CN116254159A - 一种清洗液及其应用 - Google Patents
一种清洗液及其应用 Download PDFInfo
- Publication number
- CN116254159A CN116254159A CN202111503252.2A CN202111503252A CN116254159A CN 116254159 A CN116254159 A CN 116254159A CN 202111503252 A CN202111503252 A CN 202111503252A CN 116254159 A CN116254159 A CN 116254159A
- Authority
- CN
- China
- Prior art keywords
- acid
- ammonium
- triazole
- cleaning solution
- amino
- 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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- 238000004140 cleaning Methods 0.000 title claims abstract description 70
- 239000012530 fluid Substances 0.000 title description 4
- 229910017052 cobalt Inorganic materials 0.000 claims abstract description 44
- 239000010941 cobalt Substances 0.000 claims abstract description 44
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000005260 corrosion Methods 0.000 claims abstract description 25
- 230000007797 corrosion Effects 0.000 claims abstract description 25
- 239000003112 inhibitor Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007800 oxidant agent Substances 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 230000001590 oxidative effect Effects 0.000 claims abstract description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 3
- 125000001424 substituent group Chemical group 0.000 claims abstract description 3
- -1 nitrogen-containing heterocyclic azole compound Chemical class 0.000 claims description 20
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000002738 chelating agent Substances 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 8
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 8
- LJVQHXICFCZRJN-UHFFFAOYSA-N 1h-1,2,4-triazole-5-carboxylic acid Chemical compound OC(=O)C1=NC=NN1 LJVQHXICFCZRJN-UHFFFAOYSA-N 0.000 claims description 6
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- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 4
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- FKPSBYZGRQJIMO-UHFFFAOYSA-M benzyl(triethyl)azanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC1=CC=CC=C1 FKPSBYZGRQJIMO-UHFFFAOYSA-M 0.000 claims description 4
