CN101384694B - 用于微电子基板的稳定的非水清洁组合物 - Google Patents
用于微电子基板的稳定的非水清洁组合物 Download PDFInfo
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- CN101384694B CN101384694B CN2007800056626A CN200780005662A CN101384694B CN 101384694 B CN101384694 B CN 101384694B CN 2007800056626 A CN2007800056626 A CN 2007800056626A CN 200780005662 A CN200780005662 A CN 200780005662A CN 101384694 B CN101384694 B CN 101384694B
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- pyridone
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- ZCOTXWSIYQQOQZ-UHFFFAOYSA-N OCCC[NH3+].C[NH+](C)C.[OH-].[OH-] Chemical compound OCCC[NH3+].C[NH+](C)C.[OH-].[OH-] ZCOTXWSIYQQOQZ-UHFFFAOYSA-N 0.000 description 1
- YNYNWYITBQVUSQ-UHFFFAOYSA-N OCC[NH3+].C[NH+](C)C.[OH-].[OH-] Chemical compound OCC[NH3+].C[NH+](C)C.[OH-].[OH-] YNYNWYITBQVUSQ-UHFFFAOYSA-N 0.000 description 1
- ATTZFSUZZUNHBP-UHFFFAOYSA-N Piperonyl sulfoxide Chemical compound CCCCCCCCS(=O)C(C)CC1=CC=C2OCOC2=C1 ATTZFSUZZUNHBP-UHFFFAOYSA-N 0.000 description 1
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- MVODYHNNAZGTGC-UHFFFAOYSA-N [OH-].OC(CC[NH3+])C.C[NH+](C)C.[OH-] Chemical compound [OH-].OC(CC[NH3+])C.C[NH+](C)C.[OH-] MVODYHNNAZGTGC-UHFFFAOYSA-N 0.000 description 1
- FWEFHQSWBIEPQA-UHFFFAOYSA-N [OH-].OCCCC[NH3+].C[NH+](C)C.[OH-] Chemical compound [OH-].OCCCC[NH3+].C[NH+](C)C.[OH-] FWEFHQSWBIEPQA-UHFFFAOYSA-N 0.000 description 1
- PXAJQJMDEXJWFB-UHFFFAOYSA-N acetone oxime Chemical compound CC(C)=NO PXAJQJMDEXJWFB-UHFFFAOYSA-N 0.000 description 1
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- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
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- 125000003354 benzotriazolyl group Chemical class N1N=NC2=C1C=CC=C2* 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- KTDMLSMSWDJKGA-UHFFFAOYSA-M methyl(tripropyl)azanium;hydroxide Chemical compound [OH-].CCC[N+](C)(CCC)CCC KTDMLSMSWDJKGA-UHFFFAOYSA-M 0.000 description 1
