CN103343060B - Sapphire substrate wafer cleaning solution as well as preparation method, application and cleaning method thereof - Google Patents
Sapphire substrate wafer cleaning solution as well as preparation method, application and cleaning method thereof Download PDFInfo
- Publication number
- CN103343060B CN103343060B CN201310302693.5A CN201310302693A CN103343060B CN 103343060 B CN103343060 B CN 103343060B CN 201310302693 A CN201310302693 A CN 201310302693A CN 103343060 B CN103343060 B CN 103343060B
- Authority
- CN
- China
- Prior art keywords
- sapphire substrate
- substrate wafer
- acid
- parts
- cleaning liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 111
- 239000010980 sapphire Substances 0.000 title claims abstract description 111
- 239000000758 substrate Substances 0.000 title claims abstract description 109
- 238000004140 cleaning Methods 0.000 title claims abstract description 96
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 68
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 150000001412 amines Chemical class 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 35
- 239000003513 alkali Substances 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 239000008139 complexing agent Substances 0.000 claims abstract description 28
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 31
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 27
- 230000002000 scavenging effect Effects 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 25
- -1 Starso Chemical compound 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 159000000000 sodium salts Chemical class 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 6
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229920001577 copolymer Polymers 0.000 claims description 6
- 229920002223 polystyrene Polymers 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 6
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims description 4
- 229940043276 diisopropanolamine Drugs 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011707 mineral Substances 0.000 claims description 4
- 235000010755 mineral Nutrition 0.000 claims description 4
- 150000007530 organic bases Chemical class 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
- RJFMDYQCCOOZHJ-UHFFFAOYSA-L 2-hydroxyethyl(trimethyl)azanium dihydroxide Chemical compound [OH-].[OH-].C[N+](C)(C)CCO.C[N+](C)(C)CCO RJFMDYQCCOOZHJ-UHFFFAOYSA-L 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 claims description 3
- NDKBVBUGCNGSJJ-UHFFFAOYSA-M benzyltrimethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)CC1=CC=CC=C1 NDKBVBUGCNGSJJ-UHFFFAOYSA-M 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 239000000174 gluconic acid Substances 0.000 claims description 3
- 235000012208 gluconic acid Nutrition 0.000 claims description 3
- 229960003330 pentetic acid Drugs 0.000 claims description 3
- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 235000017550 sodium carbonate Nutrition 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- 239000011718 vitamin C Substances 0.000 claims description 3
- 235000019154 vitamin C Nutrition 0.000 claims description 3
- 239000004711 α-olefin Substances 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical group CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 2
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 claims description 2
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims description 2
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 2
- QYRKIYOQYLSWIU-UHFFFAOYSA-N [OH-].CC(C[NH+](O)O)C Chemical compound [OH-].CC(C[NH+](O)O)C QYRKIYOQYLSWIU-UHFFFAOYSA-N 0.000 claims description 2
- NWEKXBVHVALDOL-UHFFFAOYSA-N butylazanium;hydroxide Chemical compound [OH-].CCCC[NH3+] NWEKXBVHVALDOL-UHFFFAOYSA-N 0.000 claims description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 2
- CCIVGXIOQKPBKL-UHFFFAOYSA-N ethanesulfonic acid Chemical compound CCS(O)(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-N 0.000 claims description 2
- 239000004310 lactic acid Substances 0.000 claims description 2
- 235000014655 lactic acid Nutrition 0.000 claims description 2
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 2
- MGFYIUFZLHCRTH-UHFFFAOYSA-N nitrilotriacetic acid Chemical compound OC(=O)CN(CC(O)=O)CC(O)=O MGFYIUFZLHCRTH-UHFFFAOYSA-N 0.000 claims description 2
- 239000000467 phytic acid Substances 0.000 claims description 2
- 229940068041 phytic acid Drugs 0.000 claims description 2
- 235000002949 phytic acid Nutrition 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- WNEYXFDRCSFJCU-UHFFFAOYSA-N propan-1-amine;hydrate Chemical compound [OH-].CCC[NH3+] WNEYXFDRCSFJCU-UHFFFAOYSA-N 0.000 claims description 2
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 2
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 2
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 2
- 229960004418 trolamine Drugs 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 239000000811 xylitol Substances 0.000 claims description 2
- 235000010447 xylitol Nutrition 0.000 claims description 2
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 2
- 229960002675 xylitol Drugs 0.000 claims description 2
- 150000004996 alkyl benzenes Chemical class 0.000 claims 1
- 235000015165 citric acid Nutrition 0.000 claims 1
- 230000003749 cleanliness Effects 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 239000000356 contaminant Substances 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 235000012431 wafers Nutrition 0.000 abstract 3
- 150000002191 fatty alcohols Chemical class 0.000 abstract 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 abstract 1
- 238000010926 purge Methods 0.000 description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 12
- 239000002585 base Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 9
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 8
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 6
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- YCOZIPAWZNQLMR-UHFFFAOYSA-N heptane - octane Natural products CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
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- 239000004743 Polypropylene Substances 0.000 description 2
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- 239000004260 Potassium ascorbate Substances 0.000 description 1
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- QDPMLKBAQOZXEF-UHFFFAOYSA-N ethanesulfonic acid;sodium Chemical compound [Na].CCS(O)(=O)=O QDPMLKBAQOZXEF-UHFFFAOYSA-N 0.000 description 1
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- CONVKSGEGAVTMB-RXSVEWSESA-M potassium-L-ascorbate Chemical compound [K+].OC[C@H](O)[C@H]1OC(=O)C(O)=C1[O-] CONVKSGEGAVTMB-RXSVEWSESA-M 0.000 description 1
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- DWWABVYIZMBHHR-UHFFFAOYSA-N propylbenzene;sodium Chemical compound [Na].CCCC1=CC=CC=C1 DWWABVYIZMBHHR-UHFFFAOYSA-N 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- DZCAZXAJPZCSCU-UHFFFAOYSA-K sodium nitrilotriacetate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC([O-])=O DZCAZXAJPZCSCU-UHFFFAOYSA-K 0.000 description 1
- NGSFWBMYFKHRBD-UHFFFAOYSA-N sodium;2-hydroxypropanoic acid Chemical compound [Na+].CC(O)C(O)=O NGSFWBMYFKHRBD-UHFFFAOYSA-N 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- IRZFQKXEKAODTJ-UHFFFAOYSA-M sodium;propan-2-yloxymethanedithioate Chemical compound [Na+].CC(C)OC([S-])=S IRZFQKXEKAODTJ-UHFFFAOYSA-M 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 1
- 125000002769 thiazolinyl group Chemical group 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Abstract
The invention relates to a sapphire substrate wafer cleaning solution as well as a preparation method, an application and a cleaning method thereof. The cleaning solution comprises an amine oxide surfactant, a fluoric surfactant, organic sulfonate, fatty alcohol polyoxyethylene polyoxypropylene ether, alkali, a complexing agent, a particle trapping agent and pure water. The sapphire substrate wafer cleaning solution has excellent cleaning capacity to sapphire substrate wafers, and can thoroughly remove contaminants to improve the cleanliness of electronic components; and moreover, the cleaning solution has multiple advantages of simplicity in preparation, low cost, environmental friendliness and the like, and has wide research values and industrial application prospects.
