CN113430063B - 用于选择性移除硬遮罩的清洗液、其制备方法及应用 - Google Patents
用于选择性移除硬遮罩的清洗液、其制备方法及应用 Download PDFInfo
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- CN113430063B CN113430063B CN202010208599.3A CN202010208599A CN113430063B CN 113430063 B CN113430063 B CN 113430063B CN 202010208599 A CN202010208599 A CN 202010208599A CN 113430063 B CN113430063 B CN 113430063B
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- cleaning solution
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- ammonium
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- 238000004140 cleaning Methods 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 30
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- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 14
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- DZPJVKXUWVWEAD-UHFFFAOYSA-N [C].[N].[Si] Chemical compound [C].[N].[Si] DZPJVKXUWVWEAD-UHFFFAOYSA-N 0.000 description 1
- NJYZCEFQAIUHSD-UHFFFAOYSA-N acetoguanamine Chemical compound CC1=NC(N)=NC(N)=N1 NJYZCEFQAIUHSD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229940043376 ammonium acetate Drugs 0.000 description 1
- 235000019257 ammonium acetate Nutrition 0.000 description 1
- 229940090948 ammonium benzoate Drugs 0.000 description 1
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- KHPLPBHMTCTCHA-UHFFFAOYSA-N ammonium chlorate Chemical compound N.OCl(=O)=O KHPLPBHMTCTCHA-UHFFFAOYSA-N 0.000 description 1
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 description 1
- 229940059265 ammonium lactate Drugs 0.000 description 1
- 235000019286 ammonium lactate Nutrition 0.000 description 1
- 239000012935 ammoniumperoxodisulfate Substances 0.000 description 1
- NHJPVZLSLOHJDM-UHFFFAOYSA-N azane;butanedioic acid Chemical compound [NH4+].[NH4+].[O-]C(=O)CCC([O-])=O NHJPVZLSLOHJDM-UHFFFAOYSA-N 0.000 description 1
- ZRDJERPXCFOFCP-UHFFFAOYSA-N azane;iodic acid Chemical compound [NH4+].[O-]I(=O)=O ZRDJERPXCFOFCP-UHFFFAOYSA-N 0.000 description 1
- RZOBLYBZQXQGFY-HSHFZTNMSA-N azanium;(2r)-2-hydroxypropanoate Chemical compound [NH4+].C[C@@H](O)C([O-])=O RZOBLYBZQXQGFY-HSHFZTNMSA-N 0.000 description 1
