CN101390198A - 蚀刻硅基材料的方法 - Google Patents
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 68
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Abstract
描述了在小的局部区域中选择性蚀刻硅衬底以在蚀刻表面中形成柱或柱体的方法。将硅衬底放在氟化氢、银盐和醇的蚀刻溶液中。醇的引入提供了更高的硅柱堆积密度。
Description
发明领域
本发明涉及蚀刻硅基材料的方法。
背景技术
已知硅基材料选择性蚀刻产生硅柱例如在制造可再充电锂电池的阳极中是有利的。在经此引用并入本文的US-7033936中描述了一种这样的方法。根据该文献,在硅衬底表面上沉积氯化铯的半球形岛,用薄膜覆盖包括岛的衬底表面,并从表面上除去半球形结构(包括覆盖它们的薄膜)以形成曾经具有半球体的裸露区域的掩膜,通过这样产生掩膜来构造柱体。然后利用反应性离子蚀刻在裸露区域中蚀刻衬底,并通过例如物理溅射除去抗蚀剂从而在未蚀刻区域中,即在半球体位置之间的区域中留下硅柱阵列。
在Peng K-Q,Yan,Y-J,Gao S-P和Zhu J.,Adv.Materials(材料),14(2002),1164-1167,Adv.Functional Materials(功能材料),(2003),13,No 2二月,127-132和Adv.Materials(先进材料),16(2004),73-76中描述了另一化学方法。Peng等人已经展示了通过化学方法在硅上产生纳米柱的一种方式。根据该方法,使用下列溶液在50℃下蚀刻硅片,该硅片可以是n或p-型并具有暴露在溶液中的{111}面:5M HF和20mM AgNO3。以大约20微米/小时形成柱体,并报道了最多24微米的柱体高度。除高度外,没有给出其它尺寸数据,例如平均柱体直径、堆积密度或表面均匀性。该方法仅在大约1平方厘米小片上进行。这些论文中假定的机理为,在初始阶段中在硅表面上无电沉积分离的银纳米簇。在第二阶段中,银纳米簇和它们周围的硅区域充当局部电极,在银纳米簇周围的区域中造成硅电解氧化形成SiF6阳离子,所述SiF6阳离子从蚀刻位置扩散开,在银纳米簇之下留下柱体形式的硅。据建议,可以使用银以外的金属,例如Ni、Fe、Co、Cr和Mg,尤其是硝酸盐形式,以形成硅柱。
K.Peng等人,Angew.Chem.Int.Ed.(德国应用化学),44(2005),2737-2742;和K.Peng等人,Adv.Funct.Mater.(先进的功能材料),16(2006),387-394涉及与Peng等人较早的论文中所述的类似的蚀刻方法,但成核/银纳米粒子沉积步骤和蚀刻步骤在不同溶液中进行。在第一(成核)步骤中,将硅片在4.6M HF和0.01M AgNO3的溶液中放置1分钟。然后第二(蚀刻)步骤在不同的溶液,即4.6M HF和0.135M Fe(NO3)3中进行30或50分钟。这两个步骤均在50℃下进行。报道了分别大约6和4微米高和大约20和20至40纳米直径的柱体。柱体在{111}平面上在{111}方向上生长。没有公开柱体堆积密度(表面均匀性),也没有公开所用硅片的尺寸。硅晶片可以是n或p-型。在这些论文中,与之前的论文相比,对蚀刻步骤提出了不同机理,即除去银(Ag)纳米粒子之下的硅且纳米粒子逐渐下沉到硅体中,在银纳米粒子正下方以外的区域中留下硅柱。
需要更高的柱体,提高的柱体密度和改进的柱体分布均匀性。此外,最好提高柱体形成(蚀刻)速度。此外,因为Peng描述的那些方法局限于{111}面,因此它们的适用性有限。
发明内容
权利要求描述了本发明。
根据现在描述的方法,提供了在硅基衬底上产生硅柱的改进的化学方法。
由从标准半导体材料中的硅晶片上获取的片(其可以为大约1至15平方厘米)开始,将所述片的一面抛光,同时做旧(粗糙化)另一面。晶片平面相当于硅的{100}或{110}晶面。硅可以掺杂以按需要使硅为n-型或p-型,例如使用任何常规掺杂剂。硅片的典型电阻率为1ohm cm乘10的+或-2次幂。例如在n-型硅的情况下,电阻率通常大致为1ohm cm,并且要指出,掺杂水平在本文所述的实施方案中并不关键。
