TWI821539B - Polishing composition for alminium nitride substrate and method for polishing alminium nitride substrate - Google Patents
Polishing composition for alminium nitride substrate and method for polishing alminium nitride substrate Download PDFInfo
- Publication number
- TWI821539B TWI821539B TW109107139A TW109107139A TWI821539B TW I821539 B TWI821539 B TW I821539B TW 109107139 A TW109107139 A TW 109107139A TW 109107139 A TW109107139 A TW 109107139A TW I821539 B TWI821539 B TW I821539B
- Authority
- TW
- Taiwan
- Prior art keywords
- acid
- aluminum nitride
- salt
- aliphatic amine
- amine compound
- Prior art date
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- 239000000758 substrate Substances 0.000 title claims abstract description 75
- 239000000203 mixture Substances 0.000 title claims abstract description 66
- 238000005498 polishing Methods 0.000 title claims abstract description 65
- 238000000034 method Methods 0.000 title claims description 18
- 150000004767 nitrides Chemical class 0.000 title 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 66
- -1 aliphatic amine compound Chemical class 0.000 claims abstract description 52
- 150000003839 salts Chemical class 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 35
- 238000000227 grinding Methods 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 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
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 7
- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 claims description 6
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 6
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims description 6
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 6
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 6
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- GVWISOJSERXQBM-UHFFFAOYSA-N n-methylpropan-1-amine Chemical compound CCCNC GVWISOJSERXQBM-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 6
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 claims description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 6
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 6
- XFNJVJPLKCPIBV-UHFFFAOYSA-N trimethylenediamine Chemical compound NCCCN XFNJVJPLKCPIBV-UHFFFAOYSA-N 0.000 claims description 6
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 5
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- ITWBWJFEJCHKSN-UHFFFAOYSA-N 1,4,7-triazonane Chemical compound C1CNCCNCCN1 ITWBWJFEJCHKSN-UHFFFAOYSA-N 0.000 claims description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 3
- LJDSTRZHPWMDPG-UHFFFAOYSA-N 2-(butylamino)ethanol Chemical compound CCCCNCCO LJDSTRZHPWMDPG-UHFFFAOYSA-N 0.000 claims description 3
- MIJDSYMOBYNHOT-UHFFFAOYSA-N 2-(ethylamino)ethanol Chemical compound CCNCCO MIJDSYMOBYNHOT-UHFFFAOYSA-N 0.000 claims description 3
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 3
- MXZROAOUCUVNHX-UHFFFAOYSA-N 2-Aminopropanol Chemical compound CCC(N)O MXZROAOUCUVNHX-UHFFFAOYSA-N 0.000 claims description 3
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 claims description 3
- BQJLEQAXRYBKPQ-UHFFFAOYSA-N 2-amino-2-methylpropane-1,1-diol Chemical compound CC(C)(N)C(O)O BQJLEQAXRYBKPQ-UHFFFAOYSA-N 0.000 claims description 3
- JCBPETKZIGVZRE-UHFFFAOYSA-N 2-aminobutan-1-ol Chemical compound CCC(N)CO JCBPETKZIGVZRE-UHFFFAOYSA-N 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 229920001174 Diethylhydroxylamine Polymers 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 3
- WUGQZFFCHPXWKQ-UHFFFAOYSA-N Propanolamine Chemical compound NCCCO WUGQZFFCHPXWKQ-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 claims description 3
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 3
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- FVCOIAYSJZGECG-UHFFFAOYSA-N diethylhydroxylamine Chemical compound CCN(O)CC FVCOIAYSJZGECG-UHFFFAOYSA-N 0.000 claims description 3
- LVTYICIALWPMFW-UHFFFAOYSA-N diisopropanolamine Chemical compound CC(O)CNCC(C)O LVTYICIALWPMFW-UHFFFAOYSA-N 0.000 claims description 3
- 229940043276 diisopropanolamine Drugs 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000001530 fumaric acid Substances 0.000 claims description 3
