TWI428435B - A method for the purification of the drug solution - Google Patents
A method for the purification of the drug solution Download PDFInfo
- Publication number
- TWI428435B TWI428435B TW096146106A TW96146106A TWI428435B TW I428435 B TWI428435 B TW I428435B TW 096146106 A TW096146106 A TW 096146106A TW 96146106 A TW96146106 A TW 96146106A TW I428435 B TWI428435 B TW I428435B
- Authority
- TW
- Taiwan
- Prior art keywords
- chemical solution
- compound
- purifying
- chelating agent
- solution
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims description 24
- 229940079593 drug Drugs 0.000 title claims description 6
- 239000003814 drug Substances 0.000 title claims description 6
- 238000000746 purification Methods 0.000 title description 5
- 150000001875 compounds Chemical class 0.000 claims description 108
- 239000000243 solution Substances 0.000 claims description 56
- 239000000126 substance Substances 0.000 claims description 51
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 229910052751 metal Inorganic materials 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 32
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 30
- 239000002738 chelating agent Substances 0.000 claims description 29
- 229910052802 copper Inorganic materials 0.000 claims description 29
- 239000010949 copper Substances 0.000 claims description 29
- 239000002002 slurry Substances 0.000 claims description 29
- 229910052759 nickel Inorganic materials 0.000 claims description 25
- 238000005498 polishing Methods 0.000 claims description 22
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 20
- 239000004065 semiconductor Substances 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 239000003463 adsorbent Substances 0.000 claims description 13
- 125000000524 functional group Chemical group 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 8
- 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 7
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 claims description 7
- 229960001231 choline Drugs 0.000 claims description 7
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000011736 potassium bicarbonate Substances 0.000 claims description 6
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 6
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 6
- 229940086066 potassium hydrogencarbonate Drugs 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 6
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 5
- 235000011181 potassium carbonates Nutrition 0.000 claims description 5
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical compound C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 125000004432 carbon atom Chemical group C* 0.000 claims description 4
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 4
- 235000017550 sodium carbonate Nutrition 0.000 claims description 4
- 239000012670 alkaline solution Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 150000003839 salts Chemical group 0.000 claims description 3
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical class NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 150000002443 hydroxylamines Chemical class 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 150000003016 phosphoric acids Chemical class 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 150000003464 sulfur compounds Chemical class 0.000 claims description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 54