Description
Technical field
The present invention relates to a kind of LED device scavenging solution, relate to especially a kind of Sapphire Substrate wafer cleaning liquid, preparation method, purposes and its purging method of use, the electronics that belongs to opto-electronic device cleans field.
Background technology
At optoelectronic areas, photodiode (LED) has the advantages such as low-work voltage, reduce power consumption, high-level efficiency, long lifetime, solidification, fast-response speed and driving circuit are simple,, as new generation of environment protection semiconductor illuminating light source, be acknowledged as one of 21 century high-tech sector most with prospects.
Sapphire wafer is the first-selected substrate slice of current LED industry, and its surface accurate processing quality and cleanliness factor have very important impact to the Performance and quality of LED device.Sapphire Substrate wafer is in residual plurality of impurities in manufacturing process rear surface such as cutting, grinding, polishings, as pollutents such as organism, abrasive grains, metal ion, inorganic impurities, this need to carry out surface cleaning to Sapphire Substrate wafer, with the clean sapphire sheet that obtains conforming to quality requirements.Meanwhile, before packaging, to carry out terminal cleaning, before extension or PSS technique, also will carry out supplied materials cleaning to the Sapphire Substrate wafer of buying, to ensure the cleanliness factor on substrate slice surface.
Along with LED luminescent properties is required to improve constantly, and Sapphire Substrate wafer is to the development of major diameter, high-quality direction, thereby the surface quality requirement to Sapphire Substrate wafer is more and more tighter, this is mainly because the impurity contamination of Sapphire Substrate wafer surface can have a strong impact on quality and the yield rate of LED.In current LED produces, more than 50% waste product is because surface contamination causes, due in substrate slice is produced almost every procedure there is cleaning problem, so the quality of Sapphire Substrate wafer cleaning has a serious impact the luminescent properties of final LED.
Prior art mainly adopts acetone, hydrofluoric acid, sulfuric acid, hydrogen peroxide, acid, oxidative chemistries etc. to the cleaning of Sapphire Substrate wafer, but these materials to the removal ability of organism and particle a little less than, operator's personnel safety has been produced to security threat, and environmental pollution is serious.
Along with LED industry and the precision machined development of Sapphire Substrate wafer, scavenging solution has been proposed to harsher and multifarious requirement, its main development requires and trend is: 1, reduce costs, this is the requirement of LED industry development; 2, improve surface cleanliness, reduce surface particles number; 3, improve cleaning efficiency, can shorten process period, enhance productivity; 4, environmental protection, environmentally safe.
Through years of researches, the method for existing multiple cleaning Sapphire Substrate wafer at present.
CN1833816A discloses a kind of method of cleaning sapphire wafer, and the scavenging solution using comprises sulfuric acid, phosphoric acid, hydrogen peroxide, water, or comprises ammonium hydroxide, hydrogen peroxide and water.
CN101468352A discloses a kind of Sapphire Substrate sheet purging method, and described purging method comprises substrate slice is positioned in Virahol and coordinates ultrasonic cleaning approximately 3 minutes.
CN101912855A discloses a kind of Sapphire Substrate sheet material surface of polished cleaning method, and the scavenging solution that wherein used is water, promoting agent, sequestrant and stopping agent.Wherein promoting agent is FA/O type tensio-active agent, and sequestrant is FA/O sequestrant, and stopping agent is hexamethylenetetramine or phenylpropyl alcohol triazole.
CN102218410A discloses the purging method after a kind of sapphire polishing, the scavenging solution that wherein used be by hydrogen peroxide, ammoniacal liquor and deionized water according to certain mass than formulated.
CN102632055A discloses a kind of purging method of Sapphire Substrate sheet, and the scavenging solution using is the mixture of ammoniacal liquor, hydrogen peroxide and water composition, or be the mixture that hydrochloric acid, hydrogen peroxide and water form, the mixture that can also form for sulfuric acid and phosphoric acid.
CN102962226A discloses the purging method after the polishing of a kind of Sapphire Substrate sheet, has wherein used the materials such as SM-007 acid, SP-2200 alkali, DP-020 alkali as scavenging solution.
CN103111434A discloses a kind of sapphire and has processed final cleaning, in described cleaning, relates to following steps: a, Virahol clean; B, ethanol clean; C, washed with de-ionized water; D, ammoniacal liquor clean; E, washed with de-ionized water; F, phosphoric acid clean; G, washed with de-ionized water; H, hydrofluoric acid clean; I, washed with de-ionized water; J, washed with de-ionized water.