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- DZLFLBLQUQXARW-UHFFFAOYSA-N tetrabutylammonium Chemical compound CCCC[N+](CCCC)(CCCC)CCCC DZLFLBLQUQXARW-UHFFFAOYSA-N 0.000 description 1
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- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
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- HPWUYZIJILJHNG-UHFFFAOYSA-M tributyl(2-hydroxyethyl)azanium;hydroxide Chemical compound [OH-].CCCC[N+](CCO)(CCCC)CCCC HPWUYZIJILJHNG-UHFFFAOYSA-M 0.000 description 1
- GFVKHYGXCQWRON-UHFFFAOYSA-N tributyl(ethyl)azanium Chemical compound CCCC[N+](CC)(CCCC)CCCC GFVKHYGXCQWRON-UHFFFAOYSA-N 0.000 description 1
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- GRNRCQKEBXQLAA-UHFFFAOYSA-M triethyl(2-hydroxyethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CCO GRNRCQKEBXQLAA-UHFFFAOYSA-M 0.000 description 1
- JAJRRCSBKZOLPA-UHFFFAOYSA-M triethyl(methyl)azanium;hydroxide Chemical compound [OH-].CC[N+](C)(CC)CC JAJRRCSBKZOLPA-UHFFFAOYSA-M 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Classifications
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/50—Solvents
- C11D7/5004—Organic solvents
- C11D7/5009—Organic solvents containing phosphorus, sulfur or silicon, e.g. dimethylsulfoxide
-
- 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/06—Hydroxides
-
- 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
-
- 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
-
- 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
- G03F7/426—Stripping or agents therefor using liquids only containing organic halogen compounds; containing organic sulfonic acids or salts thereof; containing sulfoxides
-
- 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
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
-
- C11D2111/22—
-
- 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3281—Heterocyclic compounds
