CN1204602C - 金属用研磨液及研磨方法 - Google Patents
金属用研磨液及研磨方法 Download PDFInfo
- Publication number
- CN1204602C CN1204602C CNB998127760A CN99812776A CN1204602C CN 1204602 C CN1204602 C CN 1204602C CN B998127760 A CNB998127760 A CN B998127760A CN 99812776 A CN99812776 A CN 99812776A CN 1204602 C CN1204602 C CN 1204602C
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- Prior art keywords
- acid
- diaphragm
- agent
- polishing slurry
- compound
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- Expired - Lifetime
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- XUZLXCQFXTZASF-UHFFFAOYSA-N nitro(phenyl)methanol Chemical compound [O-][N+](=O)C(O)C1=CC=CC=C1 XUZLXCQFXTZASF-UHFFFAOYSA-N 0.000 description 1
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- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
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- 235000004330 tyrosol Nutrition 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
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- C—CHEMISTRY; METALLURGY
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- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
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- Microelectronics & Electronic Packaging (AREA)
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Abstract
本发明提供金属用研磨液及研磨方法,该金属用研磨液含有(1)金属的氧化剂,(2)氧化金属溶解剂,(3)通过在金属膜表面形成物理吸附和/或化学结合而形成称为氨基酸或唑类的保护膜的第1保护膜形成剂、(4)辅助第1保护膜形成剂形成称为聚丙烯酸、聚酰胺酸或者其盐的第2保护膜形成剂,以及(5)水。
Description
技术领域
本发明是关于在半导体装置的配线形成过程中的研磨中,特别适合使用的金属用研磨液及研磨方法。
背景技术
近年来,伴随半导体集成电路(以下,称为LSI)的高集成化、高性能化,正在开发新的微细加工技术。化学机械研磨(以下,称为CMP)法也是其中的一种,是在LSI制造过程,特别是在多层配线形成过程中的层间绝缘膜的平坦化、金属插头形成、埋入配线形成中频繁使用的技术。该技术,例如在美国专利第4944836号公报中已公开。
另外,最近为了使LSI高性能化,正尝试利用铜合金作为配线材料。但是,铜合金难以利用在以往的铝合金配线的形成中频繁使用的干腐蚀法进行微细加工。因此,主要采用在预先形成沟的绝缘膜上堆积铜合金薄膜而埋入,利用CMP去除沟部以外的铜合金薄膜,形成埋入配线的所谓大马士革波形花纹(damascen)法。该技术例如在特开平2-278822号公报中已公开。
金属的CMP的一般方法是在圆形的研磨底盘(压磨板)上固定研磨垫,用金属用研磨液浸渍研磨垫,压紧形成基体的金属膜的面,从其里面以施加规定的压力(以下,称为研磨压力)的状态使研磨底盘旋转,利用研磨液和金属膜的凸部的机械摩擦,去除凸部的金属膜的方法。
在CMP中使用的金属用研磨液,一般由氧化剂和固体磨粒组成,根据需要,还可以添加氧化金属溶解剂、保护膜形成剂。被认为首先通过氧化使金属膜表面氧化,利用固体磨粒磨去该氧化层的基本机制。凹部的金属表面的氧化层不太接触研磨垫,达不到利用固体磨粒磨去的效果,因此随着CMP的进行,去除凸部的金属层,使基体表面平坦化。关于该详细情况,在Journal of eletrochemical society杂志第138卷11号(1991年发行)的3460~3464页已描述过。
