CN1526007A - 具有改进的基板相容性的无氨碱性微电子清洗组合物 - Google Patents
具有改进的基板相容性的无氨碱性微电子清洗组合物 Download PDFInfo
- Publication number
- CN1526007A CN1526007A CNA028138759A CN02813875A CN1526007A CN 1526007 A CN1526007 A CN 1526007A CN A028138759 A CNA028138759 A CN A028138759A CN 02813875 A CN02813875 A CN 02813875A CN 1526007 A CN1526007 A CN 1526007A
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- CN
- China
- Prior art keywords
- dimethyl
- pyrrolidone
- cleaning combination
- alkyl
- sterically hindered
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000758 substrate Substances 0.000 title claims abstract description 17
- 238000004377 microelectronic Methods 0.000 title claims abstract description 12
- 239000000203 mixture Substances 0.000 title abstract description 25
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- 239000002904 solvent Substances 0.000 claims abstract description 34
- 150000001408 amides Chemical class 0.000 claims abstract description 32
- 239000010949 copper Substances 0.000 claims abstract description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052802 copper Inorganic materials 0.000 claims abstract description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims abstract description 13
- 230000000269 nucleophilic effect Effects 0.000 claims abstract description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 66
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 30
- 125000000217 alkyl group Chemical group 0.000 claims description 24
- 150000001875 compounds Chemical class 0.000 claims description 22
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 20
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- 229910052751 metal Inorganic materials 0.000 claims description 17
- 239000002184 metal Substances 0.000 claims description 17
- -1 silicate compound Chemical class 0.000 claims description 17
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 16
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- 125000003118 aryl group Chemical group 0.000 claims description 14