- NGPGDYLVALNKEG-UHFFFAOYSA-N azanium;azane;2,3,4-trihydroxy-4-oxobutanoate Chemical compound [NH4+].[NH4+].[O-]C(=O)C(O)C(O)C([O-])=O NGPGDYLVALNKEG-UHFFFAOYSA-N 0.000 description 1
- YUUVAZCKXDQEIS-UHFFFAOYSA-N azanium;chlorite Chemical compound [NH4+].[O-]Cl=O YUUVAZCKXDQEIS-UHFFFAOYSA-N 0.000 description 1
- URGYLQKORWLZAQ-UHFFFAOYSA-N azanium;periodate Chemical compound [NH4+].[O-]I(=O)(=O)=O URGYLQKORWLZAQ-UHFFFAOYSA-N 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 229940078916 carbamide peroxide Drugs 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- KYQODXQIAJFKPH-UHFFFAOYSA-N diazanium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [NH4+].[NH4+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O KYQODXQIAJFKPH-UHFFFAOYSA-N 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- NPZTUJOABDZTLV-UHFFFAOYSA-N hydroxybenzotriazole Substances O=C1C=CC=C2NNN=C12 NPZTUJOABDZTLV-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- 229940102253 isopropanolamine Drugs 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000012788 optical film Substances 0.000 description 1
- AENSXLNDMRQIEX-UHFFFAOYSA-L oxido sulfate;tetrabutylazanium Chemical compound [O-]OS([O-])(=O)=O.CCCC[N+](CCCC)(CCCC)CCCC.CCCC[N+](CCCC)(CCCC)CCCC AENSXLNDMRQIEX-UHFFFAOYSA-L 0.000 description 1
- 229960003330 pentetic acid Drugs 0.000 description 1
- 229960005152 pentetrazol Drugs 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- SQBYOEGDVPZABK-UHFFFAOYSA-N pyrazolo[4,3-b]pyridin-1-amine Chemical compound C1=CC=C2N(N)N=CC2=N1 SQBYOEGDVPZABK-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- LUVHDTDFZLTVFM-UHFFFAOYSA-M tetramethylazanium;chlorate Chemical compound [O-]Cl(=O)=O.C[N+](C)(C)C LUVHDTDFZLTVFM-UHFFFAOYSA-M 0.000 description 1
- FDXKBUSUNHRUIZ-UHFFFAOYSA-M tetramethylazanium;chlorite Chemical compound [O-]Cl=O.C[N+](C)(C)C FDXKBUSUNHRUIZ-UHFFFAOYSA-M 0.000 description 1
- ZRVXFJFFJZFRLQ-UHFFFAOYSA-M tetramethylazanium;iodate Chemical compound [O-]I(=O)=O.C[N+](C)(C)C ZRVXFJFFJZFRLQ-UHFFFAOYSA-M 0.000 description 1
- ZCWKIFAQRXNZCH-UHFFFAOYSA-M tetramethylazanium;perchlorate Chemical compound C[N+](C)(C)C.[O-]Cl(=O)(=O)=O ZCWKIFAQRXNZCH-UHFFFAOYSA-M 0.000 description 1
