CN116438284A - 微电子装置清洁组合物 - Google Patents
微电子装置清洁组合物 Download PDFInfo
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- CN116438284A CN116438284A CN202180075325.4A CN202180075325A CN116438284A CN 116438284 A CN116438284 A CN 116438284A CN 202180075325 A CN202180075325 A CN 202180075325A CN 116438284 A CN116438284 A CN 116438284A
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- Prior art keywords
- acid
- composition
- amino
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- alkyl
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- GSGDTSDELPUTKU-UHFFFAOYSA-N nonoxybenzene Chemical compound CCCCCCCCCOC1=CC=CC=C1 GSGDTSDELPUTKU-UHFFFAOYSA-N 0.000 description 1
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- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- UHGIMQLJWRAPLT-UHFFFAOYSA-N octadecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCCCOP(O)(O)=O UHGIMQLJWRAPLT-UHFFFAOYSA-N 0.000 description 1
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical class CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 1
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- 239000011368 organic material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
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- HEBKCHPVOIAQTA-ZXFHETKHSA-N ribitol Chemical compound OC[C@H](O)[C@H](O)[C@H](O)CO HEBKCHPVOIAQTA-ZXFHETKHSA-N 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
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- 150000003384 small molecules Chemical class 0.000 description 1
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- 235000011069 sorbitan monooleate Nutrition 0.000 description 1
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- 238000005507 spraying Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
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- 239000001384 succinic acid Substances 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229960001367 tartaric acid Drugs 0.000 description 1
- FBWNMEQMRUMQSO-UHFFFAOYSA-N tergitol NP-9 Polymers CCCCCCCCCC1=CC=C(OCCOCCOCCOCCOCCOCCOCCOCCOCCO)C=C1 FBWNMEQMRUMQSO-UHFFFAOYSA-N 0.000 description 1
- YNJQKNVVBBIPBA-UHFFFAOYSA-M tetrabutylazanium;trifluoromethanesulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)F.CCCC[N+](CCCC)(CCCC)CCCC YNJQKNVVBBIPBA-UHFFFAOYSA-M 0.000 description 1
- BVQJQTMSTANITJ-UHFFFAOYSA-N tetradecylphosphonic acid Chemical compound CCCCCCCCCCCCCCP(O)(O)=O BVQJQTMSTANITJ-UHFFFAOYSA-N 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical compound CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- ZOMVKCHODRHQEV-UHFFFAOYSA-M tetraethylphosphanium;hydroxide Chemical compound [OH-].CC[P+](CC)(CC)CC ZOMVKCHODRHQEV-UHFFFAOYSA-M 0.000 description 1
- YQIVQBMEBZGFBY-UHFFFAOYSA-M tetraheptylazanium;bromide Chemical compound [Br-].CCCCCCC[N+](CCCCCCC)(CCCCCCC)CCCCCCC YQIVQBMEBZGFBY-UHFFFAOYSA-M 0.000 description 1
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- AHNISXOXSNAHBZ-UHFFFAOYSA-M tetrakis-decylazanium;bromide Chemical compound [Br-].CCCCCCCCCC[N+](CCCCCCCCCC)(CCCCCCCCCC)CCCCCCCCCC AHNISXOXSNAHBZ-UHFFFAOYSA-M 0.000 description 1