As mentioned above, although in prior art, there is multiple kinds of cleaning agent, but still exist various defects, for example, to a little less than organic matter removal ability; Be difficult to thoroughly remove the inorganic particles such as the silicon carbide that adsorbs in cutting, grinding and corrosion process, norbide, silicon-dioxide; Used acid and/or oxygenant, operator has been produced to security threat, and environmental pollution is serious etc.
Therefore, environment-friendly high-efficiency how to realize Sapphire Substrate wafer cheaply surface cleaning is the huge challenge that sapphire wafer manufacturing process technology faces, the Sapphire Substrate wafer cleaning agent efficient, environmental protection of exploitation is simultaneously the current place of needing badly to meet LED industry development demand, also be the focus and emphasis field of studying both at home and abroad, the starting point that the present invention is accomplished and realizes especially.
Summary of the invention
The existing many disadvantages of existing Sapphire Substrate wafer cleaning liquid based on described above, and in order to seek new Sapphire Substrate wafer cleaning liquid, preparation method and purging method, the invention provides a kind of Sapphire Substrate wafer cleaning liquid, it has functional, Environmental Safety, and can reduce particle contamination, the raising Sapphire Substrate wafer process efficiency of Sapphire Substrate wafer.
Particularly, the invention provides a kind of Sapphire Substrate wafer cleaning liquid, preparation method, purposes and use the Sapphire Substrate wafer cleaning method of this scavenging solution.
More specifically, first object of the present invention is to provide a kind of Sapphire Substrate wafer cleaning liquid, and described scavenging solution comprises the following various components in weight part:
It should be noted that, unless otherwise prescribed, " the comprising " while relating to component in this application, that its implication relates to is enclosed " by .... composition " or its equivalent definition, and open " comprising ", " comprising " etc. or its equivalent definition, and can not be limited to its simple literal meaning.
Unless otherwise prescribed, " aggregate number " that relate in this application polymerized unit number has the implication identical with " polymerization degree ", and the implication of aggregate number is equal to the polymerization degree.
In described scavenging solution of the present invention, described amine oxide surfactant structure is as follows:
Wherein x is the integer between 6-14, and y is the integer between 8-12;
Exemplarily, x can be 6,7,8,9,10,11,12,13 or 14; Y can be 8,9,10,11 or 12;
R
1for C
8-C
12straight or branched alkyl, exemplarily, for example, be n-octyl, n-nonyl, positive decyl, n-undecane base or dodecyl.
In narration, for for simplicity, described amine oxide surfactant is abbreviated as to " R below
1-x-y ", its implication is to refer to the amine oxide surfactant with said structure general formula, for example implication of " n-octyl-6-8 " is to refer in said structure general formula, R
1for n-octyl, x are 6 and the y amine oxide surfactant that is 8, similar successively, other abbreviation defines according to this and refers to.
The weight part of described amine oxide surfactant is 1-10 part, this scope has comprised any sub-range scope wherein, as 1-10 part, 3-8 part, 5-6 part, also comprise any concrete point value wherein, as 1 part, 2 parts, 3 parts, 4 points, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts or 10 parts.
In described scavenging solution of the present invention, described fluorochemical surfactant is perfluoroalkyl oxyethyl group Soxylat A 25-7, and its structural formula is C
mf
2m+1cH
2cH
2o (C
2h
4o)
nh, the aggregate number that wherein n is oxyethane, m and n are all selected from the integer of 6-12, and exemplarily, for example both can be 6,7,8,9,10,11 or 12 independently of one another.
Wherein as the C of end group
mf
2m+1in C-C skeleton form be not particularly limited, can be straight or branched.Exemplify indefiniteness ground, described C as one
mf
2m+1can be perfluor n-hexyl (C
6f
13), perfluor n-octyl (C
8f
17), the positive decyl (C of perfluor
10f
21), perfluor dodecyl (C
12f
25) or (CF
3)
2cF (CF
2)
3-etc.
Described fluorochemical surfactant can be any one or any multiple mixture that belong within the scope of this structural formula.
The weight part of described fluorochemical surfactant is 0.01-3 part, this scope has comprised any sub-range scope wherein, as 0.05-2.5 part, 0.1-2 part, 0.5-1.5 part, also comprised any concrete point value wherein, as 0.01 part, 0.05 part, 0.07 part, 0.09 part, 0.12 part, 0.15 part, 0.2 part, 0.5 part, 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts.
In described scavenging solution of the present invention, described organic sulfonate is any one sylvite or the sodium salt in methylsulphonic acid, ethylsulfonic acid, n-propyl sulfonic acid, sec.-propyl sulfonic acid, tosic acid, xylene monosulfonic acid, α-olefin sulfonic acid, C8-C12 alkyl benzene sulphonate (ABS), or is wherein sylvite and/or the sodium salt of multiple mixture arbitrarily.
Wherein, the thiazolinyl in α-olefin sulfonic acid is C
2-C
8thiazolinyl, as vinyl, allyl group, butenyl, pentenyl, hexenyl, heptenyl or octenyl.
The weight part of described organic sulfonate is 1-10 part, this scope has comprised any sub-range scope wherein, as 1-10 part, 3-8 part, 5-6 part, also comprised any concrete point value wherein, as 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts or 10 parts.
In described scavenging solution of the present invention, described aliphatic alcohol polyethenoxy polyethenoxy ether, structural formula is R
2o (C
2h
4o)
p(C
3h
6o)
qh.
Wherein p and q are respectively the aggregate number of oxyethane and propylene oxide, and wherein p is the integer between 4-12, and q is the integer between 4-10.
Exemplarily, p can be 4,5,6,7,8,9,10,11 or 12; Q can be 4,5,6,7,8,9 or 10.
Wherein R
2for C
10-C
18straight or branched alkyl, exemplarily, R
2for positive decyl, n-undecane base, dodecyl, n-tridecane base, n-tetradecane base, Pentadecane base, n-hexadecyl, n-heptadecane base or Octadecane base.