在经受本发明的方法之前,可以使用RCA-1蚀刻(即水:88氨:浓过氧化氢,体积比为1:1:1)均匀地使表面清洁且亲水。在下一制备阶段中,硅片可以在其背面(较粗糙面)上被薄Au/Cr涂层(例如10Au/1Cr,大约200纳米厚的膜)保护。
该蚀刻方法包括两个阶段。第一阶段是成核,其中在硅表面上形成离散的金属沉积物,第二阶段是衬底的实际蚀刻。根据本发明进行这两个阶段产生在密度和高度上都更均匀的柱体阵列。
第一成核阶段在硅表面上形成离散的金属沉积物。在一个实施方案中,成核阶段中所用的水溶液的化学组成为:
- 1至40%v/v的醇,例如乙醇;溶液的典型醇含量基于整个水溶液总体积为5至40%,例如15至40%,任选大约5或6%v/v;
- 1.5至10摩尔(M)氢氟酸,例如5至7.5M,例如大约6.8M(典型浓度的实例为4.5-9M,例如6.8至7.9M;应该指出,HF或氟盐的4.5M、6.8M、7.9M和9M溶液分别相当于在溶液内包含20%、30%、35%和40体积%的浓(40%)HF);
- 5至100mM,例如10至65mM的在氟离子存在下无电沉积在硅衬底上的离散区域中的金属盐,该盐任选为银盐,例如硝酸银;盐的浓度可以为12.6至24mM,例如24mM。(应该指出,12.6至22.1mM溶液相当于含40至70%的31.5mM银溶液的溶液,且24mM溶液相当于含40%的0.06M(60mM)银溶液的溶液)。
进行成核反应的温度可以为0至30℃,例如室温(20℃)。成核反应迅速发生,例如在10秒内,但衬底可以与衬底接触最多大约15分钟,例如大约10分钟。醇,例如乙醇的加入和在相对低温,例如室温下进行成核阶段的作法具有减缓化学过程的作用。因此实现金属沉积物,例如银的更均匀分布,并随后获得更均匀间隔的柱体。
第二阶段是蚀刻,在此期间形成硅柱。蚀刻阶段中所用的溶液可以与成核阶段中所用的相同或不同。如果使用相同溶液,则第二(蚀刻)阶段可以无中断地在第一(成核)阶段之后,且第一和第二阶段的总持续时间通常为5至50分钟。如果使用不同溶液,第一成核阶段通常可以为5至10分钟。蚀刻阶段中所用的溶液可以为:
- 氢氟酸(HF);氟离子的浓度可以为4至15M,例如4.5至8M;
- 可以在氟离子存在下氧化硅的金属盐;该盐任选为银盐或铁盐;并优选为硝酸银或硝酸铁盐。盐的浓度可以为10至40mM,例如20至30mM,例如大约25mM。
醇在蚀刻阶段中不是必要的。
蚀刻阶段根据掺杂密度任选在高于成核阶段的温度下进行;两个阶段之间的温度升高可以为至少20℃,例如至少35℃;蚀刻阶段可以在30至80℃,例如45至75℃,例如60至75℃的温度下进行;在大约45分钟内,可以实现具有大约70至75微米一致高度和0.2微米直径的柱体。蚀刻阶段可以进行较短时间,但柱体则较短。
附带着硅柱的所得硅基衬底可以用作可再充电锂离子电池的阳极,因为本发明人相信,硅柱可以可逆地与锂离子反应而不会分解或破坏,由此提供经过大量充/放电周期的良好电容保持。或者,所述柱体可以从尚未蚀刻的衬底部分上剪切以形成硅纤维。本发明的衬底特别可用在锂离子电池的电极中。
柱体表面密度(覆盖率)可以用下列比率F描述:
F=P/[R+P]
其中P是以柱体存在的硅的量,且R是除去的硅的量。
对于固定的柱体高度,F的值越大,每单位面积的可逆锂离子容量越高,且因此电极的电容越高。此外,F的值越高,可以割下以制造硅纤维的硅材料的量更大。成核阶段使柱体堆积密度F最大化,且申请人已经实现了高达40%的覆盖率。
在上述方法中,F通常为大约15至20%。
在一个实施方案中,本发明提供了蚀刻硅衬底的方法,包括使硅衬底与蚀刻氟酸或氟盐、银盐和醇的溶液接触。银盐是水溶性的,例如硝酸银。溶液的硝酸银含量可以为40至70%,基于31.5mM硝酸银溶液,这相当于最终溶液中的硝酸银浓度为12.6至22.1mM硝酸银。氟酸可包括氟化氢,其在溶液中的含量为30体积%至40体积%,基于浓(40%或22.6M)HF,这相当于最终溶液中的HF浓度为6.8至9M),例如35至40%(最终溶液中的HF浓度为7.9至9M),例如40%(最终溶液中的HF浓度为9M)。醇可以为乙醇,其在最终溶液中的含量可以为15至40%。该溶液也可以包括10至30%,例如20%的水。
该方法可以包括使衬底在10至30℃,例如20℃的溶液中放置5至50分钟,例如10分钟的阶段。该方法可以进一步包括将溶液温度提高至20至75℃达40至45分钟,例如45分钟。