- OKIZCWYLBDKLSU-UHFFFAOYSA-N tetramethylazanium;hydrochloride Chemical compound Cl.C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-N 0.000 description 1
- CRUVUWATNULHFA-UHFFFAOYSA-M tetramethylphosphanium;hydroxide Chemical compound [OH-].C[P+](C)(C)C CRUVUWATNULHFA-UHFFFAOYSA-M 0.000 description 1
- OORMKVJAUGZYKP-UHFFFAOYSA-M tetrapropylphosphanium;hydroxide Chemical compound [OH-].CCC[P+](CCC)(CCC)CCC OORMKVJAUGZYKP-UHFFFAOYSA-M 0.000 description 1
- 229940113082 thymine Drugs 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- 150000008648 triflates Chemical class 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- IJGSGCGKAAXRSC-UHFFFAOYSA-M tris(2-hydroxyethyl)-methylazanium;hydroxide Chemical compound [OH-].OCC[N+](C)(CCO)CCO IJGSGCGKAAXRSC-UHFFFAOYSA-M 0.000 description 1
- ZQTYRTSKQFQYPQ-UHFFFAOYSA-N trisiloxane Chemical compound [SiH3]O[SiH2]O[SiH3] ZQTYRTSKQFQYPQ-UHFFFAOYSA-N 0.000 description 1
- JVFFWGJAAQAIBS-UHFFFAOYSA-K trisodium 2,2-dioctyl-3-sulfonatobutanedioate Chemical compound [Na+].C(CCCCCCC)C(C(C(=O)[O-])S(=O)(=O)[O-])(C(=O)[O-])CCCCCCCC.[Na+].[Na+] JVFFWGJAAQAIBS-UHFFFAOYSA-K 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- 238000004876 x-ray fluorescence 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; 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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
- C11D7/3218—Alkanolamines or alkanolimines
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/28—Heterocyclic compounds containing nitrogen in the ring
-
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
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- C11D3/32—Amides; Substituted amides
- C11D3/323—Amides; Substituted amides urea or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11D3/16—Organic compounds
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- C11D3/361—Phosphonates, phosphinates or phosphonites
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- C11D7/36—Organic compounds containing phosphorus
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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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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- H01L21/02065—Cleaning during device manufacture during, before or after processing of insulating layers the processing being a planarization of insulating layers
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Abstract
本发明提供一种用于清洁微电子装置衬底的组合物。所述组合物可用于清洁具有暴露的钴、钼、铜、钼、钨和电介质表面的过程中微电子装置衬底。也提供一种清洁此类装置的方法和包含所述组合物的组分中的一或多者的试剂盒。
Description
技术领域
本发明大体上涉及含水组合物,其用于清洁微电子装置衬底的表面,如用于清洁来自微电子装置衬底表面的残留物。
背景技术
微电子装置衬底用于制备集成电路装置。微电子装置衬底包含基底,诸如具有高度平坦表面的硅晶圆。经由多次选择性放置和去除步骤,将电子功能特征的区域添加到基底的平坦表面上。所述特征通过选择性添加和去除会展示绝缘、导电或半导电性质的电子功能材料制成。这些电子功能材料通过使用包含光阻剂、化学蚀刻剂的加工材料和含有磨料粒子和帮助加工表面的化学材料的浆液按所需放置。
集成电路的一个特征为导电"互连"阵列,其也称作"线"和"通路"。作为集成电路的部分,导电互连功能为在各种其它电子特征中和之间传导电流。各互连以导电材料的线或薄膜形式,所述导电材料在绝缘材料(即,电介质材料,如电介质材料)中形成的开口内延伸并且通过所述开口定义(在形状和大小上)。电介质材料充当极其紧密间隔的互连结构之间和互连结构与集成电路的其它电子特征之间的绝缘体。
必须选择用于产生互连和介电结构的材料的类型以适当用作以高效率和高可靠性表现的集成电路的一部分。例如,互连的导电材料应为在材料之间存在电压下随时间并且在使用期间不过度迁移(例如,扩散)到相邻电介质材料的类型;互连材料到相邻电介质材料的此迁移通常被称作"电迁移"。同时,组合的互连和电介质材料结构必须具有足够完整性,包含在这些材料之间的界面,以导致低程度的缺陷和高程度的性能可靠性。例如,强结合必须在界面处存在以防止在使用期间电介质材料与互连材料分离。