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Abstract
用于清洁微电子设备的非水剥离和清洁组合物，所述组合物具有至少一种有机含硫极性化合物作为剥离溶剂，至少一种无水的强氢氧化物碱源，和至少一种羟基吡啶稳定剂以抑制有害的副反应。
Description
发明领域
本发明涉及用于微电子基板(substrate)的稳定的清洁和剥离组合物，且尤其用于从有图案的微电子基板上清洁大块光致抗蚀剂、未灰化的聚合物残余物，和灰化的残余物，而具有相当低的或基本上没有金属腐蚀。而本发明在从铝基和铜基微电子设备部件上清洁聚合物中尤其有效，而不会造成不适当的铝或铜的腐蚀，本发明也有效用于从其它微电子应用中去除聚合物而保护金属和基板不被腐蚀。本发明的方法有效用于清洁和保护硬盘生产中所用的物质(使用Fe、Co、Ni和Cr金属的合金)、晶圆凸点方法中所用的物质(例如PbSn、InSn、和其它无Pb-焊料)、前沿的线加工最后所用的物质(SiGe，各种金属闸门)、和化合物半导体。本发明还涉及这样的清洁组合物，所述清洁组合物也能够从其它通道和从金属线清洁灰化后残余物，以及从微电子基板清洁或剥离未灰化的光致抗蚀剂。本发明的另一方面为从微电子部件清洁或剥离光致抗蚀剂和残余物的方法，尤其是含铝微电子部件，而不引起在许多微电子方法中发现的不适当的金属腐蚀。
发明背景
已经提出了许多用于微电子制造的光致抗蚀剂剥离剂和残余物移除剂。微电子设备构造的许多阶段涉及光致抗蚀剂的薄膜，所述光致抗蚀剂沉积在基板材料上并形成图案以产生设计电路。使用等离子蚀刻气体或基于溶剂的化学蚀刻，所产生的图案用于成形基底材料，所述材料可为电介质层或金属层。蚀刻步骤后，抗蚀剂掩模必须从基板被保护的区域去除，使得可以进行下步操作。所述光致抗蚀剂可以直接通过湿的化学剥离剂去除，或通过灰化大块材料然后去除残余物以大量去除。发现用于移除大块抗蚀剂和灰化残余物的清洁组合物是有吸引力的。蚀刻方法可以改变大块聚合物，增加交联和使得抗蚀剂更难以去除。当灰化步骤部分或不完全的时候，可能产生相似的交联，并且在特定侧壁上的灰化残余物可能难以去除。而且，清洁溶液必须提供合适的清洁同时防止所有暴露的金属和电介质不被腐蚀或蚀刻。这在要求与许多材料同时相容(各材料具有独特的相容性要求)的微电子开发中是尤其感兴趣的。
已经提出了许多用于从此类微电子基板上移除交联的和硬化的光致抗蚀剂和其它残余物(如蚀刻后残余物)的碱性微电子剥离和清洁组合物。然而，此类剥离和清洁组合物的一个问题是使用这些清洁组合物可能产生金属腐蚀。这种腐蚀导致触须线、点蚀、金属线的切蚀，和金属从合金中的选择性损失，这至少部分是由于设备基板中的金属与所用的碱性剥离剂反应。一种这样的碱性微电子剥离和清洁组合物描述于美国专利5,308,745。而该专利的剥离和清洁组合物已经被商业上用于从基板上剥离硬化的和交联的光致抗蚀剂，已经发现用该专利的清洁组合物清洁具有多种暴露的金属层的微电子基板导致了明显的金属腐蚀或对抗蚀剂或残余物清洁不足。
因此，需要能够有效移除大块残余抗蚀剂和灰化的残余物且不产生任何明显由于剥离和清洁组合物的金属腐蚀或基板腐蚀的微电子剥离和清洁组合物。也需要这样的组合物，其提供对于在相同清洁步骤中暴露于清洁化学物质的微电子生产中存在的许多物质的腐蚀保护。
发明简述
根据本发明，提供了用于清洁微电子设备的非水剥离和清洁组合物，所述组合物包含：至少一种有机含硫极性化合物作为剥离溶剂，至少一种无水的强氢氧化物碱源，和至少一种羟基吡啶稳定剂以抑制有害的副反应。其它任选成分，例如，共溶剂、表面活性剂(surfactant)或表面活性试剂(surface-aciveagent)、金属螯合或络合剂，和腐蚀抑制剂也可存在于本发明的非水剥离和清洁组合物中。
本发明用于清洁微电子设备的非水剥离和清洁组合物将优选包含液体亚砜如二甲亚砜(DMSO)、液体砜如环丁砜，或其混合物作为含硫极性化合物，作为剥离溶剂，基于组合物的重量，其量为约20wt％至约99wt％；基于组合物的重量，作为强氢氧化物碱的碱金属金属氢氧化物、氢氧化铵或氢氧化季铵为约0.5wt％至约20wt％；和基于组合物的重量，2-或4-羟基吡啶或其混合物的量为约0.01wt％至约5wt％。
根据本发明用于清洁微电子设备的方法包括用于清洁微电子设备而不产生任何明显的金属腐蚀的方法，所述方法包含将微电子设备与非水清洁组合物接触足够的时间以清洁所述设备，其中所述清洁组合物包含至少一种有机含硫极性化合物作为剥离溶剂，至少一种无水的强氢氧化物碱源，和至少一种羟基吡啶稳定剂，且任选包含其它成分，例如，共溶剂、表面活性剂或表面活性试剂、金属络合或螯合剂和腐蚀抑制剂。