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- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 claims description 4
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- QMPFMODFBNEYJH-UHFFFAOYSA-N methyl 1h-1,2,4-triazole-5-carboxylate Chemical compound COC(=O)C1=NC=NN1 QMPFMODFBNEYJH-UHFFFAOYSA-N 0.000 claims description 4
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 4
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- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 4
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 4
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 4
- HADKRTWCOYPCPH-UHFFFAOYSA-M trimethylphenylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C1=CC=CC=C1 HADKRTWCOYPCPH-UHFFFAOYSA-M 0.000 claims description 4
- MLVNUTAJXZZPCJ-UHFFFAOYSA-N ethyl 3-amino-1h-1,2,4-triazole-5-carboxylate Chemical compound CCOC(=O)C1=NC(N)=NN1 MLVNUTAJXZZPCJ-UHFFFAOYSA-N 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 2
- FMCUPJKTGNBGEC-UHFFFAOYSA-N 1,2,4-triazol-4-amine Chemical compound NN1C=NN=C1 FMCUPJKTGNBGEC-UHFFFAOYSA-N 0.000 claims description 2
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- FYIHPNCKLYPALH-UHFFFAOYSA-N 2-[2-(2-aminophenoxy)ethenoxy]aniline Chemical compound NC1=CC=CC=C1OC=COC1=CC=CC=C1N FYIHPNCKLYPALH-UHFFFAOYSA-N 0.000 claims description 2
- FCKYPQBAHLOOJQ-UWVGGRQHSA-N 2-[[(1s,2s)-2-[bis(carboxymethyl)amino]cyclohexyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)[C@H]1CCCC[C@@H]1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UWVGGRQHSA-N 0.000 claims description 2
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- FRRMMWJCHSFNSG-UHFFFAOYSA-N diazanium;propanedioate Chemical compound [NH4+].[NH4+].[O-]C(=O)CC([O-])=O FRRMMWJCHSFNSG-UHFFFAOYSA-N 0.000 claims description 2
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- WJLUBOLDZCQZEV-UHFFFAOYSA-M hexadecyl(trimethyl)azanium;hydroxide Chemical compound [OH-].CCCCCCCCCCCCCCCC[N+](C)(C)C WJLUBOLDZCQZEV-UHFFFAOYSA-M 0.000 claims description 2
- NPZTUJOABDZTLV-UHFFFAOYSA-N hydroxybenzotriazole Substances O=C1C=CC=C2NNN=C12 NPZTUJOABDZTLV-UHFFFAOYSA-N 0.000 claims description 2