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- WDQFELCEOPFLCZ-UHFFFAOYSA-N 1-(2-hydroxyethyl)pyrrolidin-2-one Chemical compound OCCN1CCCC1=O WDQFELCEOPFLCZ-UHFFFAOYSA-N 0.000 claims description 12
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- 230000007797 corrosion Effects 0.000 claims description 12
- RJLKIAGOYBARJG-UHFFFAOYSA-N 1,3-dimethylpiperidin-2-one Chemical compound CC1CCCN(C)C1=O RJLKIAGOYBARJG-UHFFFAOYSA-N 0.000 claims description 11
- YXHVIDNQBMVYHQ-UHFFFAOYSA-N 1,5-dimethylpiperidin-2-one Chemical compound CC1CCC(=O)N(C)C1 YXHVIDNQBMVYHQ-UHFFFAOYSA-N 0.000 claims description 11
- FILVIKOEJGORQS-UHFFFAOYSA-N 1,5-dimethylpyrrolidin-2-one Chemical compound CC1CCC(=O)N1C FILVIKOEJGORQS-UHFFFAOYSA-N 0.000 claims description 11
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- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 11
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 10
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims description 9
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- LTACQVCHVAUOKN-UHFFFAOYSA-N 3-(diethylamino)propane-1,2-diol Chemical compound CCN(CC)CC(O)CO LTACQVCHVAUOKN-UHFFFAOYSA-N 0.000 claims 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N propylene glycol Substances CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims 4
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- 239000003795 chemical substances by application Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
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- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 229960002510 mandelic acid Drugs 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- NCWQJOGVLLNWEO-UHFFFAOYSA-N methylsilicon Chemical compound [Si]C NCWQJOGVLLNWEO-UHFFFAOYSA-N 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007344 nucleophilic reaction Methods 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940079877 pyrogallol Drugs 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000003335 steric effect Effects 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
- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 125000005207 tetraalkylammonium group Chemical group 0.000 description 1
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 1
- GTDKXDWWMOMSFL-UHFFFAOYSA-M tetramethylazanium;fluoride Chemical compound [F-].C[N+](C)(C)C GTDKXDWWMOMSFL-UHFFFAOYSA-M 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/28—Heterocyclic compounds containing nitrogen in the ring
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
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- C11D3/30—Amines; Substituted amines ; Quaternized amines
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- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/43—Solvents
-
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
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- C11D7/3218—Alkanolamines or alkanolimines
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Abstract
用于清洗微电子基板的无氨清洗组合物,更具体地,此组合物清洗剂对以敏感多孔、低-κ和高-κ电介质以及敷铜为特征的微电子基板一起使用、并对基板具有改进相容性。用于剥离光致抗蚀剂、清除等离子生成的有机化合物、金属有机化合物和无机化合物的残余物、清除平坦化工艺中的残余物的清洗组合物。该清洗组合物含有一种或多种含有非亲核的、带正电的反离子的不产生铵的强碱和一种或多种位阻酰胺溶剂。
Description
发明领域
本发明涉及用于清洗微电子基板的无氨清洗组合物,更具体地,本发明涉及与以敏感多孔的、低-κ和高-κ电介质以及敷铜(copper metalliztion)为特征的微电子基板一同使用的、并与这种基板的相容性得到改进的清洗组合物。本发明也涉及此清洗组合物在剥离光致抗蚀剂(photoresists)、清除等离子生成的有机化合物、金属有机化合物和无机化合物的残余物、清除来自诸如化学机械磨光(CMP)平坦化工艺的残余物以及清除平坦化工艺残余浆中的添加剂中的用途。
发明背景
在微电子工业中,多种光致抗蚀剂剥离剂和残余物清除剂已被建议用来作为制造生产线下游或后端(back end)的清洗剂。在制造工艺中,光致抗蚀剂薄膜沉积于晶片基板上,然后将电路设计成像在薄膜上。烘焙后,未聚合的抗蚀剂可用光致抗蚀剂显像剂清除。因此,生成的图像可通过活性的等离子蚀刻气体或化学蚀刻剂溶液转移到底层材料上,底层材料通常为电介质或金属。这些蚀刻气体或化学蚀刻剂溶液选择性地蚀刻基板上未被光致抗蚀剂保护的区域。因此,作为等离子蚀刻技术的结果,光致抗蚀剂、蚀刻气体和蚀刻材料的副产物成为沉积在基板上蚀刻空隙的侧部表面上或周围的残余物。
此外,在蚀刻过程完成后,必须从晶片的被保护区域上清除抗蚀剂掩膜,如此才能完成最后的修整过程。在等离子灰化步骤(plasma ashing step)中使用合适的等离子灰化气体或湿法化学剥离剂可完成此修整过程。然而,寻找一种用来清除抗蚀剂掩膜材料而对金属电路没有如腐蚀、溶解或浊化(dulling)的不利影响的、合适的清洗组合物,已证明同样是有问题的。
随着微电子制造集成水平的提高以及模式微电子器件尺寸的减小,在本领域中使用敷铜、低-κ和高-κ电介质的技术越来越普通。寻找可接受的清洗组合物对这些材料来说是另外的挑战。许多以前研发的用于“传统的”或“常规的”半导体器件的工艺组合物中包含Al/SiO2或Al(Cu)/SiO2结构,而不适用于敷铜的低-κ或高-κ电介质结构。例如,羟胺基剥离剂(stripper)或残余物清洗剂组合物能成功地用于清洗含有敷铝的器件,然而几乎不适用于敷铜的器件。如果不对组合物作重大的调整,许多适合于敷铜/低-κ的剥离剂则同样地不适用于敷铝的器件。
