KR102000726B1 - Liquid composition for cleaning/removing copper-containing adhering matter from surface of oxide comprising indium, gallium, zinc, and oxygen (igzo), method for cleaning igzo surface using said liquid composition, and substrate cleaned using said method for cleaning - Google Patents
Liquid composition for cleaning/removing copper-containing adhering matter from surface of oxide comprising indium, gallium, zinc, and oxygen (igzo), method for cleaning igzo surface using said liquid composition, and substrate cleaned using said method for cleaning Download PDFInfo
- Publication number
- KR102000726B1 KR102000726B1 KR1020157023345A KR20157023345A KR102000726B1 KR 102000726 B1 KR102000726 B1 KR 102000726B1 KR 1020157023345 A KR1020157023345 A KR 1020157023345A KR 20157023345 A KR20157023345 A KR 20157023345A KR 102000726 B1 KR102000726 B1 KR 102000726B1
- Authority
- KR
- South Korea
- Prior art keywords
- igzo
- copper
- cleaning
- liquid composition
- molybdenum
- Prior art date
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- 229910052802 copper Inorganic materials 0.000 title claims abstract description 151
- 239000010949 copper Substances 0.000 title claims abstract description 151
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 239000000203 mixture Substances 0.000 title claims abstract description 108
- 239000007788 liquid Substances 0.000 title claims abstract description 106
- 239000000758 substrate Substances 0.000 title claims abstract description 81
- 238000004140 cleaning Methods 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 43
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 15
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 15
- 239000011701 zinc Substances 0.000 title claims abstract description 15
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052738 indium Inorganic materials 0.000 title claims abstract description 13
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 13
- 239000001301 oxygen Substances 0.000 title claims abstract description 13
- 239000004065 semiconductor Substances 0.000 claims abstract description 56
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 25
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 14
- 229910052750 molybdenum Inorganic materials 0.000 claims description 83
- 239000011733 molybdenum Substances 0.000 claims description 83
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 77
- 238000005530 etching Methods 0.000 claims description 49
- 239000010410 layer Substances 0.000 claims description 45
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 43
- 235000015165 citric acid Nutrition 0.000 claims description 17
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 10
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 claims description 8
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 8
- 239000003002 pH adjusting agent Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 5
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 5
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 4
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000004310 lactic acid Substances 0.000 claims description 4
- 235000014655 lactic acid Nutrition 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- 239000001384 succinic acid Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 description 38
- 238000011282 treatment Methods 0.000 description 32
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 22
- 239000010408 film Substances 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 239000007864 aqueous solution Substances 0.000 description 19
- 229910052751 metal Inorganic materials 0.000 description 17
- 239000002184 metal Substances 0.000 description 17
- -1 molybdenum ions Chemical class 0.000 description 17
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 13
- 229910001431 copper ion Inorganic materials 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 12
- 238000005260 corrosion Methods 0.000 description 11
- 230000007797 corrosion Effects 0.000 description 11
- 238000011109 contamination Methods 0.000 description 10
- 238000007654 immersion Methods 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 229910000365 copper sulfate Inorganic materials 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- 239000013626 chemical specie Substances 0.000 description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910001385 heavy metal Inorganic materials 0.000 description 5
- 239000008139 complexing agent Substances 0.000 description 4
- 150000001991 dicarboxylic acids Chemical class 0.000 description 4
- 229910021645 metal ion Inorganic materials 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 3
- 229920001155 polypropylene Polymers 0.000 description 3
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 2
- 239000011609 ammonium molybdate Substances 0.000 description 2
- 235000018660 ammonium molybdate Nutrition 0.000 description 2
- 229940010552 ammonium molybdate Drugs 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910000000 metal hydroxide Inorganic materials 0.000 description 2
- 150000004692 metal hydroxides Chemical class 0.000 description 2
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 159000000001 potassium salts Chemical class 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical class C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 229910001887 tin oxide Inorganic materials 0.000 description 2
- 238000001039 wet etching Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- ULRPISSMEBPJLN-UHFFFAOYSA-N 2h-tetrazol-5-amine Chemical compound NC1=NN=NN1 ULRPISSMEBPJLN-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- XFTRTWQBIOMVPK-YFKPBYRVSA-N Citramalic acid Natural products OC(=O)[C@](O)(C)CC(O)=O XFTRTWQBIOMVPK-YFKPBYRVSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- ODBLHEXUDAPZAU-ZAFYKAAXSA-N D-threo-isocitric acid Chemical compound OC(=O)[C@H](O)[C@@H](C(O)=O)CC(O)=O ODBLHEXUDAPZAU-ZAFYKAAXSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- DSLZVSRJTYRBFB-UHFFFAOYSA-N Galactaric acid Natural products OC(=O)C(O)C(O)C(O)C(O)C(O)=O DSLZVSRJTYRBFB-UHFFFAOYSA-N 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- ODBLHEXUDAPZAU-FONMRSAGSA-N Isocitric acid Natural products OC(=O)[C@@H](O)[C@H](C(O)=O)CC(O)=O ODBLHEXUDAPZAU-FONMRSAGSA-N 0.000 description 1
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001464 adherent effect Effects 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- IAJILQKETJEXLJ-QTBDOELSSA-N aldehydo-D-glucuronic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-QTBDOELSSA-N 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- BYBVAYUUISIXJJ-UHFFFAOYSA-N azane;hexahydrate Chemical compound N.O.O.O.O.O.O BYBVAYUUISIXJJ-UHFFFAOYSA-N 0.000 description 1
- REROKLPNVNAPBD-UHFFFAOYSA-N azane;tetrahydrate Chemical compound N.O.O.O.O REROKLPNVNAPBD-UHFFFAOYSA-N 0.000 description 1
- 150000003851 azoles Chemical class 0.000 description 1
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
