CN1840624A - 聚合物去除剂 - Google Patents
聚合物去除剂 Download PDFInfo
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- CN1840624A CN1840624A CNA2006100596119A CN200610059611A CN1840624A CN 1840624 A CN1840624 A CN 1840624A CN A2006100596119 A CNA2006100596119 A CN A2006100596119A CN 200610059611 A CN200610059611 A CN 200610059611A CN 1840624 A CN1840624 A CN 1840624A
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- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
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- 229910052737 gold Inorganic materials 0.000 description 1
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- 150000002367 halogens Chemical class 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
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- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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- 239000010937 tungsten Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B43/00—Arrangements for separating or purifying gases or liquids; Arrangements for vaporising the residuum of liquid refrigerant, e.g. by heat
- F25B43/003—Filters
-
- 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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
- H01L21/02063—Cleaning during device manufacture during, before or after processing of insulating layers the processing being the formation of vias or contact holes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
- C09K13/04—Etching, surface-brightening or pickling compositions containing an inorganic acid
- C09K13/08—Etching, surface-brightening or pickling compositions containing an inorganic acid containing a fluorine compound
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/04—Water-soluble compounds
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/2082—Polycarboxylic acids-salts thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/2086—Hydroxy carboxylic acids-salts thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/245—Organic compounds containing halogen containing fluorine
