下,可以在基质上形成含α和β结构相、具有约等于硒化银溅射靶银浓度的银浓度且无表面缺陷的硒化银膜。
虽然已经描述并说明了本发明的示范性实施方案,但是可以进行变化和改变而不背离本发明的精神或范围。因此,本发明不受上述说明的限制,而只受附加的权利要求的范围限制。
Claims (79)
1.一种沉积硒化银的方法,包括:
在溅射沉积室中提供硒化银溅射靶;
将溅射气体引入所述室中,其中将所述溅射气体保持在约0.3-约10mTorr的压力下;和
在所述靶上进行溅射工艺,从而制造沉积的硒化银膜。
2.权利要求1的方法,其中所述沉积的硒化银膜具有的银浓度约等于所述硒化银靶的银浓度。
3.权利要求2的方法,其中所述硒化银靶具有约66.7%的银浓度。
4.权利要求3的方法,其中所述沉积硒化银膜具有小于约67.5%的银浓度。
5.权利要求3的方法,其中所述沉积硒化银膜具有约67%的银浓度。
6.权利要求3的方法,其中所述沉积硒化银膜具有约66.7%的银浓度。
7.权利要求2的方法,其中所述硒化银膜基本上没有结节缺陷。
8.权利要求1的方法,其中所述溅射沉积方法是RF溅射沉积方法。
9.权利要求8的方法,其中所述溅射压力为约2-约3mTorr。
10.权利要求1的方法,其中使用约100-约500瓦的溅射功率进行所述溅射沉积。
11.权利要求10的方法,其中所述功率为约150瓦。
12.权利要求8的方法,其中使用约100kHz-约20MHz的频率进行所述沉积方法。
13.权利要求12的方法,其中所述频率约为13.5MHz。
14.权利要求1的方法,其中所述溅射沉积方法是脉冲DC溅射沉积方法。
15.权利要求14的方法,其中所述压力为约4-约5mTorr。
16.权利要求14的方法,其中使用约100-约250kHz的频率进行所述沉积方法。
17.权利要求16的方法,其中所述频率约为200kHz。
18.权利要求14的方法,其中使用约1000-约1200ns的脉冲宽度进行所述溅射沉积方法。
19.权利要求18的方法,其中所述脉冲宽度约为1056ns。
20.一种控制溅射沉积硒化银膜的化学计量比的方法,包括:
使用约0.3-约10mTorr的溅射沉积压力溅射沉积具有预定银浓度的硒化银膜;和
在沉积所述硒化银膜的同时,在所述范围内改变所述溅射沉积压力。
21.权利要求20的方法,其中所述硒化银膜具有小于约67.5%的银浓度。
22.权利要求21的方法,其中所述硒化银膜具有约67%的银浓度。
23.权利要求21的方法,其中所述硒化银膜具有约66.7%的银浓度。
24.权利要求21的方法,其中所述硒化银膜基本上没有结节缺陷。
25.权利要求20的方法,其中使用约100-约300瓦的功率进行所述溅射沉积。
26.权利要求25的方法,其中所述功率约为150瓦。
27.权利要求20的方法,其中使用RF溅射沉积方法进行所述溅射沉积。
28.权利要求27的方法,其中使用约100kHz-约20MHz的频率进行所述RF溅射沉积方法。
29.权利要求28的方法,其中所述频率约为13.5MHz。
30.权利要求20的方法,其中使用脉冲DC溅射沉积方法进行所述溅射沉积。
31.权利要求30的方法,其中使用约100-约250kHz的频率进行所述脉冲DC溅射沉积方法。
32.权利要求31的方法,其中所述频率约为200kHz。
33.权利要求30的方法,其中使用约1000-约1200ns的脉冲宽度进行所述脉冲DC溅射沉积方法。
34.权利要求33的方法,其中所述脉冲宽度约为1056ns。
35.一种沉积硒化银的方法,包括:
提供银浓度约为66.7%的硒化银溅射靶,
保持约0.3-约10mTorr的溅射沉积压力;和
在所述硒化银溅射靶上进行RF溅射方法,其中所述RF溅射方法形成沉积的硒化银膜。
36.权利要求35的方法,其中所述硒化银膜具有小于约67.5%的银浓度。
37.权利要求35的方法,其中所述硒化银膜具有约67%的银浓度。
38.权利要求35的方法,其中所述硒化银膜基本上没有结节缺陷。
39.权利要求35的方法,其中所述压力为约2-约3mTorr。
40.权利要求35的方法,其中使用约100-约300瓦的功率进行所述RF溅射沉积方法。
41.权利要求40的方法,其中所述功率约为150瓦。
42.权利要求35的方法,其中使用约100kHz-约20MHz的频率进行所述RF溅射沉积方法。
43.权利要求42的方法,其中所述频率约为13.5MHz。
44.一种沉积硒化银的方法,包括:
提供银浓度约为66.7%的溅射硒化银靶;和
在约0.3-约10mTorr的压力下进行脉冲DC溅射沉积方法,其中所述DC溅射沉积方法形成沉积的硒化银膜。
45.权利要求44的方法,其中所述硒化银膜具有小于约67.5%的银浓度。
46.权利要求44的方法,其中所述硒化银膜具有约67%的银浓度。
47.权利要求44的方法,其中所述硒化银膜具有约66.7%的银浓度。
48.权利要求45的方法,还包括由所述溅射靶形成基本上没有结节缺陷的硒化银膜。
49.权利要求44的方法,其中所述压力约为4-约5mTorr。
50.权利要求44的方法,其中使用约100-约250kHz的频率进行所述脉冲DC溅射沉积方法。