- 239000003456 ion exchange resin Substances 0.000 description 52
- 229920003303 ion-exchange polymer Polymers 0.000 description 52
- 239000000835 fiber Substances 0.000 description 29
- 230000002378 acidificating effect Effects 0.000 description 24
- 239000012488 sample solution Substances 0.000 description 24
- -1 for example Substances 0.000 description 14
- 238000012360 testing method Methods 0.000 description 14
- 238000005342 ion exchange Methods 0.000 description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 description 13
- 239000011550 stock solution Substances 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 7
- 239000010953 base metal Substances 0.000 description 7
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical class [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 150000002739 metals Chemical class 0.000 description 6
- 229910021642 ultra pure water Inorganic materials 0.000 description 6
- 239000012498 ultrapure water Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 229920001577 copolymer Polymers 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- FSVCELGFZIQNCK-UHFFFAOYSA-N N,N-bis(2-hydroxyethyl)glycine Chemical compound OCCN(CCO)CC(O)=O FSVCELGFZIQNCK-UHFFFAOYSA-N 0.000 description 4
- 239000004743 Polypropylene Substances 0.000 description 4
- 239000003957 anion exchange resin Substances 0.000 description 4
- 239000002585 base Substances 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- MYRTYDVEIRVNKP-UHFFFAOYSA-N divinylbenzene Substances C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 4
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 229920002125 Sokalan® Polymers 0.000 description 3
- 125000003158 alcohol group Chemical group 0.000 description 3
- 238000005349 anion exchange Methods 0.000 description 3
- 239000003729 cation exchange resin Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 159000000000 sodium salts Chemical class 0.000 description 3
- OWQUYBAASOSGNO-CDNKMLFNSA-N 2-[[(Z)-N-(2-hydroxy-5-sulfoanilino)-C-phenylcarbonimidoyl]diazenyl]benzoic acid Chemical compound C1=CC=C(C=C1)/C(=N/NC2=C(C=CC(=C2)S(=O)(=O)O)O)/N=NC3=CC=CC=C3C(=O)O OWQUYBAASOSGNO-CDNKMLFNSA-N 0.000 description 2
- WYMDDFRYORANCC-UHFFFAOYSA-N 2-[[3-[bis(carboxymethyl)amino]-2-hydroxypropyl]-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)CN(CC(O)=O)CC(O)=O WYMDDFRYORANCC-UHFFFAOYSA-N 0.000 description 2
- SZHQPBJEOCHCKM-UHFFFAOYSA-N 2-phosphonobutane-1,2,4-tricarboxylic acid Chemical compound OC(=O)CCC(P(O)(O)=O)(C(O)=O)CC(O)=O SZHQPBJEOCHCKM-UHFFFAOYSA-N 0.000 description 2
- LMBABJNSZGKTBA-UHFFFAOYSA-N 3,6-bis[(4-chloro-2-phosphonophenyl)diazenyl]-4,5-dihydroxynaphthalene-2,7-disulfonic acid Chemical compound OS(=O)(=O)C1=CC2=CC(S(O)(=O)=O)=C(N=NC=3C(=CC(Cl)=CC=3)P(O)(O)=O)C(O)=C2C(O)=C1N=NC1=CC=C(Cl)C=C1P(O)(O)=O LMBABJNSZGKTBA-UHFFFAOYSA-N 0.000 description 2
- FNTOMPCYJCXKDL-UHFFFAOYSA-N 3-(3-hydroxy-4-nitroso-n-propylanilino)propane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCN(CCC)C1=CC=C(N=O)C(O)=C1 FNTOMPCYJCXKDL-UHFFFAOYSA-N 0.000 description 2
- BZRWWAYVITZYRZ-UHFFFAOYSA-N 3-[4-[(5-bromopyridin-2-yl)diazenyl]-3-hydroxy-N-propylanilino]propane-1-sulfonic acid Chemical compound OC1=CC(N(CCCS(O)(=O)=O)CCC)=CC=C1N=NC1=CC=C(Br)C=N1 BZRWWAYVITZYRZ-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