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/33—Amino carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D7/265—Carboxylic acids or salts thereof
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D7/30—Halogenated hydrocarbons
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D7/32—Organic compounds containing nitrogen
- C11D7/3209—Amines or imines with one to four nitrogen atoms; Quaternized amines
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/425—Stripping or agents therefor using liquids only containing mineral alkaline compounds; containing organic basic compounds, e.g. quaternary ammonium compounds; containing heterocyclic basic compounds containing nitrogen
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- G—PHYSICS
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- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/26—Processing photosensitive materials; Apparatus therefor
- G03F7/42—Stripping or agents therefor
- G03F7/422—Stripping or agents therefor using liquids only
- G03F7/426—Stripping or agents therefor using liquids only containing organic halogen compounds; containing organic sulfonic acids or salts thereof; containing sulfoxides
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
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- H01L21/02057—Cleaning during device manufacture
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- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B2400/00—General features or devices for refrigeration machines, plants or systems, combined heating and refrigeration systems or heat-pump systems, i.e. not limited to a particular subgroup of F25B
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Abstract
提供一种用来从电子器件之类的基片上除去等离子体处理后聚合物残余物的组合物。还提供使用该组合物除去等离子体处理后残余物的方法和制造集成电路的方法。
Description
技术领域
本发明一般涉及从基片上除去聚合物材料的领域。具体来说,本发明涉及用来在电子器件制造中,在等离子体处理之后除去聚合物材料的组合物和方法。
背景技术
许多包含聚合物的材料被用于制造集成电路、磁盘驱动器、存储介质器件等之类的电子器件的制造中。这些聚合物材料存在于光刻胶、减反射涂层、通路填充层、蚀刻停止层等中。例如,现代技术使用正性光刻胶材料在基片上通过平板印刷绘制图案,使得该图案能够随后通过蚀刻或其它方法在基片材料中形成。以膜的形式沉积光刻胶,将光刻胶膜曝光于高能辐射之下,从而形成所需的图案。然后使用合适的显影液对曝光的区域进行溶解。通过这种方法在基片上形成图案之后,必须从基片上完全除去光刻胶材料以免对随后的操作或加工步骤造成负面影响或妨碍。
