CN107022421A - 清洗方法、及半导体装置的制造方法 - Google Patents
清洗方法、及半导体装置的制造方法 Download PDFInfo
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- CN107022421A CN107022421A CN201610815832.8A CN201610815832A CN107022421A CN 107022421 A CN107022421 A CN 107022421A CN 201610815832 A CN201610815832 A CN 201610815832A CN 107022421 A CN107022421 A CN 107022421A
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- Prior art keywords
- acid
- cleaning
- composition
- cleaning combination
- ingredient
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- 238000000034 method Methods 0.000 title claims abstract description 93
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- 238000001020 plasma etching Methods 0.000 claims abstract description 70
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- 239000004615 ingredient Substances 0.000 claims abstract description 36
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- -1 lactic acid compound Chemical class 0.000 claims description 24
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- 238000005530 etching Methods 0.000 claims description 18
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- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical compound C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 claims description 7
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- QTECDUFMBMSHKR-UHFFFAOYSA-N prop-2-enyl prop-2-enoate Chemical group C=CCOC(=O)C=C QTECDUFMBMSHKR-UHFFFAOYSA-N 0.000 description 1
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- SFVFIFLLYFPGHH-UHFFFAOYSA-M stearalkonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)CC1=CC=CC=C1 SFVFIFLLYFPGHH-UHFFFAOYSA-M 0.000 description 1
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- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
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- 229940095064 tartrate Drugs 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
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- 238000004448 titration Methods 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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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- 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
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- 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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- 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
-
- 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
- C09K13/06—Etching, surface-brightening or pickling compositions containing an inorganic acid with organic material
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- C—CHEMISTRY; METALLURGY