在蚀刻和/或灰化过程后,能否有效清除蚀刻和/或灰化的残余物已证实是有问题的。如不能完全清除或中和这些残余物,湿气将被会吸收,并且能生成腐蚀金属结构的不必要的物质,电路材料因此被这些不必要的物质腐蚀,在电路线圈中生成不连续区域以及使电阻不必要增大。
该发明的后端清洗剂显示出与某些敏感的电介质和涂敷金属有着广泛的相容性:从彻底的不接受到相对满意。大多数当前的剥离剂或残余物清洗剂对高级互连的材料比如低-κ和高-κ的电介质和敷铜是不可接受的。此外,普通的碱性清洗溶液对低-κ和高-κ的电介质和/或敷铜具有过度的攻击性。而且,大多数碱性清洗组合物含有稳定性差的有机溶剂,特别在高pH值范围和高温的过程中稳定性更差。
发明概述
因此,开发出适用于后端清洗过程的微电子清洗组合物迫在眉睫,这种组合物应是有效的清洗剂,并适用于剥离光致抗蚀剂和清洗来自等离子过程中生成的有机、有机金属和无机材料的残余物,以及来自平坦化工艺(planarization process step)如化学机械磨光等中的残余物。本发明涉及能有效剥离光致抗蚀剂,制备/清洗半导体表面和结构,并与高级互连的材料和敷铜具有好的相容性的组合物。
实验已经发现,氨(NH3)及其衍生的碱如氢氧化铵和其它盐(NH4X,X=OH、碳酸根等)通过形成络合物能溶解/腐蚀金属如铜。因此,当要求与多孔的、低-κ和高-κ电介质和敷铜具有相容性时,在半导体清洗配方中使用它们是不好的选择。在平衡过程中,这些化合物可产生氨。氨可与金属如铜形成络合物,且导致金属腐蚀/溶解,如下述方程式所示。
因此,通过方程1所描述的平衡过程,氢氧化铵及其铵盐能提供亲核的,能与金属鳌合的氨(NH3),特别是当加入其它碱性物质如胺和链烷醇胺时。在氧气存在下,金属如铜可通过与氨形成络合物而被溶解/腐蚀,如方程2所示。这种络合物的形成可进一步使平衡(方程1)向右边移动,并提供更多的氨,这导致进一步的金属溶解/腐蚀。
通常,敏感的低-κ电介质在强碱性条件下显著地降解。氨和氨-衍生的碱也显示出与敏感电介质如氢硅倍半氧丙环(hydrogensilsesquioxane,HSQ)和甲基硅倍半氧丙环(methyl silsesquioxane,MSQ)有不良的相容性。此外,它们能提供氨和/或其它的亲核体,因此能导致敏感的电介质发生反应/降解。
已发现,在位阻酰胺溶剂中,含有非亲核的、带正电的反离子的不产生铵的强碱性清洗制剂(如四烷基铵)呈现出与敏感多孔、低-κ和高-κ电介质以及敷铜具有显著改进的相容性。优选的溶剂基质耐强碱性条件,这是由于位阻效应和/或对亲核反应低或没有反应性(相对于亲核体如氢氧根离子)导致的。由于在组合物内不存在不必要的亲核体,所以可部分地获得改进的电介质相容性。通过选择地使用一些铜-相容的位阻酰胺溶剂,可实现与敷铜具有良好的相容性。这些组分可被配制成半含水直到几乎不含水(基于有机溶剂的)的清洗溶液或浆液中。
发明详述
本发明的新型后端清洗组合物包括一种或多种任何合适的含非亲核的、带正电的反离子的不产生铵的强碱(non-ammonium producing strong base)和一种或多种在强碱性条件下稳定的任何合适的位阻酰胺溶剂。在适用于本发明清洗组合物的合适的含非亲核的、带正电的反离子的不生长铵的强碱当中,可提及的含有下式四烷基氢氧化铵:
[(R)4N+]p[X]-q
其中R分别独立地为取代或未取代的烷基,优选地含有1-22个,更优选地含有1-6个碳原子的烷基或羟烷基(R≠H);X=OH或合适的盐阴离子,如碳酸根等;p与q相同且为1-3的整数。合适的强碱也包括KOH和NaOH。包括含非亲核的、带正电的反离子的不产生铵的强碱的清洗组合物显示出与低-κ电介质和敷铜显著改进的相容性。无氨的四烷基氢氧化铵(TAAH)是非常强的碱,但发现它们与含有氢氧化铵的清洗组合物相比,令人惊奇地提供改进的低-κ相容性。特别优选四甲基氢氧化铵、四丁基氢氧化铵、氢氧化胆碱和碳酸四甲铵。
尽管以前尝试过通过仔细控制pH值和/或使用其它腐蚀抑制化合物,如:小于2%重量的苯并三唑(BT)来控制和抑制金属腐蚀,但已经发现,当使用一种或多种位阻酰胺溶剂时,本发明的清洗组合物意想不到地、显著地改善和控制铜的金属腐蚀状况。可在本发明的清洗组合物内使用任何合适的位阻酰胺溶剂。此类位阻酰胺溶剂优选地为下述通式的位阻无环的和位阻环状酰胺:
R1CONR2R3和
其中n是1-22的数,优选1-6;R1、R2、R3、R4、R5、R6、R7和R8分别自独立地选自H、(取代的或未取代的)烷基,优选为含有1-6个碳原子的烷基和(取代的或未取代的)芳基,优选为含有3-14个碳原子的芳基,条件是R1、R2和R3中的至少一个以及R4、R5、R6、R7和R8中的至少一个不是H。