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- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- YDONNITUKPKTIG-UHFFFAOYSA-N [Nitrilotris(methylene)]trisphosphonic acid Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CP(O)(O)=O YDONNITUKPKTIG-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 125000004202 aminomethyl group Chemical group [H]N([H])C([H])([H])* 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000003011 anion exchange membrane Substances 0.000 description 2
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
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- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 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 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- NBZBKCUXIYYUSX-UHFFFAOYSA-N iminodiacetic acid Chemical compound OC(=O)CNCC(O)=O NBZBKCUXIYYUSX-UHFFFAOYSA-N 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
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- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 description 1
- KUQNCHZOCSYKOR-UHFFFAOYSA-N 1,1-dioxospiro[2,1$l^{6}-benzoxathiole-3,9'-xanthene]-3',4',5',6'-tetrol Chemical compound O1S(=O)(=O)C2=CC=CC=C2C21C1=CC=C(O)C(O)=C1OC1=C(O)C(O)=CC=C21 KUQNCHZOCSYKOR-UHFFFAOYSA-N 0.000 description 1
- ZYHQGITXIJDDKC-UHFFFAOYSA-N 2-[2-(2-aminophenyl)ethyl]aniline Chemical group NC1=CC=CC=C1CCC1=CC=CC=C1N ZYHQGITXIJDDKC-UHFFFAOYSA-N 0.000 description 1
- RAEOEMDZDMCHJA-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-[2-[2-[bis(carboxymethyl)amino]ethyl-(carboxymethyl)amino]ethyl]amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CCN(CC(O)=O)CC(O)=O)CC(O)=O RAEOEMDZDMCHJA-UHFFFAOYSA-N 0.000 description 1
- XNCSCQSQSGDGES-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)C(C)CN(CC(O)=O)CC(O)=O XNCSCQSQSGDGES-UHFFFAOYSA-N 0.000 description 1
- DMQQXDPCRUGSQB-UHFFFAOYSA-N 2-[3-[bis(carboxymethyl)amino]propyl-(carboxymethyl)amino]acetic acid Chemical compound OC(=O)CN(CC(O)=O)CCCN(CC(O)=O)CC(O)=O DMQQXDPCRUGSQB-UHFFFAOYSA-N 0.000 description 1
- FCKYPQBAHLOOJQ-NXEZZACHSA-N 2-[[(1r,2r)-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-NXEZZACHSA-N 0.000 description 1
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- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 description 1
- DHDQNNWWBWIKQH-UHFFFAOYSA-N 20-benzo[a]anthracen-1-yl-21,23-dihydroporphyrin-2,3,5,7-tetrasulfonic acid Chemical compound C1(=CC=CC2=CC=C3C=C4C=CC=CC4=CC3=C12)C1=C2C=CC(C=C3C=CC(=CC=4C=C(C(=C(C5=C(C(=C1N5)S(=O)(=O)O)S(=O)(=O)O)S(=O)(=O)O)N=4)S(=O)(=O)O)N3)=N2 DHDQNNWWBWIKQH-UHFFFAOYSA-N 0.000 description 1
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- 239000002156 adsorbate Substances 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- AFYNADDZULBEJA-UHFFFAOYSA-N bicinchoninic acid Chemical compound C1=CC=CC2=NC(C=3C=C(C4=CC=CC=C4N=3)C(=O)O)=CC(C(O)=O)=C21 AFYNADDZULBEJA-UHFFFAOYSA-N 0.000 description 1
- 239000007998 bicine buffer Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- LZBFYQQOKGIGIS-UHFFFAOYSA-N chembl2006239 Chemical compound CC1=CC(C)=CC=C1NC(=O)C1=CC2=CC=CC=C2C(N=NC=2C(=CC=C(C=2)S(O)(=O)=O)O)=C1O LZBFYQQOKGIGIS-UHFFFAOYSA-N 0.000 description 1
- PBHVCRIXMXQXPD-UHFFFAOYSA-N chembl2369102 Chemical compound C1=CC(S(=O)(=O)O)=CC=C1C(C1=CC=C(N1)C(C=1C=CC(=CC=1)S(O)(=O)=O)=C1C=CC(=N1)C(C=1C=CC(=CC=1)S(O)(=O)=O)=C1C=CC(N1)=C1C=2C=CC(=CC=2)S(O)(=O)=O)=C2N=C1C=C2 PBHVCRIXMXQXPD-UHFFFAOYSA-N 0.000 description 1