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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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- 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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- 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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- C11D3/2044—Dihydric alcohols linear
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- C11D3/2068—Ethers
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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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- C11D3/28—Heterocyclic compounds containing nitrogen in the ring
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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
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- C11D7/265—Carboxylic acids or salts thereof
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- 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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- 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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- C11D7/34—Organic compounds containing sulfur
-
- 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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- 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
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- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
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Abstract
本发明提供一种清洗组合物,其为除去在半导体用基板上形成的等离子蚀刻残渣及/或灰化残渣用的清洗组合物,其特征在于,包含(成分a)水、(成份b)羟基胺及/或其盐、(成分c)碱性有机化合物和(成分d)有机酸,所述清洗组合物的pH为7~9。还提供使用所述清洗组合物的清洗方法及半导体装置的制造方法。
Description
本申请是申请日为2010年09月28日、申请号为201010297139.9、发明名称为“清洗组合物、清洗方法、及半导体装置的制造方法”的申请的分案申请。
技术领域
本发明涉及在微电子学的制造中使用的新型清洗组合物、及使用该清洗组合物的清洗方法以及半导体装置的制造方法,尤其涉及在基板上蒸镀的金属层及氧化层的等离子蚀刻后,用于除去在晶片基板等半导体基板上形成的等离子蚀刻残渣的非蚀刻性清洗组合物、及使用该清洗组合物的清洗方法及半导体装置的制造方法。
背景技术
在集成电路的制造中,正型光致抗蚀剂通过一系列的照相平板和等离子蚀刻阶段,作为在晶片基板上用于移动聚焦屏下面的掩模图案的中间掩模使用。集成电路的制造工序的最终阶段之一是将图案化的光致抗蚀膜从基板上除去。一般地,该阶段用2个方法中的1个进行。方法之一包含使覆盖了光致抗蚀剂的基板首先与由有机溶剂和胺组成的光致抗蚀剂的脱膜剂(stripper)液接触的湿法脱模阶段。但是,剥离液,特别是在制造中光致抗蚀膜被暴露在紫外线照射或等离子处理中的情况下,不能完全、确实地除去光致抗蚀膜。若干光致抗蚀膜由于这种处理而变质,不容易在剥离液中溶解。另外,在这样的惯用的湿法脱模法中所使用的化学物质,对于除去在使用含卤气体的金属或氧化物层的等离子蚀刻中形成的无机残渣物质,屡屡失效。
除去光致抗蚀膜的其他的方法,包含在作为等离子灰化已知的工序中,为了使基板表面的抗蚀膜燃烧,将进行了光致抗蚀剂涂布的晶片暴露在以氧气为基础的等离子中的方法。由于等离子灰化在真空室内进行,可以期待其不容易受到空中的微粒及金属污染的影响,所以在集成电路的制造工序中,极为普遍。
但是,等离子灰化对除去上述的等离子蚀刻的副产物也不是完全有效的。作为其替代,这些等离子蚀刻副产物的除去,其后,必须通过将光致抗蚀膜暴露在某清洗溶液中来完成。用于除去由于等离子灰化后的等离子蚀刻而残留的等离子蚀刻副产物的任何市售品现在均可购入。例如,从EKCTechnologyInc.可以购入的EKC265为水、链烷醇胺、儿茶酚及羟胺组成的后蚀刻清洗溶液。此类组合物公开在Lee的美国专利第5279771号说明书中。从Ashland Chemical可以购入的ACT 935为另一个后蚀刻清洗溶液,由水、链烷醇胺、及羟胺组成。此类组合物公开在Ward的美国专利第5419779号说明书中。从Mitsubishi GasChemical可以购入的ELMC-30由水、N、N-二甲基甲酰胺、氟化合物、有机羧酸盐及糖醇组成,这里,糖醇作为腐蚀剂起作用。此类组合物公开在Aoyama等申请的美国专利第5630904号说明书中。