此类位阻酰胺无环溶剂的一些合适的实例包括例如乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、苯甲酰胺等。位阻环状酰胺的一些合适的实例包括例如N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮、1,5-二甲基-2-哌啶酮等。
可将含有不产生铵的强碱的本发明清洗组合物配制成含水、半含水或有机溶剂基组合物。含非亲核的、带正电的反离子的不产生铵的强碱可与单独的位阻酰胺溶剂一起使用,或结合其它稳定溶剂,优选一种或多种耐强碱且不含有未受阻亲核体的极性有机溶剂如二甲基亚砜(DMSO)、环丁砜(SFL)、二甲基哌啶酮、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇、3-(二甲基氨基)-1,2-丙二醇等一起使用。清洗组合物也可任选地含有有机或无机酸,优选有机弱酸或无机弱酸、位阻胺、位阻链烷醇胺和位阻羟胺和其它腐蚀抑制剂,如苯并三唑、儿茶酚、甘油、乙二醇等。清洗组合物也可含有任何合适的表面活性剂,如二甲基己炔醇(Surfynol-61)、乙氧化四甲基癸炔二醇(Surfynol-465)、聚四氟乙烯十六烷氧基丙基甜菜碱(Zonyl FSK)、(Zonyl FSH)等。因此,把操作/运行的pH值和温度控制在一个宽的区域内,能有效地从多孔或低-κ或高-κ电介质或敷铜的基板上去除光致抗蚀剂,等离子蚀刻/灰烬残余物、牺牲光吸收材料(sacrifical light absorbing materials)和抗反射层(anti-reflectivecoatings,ARC)。也已发现,对于清洗在其结构中含有钽(Ta)或氮化钽阻挡层和氧化钽的非常难以清洗的试样,此类中的一些制剂特别有效。
可在本发明的组合物中使用任何合适的无金属离子的硅酸盐。硅酸盐优选季铵硅酸盐如四烷基硅酸铵(包括通常在烷基或烷氧基中具有1-4个碳原子的含羟基和烷氧基的烷基)。最优选的无金属离子的硅酸盐组分是四甲基硅酸铵。可通过溶解任何一种或多种下述材料在高度碱性的清洗剂中,来就地生成用于本发明的其它合适的无金属离子的硅酸盐原料。适用于在清洗剂中生成硅酸盐的、合适的无金属离子的硅酸盐物质包括:固体硅晶片、硅酸、硅溶胶、热解法二氧化硅或其它任何形式的硅或硅石。可以使用金属硅酸盐,如硅酸钠盐,但是因为金属对集成电路具有危害性的影响,所以并不推荐使用金属硅酸盐。组合物中硅酸盐重量百分比为约0-10%之间,优选地含量为约0.1-5%之间。
为提高制剂在溶液中维持金属的能力以及提高晶片基板上金属残余物的溶解性能,可以往本发明的组合物中调配合适的金属螯合剂。通常,螯合剂在组合物中的重量百分比为约0-5%重量,优选的含量为约0.1-2%重量。能满足此目的的螯合剂的典型实例有以下的有机酸及其异构体和相应的盐:乙二胺四乙酸(EDTA)、丁二胺四乙酸、(1,2-环己二胺)四乙酸(CyDTA)、二亚乙基三胺五乙酸(DEPTA)、乙二胺四丙酸、(羟乙基)乙二胺三乙酸(HEDTA)、N,N,N`,N`-亚乙基二胺四(亚甲基膦酸)(EDTMP)、三亚乙基四胺六乙酸(TTHA)、1,3-二氨基-2-羟丙烷-N,N,N`,N`-四乙酸(DHPTA)、甲基亚氨基二乙酸、丙二胺四乙酸、氨三乙酸(NTA)、柠檬酸、酒石酸、葡糖酸、糖酸、甘油酸、草酸、邻苯二甲酸、马来酸、苦杏仁酸、丙二酸、乳酸、水杨酸、儿茶酚、鞣酸(没食子酸)、鞣酸丙酯、焦棓酸、8-羟基喹啉和巯基丙氨酸(半胱氨酸)。优选的螯合剂是氨基羧酸如EDTA、CyDTA和EDTMP。
在清洗组合物内,清洗组合物也可任选地含有氟化物,如四甲基氟化铵、四丁基氟化铵和氟化铵。其它合适的氟化物包括例如氟硼酸盐、四丁基氟硼酸铵、六氟化铝、氟化锑等。氟化物组分的量为约0-10%重量,优选约0.1-5%重量。
本发明的清洗组合物通常包括约0.05-30%重量不产生铵的强碱;约5-99.95%重量位阻酰胺溶剂组分;约0-95%重量水或其它有机共溶剂;约0-40%重量位阻胺或链烷醇胺;约0-40%重量有机或无机酸;约0-40%重量金属腐蚀抑制剂化合物如苯并三唑、儿茶酚、甘油、乙二醇等;约0-5%重量的表面活性剂;约0-10%重量无金属离子的硅酸盐;约0-5%重量的金属螯合剂和约0-10%重量的氟化物。
在下表1中列出了这些类型配方的实例。
表1
组合物-重量份数
组分 A B C D E F G H
DMPH 32 16 16 20 50 16
H2O 32 32 32 32
TMAH 16 16 16 10 10 10 10 16
TEA 16
CyDTA 0.2
SFL 16 30
HEP 50
NMP 50
EDTMP 0.4
DMPD=二甲基哌啶酮
TMAH=25%四甲基氢氧化铵
TEA=三乙醇胺
CyDTA=反式-1,2-环己二胺四乙酸
SFL=环丁砜
HEP=1-(2-羟乙基)-2-吡咯烷酮