- MVQBFZXBLLMXGS-UHFFFAOYSA-N chembl331220 Chemical compound C1=CC=C2C(N=NC=3C4=CC=CC=C4C=C(C=3O)C(=O)O)=C(O)C=C(S(O)(=O)=O)C2=C1 MVQBFZXBLLMXGS-UHFFFAOYSA-N 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 description 1
- 229960003178 choline chloride Drugs 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- TVMUHOAONWHJBV-UHFFFAOYSA-N dehydroglycine Chemical compound OC(=O)C=N TVMUHOAONWHJBV-UHFFFAOYSA-N 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- VFNGKCDDZUSWLR-UHFFFAOYSA-N disulfuric acid Chemical compound OS(=O)(=O)OS(O)(=O)=O VFNGKCDDZUSWLR-UHFFFAOYSA-N 0.000 description 1
- AWZOLILCOUMRDG-UHFFFAOYSA-N edifenphos Chemical compound C=1C=CC=CC=1SP(=O)(OCC)SC1=CC=CC=C1 AWZOLILCOUMRDG-UHFFFAOYSA-N 0.000 description 1
- NFDRPXJGHKJRLJ-UHFFFAOYSA-N edtmp Chemical compound OP(O)(=O)CN(CP(O)(O)=O)CCN(CP(O)(O)=O)CP(O)(O)=O NFDRPXJGHKJRLJ-UHFFFAOYSA-N 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- OUDSFQBUEBFSPS-UHFFFAOYSA-N ethylenediaminetriacetic acid Chemical compound OC(=O)CNCCN(CC(O)=O)CC(O)=O OUDSFQBUEBFSPS-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- DJQJFMSHHYAZJD-UHFFFAOYSA-N lidofenin Chemical compound CC1=CC=CC(C)=C1NC(=O)CN(CC(O)=O)CC(O)=O DJQJFMSHHYAZJD-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- LJYRLGOJYKPILZ-UHFFFAOYSA-N murexide Chemical compound [NH4+].N1C(=O)NC(=O)C(N=C2C(NC(=O)NC2=O)=O)=C1[O-] LJYRLGOJYKPILZ-UHFFFAOYSA-N 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
- 229960002378 oftasceine Drugs 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000284 resting effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- ZLLMYPVFZJLNKV-UHFFFAOYSA-M sodium 3-[3-hydroxy-4-[(5-nitropyridin-2-yl)diazenyl]-N-propylanilino]propane-1-sulfonate Chemical compound [Na+].CCCN(CCCS([O-])(=O)=O)c1ccc(N=Nc2ccc(cn2)[N+]([O-])=O)c(O)c1 ZLLMYPVFZJLNKV-UHFFFAOYSA-M 0.000 description 1
- LKSHJHJGLORTGD-UHFFFAOYSA-M sodium 3-[[3-[(2,4-dimethylphenyl)carbamoyl]-2-hydroxynaphthalen-1-yl]diazenyl]-4-hydroxybenzenesulfonate Chemical compound [Na+].CC1=C(C=CC(=C1)C)NC(=O)C=1C(=C(C2=CC=CC=C2C1)N=NC=1C=C(C=CC1O)S(=O)(=O)[O-])O LKSHJHJGLORTGD-UHFFFAOYSA-M 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 150000003512 tertiary amines Chemical group 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- MYXKPFMQWULLOH-UHFFFAOYSA-M tetramethylazanium;hydroxide;pentahydrate Chemical compound O.O.O.O.O.[OH-].C[N+](C)(C)C MYXKPFMQWULLOH-UHFFFAOYSA-M 0.000 description 1
- UZVUJVFQFNHRSY-OUTKXMMCSA-J tetrasodium;(2s)-2-[bis(carboxylatomethyl)amino]pentanedioate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CC[C@@H](C([O-])=O)N(CC([O-])=O)CC([O-])=O UZVUJVFQFNHRSY-OUTKXMMCSA-J 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940043798 zincon Drugs 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/04—Processes using organic exchangers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
- B01J41/04—Processes using organic exchangers
- B01J41/07—Processes using organic exchangers in the weakly basic form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/10—Ion-exchange processes in general; Apparatus therefor with moving ion-exchange material; with ion-exchange material in suspension or in fluidised-bed form