如果利用固体磨粒磨去的金属氧化物的颗粒通过氧化金属溶解剂溶解于研磨液中,就增加利用固体磨粒磨去的效果。但是,凹部的金属膜表面的氧化层也溶解(以下,称为腐蚀),金属膜表面露出时,由于氧化剂使金属膜表面进一步氧化,并且其反复进行时,也进行了凹部的金属膜的腐蚀,因此就有平坦化效果受损的担心。为了防止平坦化效果受到损害,再添加保护膜形成剂。达到氧化金属溶解剂和保护膜形成剂的效果平衡是非常重要的,希望金属膜表面的氧化层不太被腐蚀、磨去的氧化层的颗粒效率良好地被溶解、利用CMP的研磨速度大。
像这样,通过添加氧化金属溶解剂和保护膜形成剂来增加化学反应的效果,在提高CMP速度(即由CMP产生的研磨速度)的同时,也得到减低由CMP引起的金属层表面的损伤的效果。
但是,在使用含有以往的固体磨粒的金属用研磨液,进行利用CMP的埋入配线形成时,产生以下的问题:(1)埋入的金属配线的表面中央部分发生各向相同的腐蚀,发生像盘子样的洼下现象(以下称为洼曲);(2)发生来自固体磨粒的研磨伤(擦伤);(3)用于去除残留在研磨后的基体表面的固体磨粒的洗净过程是复杂的;以及(4)起因于固体磨粒本身的成本或废液处理的成本提高等。
为了抑制洼曲或研磨中的铜合金的腐蚀、形成可靠性高的LSI配线,提倡使用含有由甘氨酸等氨基乙酸或者氨基磺酸构成的氧化金属溶解剂和苯并***(以下称为BTA)的金属用研磨液的方法。该技术例如在特开平8-83780号公报中已有记载。
但是,BTA的保护膜形成效果非常高,因而不仅腐蚀速度,而且研磨速度也显著地降低。因此,希望在金属用研磨液中使用充分降低腐蚀速度,而不降低CMP速度的保护膜形成剂。
发明的公开
本发明是提供虽然充分降低腐蚀速度,但维持高的CMP速度,并且能够形成可靠性高的金属膜的埋入图形的金属用研磨液及研磨方法。
本发明的金属用研磨液含有用于氧化金属的氧化剂、氧化金属溶解剂、第1保护膜形成剂、与第1保护膜形成剂不同的第2保护膜形成剂及水。
保护膜形成剂是在金属表面形成保护膜的保护膜形成剂。
作为第1保护膜形成剂,最好是选自氨、烷基胺、氨基酸、亚胺、唑等含氮化合物及其盐,以及硫醇、葡萄糖和纤维素中的至少一种。这些第1保护膜形成剂是通过在金属膜表面物理的吸附和/或形成化学的键而形成保护膜的化合物。
作为第2保护膜形成剂,最好是选自醇(即具有醇性羟基的化合物)、苯酚类(即具有苯酚性羟基的化合物)、酯、醚、多糖类、氨基酸盐、聚羧酸及其盐、乙烯系聚合物、磺酸及其盐、芳香族胺、酰胺、偶氮化合物以及钼化合物中的至少一种。这些第2保护膜形成剂,是辅助第1保护膜形成剂形成保护膜的化合物。
作为氧化剂最好是选自过氧化氢、硝酸、过碘酸钾、次氯酸及臭氧水中的至少一种。
作为氧化金属溶解剂,最好是选自有机酸、有机酸的铵盐以及硫酸中的至少一种。
本发明提供,在不含保护膜形成剂中的第2保护膜形成剂时,相对于表现使腐蚀速度抑制在10nm/min以下的效果所必要的第1保护膜形成剂的添加浓度A,通过添加第2保护膜形成剂,含有低于上述浓度的低浓度的第1保护膜形成剂,能够表现使腐蚀速度抑制在10nm/min以下的效果的金属用研磨液。即,在此情况下,第2保护膜形成剂是为了使腐蚀速度抑制在10nm/min以下所必要的第1保护膜形成剂的添加量减少的化合物。
本发明的研磨方法是在上述本发明的金属用研磨液中通过研磨除去被研磨物表面的金属膜的研磨方法。对于去除对象的金属膜来说,铜、铜合金、铜氧化物、铜合金氧化物等是合适的。因此,本发明提供,使用上述的金属用研磨液,通过研磨含有选自铜、铜合金、铜氧化物和铜合金氧化物中的至少一种金属层的层叠膜构成的金属膜的过程,去除金属膜的至少一部分的研磨方法。
本发明提供,通过组合性质不同的第1和第2保护膜形成剂,既维持CMP速度,又充分降低腐蚀速度的研磨液及使用该研磨液的研磨方法。第1保护膜形成剂可以使用和铜容易生成螯合配位物的化合物,例如使用乙二胺四乙酸、苯并***等。它们的金属表面保护膜形成效果极强,例如在金属用研磨液中,如果含有0.5重量%以上时,不用说铜合金膜被腐蚀,连CMP也丧失。
与此相反,本发明人发现,通过同时使用和第1保护膜形成剂不同的第2保护膜形成剂,降低第1保护膜形成剂的添加浓度时也能够抑制到充分低的腐蚀速度。而且知道,在使用这样的研磨液的情况下,即使腐蚀速度低,也能得到CMP速度不太低这样的最佳特性。除此之外还发现,通过同时使用第1保护膜形成剂和第2保护膜形成剂,在研磨液中不含固体磨粒的前提下,在实用的CMP速度下的研磨成为可能。认为这是因为,与由以往的固体磨粒的摩擦产生的磨去效果相反,发现了由研磨垫的摩擦产生的磨去。
业已知道,作为应该抑制的腐蚀速度的值,如果能够抑制在10nm/min以下,就可以得到最佳的平坦化效果。如果CMP速度的降低是能够允许的范围,希望的是腐蚀速度更低者,如果能够抑制在5nm/min以下,,例如即使进行50%左右的过剩CMP(进行CMP去除金属膜所必要时间的1.5倍的CMP),洼曲也停留在不成为问题的程度。进而,如果腐蚀速度能够抑制在1nm/min以下,即使进行100%以上的过剩CMP,洼曲也不成为问题。