发明和优选实施方案详述
本发明用于清洁微电子设备的非水剥离和清洁组合物包含至少一种有机含硫极性化合物作为剥离溶剂，至少一种无水的强氢氧化物碱源，和至少一种羟基吡啶作为稳定剂以抑制有害的副反应。其它任选成分，例如，共溶剂、表面活性剂或表面活性试剂、金属络合或螯合剂和腐蚀抑制剂也可以存在于本发明的非水剥离和清洁组合物。
任何合适的有机含硫剥离溶剂极性化合物可以用于本发明组合物。这些合适的有机含硫极性化合物的实例包括，但不限于，液体二烷基亚砜和液体砜等，尤其是二甲亚砜和环丁砜。这些化合物包括，例如下式的砜，R1-S(O)(O)-R2，其中R1和R2为1-4个碳原子的烷基；下式的液体亚砜R1-S(O)-R2，其中R1和R2为1-4个碳原子的烷基，所述亚砜如二甲亚砜(DMSO)；和环状亚砜和砜化合物，例如环丁砜(四氢噻吩-1，1-二氧化物)等。这些有机含硫极性化合物存在于组合物中的量，基于所述组合物的重量，为约20wt％至约99wt％，优选约25wt％至约90wt％，更优选约50wt％至约90wt％。
任何合适的非水强氢氧化物碱可以用于本发明的组合物。这些合适的非水强氢氧化物碱的实例包括，但不限于，碱金属氢氧化物、氢氧化铵和氢氧化季铵。优选不含金属的碱，且季铵碱，尤其是氢氧化四烃基铵(tetraalkylammonium hydroxides)如氢氧化四甲基铵等是更优选的。所述碱优选氢氧化季铵，如氢氧化四烃基铵(包括含羟基-和烷氧基-的烷基(在所述烷基或烷氧基中通常具有1-4个碳原子)，还包括苄基)。最优选为氢氧化四甲基铵和三甲基-2-羟基乙基氢氧化铵(胆碱)。其它可用的氢氧化季铵的实例包括：氢氧化三甲基-3-羟基丙基铵、氢氧化三甲基-3-羟基丁基铵、氢氧化三甲基-4-羟基丁基铵、氢氧化三乙基-2-羟基乙基铵、氢氧化三丙基-2-羟基乙基铵、氢氧化三丁基-2-羟基乙基铵、氢氧化二甲基乙基-2-羟基乙基铵、氢氧化二甲基二-(2-羟基乙基)铵、氢氧化单甲基三乙醇铵、氢氧化四乙基铵、氢氧化四丙基铵、氢氧化四丁基铵、氢氧化四乙醇铵、氢氧化单甲基三乙基铵、氢氧化单甲基三丙基铵、氢氧化单甲基三丁基铵、氢氧化单乙基三甲基铵、氢氧化单乙基三丁基铵、氢氧化二甲基二乙基铵、氢氧化二甲基二丁基铵、氢氧化苄基三甲基铵等，及其混合物。在组合物所用的至少一种非水强氢氧化物碱，基于所述组合物的重量，一般为约0.5wt％至约20wt％，优选约0.5wt％至约10wt％，且更优选约0.5wt％至约5wt％。
任何合适的羟基吡啶化合物可以在本发明的组合物中用作稳定剂成分。这些合适的羟基吡啶的实例可以为2-、3-和4-羟基吡啶。所述羟基吡啶优选为2或4-羟基吡啶，更优选为2-羟基吡啶。本发明组合物中的羟基吡啶化合物的量，基于所述组合物的重量，一般为约0.01wt％至约5wt％，优选为约0.01wt％至约2wt％，且更优选为约0.01wt％至约0.5wt％，该组合物的羟基吡啶成分作为稳定剂存在，且认为其通过阻止强氢氧化物碱与含硫有机溶剂成分反应提供了对所述组合物的稳定作用。不存在羟基吡啶稳定剂时，所述组合物的pH (通常为约12)将下降，且所述组合物会改变颜色并失去清洁作用。
所述术语“非水(non-aqueous)”是指在组合物中存在的水不超过约2％，优选水少于约1％，且更优选水为0.5％至基本上不含水。
任何合适的有机共溶剂化合物任选可以包含在本发明的组合物中，通常作为非水强氢氧化物碱的载体或改善组合物的总溶剂的性质的化合物。这些共溶剂包括，但不限于，脂肪醇和多元醇，以及它们的醚，如甲醇、乙二醇、丙二醇、二乙二醇、二乙二醇单烷基醚(如下式HOCH2.CH2-O-CH2-CH2-O-R，其中R为1-4个碳原子的烷基)，尤其是二乙二醇单乙基醚等，烷基酯(如乙酸1-甲氧基-2-丙基酯和γ-丁内酯等)，和其它非质子溶剂。所述共溶剂成分，如果存在的话，基于所述组合物的总重量，可以为约0.1wt％至约30wt％，优选最多25wt％，和更优选最多20wt％。
本发明的组合物也可任选含有其它附加成分。这些任选附加成分包括金属络合或螯合剂、腐蚀抑制化合物，和表面活性剂或表面活性试剂。