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- OSZNPKRMPBUQLB-UHFFFAOYSA-N methyl 3-amino-1h-1,2,4-triazole-5-carboxylate Chemical compound COC(=O)C1=NC(N)=NN1 OSZNPKRMPBUQLB-UHFFFAOYSA-N 0.000 claims description 2
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- UKODFQOELJFMII-UHFFFAOYSA-N pentamethyldiethylenetriamine Chemical compound CN(C)CCN(C)CCN(C)C UKODFQOELJFMII-UHFFFAOYSA-N 0.000 claims description 2
- XCRBXWCUXJNEFX-UHFFFAOYSA-N peroxybenzoic acid Chemical compound OOC(=O)C1=CC=CC=C1 XCRBXWCUXJNEFX-UHFFFAOYSA-N 0.000 claims description 2
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- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 3
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- 238000001035 drying Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
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- 229920002873 Polyethylenimine Polymers 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000000010 aprotic solvent Substances 0.000 description 1
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- 125000003354 benzotriazolyl group Chemical group N1N=NC2=C1C=CC=C2* 0.000 description 1
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- DHZYWCBUDKTLGD-UHFFFAOYSA-N ethyl 1h-1,2,4-triazole-5-carboxylate Chemical compound CCOC(=O)C1=NC=NN1 DHZYWCBUDKTLGD-UHFFFAOYSA-N 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
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- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical group 0.000 description 1
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- 239000003381 stabilizer Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000004381 surface treatment Methods 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
- 238000010998 test method Methods 0.000 description 1
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- BDTOTMBOHYUNSQ-UHFFFAOYSA-N triazole-1-carboxylic acid Chemical compound OC(=O)N1C=CN=N1 BDTOTMBOHYUNSQ-UHFFFAOYSA-N 0.000 description 1
Images
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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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- C11D7/22—Organic compounds
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- C11D7/3281—Heterocyclic compounds