在本说明书中的腐蚀速度,是被研磨物浸渍在研磨液中,在液温25℃,搅拌速度100r/min进行搅拌时的被研磨物表面的金属膜(利用溅射形成的铜膜)被腐蚀的速度,并且是从电阻值换算求出浸渍前后的金属膜厚度差,以浸渍时间除以金属膜厚度差求出的速度。
另外,CMP速度(即化学机械研磨速度),是在研磨压力210g/cm2、被研磨物和研磨底盘的相对速度36m/min、液温25℃的条件下,研磨被研磨物表面的金属膜(利用溅射形成的铜膜),从电阻值换算求出浸渍前后的金属膜厚度差,以处理时间除以膜厚度差求出的速度。
按照本发明,与仅用第1保护膜形成剂的研磨液不同,在不依赖于由固体磨粒产生的强机械摩擦条件下,利用远比上述摩擦柔软的研磨垫的摩擦能够实现CMP平坦化。
进而,本发明提供,使用本发明的金属用研磨液,研磨在表面具有凹部的基体上形成.充填含有铜、铜合金(铜/铬等)等金属膜的基体的研磨方法。如果使用本发明的研磨液将这样的基体进行化学机械研磨(CMP),基体凸部的金属膜就选择性地进行化学机械研磨,在凹部残留金属膜,从而得到所希望的导体图形。在本发明的研磨液中,实质上不含固体磨粒也可以,利用远比固体磨粒柔软的机械研磨垫的摩擦进行化学机械研磨,因而使研磨伤急剧减低。
本发明的金属用研磨液,以氧化剂、氧化金属溶解剂、第1保护膜形成剂、第2保护膜形成剂和水作为必须成分。实质上可以不含固体磨粒,也可以使用。
接着,说明包含在本发明的金属用研磨液中的各成分的具体例。
金属的氧化剂可举出过氧化氢(H2O2)、硝酸、过碘酸钾、次氯酸、臭氧水等。在基体是包含集成电路用元件的硅基板时,希望没有由碱金属、碱土金属、卤化物等产生的污染,因而希望是不含不挥发成分的氧化剂,但由于臭氧水的组成随时间的变化激烈,因此以上列举的氧化剂中,最好是过氧化氢。但是,在使用对象的基体是不含半导体元件的玻璃基板等时,即使是含有不挥发成分的氧化剂,也没关系。
氧化金属溶解剂希望是水溶性的氧化金属溶解剂。在水溶性氧化金属溶解剂中,可举出甲酸、乙酸、丙酸、丁酸、戊酸、2-甲基丁酸、正己酸、3,3-二甲基丁酸、2-乙基丁酸、4-甲基戊酸、正庚酸、2-甲基己酸、正辛酸、2-乙基己酸、苯甲酸、乙醇酸、水杨酸、甘油酸、草酸、丙二酸、琥珀酸、戊二酸、己二酸、庚二酸、马来酸、邻苯二甲酸、苹果酸、酒石酸、柠檬酸等有机酸,这些有机酸的铵盐或过硫酸铵、硝酸铵、氯化铵等铵盐类;硫酸、铬酸等无机酸,以及氨配位物等。它们可以单独使用,也可以组合任一种使用。
对于含有由铜、铜合金、铜氧化物和/或铜合金氧化物构成的金属层的层叠膜来说,其中,甲酸、丙二酸、苹果酸、酒石酸、柠檬酸是合适的。这些酸在得到和后述的第1和第2保护膜形成剂的平衡上是优选的。尤其,就苹果酸、酒石酸、柠檬酸来说,在既维持实用的CMP速度,又能够有效地抑制腐蚀速度方面是优选的。
作为第1保护膜形成剂,可举出氨;二甲胺、三甲胺、三乙胺、丙二胺等烷基胺或乙二胺四乙酸(以下简称为EDTA)、二乙基二硫代氨基甲酸钠及壳聚糖等的胺;氨基乙酸、L-丙氨酸、β-丙氨酸、L-2-氨基丁酸、L-戊氨酸、L-缬氨酸、L-亮氨酸、L-正亮氨酸、L-异亮氨酸、L-别亮氨酸、L-苯基丙氨酸、L-脯氨酸、肌氨酸、L-鸟氨酸、L-赖氨酸、牛磺酸、L-丝氨酸、L-苏氨酸、L-别苏氨酸、L-高丝氨酸、L-酪氨酸、3,5-二碘-L-酪氨酸、β-(3,4-二羟苯基)-L-丙氨酸、L-酪毒素、4-羟基-L-脯氨酸、L-半胱氨酸、L-蛋氨酸、L-乙硫氨酸、L-羊毛硫氨酸、L-胱硫醚、L-胱氨酸、L-磺基丙氨酸、L-天冬氨酸、L-谷氨酸、S-(羧甲基)-L-半胱氨酸、4-氨基丁酸、L-天冬氨酰胺、L-谷氨酰胺、重氮乙酰丝氨酸、L-精氨酸、L-刀豆氨酸、L-瓜氨酸、δ-羟基-L-赖氨酸、肌酸、L-犬尿氨酸、L-组氨酸、1-甲基-L-组氨酸、3-甲基-L-组氨酸、巯组氨酸三甲基内盐、L-色氨酸、放线菌素C1、阿巴安酸(ァパミン)、血管紧张肽I、血管紧张肽II及抗木瓜酶等氨基酸;双硫腙、联喹啉(2,2’-双喹啉)、新联喹啉(2,9-二甲基-1,10-菲绕啉)、巴索联喹啉(2,9-二甲基-4,7-二苯基-1,10-菲绕啉)及球丙拉嗪(キュペラゾン)(双环己酮乙二酰腙)等亚胺;苯并咪唑-2-硫醇、2-[2-(苯并噻唑基)]硫代丙酸、2-[2-(苯并噻唑基)]硫代丁酸、2-巯基苯并噻唑、1,2,3-***、1,2,4-***、3-氨基-1H-1,2,4-***、苯并***、1-羟基苯并***、1-二羟丙基苯并***、2,3-二羧丙基苯并***、4-羟基苯并***、4-羧基-1H-苯并***、4-甲氧基羰基-1H-苯并***、4-丁氧基-1H-苯并***、4-辛氧基羰基-1H-苯并***、5-己基苯并***、N-(1,2,3-苯并***啉基-1-甲基)-N-(1,2,4-***啉基-1-甲基)-2-乙基己胺、甲苯***、萘并***、双[(1-苯并***啉基)甲基]膦酸等唑;壬硫醇、十二烷硫醇、三嗪硫醇、三嗪二硫醇、三嗪三硫醇等硫醇;以及葡萄糖、纤维素等糖类。它们可以单独使用,也可以适当组合使用。