The weight part of described aliphatic alcohol polyethenoxy polyethenoxy ether is 1-20 part, this scope has comprised any sub-range scope wherein, as 1-20 part, 3-18 part, 5-16 part, 7-14 part, 9-11 part, also comprised any concrete point value wherein, as 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts or 20 parts.
In described scavenging solution of the present invention, described alkali is organic bases, mineral alkali or both mixtures.
Wherein, described organic bases is any one or the multiple mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, four n-propyl ammonium hydroxide, 4-n-butyl ammonium hydroxide, trimethyl benzyl ammonium hydroxide, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, diethylamine, triethylamine, quadrol, monoethanolamine, diethanolamine, trolamine, α-amino isopropyl alcohol, diisopropanolamine (DIPA), tri-isopropanolamine.
Described mineral alkali is any one or the multiple mixture in sodium carbonate, salt of wormwood, Sodium Hydrogen Carbonate, potassium bicarbonate, Starso, sodium hydroxide, potassium hydroxide.
The weight part of described alkali is 1-5 part, and this scope has comprised any concrete point value wherein, as 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts or 5 parts.
In described scavenging solution of the present invention, described complexing agent is any one or the multiple mixture in ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, citric acid, xitix, vitamins C, phytic acid, nitrilotriacetic acid(NTA), gluconic acid, Sorbitol Powder, Xylitol, lactic acid, oxysuccinic acid, or be any one sylvite or sodium salt wherein, or be multiple sylvite and/or sodium salt arbitrarily wherein.
The weight part of described complexing agent is 0.5-2 part, and this scope has comprised any sub-range scope wherein, as 0.5-2 part, 1-1.5 part, has also comprised any concrete point value wherein, as 0.5 part, 0.75 part, 1 part, 1.25 parts, 1.5 parts, 1.75 parts or 2 parts.
In described scavenging solution of the present invention, any one in segmented copolymer, polyacrylic acid or its salt, polyoxyethylene glycol (PEG) or polymine that described particle capture agent is polyvinyl alcohol and polystyrene or multiple mixture.
Wherein the general structure of the segmented copolymer of polyvinyl alcohol and polystyrene is, (CH
2cH (C
6h
5))
s(CH
2cHOH)
twherein s, t are respectively the aggregate number of vinylbenzene and vinyl alcohol, be the integer between 20-100 independently of one another, as respectively done for oneself 20,30,40,50,60,70,80,90,100,110,120,130,140,150,160,170,180,190 or 200.
Described polyacrylic molecular weight is 1000-6000, for example, be 1000,2000,3000,4000,5000 or 6000.
The molecular weight of described polyoxyethylene glycol is 200-1000, for example, can be 200 (PEG-200), 300 (PEG-300), 400 (PEG-400), 500 (PEG-500), 600 (PEG-600), 700 (PEG-700), 800 (PEG-800), 900 (PEG-290) or 1000 (PEG-1000).Be that described polyoxyethylene glycol can be PEG-200, PEG-300, PEG-400, PEG-500, PEG-600, PEG-700, PEG-800, PEG-900 or PEG-1000.
The general structure of polymine is (CH
2cH
2nH)
v, wherein v is the polymerization degree, it is the integer between 50-100, as 50,55,60,65,70,75,80,85,90,95 or 100.
The weight part of described particle capture agent is 0.5-5 part, this scope has comprised any sub-range scope wherein, as 0.5-5 part, 1-4 part, 2-3 part, also comprise any concrete point value wherein, as 0.5 part, 1 part, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 3.5 parts, 4 parts, 4.5 parts or 5 parts.
In described scavenging solution of the present invention, described pure water preferably its resistance is 18M Ω.
The weight part of described pure water is 10-80 part, this scope has comprised any sub-range scope wherein, as 10-80 part, 20-70 part, 30-60 part, 40-50 part, also comprised any concrete point value wherein, as 10 parts, 15 parts, 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 50 parts, 55 parts, 60 parts, 65 parts, 70 parts, 75 parts or 80 parts.
Give an example as one, the various components that comprise following weight parts of Sapphire Substrate wafer cleaning liquid of the present invention:
As another kind for example, the various components that comprise following weight parts of Sapphire Substrate wafer cleaning liquid of the present invention:
Second object of the present invention relates to the preparation method of above-mentioned Sapphire Substrate wafer cleaning liquid, and described preparation method comprises the steps:
(1) take respectively the various components of above-mentioned weight part separately;
(2) pure water is joined in stirring tank, then add in turn alkali, complexing agent, be stirred to homogeneous transparent;
(3) in the homogeneous transparent mixture in step (2), add in turn organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and particle capture agent, be stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid.
Wherein, in above-mentioned steps (2) and (3), stirring velocity can be 40-100rpm/min, is preferably 60-80rpm/min.
The 3rd object of the present invention relates to the method that uses above-mentioned Sapphire Substrate wafer cleaning liquid to clean Sapphire Substrate wafer, and described purging method comprises the steps:
(1) Sapphire Substrate wafer is positioned in pure water to ultrasonic cleaning 2-10 minute;
(2) the Sapphire Substrate wafer cleaning liquid of the invention described above is mixed with to the aqueous solution that mass concentration is 1-15%, the Sapphire Substrate wafer after then step (1) being cleaned is positioned in the described aqueous solution, ultrasonic cleaning 3-10 minute;
(3) the Sapphire Substrate wafer after step (2) cleaning is positioned in pure water, ultrasonic cleaning 2-10 minute, repeats this step 2-4 time;
(4) by step (3) clean after Sapphire Substrate wafer at 80-100 DEG C, bake drying 8-12 minute;
Wherein the cleaning temperature in step (1), (2) and (3) is 40-60 DEG C, ultrasonic frequency and is 20-50kHz.
Give an example as one, the cleaning temperature in step (1), (2) and (3) can be 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C or 60 DEG C.
Give an example as one, the scavenging period in step (1) and (3) can be 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes or 10 minutes.