互连过去通常由铝或钨制成,且最近由铜制成。铜相对于铝和钨具有有利高的导电性。此外,铜基互连如与铝相比提供对电迁移的更好的抗性,从而提高集成电路随时间的可靠性。然而,铜离子可倾向于在足够电偏压下扩散到二氧化硅(SiO2),并且铜与二氧化硅和其它电介质材料的粘附可为差的。
为防止铜与电介质材料的这些负相互作用,最近集成电路结构已经设计以包含铜互连结构与相邻电介质材料之间的阻挡层。实例阻挡层可为导电材料或非导电材料,实例包括钽(Ta)、氮化钽(TaNx)、钨(W)、钛(Ti)、氮化钛(TiN)、钌(Ru)、钴(Co)、钼(Mo)、铼(Rh)及其合金。
将微电子装置的各种特征放在衬底上的方法包括将绝缘材料(例如,电介质等)、半导体材料、金属材料(例如,导电线和通路(即,互连))等选择性放在衬底表面上。这些材料的选择性放置和去除可涉及在诸如光阻剂涂覆、蚀刻(例如,湿法蚀刻、等离子体蚀刻)、化学-机械加工(也称作化学-机械抛光、化学-机械平坦化或简称作"CMP")和灰化("等离子体灰化")的步骤中使用加工组合物,诸如尤其光阻剂、蚀刻剂、含有磨料和化学材料的CMP浆液和等离子体。
化学-机械加工为一种工艺,通过所述工艺将其极少量(厚度)的材料自微电子装置衬底表面精确去除以抛光(或"平坦化")所述表面,从而准备后续材料层待施覆到经加工表面。化学-机械加工涉及表面的高度精确机械研磨,联合化学材料的可控相互作用(诸如存在于表面或自表面去除的材料的氧化、还原或螯合)。通常,以高选择性优先去除衬底表面上的一种类型的材料(例如,金属超载荷),与也存在于所述表面处的一或多种其它材料(例如,电介质材料)的减少去除程度相比。
CMP工艺涉及将"浆液"施覆到表面连同使所述表面与正在移动的CMP垫接触。"浆液"为液体组合物,其含有提供表面的机械研磨的微磨料粒子,连同与表面的材料化学相互作用以促进某种材料自表面选择性去除且通常抑制另一表面材料的去除的化学材料。将浆液施覆到表面,同时CMP垫以所需量的压力和移动与所述表面接触以促进研磨所选材料和自所述表面化学去除。垫的机械作用和磨料粒子抵靠表面移动,连同化学成分作用的组合达成表面的具有所需低水平的缺陷和残留物的所需去除、平坦化和抛光。所述CMP工艺应产生高度平面、低缺陷、低残留物表面,可向所述表面施覆微电子装置之后续层。
在加工步骤(例如,化学-机械加工、蚀刻、灰化等)后,至少一定量的残留物将存在于衬底表面处。残留物可包含来自CMP浆液的磨料粒子或其它加工材料;为CMP浆液的一部分的活性化学成分(例如,氧化剂、催化剂、抑制剂)或其它加工组合物(例如,蚀刻剂);加工材料或其成分的反应产物或副产物;化学蚀刻剂;光阻剂聚合物或其它固体加工成分等。任何此残留物必须在进行微电子装置制造工艺之后续步骤之前通过清洁表面来去除,以避免缺陷或降低装置性能或可靠性的其它潜在来源。
在(例如)蚀刻步骤后,在CMP步骤后,或用于制造多层微电子装置的另一步骤后通常用于清洁微电子衬底表面的某些方法和设备包括涉及清洁溶液在表面上方的流动与超高频音波、喷射或刷洗组合以去除残留物和污染物的那些。典型清洁溶液为碱性溶液,例如,含有适宜氢氧化物化合物连同其它化学材料,所述其它化学材料一起通过与残留物化学相互作用将残留物自表面去除。清洁溶液不仅应自表面有效去除高百分比的残留物,而且必须关于衬底的功能特征为安全。清洁溶液必须不引起对那些特征的损害。例如,清洁溶液应不引起对衬底的金属特征的腐蚀(即,氧化),例如,不应氧化可作为互连或阻挡特征存在的衬底的铜或钴金属特征。
不断寻求新颖可用并且改良的清洁组合物和特定成分,尤其与新颖微电子装置结构,如现可包含钨、铜、钴、钼和电介质材料的暴露表面的那些结构一起使用。
发明内容
存在对于自过程中微电子装置衬底表面去除残留物方面有效的组合物和方法的持续需求。本发明提供这些组合物和方法,同时也抑制对某些金属特征,如钴、铜、钼和钨,以及介电表面电介质材料,包括(但不限于)二氧化硅、氮化硅、碳化硅、氧氮化硅、氧碳化硅、硅、碳、电介质(如SiLKTM电介质(陶氏化学公司(Dow Chemical)))、倍半硅氧烷或BlackPECVD(应用材料公司(Applied Materials))的损害(即,腐蚀),其等可在微电子装置上以暴露特征存在。
在一个方面,本发明提供组合物,其包含:
a.水;
b.络合剂;和
c.氨基(C6-C12烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂。
也提供一种使用这些组合物清洁微电子装置衬底的方法和包含所述组合物的一或多种组分于一或多个容器中的试剂盒。
具体实施方式
在第一方面,本发明提供组合物,其包含:
a.水;
b.络合剂;和
c.氨基(C6-C12烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂。
在一个实施例中,所述组合物包含约60到90重量%水,约0.01到约10重量%络合剂,和约0.1到约5重量%,或约0.1到约2重量%氨基(C6-C12烷基)醇。
在一个实施例中,所述组合物由以上组分a.到d.组成或基本上由其组成。
如本文中所用,除非另有指定,否则描述为"基本上由一或多个指定条项组成"的组合物或组合物的成分是指仅由那些指定条项与不超过无实质量的其它(另外)材料组成,例如,基于组合物或成分的总重量计,仅含有指定条项并且不超过5、3、2、1、0.5、0.1、0.05或0.01重量%另外成分的组合物或成分。如本文中所用,描述为"由一或多个指定条项组成"的组合物或组合物的成分是指仅由那些指定条项组成的组合物或成分。
在某些实施例中,pH将为酸性,例如,约1.5到约6且在其它实施例中,pH将为碱性,例如,约9到约14。本领域一般技术人员将知晓适用于这个目的的那些酸和碱。
在一个实施例中,pH调节剂为碱。出于这个目的,pH调节剂的非限制性实例包括:氢氧化胆碱、四丁基氢氧化鏻(TBPH)、四甲基氢氧化鏻、四乙基氢氧化鏻、四丙基氢氧化鏻、苄基三苯基氢氧化鏻、甲基三苯基氢氧化鏻、乙基三苯基氢氧化鏻、N-丙基三苯基氢氧化鏻、四乙基氢氧化铵(TEAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵(TBAH)、三甲基乙基氢氧化铵、二乙基二甲基氢氧化铵、三丁基甲基氢氧化铵(TBMAH)、苄基三甲基氢氧化铵(BTMAH)、四甲基铵盐酸盐(TMAC)、三(2-羟乙基)甲基氢氧化铵、二乙基二甲基氢氧化铵、精氨酸、氢氧化钾、氢氧化铯及其组合。
在一个实施例中,所述pH调节剂选自氢氧化胆碱和四乙基氢氧化铵(TEAH)。
在另一实施例中,所述pH调节剂为酸,并且可选自硝酸、柠檬酸、硫酸、磷酸、盐酸、氢溴酸、甲磺酸、苯磺酸和对甲苯磺酸、三氟甲磺酸、乙酸、乳酸、乙醇酸或其任何组合。
在一个实施例中,所述络合剂选自:胺、氨基酸和季铵化氨基酸,包括(但不限于)4-(2-羟乙基)吗啉(HEM)、1,2-环己二胺-N,N,N',N'-四乙酸(CDTA)、羟乙基二亚乙基四胺三乙酸(HEDTA)、乙二胺四乙酸(EDTA)、间苯二甲胺(MXDA)、亚氨基二乙酸(IDA)、三甲胺、异丙醇胺、二异丙醇胺、哌嗪、羟乙基哌嗪、二羟基乙基哌嗪、葡糖胺、N-甲基葡糖胺、2-(羟乙基)亚氨基二乙酸(HIDA)、次氮基三乙酸、硫脲、1,1,3,3-四甲基脲、脲、脲衍生物、尿酸、丙氨酸、精氨酸、天冬酰胺、天冬氨酸、半胱氨酸、谷氨酸、谷胺酰胺、组氨酸、异亮氨酸、亮氨酸、赖氨酸、甲硫氨酸、苯丙氨酸、脯氨酸、丝氨酸、苏氨酸、色氨酸、酪氨酸、缬氨酸、牛磺酸、甜菜碱及其组合。