其中,在高的CMP速度和低的腐蚀速度并立方面,以壳聚糖、乙二胺四乙酸、L-色氨酸、球丙拉嗪(キュペラゾン)、三嗪二硫醇、苯并***、4-羟基苯并***、4-羧基-1H-苯并***丁酯、甲苯***及萘并***为佳。尤其,苯并***及其衍生物最佳。对于苯并***衍生物来说,可举出上述的唑等。
作为第2保护膜形成剂,可举出1-丙醇、2-丙醇、2-亚丙基-1-醇、烯丙醇、亚乙基氰醇、1-丁醇、2-丁醇、(S)-(+)-2-丁醇、2-甲基-1-丙醇、叔丁醇、全氟-叔丁醇、巴豆醇、1-戊醇、2,2-二甲基-1-丙醇、2-甲基-2-丁醇、3-甲基-1-丁醇、仲戊醇、1-己醇、4-羟基-4-甲基-2-戊醇、4-甲基-2-戊醇、环己醇、DL-3-己醇、1-庚醇、2-乙基己醇、(S)-(+)-2-辛醇、1-辛醇、DL-辛醇、2-羟基苄醇、2-硝基苄醇、3,5-二羟基苄醇、3,5-二硝基苄醇、3-氟代苄醇、3-羟基苄醇、4-氟代苄醇、4-羟基苄醇、苄醇、间(三氟甲基)苄醇、间氨基苄醇、间硝基苄醇、邻氨基苄醇、邻羟基苄醇、对羟基苄醇、对硝基苄醇、2-(对氟苯基)乙醇、2-氨基苯乙醇、2-甲氧基苄醇、2-甲基-3-硝基苄醇、2-甲基苄醇、2-硝基苯乙醇、2-苯基乙醇、3,4-二甲基苄醇、3-甲基-2-硝基苄醇、3-甲基-4-硝基苄醇、3-甲基苄醇、4-氟代苯乙醇、4-羟基-3-甲氧基苄醇、4-甲氧基苄醇、4-甲基-3-硝基苄醇、5-甲基-2-硝基苄醇、DL-α-羟乙基苯、邻(三氟甲基)苄醇、对(三氟甲基)苄醇、对氨基苯乙醇、对羟苯基乙醇、对甲基苄醇及仲苯乙醇等的醇类;4-甲基苯酚、4-乙基苯酚及4-丙腈苯酚等酚类;甘油酯、脱水三梨糖醇酯、甲氧基乙酸、乙氧基乙酸、3-乙氧基丙酸及丙氨酸乙酯等酯;聚乙二醇、聚丙二醇、聚丁二醇、聚乙二醇烷基醚、聚乙二醇链烯基醚、烷基聚乙二醇、烷基聚乙二醇烷基醚、烷基聚乙二醇链烯基醚、链烯基聚乙二醇、链烯基聚乙二醇烷基醚、链烯基聚乙二醇链烯基醚、聚丙二醇烷基醚、聚丙二醇链烯基醚、烷基聚丙二醇、烷基聚丙二醇烷基醚、烷基聚丙二醇链烯基醚、链烯聚丙二醇、链烯基聚丙二醇烷基醚及链烯基聚丙二醇链烯基醚等醚;藻酸、果酸、羧甲基纤维素、凝多糖(カ-ドラン)及茁霉多糖等多糖类;甘氨酸铵盐及甘氨酸钠盐等氨基酸盐;聚天冬氨酸、聚谷氨酸、聚赖氨酸、聚苹果酸、聚甲基丙烯酸、聚甲基丙烯酸铵盐、聚甲基丙烯酸钠盐、聚酰胺酸、聚马来酸、聚衣康酸、聚富马酸、聚(对苯乙烯羧酸)、聚丙烯酸、聚丙烯酰胺、氨基聚丙烯酰胺、聚丙烯酸铵盐、聚丙烯酸钠盐、聚酰胺酸铵盐、聚酰胺酸钠盐及聚乙醛酸等聚羧酸及其盐;聚乙烯醇、聚丙烯吡咯烷酮及聚丙烯醛等乙烯系聚合物;甲基牛磺酸铵盐、甲基牛磺酸钠盐、硫酸甲基钠盐、硫酸乙基铵盐、硫酸丁基铵盐、乙烯基磺酸钠盐、1-烯丙基磺酸钠盐、2-烯丙基磺酸钠盐、甲氧基甲基磺酸钠盐、乙氧基甲基磺酸铵盐、3-乙氧基丙基磺酸钠盐及磺基琥珀酸钠盐等磺酸及其盐;苯胺、N,N-二甲基苯胺及苄基胺等芳香族胺;丙酰胺、丙烯酰胺、甲基尿素、烟酰胺、琥珀酸酰胺、苯基乙酸酰胺、吡啶-4-カルボキサミド、N’,N-二苄基-L-酒石酸酰胺及磺胺等酰胺;1’,1-偶氮双(环己烷-1-腈)、1’,1-偶氮双(1-乙酰氧基-1-苯基乙烷)、2’,2-偶氮双(2,4-二甲基-戊腈)、2,2’-偶氮双(4-甲氧基-2,4-二甲基-戊腈)、2,2’-偶氮双(异丁酸)二甲酯、2,2’-偶氮双(异丁腈)、2-[2-(3,5-二溴代吡啶基)偶氮]-5-二甲基氨基苯甲酸、4,4’-偶氮双(4-氰基戊酸)、4,4’-氧化偶氮茴香醚、氧化偶氮基甲烷、偶氮基苯、氧化偶氮基苯、偶氮二羧基酰胺、偶氮二羧酸二异丙酯、偶氮二羧酸二(叔丁酯)、吩嗪、孔雀绿、甲基橙、刚果红及龙胆紫等偶氮化合物;及其钼(VI)酸二钠二水合物及七钼(VI)酸六铵四水合物等钼化合物等。这些化合物可以单独使用,也可以适当组合使用。
在所使用的基体是半导体集成电路用硅基板等的情况下,希望没有由碱金属、碱土金属、卤化物等产生的污染,因而希望是酸或其铵盐。但是,在基体是玻璃基板等的情况下,没有该限制。
其中,在高CMP速度和低腐蚀速度并立方面,以2-甲基-3-硝基苄醇、聚丙二醇、聚天冬氨酸、聚苹果酸、聚丙烯酸、聚甲基丙烯酸、聚丙烯酸铵、聚甲基丙烯酸铵、聚酰胺酸、聚酰胺酸铵、聚丙烯酰胺、甲基牛磺酸钠、苄胺、烟酰胺、对氨基苯磺酰胺、刚果红、七钼(VI)酸六铵四水合物为佳,尤其,聚丙烯酸、聚甲基丙烯酸、聚酰胺酸、聚丙烯酸铵、聚甲基丙烯酸铵、聚酰胺酸铵及聚丙烯酰胺最佳。
作为本发明适用的金属膜,是包含选自铜、铜合金、铜氧化物及铜合金氧化物(以下,将这些合并称为铜合金)中的至少一种的层叠膜。
另外,本发明提供CMP速度是100nm/min以上、腐蚀速度是10nm/min以下的金属用研磨液。具有这样特性的研磨液,根据本发明是初次实现,含有金属的氧化剂、氧化金属溶解剂和水,再通过组合第1保护膜形成剂和与该第1保护膜形成剂不同的第2保护膜形成剂而进行配合,就能够完成。