- 239000012964 benzotriazole Substances 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 150000001244 carboxylic acid anhydrides Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- XFTRTWQBIOMVPK-UHFFFAOYSA-N citramalic acid Chemical compound OC(=O)C(O)(C)CC(O)=O XFTRTWQBIOMVPK-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- QSAWQNUELGIYBC-UHFFFAOYSA-N cyclohexane-1,2-dicarboxylic acid Chemical compound OC(=O)C1CCCCC1C(O)=O QSAWQNUELGIYBC-UHFFFAOYSA-N 0.000 description 1
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 description 1
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 description 1
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001312 dry etching Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LMJKLTNTDHKUGO-UHFFFAOYSA-N ethane-1,2-diol;2-(2-hydroxypropoxy)propan-1-ol Chemical compound OCCO.CC(O)COC(C)CO LMJKLTNTDHKUGO-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- DSLZVSRJTYRBFB-DUHBMQHGSA-N galactaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)C(O)=O DSLZVSRJTYRBFB-DUHBMQHGSA-N 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229940097043 glucuronic acid Drugs 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000002443 hydroxylamines Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-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
- ODBLHEXUDAPZAU-UHFFFAOYSA-N threo-D-isocitric acid Natural products OC(=O)C(O)C(C(O)=O)CC(O)=O ODBLHEXUDAPZAU-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- TYHJXGDMRRJCRY-UHFFFAOYSA-N zinc indium(3+) oxygen(2-) tin(4+) Chemical compound [O-2].[Zn+2].[Sn+4].[In+3] TYHJXGDMRRJCRY-UHFFFAOYSA-N 0.000 description 1
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
- C11D7/265—Carboxylic acids or salts thereof
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/06—Hydroxides
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/26—Organic compounds containing oxygen
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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
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/22—Organic compounds
- C11D7/32—Organic compounds containing nitrogen
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- 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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02071—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a delineation, e.g. RIE, of conductive layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/66007—Multistep manufacturing processes
- H01L29/66969—Multistep manufacturing processes of devices having semiconductor bodies not comprising group 14 or group 13/15 materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/66—Types of semiconductor device ; Multistep manufacturing processes therefor
- H01L29/68—Types of semiconductor device ; Multistep manufacturing processes therefor controllable by only the electric current supplied, or only the electric potential applied, to an electrode which does not carry the current to be rectified, amplified or switched
- H01L29/76—Unipolar devices, e.g. field effect transistors
- H01L29/772—Field effect transistors
- H01L29/78—Field effect transistors with field effect produced by an insulated gate
- H01L29/786—Thin film transistors, i.e. transistors with a channel being at least partly a thin film
- H01L29/7869—Thin film transistors, i.e. transistors with a channel being at least partly a thin film having a semiconductor body comprising an oxide semiconductor material, e.g. zinc oxide, copper aluminium oxide, cadmium stannate
Abstract
The present invention relates to a liquid composition for cleaning and removing deposits including copper from the surface of an oxide (IGZO) made of indium, gallium, zinc, and oxygen without corroding wirings containing the IGZO semiconductor layer or copper, A method of cleaning an IGZO surface using the liquid composition, and a substrate to be cleaned by the cleaning method. In the present invention, a liquid composition containing at least one member selected from the group consisting of hydroxycarboxylic acid and dicarboxylic acid or a salt thereof and having a pH value of 1.5 to 10 is used.
Description
The present invention relates to a liquid composition, and more particularly to a liquid composition for cleaning and removing deposits containing copper from the surface of IGZO without corrosion of the wiring including the IGZO semiconductor layer or copper, A cleaning method, and a substrate that is cleaned by the cleaning method.
In a liquid crystal display device, a method using a thin film transistor (TFT: Thin Film Transistor) in a display region constituting a pixel is employed in many electronic material parts applications including television. In this TFT structure, amorphous silicon is generally used for the semiconductor layer, and aluminum or an aluminum alloy is used for the wiring material. However, with the increase in the size and resolution of the display, such a material tends to cause a problem of signal delay due to the characteristics of field effect mobility and wiring resistance and to make it difficult to display a uniform screen.
Accordingly, in recent years, various oxide semiconductor materials have been developed as semiconductor layers. The oxide semiconductor material includes indium-gallium-zinc oxide (IGZO), indium-gallium oxide (IGO), indium-tin-zinc oxide (ITZO), indium-gallium The use of various compositions such as zinc · tin oxide (IGZTO), gallium · zinc oxide (GZO), and zinc · tin oxide (ZTO) has been studied. Recently, particularly IGZO has been actively studied.
Further, as the wiring material, a structure in which copper or copper alloy, which is a material having a lower electric resistance, is used as a wiring material from aluminum or an aluminum alloy has been studied. However, copper has a low resistance. On the other hand, when it is used in a gate wiring, in addition to the problem that adhesiveness to a substrate such as glass is not sufficient, copper is used as a source And diffusion of copper metal into the layer may occur. In order to prevent this, a lamination of a barrier film having high adhesion to a substrate such as glass, difficulty of diffusion to a semiconductor layer, and the like, in which a metal having both barrier properties is disposed, has been studied, and molybdenum or molybdenum alloy It is getting attention.
The multilayer wiring including these copper wirings is obtained by forming on a substrate by using a known film forming technique such as a sputtering method and then etching it with a resist or the like as a mask to form an electrode pattern. The etching method includes a wet method (wet etching) using an etching solution and a dry method (dry etching) using an etching gas such as plasma. Regarding wet etching of multi-layered wiring including copper, for example, Patent Document 1 discloses an etching solution for etching copper / molybdenum containing at least one selected from a neutral salt, an inorganic acid and an organic acid, and hydrogen peroxide.
Also, Patent Document 2 is introduced as a copper / molybdenum etchant which does not corrode IGZO.