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical compound OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 3
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 claims description 3
- SCZVXVGZMZRGRU-UHFFFAOYSA-N n'-ethylethane-1,2-diamine Chemical compound CCNCCN SCZVXVGZMZRGRU-UHFFFAOYSA-N 0.000 claims description 3
- QHJABUZHRJTCAR-UHFFFAOYSA-N n'-methylpropane-1,3-diamine Chemical compound CNCCCN QHJABUZHRJTCAR-UHFFFAOYSA-N 0.000 claims description 3
- XCVNDBIXFPGMIW-UHFFFAOYSA-N n-ethylpropan-1-amine Chemical compound CCCNCC XCVNDBIXFPGMIW-UHFFFAOYSA-N 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 claims description 3
- 239000011975 tartaric acid Substances 0.000 claims description 3
- 235000002906 tartaric acid Nutrition 0.000 claims description 3
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 3
- MRNZSTMRDWRNNR-UHFFFAOYSA-N bis(hexamethylene)triamine Chemical compound NCCCCCCNCCCCCCN MRNZSTMRDWRNNR-UHFFFAOYSA-N 0.000 claims description 2
- TXXWBTOATXBWDR-UHFFFAOYSA-N n,n,n',n'-tetramethylhexane-1,6-diamine Chemical compound CN(C)CCCCCCN(C)C TXXWBTOATXBWDR-UHFFFAOYSA-N 0.000 claims description 2
- IYNGLSRZLOHZJA-UHFFFAOYSA-N 1,4,7-triazabicyclo[5.2.2]undecane Chemical compound C1CN2CCN1CCNCC2 IYNGLSRZLOHZJA-UHFFFAOYSA-N 0.000 claims 1
- HXKKHQJGJAFBHI-UHFFFAOYSA-N 1-aminopropan-2-ol Chemical compound CC(O)CN HXKKHQJGJAFBHI-UHFFFAOYSA-N 0.000 claims 1
- 239000007983 Tris buffer Substances 0.000 claims 1
- 229940102253 isopropanolamine Drugs 0.000 claims 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 27
- 239000006061 abrasive grain Substances 0.000 description 8
- 230000003746 surface roughness Effects 0.000 description 8
- 239000007800 oxidant agent Substances 0.000 description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000007517 polishing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 229910001679 gibbsite Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 229910001648 diaspore Inorganic materials 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- LSHROXHEILXKHM-UHFFFAOYSA-N n'-[2-[2-[2-(2-aminoethylamino)ethylamino]ethylamino]ethyl]ethane-1,2-diamine Chemical compound NCCNCCNCCNCCNCCN LSHROXHEILXKHM-UHFFFAOYSA-N 0.000 description 2
- TWLXDPFBEPBAQB-UHFFFAOYSA-N orthoperiodic acid Chemical compound OI(O)(O)(O)(O)=O TWLXDPFBEPBAQB-UHFFFAOYSA-N 0.000 description 2
- KHIWWQKSHDUIBK-UHFFFAOYSA-N periodic acid Chemical compound OI(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-N 0.000 description 2
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- KHIWWQKSHDUIBK-UHFFFAOYSA-M periodate Chemical compound [O-]I(=O)(=O)=O KHIWWQKSHDUIBK-UHFFFAOYSA-M 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- RKBCYCFRFCNLTO-UHFFFAOYSA-N triisopropylamine Chemical compound CC(C)N(C(C)C)C(C)C RKBCYCFRFCNLTO-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- 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
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Abstract
本發明提供一種以高研磨速度將氮化鋁基板精加工成良好之表面平滑性的氮化鋁基板用研磨劑組合物。氮化鋁基板用研磨劑組合物包含氧化鋁粒子、脂肪族胺化合物、酸及/或其鹽以及水。又，pH值(25℃)為7.5以上且小於11.5。 The present invention provides an abrasive composition for aluminum nitride substrates that can be polished at a high polishing speed to achieve good surface smoothness. The abrasive composition for aluminum nitride substrates contains aluminum oxide particles, an aliphatic amine compound, an acid and/or its salt, and water. Moreover, the pH value (25°C) is 7.5 or more and less than 11.5.
Description
本發明係關於一種可作為以積體電路或積體電路封裝體等材料為代表之各種電子材料使用的陶瓷材料。特別係關於一種用於研磨用以製造半導體元件的氮化鋁單晶基板或作為半導體安裝用之高功能散熱板而普及的氮化鋁多晶基板的研磨劑組合物，其中係關於一種對於有效果地研磨散熱性優異之氮化鋁多晶基板有用的研磨劑組合物。 The present invention relates to a ceramic material that can be used as various electronic materials represented by materials such as integrated circuits or integrated circuit packages. In particular, it relates to an abrasive composition for polishing aluminum nitride single crystal substrates used to manufacture semiconductor elements or aluminum nitride polycrystalline substrates popularized as high-function heat dissipation plates for semiconductor mounting. An abrasive composition useful for effectively polishing aluminum nitride polycrystalline substrates with excellent heat dissipation properties.