下面,示出以能够使用的第1保护膜形成剂和第2保护膜形成剂的组合作为第1保护膜形成剂/第2保护膜形成剂。这些组合仅是简单的例示,本发明并不受这些组合的限制。根据需要,也可以使用适宜的其他组合。
作为形成CMP速度是100nm/min以上、腐蚀速度是10nm/min以下的组合,例如,可举出球丙拉嗪/聚苹果酸、球丙拉嗪/聚天冬氨酸、球丙拉嗪/聚丙烯酰胺、L-色氨酸/聚丙烯酰胺、L-色氨酸/聚丙烯酸铵、L-色氨酸/聚苹果酸、苯并***/聚丙烯酰胺、苯并***/聚丙烯酸铵、萘并***/聚苹果酸、萘并***/2-甲基-3-硝基苄醇、三嗪二硫醇/聚天冬氨酸、三嗪二硫醇/聚丙烯酰胺等。
另外,作为形成CMP速度是100nm/min以上、腐蚀速度是1nm/min以下的组合,例如,可举出球丙拉嗪/聚丙烯酰胺、L-色氨酸/聚丙烯酰胺、L-色氨酸/聚丙烯酸铵、苯并***/聚丙烯酰胺、苯并***/聚丙烯酸铵、萘并***/聚苹果酸、三嗪二硫醇/聚天冬氨酸、三嗪二硫醇/聚丙烯酰胺等。
作为CMP速度250mm/min以上,腐蚀速度10nm/min以下的组合,可以举出球丙拉嗪/聚苹果酸等。
接着,说明各成分的配合量。
氧化剂成分的配合量,相对于100g的氧化剂、氧化金属溶解剂、第1保护膜形成剂、第2保护膜形成剂及水的总量,较好是0.003mol~0.7mol,更好是0.03mol~0.5mol,特别好是0.2mol~0.3mol。在该配合量不到0.003mol时,金属的氧化是不充分的,因而CMP速度低,如果超过0.7mol,就有研磨面产生表面粗糙的倾向。
在本发明中的氧化金属溶解剂成分的配合量,相对于100g的氧化剂、氧化金属溶解剂、第1保护膜形成剂、第2保护膜形成剂及水的总量,较好是0.~0.005mol,更好是0.00005mol~0.0025mol,特别好是0.0005mol~0.0015mol。该配合量如果超过0.005mol,存在难以抑制腐蚀的倾向。
第1保护膜形成剂的配合量,相对于100g的氧化剂、氧化金属溶解剂、第1保护膜形成剂、第2保护膜形成剂及水的总量,较好是0.0001mol~0.05mol,更好是0.0003mol~0.005mol,特别好是0.0005mol~0.0035mol。在该配合量不到0.0001mol时,存在难以抑制腐蚀的倾向,如果超过0.05mol,就有CMP速度降低的倾向。
第2保护膜形成剂的配合量,相对于100g的氧化剂、氧化金属溶解剂、第1保护膜形成剂、第2保护膜形成剂及水的总量,较好是0.001~0.3重量%,更好是0.003重量%~0.1重量%,特别好是0.01重量%~0.08重量%。在该配合量不到0.001重量%时,存在在控制腐蚀中不能体现和第1保护膜形成剂并用的效果,如果超过0.3重量%,就存在CMP速度降低的倾向。
虽然本发明的研磨液及研磨方法中的效果表现的作用机理尚不清楚,但可以推测为,通过并用第1和第2保护膜形成剂,既抑制腐蚀,又对于由研磨垫产生的摩擦,在不作为金属表面保护膜发生作用下进行CMP。
一般地说,在CMP中,发生研磨伤的程度依存于固体磨粒的粒径或粒径分布或形状,由绝缘膜的磨去引起的膜厚减少(以下,称为磨损)或平坦化效果的劣化,也依存于固体磨粒的粒径或研磨垫的物理性质,在用BTA处理金属膜,尤其是铜膜表面时,认为金属膜的洼曲也依存于研磨垫的硬度或研磨液的化学性质。即,硬的固体磨粒是进行CMP时所必要的,但为了提高CMP中的平坦化效果或CMP面的完全性(没有研磨伤等损伤),是不希望的。业已知道,平坦化效果实际上依赖于比固体磨粒更柔软的研磨垫的特性。
像这样,认为本发明在没有固体磨粒下能够进行CMP这点上,在铜合金的CMP、继而在使用铜合金的CMP的埋入图形的形成中是极希望的。
第1保护膜形成剂具有在金属表面形成牢固的保护膜的作用。例如,如果铜合金膜表面暴露在含有BTA的溶液中时,由于铜(Cu)或者其氧化物BTA的反应,形成以Cu(I)BTA或者Cu(II)BTA的结构为主骨架的聚合物状配位化合物保护膜。该保护膜是相当牢固的,在使用含有0.5重量%BTA的金属用研磨液时,即使在该研磨液中含有固体磨粒,一般也几乎不发生研磨。
另一方面,在不使用第1保护膜形成剂,仅单独使用第2保护膜形成剂调制金属用研磨液时,尤其难以抑制腐蚀速度,保护效果不充分。
像这样,第1保护膜形成剂和第2保护膜形成剂,其作用是不同的,根据保护膜形成剂的种类形成不同种类的保护膜。本发明是基于以下的新认识,即,通过组合使用上述的第1和第2保护膜形成剂,能够使腐蚀速度的抑制和CMP速度维持并立,而且也不需要由固体磨粒产生的强摩擦。
实施发明的最佳方式
以下,根据实施例说明本发明。但本发明不不受这些实施例的限制。
实施例1~12、比较例1~5
研磨液调制方法
在0.15重量份数DL-苹果酸(试剂特级)中加入70重量份数水,并溶解,向其中加入在0.8重量份数甲醇中溶解0.2重量份数第1保护膜形成剂形成的溶液后,再加入0.05重量份数第2保护膜形成剂,最后加入33.2重量份数过氧化氢水(试剂特级,30%水溶液),得到金属用研磨液。在表1中示出在各实施例和比较例中使用的保护膜形成剂。