图案形成(或图案转移)技术和聚合物去除技术经常包括一步或多步等离子体处理步骤,例如等离子体蚀刻、活性离子蚀刻、离子铣、等离子体灰化等。这些等离子体处理步骤通常用于制造集成电路和其它电子器件。在这些等离子体处理过程中,通常会除去聚合物材料,但是基片上会残留残余物(包括聚合残余物)。这些“残余物”包括未完全除去的光刻胶(以及其它聚合物材料),残留在接线结构侧壁上或通路之类凹槽内的侧壁聚合物,以及残留在凹槽侧壁和/或底部的有机金属聚合物和金属氧化物。使用常规的光刻胶去除剂无法完全除去这种等离子体后的残余物。例如,目前在极端条件下使用丙酮或N-甲基吡咯烷酮,所述极端条件包括高温和增加循环次数。这些使用条件通常高于溶剂的闪点,给环境、操作人员的健康和安全方面带来了一定的问题。另外,增加加工循环次数会对生产率和生产能力造成负面影响。即使在这种极端的剥离条件下,器件可能仍然不得不进行湿-干-湿剥离过程,即进行湿法剥离,然后清除浮渣(O2等离子体灰化),然后进行湿法清洁。
美国专利第5,792,274号(Tanabe等)揭示了一种聚合物去除组合物,该组合物包含a)氢氟酸与金属游离碱的盐;b)水溶性有机溶剂;c)水;和任选的d)防腐剂,该组合物的pH值为5-8。根据该专利,很重要的是将pH值保持在5-8。该专利揭示的组合物在所有条件下都无法有效地除去等离子体处理后的残余物,而且具有一个或多个以下缺点:处理浴寿命(bath life)短、对pH不稳定、对等离子体处理后的残余物的去除能力差。
另外,其它已知的用于等离子体处理后的残余物去除应用的剥离组合物具有许多缺点,这些缺点包括不希望有的可燃性、毒性、挥发性、气味、需要在例如高达100℃的升高的温度下使用、由于处理规定的材料造成的高成本。高级的下一代半导体器件的一个特别的问题是已知的剥离组合物不能与这些器件中的各种薄膜相容,也就是说,这些已知的剥离组合物会造成这些高级器件中的薄膜、特别是铜,以及低-k介电材料的腐蚀。
对能够有效去除聚合物材料并具有更高环境适用性,不会破坏基片(特别是金属薄膜)的细部和几何结构,不会造成基片腐蚀、尤其是金属薄膜腐蚀,不会蚀刻基片中的介电层的剥离剂和等离子体处理后的残余物去除剂有持续的需要。
发明内容
已惊奇地发现,可以从基片(例如具有介电材料的100%铜基片)上简单而干净地除去等离子体处理后聚合物残余物。根据本发明可以在不腐蚀下面的金属层,特别是铜的条件下除去这些聚合物材料,同时减少或消除对二氧化硅之类的介电材料和氢硅倍半氧烷(silsesquioxane)、甲基硅倍半氧烷、聚亚芳基醚等之类的低介电常数(“低k”)材料的蚀刻。还惊奇地发现含水组合物能够在减少或消除对介电材料的蚀刻的条件下有效去除聚合物材料。
本发明提供一种包含以下组分的组合物:a)氟离子源;b)水;c)选自三卤乙酸、有机多羧酸化合物、有机羟基羧酸化合物和氨基酸的有机酸化合物;以及任选的d)有机溶剂,该组合物的pH值≤4.5。
本发明还提供了一种从基片上除去聚合物材料、特别是等离子体处理后残余物的方法,该方法包括使包含等离子体处理后残余物的基片与上述组合物接触的步骤。
本发明还提供了一种制造集成电路的方法,该方法包括以下步骤:a)在制造集成电路时所用的基片上沉积聚合物材料层;b)对该聚合物材料层进行等离子体处理,产生等离子体处理后残余物;c)使所述等离子体处理后残余物与上述组合物接触。
具体实施方式
在本说明书中,除非上下文另外清楚说明,以下缩写具有以下含义:g=克;℃=摄氏度;=埃;重量%=重量百分数;nm=纳米;mL=毫升;UV=紫外;min.=分钟;PVD=物理气相沉积;DI=去离子的;AF=氟化铵;ABF=氟化氢铵;TMAF=氟化四甲铵;EL=乳酸乙酯;DPM=二丙二醇单甲醚;PGMEA=丙二醇单甲醚乙酸酯;PDO=1,3-丙二醇;MP-二醇=2-甲基-1,3-丙二醇。
在本说明书中,术语“剥离”和“去除”可互换使用。同样的,术语“剥离剂”和“去除剂”可互换使用。“烷基”表示直链的、支链的和环状烷基。术语“取代烷基”表示其一个或多个氢原子被另一取代基替代的烷基,所述取代基是例如但不限于卤素、氰基、硝基、(C1-C6)烷氧基、巯基和(C1-C6)烷硫基。
术语“一个”和“一种”表示单数和复数。所有的百分数均以重量计。所有的数值范围均包括端值而且可以组合。