或者,或除了以上提及的络合剂外,另外络合剂可包括膦酸盐(例如,1-羟基亚乙基-1,1-二膦酸(HEDP)、1,5,9-三氮杂环十二烷-N,N',N”-三(亚甲基膦酸)(DOTRP)、1,4,7,10-四氮杂环十二烷-N,N',N”,N”'-四(亚甲基膦酸)(DOTP)、次氮基三(亚甲基)三膦酸、二亚乙基三胺五(亚甲基膦酸)(DETAP)、氨基三(亚甲基膦酸)、双(六亚甲基)三胺五亚甲基膦酸、1,4,7-三氮杂环壬烷-N,N',N”-三(亚甲基膦酸)(NOTP)、羟乙基二膦酸盐、次氮基三(亚甲基)膦酸、2-膦酰基-丁烷-1,2,3,4-四甲酸、羧基乙基膦酸、氨基乙基膦酸、草甘膦、乙二胺四(亚甲基膦酸)苯基膦酸、其盐及其衍生物)和/或羧酸(例如,草酸、琥珀酸、马来酸、苹果酸、丙二酸、己二酸、酞酸、柠檬酸、柠檬酸钠、柠檬酸钾、柠檬酸铵、丙三羧酸、三羟甲基丙酸、吡啶甲酸、吡啶二甲酸、水杨酸、磺基水杨酸、磺基酞酸、磺基琥珀酸、无水甜菜碱、葡糖酸、酒石酸、葡糖醛酸、2-羧基吡啶)和/或磺酸,如(4,5-二羟基-1,3-苯二磺酸二钠盐无水甜菜碱)。在某些实施例中,所述络合剂包括次氮基(三亚甲基膦酸)和亚氨基二乙酸。在某些实施例中,所述至少一种络合剂包括选自单乙醇胺、三乙醇胺、硫酸、柠檬酸及其组合的物质。在一个实施例中,络合剂于组合物中的量在基于所述去除组合物的总重量计约0.01重量%到约10重量%的范围内。
在一个实施例中,所述络合剂选自1-羟基亚乙基-1,1-二膦酸、1,5,9-三氮杂环十二烷-N,N',N”-三(亚甲基膦酸)、1,4,7,10-四氮杂环十二烷-N,N',N”,N”'-四(亚甲基膦酸)、次氮基三(亚甲基)三膦酸、二亚乙基三胺五(亚甲基膦酸)、琥珀酸、柠檬酸、柠檬酸铵、酒石酸、亚氨基二乙酸、氨基三(亚甲基膦酸)、双(六亚甲基)三胺膦酸、1,4,7-三氮杂环壬烷-N,N',N”-三(亚甲基膦酸)、其盐及其衍生物。在一个实施例中,所述络合剂为1-羟基亚乙基-1,1-二膦酸或其盐。
在一个实施例中,所述氨基(C8-C12烷基)醇选自3-氨基-4-辛醇、DL-2-氨基-1-己醇、2-(丁氨基)乙醇、1-氨基环己醇和8-氨基-1-辛醇。在一个实施例中,所述氨基(C6-C10烷基)醇包括3-氨基-4-辛醇。
如上所指定,本发明的组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂。在另一实施例中,本发明的组合物也不含选自草酸、琥珀酸、L-酒石酸及其组合的腐蚀抑制剂。在另一实施例中,所述组合物不含任何腐蚀抑制剂。
在另一方面,本发明提供组合物,其包含:
a.水;
b.氢氧化胆碱;
c.1-羟基亚乙基-1,1-二膦酸;或
d.单乙醇胺;和
e.氨基(C6-C10烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂。
在一个实施例中,所述氨基(C8-C12烷基)醇选自3-氨基-4-辛醇、DL-2-氨基-1-己醇、2-(丁氨基)乙醇、1-氨基环己醇和8-氨基-1-辛醇。在另一实施例中,所述氨基(C8-C12烷基)醇包括3-氨基-4-辛醇。在另一实施例中,所述组合物基本上由以上组分a.到e.组成。
在本发明的方面的另外实施例中,所述组合物进一步包含水可分散性或水溶性聚合物。当存在时,这些聚合物包括(但不限于)甲基丙烯酸均聚物和与(例如)丙烯酰胺基甲基丙磺酸和马来酸的共聚物;马来酸/乙烯基醚共聚物;聚(乙烯基吡咯烷酮)/乙酸乙烯酯;均聚物,如磷酸化的聚乙二醇低聚物、聚(丙烯酸)(PAA)、聚(丙烯酰胺)、聚(乙酸乙烯酯)、聚(乙二醇)(PEG)、聚丙二醇(PPG)、聚(苯乙烯磺酸)、聚(乙烯基磺酸)、聚(乙烯基膦酸)、聚(乙烯基膦酸)、聚(乙烯亚胺)、聚(丙烯亚胺)、聚烯丙胺、聚环氧乙烷(PEO)、聚乙烯基吡咯烷酮(PVP)、PPG-PEG-PPG嵌段共聚物、PEG-PPG-PEG嵌段共聚物、聚(乙烯醇)、聚丙烯酸(羟乙基)酯、聚甲基丙烯酸(羟乙基)酯、羟乙基纤维素、甲基羟乙基纤维素、羟丙基纤维素、甲基羟丙基纤维素、黄原胶、藻酸钾、果胶、羧甲基纤维素、葡糖胺、聚(二烯丙基二甲基铵)氯化物、PEG化(即,聚乙二醇化)甲基丙烯酸酯/丙烯酸酯共聚物、聚MADQuat(聚(2-甲基丙烯酰氧基乙基三甲基氯化铵)CAS号26161-33-1)及其共聚物、二甲氨基甲基丙烯酸酯聚合物及其共聚物、三甲基铵甲基丙烯酸甲酯聚合物及其共聚物、及其组合。以上共聚物可为无规或嵌段共聚物。当存在时,聚合物于组合物中的量基于所述组合物的总重量在约0.0001重量%到约5重量%的范围内。
在另一实施例中,所述组合物进一步包含表面活性剂。如本文中所用,术语“表面活性剂”是指降低两种液体之间或液体与固体之间的表面张力(或界面张力)的有机化合物,通常含有疏水性基团(例如,烃(例如,烷基)“尾”)和亲水性基团的有机两亲性化合物。当存在时,用于本文中所述组合物中的表面活性剂包括(但不限于)两性盐、阳离子表面活性剂、阴离子表面活性剂、两性离子表面活性剂、非离子表面活性剂及其组合,包括(但不限于)癸基膦酸、十二烷基膦酸(DDPA)、十四烷基膦酸、十六烷基膦酸、双(2-乙基己基)磷酸盐、十八烷基膦酸、全氟庚酸、全氟癸酸、三氟甲磺酸、膦酰基乙酸、十二烷基苯磺酸(DDBSA)、苯磺酸或其盐(任选经一或多个C8-C18直链或支链烷基取代)、十二烯基琥珀酸、二(十八烷基)磷酸氢盐、十八烷基磷酸二氢盐、十二烷基胺、十二烯基琥珀酸单二乙醇酰胺、月桂酸、棕榈酸、油酸、桧酸、12-羟基硬脂酸、十八烷基膦酸(ODPA)、十二烷基磷酸盐。涵盖的非离子表面活性剂包括(但不限于)聚氧乙烯月桂基醚、十二烯基琥珀酸单二乙醇酰胺、乙二胺四(乙氧基化物-嵌段-丙氧基化物)四醇、聚乙二醇、聚丙二醇、聚乙二醇或聚丙二醇醚、基于环氧乙烷和环氧丙烷的嵌段共聚物、聚氧丙烯蔗糖醚、叔辛基苯氧基聚乙氧基乙醇、10-乙氧基-9,9-二甲基癸-1-胺、聚氧乙烯(9)壬基苯基醚、支链聚氧乙烯(40)壬基苯基醚、支链二壬基苯基聚氧乙烯、壬基酚烷氧基化物、聚氧乙烯山梨糖醇六油酸酯、聚氧乙烯山梨糖醇四油酸酯、聚乙二醇脱水山梨糖醇单油酸酯、脱水山梨糖醇单油酸酯、醇烷氧基化物、烷基-聚葡糖苷、全氟丁酸乙酯、1,1,3,3,5,5-六甲基-1,5-双[2-(5-降冰片烯-2-基)乙基]三硅氧烷、单体十八烷基硅烷衍生物、经硅氧烷改性的聚硅氮烷、聚硅氧-聚醚共聚物和乙氧基化含氟表面活性剂。涵盖的阳离子表面活性剂包括(但不限于)鲸蜡基三甲基溴化铵(CTAB)、十七烷氟辛烷磺酸、四乙基铵、硬脂酰基三甲基氯化铵、溴化4-(4-二乙氨基苯基偶氮基)-1-(4-硝基苄基)吡啶鎓、氯化鲸蜡基吡啶鎓单水合物、苯扎氯铵、苄索氯铵(benzethonium chloride)、苄基二甲基十二烷基氯化铵、苄基二甲基十六烷基氯化铵、十六烷基三甲基溴化铵、二甲基二-(十八烷基)氯化铵、十二烷基三甲基氯化铵、十六烷基三甲基对甲苯磺酸铵、二-(十二烷基)二甲基溴化铵、二(氢化牛脂)二甲基氯化铵、四庚基溴化铵、四(癸基)溴化铵和奥芬溴铵(oxyphenonium bromide)、盐酸胍(C(NH2)3Cl)或三氟甲磺酸盐(如四丁基三氟甲磺酸铵)、二甲基二-(十八烷基)氯化铵、二甲基二-(十六烷基)溴化铵、二(氢化牛脂)二甲基氯化铵和聚氧乙烯(16)牛脂乙基乙硫酸铵。涵盖的阴离子表面活性剂包括(但不限于)聚(丙烯酸钠盐)、聚丙烯酸铵、聚氧乙烯月桂基醚钠、二己基磺基琥珀酸钠、十二烷基硫酸钠、二辛基磺基琥珀酸盐、2-磺基琥珀酸盐、2,3-二巯基-1-丙磺酸盐、二环己基磺基琥珀酸钠盐、7-乙基-2-甲基-4-十一烷基硫酸钠、磷酸盐含氟表面活性剂、含氟表面活性剂和聚丙烯酸盐。两性离子表面活性剂包括(但不限于)炔二醇或经改性的炔二醇、环氧乙烷烷基胺、N,N-二甲基十二烷基胺N-氧化物、椰油丙酸钠、3-(N,N-二甲基豆蔻基铵基)丙磺酸酯和(3-(4-庚基)苯基-3-羟丙基)二甲铵基丙磺酸酯。