接着,使用得到的研磨液,研磨被研磨物。研磨条件等如下。
研磨条件
被研磨基板:形成厚1μm的铜膜的硅基板
研磨垫:IC1000(ロデ-ル公司制)
研磨压力:210g/cm2
基体和研磨底盘的相对速度:36m/min
研磨品评价项目
CMP速度:从电阻值换算求出铜膜的CMP前后的膜厚差,除以处理时间而求出CMP速度。处理时间是1分钟。
腐蚀速度:另外准备和上述的被研磨基板相同的基板,在室温(25℃),一边搅拌(搅拌速度100r/min),一边在研磨液中浸渍,从电阻值换算出浸渍前后的铜层膜厚差,除以浸渍时间而求出腐蚀速度。浸渍时间是10分钟。
另外,为了评价实际的CMP特性,在绝缘层中形成深0.5μm的沟,按照公知的溅射方法形成铜膜,再按照公知的热处理埋入的硅基板作为基体使用,进行CMP。通过CMP后的基体的目测、光学显微镜观察及电子显微镜观察确认有无发生磨蚀及研磨伤。其结果,没有看到发生磨蚀及研磨伤。在实施例1~12和比较例1~5中的CMP速度和腐蚀速度的评价结果示于表1中。
表1
第1保护膜形成剂 | 第2保护膜形成剂 | CMP速度 | 腐蚀速度 | |
实施例1 | 球丙拉嗪 | 聚苹果酸 | 281 | 3.5 |
实施例2 | 球丙拉嗪 | 聚天冬氨酸 | 234 | 1.9 |
实施例3 | 球丙拉嗪 | 聚丙烯酰胺 | 187 | 0.3 |
实施例4 | L-色氨酸 | 聚丙烯酰胺 | 219 | 0.9 |
实施例5 | L-色氨酸 | 聚丙烯酸铵 | 210 | 0.7 |
实施例6 | L-色氨酸 | 聚苹果酸 | 252 | 2.2 |
实施例7 | 苯并*** | 聚丙烯酸铵 | 185 | 0.2 |
实施例8 | 苯并*** | 丙烯酰胺 | 196 | 0.4 |
实施例9 | 萘并*** | 聚苹果酸 | 203 | 0.5 |
实施例10 | 萘并*** | 2-甲基-3-硝苄基醇 | 212 | 1.1 |
实施例11 | 三嗪二硫醇 | 聚天冬氨酸 | 186 | 0.4 |
实施例12 | 三嗪二硫醇 | 聚丙烯酰胺 | 224 | 1.0 |
比较例1 | 球丙拉嗪 | (无) | 255 | 15.3 |
比较例2 | L-色氨酸 | (无) | 287 | 10.3 |
比较例3 | 苯并*** | (无) | 93 | 2.4 |
比较例4 | 萘并*** | (无) | 72 | 2.1 |
比较例5 | 三嗪二硫醇 | (无) | 98 | 4.8 |
实施例13
在0.15重量份数DL-苹果酸(试剂特级)中加入70重量份数水,并溶解,向其中加入在0.8重量份数甲醇中溶解0.1重量份数BTA而形成的溶液后,再以0.025重量份数聚丙烯酸铵作为40%水溶液加入,最后加入33.2重量份数过氧化氢水(试剂特级,30%水溶液),得到金属用研磨液。在本实施例中,作为氧化金属溶解剂使用的是水溶性高的有机酸的DL-苹果酸,作为第2保护膜形成剂使用的是水溶性的聚丙烯酸铵盐。
使用该金属用研磨液,在和实施例1相同的条件下进行CMP实验时,CMP速度是287nm/min、腐蚀速度是3.6nm/min都是良好的。但是,关于形成沟图形的基体,比CMP去除规定的厚度所必需的CMP时间要多进行50%的CMP研磨,电子显微镜观察的结果,宽10μm的沟部(成为埋入配线的部分)的洼曲是约200nm。为了将洼曲抑制在100nm以下,需要将过剩CMP时间限制在20%。不发生磨蚀和研磨伤。
实施例14
在0.15重量份数DL-苹果酸(试剂特级)中加入70重量份数水,并溶解,向其中加入在0.8重量份数甲醇中溶解0.2重量份数BTA而形成的溶液后,再以0.125重量份数聚丙烯酸铵盐作为40%水溶液加入,最后加入33.2重量份数过氧化氢水(试剂特级,30%水溶液),得到金属用研磨液。在本实施例中,作为氧化金属溶解剂使用的是水溶性高的有机酸的DL-苹果酸,作为第2保护膜形成剂使用的是水溶性的丙烯酸铵盐。
使用该金属用研磨液,在和实施例1相同的条件下进行CMP实验。其结果,得到CMP速度高到185nm/imn、腐蚀速度低到0.2nm/min的结果。另外,关于实际上形成沟图形的基体,也和上述CMP条件相同地实施CMP,进行像上述的观察时,即便使过剩CMP进行相当50%的时间,洼曲也是50nm以下,也不发生磨蚀及研磨伤。
实施例15
除了使用DL-酒石酸代替DL-苹果酸以外,和实施例14相同地调制金属用研磨液,和实施例1相同地进行CMP实验。其结果,研磨速度高到194nm/min,腐蚀速度是0.8nm/min。另外,将形成和实施例13相同的沟图形的基体进行CMP后,当观察基板时,使过剩CMP研磨进行相当50%的时间时的洼曲是约70nm,不发生磨蚀及研磨伤。
实施例16
除了使用柠檬酸代替DL-苹果酸以外,和实施例13相同地调制金属用研磨液,和实施例1相同地进行CMP实验。其结果,研磨速度高到213nm/min,但腐蚀速度是4.6nm/min,稍差。另外,将形成和实施例13相同的沟图形的基体相当30%的时间过剩CMP研磨后的观察结果,洼曲是约150nm以下,不发生磨蚀及研磨伤。