这些市售制品,虽然有效地分解等离子蚀刻残渣,但也侵袭基板上的金属及氧化物的蒸镀图案。这是因为EKC265和ACT935的pH为11以上,ELMC-30包含氟化合物。在这些制品中使用的防腐蚀剂,由于铜、铝、铝合金(例如,Al-Cu-Si)等金属层对于腐蚀特别敏感,对于防止腐蚀完全无效。进而,添加适当的防腐蚀剂,虽然对于防止基板金属层的腐蚀是不可缺少的,但多数防腐蚀剂存在妨碍除去等离子蚀刻残渣的倾向,及/或除去在金属基板表面上蒸镀的不溶性膜的倾向。
因此,存在有对用于从基板除去等离子蚀刻残渣的新型清洗组合物的要求。另外,存在有不给基板带来有害影响的那样的清洗组合物的要求,存在有对为水溶性基础剂、无危险、不对环境造成危害的清洗组合物的要求。
针对这些铜、铝、铝合金等的腐蚀,本田等设计发明了包含(a)水、(b)羟胺化合物、(c)碱性化合物、(d)有机羧酸的清洗组合物。由此可以维持清洗性,同时可以实现防腐蚀。这些技术记载在专利第3871257号公报中。
进而,本田等构筑了如专利第3513491号公报及专利第4147320号公报公开的防腐蚀技术。
在本田等公开的专利第3871257号公报、专利第3513491号公报、及专利第4147320号公报所记载的技术中,使用水基础的组合物,不仅可以防止金属腐蚀也不会对环境造成危害。
但是,伴随近年来的半导体基板制造技术的发展,为了制作各种各样的具有金属层及绝缘膜层(铝、铝/硅酮/铜、钛、氮化钛、钛/钨、钨、氧化硅、聚硅酮结晶等)的集成电路,等离子蚀刻残渣物的组成复杂化,产生不能充分除去的情况。因此,期待将此类残渣物没有金属腐蚀问题地除去的清洗组合物。
如上所述,随着技术的发展,在半导体基板上形成的结构采用具有各种化学组成的配线结构及层间绝缘结构,用于除去在等离子蚀刻时作为掩模使用的抗蚀剂的灰化中产生的残渣的特性也发生变化。用于除去在等离子蚀刻及灰化中产生的残渣的清洗组合物,要求能够充分地除去残渣的组合物及不损伤配线结构及层间绝缘结构的组合物。
发明内容
本发明需要解决的课题在于,提供一种清洗组合物,其不损伤配线结构及层间绝缘结构,可以充分除去半导体基板上的等离子蚀刻残渣及灰化残渣,以及提供使用所述清洗组合物的清洗方法及半导体装置的制造方法。
本发明的上述课题通过下述<1>、<20>、<21>或<23>中所述的方法来解决。作为优选的实施方式的<2>~<19>、<22>、及<24>一起如下所示。
<1>一种清洗组合物,其为除去在半导体用基板上形成的等离子蚀刻残渣及/或灰化残渣用的清洗组合物,其特征在于,包含(成分a)水、(成份b)羟基胺及/或其盐、(成分c)碱性有机化合物和(成分d)有机酸,所述清洗组合物的pH为7~9。
<2>如上述<1>所述的清洗组合物,其中,成分a相对于清洗组合物的总重量的含量为50~99.5重量%。
<3>如上記<1>或<2>所述的清洗组合物,其中,成份b为选自于羟基胺、羟胺硫酸盐、羟胺盐酸盐、羟胺硝酸盐及羟胺磷酸盐组成的组中的至少一种化合物。
<4>如上述<3>所述的清洗组合物,其中,成份b为羟胺硫酸盐。
<5>如上述<1>~<4>任一项所述的清洗组合物,其中,成份b相对于清洗组合物的总重量的含量为0.01~30.0重量%。
<6>如上述<1>~<5>任一项所述的清洗组合物,其中,成份c为选自于有机胺及季铵氢氧化物组成的组中的至少一种化合物。
<7>如上述<6>所述的清洗组合物,其中,成份c为具有羟基的有机胺。
<8>如上述<6>所述的清洗组合物,其中,成份c为四烷基氢氧化铵。
<9>如上述<1>~<8>任一项所述的清洗组合物,其中,成份c相对于清洗组合物总重量的含量为0.01~20.0重量%。
<10>如上述<1>~<9>任一项所述的清洗组合物,其中,成分d为单官能性、双官能性、三官能性或四官能性有机酸。
<11>如上述<10>所述的清洗组合物,其中,成分d为选自于柠檬酸、乳酸、醋酸、丙酸、苹果酸、酒石酸、丙二酸、乙二酸、琥珀酸、葡糖酸、乙醇酸、二乙醇酸、马来酸、苯甲酸、邻苯二甲酸、水杨酸、水杨基氧肟酸、及邻苯二甲基氧肟酸组成的组中的至少一种化合物。
<12>如上述<10>所述的清洗组合物,其中,成分d为羟基羧酸。
<13>如上述<12>所述的清洗组合物,其中,成分d为选自于柠檬酸、苹果酸、酒石酸、乙醇酸、葡糖酸及乳酸组成的组中的至少一种化合物。
<14>如上述<1>~<13>任一项所述的清洗组合物,其中,成分d相对于清洗组合物的总重量的含量为0.01~20.0重量%。
<15>如上述<1>~<14>任一项所述的清洗组合物,其中,pH为7.0~8.5。
<16>如上述<15>所述的清洗组合物,其中,pH为7.2~8.4。
<17>如上述<1>~<16>任一项所述的清洗组合物,其中,进一步含有(成分e)含氨基羧酸。
<18>如上述<17>所述的清洗组合物,其中,成分e为组氨酸及/或精氨酸。
<19>如上述<17>或<18>所述的清洗组合物,其中,成分e相对于清洗组合物的总重量的含量为0.01~5.0重量%。
<20>上述<1>~<19>中任一项所述的清洗组合物作为除去等离子蚀刻残渣及/或灰化残渣的清洗组合物的应用。
<21>一种清洗方法,其包含制备如上述<1>~<19>中任一项所述的清洗组合物的制备工序及利用所述清洗组合物清洗在半导体上形成的等离子蚀刻残渣及/或灰化残渣的清洗工序。
<22>如上述<21>所述的清洗方法,其中,所述半导体基板含有铝及/或铜。
<23>一种半导体装置的制造方法,其包含:对于半导体基板进行等离子蚀刻的蚀刻工序、及/或对于半导体基板的抗蚀剂进行灰化的灰化工序、以及利用上述<1>~<19>中任一项所述的清洗组合物,清洗在所述蚀刻工序及/或所述灰化工序中在所述半导体基板上形成的等离子蚀刻残渣及/或灰化残渣的清洗工序。
<24>如上述<23>所述的半导体装置的制造方法,其中,所述半导体基板含有铝及/或铜。
本发明提供一种清洗组合物,其可以不损伤配线结构及层间绝缘结构,可以充分除去在半导体基板上的等离子蚀刻残渣及灰化残渣,也提供使用所述清洗组合物的清洗方法及半导体装置的制造方法。
附图说明
[图1]是表示本发明的半导体装置的制造方法的概要的工序剖面图。
[图2]是表示粘附了灰化后的等离子蚀刻残渣及灰化残渣状态的半导体装置的概略剖面图。
符号说明
10 半导体基板
12 AL合金膜
14 氮化钛膜
16 配线
18 硅酮氧化膜
20 通孔
22 通孔
24 层间绝缘膜
26 氮化钛膜
28 钛膜
30 Al合金膜