氮化鋁的導熱率高，且絕緣性與機械強度優異，因此作為積體電路或積體電路封裝體等的散熱材料而逐漸普及。其中，將以氮化鋁為主要成分之粉末進行燒結而得的氮化鋁多晶體，其絕緣性及機械強度優異，且容易與金屬導體接合，更具有高導熱特性，因此作為半導體安裝用之高功能散熱板而逐漸快速普及。此類散熱基板一般係用以下方法進行製造。 Aluminum nitride has high thermal conductivity and excellent insulation and mechanical strength, so it is gradually becoming popular as a heat dissipation material for integrated circuits, integrated circuit packages, and the like. Among them, aluminum nitride polycrystals obtained by sintering powder with aluminum nitride as the main component have excellent insulation and mechanical strength, are easily bonded to metal conductors, and have high thermal conductivity, so they are used for semiconductor mounting. High-performance heat sinks are becoming increasingly popular. This type of heat dissipation substrate is generally manufactured using the following methods.
將氮化鋁原料粉末與燒結助劑等的添加劑充分混合後，藉由各種成形法進行成形、脫脂、燒製而形成燒結基板。之後，藉由研磨而使燒結基板的表面平滑，再於燒結基板的表面形成金屬薄膜層，並於該金屬薄膜上裝設電子元件(例如雷射二極體)。 After the aluminum nitride raw material powder is thoroughly mixed with additives such as sintering aids, the mixture is formed, degreased, and fired by various molding methods to form a sintered substrate. Thereafter, the surface of the sintered substrate is smoothed by polishing, a metal thin film layer is formed on the surface of the sintered substrate, and electronic components (such as laser diodes) are installed on the metal thin film.
然而，由於近年來電子元件的小型化、高密度化的要求，亦要求裝設電子元件之氮化鋁多晶基板表面的平滑性精度顯著提升。用以使氮化鋁多晶基板的表面平滑的研磨，可藉由使研磨粒的分散液存在於研磨 面，藉由研磨墊將其壓附於研磨面並摩擦而實施。 However, due to the requirements for miniaturization and high density of electronic components in recent years, the smoothness accuracy of the surface of the aluminum nitride polycrystalline substrate on which the electronic components are mounted is also required to be significantly improved. For polishing to smooth the surface of an aluminum nitride polycrystalline substrate, a dispersion of abrasive grains can be present in the polishing surface. The surface is pressed against the polishing surface with a polishing pad and rubbed.
然而，氮化鋁多晶基板的晶界脆弱，因此在一般的研磨加工中，具有在該研磨加工中發生脫粒等而無法達成充分之平滑性的問題。有人提出了在氮化鋁多晶基板的研磨中，一邊提高研磨速度一邊提升表面平滑性的方法(專利文獻1~4)。 However, since the grain boundaries of the aluminum nitride polycrystalline substrate are fragile, there is a problem that degranulation occurs during the general polishing process and sufficient smoothness cannot be achieved. In polishing an aluminum nitride polycrystalline substrate, a method of improving surface smoothness while increasing the polishing speed has been proposed (Patent Documents 1 to 4).