比较例6
除了不添加聚丙烯酸铵以外,和实施例13相同地调制金属用研磨液,和实施例1相同地进行CMP实验。其结果,CMP速度低到少于140nm/min,腐蚀速度低劣到10.3nm/min。将形成和实施例13相同的沟图形的基体进行相当30%时间的过剩CMP研磨后,观察基体表面的结果,洼曲增加至300nm。没有观察到磨蚀及研磨伤。
比较例7
不使用聚丙烯酸铵,并使苯并***的添加量从0.1重量份数增加到0.2重量份数,除此以外,和实施例13相同地调制金属用研磨液,使用该金属用研磨液进行和实施例1相同的CMP实验。
其结果,腐蚀速度是2.4nm/min,是良好的,但CMP速度低劣到93nm/min。另外,对形成和实施例13相同的沟图形的基体,实施相当30%时间的过剩CMP研磨后,观察基体表面的结果,洼曲是约150nm,不是能够充分满足的值。腐蚀速度低,但CMP速度也低,在CMP中需要长时间。不发生磨蚀及擦伤。
根据这些实施例和比较例已发现,仅将第1保护膜形成剂添加至规定的浓度,通过和第2保护膜形成剂并用,即使是低于第1保护膜形成剂的低浓度,也能够达到抑制在10nm/min以下的腐蚀速度的效果,而且维持高CMP速度。由此可知,抑制洼曲、磨蚀或研磨伤的发生,而且以高的CMP速度形成可靠性高的埋入图形是可能的。
产业上的应用可能性
如上所述,按照本发明,能够使腐蚀速度充分低,并能维持高的CMP速度而形成可靠性高的埋入图形。
Claims (18)
1.一种金属用研磨液,其含有:
氧化剂、
氧化金属溶解剂、
第1保护膜形成剂,其是选自氨、胺、氨基酸、亚胺、唑、硫醇及糖类中的至少一种、
第2保护膜形成剂,其是选自具有醇性或者酚性羟基的化合物、酯、醚、多糖类、氨基酸盐、聚羧酸、聚羧酸盐、乙烯基系聚合物、酰胺、偶氮化合物及钼化合物中的至少一种、
及水。
2.权利要求1所述的金属用研磨液,其中,上述第1保护膜形成剂是选自苯并***及其衍生物中的至少一种。
3.权利要求1所述的金属用研磨液,其中,上述第1保护膜形成剂是通过物理吸附和/或形成化学键而在金属膜表面形成保护膜的化合物。
4.权利要求1所述的金属用研磨液,其中,上述第2保护膜形成剂是选自聚丙烯酸、聚甲基丙烯酸、聚酰胺酸、聚丙烯酸铵、聚甲基丙烯酸铵、聚酰胺酸铵及聚丙烯酰胺中的至少一种。
5.权利要求1所述的金属用研磨液,其中,上述第2保护膜形成剂是辅助第1保护膜形成剂形成保护膜的化合物。
6.权利要求1所述的金属用研磨液,其中,上述第2保护膜形成剂是为了使腐蚀速度抑制在10nm/min以下所必需的第1保护膜形成剂的添加量减少的化合物。
7.权利要求1所述的金属用研磨液,其中,上述第2保护膜形成剂是为了使腐蚀速度抑制在10nm/min以下所必需的第1保护膜形成剂的添加量减少的化合物,且所述的腐蚀速度是在以100rpm的搅拌速度进行搅拌的条件下测定的速度。
8.权利要求1所述的金属用研磨液,其中,上述氧化剂是选自过氧化氢、硝酸、过碘酸钾、次氯酸及臭氧水中的至少一种。
9.权利要求1所述的金属用研磨液,其中,上述氧化金属溶解剂是选自有机酸、有机酸的铵盐及硫酸中的至少一种。
10.权利要求9所述的金属用研磨液,其中,上述氧化金属溶解剂是选自苹果酸、酒石酸、柠檬酸、苹果酸铵、酒石酸铵及柠檬酸铵中的至少一种。
11.权利要求1所述的金属用研磨液,其用于研磨包含铜、铜合金、铜氧化物及铜合金氧化物中的至少任一种的金属。
12.权利要求1所述的金属用研磨液,其不含磨粒。
13.一种研磨方法,其中,研磨液含有:
氧化剂、
氧化金属溶解剂、
第1保护膜形成剂,其是选自氨、胺、氨基酸、亚胺、唑、硫醇及糖类中的至少一种、
第2保护膜形成剂,其是选自具有醇性或者酚性羟基的化合物、酯、醚、多糖类、氨基酸盐、聚羧酸、聚羧酸盐、乙烯基系聚合物、酰胺、偶氮化合物及钼化合物中的至少一种、
及水,
研磨液的化学机械研磨速度是100nm/min以上、腐蚀速度是10nm/min以下,且所述的研磨速度是在研磨压力210g/cm2、基体与研磨底盘的相对速度36m/min的条件下测定的速度,所述的腐蚀速度是在以100rpm的搅拌速度进行搅拌的条件下测定的速度。
14.权利要求13所述的研磨方法,其中,上述腐蚀速度是1nm/min以下。
15.权利要求13所述的研磨方法,其中,上述化学机械研磨速度是250nm/min以上。
16.权利要求13所述的研磨方法,其用于研磨包含铜、铜合金、铜氧化物及铜合金氧化物中的至少任一种的金属。
17.权利要求13所述的研磨方法,其不含磨粒。
18.一种金属用研磨液,其含有通过物理吸附和/或形成化学键在金属膜表面形成保护膜的化合物的第1保护膜;及辅助第1保护膜形成剂形成保护膜的化合物的第2保护膜形成剂,
其中,第1保护膜形成剂是选自氨、胺、氨基酸、亚胺、唑、硫醇及糖类中的至少一种,第2保护膜形成剂是选自具有醇性或者酚性羟基的化合物、酯、醚、多糖类、氨基酸盐、聚羧酸、聚羧酸盐、乙烯基系聚合物、酰胺、偶氮化合物及钼化合物中的至少一种。