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Abstract
Description
技术领域
本发明涉及化学清洗液领域,尤其涉及一种清洗液及其应用。
背景技术
光刻胶硬掩模通常用于对半导体材料或电介质进行图案化处理,目前光刻胶硬掩模被用于双镶嵌工艺中以在微电子器件的后端金属化中形成互连。随着尺寸越来越小,集成电路(IC)的可靠性越来越受到IC制造技术的关注。跟踪互连故障机制对器件性能和可靠性的影响需要更多来自集成方案、互连材料和工艺,需要最佳的Low-k介电材料及其相关的沉积、图案光刻、蚀刻和清洁来形成双镶嵌互连图案。互连图案晶圆制造的硬掩模方案方法是能够以最严格的最佳尺寸控制将图案转移到底层。
随着技术节点发展到14nm、7nm甚至更小线宽,深宽比增加,TiN等金属硬掩模材料被用于在图案蚀刻过程中获得更好的蚀刻/去除选择性、更好的图案保留和对Low-k材料的轮廓控制。需要对TiN硬掩模进行修饰甚至完全去除,同时对铜、钴、钽、铷等金属材料,TEOS、BDII等Low-k介电材料具有良好的兼容性。此外,由于蚀刻残留物的低表面能和交联性质,以及残留物成分物理和化学性质的变化,加之清洗液与设备膜材料和结构之间的兼容性问题,使得开发能够有效去除光刻胶刻蚀残留物的同时又能保护 Low-k介电材料和非金属材料,并且金属材料表面残留低的清洗液越来越具有挑战性。
国内外对高端半导体清洗液的报道主要以欧美国家为主。美国专利US10920141B2公开了一种用于选择性刻蚀氮化钛,保护钴的组合物和方法。该清洗液主要以双氧水作为氧化剂,TMAH和含氟组分作为蚀刻剂,添加唑类和阳离子季盐作为腐蚀抑制剂,有机酸作为螯合剂,加之溶剂水,可选择性去除氮化钛和光致抗蚀剂刻蚀残留物。从公开的专利来看,该清洗液可在pH值5~12、20℃~100℃温度范围内工作,50℃条件下测试的TiN蚀刻速率大于Cu蚀刻速率小于/>Co蚀刻速率小于/> SiN蚀刻速率小于Low-k介电材料的蚀刻速率小于/>该公司产品主要在欧美国家使用,在半导体清洗液领域仍占据较大市场份额。
最新报道中,美国Versum Material公司在专利US11017995B2中公开了一种用于从电子电路器件除去TiN硬掩模的组合物、方法和系统。该组合物pH值范围为5.5~14,使用工艺温度为35℃~70℃,适用范围较广,可用于半导体基板或晶圆、平板显示器、相变存储器、太阳能电池板、微电子、集成电路或计算机芯片等领域。该清洗液主要以双氧水作为氧化剂,大分子有机酸作为双氧水稳定剂,唑类和多元醇类作为金属腐蚀抑制剂,季铵氢氧化物和铵盐作为蚀刻剂,水作为溶剂,加之以任选氟化物来增强清洗能力,选择性地除去氮化钛和来自等离子体刻蚀过程中的残留物,同时使Cu、Co、Low-k 介电材料等第二材料得到有效保护。
为了保证较好的晶圆表面处理,在14nm及以下技术节点IC领域使用较多的是配置以双氧水,采用“To drain”模式来清洗图案晶圆。德国巴斯夫公司在专利CN110713868A 中公开了一种可循环使用的清洗液组合物,该组合物主要为A剂和B剂H2O2按体积比 1:1组合,采用“Recycle”模式来调节Cu、Co、Ru和TiN的蚀刻速率。其中A剂组合物包括有机胺4-甲基吗啉4-氧化物、聚乙烯亚胺+唑类作为腐蚀抑制剂、TMAH+磷酸二氢铵作为缓冲剂、有机酸铵盐作为蚀刻剂、乙二醇醚作为有机溶剂、任选非质子溶剂和水,对碳氟(CFx)聚合物和有机残渣具有良好的清洁性能,能够完全或部分去除TiN,同时保护Cu、Co、Ru等金属材料,该产品目前主要在中国台湾地区的台湾积体电路制造股份有限公司用于加工半导体晶圆。
发明内容
因此,本发明的主要目的是,提供一种清洗液,能够选择性去除TiN硬掩模,同时能够保护金属材料、非金属材料以及Low-k介质材料的前提下,能够有效降低金属钴表面有机物的残留。
其中,R1、R2、R3表示氢原子或取代基。
优选的,所述第一化合物选自1,2,4-三氮唑-3-羧酸、1,2,4-三氮唑-3-羧酸甲酯、1,2,4- 三氮唑-3-羧酸乙酯、5-氨基-1,2,4-三氮唑-3-羧酸、5-氨基-1H--1,2,4-三氮唑-3-羧酸甲酯、 5-氨基-1H-1,2,4-三氮唑-3-羧酸乙酯、2,3,5-三-O-三乙酰-B-D-呋喃核糖基-1,2,4-三氮唑-3- 羧酸甲酯(利巴韦林缩合物)、5-氨基-1H-1,2,4-三氮唑-3-羧酸酰胺、N-(2',4'-二氯苯亚甲基)-5-氨基-1H-1,2,4-三氮唑-3-羧酸、5-X-1H-1,2,4-三氮唑-3-羧酸乙酯(X=Cl,Br,I)、5-甲基 -2H-1,2,4-三氮唑-3-羧酸中的一种或多种。
优选的,所述第一化合物的质量百分比含量为0.01wt%-10wt%。
优选的,所述氧化剂选自H2O2、N-甲基吗啉氧化物、过氧化苯甲酰、过乙酸、过氧化脲、硝酸、过氧乙酸、过氧苯甲酸、四氧嘧啶中的一种或多种;更加优选的,所述氧化剂为H2O2。
优选的,所述氧化剂的质量百分比含量为0.1wt%-30wt%。
优选的,所述钴腐蚀抑制剂为含氮杂环唑类化合物。