Fig. 1 is a schematic view of a cross section of a substrate having a TFT structure having IGZO as a semiconductor layer and wiring including copper. The etching solution of copper is in contact with the IGZO semiconductor layer during etching of a film containing copper or a film containing copper and molybdenum, and metals such as copper, molybdenum and the like are dissolved in the etching solution. Accordingly, there is a possibility that the surface of the IGZO is contaminated with deposits including transition metal elements such as copper and molybdenum in the etching solution. As used herein, the term " attachment " means a chemical species attached to the IGZO surface and present in the form of a metal oxide, metal hydroxide, metal salt, metal ion, That is, chemical species in the state of metal are not included in the adherence referred to herein. It is also pointed out that the metal element on the surface of the IGZO may be defected, and contamination may be caused by injecting a chemical species containing a transition metal element dissolved in the etching solution into the defective portion. The chemical species introduced into the IGZO surface in this way are also included in the " attachment " In general, when a chemical species containing a transition metal element adheres to a semiconductor surface, it is known that semiconductor characteristics such as electrical resistance and durability are adversely affected. On the other hand, the present inventors have confirmed that when the adherence of copper ions or molybdenum ions is adhered to the IGZO surface, the semiconductor characteristics are degraded.
Patent Document 3 discloses a liquid composition for cleaning and removing deposits containing copper on the surface of a Si semiconductor. In Patent Document 3, a liquid composition containing citric acid and hydrogen peroxide and having a pH value adjusted to 3 to 4, It is possible to clean heavy metal contamination.
Patent Document 4 discloses a cleaning liquid containing an organic acid having at least one carboxyl group and a complexing agent capable of removing metal contamination (Al, Fe, Cu) on the surface of a Si semiconductor substrate without causing corrosion of the metal wiring .
In Patent Document 5, there is a report that IGZO is etched by a liquid composition containing any one of acetic acid, citric acid, hydrochloric acid, and perchloric acid.
However, Patent Document 1 does not mention the corrosiveness of IGZO. Further, there is no disclosure on cleaning property of heavy metal contamination.
Patent Document 2 discloses that IGZO is not corroded, but there is no mention of heavy metal contamination of IGZO by copper or molybdenum dissolved in an etching solution.
Patent Document 3 does not describe the corrosion (etching rate) of the wiring including the IGZO semiconductor layer or copper. In addition, although it is described that the cleaning effect of metal contamination such as copper is improved by including hydrogen peroxide, hydrogen peroxide can not be used when a metal which is corroded by hydrogen peroxide is used for wiring (for example, When a metal such as copper or molybdenum is used for wiring, a liquid composition containing hydrogen peroxide, hydrogen peroxide and an acid is cleaned on the surface of the IGZO, and the liquid composition containing hydrogen peroxide and hydrogen peroxide (See Comparative Example 9). Further, when the chemical species containing copper in the etching liquid adheres to the surface of the IGZO, it is considered that the chemical state is different from the heavy metal contamination such as copper adhering to the surface of the Si semiconductor wafer. In addition, Although it is possible to remove the contamination, there is a possibility that all the deposits including copper adhered on the IGZO surface may not be removed. In addition, although it is possible to remove deposits including copper adhering to the surface of the IGZO semiconductor, it may not be possible to remove heavy metal contamination such as copper adhering to the surface of the Si semiconductor.
In Patent Document 4, there is no description about the corrosion resistance of the IGZO semiconductor layer. Further, although it is described that the effect of removing the metal contamination on the surface of the semiconductor substrate is improved by including the complexing agent, the IGZO may be corroded by the complexing agent (ammonium fluoride is exemplified) (see Comparative Example 10).
The liquid composition disclosed in Patent Document 5 aims at the etching of IGZO, and there is no disclosure of cleaning and removal properties of deposits including copper and molybdenum. In addition, the use of this liquid composition not only corrodes the IGZO semiconductor layer, but also has the possibility of corroding wiring including copper.
Under such circumstances, a cleaning liquid for the IGZO surface, which can clean and remove deposits containing copper or copper and molybdenum from the IGZO surface without requiring corrosion of the wiring including the IGZO semiconductor layer and copper or copper and molybdenum .
SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a liquid composition that cleans and removes copper, copper, and molybdenum-containing deposits from the surface of an IGZO without causing corrosion of the IGZO semiconductor layer or the wiring containing copper or copper and molybdenum, And a substrate that has been cleaned by the cleaning method.
As a result of intensive studies to solve the above problems, the present inventors have found that a liquid having a pH value controlled to 1.5 to 10 and containing any one selected from the group consisting of a specific hydroxyl carboxylic acid and dicarboxylic acid, It has been found that the above problems and problems in the composition can be solved.
That is, the present invention is as follows.
1. A liquid composition for cleaning and removing deposits containing copper from the surface of an oxide (IGZO) made of indium, gallium, zinc, and oxygen, without corroding wirings containing copper,
At least one selected from the group consisting of hydroxycarboxylic acid and dicarboxylic acid, or a salt thereof, and having a pH value of 1.5 to 10.
2. The liquid composition of claim 1, wherein the deposit comprising copper is a deposit comprising copper and molybdenum.
3. The liquid composition according to claim 1 or 2, wherein the hydroxycarboxylic acid is at least one selected from the group consisting of citric acid, tartaric acid, lactic acid, and glycolic acid.
4. The liquid composition according to any one of claims 1 to 3, wherein the dicarboxylic acid is at least one member selected from the group consisting of malonic acid, maleic acid, maleic anhydride, and succinic acid.
5. The liquid composition according to any one of claims 1 to 4, wherein the concentration of at least one member selected from the group consisting of hydroxycarboxylic acid and dicarboxylic acid or a salt thereof is 0.001 to 30 mass% .