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/12—Ion-exchange processes in general; Apparatus therefor characterised by the use of ion-exchange material in the form of ribbons, filaments, fibres or sheets, e.g. membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/12—Ion-exchange processes in general; Apparatus therefor characterised by the use of ion-exchange material in the form of ribbons, filaments, fibres or sheets, e.g. membranes
- B01J47/127—Ion-exchange processes in general; Apparatus therefor characterised by the use of ion-exchange material in the form of ribbons, filaments, fibres or sheets, e.g. membranes in the form of filaments or fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B55/00—Safety devices for grinding or polishing machines; Accessories fitted to grinding or polishing machines for keeping tools or parts of the machine in good working condition
- B24B55/12—Devices for exhausting mist of oil or coolant; Devices for collecting or recovering materials resulting from grinding or polishing, e.g. of precious metals, precious stones, diamonds or the like
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
-
- 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
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Description
本發明係有關於半導體製造步驟所使用之含有具有鉗合形成能之化合物之藥液的純化方法,尤其係關於自半導體製造步驟所使用之添加鉗合劑之藥液,除去鉗合劑及不純金屬所形成之鉗合配位化合物之添加鉗合劑之藥液的純化方法。
半導體晶圓係經由複數個製造步驟所形成之製品。該製造步驟中,於化學的機械研磨步驟,於研磨裝置使晶圓表面接觸布(研磨布),於該處藉由循環供給研磨劑漿料下研磨所進行。
此漿料有時混合存在銅或鎳或鐵等之離子化金屬。亦即,作為研磨劑漿料成份之-係使用鹼,尤其鹼,例如氫氧化鈉係由電解鹽所製造,所產生的氫氧化鈉係含有數ppm程度之各種金屬不純物。
另外,銅皮膜所形成之晶圓之化學機械研磨步驟中,藉由研磨,銅分散於漿料中,部份離子化。
另外,鈣、鎂、錳、鐵、鈷、鋅、鋁、鉛等之金屬雖不易擴散於晶圓內部,但殘留於表面成殘渣。
此等金屬不純物中,例如銅與鎳滲透、殘留於矽晶圓,使電氣特性變化等,阻礙表面平坦化。關於如此銅、鎳容易擴散於晶圓內部之金屬與其他停留於晶圓表面之金屬
,考慮因該濃度之影響時,容易擴散之金屬濃度與停留表面之金屬相比較,有時必須減低至1/10~1/1000。因此,使用含銅或鎳等之金屬不純物之漿料研磨晶圓時,金屬擴散於晶圓內後,因所進行之晶圓熱處理或長期保管等,於晶圓表面析出此等金屬,有使降低良率(Yield rate)之問題。
另外,因為鈣、鎂、錳、鐵、鈷、鋅、鋁、鉛等之不純金屬亦阻礙電氣特性,所以含有此等不純金屬於化學機械研磨步驟之研磨液時,將成為後段洗淨步驟之負擔。
對應如此問題,提出添加鉗合劑於漿料,形成金屬配位化合物之鉗合劑添加法(例如參考特開昭63-272460號公報)。
依據鉗合劑添加法,研磨劑漿料所添加之鉗合劑係與金屬鍵結形成金屬配位化合物,因為金屬配位化合物與晶圓電氣上互斥(repulsion),可防止金屬污染。
然而,因為金屬配位化合物若殘留於晶圓表面時,仍阻礙電氣特性,所以於鹼蝕刻步驟或研磨步驟之藥液、研磨液含有時,使後段之洗淨步驟負擔增加。
另外,隨著鉗合劑添加量的增加,金屬污染量減少,但鉗合劑添加量變多時,晶圓之研磨率將降低,因此,鉗合劑添加量係以儘量少量為宜(例如參考特開2005-103700號公報)
〔專利文獻1〕特開昭63-272460號公報
〔專利文獻2〕特開2005-103700號公報
本發明者等為解決相關傳統之困難點,努力進行研究時,發現藉由自半導體製造步驟所使用之含有具有鉗合形成能之藥液,除去鉗合配位化合物,解決上述課題,而且,可抑制鉗合劑添加量至最少限度。
因為本發明係基於相關發現所實施者,以提供藉由自半導體製造步驟所使用之含有具有鉗合形成能之化合物之藥液,除去具有鉗合形成能之化合物與不純金屬所形成之鉗合配位化合物,防止上述晶圓之金屬污染以及減輕以藥液處理晶圓之洗淨負擔之添加鉗合劑之藥液的純化方法為目的。
另外,本發明係提供可抑制鉗合劑添加量至最少限度之添加鉗合劑之藥液的純化方法為目的。
本發明之添加鉗合劑之藥液的純化方法係於半導體製造步驟所使用之含有具有鉗合形成能之化合物之藥液的純化方法,以有機配位化合物吸附體處理上述藥液,除去由上述化合物與上述藥液中所含之不純金屬所形成之鉗合配位化合物為特徵。
於半導體製造步驟所使用之含有具有鉗合形成能之化合物之藥液通常為鹼性,含有作為不純物之各種微量不純金屬,尤其鎳及銅,此等係與此藥液所添加之鉗合劑形成鉗合配位化合物。
成為本發明對象之被處理藥液通常含有至少1種選自半導體用研磨漿料或氨、四甲基銨、氫氧化鈉、氫氧化鉀、碳酸鈉、碳酸鉀、碳酸氫鈉、碳酸氫鉀、膽鹼之水溶液或水分散液,尤其添加至少1種選自氨、四甲基銨、氫氧化鈉、氫氧化鉀、膽鹼之半導體用研磨漿料。
作為本發明之被處理藥液所含之具有鉗合形成能之化合物,雖舉例至少1種選自胺類、胺基羧酸類、羥基胺類、磷酸類、硫化合物類、及具有此等化合物之具有鉗合形成能之官能基之其他物質所成者,但不侷限於此等者。典型之鉗合劑為乙二胺四乙酸(EDTA)。
作為本發明所使用之有機配位化合物吸附體,可舉例如具有如下述式(1)所示之官能基之物質。
其中,(1)式中之R1係氫原子,R2及R3係碳數為1~4個之相同或相異的烷基,有具有三級胺結構之官能基者,亦即,(1)式中以R1係氫原子、R2及R3係碳數為1~4個之相同或相異的烷基者為宜。
一般,具有作為弱鹼性陰離子交換體之性質之物質係可作為本發明之有機配位化合物吸附體使用。
此等有機配位化合物吸附體係以形成珠粒狀、纖維狀或膜狀者為宜。
另外,此等有機配位化合物吸附體係以陰離子交換性官能基之末端為鹼型(OH型),由預先以如氫氧化鈉水溶液之鹼水溶液處理過以使純化藥液之pH變化變少之陰離子交換體所成者為宜。
另外,此等有機配位化合物吸附體係可使陰離子交換性之官能基之末端基,成為形成被處理藥液之主要成份之鹽型。
此等有機配位化合物吸附體係可為例如充填一種或二種以上於管柱或塔中,二種以上時係以混合或層合之形態填充,被處理藥液係通液於此管柱或塔中被處理之系統組成。
另外,亦可為複數連接此等管柱或塔,使通液於此管柱或塔中被處理之系統組成。
另外,未使用如此管柱或塔,藉由收納有機配位化合物吸附體及被處理藥液於反應層內,使被處理藥液接觸有機配位化合物吸附體而處理被處理藥液。
此時,有機配位化合物吸附體係珠粒狀或短纖維狀時,使二者於反應層內流動後,藉由過濾被處理藥液而可處理,或長纖維狀或更提高緻密性,成為膜狀之有機配位化合物吸附體之形態為螺旋狀、多孔薄片狀時,藉由層狀配