- HLQAWDQQEJSALG-UHFFFAOYSA-M tetramethylazanium;periodate Chemical compound C[N+](C)(C)C.[O-]I(=O)(=O)=O HLQAWDQQEJSALG-UHFFFAOYSA-M 0.000 description 1
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 description 1
- 239000001393 triammonium citrate Substances 0.000 description 1
- 235000011046 triammonium citrate Nutrition 0.000 description 1
- XKWFRVVFRZYIFP-UHFFFAOYSA-N triazanium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound N.N.N.OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O XKWFRVVFRZYIFP-UHFFFAOYSA-N 0.000 description 1
- LDGFRUUNCRYSQK-UHFFFAOYSA-N triazin-4-ylmethanediamine Chemical compound NC(N)C1=CC=NN=N1 LDGFRUUNCRYSQK-UHFFFAOYSA-N 0.000 description 1
- MPSUGQWRVNRJEE-UHFFFAOYSA-N triazol-1-amine Chemical compound NN1C=CN=N1 MPSUGQWRVNRJEE-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
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/722—Ethers of polyoxyalkylene glycols having mixed oxyalkylene groups; Polyalkoxylated fatty alcohols or polyalkoxylated alkylaryl alcohols with mixed oxyalkylele groups
-
- 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2082—Polycarboxylic 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
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy 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
- 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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- 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
- 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
- C11D3/34—Organic compounds containing sulfur
- C11D3/3427—Organic compounds containing sulfur containing thiol, mercapto or sulfide groups, e.g. thioethers or mercaptales
-
- 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
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38654—Preparations containing enzymes, e.g. protease or amylase containing oxidase or reductase
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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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- C11D3/3942—Inorganic per-compounds
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Abstract