可用于本发明的组合物包含:a)氟离子源;b)水;c)选自三卤乙酸、有机多羧酸化合物、有机羟基羧酸化合物和氨基酸的有机酸化合物;以及任选的d)有机溶剂,该组合物的pH值≤4.5。可使用许多种氟离子源。在一实施方式中,氟离子源是氢氟酸与金属游离碱的盐。示例性的氟离子源包括,但不限于氟化铵、氟化氢铵、氟化四甲铵、氟化三甲铵、铵-四甲基铵二氟化物(ammonium-tetramethylammoniumbifluoride)和氢氟化单乙醇胺。也可在本发明中使用氟离子源的混合物,例如氟化铵与氟化氢铵的混合物。以组合物的总重量计,氟离子的含量通常为0.01-8重量%。氟离子源可以任意合适的量使用,例如最高为氟离子源在组合物中的溶解度限值。在一个实施方式中,氟离子源的量≥0.05重量%,更优选≥0.1重量%。在另一实施方式中,氟离子源的量≤5重量%,例如0.05-5重量%。氟离子源通常可在市场上购得,例如购自Aldrich(美国维斯康新州,密尔沃基)。可以不经进一步提纯直接使用。
可用于本发明的有机酸为三卤乙酸、有机多羧酸化合物、有机羟基羧酸化合物和氨基酸。示例性的三卤乙酸包括,但不限于三氟乙酸、三氯乙酸和三溴乙酸。术语“多羧酸化合物”表示包含两个或两个以上羧酸基团的有机化合物。“羟基羧酸化合物”表示同时包含至少一个羟基和至少一个羧酸基团的有机化合物。示例性的多羧酸化合物包括,但不限于草酸、丙二酸、马来酸、琥珀酸、戊二酸、己二酸和苯二甲酸。合适的羟基羧酸化合物包括,但不限于羟基乙酸、乳酸、柠檬酸和酒石酸。示例性的氨基酸包括,但不限于亚氨基二乙酸、天冬氨酸、氨基己二酸、丙氨酸、亮氨酸、异亮氨酸、苯基丙氨酸、甘氨酸、半胱氨酸、赖氨酸和缬氨酸。也可将有机酸化合物的混合物用于本组合物。
有机酸化合物的含量可在很大的范围内变化。通常这些化合物的含量要足以使得本发明组合物的清洁能力相对于不含有机酸化合物的组合物有所提高。以组合物总重量计,通常有机酸化合物的含量为0.01-10重量%。更优选有机酸的含量为0.05-8重量%,更加优选为0.1-8重量%,最优选为0.5-5重量%。有机酸通常可从Aldrich之类的各种来源购得,可不经提纯直接使用。
尽管本发明可使用各种合适类型的水,例如去离子水、Milli-Q水、蒸馏水等,但是通常使用去离子水。水的量可以是任意合适的量。水的实际上限约为99.5重量%。以组合物总重量计,水的含量通常为5-95重量%,更优选为5-90重量%,更加优选为10-85重量%。本发明组合物中较高的水含量对于等离子体处理后残余物的去除是特别有用的。
在本组合物中可任选地使用有机溶剂。任何至少是部分水溶性的溶剂均可使用。在一实施方式中,有机溶剂是可与水混溶的。合适的有机溶剂包括,但不限于醇、酯、酮、醚和极性非质子溶剂。也可将有机溶剂的混合物用于本发明。以组合物的总重量计,有机溶剂的用量可为0-90重量%。通常有机溶剂的用量为0-50重量%,更优选为0-35重量%。在一实施方式中,有机溶剂的含量为10-35重量%。在另一实施方式中,有机溶剂≤30重量%。
示例性的醇包括甲醇、乙醇、正丙醇、异丙醇、正丁醇、异丁醇、仲丁醇、和非环多元醇化合物。术语“多元醇化合物”表示具有两个或更多羟基的化合物。示例性的多元醇化合物包括,但不限于脂肪族多元醇化合物,例如(C2-C20)链烷二醇、取代的(C2-C20)链烷二醇、(C2-C20)链烷三醇和取代的(C2-C20)链烷三醇。合适的脂肪族多元醇化合物包括,但不限于二羟基丙烷,例如1,3-丙二醇和丙二醇、二甘醇、二丙二醇、三甘醇、三丙二醇、2-甲基-1,3-丙二醇、丁二醇、戊二醇、己二醇、和甘油。特别有用的脂肪族多元醇化合物是1,3-丙二醇、丙二醇、2-甲基-丙二醇、丁二醇和戊二醇。这些多元醇化合物通常可从Aldrich之类的来源购得,可以不经进一步提纯直接使用。当该组合物中使用多元醇化合物时,以组合物的总重量计,该化合物的用量通常为5-85重量%,更优选为10-70重量%。
可将许多种酯作为有机溶剂用于本组合物。示例性的酯包括,但不限于羧酸烷基酯,例如乙酸乙酯、乙酸丁酯、乙酸戊酯、乳酸乙酯、己二酸乙酯和丙二醇甲醚乙酸酯之类的二醇酯。
任何合适的酮均可用作本发明的有机溶剂。示例性的酮包括,但不限于丙酮、甲基乙基酮和2-庚酮。
可将许多种醚用作本发明的溶剂,这些醚包括,但不限于四氢呋喃和四氢吡喃之类的环醚,以及二醇醚。示例性的二醇醚包括,但不限于二醇单(C1-C6)烷基醚和二醇二(C1-C6)烷基醚,例如,但不限于(C1-C20)链烷二醇(C1-C6)烷基醚和(C1-C20)链烷二醇二(C1-C6)烷基醚。合适的二醇醚包括,但不限于乙二醇单甲醚、二甘醇单甲醚、丙二醇单甲醚、丙二醇二甲醚、丙二醇单正丁醚、二丙二醇单甲醚、二丙二醇二甲醚、二丙二醇单正丁醚和三丙二醇单甲醚。这些二醇醚通常可在市场上购得,可以不经提纯直接使用。以组合物总重量计,本发明组合物中二醇醚的含量通常为5-85重量%,更优选为10-70重量%。
示例性的极性非质子溶剂包括二甲基亚砜、环丁砜、二甲基甲酰胺和二甲基乙酰胺,但是也可使用其它极性非质子溶剂。其它可用于本发明的合适有机溶剂包括,但不限于氨基乙基氨基乙醇之类的氨基醇、碳酸丙二酯之类的碳酸酯、N-甲基吡咯烷酮之类的内酰胺和内酯。