6. The method according to item 1, wherein the pH adjusting agent is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, ammonia, tetramethylammonium hydroxide, 2-aminoethanol and 1-amino- The liquid composition according to any one of claims 1 to 5,
7. It is possible to clean and remove deposits containing copper from the surface of an oxide (IGZO) made of indium, gallium, zinc, and oxygen, without corroding the IGZO semiconductor layer and without corroding copper- A method of cleaning an IGZO surface comprising contacting a liquid composition according to any one of claims 1 to 6 to an IGZO surface on a substrate having a wiring comprising an IGZO semiconductor layer and copper.
8. From the surface of an oxide (IGZO) made of indium, gallium, zinc, and oxygen, it is possible to prevent the IGZO semiconductor layer from being corroded and the copper- Comprising contacting an IGZO semiconductor layer and an IGZO surface on a substrate having a wiring comprising copper and molybdenum with a liquid composition as claimed in any one of claims 1 to 6, Cleaning method of IGZO surface.
9. A substrate having an oxide (IGZO) semiconductor layer made of indium, gallium, zinc, and oxygen and a wiring comprising copper or copper and molybdenum, which has been cleaned by the method according to claim 7 or 8.
By using the liquid composition of the present invention, it is possible to clean and remove deposits including copper from the IGZO surface without corroding the wiring including the IGZO semiconductor layer and copper. Accordingly, it is possible to provide a liquid composition for surface cleaning of the IGZO semiconductor layer corresponding to a larger display, a higher resolution, and a lower power consumption.
1 is a schematic view of a substrate section having a TFT structure in which IGZO is a semiconductor layer and a film including copper is used as a wiring.
2 is an XPS spectrum of the IGZO surface after adhering copper ions.
Fig. 3 is an XPS spectrum of the IGZO surface after adhering copper ions and subsequently cleaning the IGZO surface with the liquid composition of Example 1. Fig.
<Liquid composition>
The liquid composition according to the present invention is a liquid composition for cleaning and removing deposits containing copper from the IGZO surface without corroding wirings containing the IGZO semiconductor layer or copper and the liquid composition comprising a hydroxycarboxylic acid and a dicar Or a salt thereof, and has a pH value of from 1.5 to 10.
In the present specification, the term " deposit including copper " refers to a metal compound such as an oxide, a hydroxide, or a salt of a metal containing at least copper, or an ion of a metal containing at least copper attached to the surface of the IGZO, Excludes metal objects. On the other hand, this " deposit containing copper " also includes chemical species including transition metal elements dissolved in the etching solution, which are taken into the defective portion of the IGZO surface.
In this specification, "no corrosion of the IGZO semiconductor layer" means that the etching rate of IGZO is less than 30 Å / min. In addition, "no corrosion of the wiring including copper" means that the etching rate of copper is less than 30 Å / min. In addition, "no corrosion of the wiring including copper and molybdenum" means that the etching rate of copper is less than 30 Å / min and the etching rate of molybdenum is less than 30 Å / min.
By using the liquid composition containing such a specific component, it is possible to clean and remove the deposit including copper from the IGZO surface without corroding the wiring including the IGZO semiconductor layer or copper. Further, according to a preferred embodiment of the present invention, the deposit including molybdenum may be washed and removed. It is also possible to simultaneously remove deposits containing copper and deposits containing molybdenum.
The liquid composition according to the present invention is used for cleaning the IGZO surface, and is capable of cleaning the IGZO semiconductor layer without causing the IGZO semiconductor layer to corrode and also preventing the copper- Can be removed. Further, according to a preferred aspect of the present invention, the liquid composition according to the present invention can remove at least the copper-containing deposit from the IGZO surface without corroding the IGZO semiconductor layer and without corroding the wiring containing molybdenum can do. Further, according to a preferred embodiment of the present invention, the liquid composition according to the present invention can prevent copper from escaping from the IGZO surface without corroding the single-layer film or multilayer wiring including copper and molybdenum, without corroding the IGZO semiconductor layer And the deposits including molybdenum can be cleaned and removed.
In a particularly preferred embodiment of the liquid composition according to the present invention, in a substrate having a TFT structure in which IGZO is a semiconductor layer and a single layer film containing copper or a multilayer film is a wiring, the IGZO semiconductor layer is not corroded, In addition, copper or an adherend containing copper and molybdenum can be cleaned and removed from the IGZO surface without corroding copper or a wiring including copper and molybdenum.
Hereinafter, each component constituting the liquid composition according to the present invention will be described in detail.
(A) Hydroxycarboxylic acid
The hydroxycarboxylic acid contained in the liquid composition according to the present invention has a function of forming a complex with the metal ion and cleaning and removing the deposit including copper from the IGZO surface. The hydroxycarboxylic acid is selected from the group consisting of hydroxycarboxylic acid and hydroxycarboxylic acid. The term " hydroxycarboxylic acid " as used herein refers to a compound containing at least one hydroxyl group and at least one carboxyl group in the molecule. Examples of the hydroxycarboxylic acid include citric acid, tartaric acid, lactic acid, glycolic acid, malic acid, citramalic acid, isocitric acid, glucuronic acid and galactaric acid. Of these, citric acid, tartaric acid, lactic acid and glycolic acid are particularly preferable. These hydroxycarboxylic acids may be used alone, or a plurality of hydroxycarboxylic acids may be used in combination. In addition, salts of these hydroxycarboxylic acids may be used, and examples thereof include sodium salts, potassium salts, ammonium salts and tetramethylammonium salts.