不需要有机或无机螯合或金属络合剂，但其可以任选包含在本发明的组合物中，且提供了明显的益处，例如当加入到本发明的非水清洁组合物时，增强了产物的稳定性。合适的螯合或络合剂的实例包括，但不限于，反-1，2-环己烷二胺四乙酸(CyDTA)、乙二胺四乙酸(EDTA)、锡酸盐、焦磷酸盐、亚烷基-二膦酸衍生物(如，1-羟基-亚乙基-1，1-二膦酸盐(ethane-1-hydroxy-1，1-diphosphonate))、含乙二胺的膦酸盐、二亚乙基三胺或三亚乙基四胺官能部分[如，乙二胺四(亚甲基膦酸)(EDTMP)、二亚乙基三胺五(亚甲基膦酸)、三亚乙基四胺己(亚甲基膦酸)。金属络合或螯合剂，如果在组合物中存在，基于所述组合物的重量，存在的量为0.1wt％至约5wt％，优选为约0.1至约2wt％。
本发明的非水清洁组合物也可任选含有其它腐蚀抑制剂和微电子清洁组合物中所用的相似的非腐蚀成分。所述化合物可以包括，但不限于，间苯二酚、没食子酸、没食子酸丙基酯、连苯三酚、对苯二酚、苯并三唑和苯并三唑衍生物。这些其它腐蚀抑制剂，基于所述组合物的重量，可以以任何合适的量存在，通常为约0.1wt％至约5wt％，优选约0.1wt％至约3wt％，且更优选约0.2wt％至约2wt％。
本发明的组合物也可以任选含有任何合适的两性、非离子、阳离子或阴离子表面活性试剂或表面活性剂。加入表面活性剂会降低制剂的表面张力并增加将被清洁的表面的润湿，且因此提高了组合物的清洁作用。而且，表面活性剂的性质可以辅助颗粒分散、促进更好的清洁。任何合适的两性、阳离子或非离子表面活性可以用于本发明的组合物中。尤其合适的表面活性剂的实例包括，但不限于，3，5-二甲基-1-己炔-3-醇(Surfynol-61)，乙氧基化的2，4，7，9-四甲基-5-癸炔-4，7-二醇(Surfynol-465)、聚四氟亚乙基十六烷氧基丙基甜菜碱(polytetrafluoroethylene cetoxypropylbetaine)(Zonyl FSK)、Zonyl FSH、Triton X-100，即辛基苯氧基聚乙氧基乙醇，等。所述表面活性剂，如果存在于组合物中，基于所述组合物的重量，一般存在的量为0.1wt％至约5wt％，优选0.001wt％至约3wt％。
本发明优选的组合物包括约72wt％的DMSO、18wt％的环丁砜、1.4wt％的氢氧化四甲基铵，8.1％的丙二醇和0.5wt％的2-羟基吡啶的组合物。本发明的另一种组合物包括66％的DMSO、17.4％的环丁砜、14％的丙二醇、2.4％的TMAH和0.2％的2-羟基吡啶的组合物。
本发明的组合物和它们作为清洁组合物用于清洁微电子设备的效果通过下述实施例说明。
实施例1
下述测试证明了羟基吡啶稳定添加剂对制剂的必要性。溶液1含有(重量)：66％的DMSO、22％的环丁砜、11.2％的丙二醇和0.8％的TMAH。溶液2含有：66％的DMSO、22％的环丁砜、10.2％的丙二醇和1.8％的TMAH。如下所示，向这些溶液中加入0.5％的2-羟基吡啶(HP)。将每种溶液加热至85℃，并实时监测。在不稳定的浴液(bath)中(不含羟基吡啶的浴液)，pH下降通过浴液颜色的改变表示。在该pH值或该pH以下，浴液不能表现出有效的清洁作用。
表1
| 溶液 | 在85℃下的时间 | 浴液颜色 |
| 溶液1 | 0小时 | 浅黄色 |
| 溶液1 | 2小时 | 浅黄色 |
| 溶液1 | 4小时 | 褐色 |
| 溶液1+0.5％2-HP | 0小时 | 浅黄色 |
| 溶液1+0.5％2-HP | 2小时 | 浅黄色 |
| 溶液1+0.5％2-HP | 4小时 | 浅黄色 |
| 溶液1+0.5％2-HP | 7小时 | 浅黄色 |
| 溶液1+0.5％2-HP | 22小时 | 浅黄色 |
| 溶液2 | 0小时 | 黄色 |
| 溶液2 | 2小时 | 黄色 |
| 溶液2 | 4小时 | 褐色 |
| 溶液2+0.5％2-HP | 0小时 | 黄色 |
| 溶液2+0.5％2-HP | 2小时 | 黄色 |
| 溶液2+0.5％2-HP | 4小时 | 黄色 |
| 溶液2+0.5％2-HP | 7小时 | 黄色 |
| 溶液2+0.5％2-HP | 22小时 | 黄色 |
实施例2