NMP=N-甲基吡咯烷酮
EDTMP=亚乙基二胺四(亚甲基膦酸)
通过下表2和3中的蚀刻速率数据显示表1的清洗组合物D、E、F、G和H的铜蚀刻速率。使用下述测试程序,确定蚀刻速率。
使用约13×50mm的铜箔片。测量箔片的厚度。用2-丙醇、蒸馏水和丙酮清洗箔片之后,在干燥烘箱中干燥箔片。然后将清洗过的干燥的箔片置于装有预先加热的本发明清洗组合物瓶中,其瓶盖松散地盖在瓶上;并在指定温度下,将其放置在真空烘箱中2-4小时。从烘箱和瓶子中处理和清除后,用非常大量的蒸馏水漂洗清洗过的箔片,并在干燥烘箱中干燥约1小时,然后使之冷却到室温,并根据计算重量损失或变化来确定蚀刻速率。
结果见表2和3。
表2
组合物 | 在70-75℃下的Cu蚀刻速率(/hr)(24小时试验) |
D | <10 |
E | <10 |
F | <10 |
G | <10 |
表3
组合物 | 在65℃下的Cu蚀刻速率(/hr)(24小时试验) |
H | 1 |
在下述试验中说明了本发明组合物的清洗能力,其中在指定温度和时间下,将包括下述结构晶片的微电子结构体,即PR/ARC/CDO/SiN/Cu双镶嵌(后沟槽蚀刻)(其中PR=光致抗蚀剂和ARC=抗反射层)浸渍在清洗溶液中,然后用水漂洗,干燥,接着通过SEM检测,确定清洗程度。结果见表4。
表4
组合物和工艺条件 | 清洗性能 | 基板相容性 |
组合物H,75℃20分钟 | 100%清洁;清除全部的PR、ARC和残余物 | 与Cu和CDO相容 |
根据本发明的前述说明,本领域的技术人员应理解可在没有脱离本发明的精神和范围的情况下对本发明作出改性。因此,不打算将本发明的范围限制到所例举的和描述的具体实施方案。
Claims (46)
1.一种用于清洗微电子基板中残余物的清洗组合物,所述清洗组合物包括:
约0.05-30%重量的一种或多种含有非亲核的、带正电的反离子的不产生铵的强碱;
约5-99.95%重量的一种或多种位阻酰胺溶剂;
约0-95%重量的水或其它有机共溶剂;
约0-40%重量的位阻胺或链烷醇胺;
约0-40%重量的有机或无机酸;
约0-40%重量的其它金属腐蚀抑制剂化合物;
约0-5%重量的表面活性剂;
约0-10%重量的无金属离子的硅酸盐化合物;
约0-5%重量的金属螯合剂;和
约0-10%重量的氟化物。
2.权利要求1的清洗组合物,其中不产生铵的强碱是四烷基氢氧化铵或其盐。
3.权利要求2的清洗组合物,其中四烷基氢氧化铵或盐是下式的化合物:
[(R)4N+]p[X]-q
其中各R为取代或未取代的烷基;X是OH或盐阴离子;p与q相同且为1-3的整数。
4.权利要求3的清洗组合物,其中R是含有1-22个碳原子的烷基,X是OH或碳酸根。
5.权利要求4的清洗组合物,其中R是含有1-6个碳原子的烷基。
11.权利要求10的清洗组合物,其中在R1-R8基团的定义中,烷基含有1-6个碳原子和芳基含有3-14个碳原子。
12.权利要求1的清洗组合物,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
13.权利要求2的清洗组合物,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
14.权利要求3的清洗组合物,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
15.权利要求4的清洗组合物,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
16.权利要求5的清洗组合物,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
17.权利要求1的清洗组合物,包括水或至少一种其它的有机共溶剂,所述有机共溶剂选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇。
18.权利要求6的清洗组合物,包括水或至少一种其它的有机共溶剂,所述有机共溶剂选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇。
19.权利要求11的清洗组合物,包括水或至少一种其它的有机共溶剂,所述有机共溶剂选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇。
20.权利要求16的清洗组合物,它包括水或至少一种其它的有机共溶剂,所述有机共溶剂选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇。
21.权利要求1的清洗组合物,包括四甲基氢氧化铵、二甲基哌啶酮、三乙醇胺、反式-1,2-环己二胺四乙酸和水。
22.权利要求1的清洗组合物,包括四甲基氢氧化铵、二甲基哌啶酮和水。