该方法可以包括随后加入另外的银或硝酸银,例如另外的5至10%的银或硝酸银,例如6%。当如前段中提到的那样升高温度时,可以在升高温度时加入银,并可以分别在随后的10和20分钟添加另外两份。
该蚀刻可以在{100}或{110}平面上进行。
本发明还提供了通过上述方法制成的蚀刻硅衬底。
下列两个实施例例证了要求保护的方法:
实施例1
将清洁的硅样品(大约1平方厘米,2-5ohm cm n-型材料,已经如上所述背部涂布)面朝上({100}面)放在含有50毫升蚀刻溶液的聚丙烯烧杯中。蚀刻溶液的组成为:
12.5毫升HF(40%);
2.5毫升乙醇;
35毫升31.5mM AgNO3。
其相当于这样的水溶液,其含有:
5.7M的HF;
5%v/v乙醇;
22mM的AgNO3。
将样品在室温(大约20℃)下放置10分钟以获得在样品面上的均匀银成核。如下所述,乙醇(或其它醇)在其对HF化学的改性中是重要的。
在成核阶段后进行蚀刻阶段。在蚀刻阶段中,将浸没在上述溶液中的硅衬底在恒温浴中在例如75℃下放置45分钟;换言之,蚀刻阶段中所用的溶液与成核阶段中所用的溶液相同。根据确切条件,尤其是该方法的持续时间,该处理蚀刻硅并产生20至100微米高,通常60至100微米高的柱体。
实施例2
根据另一方法,以如下构成的母溶液为原料:
- 20毫升0.06M AgNO3(最终溶液中24mM);
- 17.5毫升浓HF(最终溶液中7.0M);
- 2.5毫升EtOH(最终溶液中5%v/v);和
- 10毫升H2O
(总共50毫升)。然后进行下列程序(a)至(c)之一:
(a)将清洁的硅样品(大约1平方厘米,2-5ohm cm n-型材料,已经如上所述背部涂布)面朝上({100}面)在含有50毫升上述母溶液的聚丙烯烧杯中在20℃下放置10分钟。紧随此后,将温度升至53℃,并同时加入另外的银盐,在这种情况下通过添加3毫升0.6M AgNO3溶液来加入。在45分钟后,取出并漂洗所述片。所得柱体为~85微米高,这比不二次添加3毫升0.6M AgNO3溶液时获得的高50%。
(b)将清洁的硅样品(大约1平方厘米,2-5ohm cm n-型材料,已经如上所述背部涂布)面朝上({100}面)在含有50毫升上述母溶液的聚丙烯烧杯中在20℃下放置10分钟。紧随在此阶段后,对蚀刻阶段,将温度升至53℃,并同时加入1毫升0.6M AgNO3溶液。在10分钟后,再加入1毫升0.6M AgNO3溶液,并再在10分钟后,加入另外1毫升0.6M AgNO3溶液。在53℃下的总时间为45分钟,产生高85至100微米和平均直径0.2微米的均匀柱体。
硝酸银溶液的这种额外添加可以在蚀刻阶段过程中进行,例如在反应的第15、25和35分钟,例如在反应的第10和20分钟。在此方法中,覆盖率F经计算为15至20%。
(c)将清洁的硅样品(大约1平方厘米,10ohm cm n-型材料,已经如上所述背部涂布)面朝上({100}面)在含有50毫升上述母溶液的聚丙烯烧杯中在20℃下放置10分钟,然后转移到用于蚀刻阶段的新溶液中,该溶液可以例如如下构成:
20毫升水;
12.5毫升60mM Fe(NO3)3(aq);和
17.5毫升40%HF。
在45分钟内获得高40微米的均匀柱体。使用SEM分析测量F,大约为30%。Fe(NO3)3浓度变化造成柱体直径变化,在大约0.2至0.6微米。
Fe(NO3)3和/或AgNO3溶液在蚀刻过程中的连续或逐步添加同时导致改进的均匀性和提高的柱体高度。
据发现,本发明的方法获得了为之前获得的高度的大约5倍的增加的柱体高度,并在若干平方厘米上显著改进了柱体均匀性。因此,可以在10至15厘米直径的晶片上以均匀的高度和堆积密度构造硅基电极。或者,可以使柱体生长以便随后脱离,或“收割”,例如以便制造电池阳极,如更详细地描述在也待审的名称为“A method of fabricating fibres composed ofsilicon or a silicon-based material and their use in lithium rechargeablebatteries(由硅或硅基材料构成的纤维的构造方法及其在可再充电锂电池中的用途)”的专利申请UK 0601319.7(其与本专利共同转让并经此引用并入本文)中。