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- 1999-08-31 JP JP2000568110A patent/JP3337464B2/ja not_active Expired - Lifetime
- 1999-08-31 KR KR10-2004-7006306A patent/KR100491465B1/ko not_active IP Right Cessation
- 1999-08-31 CN CNB998127760A patent/CN1204602C/zh not_active Expired - Lifetime
- 1999-08-31 WO PCT/JP1999/004694 patent/WO2000013217A1/ja active IP Right Grant
- 1999-08-31 CA CA002342332A patent/CA2342332A1/en not_active Abandoned
- 1999-08-31 AU AU54458/99A patent/AU5445899A/en not_active Abandoned
- 1999-08-31 EP EP99940570.7A patent/EP1137056B1/en not_active Expired - Lifetime
- 1999-08-31 TW TW088114986A patent/TW476777B/zh not_active IP Right Cessation
- 1999-08-31 US US09/763,891 patent/US6896825B1/en not_active Expired - Lifetime
- 1999-08-31 EP EP10168136.9A patent/EP2242091B1/en not_active Expired - Lifetime
- 1999-08-31 CN CNB2005100681600A patent/CN100381537C/zh not_active Expired - Lifetime
-
2001
- 2001-10-15 US US09/976,001 patent/US6899821B2/en not_active Expired - Lifetime
-
2004
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2011
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100381537C (zh) * | 1998-08-31 | 2008-04-16 | 日立化成工业株式会社 | 金属用研磨液及研磨方法 |
CN101440259B (zh) * | 1998-08-31 | 2012-11-21 | 日立化成工业株式会社 | 金属用研磨液及研磨方法 |
Also Published As
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EP1137056A1 (en) | 2001-09-26 |
CN100381537C (zh) | 2008-04-16 |
US20020017630A1 (en) | 2002-02-14 |
CN1680511A (zh) | 2005-10-12 |
AU5445899A (en) | 2000-03-21 |
US6899821B2 (en) | 2005-05-31 |
EP1137056A4 (en) | 2004-09-22 |
WO2000013217A1 (fr) | 2000-03-09 |
TW476777B (en) | 2002-02-21 |
EP2242091A1 (en) | 2010-10-20 |
US20050095860A1 (en) | 2005-05-05 |
EP2242091B1 (en) | 2013-07-31 |
US6896825B1 (en) | 2005-05-24 |
KR20010073037A (ko) | 2001-07-31 |
US8038898B2 (en) | 2011-10-18 |
US8491807B2 (en) | 2013-07-23 |
KR100462132B1 (ko) | 2004-12-17 |
KR100491465B1 (ko) | 2005-05-25 |
CN1325540A (zh) | 2001-12-05 |
EP1137056B1 (en) | 2013-07-31 |
JP3337464B2 (ja) | 2002-10-21 |
CA2342332A1 (en) | 2000-03-09 |
US20120048830A1 (en) | 2012-03-01 |
KR20040058017A (ko) | 2004-07-02 |
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