32 氮化钛膜
34 配线
36 残渣(等离子蚀刻残渣及灰化残渣)
具体实施方式
在半导体装置的制造工序中,通过将抗蚀图等作为掩模使用的等离子蚀刻,蚀刻半导体基板上的金属层、半导体层、绝缘层等,对金属层及半导体层图案化,可以在绝缘层上形成通孔及配线槽等开口部。
在上述等离子蚀刻中,在半导体基板上产生作为掩模使用的抗蚀剂及源自蚀刻的金属层、半导体层、绝缘层的残渣。本发明中,通过这种等离子蚀刻产生的残渣称为“等离子蚀刻残渣”。
另外,作为掩模使用的抗蚀图,在蚀刻后除去。除去抗蚀图采用使用脱模剂溶液的湿式的方法,或使用例如等离子、臭氧等的进行灰化的干式的方法。
在上述灰化(ashing)中,在半导体基板上产生通过等离子蚀刻产生的等离子蚀刻残渣及变质的残渣、及源自除去的抗蚀剂的残渣。本发明中,将这样通过灰化产生的残渣称为“灰化残渣”。
这种蚀刻后的残渣(Post Etch Residue)的等离子蚀刻残渣及灰化残渣,使用清洗组合物清洗除去。本发明的清洗组合物,用于除去通过等离子蚀刻产生的等离子蚀刻残渣及/或通过灰化产生的灰化残渣。
本发明的清洗组合物,可以为了除去等离子蚀刻残渣及灰化残渣的任一方面而使用,优选在接着等离子蚀刻进行的灰化后,为了除去等离子蚀刻残渣及灰化残渣而使用。
以下,详细说明本发明。另外,本发明中,表示数值范围“A~B”的记载,没有特别的限定,是指“A以上B以下”,是指包含端点的A及B的数值范围。
(清洗组合物)
本发明的清洗组合物,其特征在于,包含(成分a)水、(成分b)羟胺及/或其盐、(成分c)碱性有机化合物、及(成分d)有机酸,所述清洗组合物的pH为7~9,是除去在半导体用基板上形成的等离子蚀刻残渣及/或灰化残渣用的清洗组合物。
以下、依次说明本发明的清洗组合物中必需的成分(成分a)~(成分d)、及pH。
<(成分A)水>
本发明的清洗组合物,为作为溶剂的含有水的水溶液。水的含量相对于清洗组合物的总重量优选为50~99.5重量%。这样,以水为主成分的清洗组合物,和目前的有机溶剂的比率高的清洗组合物相比,从不对环境造成危害的方面考虑,优选。
作为水,优选在半导体制造中使用的超纯水。
<(成分B)羟胺及/或其盐>
本发明的清洗组合物包含至少一种羟胺及/或其盐。羟胺的盐,优选为羟胺的无机酸盐或有机酸盐,更优选Cl、S、N、P等非金属可以和氢键合的无机酸盐,进一步优选为盐酸、硫酸、硝酸任一个酸的盐。
作为形成本发明的清洗组合物使用的羟胺的盐,可以示例有,羟胺硝酸盐(也称为HAN)、羟胺硫酸盐(也称为HAS)、羟胺磷酸盐、羟胺盐酸盐等。
在清洗组合物中也可以使用羟胺的有机酸盐,举出示例:羟胺柠檬酸盐、羟胺乙二酸盐等。
这些羟胺的盐中,羟胺硝酸盐、羟胺硫酸盐、羟胺磷酸盐、羟胺盐酸盐等无机酸盐由于对铝及铜、钛等金属是惰性的,故优选。特别优选羟胺硝酸盐、羟胺硫酸盐。
这些羟胺及/或其盐,可以单独1种或混合2种以上使用。
羟胺及/或其盐,相对于本发明的清洗组合物的总重量,优选在约0.01~约30重量%的范围内含有,更优选含有0.1~15重量%。
羟胺及/或其盐,等离子蚀刻残渣的除去简单,防止金属基板的腐蚀。
<(成分c)碱性有机化合物>
本发明的清洗组合物包含碱性有机化合物
碱性有机化合物,优选具有作为构成元素的碳及氮,更优选具有氨基。具体的说,碱性有机化合物优选选自于有机胺及季铵氢氧化物组成的组中选择的至少1种化合物。另外,所谓的有机胺,是指含有作为构成元素的碳的胺。
碱性有机化合物的碳数优选为4~30,从在水中沸点和溶解度的观点考虑更优选为6~16。
作为本发明的清洗组合物的碱性有机化合物使用的有机胺,包含单乙醇胺、二乙醇胺、三乙醇胺、二乙二醇胺、N-羟乙基哌嗪等链烷醇胺,及/或乙胺、苄胺、二乙胺、n-丁胺、3-甲氧基丙胺、叔丁胺、n-己胺、环己胺、n-辛胺、2-乙基己胺、邻苯二甲胺、间苯二甲胺、1-甲基丁胺、乙二胺(EDA)、1,3-丙二胺、2-氨基苄胺、N-苄基乙二胺、二乙烯三胺、三乙烯四胺等不具有羟基的有机胺。从金属防止腐蚀的观点考虑,比起链烷醇胺,更优选不具有羟基的有机胺。进而特别优选可以和金属配位的乙二胺、1,3-丙二胺、邻苯二甲胺、间苯二甲胺。
作为本发明的清洗组合物的碱性有机化合物优选使用的氢氧化季铵,优选氢氧化四烷基铵,更优选以低级(碳数为1~4)烷基取代的氢氧化四烷基铵,具体的可以举出:四甲基氢氧化铵(TMAH)、四乙基氢氧化铵(TEAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵(TBAH)等。进而也可以举出:作为季铵氢氧化物的三甲基羟乙基氢氧化铵(胆碱)、甲基三(羟乙基)氢氧化铵、四(羟乙基)氢氧化铵、苄基三甲基氢氧化铵(BTMAH)等。另外,氢氧化铵可以和1个或1个以上的季铵氢氧化物组合使用。其中,更优选为TMAH、TEAH、TPAH、TBAH、胆碱,特别优选为TMAH、TBAH。
这些有机胺及季铵氢氧化物可以单独使用1种也可以2种以上混合使用。
碱性有机化合物的含量,对于本发明的清洗组合物的总重量,优选为约0.01~约20.0重量%,更优选为1.0~10.0重量%。
<(成分d)有机酸>
本发明的清洗组合物,含有至少一个有机酸,该有机酸优选为单官能性、双官能性、三官能性、或四官能性有机酸。有机酸作为金属的防腐蚀剂起作用。
在有机酸中,羧酸由于可以有效防止铝、铜及其合金的金属腐蚀,故优选,具有羟基的羟基羧酸由于可以特别有效的防止金属腐蚀,故更优选。羧酸对于这些金属具有螯合效果。对于优选的羧酸包含单羧酸及多元羧酸。作为羧酸,并不限定于此,可以示例有,甲酸、醋酸、丙酸、戊酸、异戊酸、乙二酸、丙二酸、琥珀酸、戊二酸、马来酸、富马酸、邻苯二甲酸、1,2,3-均苯三甲酸、乙醇酸、乳酸、柠檬酸、水杨酸、酒石酸、葡糖酸、二乙醇酸、苹果酸、乙酰氧肟酸、苯基氧肟酸、水杨基氧肟酸、邻苯二甲基氧肟酸、苯甲酸、二羟基苯甲酸及其混合物。其中,优选使用羟基羧酸的柠檬酸、苹果酸、酒石酸、乙醇酸、葡糖酸、乳酸。
另外,羧酸优选以构成元素仅为C、H、及O,更优选不具有氨基。
另外,这些有机酸,可以单独使用1种或2种以上混合使用,从有效防止金属腐蚀的观点考虑,优选2种以上合用。
有机酸,对于本发明的清洗组合物的总重量,优选在约0.01~约20.0重量%之间的量加入,更优选加入约0.05~约20.0重量%,进一步加入0.1~10.0重量%。
<pH>