优选的,所述钴腐蚀抑制剂选自苯并三氮唑(BTA)、1,2,4-三氮唑、5-甲基苯并三氮唑(TTA)、羟基苯并三唑、吡唑、甲苯三唑、3,5-二甲基吡唑、四氮唑、4-氨基-1,2,4- 三唑、苯并噻唑、甲基-1H-苯并三唑(TTL)、2-氨基苯并噻唑、2-巯基苯并噻唑、3-氨基-5- 羟基吡唑、1-苯基吡唑、巯基苯并咪唑、5-氨基四唑、3-巯基-1,2,4-三唑、3-异丙基-1,2,4-三唑、2-(5-氨基-戊基)-苯并三唑、5-苯硫醇-苯并三唑、甲基四唑、5-苯基-苯并三唑、5-硝基-苯并三唑、3-氨基-5-巯基-1,2,4-三唑、1-氨基-1,2,4三唑、1-氨基-1,2,3-苯并三唑、噻唑中的一种或多种;更加优选的,所述钴腐蚀抑制剂为苯并三氮唑。
优选的,所述钴腐蚀抑制剂的质量百分比含量为0.01wt%-10wt%。
优选的,还包括螯合剂,所述螯合剂为有机酸。
优选的,所述螯合剂为选自甘氨酸、丝氨酸、脯氨酸、亮氨酸、丙氨酸、天冬氨酸、天冬酰胺、谷氨酰胺、缬氨酸、赖氨酸、胱氨酸、乙二胺四乙酸(EDTA)、反式-1,2环己二胺四乙酸(CDTA)、尿酸、吡啶甲酸、次氮基三乙酸(NTA)、乙二胺-N,N’-二琥铂酸 (EDDS)、谷氨酸、二乙烯三胺五乙酸(DTPA)、羟乙基乙二胺三乙酸(HEDTA)、亚氨基二乙酸(IDA)、氨三乙酸、水杨酸、葡萄糖酸、烟酸、酒石酸、柠檬酸、1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸(DOTA)、乙二醇四乙酸(EGTA)、1,2-双(邻氨基苯氧基)乙烷 -N,N,N’,N’-四乙酸、乙二胺-N,N’-双(2-羟基苯乙酸)(HDDHA)、丙二胺四乙酸中的一种或多种。
优选的,所述螯合剂的质量百分比含量为0.05-1000ppm;更加优选的,所述螯合剂的质量百分比含量为0.1-100ppm。
优选的,进一步包括有机碱,选自季胺氢氧化合物、有机胺、有机醇胺中的一种或多种;更加优选金属离子含量少(<50ppb)的有机碱。
优选的,所述季胺氢氧化合物选自四甲基氢氧化铵(TMAH)、四乙基氢氧化铵(TEAH)、三甲基苯基氢氧化铵(TMPAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵 (TBAH)、苄基三甲基氢氧化铵(BTMAH)、苄基三乙基氢氧化铵(BTEAH)、胆碱氢氧化物、氢氧化铵、十二烷基三甲基氢氧化铵(DTAH)、十六烷基三甲基氢氧化铵(CTOH) 中的一种或多种;
所述有机胺选自单乙胺、二乙胺、三乙胺、三丙胺、N'N-二乙基乙二胺、羟乙基乙二胺、环己胺、1,2-丙二胺、五甲基二乙烯三胺中的一种或多种;
所述有机醇胺选自单乙醇胺(MEA)、二乙醇胺(DEA)、三乙醇胺(TEA)、二甘醇胺(DGA)、异丙醇胺、N-甲基乙醇胺中的一种或多种。
优选的,所述有机碱的质量百分比含量为0.1wt%-10wt%。
优选的,进一步包括有机酸铵盐。
优选的,所述有机酸铵盐选自甲酸铵、草酸铵、乳酸铵、酒石酸铵、柠檬酸三铵、乙酸铵、氨基甲酸铵、碳酸铵、苯甲酸铵、EDTA四铵、EDTA三铵、EDTA二铵、琥珀酸铵、1-H-吡唑-3-甲酸铵、丙二酸铵、己二酸铵、亚氨基二乙酸铵中的一种或多种。
优选的,所述有机酸铵盐的质量百分比含量为0.01wt%-50wt%。
本发明的另一方面,提供一种将以上任一所述的化学清洗液用于清洗钴的应用方法。
优选的,应用的温度为20-80℃;应用的pH值为4~12
通过添加三氮唑化合物,可有效降低钴表面有机物的残留,配合以氧化剂、钴腐蚀抑制剂、水等,可有效去除氮化钛硬掩模和光致抗蚀剂刻蚀残留物,并且在高速旋转单片机清洗中对金属材料、非金属材料以及Low-k介电材料等均表现出较小的腐蚀速率,提高了半导体器件的电性能,产品良率也有较大提升,操作窗口较大,在集成电路14nm 及以下技术节点等高端半导体清洗领域具有良好的应用前景。
附图说明
图1为经本发明实施例21与对比例1清洗液清洗后钴表面的XPS图谱;
图2为经本发明实施例22与对比例2清洗液清洗后钴表面的XPS图谱;
图3为经本发明实施例23与对比例3清洗液清洗后钴表面的XPS图谱。
具体实施方式
以下结合具体实施例及附图进一步阐述本发明的优点。
根据表1中的各组分及其含量配制实施例1-30及对比例1-3的清洗液。并且在相应温度下使用。
表1实施例1-30及对比例1-3中清洗液的组分及其含量
为了进一步测试上述清洗液的抛光性能,用实施例21-23清洗液对不同的材料进行蚀刻测试。具体测试条件如下:
用于测试蚀刻速率的测试对象及其来源:
TiN(氮化钛)空白晶片——Ramco Specialties Inc.(美国拉姆科专业有限公司)
Cu(铜)空白晶片——Ramco Specialties Inc.
Co(钴)空白晶片——Ramco Specialties Inc.
SiON(氮氧化硅)空白晶片——Ramco Specialties Inc.
TEOS(二氧化硅)空白晶片——Ramco Specialties Inc.
BDII(低介电常数氧化硅)空白晶片——Ramco Specialties Inc.