已经发现,醇(例如C1-4链烷醇,如乙醇)在成核步骤中的引入,提供了许多优点。
首先,在成核作用方面,乙醇添加在第一关键时期(大约10秒持续时间)中导致更均匀的银沉积。这造成柱体的更均匀空间分布。
在考虑组成的影响时,可以进一步理解乙醇添加的作用。特别地,改变乙醇浓度(通过改变水/醇比率但保持50毫升的总体积)对柱体高度具有重要影响,这被认为在成核阶段中发生。因此,如果浓度提高超过5%v/v(即在50毫升总溶液量中2.5毫升乙醇),趋势是降低柱体高度。在下表中列出进一步数据:
乙醇(EtOH)浓度对柱体高度的影响
在50毫升总溶液体积中EtOH体积(毫升) | 成核时间(分钟)/温度℃ | 柱体生长时间(分钟)/温度℃ | 柱体高度微米* |
5(10%) | 10/20 | 45/20 | 20 |
5(10%) | 10/20 | 45/45 | 35 |
5(10%) | 10/20 | 45/70 | 40 |
10(20%) | 10/20 | 45/20 | 13 |
10(20%) | 10/20 | 45/45 | 22 |
10(20%) | 10/20 | 45/70 | 20 |
20(40%) | 10/20 | 45/20 | 10 |
20(40%) | 10/20 | 45/45 | ~0 |
20(40%) | 10/20 | 45/70 | ~0 |
在温度影响方面,成核非常迅速发生,<10秒。
室温成核的柱体高于在更高成核温度下获得的那些,因此本发明人相信,对成核阶段使用室温时对该方法具有更好的控制。如果对于10ohm cmn-型硅晶片,温度在室温下(20至25℃)保持10分钟以便成核,然后提高至50℃达45分钟以进行蚀刻阶段,则柱体高度为~30微米。在70℃和75℃之间,柱体高度为~60微米。
高度在~75微米范围内的柱体可以在45分钟内获得。也已经获得高达120微米高的柱体。利用该方法观察到提高的高度的原因是在Fe(NO3)3蚀刻溶液中包含了少量AgNO3(1毫升,在50毫升中加入60mM)。
如果蚀刻阶段在80℃下进行相同时间,则尽管在最初形成柱体,但其被破坏。但是,如果在80℃下进行的蚀刻阶段的蚀刻时间减少,则柱体可见。最后这种结果的出现可能是因为一定的横向蚀刻,这种横向蚀刻会造成锥形的柱体结构,且横向与竖直蚀刻速率的比率随温度而提高。但是,在80℃下在柱体形成中的沉淀物坍塌更可能解释为{110}平面上保护性被吸附物的损失。
据发现,0.1ohm cm至1,000ohm cm范围内的电阻掺杂水平没有影响。此外,该方法对n-和p-型硅均适用。发现,在1至10ohm cm范围内,p-型硅比n-型硅略快地蚀刻。此外,柱体生长不限于{100}平面。在{110}平面上也观察到硅结构的生长,包括与表面倾角为大约45°的柱体和片体。
在{100}平面上的蚀刻产生与晶片表面呈直角的柱体。在{110}平面上,制成与晶片表面呈45°角的柱体。此外,可以在{111}上生长竖直柱体,而在(110)面上具有保护性被吸附物。蚀刻速率为{100}>{111}>>{110}。
通常使用超声进行硅纤维的收割,因为使用刀收割会在纤维材料之外还产生大量微粒硅。
蚀刻方法也可以在极大规模集成(VLSI)电子级单晶片或其不合格样品上进行。作为更便宜的替代物,也可以使用光电级多晶材料。可用的更便宜材料是结晶金属级硅。
会认识到,通过上述方法制成的柱体结构可用在任何适当的实施中,包括可再充电锂离子电池中所用的硅阳极。尽管本文所述的结构被称作“柱体”,但要认识到,包括任何适当的柱状、纤维状或毛状结构。要进一步认识到,上文列出的参数可以适当改变,且所述材料可以由具有适当掺杂的纯硅基材料扩展到例如硅锗混合物。
本文提到的硅基材料包括纯硅或掺杂硅或其它硅基材料,例如硅-锗混合物,或任何其它合适的混合物。制造柱体用的衬底可以是100至0.001Ohm cm的n-或p-型,或其可以是硅的合适合金,例如SixGe1-x。
可以使用其它醇代替乙醇,并且可以使用其它蚀刻剂,例如氟盐,例如氟化铵。
蚀刻和成核都是电流交换反应,例如
Si+6F-+4Ag+=(SiF6)2-+4Ag