Give an example as one, the scavenging period in step (2) can be 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes or 10 minutes.
Give an example as one, the ultrasonic frequency in step (1), (2) and (3) can be 20kHz, 30kHz, 40kHz or 50kHz.
Give an example as one, the scavenging solution mass concentration in step (2) can be 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 15%.
Give an example as one, the temperature in step (4) can be 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C or 100 DEG C.
Give an example as one, can be 8 minutes the time of drying in step (4), 9 minutes, 10 minutes, 11 minutes or 12 minutes.
The 4th object of the present invention relates to above-mentioned Sapphire Substrate wafer cleaning liquid in the purposes of cleaning in Sapphire Substrate wafer, by using described scavenging solution to clean, can effectively remove various impurity residual on Sapphire Substrate wafer, meet the high-cleanness, high requirement of electron device following process and use.
In sum, the present invention is by providing Sapphire Substrate wafer cleaning liquid, the Preparation Method And The Use with specific components, content, and develop a kind of Novel washing liquid, it has the plurality of advantages such as cleaning efficiency is high, cleanliness factor is high, safety and environmental protection, has prospects for commercial application and researching value very widely.
Brief description of the drawings
Fig. 1 is the Sapphire Substrate wafer surface of cleaning and the surface contact angle survey sheet of water.
Fig. 2 be use the embodiment of the present invention 1 gained sample 1 scavenging solution clean after Sapphire Substrate wafer surface and the surface contact angle survey sheet of water.
Fig. 3 is the Sapphire Substrate wafer surface electron microscope photo scanning of 400 times of the amplifications of cleaning.
Fig. 4 is the Sapphire Substrate wafer surface electron microscope photo scanning that uses 400 times of amplifications after the embodiment of the present invention 1 gained sample 1 scavenging solution cleans.
Embodiment
Below by specific embodiment, the present invention is described in detail; but the purposes of these exemplary embodiments and object are only used for exemplifying the present invention; not real protection scope of the present invention is formed to any type of any restriction, more non-protection scope of the present invention is confined to this.
Embodiment 1
(1), in weight part, take respectively the amine oxide surfactant " n-octyl-6-8 " of 1 weight part, the fluorochemical surfactant C of 0.01 weight part
6f
13cH
2cH
2o (C
2h
4o)
6h (wherein C
6f
13for perfluor n-hexyl), the organic sulfonate novalgin of 1 weight part, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 1 weight part
2o (C
2h
4o)
4(C
3h
6o)
10h (wherein R
2for positive decyl), the alkali Tetramethylammonium hydroxide of 1 weight part, complexing agent ethylenediamine tetraacetic acid (EDTA), the particle capture agent polyvinyl alcohol of 0.5 weight part and the segmented copolymer (CH of polystyrene of 0.5 weight part
2cH (C
6h
5))
20(CH
2cHOH)
100be at least the pure water of 18M Ω with the resistance of 10 weight parts;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 1.
Embodiment 2
(1), in weight part, take respectively the amine oxide surfactant " positive decyl-8-10 " of 5 weight parts, the fluorochemical surfactant C of 1 weight part
8f
17cH
2cH
2o (C
2h
4o)
8h (wherein C
8f
17for perfluor n-octyl), the organic sulfonate paratoluenesulfonic acid sodium salt of 5 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 10 weight parts
2o (C
2h
4o)
6(C
3h
6o)
8h (wherein R
2for dodecyl), the alkali trimethyl benzyl ammonium hydroxide of 3 weight parts, complexing agent triethylenetetraaminehexaacetic acid sodium, the particle capture agent polyacrylic acid (molecular weight 1000) of 2.5 weight parts and the resistance of 40 weight parts of 1 weight part is at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 2.
Embodiment 3
(1), in weight part, take respectively the amine oxide surfactant " dodecyl-10-12 " of 10 weight parts, the fluorochemical surfactant C of 3 weight parts
10f
21cH
2cH
2o (C
2h
4o)
10h (wherein C
10f
21for the positive decyl of perfluor), the organic sulfonate sodium vinyl sulfonate of 10 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 20 weight parts
2o (C
2h
4o)
8(C
3h
6o)
10the alkali trimethyl hydroxyethylammoniumhydroxide hydroxide of H (wherein R2 is n-tetradecane base), 5 weight parts, complexing agent citric acid, the particle capture agent PEG-400 of 5 weight parts and the resistance of 80 weight parts of 2 weight parts are at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 3.
Embodiment 4
(1), in weight part, take respectively the amine oxide surfactant " n-octylcyclam 2-10 " of 8 weight parts, the fluorochemical surfactant C of 0.03 weight part
12f
25cH
2cH
2o (C
2h
4o)
12h (wherein C
12f
25for perfluor dodecyl), the organic sulfonate 2 of 1 weight part, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 4-acid dimethyl sodium, 3 weight parts
2o (C
2h
4o)
10(C
3h
6o)
4h (wherein R
2for n-hexadecyl), the alkali triethylamine of 1.5 weight parts, the complexing agent sodium nitrilo triacetate of 1.5 weight parts, the particle capture agent polymine (CH of 4 weight parts
2cH
2nH)
vthe resistance of (wherein v is 50) and 70 weight parts is at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 4.
Embodiment 5
(1), in weight part, take respectively the amine oxide surfactant " positive decyl-14-12 " of 3 weight parts, the fluorochemical surfactant C of 0.2 weight part
6f
13cH
2cH
2o (C
2h
4o)
12h (wherein C
6f
13for (CF
3)
2cF (CF
2)
3-), the organic sulfonate 4-n-octyl sodium sulfonate of 2.5 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 5 weight parts
2o (C
2h
4o)
12(C
3h
6o)
6h (wherein R
2for Octadecane base), the alkali α-amino isopropyl alcohol of 4.5 weight parts, the complexing agent gluconic acid of 0.7 weight part, the particle capture agent polymine (CH of 0.8 weight part
2cH
2nH)
vthe resistance of (wherein v is 70) and 50 weight parts is at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 5.