本发明公开了一种用于选择性移除硬遮罩的清洗液、其制备方法及应用,所述的清洗液由下述原料制得,所述的原料包括以下质量分数的组分:10%‑50%的氧化剂、0‑1%的D‑氨基酸氧化酶、0‑2%的D型氨基酸、0.1%‑10%的有机碱、0.001%‑10%的螯合剂、0.005%‑10%的缓蚀剂、0.05%‑10%的羧酸铵、0.005%‑1.2%的EO‑PO聚合物L42、0.005%‑2%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。本发明清洗液对多种金属及电介质缓蚀性强,清洗效果佳;并且本发明的清洗液可回收并可多次循环使用,最大使用次数可达10次,大大降低了芯片制造的成本。
Description
技术领域
本发明涉及一种用于选择性移除硬遮罩的清洗液、其制备方法及应用。
背景技术
在芯片制造技术中,铜互联等离子刻蚀后残余物清洗液以含氟清洗液为主。随着技术节点的不断前进,越来越多的材料被引入,如钛、钨、氮化钛等金属材料,以及低k介质材料等,进而对传统的含氟清洗液与多种材料的兼容性形成挑战。
等离子干蚀刻常用于在铜(Cu)/低介电常数双镶嵌制造工艺中制造垂直侧壁沟槽和各向异性互连通路。随着技术节点发展至45nm及更小(比如28-14nm),半导体设备尺寸的缩小使得达到通路与沟槽的精准轮廓控制更具挑战性。集成电路设备公司正在研究利用各种硬遮罩来改善对低介电常数材料的蚀刻选择性,从而获得更佳的轮廓控制。硬遮罩材料(例如Ti/TiN)在发挥蚀刻保护作用后需移除,在移除硬遮罩材料的清洗工艺中,需对其他金属及介电材料进行保护,因此对传统的含氟清洗液与多种材料的兼容性形成挑战。
开发兼容性强的选择性移除硬遮罩的清洗液成为本领域亟待解决的一个问题。
发明内容
本发明要解决的技术问题在于克服现有的用于移除硬遮罩材料的清洗液对其他金属及介电材料的兼容性和缓蚀性能差,清洗效果不佳等缺陷,而提供了一种用于选择性移除硬遮罩的清洗液、其制备方法及应用。本发明清洗液可用于从集成电路(IC)湿制程清洗工艺中选择性移除硬遮罩和其它残留物,更具体地可用于从包含低介电常数介电材料、TEOS、铜、钴、和其它低介电常数介电材料的此类芯片或晶圆上选择性移除TiN、TaN、TiNxOy、Ti硬遮罩、和包含上述物质的合金的硬遮罩、以及其它残留物。本发明清洗液清洗效果佳,可多次循环使用。
本发明通过以下技术方案来解决上述技术问题。
本发明提供了一种清洗液,其由下述原料制得,所述的原料包括以下质量分数的组分:
10%-50%的氧化剂、0-1%的D-氨基酸氧化酶、0-2%的D型氨基酸、0.1%-10%的有机碱、0.001%-10%的螯合剂、0.005%-10%的缓蚀剂、0.05%-10%的羧酸铵、0.005%-1.2%的EO-PO聚合物L42、0.005%-2%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
所述的清洗液中,所述的氧化剂可为本领域常规使用的氧化剂,例如过氧化氢(H2O2)、n-甲基吗啉氧化物(NMMO或NMO)、过氧化苯甲酰、过氧单硫酸四丁铵、臭氧、氯化铁、高锰酸盐、过硼酸盐、高氯酸盐、过硫酸盐、过氧二硫酸铵、过乙酸、过氧化脲、硝酸(HNO3)、亚氯酸铵(NH4ClO2)、氯酸铵(NH4ClO3)、碘酸铵(NH4IO3)、过硼酸铵(NH4BO3)、高氯酸铵(NH4ClO4)、高碘酸铵(NH4IO3)、过硫酸铵((NH4)2S2O8)、亚氯酸四甲铵((N(CH3)4)ClO2)、氯酸四甲铵((N(CH3)4)ClO3)、碘酸四甲铵((N(CH3)4)IO3)、过硼酸四甲铵((N(CH3)4)BO3)、高氯酸四甲铵((N(CH3)4)ClO4)、高碘酸四甲铵((N(CH3)4)IO4)、过硫酸四甲铵((N(CH3)4)S2O8)、过氧化脲((CO(NH2)2)H2O2)和过氧乙酸(CH3(CO)OOH)中的一种或多种,再例如为过氧化氢和/或过氧乙酸。
所述的清洗液中,所述的氧化剂的质量分数可为10%-40%,例如10%-30%(例如10%、15%、30%),所述的质量分数为所述的氧化剂的质量占原料的总质量的百分比。
所述的清洗液中,所述的D-氨基酸氧化酶的质量分数可为0-0.1%,例如0-0.01%(例如0、0.005%、0.01%),再例如0.005%-0.1%(例如0.005%、0.01%),所述的质量分数为所述的D-氨基酸氧化酶的质量占原料的总质量的百分比。
所述的清洗液中,所述的D型氨基酸可为本领域常规使用的D型氨基酸,例如D-甘氨酸、D-丙氨酸、D-缬氨酸、D-亮氨酸、D-异亮氨酸、D-苯丙氨酸、D-脯氨酸、D-色氨酸、D-丝氨酸、D-酪氨酸、D-半胱氨酸、D-蛋氨酸、D-天冬酰胺、D-谷氨酰胺、D-苏氨酸、D-天冬氨酸、D-谷氨酸、D-赖氨酸、D-精氨酸和D-组氨酸中的一种或多种,再例如D-脯氨酸、D-精氨酸和D-组氨酸中的一种或多种。
所述的清洗液中,所述的D型氨基酸的质量分数可为0-1%,例如0-0.5%(例如0、0.25%、0.5%),再例如0.1%-1%(例如0.25%、0.5%),所述的质量分数为所述的D型氨基酸的质量占原料的总质量的百分比。