(B) Dicarboxylic acid
The dicarboxylic acid contained in the liquid composition according to the present invention has a function of forming a complex with the metal ion and cleaning and removing the deposit including copper from the IGZO surface. The dicarboxylic acid is selected from the group consisting of dicarboxylic acid, dicarboxylic acid salt, and carboxylic acid anhydride. The term "dicarboxylic acid" as used herein refers to a compound having two carboxyl groups in the molecule and not having a hydroxyl group. The dicarboxylic acid is preferably oxalic acid, malonic acid, maleic acid, maleic anhydride, glutaric acid, succinic acid, adipic acid, 1,2-cyclohexanedicarboxylic acid, phthalic acid and the like. These dicarboxylic acid compounds may be used alone, or a plurality of dicarboxylic acid compounds may be used in combination. Further, salts of these dicarboxylic acids may be used, and examples thereof include sodium salts, potassium salts, ammonium salts and tetramethylammonium salts.
The concentration of at least one member selected from the group consisting of hydroxycarboxylic acids or salts thereof (which may be simply referred to as component (A)), dicarboxylic acid or a salt thereof (simply referred to as component (B) More preferably 0.01 to 25% by mass, particularly preferably 0.02 to 20% by mass, and more preferably 0.1 to 10% by mass, in the liquid composition By mass, more preferably from 1 to 5% by mass.
(C) pH Modulator
The liquid composition according to the present invention may contain a pH adjusting agent (sometimes referred to simply as component (C)), if necessary. The pH adjusting agent has a role of adjusting the pH value of the liquid composition to a range of 1.5 to 10.
The pH adjusting agent (component (C)) is not particularly limited as long as it does not inhibit the effect of the liquid composition described above. Examples thereof include ammonia (NH 3 ); Metal hydroxides such as sodium hydroxide (NaOH) or potassium hydroxide (KOH); Amines such as isopropylamine, tert-butylamine, 2-aminoethanol and 1-amino-2-propanol; Hydroxyl amines such as hydroxylamine; And alkylammonium hydroxides such as tetramethylammonium hydroxide (TMAH), tetraethylammonium hydroxide and tetrapropylammonium hydroxide, and the like. These pH adjusting agents may be used alone, or a plurality of pH adjusting agents may be used in combination. Among these, ammonia, potassium hydroxide, tetramethylammonium hydroxide, 2-aminoethanol and 1-amino-2-propanol are preferable.
The liquid composition according to the present invention comprises at least one selected from the group consisting of (A) hydroxycarboxylic acid and (B) dicarboxylic acid, or a salt thereof, and has a pH value of 1.5 to 10 Range. By setting the pH value range of the liquid composition within the above-mentioned range, it is possible to clean and remove deposits including copper from the IGZO surface without corroding the wiring including the IGZO semiconductor layer and copper. If the pH value is less than 1.5, damage to the IGZO semiconductor layer or wiring tends to increase, which is not preferable. On the other hand, if the pH value exceeds 10, the ability to clean and remove the adhered material including copper tends to be lowered. The preferred range of pH values of the liquid composition is 1.5-10. A more preferable range of the pH value is 1.6 to 9.5, particularly preferably 1.7 to 9.2.
The content of the pH adjuster in the liquid composition according to the present invention is appropriately determined according to the content of the other components so that the pH value of the liquid composition becomes a desired value.
The liquid composition according to the present invention may contain various water-soluble organic solvents, such as water and other commonly used liquid compositions for cleaning, in addition to the components (A), (B) and (C) The additive may be included in an amount not to impair the effect of the liquid composition described above. For example, as the water, it is preferable that metal ions, organic impurities, particle particles, and the like are removed in advance by distillation, ion exchange treatment, filter treatment, various adsorption treatments, etc., and pure water is more preferable, (Ultrapure water) is preferable.
The water-soluble organic solvent is not particularly limited as long as it does not inhibit the effect of the liquid composition described above. Examples thereof include diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, dipropylene glycol Ethylene glycol such as monomethyl ether; Alcohols such as methanol, ethanol, 1-propanol, 2-propanol, 1-butanol and t-butanol; Ethylene glycol, propylene glycol, glycerin and the like can be used suitably.
The liquid composition according to the present invention may contain known additives as an anticorrosive agent for copper. For example, azole compounds such as benzotriazole, 5-amino-1H-tetrazole, imidazole, pyrazole, and phosphoric acid.
<Cleaning Method of IGZO Surface>
The cleaning method of the IGZO surface according to the present invention is a cleaning method for cleaning and removing deposits including copper without corroding the IGZO semiconductor layer or the wiring including copper from the IGZO surface, And a step of bringing the liquid composition into contact with the surface of the IGZO on the substrate having the wiring. According to the method of the present invention, deposits including copper can be cleaned and removed without corroding the IGZO semiconductor layer from the IGZO surface and without corroding the wiring including copper.
Further, a cleaning method according to the present invention is a method of forming an IGZO semiconductor layer on a substrate, and a substrate having copper or wiring including copper and molybdenum thereon, as an object to be cleaned.
The object to be cleaned is, for example, a substrate made of glass or the like, a layer made of IGZO, a layer made of molybdenum and a layer made of copper are successively laminated, a resist is coated thereon, a desired pattern mask is exposed and transferred, Thereby forming a resist pattern. And then selectively etching the multilayer wiring including copper and molybdenum by an etching solution.
There is no particular limitation on the method of bringing the liquid composition into contact with the object to be cleaned. For example, there are a method of immersing the object to be cleaned in the liquid composition, a method of contacting the object in accordance with a form such as dropping (sheet- Etc. may be employed. In the present invention, any method can be used for cleaning.
The use temperature of the liquid composition is preferably from 10 to 70 占 폚, particularly preferably from 20 to 50 占 폚. If it is 70 DEG C or more, the damage to the IGZO semiconductor layer becomes large, which is not preferable. In addition, if the temperature of the liquid composition is increased, the concentration of the liquid composition changes due to the evaporation of water, which is not preferable. A cooling device is required at a temperature lower than 10 DEG C, and the cost is increased, which is not preferable in practice. It is only necessary to appropriately determine the optimum processing temperature.
Example
EXAMPLES Next, the present invention will be described in more detail by way of examples, but the scope of the present invention is not limited to these examples at all.