在一实施方式中,该组合物包含一种或多种多元醇化合物以及一种或多种二醇醚。通常一种或多种多元醇化合物与一种或多种二醇醚的比例为1∶5至5∶1。更优选一种或多种多元醇化合物与一种或多种二醇醚的比例为1∶3至3∶1,更加优选为1∶2至2∶1。
本发明的组合物可任选包含一种或多种添加剂。合适的添加剂包括,但不限于缓蚀剂和表面活性剂。能够减少对金属膜层腐蚀的任何缓蚀剂均适用于本发明。合适的缓蚀剂包括,但不限于:邻苯二酚;(C1-C6)烷基邻苯二酚,例如甲基邻苯二酚、乙基邻苯二酚和叔丁基邻苯二酚;苯并***;羟基苯甲醚;(C1-C10)烷基苯并***;羟基(C1-C10)烷基苯并***;2-巯基苯并咪唑;五倍子酸;五倍子酸甲酯和五倍子酸丙酯之类的五倍子酸酯;以及硅酸四甲铵之类的硅酸四(C1-C4)烷基铵。这些缓蚀剂通常可从Aldrich之类的各种来源购得,可不经进一步提纯直接使用。
当在本发明组合物中使用缓蚀剂时,以组合物的总重量计,缓蚀剂的含量通常为0.01-10重量%。缓蚀剂的含量更优选为0.2至5重量%,更加优选为0.5-3重量%,最优选为1.5-2.5重量%。
可将非离子型表面活性剂、阴离子表面活性剂和阳离子表面活性剂用于本发明的组合物。通常使用非离子型表面活性剂。这些表面活性剂通常可在市场上购得。以组合物的总重量计,表面活性剂的用量通常为0.2-5重量%,更优选为0.5-3重量%,更加优选为1-2.5重量%。
本发明特别有用的组合物包含0.05-5重量%的氟离子源、0.1-8重量%的有机酸化合物、0-50重量%的有机溶剂和余量的水。
该组合物的pH值≤4.5。更优选该组合物的pH值≤4,更加优选≤3.5,最优选≤3。在一实施方式中,该组合物的pH值为0-4.5。在另一实施方式中,该组合物的pH值为1-3.5。pH值较低(即酸含量较高)的本发明组合物的清洁能力,高于较高pH值(即较低酸含量)的类似组合物。
本发明的组合物可通过将氟离子源、有机酸化合物、水、任选的有机溶剂和任选的添加剂以任意次序混合制得。在一实施方式中,首先向容器中加入水,然后以任意次序加入余下的组分。
本发明的组合物适合用来从基片上除去等离子体蚀刻后聚合物材料。在等离子体处理(例如等离子体蚀刻、等离子体灰化、离子注入和离子铣削处理)条件下处理过的任何聚合物材料,例如,但不限于光刻胶、焊接掩模、减反射涂层等,均可根据本发明将其从基片上有效地除去。本领域技术人员能够理解,本发明同样适用于除去未进行等离子体处理的聚合物材料。
可以通过使聚合物残余物、特别是等离子体处理后聚合物残余物与本发明组合物接触,从而将其从基片上除去。包括残余物的基片与该组合物接触足够的时间,从而从基片上除去残余物。可通过任何合适的方法使残余物与本发明的组合物接触,例如将基片浸入包含本发明组合物的浴(例如湿化学台(wet chemical bench))中,或者将本发明组合物喷在基片表面上。在使基片与本发明的去除剂组合物接触之后,通常使用例如去离子水对基片进行漂洗,然后通过旋转干燥进行干燥。在将本发明组合物喷在基片上的情况下,喷雾操作通常在喷雾室(例如可购自Semitool,有限公司(Kalispell,Montana)的溶剂清洁喷雾设备)内进行。
该去除剂组合物可在室温下或加热条件下使用。通常本发明的聚合物残余物去除过程可在环境温度下、或在任意温度下进行,例如由室温至80℃,优选20℃-65℃,更优选20℃-50℃下进行。
本发明组合物的另一优点在于,可使用该组合物从具有一层或多层介电层的基片上有效地去除聚合物材料,同时基本不会蚀刻介电材料。通常本发明的组合物能够除去不想要的等离子体处理后残余物,同时对基片上其它材料,例如介电材料、金属线路和阻挡层的蚀刻减小或消除。因此,该组合物适用于许多种用于制造电子器件的材料,例如介电材料,特别是低介电常数(“低-k”)材料,例如,但不限于硅氧烷;二氧化硅;硅倍半氧烷,例如氢硅倍半氧烷、甲基硅倍半氧烷、苯基硅倍半氧烷及其混合物;苯并环丁烯;聚亚芳基醚;聚芳烃;以及氟化硅玻璃。本发明组合物的另一优点是可以在不对金属线路下面的热氧化物层造成蚀刻的前提下从基片上除去等离子体处理后聚合物残余物。
当其它常规剥离剂不能去除等离子体处理后残余物、特别是聚合物残余物时,本发明组合物能够特别有效地除去这些残余物。另外,本发明组合物对包含金属、特别是包含铜和铝的基片基本没有腐蚀性。
在另一实施方式中,该组合物能够高效地除去涂布在难以除去的有机交联聚合减反射涂层(“ARC”)聚合物层上的光刻胶。众所周知,这些ARC是极难通过常规光刻胶剥离剂除去的交联聚合物材料。