所述的清洗液中,所述的有机碱可为本领域常规使用的有机碱,例如四甲基氢氧化铵、四丙基氢氧化铵、四丁基氢氧化铵、四乙基氢氧化铵(TEAH)、苄基三甲基氢氧化铵(BTAH)、胆碱、(2-羟基乙基)三甲基氢氧化铵、三(2-羟乙基)甲基氢氧化铵、单乙醇胺(MEA)、二甘醇胺(DGA)、三乙醇胺(TEA)、异丁醇胺、异丙醇胺、四丁基氢氧化鏻(TBPH)和四甲基胍中的一种或多种,再例如为四甲基氢氧化铵和/或胆碱。
所述的清洗液中,所述的有机碱的质量分数可为0.5%-8%,例如1%-5%(例如1%、2.5%、5%),所述的质量分数为所述的有机碱的质量占原料的总质量的百分比。
所述的清洗液中,所述的螯合剂可为本领域常规使用的螯合剂,例如1,2-环己二胺-N,N,N',N'-四乙酸(CDTA)、乙二胺四乙酸、次氮基三乙酸、二亚乙基三胺五乙酸、1,4,7,10-四氮杂环十二烷-1,4,7,10-四乙酸、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、N-{2-[双(羧甲基)氨基]乙基}-N-(2-羟乙基)甘氨酸(HEDTA)、乙二胺-N,N'-双(2-羟基苯乙酸)(EDDHA)、二氧杂八亚甲基二氮基四乙酸(DOCTA)和三亚乙基四胺六乙酸(TTHA)中的一种或多种,再例如乙二胺四乙酸和/或1,2-环己二胺-N,N,N',N'-四乙酸。
所述的清洗液中,所述的螯合剂的质量分数可为0.01%-5%,例如0.01%-2%(例如0.01%、1%、2%),所述的质量分数为所述的螯合剂的质量占原料的总质量的百分比。
所述的清洗液中,所述的缓蚀剂可为本领域常规使用的缓蚀剂,例如苯并三唑(BTA)、甲苯三唑、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、羟苯并三唑、2-(5-氨基-戊基)-苯并三唑、1-氨基-1,2,3-三唑、1-氨基-5-甲基-1,2,3-三唑、3-氨基-1,2,4-三唑、3-巯基-1,2,4-三唑、3-异丙基-1,2,4-三唑、5-苯硫醇-苯并三唑、卤代-苯并三唑(卤素为F、Cl、Br或I)、萘并三唑、2-巯基苯并咪唑(MBI)、2-巯基苯并噻唑、4-甲基-2-苯基咪唑、2-巯基噻唑啉、5-氨基四唑、5-氨基四唑一水合物、5-氨基-1,3,4-噻二唑-2-硫醇、2,4-二氨基-6-甲基-1,3,5-三嗪、噻唑、三嗪、甲基四唑、1,3-二甲基-2-咪唑啉酮、1,5-五亚甲基四唑、1-苯基-5-巯基四唑、二氨基甲基三嗪、咪唑啉硫酮、巯基苯并咪唑、4-甲基-4H-1,2,4-三唑-3-硫醇、5-氨基-1,3,4-噻二唑-2-硫醇和苯并噻唑中的一种或多种,再例如苯并三唑和/或甲苯三唑。
所述的清洗液中,所述的缓蚀剂的质量分数可为0.01%-5%,例如0.01%-2%(例如0.01%、0.5%、2%),所述的质量分数为所述的缓蚀剂的质量占原料的总质量的百分比。
所述的清洗液中,所述的羧酸铵可为本领域常规使用的羧酸铵,例如草酸铵、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、乙二胺四乙酸铵、乙二胺四乙酸二铵、乙二胺四乙酸三铵、乙二胺四乙酸四铵、琥珀酸铵、甲酸铵和1-H-吡唑-3-甲酸铵中的一种或多种,再例如草酸铵和/或柠檬酸三铵。
所述的清洗液中,所述的羧酸铵的质量分数可为0.1%-5%,例如0.5%-3%(例如0.5%、1%、3%),所述的质量分数为所述的羧酸铵的质量占原料的总质量的百分比。
所述的清洗液中,所述的EO-PO聚合物L42的质量分数可为0.005%-1%,例如0.01%-1%(例如0.01%、0.05%、1%),所述的质量分数为所述的EO-PO聚合物L42的质量占原料的总质量的百分比。
本发明中,所述的EO-PO聚合物为聚氧乙烯聚氧丙烯嵌段聚合物。
所述的清洗液中,所述的钝化剂可为本领域常规使用的钝化剂,例如2-((1H-苯并[d][1,2,3]三唑-1-基)甲基)-5-(2-硝基苄基巯基)-1,3,4-恶二唑,所述的2-((1H-苯并[d][1,2,3]三唑-1-基)甲基)-5-(2-硝基苄基巯基)-1,3,4-恶二唑的制备方法为本领域常规。
所述的清洗液中,所述的钝化剂的质量分数可为0.005%-1.5%,例如0.01%-1%(例如0.01%、0.7%、1%),所述的质量分数为所述的钝化剂的质量占原料的总质量的百分比。
所述的清洗液中,所述的水可为去离子水、纯水和超纯水中的一种或多种,优选离子水。
在本发明某些优选实施方案中,所述的清洗液由下述原料制得,所述的原料包括以下质量分数的组分:10%-40%的氧化剂、0-0.1%的D-氨基酸氧化酶、0-1%的D型氨基酸、0.5%-8%的有机碱、0.01%-5%的螯合剂、0.01%-5%的缓蚀剂、0.1%-5%的羧酸铵、0.005%-1%的EO-PO聚合物L42、0.005%-1.5%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