在另一实施例中,所述组合物进一步包含水可混溶溶剂和/或佐剂。
在一个实施例中,所述水可混溶溶剂选自二醇和二醇醚、甲醇、乙醇、异丙醇、丁醇和选自C2-C4二醇和C2-C4三醇、四氢呋喃甲醇的高级醇(如3-氯-1,2-丙二醇、3-氯-1-丙硫醇、1-氯-2-丙醇、2-氯-1-丙醇、3-氯-1-丙醇、3-溴-1,2-丙二醇、1-溴-2-丙醇、3-溴-1-丙醇、3-碘-1-丙醇、4-氯-1-丁醇、2-氯乙醇)、二氯甲烷、氯仿、乙酸、丙酸、三氟乙酸、四氢呋喃、N-甲基吡咯烷酮、环己基吡咯烷酮、N-辛基吡咯烷酮、N-苯基吡咯烷酮、甲基二乙醇胺、甲酸甲酯、二甲基甲酰胺、二甲亚砜、四亚甲基砜、乙醚、苯氧基-2-丙醇、丙酰苯、乳酸乙酯、乙酸乙酯、苯甲酸乙酯、乙腈、丙酮、乙二醇、丙二醇、1,3-丙二醇、二噁烷、丁酰内酯、碳酸伸丁酯、碳酸乙二酯、碳酸丙二酯、二丙二醇、二乙二醇单甲醚、三乙二醇单甲醚、二乙二醇单乙醚、三乙二醇单乙醚、乙二醇单丙醚、乙二醇单丁醚、二乙二醇单丁醚、三乙二醇单丁醚、乙二醇单己醚、二乙二醇单己醚、乙二醇苯基醚、丙二醇甲醚、二丙二醇甲醚、三丙二醇甲醚、二丙二醇二甲醚、二丙二醇乙醚、丙二醇正丙醚、二丙二醇正丙醚、三丙二醇正丙醚、丙二醇正丁醚、二丙二醇正丁醚、三丙二醇正丁醚、丙二醇苯醚、乙二醇单苯醚、二乙二醇单苯醚、六乙二醇单苯醚、二丙二醇甲醚乙酸酯、四乙二醇二甲醚、二元酯、碳酸甘油酯、N-甲酰基吗啉、膦酸三乙酯、单糖和二糖(包括但不限于木糖醇、果糖、蔗糖、葡萄糖、肌糖、半乳糖、麦芽糖)及其组合。
另外示例性佐剂和/或溶剂包括甘油、山梨醇、二醇醚、脲和双氰胺。
在一个实施例中,所述佐剂选自功能为氢键结添加剂的化合物,所述添加剂用于减少二氧化硅粒子粘到CMP后微电子装置的清洁中所利用的刷子。参见,例如,美国专利公布第2019/0168265号,其以引用的方式并入本文中。示例性化合物包括非离子、阴离子、阳离子和两性离子小分子和可在中性pH下表现为聚电解质的聚合物。阴离子聚合物或阴离子聚电解质可为天然聚合物、经改性的天然聚合物或合成聚合物。可包含于组合物中的示例性天然和经改性的天然阴离子聚合物包括(但不限于)藻酸(或盐)、羧甲基纤维素、硫酸葡聚糖、聚(半乳糖醛酸)及其盐。示例性合成阴离子聚电解质包括(但不限于):(甲基)丙烯酸(或盐)、聚(丙烯酸)、马来酸(或酸酐)、苯乙烯磺酸(或盐)、乙烯基磺酸(或盐)、烯丙基磺酸(或盐)、丙烯酰胺基丙基磺酸(或盐)和类似者的均聚物或共聚物,其中羧酸和磺酸的盐较佳地经铵或烷基铵阳离子中和。在一个实施例中,聚电解质阴离子聚合物的阳离子为铵阳离子(NH4 +)、胆碱鎓+N(CH3)3(CH2CH2OH)和+N(CH3)4。因此,组合的合成和天然聚电解质阴离子聚合物的实例为(甲基)丙烯酸、马来酸(或酸酐)、苯乙烯磺酸、乙烯基磺酸、烯丙基磺酸、乙烯基膦酸、丙烯酰胺基丙基磺酸、藻酸、羧甲基纤维素、硫酸葡聚糖、聚(半乳糖醛酸)及其盐的均聚物或共聚物。
阳离子聚合物和阳离子聚电解质可为天然聚合物、经改性的天然聚合物或合成聚合物。示例性天然和经改性的天然阳离子聚合物包括(但不限于):壳聚糖、阳离子淀粉、聚赖氨酸及其盐。示例性阳离子合成聚电解质包括(但不限于):二烯丙基二甲基氯化铵(DADMAC)、二烯丙基二甲基溴化铵、二烯丙基二甲基硫酸铵、二烯丙基二甲基膦酸铵、二甲基烯丙基二甲基氯化铵、二乙基烯丙基二甲基氯化铵、二烯丙基二(β-羟乙基)氯化铵、二烯丙基二(β-乙氧基乙基)氯化铵、(甲基)丙烯酸二甲氨基乙酯酸加成盐和季铵化盐、(甲基)丙烯酸二乙氨基乙酯酸加成盐和季铵化盐、(甲基)丙烯酸7-氨基-3,7-二甲基辛酯酸加成盐和季铵化盐、N,N'-二甲氨基丙基丙烯酰胺酸加成盐和季铵化盐(其中所述季铵化盐包括烷基和苄基季铵化的盐)、烯丙胺、二烯丙胺、乙烯胺(通过乙烯基烷基酰胺聚合物的水解获得)、乙烯基吡啶、壳聚糖、阳离子淀粉、聚赖氨酸及其盐的均聚物或共聚物。
其它实例包括2-吡咯烷酮、1-(2-羟乙基)-2-吡咯烷酮(HEP)、甘油、1,4-丁二醇、四亚甲基砜(环丁砜)、二甲基砜、乙二醇、丙二醇、二丙二醇、四乙二醇二甲醚和二乙二醇二甲醚。
或者,或此外,所述氢键结添加剂包括羟丙基纤维素、羟乙基纤维素、羟乙基甲基纤维素、羟丙基甲基纤维素、羧甲基纤维素、羧甲基纤维素钠、聚乙烯基吡咯烷酮(PVP)、使用N-乙烯基吡咯烷酮单体制得的任何聚合物、聚丙烯酸酯和聚丙烯酸酯的类似物、聚氨基酸(例如,聚丙氨酸、聚亮氨酸、聚甘氨酸)、聚酰胺基羟基氨基甲酸酯、聚内酯、聚丙烯酰胺、黄原胶、壳聚糖、聚环氧乙烷、聚乙烯醇(PVA)、聚乙酸乙烯酯、聚丙烯酸、聚乙烯亚胺、糖醇(诸如山梨醇、蔗糖、果糖、乳糖、半乳糖、麦芽糖、赤藓糖醇、麦芽糖醇、苏糖醇、阿拉伯糖醇、核糖醇、甘露醇、半乳糖醇、肌醇和木糖醇)、脱水山梨糖醇的酯、二级醇乙氧基化物(如TERGITOLTM表面活性剂)、多官能基醇(包括季戊四醇、二季戊四醇、三羟甲基丙烷、二甲基丙酸和木糖酸)、核碱基(如尿嘧啶、胞嘧啶、鸟嘌呤、胸腺嘌呤)及其组合。
氢键结添加剂的还有其它实例包括乳酸、马来酸、脲、乙醇酸、山梨醇、硼砂(即,硼酸钠)、脯氨酸、甜菜碱、甘氨酸、组氨酸、TRIS(三(羟甲基)氨基甲烷)、二甲亚砜、环丁砜、甘油、SDS(十二烷基硫酸钠)、十二烷基膦酸或其组合。
在另一实施例中,所述组合物进一步包含杀生物剂。示例性杀生物剂包括5-氯-2-甲基-4-异噻唑啉-3-酮、2-甲基-4-异噻唑啉-3-酮、苯并异噻唑酮、1,2-苯并异噻唑-3[2H]-酮、甲基异噻唑啉酮、甲基氯异噻唑啉酮及其组合。
在其它实施例中,本发明的组合物包含:
A.针对具有钨表面的微电子装置:
3-氨基-4-辛醇,
山梨醇,
甘油,
聚(苯乙烯磺酸),
聚丙烯酸,
乙醇胺,
依替膦酸(etidronic acid),
柠檬酸,
羟乙基纤维素,
乙醇胺,
氢氧化胆碱,三乙醇胺,
苯并异噻唑啉酮,和
磷酸;
B.针对具有钴表面和疏水性电介质表面的微电子装置:3-氨基-4-辛醇,
聚(乙烯基吡咯烷酮),
乙醇胺,
氢氧化胆碱,
KOH,
依替膦酸,
三乙二醇单丁醚,和
Brij 23(乙氧基化C12醇);和
C.针对具有铜表面的微电子装置:3-氨基-4-辛醇,
聚(乙烯基吡咯烷酮),
乙醇胺,
氢氧化胆碱,
KOH,
依替膦酸,
三乙二醇单丁醚,
半胱氨酸,
吗啉,
琥珀酸,
草酸,
酒石酸,
双氰胺,
丙二醇单丁醚,和
二乙二醇单丁醚。
如本文中所用,术语"残留物"(其包含"污染物")是指为于用于制造微电子装置的加工步骤,例如包括等离子体蚀刻、等离子体灰化(以将光阻剂自经蚀刻晶圆去除)、化学-机械加工、湿法蚀刻等的加工步骤后仍存在于微电子装置衬底表面处的化学物或微粒材料的任何材料。所述残留物可为任何非水性化学材料,其为用于加工步骤中的加工组合物的一部分,如化学蚀刻剂、光阻剂、CMP浆液等。所述残留物或者可为在加工步骤期间自加工组合物的材料衍生的物质。这些类型的残留物的实例包括在加工后仍在衬底表面处的非水性微粒或非微粒化学或磨料材料(例如,磨料粒子、表面活性剂、氧化剂、腐蚀抑制剂、催化剂)。所述残留物可最初存在于如CMP浆液或蚀刻组合物的材料中,如存在于CMP研磨浆液中的固体磨料粒子或化学品材料。或者,残留物可为在加工期间产生的副产物或反应产物(呈微粒(例如,聚集物、沉淀)或非微粒形式),例如,在加工组合物(如CMP浆液或湿法蚀刻组合物)中存在的化学品,或在等离子体蚀刻或等离子体灰化过程期间存在、使用或产生的化学品的副产物或反应产物。