可以使用其它可溶银盐代替硝酸银,并且可以以可溶盐,尤其是硝酸盐形式采用其它金属以提供电流交换反应,例如电正性接近或低于银的金属。成核需要金属盐,而蚀刻可以使用金属离子或非金属离子,例如氢离子或硝酸根离子(或两者),只要它们的还原电势在正常氢标度下在0至0.8V范围内或与之接近。上文提到的Peng等人的文章提到了可代替银使用的其它金属。可以使用具有+0.8V至0.0V的电势的金属离子(vs标准氢电极(SHE)),例如Cu2+离子(+0.34V(vs SHE))代替银离子。
Claims (29)
1.蚀刻硅衬底的方法,包括使硅衬底与下列物质的水溶液接触:
■氟酸或氟盐,
■能够在氟离子存在下在硅上无电沉积金属的金属盐,和
■醇。
2.如权利要求1所述的方法,其中金属盐是银盐,任选硝酸银。
3.如权利要求2所述的方法,其中溶液的硝酸银含量为0.2至16重量%,例如0.75至0.7重量%。
4.如权利要求1或2所述的方法,其中溶液的金属盐含量,例如银或硝酸银含量为5至100mM,例如12.6至24mM,例如12.6至22.1mM。
5.如前述权利要求任一项所述的方法,其中氟酸包括氟化氢,其含量为3至20重量%,例如8至20%,例如10至15%,例如大约12或13.6%。
6.如前述权利要求任一项所述的方法,其中蚀刻氟酸包括氟化氢,其含量为1.5至10M,例如5至7.5M,例如大约6.8M。
7.如前述权利要求任一项所述的方法,其中所述醇为乙醇。
8.如前述权利要求任一项所述的方法,其中醇含量为最多40体积%,例如3%至40%,例如5至40%,例如15至30%。
9.如前述权利要求任一项所述的方法,进一步包括使衬底放置在0℃至30℃,例如20℃的溶液中的阶段。
10.如权利要求9所述的方法,其中所述放置步骤持续5至50分钟,例如大约10分钟。
11.如前述权利要求任一项所述的方法,进一步包括将溶液温度升至40℃至75℃。
12.如权利要求11所述的方法,其中使衬底在所述升高的温度下在溶液中放置30至100分钟,例如大约45分钟。
13.如前述权利要求任一项所述的方法,进一步包括在该方法过程中加入另外的银盐,例如硝酸银,或铁盐,例如硝酸铁。
14.如权利要求13所述的方法,其中加入的银盐或铁盐的量为0.1至2重量%,例如大约1重量%。
15.如权利要求13或14所述的方法,其中另外的银盐或铁盐的加入量使溶液的银或铁浓度提高2mM至6mM,例如2.85mM至5.45mM。
16.如权利要求13至15任一项所述的方法,当从属于权利要求11或12时,在该方法中在升高温度时加入所述另外的银盐或铁盐。
17.如权利要求16所述的方法,其中在升高温度时加入第一份银盐或铁盐,然后加入另外的至少一份,例如在随后的10和20分钟加入。
18.如权利要求1至11任一项所述的蚀刻硅衬底的方法,其中所述接触步骤构成使用第一溶液的第一阶段,且该方法进一步包括:
第二阶段,包括使硅衬底与包含氟酸和铁盐,例如Fe(NO3)3的第二溶液接触。
19.如权利要求18所述的方法,其中使衬底在第一溶液中放置最多15分钟,例如大约10分钟。
20.如权利要求18或19所述的方法,其中第二阶段在比第一阶段高的温度进行,例如30至80℃,例如45至75℃,例如60至75℃。
21.如权利要求18至20任一项所述的方法,其中第二阶段进行40至50分钟,例如大约45分钟。
22.如权利要求18至21任一项所述的方法,其中第二溶液包括银盐,例如最多60mM的量。
23.如权利要求18至22任一项所述的方法,进一步包括在该方法的过程中向溶液中,尤其是在第二阶段过程中向第二溶液中,加入银盐或铁盐,例如Fe(NO3)3和/或AgNO3。
24.如权利要求23所述的方法,其中加入的另外的银盐或铁盐的量是使溶液的银或铁浓度提高最多10mM,例如2mM至6mM的量。
25.如权利要求23或24所述的方法,其中两次或更多次向第二溶液中加入银或铁盐。
26.如权利要求18至25任一项所述的方法,其中使衬底在第二溶液中放置40至50分钟,例如45分钟。
27.如前述权利要求任一项所述的方法,其中蚀刻在{100}平面或{110}平面或{111}平面上进行。
28.通过如前述权利要求任一项所述的方法制成的蚀刻硅衬底。
29.可再充电锂电池,其阳极包含如权利要求28所述的蚀刻硅衬底。