本发明的清洗组合物的pH为7~9,优选为7.0~8.5,更优选为7.2~8.4,进一步优选为7.2~8.0。pH如果在上述数值的范围,能够兼备充分除去光致抗蚀剂、防反射膜、蚀刻残渣、及灰化残渣,同时防止金属腐蚀。通过设定在该pH范围,可以完全除去通过对氧化硅和金属层进行等离子蚀刻而形成通路图案时的残渣。
作为pH的测定方法,可以使用市售的pH计进行测定。
为了将清洗组合物调节到要求的pH,可以通过调节有机胺及/或季铵氢氧化物的添加量的滴定来进行。
本发明中,pH的选定非常重要。干预残渣的清洗的羟胺的共轭酸的pKa约为6,如果清洗组合物的pH不到7,则清洗性下降。另一方面,如果pH为7以上,则清洗性显著上升。仅考虑残渣的清洗性能时,pH为7以上就可以,越高则清洗性越上升。但是如果pH过高则产生腐蚀,pH超过9时不能实现满意的防腐性能。本发明中,发现兼备清洗性和防腐蚀性的pH范围,发现在7~9的范围可以同时满足,优选为7.0~8.5,更优选为7.2~8.4、进一步优选为7.2~8.0。
本发明的清洗组合物,除上述成分(成分a)~(成分d)以外,可以包含如以下举出的1或2种以上的任意成分(成分e)~(成分h)。
<(成分e)含氨基羧酸>
本发明的清洗组合物,可以含有含氨基羧酸。含氨基羧酸从有效率防止金属腐蚀的方面考虑优选。
作为含氨基羧酸,可以举出:甘氨酸、丙氨酸、天冬酰胺、天冬氨酸、精氨酸、谷酰胺、谷氨酸、组氨酸、丝氨酸、巯基丙氨酸、酪氨酸、苯丙氨酸等氨基酸及/或由以下组成的氨基聚羧酸盐组{乙二胺四醋酸盐(EDTA)、二乙烯三胺五醋酸盐(DTPA)、羟乙基乙二胺三醋酸盐(HEDTA)、二羟乙基乙二胺四醋酸盐(DHEDDA)、硝基三醋酸盐(NTA)、羟乙基亚氨基二醋酸盐(HIDA)、β-丙氨酸二醋酸盐、天冬氨酸二醋酸盐、甲基甘氨酸二醋酸盐、亚氨基二琥珀酸盐、丝氨酸二醋酸盐、羟基亚氨基二琥珀酸盐、二羟乙基甘氨酸盐、天冬氨酸盐、谷氨酸盐等}、由以下组成的羟基羧酸盐组{羟基醋酸盐、酒石酸盐、柠檬酸盐、葡糖酸盐等}、由以下组成的环羧酸盐组{均苯四甲酸盐、苯并聚羧酸盐、环戊烷四羧酸盐等}、由以下组成的醚羧酸盐组{羧甲基丙醇二酸盐、羧基甲氧基琥珀酸盐、氧基二琥珀酸盐、酒石酸单琥珀酸盐、酒石酸二琥珀酸等}、由以下组成的其它羧酸盐组{马来酸衍生物、乙二酸盐等}、由以下组成的有机羧酸(盐)聚合物组{丙烯酸聚合物及共聚物(丙烯酸-烯丙醇共聚物、丙烯酸-马来酸共聚物、羟基丙烯酸聚合物、多糖类-丙烯酸共聚物等)、由以下组成的多元羧酸聚合物及共聚物组{马来酸、衣康酸、富马酸、四亚甲基-1,2-二羧酸、琥珀酸、天冬氨酸、谷氨酸等单体的聚合物及共聚物}、由以下组成的乙醛酸聚合物、多糖类组{淀粉、纤维素、直链淀粉、果胶、羧甲基纤维素等}、由以下组成的膦酸盐组{甲基二膦酸盐、氨基三亚甲基膦酸盐、亚乙基二膦酸盐、1-羟基亚乙基-1,1-二膦酸盐、乙基氨基双亚甲基膦酸盐、乙二胺双亚甲基膦酸盐、乙二胺四亚甲基膦酸盐、六亚甲基二胺四亚甲基膦酸、亚丙基二胺四亚甲基膦酸盐、二乙烯三胺五亚甲基膦酸盐、三乙烯四胺六亚甲基膦酸盐及四亚乙基五胺七亚甲基膦酸盐等}等。
需要补充的是,作为这些盐,可以举出:铵盐、链烷醇胺(单乙醇胺、三乙醇胺等)盐等。这些可以1种或2种以上组合使用。
这些含氨基羧酸中,优选为精氨酸、组氨酸、谷酰胺、EDTA、DTPA、HIDA,更优选精氨酸、组氨酸。
这些含氨基羧酸,可以1种单独使用也可以2种以上混合使用。
本发明的清洗组合物中,含有含氨基羧酸时,其添加量可以适当选择,对于本发明的清洗组合物的总重量,优选为约0.01~约5.0重量%,更优选为0.01~3重量%。
<(成分f)表面活性剂>
本发明的清洗组合物可以含有表面活性剂。作为表面活性剂,可以使用非离子性、阴离子性、阳离子性表面活性剂、及两性表面活性剂。
作为在本发明中使用的表面活性剂,通过添加调节清洗组合物的粘度,从可以改良对于清洗对象的润湿性的方面,及对于绝缘膜等防腐蚀性两者更优异的方面考虑,优选使用非离子性表面活性剂。作为非离子性表面活性剂,例如可以使用,聚环氧烷烃烷基苯基醚类表面活性剂、聚环氧烷烃烷基醚系表面活性剂、聚环氧乙烷和聚环氧丙烷组成的嵌段聚合物类表面活性剂、聚氧亚烷基二苯乙烯化苯基醚类表面活性剂、聚亚烷基三苄基苯基醚表面活性剂、乙炔聚环氧烷烃类表面活性剂等。
其中优选为聚亚烷基氧(以下PAO)烷基醚类表面活性剂,为选自于PAO癸醚、PAO十二烷基醚、PAO三癸醚、PAO亚烷基癸醚、PAO山梨糖醇酐单月桂酸酯、PAO单油酸山梨糖醇酯、PAO山梨糖醇酐单硬脂酸酯、四油酸聚环氧乙烷山梨糖醇、PAO烷基胺、PAO乙炔二醇中选择的聚环氧烷烃烷基醚类表面活性剂。作为聚环氧烷烃,优选聚环氧乙烷、聚环氧丙烷或聚环氧丁烷的聚合物。
另外,作为在本发明中使用的表面活性剂,对于残渣物的除去性和基板及绝缘膜等腐蚀性两者更优异的方面考虑,优选使用阳离子性表面活性剂。作为阳离子性表面活性剂,优选为季铵盐类表面活性剂或烷基吡啶类表面活性剂。
作为季铵盐类表面活性剂,优选以下述式(1)表示的化合物。
[化1]
(式(1)中、X-表示氢氢氧根离子、氯离子、溴离子、或硝酸根离子,R5表示碳数为8~18的烷基,R6及R7表示各自独立的碳数为1~18的烷基,芳基、碳数为1~8的羟基烷基、或苄基,R8表示碳数为1~3的烷基。)
式(1)中、X-表示平衡离子,具体的表示氢氧根离子、氯离子、溴离子、或硝酸根离子。
式(1)中,R5表示碳数为8~18的烷基(优选碳数为12~18,例如,十六烷基、十八烷基等)。
式(1)中,R6及R7表示各自独立的碳数为1~18的烷基、碳数为1~8的羟基烷基(例如,羟乙基等)、芳基(例如、苯基等)、或苄基。
式(1)中、R8表示碳数为1~3的烷基(例如,甲基、乙基等)。
作为以式(1)表示的化合物的具体例,可以举出:十六烷基三甲基氯化铵、二(十二烷基)二甲基氯化铵、三(十二烷基)甲基氯化铵、十八烷基苄基二甲基氯化铵等。这些化合物的平衡离子不限定于氯离子,可以为溴离子或氢氧根离子。
另外,作为烷基吡啶类表面活性剂的具体的可以举出十六烷基氯化吡啶等。这些化合物的平衡离子不限定于氯离子,也可以为溴离子或氢氧根离子。
清洗组合物中的表面活性剂的含量相对于清洗组合物的总重量,优选为0.0001~5重量%,更优选为0.0001~1重量%。由于通过将表面活性剂添加在清洗组合物中来调节清洗组合物的粘度,可以改良对于清洗对象物的润湿性,故优选,加上由于对于基板及绝缘膜等的腐蚀性两者更优异的方面考虑,也优选。此类表面活性剂一般可以商业性购入。这些表面活性剂可以单独或多种组合使用。
<(成分g)水溶性有机溶剂>