术语"CMP后残留物"是指在CMP加工步骤结束时存在的残留物,例如,在CMP浆液中存在或自CMP浆液衍生的粒子或化学品材料;特定实例包括磨料粒子(例如,含二氧化硅或二氧化硅基磨料粒子、金属氧化物(例如,氧化铝)粒子、二氧化铈或二氧化铈基粒子和类似者);最初存在于浆液中的化学品,如氧化剂、触媒、表面活性剂、抑制剂、络合剂等;自正在加工的衬底表面去除的金属材料衍生的金属(例如,铁)、金属氧化物或金属络合物;或使用浆液的化学品与浆液的另一化学品或与源自衬底的化学品材料(诸如金属离子)产生的反应产物或络合物;垫粒子或为CMP工艺的产物的任何其它材料。
"蚀刻后残留物"是指在气相等离子体蚀刻工艺(例如,线后端("BEOL")双镶嵌加工)或湿法蚀刻工艺后保留的材料。蚀刻后残留物本质上可为有机、有机金属、有机硅或无机,例如,含硅材料、碳基有机材料和蚀刻气体残留物(如氧和氟)。
"灰化后残留物"是指在氧化性或还原性等离子体灰化以去除硬化光阻剂和/或底部抗反射涂层(BARC)材料后保留的材料。灰化后残留物本质上可为有机、有机金属、有机硅或无机。
如本文中所用,"低k电介质材料"为于多层微电子装置中用作电介质材料的材料,其中所述材料具有小于约3.5的介电常数。示例性低k电介质材料包括低极性材料,如含硅有机聚合物、含硅混杂有机-无机材料、有机硅酸盐玻璃(OSG)、原硅酸四乙酯(TEOS)、氟化硅酸盐玻璃(FSG)和掺杂碳的氧化物(CDO)玻璃。低k电介质材料可具有来自可用密度范围和来自可用孔隙率范围的密度和孔隙率。
如以上所指定,本发明涉及可用于清洁方法中的组合物("清洁组合物"或"清洁溶液"),所述方法自其上具有残留物的微电子装置衬底表面去除残留物。所述组合物为碱性组合物,其含有含水载体(即,水)连同非水性成分的组合,所述非水性成分包括:络合剂和氨基(C6-C12烷基)醇。在某些实施例中,在用于清洁工艺之前,所述组合物为包含水和所溶解的非水性成分,由其组成,或基本上由其组成的均匀溶液,不存在任何固体或悬浮材料,如固体磨料粒子、聚结物、凝结物等。
如所述组合物可用于清洁微电子装置及其前体,尤其包括微电子装置衬底,意指半导体晶圆在表面上包括一或多个微电子装置或处在制造成最终完成并且功能性微电子装置的工艺中的其前体。如本文中所用,微电子装置为包含电路及其上形成的极小(例如,微米尺度或更小)尺寸的相关结构的装置。示例性微电子装置包括平板显示器、集成电路、记忆装置、太阳能面板、光伏和微电机系统(MEMS)。微电子装置衬底为如晶圆(例如,半导体晶圆)的结构,其包含一或多个微电子装置或处于正在制备以形成最终微电子装置的状态的其前体。
本文中所述的组合物和方法可用于在加工的任何阶段清洁各种形式的微电子装置中的任一者。可以特定效用和效益进行清洁的微电子装置衬底(或本文中简称为"衬底")包括在衬底表面处包含暴露的钴、钨、钼或电介质或所有三者的衬底。
根据本发明,所述组合物可用于清洁这些一般类型和特定类型的微电子装置衬底以去除残留物,如(但不限于)CMP后残留物、灰化后残留物、蚀刻后残留物、或在加工微电子装置衬底的步骤后存在于衬底表面处的其它残留物。所述清洁组合物提供有用或有利清洁性质,意指所述清洁组合物能与已知设备(例如,CMP后清洁设备)一起使用以实质上减少微电子装置衬底表面上的残留物、污染物或二者的量,对这些钴、钨和电介质表面具有改善的不利效应程度。存在于衬底表面处的高百分比的残留物可通过使用本文中所述的清洁组合物和方法自表面成功去除,例如,可去除至少70%、80%、85%、90%、95%或99%的残留物(也称作"清洁效率")。
用于测量微电子装置衬底表面处的残留物的方法和设备已熟知。清洁功效可基于清洁后存在于微电子装置表面上的残留物粒子的量(例如,数目)与在清洁之前存在的残留物粒子的量(例如,数目)相比的减少来评定。例如,可使用原子力显微镜进行清洁前和清洁后分析。表面上的残留物粒子可登记为像素的范围。可应用直方图(例如,Sigma Scan Pro)以过滤某个强度(例如,231到235)的像素,和将残留物粒子的数目计数。残留物粒子去除的量(即,清洁效率)可使用以下比率进行计算:
(表面上的清洁前残留物粒子的数目-表面上的清洁后残留物粒子的数目)/(表面上的清洁前残留物粒子的数目)。
或者,清洁功效可考虑为在清洁之前与在清洁后相比由残留微粒物质覆盖的衬底表面的总量的百分比。例如,可将原子力显微镜程序化以进行z-平面扫描以识别高于某个高度临限值的受关注地形区域,和然后计算由受关注区域覆盖的总表面的面积。在清洁后,测定为受关注区域的面积的减少的量指示更有效清洁组合物和清洁工艺。
除了良好清洁功效外,如所述的清洁工艺和清洁组合物也产生经清洁的衬底表面,所述衬底表面受有利低量的暴露的金属表面(如暴露的金属钨、钼、暴露的金属钴)或暴露的电介质的腐蚀影响。可通过此工艺清洁的示例性衬底为在表面处具有金属钨或金属钴(例如,作为金属互连(例如,钨或钴互连))或位于金属互连与电介质或介电材料之间的阻挡层材料(例如,钴)的衬底。以特别有用或有利结果进行清洁的微电子装置衬底的某些实例包括在表面处含有暴露的结构(其包括金属钨(例如,钨或其合金)、金属钴(例如,钴或其合金)和介电材料)的那些。清洁组合物的腐蚀抑制可在金属蚀刻速率(如静态蚀刻速率)的测量中反映,所述测量可通过已知方法使用已知设备进行。
可制备本发明的组合物,然后以浓缩物的形式销售,所述浓缩物含有相对低量的水,和因此,相对浓缩量的非水性成分。所述浓缩物在市面上经制备以销售和运输,同时含有浓缩量的非水性成分和相对减少量的水,并且在使用点时由浓缩物的购买者最终稀释。浓缩物中的不同非水性成分的量为在稀释浓缩物后将导致存在于使用组合物中的那些非水性成分的所需量的量。
如所述的组合物包含水作为液体载体,即,非水性成分的溶质。所述水可为去离子(DIW)水。水可自任何来源存在于组合物中,如通过含于与其它成分组合以产生浓缩物形式的组合物的成分中;或作为以纯形式与浓缩物的其它成分组合的水;或作为(例如)在使用点时由使用者添加到浓缩物的水,作为出于稀释浓缩物以形成使用组合物的目的的稀释水。
组合物中的水的量可为浓缩物的所需量,或使用组合物的所需量,其一般为相对于浓缩物中的水的量的更高总量。浓缩组合物中的水的示例性量(不被视为限制性)可为基于浓缩组合物的总重量计约30重量%、40重量%或50重量%到约85重量%或90重量%,例如,约60重量%、65重量%或70重量%到约80重量%水。在稀释后,此等量将以稀释倍率减少。使用组合物中的水的示例性量可为基于使用组合物的总重量计约75重量%到约95重量%,例如,约82重量%或85重量%到约90重量%或93重量%水。
本发明的组合物含有氨基(C6-C12烷基)醇作为主要清洁化合物。作为次要清洁化合物,所述组合物可任选进一步含有C2-C4烷醇胺(诸如单乙醇胺)作为次要清洁化合物。
在另一实施例中,所述组合物进一步包含另外清洁化合物。这些另外清洁化合物的一些特定实例包括:
a.吗啉、L-半胱氨酸、双氰胺、羟基乙基纤维素、聚乙烯基吡咯烷酮、聚胺、及其组合;和