23.权利要求1的清洗组合物,包括四甲基氢氧化铵、二甲基哌啶酮、三乙醇胺、乙二胺四(亚甲基膦酸)和水。
24.用于清洗含有多孔电介质、低-κ电介质、高-κ电介质或敷铜中至少之一的微电子基板的方法,所述的方法包括将基板和清洗组合物接触足以清洗基板的时间,其中清洗组合物包括
约0.05-30%重量的一种或多种含有非亲核的、带正电的反离子的不产生铵的强碱;
约5-99.95%重量的位阻酰胺溶剂;
约0-95%重量的水或其它有机共溶剂;
约0-40%重量的位阻胺或链烷醇胺;
约0-40%重量的有机或无机酸;
约0-40%重量的其它金属腐蚀抑制剂化合物;
约0-5%重量的表面活性剂;
约0-10%重量无金属离子的硅酸盐;
约0-5%重量的金属螯合剂;和
约0-10%重量的氟化物。
25.权利要求24的方法,其中不产生铵的强碱是四烷基氢氧化铵或其盐。
26.权利要求25的方法,其中四烷基氢氧化铵或盐是下述分子式的化合物:
[(R)4N+]p[X]-q
其中各R为取代或未取代的烷基;X是OH或盐阴离子;p与q相同且为1-3的整数。
27.权利要求26的方法,其中R是含有1-22个碳原子的烷基,X是OH或碳酸根。
28.权利要求27的方法,其中R是含有1-6个碳原子的烷基。
29.权利要求24的方法,其中位阻酰胺溶剂是选自下述那些分子式中的化合物:
R1CONR2R3和
其中n是1-22的数;R1,R2,R3,R4,R5,R6,R7和R8分别独立地选自H、烷基和芳基,条件是R1,R2和R3中的至少一个以及R4,R5,R6,R7和R8中的至少一个不是H。
30.权利要求25的方法,其中位阻酰胺溶剂是选自下述那些分子式中的化合物:
R1CONR2R3和
其中n是1-22的数;R1,R2,R3,R4,R5,R6,R7和R8分别独立地选自H、烷基和芳基,条件是R1,R2和R3中的至少一个以及R4,R5,R6,R7和R8中的至少一个不是H。
31.权利要求26的方法,其中位阻酰胺溶剂是选自下述那些分子式中的化合物:
R1CONR2R3和
其中n是1-22的数;R1,R2,R3,R4,R5,R6,R7和R8分别独立地选自H、烷基和芳基,条件是R1,R2和R3中的至少一个以及R4,R5,R6,R7和R8中的至少一个不是H。
32.权利要求27的方法,其中位阻酰胺溶剂是选自下述那些分子式中的化合物:
R1CONR2R3和
其中n是1-22的数;R1,R2,R3,R4,R5,R6,R7和R8分别独立地选自H、烷基和芳基,条件是R1,R2和R3中的至少一个以及R4,R5,R6,R7和R8中的至少一个不是H。
33.权利要求28的方法,其中位阻酰胺溶剂是选自下述那些分子式中的化合物:
R1CONR2R3和
其中n是1-22的数;R1,R2,R3,R4,R5,R6,R7和R8分别独立地选自H、烷基和芳基,条件是R1,R2和R3中的至少一个以及R4,R5,R6,R7和R8中的至少一个不是H。
34.权利要求33的方法,其中在R1-R8基团的定义中,烷基含有1-6个碳原子,芳基含有3-14个碳原子。
35.权利要求24的方法,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
36.权利要求25的方法,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
37.权利要求26的方法,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
38.权利要求27的方法,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
39.权利要求28的方法,其中位阻酰胺溶剂选自乙酰胺、二甲基甲酰胺(DMF)、N,N`-二甲基乙酰胺(DMAc)、N-甲基-2-吡咯烷酮(NMP)、1,5-二甲基-2-吡咯烷酮、1,3-二甲基-2-哌啶酮、1-(2-羟乙基)-2-吡咯烷酮和1,5-二甲基-2-哌啶酮。
40.权利要求24的方法,其中清洗组合物包括水或选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇中至少一种的其它共溶剂。
41.权利要求28的方法,其中清洗组合物包括水或选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇中至少一种的其它共溶剂
42.权利要求34的方法,其中清洗组合物包括水或选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇中至少一种的其它共溶剂。
43.权利要求39的方法,其中清洗组合物包括水或至少选自二甲基亚砜、环丁砜、二乙醇胺、三乙醇胺、2-(甲基氨基)乙醇和3-(二乙基氨基)-1,2-丙二醇中至少一种的其它共溶剂。