TiN、Cu、Co等金属蚀刻速率测试方法:
(1)利用Napson四点探针仪测试5*5cm金属空白晶片(TiN空白晶片、Cu空白晶片、Co空白晶片)的电阻初值(Rs1);
(2)将该5*5cm金属空白晶片在迷你单片机mini-SWT上400rpm,TiN空白晶片经清洗液处理5min,Cu空白晶片和Co空白晶片化学处理10min;
(3)取出该5*5cm金属空白晶片,用去离子水(DIW)清洗,高纯氮气吹干,再利用Napson四点探针仪测试5*5cm金属空白晶片的电阻值(Rs2);
(4)将上述电阻值和蚀刻时间输入到合适的程序可计算出金属的蚀刻速率。
SiON、TEOS、BDII等非金属蚀刻速率测试方法:
1)按照标准开启Nanospec6100测厚仪,选用合适的测试程序,将5*5cm非金属空白晶片(SiON空白晶片、TEOS空白晶片、BDII空白晶片)放入Nanospec6100测厚仪上测试非金属空白晶片厚度,将非金属空白晶片旋转90°继续测试,连续测试4次,记录数值;
2)若非金属空白晶片为BDII,需用水冲洗干净,马弗炉350℃处理20min,干燥器冷却至室温再测试前值;(其他晶片无需步骤2)
3)将该5*5cm非金属空白晶片在mini-SWT上400rpm,清洗液处理10min;
4)取出该5*5cm非金属空白晶片,用DIW清洗,高纯氮气吹干,在Nanospec6100 测厚仪上按程序1测试晶片厚度,记录数值;
5)若非金属空白晶片为BDII,需用水冲洗干净,马弗炉350℃处理20min,干燥器冷却至室温再测试后值;(其他晶片无需步骤5)
6)将上述前后厚度值和蚀刻时间输入合适的程序中,蚀刻速率计算为厚度变化除以化学处理时间。
按照上述蚀刻速率测试方法测试不同空白晶片的蚀刻速率。由于钴腐蚀抑制剂基本都是含N的杂环化合物,利用X射线光电子能谱分析仪(XPS)测试清洗液中的金属缓蚀剂在钴表面的吸附情况,基于N元素的信号强度如图1~图3所示。同时在50℃、 400rpm/min的条件下,使用mini-SWT单片机清洗图案晶圆90s,水漂洗干净,氮气吹干, SEM观察评估晶圆清洗效果。不同空白晶片的蚀刻速率、表面吸附结果及清洗效果见表 2。
表2实施例21-23与对比例1-3的蚀刻测试及清洗结果
金属钴表面吸附结果(XPS) | 晶圆清洗结果 |
◎基本无吸附 | ◎基本清洗干净 |
○轻微吸附 | ○少量残留物 |
△较多吸附 | △较多残留物 |
×严重吸附 | ×大量残留物 |
从表2中可以看出:本发明的清洗液在TiN硬掩模完全去除的情况下,对半导体制程中所用的金属材料(如Cu和Co)和非金属材料(SiON、TEOS、BDII)基本没有刻蚀,其腐蚀情况均满足半导体业界通常在高速旋转单片机清洗的要求。
对比例1与实施例21对照表明,添加了1,2,4-三氮唑-3-羧酸的体系,晶圆的蚀刻速率变化不大,均满足刻蚀要求。结合图1可知,添加了1,2,4-三氮唑-3-羧酸的清洗液处理的钴表面N元素相对强度要弱,说明有机物在金属钴表面的吸附量实施例21比不添加 1,2,4-三氮唑-3-羧酸体系的对比例1要少很多,进而在钴表面的有机残留物要更少。从表 2的图形晶圆的清洗效果也可以看出,添加了1,2,4-三氮唑-3-羧酸的体系处理的图形晶圆基本清洗干净,这样有利于提高半导体器件的良率。