b.藻酸及其盐;羧甲基纤维素;硫酸葡聚糖及其盐;聚(半乳糖醛酸)及其盐;(甲基)丙烯酸及其盐、马来酸、马来酸酐、苯乙烯磺酸及其盐、乙烯基磺酸及其盐、烯丙基磺酸及其盐、丙烯酰胺基丙基磺酸及其盐的均聚物;(甲基)丙烯酸及其盐、马来酸、马来酸酐、苯乙烯磺酸及其盐、乙烯基磺酸及其盐、烯丙基磺酸及其盐、丙烯酰胺基丙基磺酸及其盐的共聚物;壳聚糖;阳离子淀粉;聚赖氨酸及其盐;二烯丙基二甲基氯化铵(DADMAC)、二烯丙基二甲基溴化铵、二烯丙基二甲基硫酸铵、二烯丙基二甲基膦酸铵、二甲基烯丙基二甲基氯化铵、二乙基烯丙基二甲基氯化铵、二烯丙基二(β-羟乙基)氯化铵、二烯丙基二(β-乙氧基乙基)氯化铵、(甲基)丙烯酸二甲氨基乙酯酸加成盐和季铵化盐、(甲基)丙烯酸二乙氨基乙酯酸加成盐和季铵化盐、(甲基)丙烯酸7-氨基-3,7-二甲基辛酯酸加成盐和季铵化盐、N,N'-二甲氨基丙基丙烯酰氨酸加成盐和季铵化盐、烯丙胺、二烯丙胺、乙烯胺、乙烯基吡啶的均聚物;和二烯丙基二甲基氯化铵、二烯丙基二甲基溴化铵、二烯丙基二甲基硫酸铵、二烯丙基二甲基膦酸铵、二甲基烯丙基二甲基氯化铵、二乙基烯丙基二甲基氯化铵、二烯丙基二(β-羟乙基)氯化铵、二烯丙基二(β-乙氧基乙基)氯化铵、(甲基)丙烯酸二甲氨基乙酯酸加成盐和季铵化盐、(甲基)丙烯酸二乙氨基乙酯酸加成盐和季铵化盐、(甲基)丙烯酸7-氨基-3,7-二甲基辛酯酸加成盐和季铵化盐、N,N'-二甲氨基丙基丙烯酰氨酸加成盐和季铵化盐、烯丙胺、二烯丙胺、乙烯胺、乙烯基吡啶的共聚物;椰油基二甲基羧甲基甜菜碱;月桂基二甲基羧甲基甜菜碱;月桂基二甲基-α-羧乙基甜菜碱;鲸蜡基二甲基羧甲基甜菜碱;月桂基-双(2-羟乙基)羧甲基甜菜碱;硬脂酰基-双(2-羟丙基)羧甲基甜菜碱;油烯基二甲基-γ-羧丙基甜菜碱;月桂基-双(2-羟丙基)α-羧乙基甜菜碱;椰油基二甲基磺丙基甜菜碱;硬脂酰基二甲基磺丙基甜菜碱;月桂基-双(2-羟乙基)磺丙基甜菜碱;十二烷基硫酸钠;二辛基磺基琥珀酸钠盐;月桂基醚硫酸钠;支链聚乙二醇-壬基苯基醚硫酸铵盐;2-十二烷基-3-(2-磺酸根基苯氧基)二钠;PEG25-PABA;聚乙二醇单C10-16烷基醚硫酸钠盐;(2-N-丁氧乙氧基)乙酸;十六烷基苯磺酸;鲸蜡基三甲基氢氧化铵;十二烷基三甲基氢氧化铵;十二烷基三甲基氯化铵;鲸蜡基三甲基氯化铵;N-烷基-N-苄基-N,N-二甲基氯化铵;十二烷胺;聚氧乙烯月桂基醚;十二烯基琥珀酸单二乙醇酰胺;乙二胺四(乙氧基化物-嵌段-丙氧基化物);2-吡咯烷酮;和1-(2-羟乙基)-2-吡咯烷酮(HEP)。
本发明的组合物可通过简单添加相应成分和混合到均匀条件(如溶液)容易制备。此外,组合物可容易调配成单包装调配物或在使用点时或在使用点之前混合的多部分调配物,例如,多部分调配物的个别部分可由使用者在加工工具(清洁装置)处或在加工工具上游的储存槽中混合。
因此,本发明的另一方面涉及试剂盒,其于一或多个容器中包含如本文中所阐述的组合物的一或多种组分。所述试剂盒可于一或多个容器中包含(i)pH调节剂;(ii)络合剂;(iii)氨基(C6-C10烷基)醇,用于在晶圆厂或使用点时与另外溶剂(例如,水)组合。所述试剂盒也可包含本文中所详述的其它任选可选的成分。试剂盒的容器必须适用于储存和船运组合物并可为(例如)容器(美国马萨诸塞州比勒里卡的应特格公司(Entegris,Inc.,Billerica,Mass.,USA))。
另外,如本文中所述的组合物可以浓缩物的形式在市面上提供用于销售,可在使用点时将所述浓缩物利用适宜量的水稀释。以浓缩物形式,所述组合物(浓缩物)包含如本文中所阐述的非水性成分,其将以使得当将浓缩物用所需量的水(例如,DI水)稀释时,清洁组合物的各组分将以用于清洁步骤(如CMP后清洁步骤)所需的量存在于经稀释的使用组合物中的量存在于浓缩物中。添加到浓缩物中以形成使用组合物的水的量可为一或多体积的水/体积的浓缩物,例如,2体积的水(例如,3体积、4体积、5体积或10体积的水)/体积的浓缩物。当将浓缩物用此量的水稀释时,浓缩物的固体组分每一者将以某种浓度存在于使用组合物中,所述浓度基于经添加以稀释浓缩物的水的体积数减少。
如所述的清洁组合物可用于微电子装置加工应用中,所述应用包括通过诸如蚀刻后残留物去除、灰化后残留物去除表面制备、CMP后残留物去除和类似者的方法清洁衬底表面的工艺。可通过此工艺清洁的示例性衬底包括包含金属钨、金属钴、低k电介质材料或所有三者的衬底。
清洁组合物和清洁方法对自表面去除相对于在清洁步骤之前最初存在于表面上的量的实质量的残留物有效。同时,所述组合物和方法有效而不对可存在于表面处的电介质材料造成不当损害,并且不对也存在于所选衬底表面处的如金属钼、钨、铜或钴的材料造成不当腐蚀。在一个实施例中,所述清洁组合物可在清洁步骤中有效,以去除至少85%的在通过清洁步骤去除残留物之前存在于衬底表面上的残留物,或至少90%的在清洁步骤之前最初存在的残留物或至少95%的残留物或至少99%的残留物。
在清洁步骤(如CMP后残留物清洁步骤)中,清洁组合物可使用各种已知习知市售清洁工具中的任一者,如超高频音波和刷子擦洗,包括(但不限于)Verteq单晶圆超高频音波Goldfinger、OnTrak系统DDS(双面洗涤器)、SEZ或其它单晶圆喷雾冲洗、应用材料公司(Applied Materials)的Mirra-MesaTM/ReflexionTM/Reflexion LKTM、和超高频音波分批湿式工作台系统、和荏原技术公司(Ebara Technologies,Inc.)产品,如300mm型号(FREX300S2和FREX300X3SC)和200mm CMP系统(FREX200M)。
清洁步骤的条件和时序可如所需,并且可取决于衬底和残留物的类型变化。在使用组合物用于自其上具有CMP后残留物、蚀刻后残留物、灰化后残留物或污染物的微电子装置衬底清洁CMP后残留物、蚀刻后残留物、灰化后残留物或污染物中,所述清洁组合物可在约20℃到约90℃,或约20℃到约50℃的范围的温度下与衬底表面接触约1秒到约20分钟,例如,约5秒到10分钟,或约15秒到约5分钟的时间。此等接触时间和温度是说明性,并且若对自表面至少部分,较佳地实质上清洁初始量的残留物有效,则任何其它适宜时间和温度条件可为可用。
在装置衬底表面的所需程度的清洁后,用于清洁步骤中的清洁组合物可容易自装置表面去除,如可于给定最终用途应用中所需并且有效。例如,去除可通过使用包含去离子水的冲洗溶液进行。之后,可将装置如所需进行加工,诸如通过干燥(例如,使用氮气或旋干循环),接着后续加工经清洁和经干燥的装置表面。
在其它更一般或特定方法中,微电子装置衬底可首先经受包含CMP加工、等离子体蚀刻、湿法蚀刻、等离子体灰化或类似者中的任一者或多者的加工步骤,接着包含将衬底表面用本发明的组合物清洁的清洁步骤。在第一加工步骤结束时,残留物(例如,蚀刻后残留物、CMP后残留物、灰化后残留物等)将存在于衬底表面处。使用如所述的清洁组合物的清洁步骤将对自微电子装置表面清洁实质量的残留物有效。
因此,在另一方面,本发明提供一种自其上具有残留物的微电子装置衬底去除所述残留物的方法,其中所述衬底具有包含选自铜、钴、钨或电介质组合物的物质的至少一个表面,所述方法包括:
使微电子装置衬底的表面与组合物接触,所述组合物包含:
a.水;
b.络合剂;和
c.氨基(C6-C12烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂,和自所述衬底至少部分去除所述残留物。