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PCT/GB2007/000204 WO2007083152A1 (en) | 2006-01-23 | 2007-01-23 | Method of etching a silicon-based material |
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- 2007-01-23 TW TW096102457A patent/TWI446432B/zh not_active IP Right Cessation
- 2007-01-23 WO PCT/GB2007/000204 patent/WO2007083152A1/en active Application Filing
- 2007-01-23 CN CN2007800063282A patent/CN101390198B/zh not_active Expired - Fee Related
- 2007-01-23 EP EP07704981A patent/EP1977443A1/en not_active Withdrawn
- 2007-01-23 RU RU2008132685/28A patent/RU2429553C2/ru not_active IP Right Cessation
- 2007-01-23 JP JP2008551860A patent/JP5043041B2/ja not_active Expired - Fee Related
- 2007-01-23 US US12/161,657 patent/US8585918B2/en not_active Expired - Fee Related
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- 2007-01-23 KR KR1020087019666A patent/KR101182681B1/ko not_active IP Right Cessation
- 2007-01-23 MX MX2008009435A patent/MX2008009435A/es unknown
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Also Published As
Publication number | Publication date |
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NO20083502L (no) | 2008-08-13 |
CN101390198B (zh) | 2011-04-13 |
US20100233539A1 (en) | 2010-09-16 |
RU2429553C2 (ru) | 2011-09-20 |
IL192969A0 (en) | 2009-02-11 |
GB0601318D0 (en) | 2006-03-01 |
EP1977443A1 (en) | 2008-10-08 |
CA2637737C (en) | 2016-03-01 |
KR20090004858A (ko) | 2009-01-12 |
TW200735205A (en) | 2007-09-16 |
WO2007083152A1 (en) | 2007-07-26 |
MX2008009435A (es) | 2009-01-13 |
JP5043041B2 (ja) | 2012-10-10 |
US8585918B2 (en) | 2013-11-19 |
JP2009524264A (ja) | 2009-06-25 |
KR101182681B1 (ko) | 2012-09-14 |
TWI446432B (zh) | 2014-07-21 |
RU2008132685A (ru) | 2010-02-27 |
CA2637737A1 (en) | 2007-07-26 |
BRPI0707164A2 (pt) | 2011-08-02 |
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