本发明的清洗组合物可以含有水溶性有机溶剂。水溶性有机溶剂从防止腐蚀的观点可以适用。例如,甲醇、乙醇、1-丙醇、2-丙醇、2-丁醇、乙二醇、丙二醇、丙三醇、1,6-己二醇、环己二醇、山梨糖醇、木糖醇、2-甲基-2,4-戊二醇、1,3-丁二醇、1,4-丁二醇等醇类溶剂、乙二醇单甲醚、二乙二醇、二丙二醇、丙二醇单甲醚、二乙二醇单甲醚、三乙二醇、聚乙二醇、丙二醇单甲醚、二丙二醇单甲醚、三丙二醇单甲醚、二乙二醇单丁醚、二乙二醇单丁醚等醚类溶剂、甲酰胺、单甲基甲酰胺、二甲基甲酰胺、乙酰胺、单甲基乙酰胺、二甲基乙酰胺、单乙基乙酰胺、二乙基乙酰胺、N-甲基吡咯烷酮等酰胺类溶剂、二甲基砜、二甲基亚砜、环丁砜等含硫类溶剂、γ-丁内酯、σ-戊内酯等内酯类溶剂等。其中优选的为乙醇类、醚类,更优选的为1,6-己二醇、二乙二醇、丙二醇、二丙二醇、丙二醇单甲醚、二丙二醇单甲醚。水溶性有机溶剂可以单独使用或2种以上组合使用。
清洗组合物中的水溶性有机溶剂的含量,相对于清洗组合物的总重量,优选以0~40重量%的浓度使用,更优选以0~20重量%的浓度使用。进一步优选以0.01~15重量%的浓度使用。由于通过将水溶性有机溶剂添加在清洗组合物中可以防止金属膜的腐蚀,故优选。
<(成分h)防腐蚀剂>
本发明的清洗组合物可以含有防腐蚀剂。
蚀刻剂优选为杂环化合物,更优选为苯并三唑及其衍生物。作为所述衍生物,优选为5,6-二甲基-1,2,3-苯并三唑(DBTA)、1-(1,2-二羧乙基)苯并三唑(DCEBTA)、1-[N,N-双(羟乙基)氨甲基]苯并三唑(HEABTA)、1-(羟甲基)苯并三唑(HMBTA)。
本发明中使用的防腐蚀剂,可以单独使用,也可以2种以上合用。另外,本发明中使用的防腐蚀剂,除可以使用标准法合成以外,也可以使用市售品。
另外,防腐蚀剂的添加量优选为0.01重量%以上、0.2重量%以下,更优选为0.05重量%以上、0.2重量%以下。
(清洗方法)
接下来,对本发明的清洗方法进行说明。
本发明的清洗方法包含制备上述本发明的清洗组合物的制备工序、及利用所述清洗组合物清洗半导体基板上形成的等离子蚀刻残渣及/或灰化残渣的清洗工序。
所述制备工序为制备本发明的清洗组合物的工序。本发明的清洗组合物,可以通过必需成分的成分a~成分d、及根据需要混合任意成分的成分e~成分h进行制备。
本发明的清洗组合物的pH,调节为7~9的范围内,优选调节为7.0~8.5的范围内、更优选调节为7.2~8.4的范围内、进一步优选调节为7.2~8.0的范围内。pH的调节,优选通过调节成分c的碱性有机化合物的添加量进行。
所述清洗工序为利用本发明的清洗组合物清洗半导体基板上形成的等离子蚀刻残渣及/或灰化残渣的工序。
所述清洗工序中清洗除去的等离子蚀刻残渣,是在进行等离子蚀刻的蚀刻工序中,通过等离子蚀刻在半导体基板上形成的残渣。
所述蚀刻工序中,作为等离子蚀刻时的掩模,有时使用抗蚀图案。此时,优选在所述蚀刻工序后且所述清洗工序前,例如通过使用等离子、氧等的灰化,进行除去抗蚀图案的灰化工序。所述清洗工序中清洗除去的灰化残渣,是在所述灰化工序中通过灰化在半导体基板上形成的残渣。
所述半导体基板,例如优选形成有通路及配线等金属层的基板,更优选含有铝及/或铜的基板。
所述清洗工序中的清洗方式,只要是至少使形成有等离子蚀刻残渣及/或灰化残渣的半导体基板的面与本发明的清洗组合物接触的方式,就没有特别的限定,优选该半导体基板浸渍在本发明的清洗组合物中的方式。
(半导体装置的制造方法)
接下来,详细叙述本发明的半导体装置的制造方法。
本发明的半导体装置的制造方法,包含对于半导体基板进行等离子蚀刻的蚀刻工序,及/或对于半导体基板上的抗蚀剂进行灰化的灰化工序,及利用本发明的清洗组合物,在所述蚀刻工序及/或所述灰化工序中清洗所述半导体基板上形成的等离子蚀刻残渣及/或灰化残渣的清洗工序。具体地说,本发明的半导体装置的制造方法,是在形成通孔或配线后的半导体基板的清洗中,优选适用本发明的清洗组合物的制造方法。
需要补充的是,本发明中所谓的“半导体基板”,表示半导体装置使用的基板,只要没有特别说明,不仅是硅酮晶片等狭义的半导体基板,例如,也可以是在硅酮晶片上形成层间绝缘膜及钨塞(tungsten plug)、通孔、配线等的基板。
以下示例若干的实施方式。
[第一实施方式]
图1是表示基于本发明的第1实施方式的半导体装置的制造方法的概要的工序剖面图。
首先,通过通常的半导体装置的制造工序,在硅酮晶片等半导体基板10上,形成晶体管以外的元件及1层或2层以上的配线。接下来,在形成有元件等的半导体基板10上,形成层间绝缘膜。
接下来,在整个面,例如通过CVD(Chemical Vapor Deposition、化学气相沉淀)法,依次层叠例如膜厚约500nm的Al合金膜12和例如膜厚约50nm的氮化钛膜14。这样,形成依次层叠Al合金膜12和氮化钛膜14的导体膜。需要补充的是,Al合金膜12为例如含有0.1~5%的Cu的Al和Cu的合金膜。
接下来,通过光刻及干式蚀刻将导体膜形成图案。这样一来,形成Al合金膜12和氮化钛膜14组成的配线16。
接下来,在表面,例如通过CVD法,形成例如膜厚约500nm的硅酮氧化膜18。
接下来,例如通过CMP(Chemical Mechancal Polishing、化学性机械性抛光)法,抛光硅酮氧化膜18的表面,使硅酮氧化膜18的表面平坦(参照图1(a))。
接下来,在硅酮氧化膜18上,通过光刻形成具有通路图案的光致抗蚀剂膜。接着将该光致抗蚀剂膜作为掩模,通过等离子蚀刻,蚀刻硅酮氧化膜18。此时,也对硅酮氧化膜18下的氮化钛膜14的上部进行蚀刻。这样,在硅酮氧化膜18上形成达到配线16的氮化钛膜14的通孔(通路图案A)20(参照图1(b))。硅酮氧化膜18及氮化钛膜14的上部的等离子蚀刻,可以分别使用公知的方法进行。
接下来,例如通过使用等离子、氧等灰化,除去作为掩模使用的光致抗蚀剂膜。光致抗蚀剂膜的灰化,可以使用公知的方法进行。
在用于除去用于形成通孔20的的等离子蚀刻及光致抗蚀剂膜的灰化中,在包含通孔20周围的表面的基板表面,附着源自变质的光致抗蚀剂膜、硅酮氧化膜18、及露出于通孔20底的氮化钛膜14的残渣(等离子蚀刻残渣及灰化残渣)。
因此,用于除去光致抗蚀剂膜的灰化后,利用本发明的清洗组合物,清洗直到通孔20为止形成的半导体基板10。这样,除去粘附在直到通孔20为止形成的半导体基板10的表面上的等离子蚀刻残渣及灰化残渣。
接下来,在表面,例如通过CVD法,形成钨膜。