在本发明某些优选实施方案中,所述的清洗液由下述原料制得,所述的原料包括以下质量分数的组分:10%-30%的氧化剂、0-0.01%的D-氨基酸氧化酶、0-0.5%的D型氨基酸、1%-5%的有机碱、0.01%-2%的螯合剂、0.01%-2%的缓蚀剂、0.5%-3%的羧酸铵、0.01%-1%的EO-PO聚合物L42、0.01%-1%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
在本发明某些优选实施方案中,所述的清洗液由下述原料制得,所述的原料包括以下质量分数的组分:10%-30%的氧化剂、0.005%-0.1%(例如0.005%-0.01%)的D-氨基酸氧化酶、0.1-1%(例如0.25%-0.5%)的D型氨基酸、1%-5%的有机碱、0.01%-2%的螯合剂、0.01%-2%的缓蚀剂、0.5%-3%的羧酸铵、0.01%-1%的EO-PO聚合物L42、0.01%-1%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
在本发明某些优选实施方案中,所述的清洗液由下述原料制得,所述的原料由以下质量分数的组分组成:10%-40%的氧化剂、0-0.1%的D-氨基酸氧化酶、0-1%的D型氨基酸、0.5%-8%的有机碱、0.01%-5%的螯合剂、0.01%-5%的缓蚀剂、0.1%-5%的羧酸铵、0.005%-1%的EO-PO聚合物L42、0.005%-1.5%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
在本发明某些优选实施方案中,所述的清洗液由下述原料制得,所述的原料由以下质量分数的组分组成:10%-30%的氧化剂、0-0.01%的D-氨基酸氧化酶、0-0.5%的D型氨基酸、1%-5%的有机碱、0.01%-2%的螯合剂、0.01%-2%的缓蚀剂、0.5%-3%的羧酸铵、0.01%-1%的EO-PO聚合物L42、0.01%-1%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
在本发明某些优选实施方案中,所述的清洗液由下述原料制得,所述的原料由以下质量分数的组分组成:10%-30%的氧化剂、0.005%-0.1%(例如0.005%-0.01%)的D-氨基酸氧化酶、0.1-1%(例如0.25%-0.5%)的D型氨基酸、1%-5%的有机碱、0.01%-2%的螯合剂、0.01%-2%的缓蚀剂、0.5%-3%的羧酸铵、0.01%-1%的EO-PO聚合物L42、0.01%-1%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比。
本发明还提供了一种上述的清洗液的制备方法,其包括以下步骤:将所述的原料混合,得到清洗液即可。
其中,所述的混合优选将所述的原料组分中的固体组分加入到液体组分中,搅拌均匀,即可。
其中,所述的混合的温度可为室温。
本发明还提供了一种上述的清洗液在半导体器件的清洗工艺中的应用。
其中,所述的半导体器件经等离子刻蚀,所述的半导体器件例如含有硬遮罩材料,所述硬遮罩材料可为氮化钛(TiN)、氮化钽(TaN)、氮氧化钛(TiNxOy)和钛(Ti)中的一种或多种。
其中,所述的清洗工艺中清洗的温度可为本领域常规使用的温度,例如40℃-60℃(例如45℃)。所述的清洗工艺中清洗的时间可为5min-30min(例如20min)。
本发明中,如无特殊说明,“室温”是指10-40℃。
在不违背本领域常识的基础上,上述各优选条件,可任意组合,即得本发明各较佳实例。
本发明所用试剂和原料均市售可得。
本发明的积极进步效果在于:本发明清洗液对多种金属及电介质缓蚀性强,清洗效果佳;并且本发明的清洗液可回收并可多次循环使用,最大使用次数可达10次,大大降低了芯片制造的成本。
具体实施方式
下面通过实施例的方式进一步说明本发明,但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法,按照常规方法和条件,或按照商品说明书选择。
实施例中涉及的缩写如下:
TMAH:四甲基氢氧化铵;
BTA:苯并三唑;
CDTA:1,2-环己二胺-N,N,N',N'-四乙酸;
E:2-((1H-苯并[d][1,2,3]三唑-1-基)甲基)-5-(2-硝基苄基巯基)-1,3,4-恶二唑;
AlNxOy:氮氧化铝;
W:钨;
Cu:铜;
LP-TEOS:低压沉积正硅酸乙脂;
BD2:本领域常用的低k介电材料,商品名为BLACK DIAMOND(BD2);
SiCN:硅碳氮;
Co:钴;
Ti:钛;
TiN:氮化钛,本发明所述的TiN为PVD TiN,其中PVD指(Physical VaporDeposition)物理气相沉积;
TaN:氮化钽;
TiNxOy:氮氧化钛。
实施例中的EO-PO产品均购自南通锦莱化工有限公司。
实施例中的D-氨基酸氧化酶均购自上海阿拉丁生化科技股份有限公司。
实施例中的2-((1H-苯并[d][1,2,3]三唑-1-基)甲基)-5-(2-硝基苄基巯基)-1,3,4-恶二唑的制备方法参照CN103848826A中实施例五,在以下实施例中用E表示。