置此等有機配位化合物吸附體於反應槽,使被處理藥液通過此層而可處理。另外,有機配位化合物吸附體亦可為筒狀過濾器。
接著,以適用於純化半導體元件(晶圓)之化學機械研磨步驟中使用之漿料時為例,說明本發明之作用效果。
化學機械研磨步驟中,溶解氨、四甲基銨、氫氧化鈉、氫氧化鉀、膽鹼等之漿料係由漿料供給槽供給於研磨裝置。此漿料係抽出部份用以測定金屬量或成份,殘餘再回流於漿料供給槽,於漿料供給槽與研磨裝置間循環。
由研磨裝置所回流之漿料中,因為含有金屬成份,所以鉗合化此金屬成份之計算量之鉗合劑係添加於漿料,另一方面,添加不足成份以進行成份調製。
然而,因研磨半導體元件之漿料中,因接連被供給金屬成份,使漿料直接循環於漿料供給槽與研磨裝置間時,漿料中逐漸累積鉗合配位化合物,此附著於半導體元件表面,提高洗淨負擔,不能由洗淨而完全除去之鉗合配位化合物於後續之熱處理步驟中,成為碳化物,成為發生不良半導體元件之原因。
本發明中,如此之含鉗合配位化合物之漿料係由有機配位化合物吸附體處理所除去。
作為如此之有機配位化合物吸附體,例如可使用陰離子交換體。
亦即,因為一般鉗合配位化合物係由如羧基之鹼性水溶液或水分散液中放出氫離子,形成陰離子之化合物所形
成,所以可由陰離子交換體除去。另外,此時,使不改變漿料之pH,以弱鹼性陰離子為宜,以具有三級銨基之陰離子交換體尤其適合。
如此一來,吸附除去鉗合劑或鉗合配位化合物之漿料係經成份調整,再次供給於研磨裝置。
依據本發明,因為藥液中之不純金屬離子係因鉗合劑作為鉗合配位化合物而被除去,進而此鉗合配位化合物係由有機配位化合物吸附體除去於系外,所以可減輕事後之洗淨負擔。
另外,預先處理有機配位化合物吸附體之陰離子交換體之末端基為OH型,可除去鹼水溶液中以陰離子存在之許多金屬化學種(不純物),而且,鹼水溶液之濃度不改變,可維持高研磨效率。
接著,說明關於本發明之實施例。
[調整試料溶液]
使用旭硝子公司製之48%之氫氧化鈉水溶液、旭硝子公司製之48%之氫氧化鉀水溶液、和光純藥工業公司製特級之碳酸鈉、碳酸鉀、碳酸氫鈉、碳酸氫鉀、富山藥品工業股份有限公司製之28%之氨水、關東化學股份有限公司
製之特級之四甲基氫氧化銨五水合物、三菱氣體化學製之75%之氯化膽鹼水溶液,於各種溶液中,使溶解20ppm之下述No.1~4之鉗合劑後,加入濃度成為0.1ppm之鎳、0.1ppm之銅於試料溶液中,使形成鎳鉗合配位化合物及銅鉗合配位化合物。
另外,使溶解20ppm之EDTA於Cabot公司製Silica Base半導體研磨漿料SS25後,加入濃度成為0.1ppm之鎳、0.1ppm之銅於試料溶液中,使形成鎳鉗合配位化合物及銅鉗合配位化合物。
[除去鉗合配位化合物]
以下述方法除去調製試料溶液中之鎳鉗合配位化合物及銅鉗合配位化合物。
另外,實驗中溶解或稀釋試料等之操作皆使用超純水,測定金屬不純物,使用ICP-AES(Rigaku製CIROS120)進行。
以下之實施例及比較例使用之處理裝置及處理體(有機配位化合物吸附體)係如下所示。
[處理裝置]:處理體充填管柱3/4吋PFA管柱200mm
(PFA:四氟乙烯-全氟烷基乙烯醚共聚物)
試驗系及使用桶之材質PTFE(聚四氟乙烯)
膜試驗用支架47PTFE
[使用處理體]:(A)強鹼性陰離子交換纖維:廠商:(股)Nichibi
商品名:IEF-SA
母材:聚乙烯醇
官能基:4級銨基
形狀:直徑為100 μm,長度為2~5mm纖維狀
(B)弱鹼性陰離子交換纖維:廠商:(股)Nichibi
商品名:IEF-WA
母材:聚乙烯醇
官能基:1級~3級銨基
形狀:直徑為100 μm,長度為2~5mm纖維狀
(C)弱鹼性陰離子交換樹脂:廠商:Rohm and Haas日本(股)
商品名:DUOLITE A378D
母材:苯乙烯.二乙烯基苯共聚物
官能基:1級~3級銨基
形狀:直徑為400~650 μm之珠粒狀
(D)強鹼性陰離子交換樹脂(I型):廠商:Rohm and Haas日本(股)
商品名:A201CL
母材:苯乙烯.二乙烯基苯共聚物
官能基:4級銨基(I型)
形狀:粒徑為500~750 μm之珠粒狀
(E)強鹼性陰離子交換樹脂(II型):廠商:Rohm and Haas日本(股)
商品名:A162LF
母材:苯乙烯.二乙烯基苯共聚物
官能基:4級銨基(II型)
形狀:粒徑為500~1100 μm之珠粒狀
(F)強酸性陽離子交換樹脂:廠商:Rohm and Haas日本(股)
商品名:DUOLITE C255LFH
母材:苯乙烯.二乙烯基苯共聚物
官能基:磺酸基
形狀:粒徑為550 μm之珠粒狀
(G)弱酸性陽離子交換樹脂:廠商:Rohm and Haas日本(股)
商品名:DUOLITE C433LF
母材:丙烯酸系
官能基:羧酸基
形狀:粒徑為600~800 μm之珠粒狀
(H)鉗合纖維:廠商:(股)Nichibi
商品名:IEF-IAc
母材:聚乙烯醇
官能基:亞氨基醋酸
形狀:直徑為100 μm,長度為2~5mm纖維狀
(I)弱鹼性陰離子交換膜:廠商:旭硝子(股)
商品名:Selemion AAV
膜厚:130 μm,膜形狀:100cm×50cm
[使用鉗合劑]
1:EDTA ethylenediamine triacetic acid
2:BAPTA O,O’-Bis(2-aminophenyl)ethyleneglycol-N,N,N’,N’-tetraacetic acid,tetrapotassium salt, hydrate
3:Bicine N,N-Bis(2-hydroxyethyl)glycine
4:CyDTA trans-1,2-Diaminocyclohexane-N,N,N’,N’-tetraacetic acid, monohydrate
5:DTPA Diethylenetriamine-N,N,N’,N”,N”-pentaacetic acid
6:EDDP Ethylenediamine-N,N’-dipropionic acid, dihydrochloride
7:EDTA-OH N-(2-hydroxyethyl)ethylenediamine-N,N’,N’-triacetic acid
8:GEDTA(EGTA)O,O’-Bis(2-aminoethyl)ethyleneglycol-N,N,N’,N’-tetraacetic acid
9:HIDA N-(2-Hydroxyethyl)iminodiacetic acid
10:IDA Iminodiacetic acid
11:NTA Nitrilotriacetic acid
12:NTPO Nitrilotris(methylenephosphonic acid),trisodium salt
13:TTHA Triethylenetetramine-N,N,N’,N”,N''',N'''-hexaacetic acid
14:5-Br-PAPS 2-(5-Bromo-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl)amino]phenol,disodium salt,dehydrate
15:5-Br-PSAA 2-(5-Bromo-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl) amino]aniline,sodium salt
16:Azomethine H 8-Hydroxy-1-( salicylideneamino )-3,6-naphthalenedisulfonic acid,disodium salt
17:BT 2-Hydroxy-1-(1-hydroxy-2-naphthylazo)-6-nitro-4-naphthalenedisulfonic acid, sodium salt