接下来,例如通过CMP法,对钨膜进行抛光,直到硅酮氧化膜18的表面露出为止。这样,在通孔20内嵌入由钨组成的通路。
[第2实施方式]
接下来,对于本发明的第2实施方式的半导体装置的制造方法的概要,使用相同的图1进行说明。通过本实施方式的半导体装置的制造方法,在形成达到配线16的Al合金膜12的通孔22的方面,和通过第1实施方式的半导体装置的制造方法不同。
首先,与第1实施方式的半导体装置的制造方法相同,在半导体基板10上形成由Al合金膜12和氮化钛膜14组成的配线16、及硅酮氧化膜18(参照图1(a))。
接下来,在硅酮氧化膜18上,通过光刻形成具有通路图案的光致抗蚀剂膜。接着将该光致抗蚀剂膜作为掩模,通过等离子蚀刻,蚀刻硅酮氧化膜18及氮化钛膜14。此时,也蚀刻氮化钛膜14下的Al合金膜12的上部。这样,在硅酮氧化膜18及氮化钛膜14上,形成达到配线16的Al合金膜12的通孔22(通路图案B)(参照图1(c))。硅酮氧化膜18、氮化钛膜14、及Al合金膜12上部的等离子蚀刻可以各自使用公知的方法进行。
接下来,例如通过使用等离子、氧等的灰化,除去作为掩模使用的光致抗蚀剂膜。光致抗蚀剂膜的灰化可以使用公知的方法进行。
本实施方式的情况,在为了除去形成通孔22的等离子蚀刻及光致抗蚀剂膜的灰化中,在包含通孔22周围的表面及通孔22的壁面的基板表面上粘附等离子蚀刻残渣及灰化残渣。本实施方式的情况,等离子蚀刻残渣及灰化残渣,不仅源自变质的光致抗蚀剂膜、硅酮氧化膜18及氮化钛膜14,而且也源自露出于通孔22底的Al合金膜12。
因此,用于除去光致抗蚀剂膜的灰化后,利用本发明的清洗组合物,清洗直到通孔22为止形成的半导体基板10。这样,除去粘附在直到通孔22为止形成的半导体基板10的表面上的等离子蚀刻残渣及灰化残渣。
接下来,和第1实施方式的半导体装置的制造方法相同,形成嵌入通孔22的通路。
[第3实施方式]
接下来,对于本发明第3实施方式的半导体装置的制造方法的概要,使用图1及图2进行说明。
首先,与第1实施方式的半导体装置的制造方法相同,在形成有元件等的半导体基板10上,形成层间绝缘膜24。
接下来,在表面,例如通过CVD法,依次层叠例如膜厚约50nm的氮化钛膜26和例如膜厚约20nm的钛膜28和例如膜厚约500nm的Al合金膜30和例如膜厚约50nm的氮化钛膜32。需要补充的是,Al合金膜30为例如含有0.1~5%的Cu的Al和Cu的合金膜。
接下来,在氮化钛膜32上,通过光刻形成具有配线图案的光致抗蚀剂膜。接着将该光致抗蚀剂膜作为掩模,通过等离子蚀刻依次蚀刻氮化钛膜32、Al合金膜30、钛膜28及氮化钛膜26。这样,图案化氮化钛膜32、Al合金膜30、钛膜28及氮化钛膜26,形成由这些导体膜组成的配线(配线图案)34。
接下来,通过使用药水进行湿式处理,剥离除去作为掩模使用的大部分光致抗蚀剂膜。接着,通过使用例如等离子、氧等的灰化,除去光致抗蚀剂膜的剩余部分(参照图1(d))。
在用于除去形成配线34的等离子蚀刻及光致抗蚀剂膜的剩余部分的灰化中,如图2所示,在包含配线34的上面及侧面的基板表面上,粘附残渣(等离子蚀刻残渣及灰化残渣)36。该残渣36源自变质的光致抗蚀剂膜、氮化钛膜32、Al合金膜30、钛膜28、及氮化钛膜26。
因此,用于除去光致抗蚀剂膜的剩余部分的灰化后,利用本发明的清洗组合物,清洗直到配线34为止形成的半导体基板10。这样,除去附着在直到配线34为止形成的半导体基板10的表面上的等离子蚀刻残渣及灰化残渣。
另外、上述实施方式中,对于形成包含Al合金膜12、30的配线16、34的情况进行了说明,但配线的材料并不限定于上述的材料。作为配线,除以Al或Al合金组成的Al为主材料的配线以外,可以形成以Cu或Cu合金组成的Cu为主材料的配线。
另外,本发明的清洗组合物可以广泛应用于从包含铝及/或铜的半导体基板清洗等离子蚀刻残渣及/或灰化残渣的工序,铝或铜优选包含在半导体用基板上形成的配线结构中。
[实施例]
以下,通过实施例对本发明进一步详细地进行说明。但是,本发明并不限定于这些实施例。
<通过扫描型电子显微镜观察残渣>
对于上述第1及第2实施方式,通孔形成后,在利用本发明的清洗组合物清洗前,通过扫描电子显微镜(SEM:Scanning Electron Microsope)观察图案晶片,结果任意通孔壁面上都看到了等离子蚀刻残渣及灰化残渣。另外,对于上述第3实施方式,配线形成后,利用本发明的清洗组合物清洗前,通过SEM进行观察图案晶片,结果配线的上面及侧面观察到了等离子蚀刻残渣及灰化残渣。
<实施例1~62、比较例1~7>
接下来,制备以下表1~3中表示的组成的清洗组合物1~69(实施例1~62、比较例1~7)。上述图案晶片的切片(约2cm×2cm)浸渍在调温到表1~3中所述的温度的各清洗组合物中,在表1~3中所述的浸渍时间后取出图案晶片,立即用超纯水水洗、N2干燥。通过SEM观察浸渍试验后的图案晶片的切片的断面及表面,对光致抗蚀剂及残渣(等离子蚀刻残渣及灰化残渣)的除去性、以及Al及TiN的腐蚀性,根据下述的判断基准进行评价。除去性及腐蚀性的评价结果汇总在以下的表4及表5。
评价标准如下所示。
[第1实施方式:通路图案A]
<除去通孔周围表面的残渣>
◎:完全除去光致抗蚀剂及残渣。
○:几乎完全除去光致抗蚀剂及残渣。
△:残留光致抗蚀剂及残渣的溶解不良物。
×:几乎没有除去光致抗蚀剂及残渣。
<通孔底的TiN腐蚀>
◎:没有发现TiN的腐蚀。
○:相对于配线在5%以下引起了TiN的腐蚀。
△:相对于配线在10%以下引起了TiN的腐蚀。
×:TiN完全消失。
[第2实施方式:通路图案B]
<除去通孔周围的表面的残渣>
◎:完全除去光致抗蚀剂及残渣。
○:几乎完全除去光致抗蚀剂及残渣。
△:残留光致抗蚀剂及残渣的溶解不良物。
×:几乎没有除去光致抗蚀剂及残渣。
<通孔底的Al腐蚀>
◎:没有发现Al的腐蚀。
○:相对于配线在5%以下引起了Al的腐蚀。
△:相对于配线在10%以下引起了Al的腐蚀。
×:Al配线完全消失。
[第3实施方式:配线图案]
<除去配线侧面·上面的残渣>
◎:完全除去光致抗蚀剂及残渣。
○:几乎完全除去光致抗蚀剂及残渣。
△:残留光致抗蚀剂及残渣的溶解不良物。
×:几乎没有除去光致抗蚀剂及残渣。
<Al腐蚀(凹窝)>
◎:没有发现Al的凹窝。
○:相对于配线在5%以下引起了Al的凹窝。
△:相对于配线在10%以下引起了Al的凹窝。
×:Al配线完全消失。
另外,在上記评价中,期望除去性及腐蚀性中全部评价为◎。另外,进一步期望短时间、低温度下评价为◎。