对比例2与实施例22对照表明,添加了1,2,4-三氮唑-3-羧酸甲酯的体系,处理的晶圆蚀刻速率与不添加该组分的体系处理的基本一致,变化不大。结合X射线光电子能谱分析仪分析结果图2可知,添加了1,2,4-三氮唑-3-羧酸甲酯的体系实施例22处理的钴表面N元素相对强度要弱一些,有机物在钴表面的吸附量比不添加的体系对比例2要更低,图形晶圆的大马士革金属孔道清洗效果更好,钴表面的有机残留物得到进一步的改善。
对比例3与实施例23对照表明,添加了5-氨基-1,2,4-三氮唑-3-羧酸与不添加的体系晶圆蚀刻速率变化不大。从图3的X射线光电子能谱分析仪结果分析可知,添加了5-氨基-1,2,4-三氮唑-3-羧酸的体系处理的金属钴表面N元素的相应强度要弱一些,表明有机物的吸附要更少,有利于提高图形晶圆的导电性能。
含N唑类杂环化合物是很好的金属钴保护剂,其吸附在金属钴表面可有效控制钴的腐蚀,但该有机保护膜也影响了半导体器件的导电性能。XPS结果显示N元素的吸收峰响应强度能够反映有机物保护膜在金属钴表面的吸附程度,三氮唑化合物中存在活性阴离子,在金属钴表面与钴腐蚀抑制剂形成竞争性吸附,使得金属缓蚀剂在保护钴的同时可以在短时间内从钴表面脱附,进一步降低了金属钴表面有机物的残留。
综上,本发明的积极进步效果在于:通过添加第一化合物,可有效降低钴表面有机物的残留。配合以氧化剂、钴腐蚀抑制剂、水等,可有效去除氮化钛硬掩模和光致抗蚀剂刻蚀残留物,并且在高速旋转单片机清洗中对金属材料、非金属材料以及Low-k介电材料等均表现出较小的腐蚀速率,提高了半导体器件的电性能,产品良率也有较大提升,操作窗口较大,在集成电路14nm及以下技术节点等高端半导体清洗领域具有良好的应用前景。
应当注意的是,本发明的实施例有较佳的实施性,且并非对本发明作任何形式的限制,任何熟悉该领域的技术人员可能利用上述揭示的技术内容变更或修饰为等同的有效实施例,但凡未脱离本发明技术方案的内容,依据本发明的技术实质对以上实施例所作的任何修改或等同变化及修饰,均仍属于本发明技术方案的范围内。
Claims (19)
2.如权利要求1所述的清洗液,其特征在于,
所述第一化合物选自1,2,4-三氮唑-3-羧酸、1,2,4-三氮唑-3-羧酸甲酯、1,2,4-三氮唑-3-羧酸乙酯、5-氨基-1,2,4-三氮唑-3-羧酸、5-氨基-1H--1,2,4-三氮唑-3-羧酸甲酯、5-氨基-1H-1,2,4-三氮唑-3-羧酸乙酯、2,3,5-三-O-三乙酰-B-D-呋喃核糖基-1,2,4-三氮唑-3-羧酸甲酯(利巴韦林缩合物)、5-氨基-1H-1,2,4-三氮唑-3-羧酸酰胺、N-(2',4'-二氯苯亚甲基)-5-氨基-1H-1,2,4-三氮唑-3-羧酸、5-X-1H-1,2,4-三氮唑-3-羧酸乙酯(X=Cl,Br,I)、5-甲基-2H-1,2,4-三氮唑-3-羧酸中的一种或多种。
3.如权利要求1所述的清洗液,其特征在于,
所述第一化合物的质量百分比含量为0.01wt%-10wt%。
4.如权利要求1所述的清洗液,其特征在于,
所述氧化剂选自H2O2、N-甲基吗啉氧化物、过氧化苯甲酰、过乙酸、过氧化脲、硝酸、过氧乙酸、过氧苯甲酸、四氧嘧啶中的一种或多种。
5.如权利要求1所述的清洗液,其特征在于,
所述氧化剂的质量百分比含量为0.1wt%-30wt%。
6.如权利要求1所述的清洗液,其特征在于,
所述钴腐蚀抑制剂为含氮杂环唑类化合物。
7.如权利要求6所述的清洗液,其特征在于,