实施例1-12
将清洗液的原料组分:氧化剂、D-氨基酸氧化酶、D型氨基酸、有机碱、螯合剂、缓蚀剂、羧酸铵、EO-PO聚合物L42、钝化剂的种类和含量列于表1中,用水补足余量,清洗液中的水为去离子水。
下述实施例中,清洗液的制备方法均为将实施例中原料组分中的固体组分加入到液体组分中,搅拌均匀。
下述实施例中,未限定具体操作温度的,均是指在室温条件下进行。
表1清洗液的各原料组分的种类和质量分数
应用实施例1
(1)刻蚀速率测定
刻蚀速率待检测样品:硅晶片上沉积了单一材料的dummy片子(假片),如铝、铜、氮化钛、钨、钴、介电材料(低k或高k)等。
刻蚀实验:将待检测样品在45℃下在清洗液中静态浸渍30min,然后去离子水清洗后氮气吹干。
测量蚀刻速率(A/min)的方法:分别检测样品在刻蚀前后的厚度,其中金属样品采用四点探针仪器(日本Napson的CRESTEST-e)测试厚度,非金属样品采用光学膜厚测量仪(美国Filmetrics F20)测试厚度。
刻蚀效果分四个等级:A-相容性佳,无底切;B-有极轻微底切;C-有少量底切;D-底切较为明显和严重。
(2)清洗效果测定
清洗效果待检测样品:具有图形特征(金属线metal、孔via、金属垫pad或沟槽trench等)的具有等离子刻蚀后残余物和灰化后残余物的图案化晶片。
清洗效果实验方法:将样品在45℃下在清洗液中静态浸渍20min,然后去离子水清洗后氮气吹干。用电子显微镜SEM观测清洗和腐蚀效果。
清洗效果分四个等级:A-观察不到残留物;B-观察到极少量残留物;C-观察到少量残留物;D-观察到有明显较多残留物。
实施例1-12和对比例1-10的清洗液的刻蚀速率如表2所示,刻蚀效果和清洗效果如表3所示。
表2
表3
从表2、3可以看出,本发明的清洗液对AlNxOy、W、Cu、LP-TEOS、BD2、SiCN、Co、Ti、TiN、TaN、TiNxOy等均具有较低的刻蚀速率,说明其缓蚀性能较佳;且用本发明的清洗液清洗具有通孔特征的图案化晶片和具有金属线特征的图案化晶片后,几乎未观察到底切现象,说明其对多种金属及电介质具有很好的兼容性。另外,用本发明的清洗液清洗具有通孔特征的图案化晶片和具有金属线特征的图案化晶片后,几乎观察不到残留物,说明清洗效果佳。
相较于实施例1-12,对比例1-10的清洗液或者对AlNxOy、W、Cu、LP-TEOS、BD2、SiCN和Co等的刻蚀速率明显增高,其缓蚀性能差,或者对Ti、TiN、TaN和TiNxOy等刻蚀速率明显降低,无法有效移除硬遮罩材料。由此可见,对比例1-10的清洗液无法实现选择性移除硬遮罩材料,对其他金属及介电材料的兼容性差。并且,用对比例1-10的清洗液清洗具有通孔特征的图案化晶片和具有金属线特征的图案化晶片后,出现了较为严重的底切现象,有较多的残留物。
应用实施例2
以实施例1和4的清洗液为例进行回收并循环使用,对回收后循环使用的清洗液进行上述的刻蚀实验和清洗效果实验,测试方法同应用实施例1,结果如表4和表5所示。
表4
表5
由上述结果可知,本发明清洗液可回收并可多次循环使用,最大使用次数可达10次,大大降低了芯片制造的成本。
Claims (5)
1.一种清洗液,其特征在于,由下述原料制得,所述的原料包括以下质量分数的组分:
10%-30%的氧化剂、0-0.01%的D-氨基酸氧化酶、0-0.5%的D型氨基酸、1%-5%的有机碱、0.01%-2%的螯合剂、0.01%-2%的缓蚀剂、0.5%-3%的羧酸铵、0.01%-1%的EO-PO聚合物L42、0.01%-1%的钝化剂和余量的水,所述的质量分数为各组分质量占各组分总质量的百分比;
其中,所述的氧化剂为过氧化氢和/或过氧乙酸;
所述的D型氨基酸为D-脯氨酸、D-精氨酸和D-组氨酸中的一种或多种;
所述的螯合剂为乙二胺四乙酸和/或1,2-环己二胺-N,N,N',N'-四乙酸;
所述的缓蚀剂为苯并三唑和/或甲苯三唑;
所述的羧酸铵为草酸铵和/或柠檬酸三铵;
所述的水为离子水;
所述的钝化剂为2-((1H-苯并[d][1,2,3]三唑-1-基)甲基)-5-(2-硝基苄基巯基)-1,3,4-恶二唑。
2.如权利要求1所述的清洗液,其特征在于,所述的D-氨基酸氧化酶的质量分数为0.005%-0.01%;
和/或,所述的D型氨基酸的质量分数为0.25%-0.5%。
3.一种如权利要求1或2所述的清洗液的制备方法,其特征在于,包括以下步骤:将所述的原料混合,得到清洗液即可。
4.一种如权利要求1或2所述的清洗液在半导体器件的清洗工艺中的应用。
5.如权利要求4所述的清洗液在半导体器件的清洗工艺中的应用,其特征在于,所述的半导体器件经等离子刻蚀;
和/或,所述的半导体器件含有硬遮罩材料,所述硬遮罩材料为氮化钛、氮化钽、氮氧化钛和钛中的一种或多种;
和/或,所述的清洗工艺中清洗的温度为40℃-60℃;
和/或,所述的清洗工艺中清洗的时间为5min-30min。
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