下述测试证明了本发明的新的和不可预料的方面，其与David Skee的美国专利6,599,370和6,585,825公开的内容相关。在Skee的专利中，公开了许多化合物作为用于含有TMAH和无金属硅酸盐的水溶液的有效浴液寿命延长剂(bath life extender)。Skee的专利中延长浴液寿命的化合物在那些水性组合物中作为缓冲剂使用。然而，本发明的组合物为非水组合物，且因此羟基吡啶稳定化合物并不能起缓冲剂的作用。因此，惊奇的发现羟基吡啶化合物能够作为本发明非水组合物中的稳定剂，相反Skee专利中的其它缓冲剂不能起相同的作用，这通过表2中表明的结果来证明。对于每次测试，将从上述得到的溶液2(66％的DMSO、22％的环丁砜、10.2％的丙二醇和1.8％的TMAH)与各种添加剂组合，使得添加剂为总溶液重量的1％。然后将溶液再在85℃下加热24小时。如果24小时浴液颜色没有改变或pH没有低于11说明添加剂的作用很好，如果浴液在7-24内稳定说明添加剂的作用中等，且如果浴液在小于7小时改变说明添加剂的作用很差。
表2
| 添加的化合物 | 结果 |
| 抗坏血酸 | 差 |
| 丙酮肟 | 差 |
| 间苯二酚 | 差 |
| 2-羟基吡啶 | 好 |
| 2-甲基间苯二酚 | 差 |
| 4-羟基吡啶 | 中 |
| 糖精 | 差 |
实施例3
制备清洁溶液(溶液3)，该清洁溶液含有约：66％的DMSO、17.4％的环丁砜、14％的丙二醇、2.4％的TMAH和0.2％的2-羟基吡啶。将具有“穿通(punch-through)”通道结构(从Si和TiN至Al层的蚀刻通道)的具有图形的Al技术晶片样品置于这些加热至表3中所述的温度的溶液中10分钟，然后除去溶液，用DI水淋洗2分钟，然后用氮气吹干。作为比较，将相同的晶片在ALEG-625(J.T.Baker)中清洁，所述ALEG-625为市售的其它相似组合物的半水性产品(含有DMSO、环丁砜、TMAH和水)。然后评估清洁后晶片的灰化残余物的移除率(0-100％移除)和铝的腐蚀率(0-100％暴露的Al金属损失)。
表3
| 清洁溶液 | 温度(℃) | 铝腐蚀率 | 灰化残余物移除率 |
| 溶液3 | 45 | 0 | 100 |
| 溶液3 | 65 | 0 | 100 |
| 溶液3 | 85 | 0 | 100 |
| ALEG-625 | 45 | 100 | 100 |
| ALEG-625 | 65 | 100 | 100 |
| ALEG-625 | 85 | 100 | 100 |
实施例4
制备清洁溶液(溶液3)，该清洁溶液含有约：66％的DMSO、17.4％的环丁砜、14％的丙二醇、2.4％的TMAH和0.2％的2-羟基吡啶。通过将晶片以设定的间隔暴露于化学物质并通过四探针(point probe)检测金属厚度的改变，从而来测定对于涂层(blanket)Al和Cu晶片的腐蚀速度。作为比较，将相同的晶片在ALEG-625(J.T.Baker)中清洁，所述ALEG-625为市售的其它相似组合物的半水性产品。代表不同操作温度的结果见下表。
表4
实施例5
将从上述实施例得到的清洁溶液3用于从具有暴露的Cr图案的有图案的晶片和具有PbSn焊料块(bump)的分离的晶片上去除光致抗蚀剂。将该溶液的清洁能力和相容性与上述实施例中所述的ALEG-625比较。在每种情况中，将晶片样品以设定好的时间和温度暴露于溶液，然后用DI水中洗涤1分钟，然后在流动的N2下干燥。使用样品的SEM分析确定清洁效果和相容性。清洁效果以去除光致抗蚀剂的百分比表示，而如果观察到任何点蚀或观察到图案形状改变则确定溶液为不相容的。
表5
本文已经通过引用其具体实施方式描述了本发明，应该理解在不背离本文所述的本发明的精神和范围的情况下，可以进行改变、修改和变化。因此本发明包括落入所述权利要求书的精神和范围的所有改变、修改和变化。
Claims (10)
1.用于清洁微电子设备的非水的剥离和清洁组合物，所述组合物包含：
a)至少一种有机含硫极性化合物作为剥离溶剂，
b)至少一种无水的强氢氧化物碱源，和
c)至少一种羟基吡啶稳定剂。
2.权利要求1的组合物，其中基于组合物的重量，所述至少一种作为剥离溶剂的有机含硫极性化合物存在于组合物中的量为20wt％至99wt％；其中基于组合物的重量，所述无水的强氢氧化物碱源存在于组合物中的量为0.5wt％至20wt％；和其中基于组合物的重量，所述羟基吡啶存在于组合物中的量为0.01wt％至5wt％。
3.权利要求2的组合物，其中所述至少一种作为剥离溶剂的有机含硫极性化合物选自亚砜、砜，及其混合物；所述无水的强氢氧化物碱源选自碱金属氢氧化物、氢氧化铵、氢氧化季铵，及其混合物；和所述至少一种羟基吡啶选自2-羟基吡啶、4-羟基吡啶，及其混合物。
4.权利要求3的组合物，其中所述砜为环丁砜。
5.权利要求3的组合物，其中所述至少一种作为剥离溶剂的有机含硫极性化合物选自二甲亚砜、环丁砜，及其混合物；所述无水的强氢氧化物碱源选自氢氧化四烃基铵；和所述至少一种羟基吡啶选自2-羟基吡啶。