为了得到亚半微米几何形状的金属线路和高长度与直径比的通路孔,使用氟化等离子体气体处理远-UV光刻胶和相应的ARC层,例如高密度等离子体蚀刻器使用的等离子体气体。远-UV正性作用光刻胶和ARC聚合物在此条件下高度交联,生成极难通过常规剥离法除去的氟代有机金属聚合物残余物。已惊奇地发现,本发明组合物能够在室温下,以较短的处理时间有效除去这些聚合物残余物。
在一实施方式中,本发明还提供了一种制造集成电路的方法,该方法包括以下步骤:a)在制造集成电路时所用的的基片上沉积聚合物材料层;b)对该聚合物材料层进行等离子体处理,产生等离子体处理后残余物;c)使所述等离子体处理后残余物与上述组合物接触。
因此,本发明的组合物可用于使用苛刻或极端处理条件的其它应用,这些应用是例如,但不限于平板显示器TFT/LCD制造,磁阻和巨型磁阻薄膜头制造,以及读-写器件的制造。本发明组合物对磁阻和巨型磁阻薄膜头制造中所用的金属膜以及其它用来制造半导体材料和电子材料的金属基本是惰性的,所述金属膜是例如,但不限于氧化铝(“Al2O3”)、金(“Au”)、钴(“Co”)、铜(“Cu”)、铁(“Fe”)、铱(“Ir”)、锰(“Mn”)、钼(“Mo”)、镍(“Ni”)、铂(“Pt”)、钌(“Ru”)和锆(“Zr”),所述其他金属是例如,但不限于铜、铝、镍-铁、钨、钛、氮化钛、钽、氮化钽。
以下实施例是为了进一步说明本发明的各方面,但是并非对本发明任何方面的范围构成限制。
实施例
实施例1
将下表中的组分依照所示的量混合,制得组合物。缩写“BTA”表示苯并***,缩写“TBC”表示叔丁基邻苯二酚。各样品的pH值是对其5%的去离子水溶液(即包含5重量%各样品组合物的去离子水溶液)测得的。
样品 | 氟离子源(重量%) | 去离子水(重量%) | 1,3-丙二醇(重量%) | DPM(重量%) | 有机酸(重量%) | 其它组分(重量%) | pH |
1 | ABF(0.13) | 72.87 | 12.5 | 12.5 | 柠檬酸(2) | - | 3.6 |
2 | ABF(0.13) | 73.5 | 12.5 | 12.5 | 草酸(1.3) | - | 2.5 |
3 | ABF(0.18) | 55.12 | 22 | 22 | 草酸(0.7) | - | 2.6 |
对比1 | ABF(0.65)AF(1.15) | 32.1 | 32.1 | 32.1 | - | BTA(1)TBC(1) | 3.8 |
对比2 | ABF(0.13) | 70.87 | 12.5 | 12.5 | 乙酸(4) | - | 4.9 |
对比3 | - | 96.9 | 0 | 0 | 草酸(3.4) | - | 1.2 |
实施例2
使用实施例1的样品清洁硅晶片(约2.5×2.5厘米),该硅晶片包括双镶嵌结构,此结构具有碳掺杂的氧化物介电材料和铜,在介电材料上有原硅酸四乙酯(“TEOS”)层,在TEOS层上有TiN层,该硅晶片还具有等离子体后的灰残余物。在室温下(约20℃)将晶片浸入装有实施例1的一种样品的烧杯内。浸入3分钟后,从烧杯取出晶片,用去离子水洗涤并干燥。观察清洁晶片的扫描电子显微照片(SEM),结果列于下表。根据目视观察比较晶片的SEM照片与清洁前的SEM照片,得到残余物的去除百分数。观察SEM图像测定覆盖层的蚀刻。
样品 | 去除残余物(%) | 覆盖层蚀刻(纳米) |
1 | 80 | 5 |
2 | 90 | 0 |
3 | 100 | 2 |
对比1 | 10 | 60 |
对比2 | 40 | 5 |
对比3 | 0 | 0 |
从这些结果可以清楚地看出,本发明组合物能够有效地去除等离子体处理后残余物。覆盖层的蚀刻速率较低说明其下层腐蚀(undercutting)较少。
实施例3
使用下表所述的样品对包含热生长的氧化铜膜(约380)的硅晶片(约2.5×2.5厘米)进行清洁。在室温下,将晶片在烧杯内的各样品中浸没下表所示的时间。浸没了合适的时间后,从烧杯取出各样品,用去离子水漂洗,然后干燥。对比样品中所用的有机溶剂是PDO和DPM为1∶1(重量比)的混合物。
使用常规的反射仪在408纳米测定各晶片的反射率。对反射仪进行校准,使得清洁的酸洗的纯铜(不含氧化物)的反射率为100%。使用校准的反射仪测得,未处理的氧化铜的反射率为2%。
样品 | 配方 | 1分钟 | 2分钟 | 3分钟 | 4分钟 |
3 | 见实施例1 | 100% | 100% | 100% | 100% |
对比4 | ABF(0.178);水(62.3);有机溶剂(37.5) | 93% | 100% | 100% | 100% |
对比5 | ABF(0.178);水(55.8);有机溶剂(44) | 70% | 90% | 93% | 100% |
对比6 | ABF(0.18);水(49.8);有机溶剂(50) | 45% | 80% | 85% | 93% |