Embodiment 6
(1), in weight part, take respectively the amine oxide surfactant " dodecyl-1-8 " of 2 weight parts, the fluorochemical surfactant C of 2.5 weight parts
8f
17cH
2cH
2o (C
2h
4o)
10h (wherein C
8f
17for perfluor n-octyl), the organic sulfonic acid salt pair Sodium dodecylbenzene sulfonate of 6 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 15 weight parts
2o (C
2h
4o)
12(C
3h
6o)
8h (wherein R
2for positive decyl), the alkali TBAH of 2.5 weight parts, the complexing agent potassium ascorbate of 1.7 weight parts, the particle capture agent polymine (CH of 3.5 weight parts
2cH
2nH)
vthe resistance of (wherein v is 100) and 20 weight parts is at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 6.
Embodiment 7
(1), in weight part, take respectively the amine oxide surfactant " n-octyl-6-12 " of 4 weight parts, the fluorochemical surfactant C of 2 weight parts
10f
21cH
2cH
2o (C
2h
4o)
8h (wherein C
10f
21for the positive decyl of perfluor), the organic sulfonate n-propylbenzene sodium sulfonate of 1.5 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 2 weight parts
2o (C
2h
4o)
10(C
3h
6o)
4h (wherein R
2for dodecyl), the alkali diethanolamine of 2 weight parts, complexing agent vitamins C, the particle capture agent polypropylene (its molecular weight is 3000) of 1.5 weight parts and the resistance of 30 weight parts of 0.6 weight part be at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 7.
Embodiment 8
(1), in weight part, take respectively the amine oxide surfactant " n-nonyl-8-8 " of 6 weight parts, the fluorochemical surfactant C of 1.5 weight parts
12f
25cH
2cH
2o (C
2h
4o)
6h (wherein C
12f
25for perfluor dodecyl), the organic sulfonate sodium allyl sulfonate of 9 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 8 weight parts
2o (C
2h
4o)
6(C
3h
6o)
10h (wherein R
2for Octadecane base), the alkali quadrol of 1.2 weight parts, complexing agent Sodium.alpha.-hydroxypropionate, the particle capture agent polypropylene (its molecular weight is 5000) of 4.5 weight parts and the resistance of 60 weight parts of 1.8 weight parts be at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 8.
Embodiment 9
(1), in weight part, take respectively the amine oxide surfactant " positive decyl-1-8 " of 9.5 weight parts, the fluorochemical surfactant C of 3 weight parts
10f
21cH
2cH
2o (C
2h
4o)
6h (wherein C
10f
21for the positive decyl of perfluor), the organic sulfonate Sodium dodecylbenzene sulfonate of 8 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 4 weight parts
2o (C
2h
4o)
8(C
3h
6o)
4h (wherein R
2for n-tetradecane base), the alkali sodium carbonate of 1 weight part, complexing agent oxysuccinic acid, the particle capture agent PEG-800 of 2 weight parts and the resistance of 15 weight parts of 0.5 weight part is at least the pure water of 18M Ω;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 9.
Embodiment 10
(1), in weight part, take respectively the amine oxide surfactant " dodecyl-12-12 " of 10 weight parts, the fluorochemical surfactant C of 0.1 weight part
6f
13cH
2cH
2o (C
2h
4o)
10h (wherein C
6f
13for perfluor n-hexyl), the organic sulfonate ethylsulfonic acid sodium of 7.5 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 16 weight parts
2o (C
2h
4o)
12(C
3h
6o)
6h (wherein R
2for dodecyl), the alkali Starso of 2 weight parts, complexing agent Sorbitol Powder, the particle capture agent polyvinyl alcohol of 3 weight parts and the segmented copolymer (CH of polystyrene of 1.5 weight parts
2cH (C
6h
5))
40(CH
2cHOH)
70be at least the pure water of 18M Ω with the resistance of 75 weight parts;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 10.
Embodiment 11
(1), in weight part, take respectively the amine oxide surfactant " n-octylcyclam 4-8 " of 1.5 weight parts, the fluorochemical surfactant C of 0.5 weight part
8f
17cH
2cH
2o (C
2h
4o)
12h (wherein C
8f
17for perfluor n-octyl), the organic sulfonate sodium isopropyl xanthate of 6 weight parts, the aliphatic alcohol polyethenoxy polyethenoxy ether R of 3.5 weight parts
2o (C
2h
4o)
4(C
3h
6o)
10h (wherein R
2for positive decyl), the alkali potassium hydroxide of 4 weight parts, complexing agent diethylene triaminepentaacetic acid(DTPA) sodium, the particle capture agent polyvinyl alcohol of 1.5 weight parts and the segmented copolymer (CH of polystyrene of 0.8 weight part
2cH (C
6h
5))
80(CH
2cHOH)
30be at least the pure water of 18M Ω with the resistance of 25 weight parts;
(2) pure water of above-mentioned weight part is joined in stirring tank, then add in turn alkali, the complexing agent of above-mentioned weight part, be stirred to homogeneous transparent with the speed of 70rpm/min;
(3) to the organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and the particle capture agent that add in turn weight part described in step (1) in the homogeneous transparent mixture in step (2), speed with 70rpm/min is stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid, by its called after sample 11.