≪ Evaluation of Cleaning and Removal Performance of Attachment Containing Copper >
(IGZO / glass substrate, manufactured by Wako Pure Chemical Industries, Ltd., reagent grade, molecular weight: 249.69) (containing 1000 ppm as copper ion) in an aqueous solution of 0.25 mass% - copper sulfate (copper sulfate pentahydrate) At 25 占 폚 for 1 minute. The excess copper sulfate aqueous solution on the substrate was rinsed with pure water (rinsing treatment) and then dried with a blower. Subsequently, the substrate was immersed in the liquid composition shown in Tables 1 to 4 at 25 占 폚 for 1 minute, the substrate after the immersion of the liquid composition was rinsed with pure water, and then dried with a blower. The copper element on the surface of the IGZO was analyzed using the X-ray photoelectron spectrometer K-alpha manufactured by Thermo Fisher Scientific Inc. (the peak position of C1s (285.2 eV) was used as a standard and the peak position was corrected for the obtained IGZO / glass substrate ). A sample in which no copper element (peak of Cu2p) was detected was regarded as an acceptable product.
≪ Evaluation of cleaning and removing performance of deposits containing molybdenum &
As the molybdenum ion attachment treatment, the IGZO / glass substrate obtained in Reference Example 1 was immersed in an aqueous 0.17 mass% -7 molybdic ammonium molybdate solution (7 ammonium molybdic acid ammonium hexahydrate, Wako Pure Chemical Industries, Ltd., reagent grade, molecular weight 1235.86) (Containing 1000 ppm as molybdenum ion) at 25 DEG C for 1 minute. An excess amount of ammonium hexamolybdate 7 ammonium on the substrate was rinsed with pure water (rinsing treatment) and then dried with a blower. Subsequently, the substrate was immersed in the liquid composition shown in Table 1 at 25 占 폚 for 1 minute, the substrate after the immersion of the liquid composition was rinsed with pure water, and then dried with a blower. The molybdenum element on the IGZO surface was analyzed using the X-ray photoelectron spectrometer K-alpha manufactured by Thermo Fisher Scientific Inc. (the peak position of C1s (285.2 eV) was used as a standard and the peak position was corrected for the obtained IGZO / glass substrate ). And a molybdenum element (peak of Mo3d) was not detected.
≪ Evaluation of cleaning and removing performance of deposits including copper and deposits containing molybdenum >
As the adhesion treatment of molybdenum ions, the IGZO / glass substrate obtained in Reference Example 1 was immersed in an aqueous solution of 0.17 mass% -7 molybdic acid-6 ammonium hydroxide (7 molybdic acid 6 ammonium tetra hydrate, product of Wako Pure Chemical Industries, Ltd., 1235.86) (containing 1000 ppm as molybdenum ion) at 25 占 폚 for 1 minute. An excess of aqueous 7 molybdic ammonium molybdate on the substrate was rinsed with pure water and then immersed in a 0.25 mass% aqueous copper sulfate solution (copper sulfate pentahydrate, Wako Pure Chemical Industries, Ltd., reagent grade, molecular weight 249.69) Containing 1000 ppm of copper ions) at 25 캜 for 1 minute. The excess copper sulfate aqueous solution on the substrate was rinsed with pure water and dried with a blower. Subsequently, the substrate was immersed in the liquid composition shown in Table 1 at 25 占 폚 for 1 minute, the substrate after the immersion of the liquid composition was rinsed with pure water, and then dried with a blower. Copper elements and molybdenum elements on the IGZO surface were analyzed using the X-ray photoelectron spectrometer K-alpha manufactured by Thermo Fisher Scientific Inc. (the peak of C1s (285.2 eV) was used as a standard and the peak position . The copper element (peak of Cu2p) and the molybdenum element (peak of Mo3d) were not detected.
≪ Evaluation of etching rate (anticorrosive property) of IGZO >
The IGZO / glass substrate obtained in Reference Example 1 was immersed in the liquid composition shown in Tables 1 to 4 at 25 占 폚 for 1 minute, and the thickness of the IGZO film before and after the treatment was measured by an optical thin film property measuring apparatus n & k Analyzer 1280 , And the etching rate was calculated by dividing the film thickness difference before and after the treatment by the etching time. And an etching rate of IGZO of less than 30 A / min was regarded as acceptable product.
≪ Evaluation of etching rate of copper (anticorrosiveness) >
The copper / molybdenum / glass substrate obtained in Reference Example 2 was immersed in the liquid compositions shown in Tables 1 to 4 at 25 占 폚 for 60 minutes. The film thickness of copper before and after the immersion treatment was measured by a fluorescent X-ray analyzer SEA1200VX manufactured by SII NanoTechnology Inc., and the etching rate was calculated by dividing the film thickness difference before and after the treatment by the etching time. And an etching rate of copper of less than 30 A / min was regarded as acceptable product.
≪ Evaluation of etch rate of molybdenum (anticorrosiveness) >
The molybdenum / glass substrate obtained in Reference Example 3 was immersed in the liquid compositions shown in Tables 1 to 4 at 25 占 폚 for 60 minutes. The film thickness of molybdenum before and after the immersion treatment was measured by a fluorescent X-ray analyzer SEA1200VX manufactured by SII NanoTechnology Inc., and the film thickness difference before and after treatment was divided by the etching time to calculate the etching rate. The etching rate of molybdenum was less than 30 Å / min.
≪ Reference Example 1: Fabrication of IGZO / glass substrate >
IGZO having an atomic ratio of indium, gallium, zinc and oxygen of 1: 1: 1: 4 was formed on a glass substrate (dimension: 150 mm x 150 mm) by the sputtering method to form a layer (IGZO film thickness: 500 Å) To prepare an IGZO / glass substrate.