51.权利要求50的方法,其中所述频率约为200kHz。
52.权利要求44的方法,其中使用约1000-约1200ns的脉冲宽度进行所述脉冲DC溅射沉积方法。
53.权利要求52的方法,其中所述脉冲宽度约为1056ns。
54.一种沉积硒化银的方法,包括:
提供银浓度约为66.7%的硒化银溅射靶;和
使用硒化银溅射靶进行溅射工艺,从而形成银浓度小于约67.5%的硒化银膜。
55.权利要求54的方法,其中使用约0.3-约10mTorr的沉积压力进行所述溅射沉积。
56.权利要求55的方法,其中使用RF溅射沉积方法进行所述溅射沉积。
57.权利要求56的方法,其中使用约2-约3mTorr的溅射沉积压力进行所述RF溅射沉积方法。
58.权利要求54的方法,其中使用脉冲DC溅射沉积方法进行所述溅射沉积。
59.权利要求58的方法,其中使用约4-约5mTorr的溅射沉积压力进行所述脉冲DC溅射沉积。
60.一种在约0.3-约10mTorr的压力下沉积的溅射沉积硒化银膜,所述膜基本上没有结节缺陷。
61.权利要求60的膜,其中使用银浓度小于约67.5%的硒化银靶沉积所述溅射沉积硒化银膜。
62.权利要求61的膜,其中所述硒化银膜具有约66.7%的银浓度。
63.权利要求61的膜,其中所述硒化银膜具有约67%的银浓度。
64.权利要求60的膜,其中RF溅射沉积所述硒化银膜。。
65.权利要求63的膜,其中所述压力为约2-约3mTorr。
66.权利要求60的膜,其中脉冲DC溅射沉积所述膜。
67.权利要求66的膜,其中所述压力为约4-约5mTorr。
68.一种银浓度小于约67.5%的溅射沉积硒化银膜。
69.权利要求68的膜,其中使用银浓度为约66.7%的硒化银靶沉积所述溅射沉积硒化银膜。
70.权利要求69的膜,其中所述硒化银膜具有约67%的银浓度。
71.权利要求69的膜,其中所述硒化银膜具有约66.7%的银浓度。
72.权利要求68的膜,其中RF溅射沉积所述溅射沉积硒化银。
73.权利要求68的膜,其中脉冲DC溅射沉积所述溅射沉积硒化银。
74.一种沉积硒化银的方法,包括:
在溅射沉积室中提供硒化银溅射靶;
将溅射气体引入所述室中;
在所述靶上进行溅射工艺,从而产生沉积的硒化银膜,其中所述硒化银包括α-硒化银和β-硒化银。
75.权利要求74的方法,其中在所述溅射过程中,将所述溅射气体维持在约10mTorr的压力下。
76.权利要求74的方法,其中在所述溅射过程中,将所述溅射过程的溅射功率维持在小于约250W下。
77.权利要求74的方法,其中所述沉积的硒化银膜具有的银浓度约等于所述硒化银溅射靶的银浓度。
78.权利要求77的方法,其中所述硒化银靶具有约66.7%的银浓度。
79.权利要求74的方法,其中所述硒化银膜基本上无结节缺陷。
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US20080210921A1 (en) | 2008-09-04 |
WO2004020683A2 (en) | 2004-03-11 |
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CN1871662B (zh) | 2010-05-05 |
KR20050059097A (ko) | 2005-06-17 |
EP1573081A2 (en) | 2005-09-14 |
JP4164068B2 (ja) | 2008-10-08 |
AU2003270012A1 (en) | 2004-03-19 |
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US20050098428A1 (en) | 2005-05-12 |
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WO2004020683A3 (en) | 2005-10-20 |
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KR100782244B1 (ko) | 2007-12-05 |
KR100669611B1 (ko) | 2007-01-16 |
US20140224646A1 (en) | 2014-08-14 |
KR100732498B1 (ko) | 2007-06-27 |
KR20070036803A (ko) | 2007-04-03 |
US20040040835A1 (en) | 2004-03-04 |
KR20060106937A (ko) | 2006-10-12 |
EP1573081A3 (en) | 2005-12-07 |
KR20060106936A (ko) | 2006-10-12 |
US7364644B2 (en) | 2008-04-29 |
JP2006503977A (ja) | 2006-02-02 |
KR100669612B1 (ko) | 2007-01-16 |
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