44.权利要求24的方法,其中清洗组合物包括四甲基氢氧化铵、二甲基哌啶酮、三乙醇胺、反式-1,2-环己二胺四乙酸和水。
45.权利要求24的方法,其中清洗组合物包括四甲基氢氧化铵、二甲基哌啶酮和水。
46.权利要求1的清洗组合物,它包括四甲基氢氧化铵、二甲基哌啶酮、三乙醇胺、乙二胺四(亚甲基膦酸)和水。
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CN101611130B (zh) * | 2007-02-14 | 2011-05-18 | 安万托特性材料股份有限公司 | 用于去除蚀刻残余物以过氧化物活化的金属氧酸盐为基础的制剂 |
CN104024394A (zh) * | 2012-11-21 | 2014-09-03 | 戴纳洛伊有限责任公司 | 从衬底去除物质的方法和组合物 |
CN111519190A (zh) * | 2020-05-27 | 2020-08-11 | 湖北兴福电子材料有限公司 | 一种铜制程面板中稳定蚀刻锥角的蚀刻液及稳定方法 |
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US9329486B2 (en) | 2005-10-28 | 2016-05-03 | Dynaloy, Llc | Dynamic multi-purpose composition for the removal of photoresists and method for its use |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101611130B (zh) * | 2007-02-14 | 2011-05-18 | 安万托特性材料股份有限公司 | 用于去除蚀刻残余物以过氧化物活化的金属氧酸盐为基础的制剂 |
CN104024394A (zh) * | 2012-11-21 | 2014-09-03 | 戴纳洛伊有限责任公司 | 从衬底去除物质的方法和组合物 |
CN104024394B (zh) * | 2012-11-21 | 2019-07-16 | 慧盛材料美国有限责任公司 | 从衬底去除物质的方法和组合物 |
CN111519190A (zh) * | 2020-05-27 | 2020-08-11 | 湖北兴福电子材料有限公司 | 一种铜制程面板中稳定蚀刻锥角的蚀刻液及稳定方法 |
CN111519190B (zh) * | 2020-05-27 | 2022-03-18 | 湖北兴福电子材料有限公司 | 一种铜制程面板中稳定蚀刻锥角的蚀刻液及稳定方法 |
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MY139607A (en) | 2009-10-30 |
CA2452884C (en) | 2010-12-07 |
RS904A (sr) | 2007-02-05 |
WO2003006597A1 (en) | 2003-01-23 |
BR0211054A (pt) | 2004-07-20 |
KR100944444B1 (ko) | 2010-02-26 |
TWI292437B (en) | 2008-01-11 |
IL159761A (en) | 2006-12-10 |
CN102399651A (zh) | 2012-04-04 |
IN2004CH00042A (zh) | 2005-12-02 |
NO20040067L (no) | 2004-03-05 |
KR20090076934A (ko) | 2009-07-13 |
AU2002320305A1 (en) | 2003-01-29 |
ZA200400064B (en) | 2004-10-27 |
PL199501B1 (pl) | 2008-09-30 |
PL367838A1 (en) | 2005-03-07 |
EP1404796B1 (en) | 2012-02-15 |
JP2004536181A (ja) | 2004-12-02 |
IL159761A0 (en) | 2004-06-20 |
CA2452884A1 (en) | 2003-01-23 |
JP4177758B2 (ja) | 2008-11-05 |
ATE545695T1 (de) | 2012-03-15 |
KR20040018437A (ko) | 2004-03-03 |
EP1404796A1 (en) | 2004-04-07 |
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