Comparative example 1-11
Except not comprising amine oxide surfactant, to have implemented comparative example 1-11 with the same way of embodiment 1-11, make respectively 11 Sapphire Substrate wafer cleaning liquid respectively, called after comparative sample 1-comparative sample 11, its corresponding relation is as follows:
Comparative example 12-22
Remove respectively by fluorochemical surfactant C
nf
2n+1cH
2cH
2o (C
2h
4o)
yperfluoroalkyl C in H
nf
2n+1replace with C
nf
2n+1outside (replacing all F with H) outward, respectively to have implemented comparative example 12-22 with the same way of embodiment 1-11, make respectively 11 Sapphire Substrate wafer cleaning liquid samples, called after comparative sample 12-comparative sample 22, its corresponding relation is as follows:
Sapphire Substrate wafer cleaning method and testing method
Purging method:
Sapphire Substrate wafer after cutting, grinding, polishing process is carried out in turn to the cleaning of following steps:
(1) Sapphire Substrate wafer is positioned in pure water, at 50 DEG C, uses 40kHz ultrasonic cleaning 5 minutes;
(2) Sapphire Substrate wafer cleaning liquid of the present invention being mixed with to mass concentration is 10% the aqueous solution, then the Sapphire Substrate wafer after step (1) being cleaned is positioned in the described aqueous solution, uses 40kHz ultrasonic cleaning 6 minutes at 50 DEG C;
(3) the Sapphire Substrate wafer after step (2) cleaning is positioned in pure water, at 50 DEG C, uses 40kHz ultrasonic cleaning 6 minutes, repeat this step 3 time;
(4) by step (3) clean after Sapphire Substrate wafer at 90 DEG C, bake drying 10 minutes, obtains the clean Sapphire Substrate wafer after cleaning.
Testing method:
1. the Sapphire Substrate wafer relating in above-mentioned " purging method " is carried out to surface contact angle measurement respectively before cleaning and after cleaning, thereby measure its contact angle to investigate its surface clearness.
Measuring process is that deionized water is dripped to Sapphire Substrate wafer surface, uses contact angle measurement to measure its contact angle.
2. the Sapphire Substrate wafer relating in above-mentioned " purging method " is amplified to 400 times of electron-microscope scannings before cleaning and after cleaning respectively, to observe its surface topography, thereby determine on surface whether have various pollutents.
Test result:
A. according to above-mentioned purging method, use respectively above-described embodiment and comparative example gained sample 1-10, comparative sample 1-20 to clean Sapphire Substrate wafer, then measure its contact angle.
Contact angle data before cleaning and after cleaning see the following form 1.
Contact angle data before table 1. cleans and after cleaning
From table 1, after using Sapphire Substrate wafer cleaning liquid of the present invention to clean, contact angle significantly reduces as for 2.6-3.0 ° by unwashed 35 °, only for cleaning the 7.43-8.57% of first 35 ° (seeing accompanying drawing 1), wherein after embodiment 1 sample 1 cleans, contact angle is reduced to 3 ° (seeing accompanying drawing 2), this proves that Sapphire Substrate wafer contamination thing is after the cleaning of sample 1-11, residual quantity is extremely low, thereby makes water droplet in Sapphire Substrate wafer surface, to be close to and to sprawl completely.
In the time not comprising amine oxide surfactant in scavenging solution, cause Sapphire Substrate wafer surface contact angle significantly to increase to 25.2-29.5 °, this proves that Sapphire Substrate wafer surface still has a large amount of pollutents.
When by fluorochemical surfactant C in scavenging solution
nf
2n+1cH
2cH
2o (C
2h
4o)
yperfluoroalkyl C in H
nf
2n+1replace with C
nf
2n+1after, Sapphire Substrate wafer surface contact angle is 17.4-20.2 °, is less than comparative sample 1-11, this shows to work as perfluoroalkyl C
nf
2n+1replace with C
nf
2n+1time, its cleaning performance will significantly be inferior to sample 1-11, but still is better than comparative sample 1-11.
By upper table data, proved in the time there is amine oxide surfactant and fluorochemical surfactant in scavenging solution simultaneously, although amine oxide surfactant is greater than the impact of fluorochemical surfactant on the impact of cleaning, but can bring into play beyond thought collaborative cleanup action between the two, thereby obtain excellent cleaning performance.
B. as the supplementing of above-mentioned test result A, respectively the Sapphire Substrate wafer before cleaning and after cleaning has been carried out to electron-microscope scanning, thereby observed more intuitively its surface contaminant residual condition.
Accompanying drawing 3 is the Sapphire Substrate wafer surface electron microscope photo scannings (amplifying 400 times) after not cleaning, can find out significantly that Sapphire Substrate wafer topography is inhomogeneous, on it, remain a large amount of pollutents, comprise the pollutent of the different shapes such as greasy dirt, particulate matter, rectangular impurity and character.
Accompanying drawing 4 is the Sapphire Substrate wafer surface electron microscope photo scannings that use after embodiment 1 gained sample 1 cleans, can find out significantly and in Sapphire Substrate wafer surface, not remain pollutent, surface topography is clean, homogeneous, have high cleanliness factor, the amounts of particles that particle diameter is greater than 0.5 μ m in 2 cun of Sapphire Substrate wafer surface is after tested less than 40.After using sample 2-11 to clean, find not remain equally pollutent in Sapphire Substrate wafer surface, surface topography is clean, homogeneous, has high cleanliness factor, and the amounts of particles that in 2 cun of Sapphire Substrate wafer surface, particle diameter is greater than 0.5 μ m is less than 40 equally.
In sum, the invention provides the Sapphire Substrate wafer cleaning liquid of a class novelty, by the selection of specific components, act synergistically and brought into play beyond thought cleaning, obtain excellent cleaning performance, can be used for the surface cleaning of Sapphire Substrate wafer, thereby provide the foundation for the preparation of final precision electronic element.This Sapphire Substrate wafer cleaning pendular ring protects, safe, nontoxic, and cleaning performance is good, has good application prospect and a researching value industrial.
The purposes that should be appreciated that these embodiment only limits the scope of the invention for the present invention being described but not being intended to.In addition; also should understand; after having read technology contents of the present invention, those skilled in the art can make various changes, amendment and/or modification to the present invention, within these all equivalent form of values fall within the protection domain that the application's appended claims limits equally.