≪ Referential Example 2: Copper / molybdenum / glass substrate >
Molybdenum was formed on a glass substrate (dimension: 150 mm x 150 mm) by a sputtering method to form a molybdenum (molybdenum film thickness: 300 ANGSTROM) layer and then copper was sputtered to form a copper (metal) (Copper film thickness: 3000 ANGSTROM) was formed to prepare a copper / molybdenum / glass substrate.
≪ Referential Example 3: Production of molybdenum / glass substrate >
Molybdenum / glass substrate was prepared by forming a layer of molybdenum (metal) (molybdenum film thickness: 2000 ANGSTROM) on a glass substrate (dimension: 150 mm x 150 mm) by sputtering method.
Example 1
Preparation of liquid composition
9.90 kg of pure water and (A) 0.1 kg of citric acid (manufactured by Wako Pure Chemical Industries, Ltd., food additive grade, molecular weight 210.14) as a carboxylic acid compound were added to a polypropylene container having a capacity of 10 L. Followed by stirring to confirm the dissolution of citric acid to obtain a liquid composition (1% by mass-citric acid aqueous solution). The pH value of the obtained liquid composition was 2.2.
Cleaning treatment to remove deposits containing copper
The IGZO / glass substrate obtained in Reference Example 1 was immersed in an aqueous 0.25% by mass-copper sulfate solution (containing 1000 ppm as copper ion) at 25 占 폚 for 1 minute to adhere copper ions. In order to remove the extra aqueous solution of copper sulfate, the substrate after immersion was rinsed with pure water and then dried with a blower. The IGZO / glass substrate after the copper ion attachment treatment was analyzed by X-ray photoelectron spectroscopy (XPS), and as a result, a peak of Cu2p was observed at 933 eV and 953 eV. It can be seen from this peak that the deposit including copper on the surface of the IGZO is attached at 0.7at% as the copper element. The obtained spectrum is shown in Fig.
Subsequently, the IGZO / glass substrate after the copper ion attachment treatment was immersed in the liquid composition (1 mass% - citric acid aqueous solution) prepared at 25 ° C for 1 minute. The substrate after immersion was rinsed with pure water, and then dried with a blower. The IGZO / glass substrate after the cleaning treatment was subjected to XPS analysis. The obtained spectrum is shown in Fig. No peaks of 933 eV and 953 eV based on the copper element were detected on the surface of the IGZO, and it was confirmed by the cleaning treatment using the liquid composition (1 mass% - citric acid aqueous solution) that the deposit including the copper on the IGZO surface was cleaned and removed .
A cleaning treatment for removing deposits including molybdenum
The IGZO / glass substrate obtained in Reference Example 1 was immersed in an aqueous solution of 0.17 mass% -7 mol ammonium 7 molybdic acid (containing 1000 ppm as molybdenum ions) at 25 DEG C for 1 minute, and molybdenum ions were adhered thereto. 7 The substrate after immersing the aqueous ammonium hexamolybdate molybdate was rinsed with pure water and then dried with a blower. As a result of X-ray photoelectron spectroscopy (XPS) analysis of the IGZO / glass substrate after the molybdenum ion-adhered treatment, a peak of Mo3d was detected at 228 eV and 231 eV, and deposition of molybdenum containing 0.3 at% .
Subsequently, the IGZO / glass substrate after the molybdenum ion deposition treatment was immersed in the liquid composition (1 mass% - citric acid aqueous solution) prepared at 25 ° C for 1 minute. The substrate after immersion was rinsed with pure water, and then dried with a blower. The IGZO / glass substrate after the cleaning treatment was subjected to XPS analysis. Peaks of 228 eV and 231 eV based on the molybdenum element were not detected on the surface of the IGZO, and the adhered material containing molybdenum on the surface of the IGZO was cleaned and removed by a cleaning treatment using a liquid composition (1 mass% - citric acid aqueous solution) .
A cleaning treatment for removing deposits including copper and deposits containing molybdenum
The IGZO / glass substrate obtained in Reference Example 1 was immersed in an aqueous solution of 0.17 mass% -7 mol ammonium 7-molybdic acid (containing 1000 ppm as molybdenum ions) at 25 DEG C for 1 minute, and molybdenum ions were adhered. An extra aqueous solution of ammonium hexamolybdate 7 molybdate was washed with pure water and immersed in an aqueous 0.25 mass% copper sulfate solution (containing 1000 ppm as copper ion) at 25 캜 for 1 minute to adhere copper ions. In order to remove the extra aqueous solution of copper sulfate, the substrate after immersion was rinsed with pure water and then dried with a blower. Analysis of the IGZO / glass substrate after the adhesion treatment of copper ions and molybdenum ions by X-ray photoelectron spectroscopy (XPS) revealed a peak of Cu2p at 933 eV and a peak of Mo3d at 228 eV and 231 eV. From these peaks, it can be seen that the deposit including copper on the surface of the IGZO is attached at 0.4 at% as copper element and at 0.3 at% as molybdenum element in the deposit containing molybdenum.
Subsequently, the IGZO / glass substrate after the adhesion treatment of copper ion and molybdenum ion was immersed in the liquid composition (1 mass% - citric acid aqueous solution) prepared at 25 ° C for 1 minute. The substrate after immersion was rinsed with pure water, and then dried with a blower. The IGZO / glass substrate after the cleaning treatment was subjected to XPS analysis. No peak of 933 eV and 953 eV based on the copper element and 228 eV and 231 eV based on the molybdenum element were detected on the IGZO surface, and the surface of the IGZO surface was cleaned by the cleaning treatment using the liquid composition (1 mass% - citric acid aqueous solution) It was confirmed that the deposit including copper and the deposit including molybdenum were removed.