18:Calcein Bis[N,N-bis(carboxymethyl)aminomethyl]fluorescein
19:Calcein Blue 8-[N,N-Bis(carboxymethyl)aminomethyl]-4-methylumbelliferone
20:Chlorophosphonazo-III 2,7-Bis(4-chloro-2-phosphonophenylazo )-1,8-dihydroxy-3,6-naphthalenedisulfonic acid, disodium salt
21:Nitroso-PSAP 2-Nitroso-5-[N-n-propyl-N-(3-sulfopropyl )amino]phenol
22:Nitro-PAPS 2-(5-Nitro-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl)amino]phenol,disodium salt,
dehydrate
23:NN 2-Hydroxy-1-(2-hydroxy-4-sulfo-1-naphthylazo )-3-naphthoic acid
24:PAR 4-(2-Pyridylazo) resorcinol
25:PR Pyrogallol sulfonphthalein Sodium blclnchoninate 4,4’-Dicarboxy-2,2’-biquinoline,disodium salt
26:Tiron 1,2-Dihydroxy-3,5-benzenedisulfonic acid,disodium salt,monohydrate
27:TPPS 5,10,15,20-Tetraphenyl-21H,23H-porphinetetrasulfonic acid,disulfuric acid,tetrahydrate
28:XO 3,3’-Bis[N,N-bis(carboxymethyl)aminomethyl]-o-cresolsulfonphthalein,disodium salt
29:Zincon 2-[1-(2-Hydroxy-5-sulfophenyl)-3-phenyl-5-formazano]benzoic acid,monosodium
30:Murexide Purpuric acid,ammonium salt
31:XB-I 3-[3-(2,4-Dimethylphenylcarbamoyl)-2-hydroxynaphthalen-1-yl-azo]-4-hydroxybenzenesulfonic acid,sodium salt
以下之鉗合劑皆為Chelest股份有限公司製。
32:EDTMP Etylene diamine tetra(methylene phosphonic acid)
33:HEDTA Hydroxyethyl Ethylene Diamine Triacetic Acid
34:GLDA Dicarboxymethyl Glutamic Acid Tetrasodium Salt
35:DHEG Dihydroxyethyl Glycine
36:PDTA 1,3-Propanediamine Tetraacetic Acid
37:DPTA-OH 1,3-Diamino-2-hydroxypropane Tetraacetic Acid
38:HEDP Hydroxyethylidene Diphosphonic Acid
39:NTMP Nitrilotris Methylene Phosphonic Acid
40:PBTC(Phosphonobutane Tricarboxylic Acid)
以上之鉗合劑皆為同仁化學研究所製。
另外,於下述之實施例及比較例中,使用之吸附體係上述(A)、(B)、……,鉗合劑係以上述1,2,……之簡稱表示。在此處理使用之(A)、(B)、(C)、(D)、(E)之離子交換體係使用90%以上之末端基為OH基者。另外,(F)、(G)、(H)係將處理過藥液之主要成份,處理成陽離子型後使用。
(洗淨使用器具等)
PTFE製桶(容積為1200ml)、PFA製管柱(3/4吋,長度為200mm)、採樣PP(聚丙烯)製容器(容積為1000ml)、PTFE製膜試驗用支架-47皆為排除金屬污染,預先以1N硝酸浸漬1小時以上後,以超純水流水洗淨。
洗淨用硝酸係關東化學(股)製之電子工業用級(
EL),以超純水稀釋成約1N者,超純水係超純水製造系統所製造之金屬含有量為1ppt以下者。
將以上述洗淨方法所洗淨之器具,依PTFE製桶、PFA管柱之順序,以PFA配管連接。通水超純水於此系統,於PFA管柱出口,收納於PE容器時之試驗系對照組之分析結果如表1所示。由表顯示,未受到此系統之污染。
(處理操作)
填充使對象藥液之成份濃度不發生變化而對末端基施以處理之(A)~(H)之各種吸附體於PFA管柱(3/4吋,長度為200mm)。填充係以充分洗淨之PTFE之推棒輕輕推入吸附體,緩緩填充,填充使管柱內部緊密。
填充吸附體之PFA管柱中,以10ml/min通液超純水12小時以上,充分沖洗溶出的金屬或有機物。充分瀝水使PTFE製桶的內部不殘留水滴,加入試料溶液。將加入試料溶液之PTFE製桶及填充經洗淨過填充物之PFA管柱,以1/4吋之PFA管連接,於PFA管柱出口設置採樣容器。
自PTFE製桶之上方導入氮氣,加壓至容器內部之壓力至0.1MPa,操作流量調整閥,調整自PFA管柱出口流出之試料溶液之流出速度為5ml/min以下。
以pH試紙測定流出之試料溶液之pH,當pH與供給試料溶液相同時,PFA管柱出口之液體作為試樣,收納於PE容器。
PE容器收納之試料溶液立即密封,由ICP-AES(感應藕合電漿原子發射光譜儀)進行鎳及銅之分析。
由ICP-AES分析,作為導入分析器前處理,因應需要,進行脫鹽處理。
另外,此實施例及以下之各實施例以及比較例中之處理體量係40ml,試料通液速度係5ml/min以下,通液量為1000ml,通液係皆為1次通過,雖以20~25℃之溫度條件進行,但即使25℃以上之鹼水溶液,只要使用材料為耐熱性者,可以使用。
另外,與上述同樣地,以1N硝酸浸漬1小時後,以超流水洗淨之PP(聚丙烯)製容器(容積為250ml)中,添加200ml之試料溶液、(A)~(H)之吸附體,由批次法使接觸24小時,進行鎳鉗合配位化合物及銅鉗合配位化合物之除去試驗。
另外,安裝將(I)及(B)編織如圖1之平膜於PTFE製膜試驗用支架47,供給EDTA之銅鉗合配位化合物所添加之48%之氫氧化鈉,進行除去試驗。
使用28%之氨水作為試料溶液,進行上述處理操作之結果如表2~9所示。
使用28%之氨水之實施例1之表2~9中,表3之弱鹼性離子交換纖維(B)及表4之弱鹼性離子交換樹脂(C)係顯示除去鎳鉗合配位化合物及銅鉗合配位化合物之能力強。另一方面,確認表7之強酸性離子交換樹脂(F)及表8之弱酸性陽離子交換樹脂(G)無除去能力。另外,表9之鉗合纖維(H)中,可依鉗合劑種類,確認兩鉗合配位化合物之除去能力。
在此,此次使用之全部鉗合劑係水溶性,於鹼性溶液中溶解成陰離子。另外,即使鎳及銅形成鉗合配位化合物之狀態,亦為陰離子之形態。此係因為如實施例1之結果
所示,弱鹼性離子交換纖維及弱鹼性陰離子交換樹脂顯示除去鉗合配位化合物之能力強,強酸性及弱酸性離子交換樹脂未顯示除去鉗合配位化合物之能力,所以可以確認。然而,可知表2之強鹼性離子交換纖維(A)及表5之強鹼性離子交換樹脂(I型)(D)、表6之強鹼性離子交換樹脂(II型)(E)係除去能力非常低或不能確認。該理由係認為本實施例使用之28%氨水係鹼性溶液,以陰離子形態溶解於試料溶液內之鉗合配位化合物,不吸附於4級銨基,依循吸附溶液中之氫氧化物離子(OH-)之樹脂之再生方向,進行反應。
另外,雖發現鹼性離子交換樹脂(II型)之除去能力比強鹼性離子交換樹脂(I型)強之趨勢,但作為該理由,認為係II型之鹼度比I型低,所以雖微量,但吸附鉗合配位化合物。