6.权利要求5的组合物，其中所述组合物包含二甲亚砜、环丁砜、氢氧化四甲基铵和2-羟基吡啶。
7.权利要求6的组合物，所述组合物还包含丙二醇。
8.权利要求7的组合物，其中所述二甲亚砜存在的量为66wt％；所述环丁砜存在的量为17.4wt％；所述氢氧化四甲基铵存在的量为2.4wt％；所述丙二醇存在的量为14wt％；和所述2-羟基吡啶存在的量为0.2wt％。
9.根据权利要求1的组合物，其还包括一种或多种选自下述的成分：金属螯合或络合剂、共溶剂、腐蚀抑制化合物、表面活性剂。
10.用于清洁微电子设备基板而不产生任何明显的金属腐蚀的方法，所述方法包括将所述设备与清洁组合物接触足够的时间以清洁所述设备，其中所述清洁组合物包括权利要求1-9中任一项的组合物。
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| JP5305803B2 (ja) * | 2008-09-19 | 2013-10-02 | 株式会社カネカ | ポリエーテル類の製造方法 |
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| CN104195560A (zh) * | 2014-09-10 | 2014-12-10 | 昆山欣谷微电子材料有限公司 | 四甲基氢氧化铵无水剥离液 |
| US20160181087A1 (en) * | 2014-12-19 | 2016-06-23 | Intermolecular Inc. | Particle removal with minimal etching of silicon-germanium |
| KR102384908B1 (ko) * | 2015-11-25 | 2022-04-08 | 삼성전자주식회사 | 자성 패턴 세정 조성물, 자성 패턴 형성 방법 및 자기 메모리 장치의 제조 방법 |
| KR101966808B1 (ko) * | 2016-09-30 | 2019-04-08 | 세메스 주식회사 | 기판 세정 조성물, 기판 처리 방법 및 기판 처리 장치 |
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| US6551973B1 (en) | 2001-10-09 | 2003-04-22 | General Chemical Corporation | Stable metal-safe stripper for removing cured negative-tone novolak and acrylic photoresists and post-etch residue |
| WO2005043245A2 (en) * | 2003-10-29 | 2005-05-12 | Mallinckrodt Baker Inc. | Alkaline, post plasma etch/ash residue removers and photoresist stripping compositions containing metal-halide corrosion inhibitors |
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| US5308745A (en) * | 1992-11-06 | 1994-05-03 | J. T. Baker Inc. | Alkaline-containing photoresist stripping compositions producing reduced metal corrosion with cross-linked or hardened resist resins |
| EP1128222A2 (en) * | 2000-02-25 | 2001-08-29 | Shipley Company LLC | Photoresist stripping composition |
| CN1469918A (zh) * | 2000-10-16 | 2004-01-21 | ���ֿ����ر��˹�˾ | 用于清洗微电子基底的稳定的碱性组合物 |
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