对比7 | AF(3.25);水(25);有机溶剂(67.8);BTA(4) | 7% | 10% | 18% | 22% |
从上面数据可以清楚地看出,本发明组合物能够有效除去金属氧化物。
实施例4
在室温下将硅晶片(约2.5×2.5厘米)浸入装有实施例1样品3的烧杯内。该晶片具有如下表所示的不同顶层材料。浸没3分钟后,从烧杯内取出晶片,用去离子水漂洗并干燥。通过扫描电子显微镜法评估清洁的晶片,以测定已被去除剂制剂蚀刻的顶层的量。结果列于下表。
晶片上的顶层 | 蚀刻速率(/分钟) |
电镀铜 | 3.0 |
PVD铜 | 4.0 |
TEOS | 4.4 |
氟化硅玻璃 | 7.3 |
碳掺杂的氧化物介电材料 | 0 |
氮化钛(“TiN”) | 0 |
上面数据清楚地说明,该组合物具有极低的蚀刻速率。
实施例5
预期下表的组合物具有与实施例1的组合物类似的效果。
样品 | 氟离子源(重量%) | 去离子水(重量%) | 有机溶剂(重量%) | 有机酸(重量%) | 其它组分(重量%) |
4 | ABF(0.5) | 62 | DPM(15)MP-二醇(20) | 柠檬酸(2.5) | - |
5 | ABF(0.1)AF(1.5) | 70.9 | PDO(25) | 天冬氨酸(2.5) | - |
6 | AF(2) | 55 | PGMEA(12)EL(29) | 丙二酸(1.3) | 非离子型表面活性剂(0.7) |
7 | AF(2.1) | 69.8 | MP-二醇(23) | 酒石酸(5) | 五倍子酸(0.1) |
8 | ABF(0.75) | 79.25 | PDO(16.5) | 草酸(1.5)甘氨酸(2) | - |
9 | TMAF(0.7)AF(2.2) | 94.6 | 0 | 草酸(0.5)柠檬酸(2) | - |
10 | AF(3.5) | 93 | 0 | 天冬氨酸(3.5) | - |
11 | AF(3.7) | 92 | 0 | 三氟乙酸(4.3) | - |
Claims (9)
1.一种组合物,该组合物包含:a)氟离子源;b)水;c)选自三卤乙酸、有机多羧酸化合物、有机羟基羧酸化合物和氨基酸的有机酸化合物;以及任选的d)有机溶剂,该组合物的pH值≤4.5。
2.如权利要求1所述的组合物,其特征在于,所述氟离子源选自氟化铵、氟化氢铵、氟化四甲铵、氟化三甲铵、铵-四甲基铵二氟化物、氢氟化单乙醇胺及其混合物。
3.如权利要求1所述的组合物,其特征在于,所述有机酸化合物选自草酸、丙二酸、马来酸、琥珀酸、戊二酸、己二酸、苯二甲酸、羟基乙酸、乳酸、柠檬酸、酒石酸、亚氨基二乙酸、天冬氨酸、氨基己二酸、丙氨酸、亮氨酸、异亮氨酸、苯基丙氨酸、甘氨酸、半胱氨酸、赖氨酸、缬氨酸、和它们的混合物。
4.如权利要求1所述的组合物,其特征在于,所述pH值≤4。
5.如权利要求1所述的组合物,该组合物还包含一种或多种缓蚀剂和表面活性剂。
6.如权利要求1所述的组合物,其特征在于,所述有机溶剂选自醇、酯、酮、醚、极性非质子溶剂、氨基醇、碳酸酯、内酰胺和内酯。
7.如权利要求1所述的组合物,该组合物还包含多元醇化合物和二醇醚。
8.一种用来从基片上除去残余物的方法,该方法包括以下步骤:使包含等离子体处理后残余物的基片与权利要求1所述的组合物接触。
9.一种制造集成电路的方法,该方法包括以下步骤:a)在制造集成电路时所用的的基片上沉积聚合物材料层;b)对该聚合物材料层进行等离子体处理,产生等离子体处理后残余物;c)使所述等离子体处理后残余物与权利要求1所述的组合物接触。
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CN106227004B (zh) * | 2016-09-19 | 2019-07-16 | 江阴江化微电子材料股份有限公司 | 一种铜或铜合金布线用水系光阻剥离液 |
CN106833962A (zh) * | 2016-12-26 | 2017-06-13 | 上海申和热磁电子有限公司 | 用于去除半导体蚀刻腔体陶瓷涂层零件污染物的清洗剂及其制备和应用 |
CN108080334A (zh) * | 2018-01-22 | 2018-05-29 | 安徽神舟飞船胶业有限公司 | 一种使得粘贴于机器表面的玻璃胶易被清理的方法 |
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KR20060097658A (ko) | 2006-09-14 |
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TW200641562A (en) | 2006-12-01 |
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