Claims (8)
1. a Sapphire Substrate wafer cleaning liquid, described scavenging solution comprises the following various components in weight part:
Described amine oxide surfactant structure is as follows:
Wherein x is the integer between 6-14, and y is the integer between 8-12;
R
1for C
8-C
12straight or branched alkyl;
Described fluorochemical surfactant is perfluoroalkyl oxyethyl group Soxylat A 25-7, and its structural formula is C
mf
2m+1cH
2cH
2o (C
2h
4o)
nh, the aggregate number that wherein n is oxyethane, m and n are all selected from the integer of 6-12.
2. Sapphire Substrate wafer cleaning liquid as claimed in claim 1, is characterized in that:
Described organic sulfonate is methylsulphonic acid, ethylsulfonic acid, n-propyl sulfonic acid, sec.-propyl sulfonic acid, tosic acid, xylene monosulfonic acid, α-olefin sulfonic acid, C
8-C
12the sylvite of any one in alkyl benzene sulphonate (ABS) or sodium salt, or be wherein arbitrarily sylvite and/or the sodium salt of multiple mixture.
3. Sapphire Substrate wafer cleaning liquid as claimed in claim 1, is characterized in that:
The structural formula of described aliphatic alcohol polyethenoxy polyethenoxy ether is
R
2o (C
2h
4o)
p(C
3h
6o)
qh, p and q are respectively the aggregate number of oxyethane and propylene oxide, and wherein p is the integer between 4-12, and q is the integer between 4-10, R
2for C
10-C
18straight or branched alkyl.
4. Sapphire Substrate wafer cleaning liquid as claimed in claim 1, is characterized in that:
Described alkali is organic bases, mineral alkali or both mixtures;
Wherein, described organic bases is any one or the multiple mixture in Tetramethylammonium hydroxide, tetraethyl ammonium hydroxide, four n-propyl ammonium hydroxide, 4-n-butyl ammonium hydroxide, trimethyl benzyl ammonium hydroxide, trimethyl hydroxyethylammoniumhydroxide hydroxide, dimethyl dihydroxy ethyl ammonium hydroxide, diethylamine, triethylamine, quadrol, monoethanolamine, diethanolamine, trolamine, α-amino isopropyl alcohol, diisopropanolamine (DIPA), tri-isopropanolamine;
Described mineral alkali is any one or the multiple mixture in sodium carbonate, salt of wormwood, Sodium Hydrogen Carbonate, potassium bicarbonate, Starso, sodium hydroxide, potassium hydroxide.
5. Sapphire Substrate wafer cleaning liquid as claimed in claim 1, is characterized in that:
Described complexing agent is any one or the multiple mixture in ethylenediamine tetraacetic acid (EDTA), diethylene triaminepentaacetic acid(DTPA), triethylenetetraaminehexaacetic acid, citric acid, vitamins C, phytic acid, nitrilotriacetic acid(NTA), gluconic acid, Sorbitol Powder, Xylitol, lactic acid, oxysuccinic acid, or be any one sylvite or sodium salt wherein, or be multiple sylvite and/or sodium salt arbitrarily wherein.
6. Sapphire Substrate wafer cleaning liquid as claimed in claim 1, is characterized in that:
Any one in segmented copolymer, polyacrylic acid or its salt, polyoxyethylene glycol (PEG) or polymine that described particle capture agent is polyvinyl alcohol and polystyrene or multiple mixture.
7. according to the preparation method of Sapphire Substrate wafer cleaning liquid described in claim 1-6 any one, described preparation method comprises the steps:
(1) take respectively the various components of above-mentioned weight part separately;
(2) pure water is joined in stirring tank, then add in turn alkali, complexing agent, be stirred to homogeneous transparent;
(3) in the homogeneous transparent mixture in step (2), add in turn organic sulfonate, amine oxide surfactant, fluorochemical surfactant, aliphatic alcohol polyethenoxy polyethenoxy ether and particle capture agent, be stirred to homogeneous transparent, obtain described Sapphire Substrate wafer cleaning liquid.
8. a method of cleaning Sapphire Substrate wafer, comprises the steps:
(1) Sapphire Substrate wafer is positioned in pure water to ultrasonic cleaning 2-10 minute;
(2) the Sapphire Substrate wafer cleaning liquid described in claim 1-6 any one is mixed with to the aqueous solution that mass concentration is 1-15%, then the Sapphire Substrate wafer after step (1) being cleaned is positioned in the described aqueous solution, ultrasonic cleaning 3-10 minute;
(3) the Sapphire Substrate wafer after step (2) cleaning is positioned in pure water, ultrasonic cleaning 2-10 minute, repeats this step 2-4 time;
(4) by step (3) clean after Sapphire Substrate wafer at 80-100 DEG C, bake drying 8-12 minute;
Wherein the cleaning temperature in step (1), (2) and (3) is 40-60 DEG C, ultrasonic frequency and is 20-50kHz.
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| CN107164109A (en) * | 2017-03-31 | 2017-09-15 | 吴江创源新材料科技有限公司 | Cleaning fluid and preparation method thereof and cleaning before a kind of sapphire wafer annealing |
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| CN108822987A (en) * | 2018-06-06 | 2018-11-16 | 天通（嘉兴）新材料有限公司 | A kind of novel sapphire cleaning agent |
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| CN111097748A (en) * | 2019-12-27 | 2020-05-05 | 北京理工大学 | A multi-component composite cleaning method after polishing a large-size sapphire window |
| CN111185432B (en) * | 2020-01-14 | 2021-03-19 | 江苏京晶光电科技有限公司 | Cleaning process for replacing acid cleaning of sapphire substrate wafer |
| CN112266832B (en) * | 2020-09-21 | 2021-08-24 | 江苏奥首材料科技有限公司 | Semiconductor chip cleaning agent, preparation method and application |
| CN113416616A (en) * | 2021-07-05 | 2021-09-21 | 东莞市柯林奥环保科技有限公司 | Preparation method of semiconductor environment-friendly cleaning agent |
| CN114425534B (en) * | 2021-12-13 | 2024-04-16 | 金华博蓝特新材料有限公司 | A method for cleaning sapphire substrate after copper polishing |
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