除非另有明确指定,否则本发明可通过其较佳实施例的下列实例进一步说明,但是应了解,这些实例仅出于说明目的包含且不意欲限制本发明的范围。
实例
制备如表1中所提及的溶液1到10并且将其用于处理具有铜或钴表面的微电子装置衬底,以评价相对蚀刻速率。
蚀刻速率为在将表面暴露于某种电解质(如清洁组合物)后自金属表面去除的金属的量的量度。在30℃温度和500rpm搅拌下的15分钟清洁工艺之前和之后通过使用X-射线荧光(XRF)测量金属膜厚度。
表1
*1-羟基亚乙基-1,1-二膦酸
此外,如表2中所示,含有如本文中所述的腐蚀抑制剂与特定基底材料Cu和Co的本发明清洁组合物如与对照溶液相比展示更低蚀刻速率。
表2
实例2:制备表3中所示的下列组合物并且根据下列程序进行测试:
蚀刻速率程序:
试片制备:
·将晶圆切割成具有介于22mm与24mm之间的边尺寸的正方形试片。
·将晶圆用清洁压缩氮气吹除以去除切割灰尘。喷嘴应距离晶圆表面1”与2”之间。
烧杯加工:
·若指定预先测量,则预先测量试片。使用刻参考将试片以可重复方向放置。
·设置热板上的所需加工温度。在热板温度读出停止闪烁(指示已达到温度)后,再等待30分钟,之后加工试片。
·准备具有250到350ml DIW的2个400ml烧杯以用于冲洗。一个(用于第一冲洗)应位于热板附近的罩内,和另一个(用于溢流冲洗)应于DIW供应下的水槽中。
·使用蓝色夹子将试片放置于烧杯中,其中活性侧面向化学品的流动。
·在所需时间去除所有试片。
·将夹子和试片浸入填充有250到350ml DIW的400ml特氟龙(Teflon)烧杯中1到3秒。此步骤的目的为去除在溢流冲洗之前粘附到晶圆和夹子的大多数调配物。
·将夹子和试片移动到具有连续流的水槽中的烧杯中(溢流冲洗),针对Cu持续2分钟和针对Co持续10秒。
·将DIW自试片吹除。利用压缩N2吹除,其中喷嘴距离试片1"与2”之间。在夹子对面开始和将N2物流沿着晶圆向下移动。尽可能多地像床单一样移动水,避免在晶圆表面上具有小滴干燥。
·后测量试片。
表3
实例3:抛光数据:
将表3中所示的样品A和B用99份水和1份样品稀释。将TEOS(二氧化硅)和/或氮化硅晶圆用二氧化硅基市售浆液在Reflexion LK上抛光,然后在集成PVP电刷站上使用应特格公司(Entegris)的刷清洁120秒。然后将晶圆通过KLA-TENCORE SP3在65nm临限值处分析和然后通过SEMVISION SEM划痕分类和去除凹坑,因为其与清洁工艺不相关,并且总缺陷为二氧化硅缺陷加上任何有机残留物缺陷的加总。
本发明已特别参考其某些实施例详细描述,但是应了解,变化和修改可于本发明的精神和范围内实现。
表3*无缺陷
Claims (20)
1.一种组合物,其包含:
a.水;
b.络合剂;和
c.氨基(C6-C12烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂。
2.根据权利要求1所述的组合物,其中所述氨基(C6-C12烷基)醇为氨基(C8-C10烷基)醇。
3.根据权利要求1所述的组合物,其进一步包含C2-C4烷醇胺;
4.根据权利要求1所述的组合物,其中所述络合剂选自
a.4-(2-羟乙基)吗啉、1,2-环己二胺-N,N,N',N'-四乙酸、羟乙基二亚乙基四胺三乙酸、乙二胺四乙酸、间二甲苯二胺、亚氨基二乙酸、三甲胺、异丙醇胺、二异丙醇胺、哌嗪、羟乙基哌嗪、二羟乙基哌嗪、葡糖胺、N-甲基葡糖胺、2-(羟乙基)亚氨基二乙酸、次氮基三乙酸、硫脲、1,1,3,3-四甲基脲、脲、尿酸;
b.选自以下的氨基酸:丙氨酸、精氨酸、天冬酰胺、天冬氨酸、半胱氨酸、谷氨酸、谷氨酰胺、组氨酸、异亮氨酸、亮氨酸、赖氨酸、甲硫氨酸、苯丙氨酸、脯氨酸、丝氨酸、苏氨酸、色氨酸、酪氨酸、缬氨酸、牛磺酸、甜菜碱;
c.选自以下的包含膦酸部分的化合物:1-羟基亚乙基-1,1-二膦酸、1,5,9-三氮杂环十二烷-N,N',N”-三(亚甲基膦酸)、1,4,7,10-四氮杂环十二烷-N,N',N”,N”'-四(亚甲基膦酸)、次氮基三(亚甲基)三膦酸、二亚乙基三胺五(亚甲基膦酸)、氨基三(亚甲基膦酸)、双(六亚甲基)三胺五亚甲基膦酸、1,4,7-三氮杂环壬烷-N,N',N”-三(亚甲基膦酸)、羟乙基二膦酸盐、次氮基三(亚甲基)膦酸;和
d.选自2-膦酰基-丁烷-1,2,3,4-四甲酸、羧基乙基膦酸、氨基乙基膦酸、草甘膦、乙二胺四(亚甲基膦酸)、苯基膦酸的羧酸;选自草酸、琥珀酸、马来酸、苹果酸、丙二酸、己二酸、酞酸、柠檬酸、柠檬酸钠、柠檬酸钾、柠檬酸铵、丙三甲酸、三羟甲基丙酸、吡啶甲酸、吡啶二甲酸、水杨酸、磺基水杨酸、磺基酞酸、磺基琥珀酸、葡糖酸、酒石酸、葡糖醛酸、2-羧基吡啶的羧酸和/或选自4,5-二羟基-1,3-苯二磺酸二钠盐的磺酸。
5.根据权利要求1所述的组合物,其中所述氨基(C6-C10烷基)醇选自3-氨基-4-辛醇、DL-2-氨基-1-己醇、2-(丁氨基)乙醇、1-氨基环己醇和8-氨基-1-辛醇。
6.根据权利要求1所述的组合物,其中所述氨基(C8-C12烷基)醇包括3-氨基-4-辛醇。
7.根据权利要求1所述的组合物,其进一步包含水溶性或水可分散性聚合物。
8.根据权利要求1所述的组合物,其进一步包含杀生物剂。
9.根据权利要求1所述的组合物,其进一步包含表面活性剂。
10.根据权利要求1所述的组合物,其进一步包含水可混溶溶剂和/或佐剂。
11.根据权利要求10所述的组合物,其中所述水可混溶溶剂和/或佐剂选自甘油、山梨醇、二醇醚和尿素。
12.根据权利要求1所述的组合物,其包含:
a.水;
b.氢氧化胆碱;
c.1-羟基亚乙基-1,1-二膦酸;
d.单乙醇胺;和
e.氨基(C6-C10烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂。
13.根据权利要求13所述的组合物,其中所述氨基(C8-C12烷基)醇选自3-氨基-4-辛醇、DL-2-氨基-1-己醇、2-(丁氨基)乙醇、1-氨基环己醇和8-氨基-1-辛醇。
14.根据权利要求13所述的组合物,其进一步包含山梨醇。
15.根据权利要求1所述的组合物,其中所述组合物为含有小于80重量%水的浓缩物。
16.根据权利要求1所述的组合物,其进一步包含选自吗啉、L-半胱氨酸、双氰胺、羟基乙基纤维素、聚乙烯基吡咯烷酮、聚胺和其组合的化合物。
17.一种自其上具有残留物的微电子装置衬底去除所述残留物的方法,其中所述衬底具有包含选自铜、钴、钨、钼或介电组合物的物质的至少一个表面,所述方法包括:
使微电子装置衬底的所述表面与组合物接触,所述组合物包含:
a.水;
b.络合剂;和
c.氨基(C8-C12烷基)醇;
其中所述组合物不含选自含胍官能基化合物、含吡唑酮官能基化合物或羟基喹啉化合物的腐蚀抑制剂,和自所述衬底至少部分去除所述残留物。
18.根据权利要求17所述的方法,其中所述表面包含钴、铜、钨和/或钼中的至少一者。
19.根据权利要求17所述的方法,其中所述表面为选自以下的电介质:原硅酸四乙酯、含硅有机聚合物、含硅混杂有机-无机材料、有机硅酸盐玻璃、氟化硅酸盐玻璃和掺杂碳的氧化物玻璃。
20.根据权利要求26所述的方法,其中所述组合物包含:
a.水;
b.氢氧化胆碱;
c.1-羟基亚乙基-1,1-二膦酸;
d.单乙醇胺;和
e.氨基(C6-C10烷基)醇。
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