鉗合纖維係可說與鎳或銅之鉗合力比添加之鉗合劑強時,可自形成之鉗合配位化合物,奪取鎳或銅而除去。
另外,實施例1之表2~9皆為使用管柱之結果,由批次法之結果,及使用管柱之結果皆顯示相同的趨勢。
使用25%之四甲基氫氧化銨水溶液作為試料溶液,進行上述處理操作。
使用25%之四甲基氫氧化銨水溶液之實施例2中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1同
樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用48%之氫氧化鈉水溶液作為試料溶液,進行上述處理操作。
使用48%之氫氧化鈉水溶液之實施例3中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1及2同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1及2同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用48%之氫氧化鉀水溶液作為試料溶液,進行上述處理操作。
使用48%之氫氧化鉀水溶液之實施例4中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~3同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~3同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用23%之碳酸鈉水溶液作為試料溶液,進行上述處理操作。
使用23%之碳酸鈉溶液之實施例5中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~4同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~4同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用50%之碳酸鉀水溶液作為試料溶液,進行上述處理操作。
使用50%之碳酸鉀溶液之實施例6中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~5同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~5同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用8%之碳酸氫鈉水溶液作為試料溶液,進行上述處理操作。
使用8%之碳酸氫鈉溶液之實施例7中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~6同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~6同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用50%之碳酸氫鉀水溶液作為試料溶液,進行上述處理操作。
使用50%之碳酸氫鉀溶液之實施例8中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~7同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~7同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用75%之膽鹼水溶液作為試料溶液,進行上述處理操作。
使用75%之膽鹼溶液之實施例9中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~8同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~8同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖
維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用漿料SS25原液作為試料溶液,進行上述處理操作。
使用漿料SS25原液之實施例10中,相對於原液中之鎳及銅之濃度皆為0.1ppm,與實施例1~9同樣地以弱鹼性離子交換樹脂及弱鹼性離子交換纖維處理後,成為0.01ppm以下,顯示可除去鎳鉗合配位化合物及銅鉗合配位化合物。另外,與實施例1~9同樣地就上述理由,強酸性離子交換樹脂、弱酸性離子交換樹脂、強鹼性離子交換樹脂(I型)、強鹼性離子交換樹脂(II型)及鉗合纖維未能得到充分除去鎳鉗合配位化合物及銅鉗合配位化合物之能力。
使用48%之氫氧化鈉作為試料溶液,安裝將(I)及(B)編織如圖1之平膜於PTFE製膜試驗用支架47,供給添加EDTA之銅、鎳之鉗合配位化合物之結果如表10所示。
使用48%之氫氧化鈉作為試料溶液,使用弱鹼性陰離子交換膜(I)及弱鹼性陰離子交換纖維(B)平膜於PTFE製膜試驗用支架47之實施例11中,如表10所示,認為(I)及(B)平膜皆除去銅、鎳之鉗合配位化合物。
本發明係可廣泛地利用於純化含有具有鉗合形成能之化合物之藥液。
〔圖1〕本發明實施例中使用之有機配位化合物吸附體之放大照片。
Claims (10)
- 一種添加鉗合劑之藥液的純化方法,其特徵為於半導體製造步驟所使用之含有具有鉗合形成能之化合物之鹼性藥液的純化方法中,前述具有鉗合形成能之化合物係至少1種選自胺類、胺基羧酸類、羥基胺類、磷酸類、硫化合物類,以具有下述式(1)所示之官能團之有機配位化合物吸附體處理該藥液,除去因該藥液中所含之不純金屬之鎳及銅,與於鹼性水溶液中由形成陰離子之物質所成之具有鉗合形成能之化合物所形成之鉗合配位化合物,
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該藥液係含有至少1種選自半導體用研磨漿料或氨、四甲基銨、氫氧化鈉、氫氧化鉀、碳酸鈉、碳酸鉀、碳酸氫鈉、碳酸氫鉀、膽鹼之水溶液或水分散液。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該藥液係含有至少1種選自氨、四甲基銨、氫 氧化鈉、氫氧化鉀、碳酸鈉、碳酸鉀、碳酸氫鈉、碳酸氫鉀、膽鹼之半導體用研磨漿料。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該藥液中所含之具有鉗合形成能之化合物係乙二胺四乙酸。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該有機配位化合物吸附體係珠粒狀、纖維狀或膜狀所成。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該有機配位化合物吸附體係以陰離子交換性之官能基之末端基為鹼型(OH型),由預先處理過以使純化藥液之pH變化變少之陰離子交換體所成。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該有機配位化合物吸附體係使陰離子交換性之官能基之末端基,成為形成該藥液之主要成份之鹽型。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該有機配位化合物吸附體係可充填一種或二種以上於管柱或塔中,二種以上時係以混合或層合之形態充填,該藥液係通液於該管柱或塔中。
- 如申請專利範圍第8項之添加鉗合劑之藥液的純化方法,其中該管柱或塔係複數連接。
- 如申請專利範圍第1項之添加鉗合劑之藥液的純化方法,其中該有機配位化合物吸附體係與該藥液收納於反應層內,使該藥液於該反應層內流動後過濾。
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