另外,上述表1~3的(成分b)、(成分d)、(成分e)及(成分g)中所谓的“%”是指重量%,(成分a)中所谓的“剩余部分”是指(成分a)~(成分e)及(成分g)的各成分的合计为100重量%那样的剩余部分。另外,(成分C)中所谓的“(pH调节)”,是指成为示于表1~3中的pH值地添加(成分C)。各实施例及各比较例中的(成分C)相对于清洗组合物的总重量为1~10重量%的范围,并且添加到成为示于表1~3中的pH值的量。
另外,在上述表3中,比较例1相当于专利第3871257号公报中所述的实施例2。
[表4]
[表5]
如上述表4及表5所示,在使用本发明的清洗组合物的实施例1~62中,没有Al、TiN的腐蚀,光致抗蚀剂、及等离子蚀刻残渣及灰化残渣的除去性优异。
另外,从实施例4~21的评价结果中,了解到即使变更使用的有机酸也能得到优异的清洗性及防腐蚀性。其中,使用作为有机酸的柠檬酸的实施例4得到最良好的结果。
另外,从实施例22~27的评价结果中,了解到通过添加任意成分的水溶性有机溶剂,金属的防腐蚀进一步上升。
另外,从实施例28~30的评价结果中,了解到优选合用多种有机酸。
另外,从实施例31~34的评价结果中,了解到即使变更使用的羟胺及/或其盐也能得到优异的清洗性及防腐蚀性。
另外,从实施例35~40的评价结果中,了解到即使变更使用的碱性有机化合物也能得到优异的清洗性及防腐蚀性。
另外,从实施例41~50的评价结果中,了解到使用作为碱性有机化合物的有机胺时,及即使合用作为碱性有机化合物的有机胺及季铵氢氧化物时,也能得到优异的清洗性及防腐蚀性。
另外,从实施例51~53的评价结果中,了解到pH即使为比较高的7.6时,也能得到优异的清洗性及防腐蚀性。
另外,从实施例54的评价结果中,了解到即使在含有必需成分的同时含有任意成分的水溶性有机溶剂,也能得到优异的清洗性及防腐蚀性。另外,从实施例55的评价结果中,了解到即使在含有必需成分的同时含有作为任意成分的含氨基羧酸及水溶性有机溶剂,也能得到优异的清洗性及防腐蚀性。
另外,如果将实施例57的评价结果和实施例58~59的评价结果进行对比,则可了解到对于清洗组合物的pH为8以上的情况,通过使用含氨基羧酸,Al的防腐蚀性上升。从实施例60的评价结果和实施例61的评价结果的对比也可了解到相同的效果。
另外,在使用本发明的清洗组合物的清洗中,可以比较自由地选择浸渍温度、浸渍时间,可以在低温度、短时间进行清洗。进而,在使用本发明的清洗组合物的清洗中,即使在浸渍时间延长的强制条件下,也不进行Al、TiN的腐蚀。
另一方面,如上述的表5所示,在比较例1中,通路图案的清洗性变差。另外,如比较例2、3所示,和比较例1相比仅单纯提高了pH,不能充分改善通路图案的清洗性。
另外,在不使用有机酸的比较例4中,产生Al的腐蚀。
另外,在羟胺及其盐都不使用的比较例5中,对于通路图案及配线图案的哪一个都没有得到充分的清洗性。
另外,在pH超过9的比较例6、7中,产生Al、TiN的腐蚀。
进而,各比较例中,即使调节浸渍时间、浸渍温度,也没有显示充分的除去性、腐蚀性。为了兼备残渣除去和腐蚀防止,必需是实施例中所述的组成及pH。
Claims (19)
1.一种清洗方法,其包含制备清洗组合物的制备工序以及利用所述清洗组合物清洗在半导体基板上形成的等离子蚀刻残渣及/或灰化残渣的清洗工序,其中,所述半导体基板含有Al和TiN,所述清洗组合物包含:
成分a:水、
成份b:羟基胺及/或其盐、
成分c:碱性有机化合物、和
成分d:有机酸,
作为成份b单独使用1种羟胺硫酸盐,
成份c为季铵氢氧化物,
所述清洗组合物的pH为7.2~9。
2.如权利要求1所述的清洗方法,其中,成分a相对于清洗组合物的总重量的含量为50~99.5重量%。
3.如权利要求1所述的清洗方法,其中,成份b相对于清洗组合物的总重量的含量为0.01~30.0重量%。
4.如权利要求1所述的清洗方法,其中,成份c为四烷基氢氧化铵。
5.如权利要求1所述的清洗方法,其中,成份c相对于清洗组合物总重量的含量为0.01~20.0重量%。
6.如权利要求1所述的清洗方法,其中,成分d为单官能性、双官能性、三官能性或四官能性有机酸。
7.如权利要求6所述的清洗方法,其中,成分d为选自柠檬酸、乳酸、醋酸、丙酸、苹果酸、酒石酸、丙二酸、乙二酸、琥珀酸、葡糖酸、乙醇酸、二乙醇酸、马来酸、苯甲酸、邻苯二甲酸、水杨酸、水杨基氧肟酸及邻苯二甲基氧肟酸中的至少一种化合物。
8.如权利要求6所述的清洗方法,其中,成分d为羟基羧酸。
9.如权利要求8所述的清洗方法,其中,成分d为选自柠檬酸、苹果酸、酒石酸、乙醇酸、葡糖酸及乳酸中的至少一种化合物。
10.如权利要求1所述的清洗方法,其中,成分d相对于清洗组合物的总重量的含量为0.01~20.0重量%。
11.如权利要求1所述的清洗方法,其中,pH为7.2~8.5。
12.如权利要求11所述的清洗方法,其中,pH为7.2~8.4。
13.如权利要求1所述的清洗方法,其中,进一步含有成分e:含氨基羧酸。
14.如权利要求13所述的清洗方法,其中,成分e为组氨酸及/或精氨酸。
15.如权利要求13所述的清洗方法,其中,成分e相对于清洗组合物的总重量的含量为0.01~5.0重量%。
16.如权利要求1所述的清洗方法,其中,所述半导体基板还含有铜。
17.清洗组合物在除去在半导体基板上形成的等离子蚀刻残渣及/或灰化残渣中的应用,其中,所述半导体基板含有Al和TiN,所述清洗组合物包含:
成分a:水、
成份b:羟基胺及/或其盐、
成分c:碱性有机化合物、和
成分d:有机酸,
作为成份b单独使用1种羟胺硫酸盐,
成份c为季铵氢氧化物,
所述清洗组合物的pH为7.2~9。
18.一种半导体装置的制造方法,其包含:
对于半导体基板进行等离子蚀刻的蚀刻工序、及/或
对于半导体基板的抗蚀剂进行灰化的灰化工序、以及
利用清洗组合物,清洗在所述蚀刻工序及/或所述灰化工序中在所述半导体基板上形成的等离子蚀刻残渣及/或灰化残渣的清洗工序,其中,所述半导体基板含有Al和TiN,所述清洗组合物包含:
成分a:水、
成份b:羟基胺及/或其盐、
成分c:碱性有机化合物、和
成分d:有机酸,
作为成份b单独使用1种羟胺硫酸盐,
成份c为季铵氢氧化物,
所述清洗组合物的pH为7.2~9。
19.如权利要求18所述的半导体装置的制造方法,其中,所述半导体基板还含有铜。
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