所述钴腐蚀抑制剂选自苯并三氮唑(BTA)、1,2,4-三氮唑、5-甲基苯并三氮唑(TTA)、羟基苯并三唑、吡唑、甲苯三唑、3,5-二甲基吡唑、四氮唑、4-氨基-1,2,4-三唑、苯并噻唑、甲基-1H-苯并三唑(TTL)、2-氨基苯并噻唑、2-巯基苯并噻唑、3-氨基-5-羟基吡唑、1-苯基吡唑、巯基苯并咪唑、5-氨基四唑、3-巯基-1,2,4-三唑、3-异丙基-1,2,4-三唑、2-(5- 氨基-戊基)-苯并三唑、5-苯硫醇-苯并三唑、甲基四唑、5-苯基-苯并三唑、5-硝基-苯并三唑、3-氨基-5-巯基-1,2,4-三唑、1-氨基-1,2,4三唑、1-氨基-1,2,3-苯并三唑、噻唑中的一种或多种。
8.如权利要求1所述的清洗液,其特征在于,
所述钴腐蚀抑制剂的质量百分比含量为0.01wt%-10wt%。
9.如权利要求1所述的清洗液,其特征在于,
还包括螯合剂,所述螯合剂为有机酸。
10.如权利要求9所述的清洗液,其特征在于,
所述螯合剂为选自甘氨酸、丝氨酸、脯氨酸、亮氨酸、丙氨酸、天冬氨酸、天冬酰胺、谷氨酰胺、缬氨酸、赖氨酸、胱氨酸、乙二胺四乙酸(EDTA)、反式-1,2环己二胺四乙酸(CDTA)、尿酸、吡啶甲酸、次氮基三乙酸(NTA)、乙二胺-N,N’-二琥铂酸(EDDS)、谷氨酸、二乙烯三胺五乙酸(DTPA)、羟乙基乙二胺三乙酸(HEDTA)、亚氨基二乙酸(IDA)、氨三乙酸、水杨酸、葡萄糖酸、烟酸、酒石酸、柠檬酸、1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸(DOTA)、乙二醇四乙酸(EGTA)、1,2-双(邻氨基苯氧基)乙烷-N,N,N’,N’-四乙酸、乙二胺-N,N’-双(2-羟基苯乙酸)(HDDHA)、丙二胺四乙酸中的一种或多种。
11.如权利要求9所述的清洗液,其特征在于,
所述螯合剂的质量百分比含量为0.05-1000ppm。
12.如权利要求1所述的清洗液,其特征在于,
进一步包括有机碱,选自季胺氢氧化合物、有机胺、有机醇胺中的一种或多种。
13.如权利要求12所述的清洗液,其特征在于,
所述季胺氢氧化合物选自四甲基氢氧化铵(TMAH)、四乙基氢氧化铵(TEAH)、三甲基苯基氢氧化铵(TMPAH)、四丙基氢氧化铵(TPAH)、四丁基氢氧化铵(TBAH)、苄基三甲基氢氧化铵(BTMAH)、苄基三乙基氢氧化铵(BTEAH)、胆碱氢氧化物、氢氧化铵、十二烷基三甲基氢氧化铵(DTAH)、十六烷基三甲基氢氧化铵(CTOH)中的一种或多种;
所述有机胺选自单乙胺、二乙胺、三乙胺、三丙胺、N'N-二乙基乙二胺、羟乙基乙二胺、环己胺、1,2-丙二胺、五甲基二乙烯三胺中的一种或多种;
所述有机醇胺选自单乙醇胺(MEA)、二乙醇胺(DEA)、三乙醇胺(TEA)、二甘醇胺(DGA)、异丙醇胺、N-甲基乙醇胺中的一种或多种。
14.如权利要求12所述的化学清洗液,其特征在于,
所述有机碱的质量百分比含量为0.1wt%-10wt%。
15.如权利要求1所述的清洗液,其特征在于,
进一步包括有机酸铵盐。
16.如权利要求15所述的清洗液,其特征在于,
所述有机酸铵盐选自甲酸铵、草酸铵、乳酸铵、酒石酸铵、柠檬酸三铵、乙酸铵、氨基甲酸铵、碳酸铵、苯甲酸铵、EDTA四铵、EDTA三铵、EDTA二铵、琥珀酸铵、1-H-吡唑-3-甲酸铵、丙二酸铵、己二酸铵、亚氨基二乙酸铵中的一种或多种。
17.如权利要求15所述的清洗液,其特征在于,
所述有机酸铵盐的质量百分比含量为0.01wt%-50wt%。
18.一种将权利要求1-17中任一所述的清洗液用于清洗钴的应用方法。
19.如权利要求18所述的应用方法,其特征在于,
应用的温度为20-80℃,pH值为4~12。
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