IGZO of Etch rate evaluation
The IGZO / glass substrate obtained in Reference Example 1 was immersed in the liquid composition (1 mass% - citric acid aqueous solution) prepared at 25 deg. C for 1 minute. The processed IGZO / glass substrate was measured by an optical thin film property measuring apparatus n & k analyzer 1280 manufactured by n & k Technology Inc., and the etching rate was calculated by dividing the film thickness difference of IGZO before and after the processing by the etching time. The results are shown in Table 1. The etching rate of IGZO was 3.0 A / min, which was acceptable.
Copper Etch rate evaluation
The copper / molybdenum / glass substrate obtained in Reference Example 2 was immersed in the liquid composition (1 mass% - citric acid aqueous solution) prepared at 25 캜 for 60 minutes. The copper / molybdenum / glass substrate after the treatment was measured by a fluorescent X-ray analyzer SEA1200VX manufactured by SII NanoTechnology Inc., and the etching rate was calculated by dividing the film thickness difference of copper before and after the treatment by the etching time. The results are shown in Table 1. The etching rate of copper was 2.7 A / min, which was acceptable.
Molybdenum Etch rate evaluation
The molybdenum / glass substrate obtained in Reference Example 3 was immersed in the liquid composition (1 mass% - citric acid aqueous solution) prepared at 25 캜 for 60 minutes. The molybdenum / glass substrate after the treatment was measured by a fluorescent X-ray analyzer SEA1200VX manufactured by SII NanoTechnology Inc., and the etching rate was calculated by dividing the film thickness difference of molybdenum before and after the treatment by the etching time. The results are shown in Table 1. The etch rate of molybdenum was less than 1 Å / min and was acceptable.
Examples 2 to 36
A liquid composition was prepared in the same manner as in Example 1 except that the compositions shown in Table 2 and Table 3 were used. Using this liquid composition, the cleaning and removing performance of deposits including copper and the etching rates (anticorrosion) of IGZO, copper, and molybdenum were evaluated. The results are shown in Tables 2 and 3. With respect to any of the liquid compositions of Examples 2 to 36, the adherence including copper was satisfactory in cleaning (no 933eV and 953eV Cu2p peaks were detected based on the copper element), and IGZO, copper, and molybdenum The etching rates were all acceptable (less than 30 A / min).
Comparative Example 1
9.85 kg of pure water, 0.05 kg of 10% sulfuric acid (manufactured by Wako Pure Chemical Industries, Ltd., molecular weight 98.08) and 0.1 kg of acetic acid (manufactured by Wako Pure Chemical Industries, Ltd., molecular weight 60.05) were charged into a polypropylene container having a capacity of 10 L , And the mixture was stirred to prepare a liquid composition. The pH value of the obtained liquid composition was 2.0. Table 4 shows the results of various evaluations using this liquid composition. And the etching rate of IGZO was 68 Å / min, indicating that it failed.
Comparative Example 2
9.29 kg of pure water, 0.1 kg of acetic acid and 0.61 kg of 25% tetramethylammonium hydroxide (TMAH) were put into a 10 L polypropylene container and stirred to prepare a liquid composition. The pH value of the obtained liquid composition was 9.0. Table 4 shows the results of various evaluations using this liquid composition. It is impossible to clean and remove the deposit including copper, and the cleaning performance of the IGZO surface is inferior.
Comparative Examples 3 to 8
A liquid composition was prepared and evaluated in various manners in the same manner as in Example 1, except that the composition shown in Table 4 was used. The results are shown in Table 4. None of the liquid compositions of Comparative Examples 3 to 8 was rejected because the etching rate of IGZO was high or the adherents containing copper could not be cleaned or removed.
Comparative Examples 9 and 10
A liquid composition was prepared and evaluated in various manners in the same manner as in Example 1, except that the composition shown in Table 5 was used. The results are shown in Table 5. In Comparative Example 9 in which the liquid composition contains hydrogen peroxide, it is found that the etching rate of copper and the etch rate of molybdenum are high, and the corrosion resistance of copper and the corrosion resistance of molybdenum are lowered by containing hydrogen peroxide. Further, in Comparative Example 10 in which the liquid composition contains ammonium fluoride as a complexing agent, the etching rate of IGZO is high and it can not be applied to the cleaning and removal of deposits containing copper on the surface of IGZO.
As can be seen from the above evaluation results, all of the liquid compositions of the present invention can be used for cleaning an adherend containing copper or copper and molybdenum from the IGZO surface without corroding the IGZO semiconductor layer or the wiring including copper or copper and molybdenum · I was able to remove it.
[Table 1]
[Table 2]
[Table 3]
[Table 4]
[Table 5]
The liquid composition according to the present invention can be suitably used for cleaning and removing copper or copper and molybdenum-adhered materials attached to the IGZO surface. By using the liquid composition of the present invention, it is possible to clean and remove deposits containing copper or copper and molybdenum from the IGZO surface without corroding the wiring including the IGZO semiconductor layer or copper or copper and molybdenum.
Claims (10)
At least one selected from the group consisting of hydroxycarboxylic acid and dicarboxylic acid, or a salt thereof, and having a pH value of 1.5 to 10.
Wherein the deposits comprising copper are deposits comprising copper and molybdenum.
Wherein the hydroxycarboxylic acid is at least one selected from the group consisting of citric acid, tartaric acid, lactic acid, and glycolic acid.
Wherein the dicarboxylic acid is at least one member selected from the group consisting of malonic acid, maleic acid, maleic anhydride, and succinic acid.
Wherein the concentration of at least one selected from the group consisting of hydroxycarboxylic acid and dicarboxylic acid, or a salt thereof is 0.001 to 30 mass%.
A liquid composition comprising at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, ammonia, tetramethylammonium hydroxide, 2-aminoethanol, and 1-amino-2-propanol as a pH adjusting agent.
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JP2011204909A (en) | 2010-03-25 | 2011-10-13 | Fujifilm Corp | Cleaning composition, and method of manufacturing semiconductor device |
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