[先前技術文獻] [Prior technical literature]
[專利文獻] [Patent Document]
[專利文獻1]日本特開2006-272506號公報 [Patent Document 1] Japanese Patent Application Publication No. 2006-272506
[專利文獻2]日本特開平4-223852號公報 [Patent Document 2] Japanese Patent Application Publication No. 4-223852
[專利文獻3]日本特開平4-114984號公報 [Patent Document 3] Japanese Patent Application Publication No. 4-114984
[專利文獻4]日本特開2018-159033號公報 [Patent Document 4] Japanese Patent Application Publication No. 2018-159033
專利文獻1中提出了以將特定粒徑之鑽石研磨粒形成特定研磨粒密度(每單位體積的研磨粒量)的固定研磨粒來研磨氮化鋁燒結基板的方法。專利文獻2中提出了以氧化鋁與氧化鉻的複合研磨粒來研磨氮化鋁燒結基板方法。專利文獻3中提出了胺基甲酸酯樹脂製研磨墊與氧化鈰研磨粒的組合來研磨氮化鋁燒結基板的方法。專利文獻4中提出了使用含有氧化鋁粒子、分散劑、酸、氫離子供給劑及水、且pH=0.1~5.0的研磨劑組合物來研磨氮化鋁燒結基板的方法。然而，藉由該等方法亦無法達成以高研磨速度將氮化鋁基板精加工成良好之表面平滑性。 Patent Document 1 proposes a method of polishing an aluminum nitride sintered substrate by using diamond abrasive grains of a specific particle size to form fixed abrasive grains with a specific abrasive grain density (the amount of abrasive grains per unit volume). Patent Document 2 proposes a method of grinding an aluminum nitride sintered substrate using composite abrasive grains of aluminum oxide and chromium oxide. Patent Document 3 proposes a method of polishing an aluminum nitride sintered substrate using a combination of a urethane resin polishing pad and cerium oxide abrasive grains. Patent Document 4 proposes a method of polishing an aluminum nitride sintered substrate using an abrasive composition containing alumina particles, a dispersant, an acid, a hydrogen ion donor, and water and having a pH of 0.1 to 5.0. However, these methods cannot achieve good surface smoothness by finishing the aluminum nitride substrate at a high grinding speed.
本發明之課題係提供一種以高研磨速度將氮化鋁基板精加工成良好之表面平滑性的氮化鋁基板用研磨劑組合物。 An object of the present invention is to provide an abrasive composition for an aluminum nitride substrate that can be used to polish the aluminum nitride substrate at a high polishing speed to achieve good surface smoothness.
本案發明人進行深入研究的結果，發現藉由使用以下研磨劑組合物，可解決上述課題，進而達成本發明。 As a result of intensive research, the inventor of the present invention found that the above problems can be solved by using the following abrasive composition, thereby achieving the present invention.
[1]一種氮化鋁基板用研磨劑組合物，其含有氧化鋁粒子、脂肪族胺化合物、酸及/或其鹽以及水，且pH值(25℃)為7.5以上且小於11.5。 [1] An abrasive composition for aluminum nitride substrates, which contains aluminum oxide particles, an aliphatic amine compound, an acid and/or its salt, and water, and has a pH value (25° C.) of 7.5 or more and less than 11.5.
[2]如[1]之氮化鋁基板用研磨劑組合物，其中該脂肪族胺化合物為具有羥基之脂肪族胺化合物。 [2] The abrasive composition for aluminum nitride substrates according to [1], wherein the aliphatic amine compound is an aliphatic amine compound having a hydroxyl group.
[3]如[1]之氮化鋁基板用研磨劑組合物，其中該脂肪族胺化合物為不具有羥基之脂肪族胺化合物。 [3] The abrasive composition for aluminum nitride substrates according to [1], wherein the aliphatic amine compound is an aliphatic amine compound without a hydroxyl group.
[4]如[1]之氮化鋁基板用研磨劑組合物，其包含各一種以上的具有羥基之脂肪族胺化合物與不具有羥基之脂肪族胺化合物作為該脂肪族胺化合物。 [4] The abrasive composition for aluminum nitride substrates according to [1], which contains at least one aliphatic amine compound having a hydroxyl group and an aliphatic amine compound not having a hydroxyl group as the aliphatic amine compound.
[5]如[2]或[4]之氮化鋁基板用研磨劑組合物，其中該具有羥基之脂肪族胺化合物係選自單乙醇胺、1-胺基丙醇、3-胺基丙醇、2-甲胺基乙醇、2-胺基-1-丁醇、2-胺基-2-甲基-1-丙醇、N,N-二乙基羥基胺、N,N-二甲基乙醇胺、2-乙基胺基乙醇、2-(丁基胺基)乙醇、二乙醇胺、二異丙醇胺、2-胺基-2-甲基丙二醇、N-甲基二乙醇胺、三異丙醇胺、三乙醇胺的至少一者。 [5] The abrasive composition for aluminum nitride substrates according to [2] or [4], wherein the aliphatic amine compound having a hydroxyl group is selected from the group consisting of monoethanolamine, 1-aminopropanol, and 3-aminopropanol. , 2-methylaminoethanol, 2-amino-1-butanol, 2-amino-2-methyl-1-propanol, N,N-diethylhydroxylamine, N,N-dimethyl Ethanolamine, 2-ethylaminoethanol, 2-(butylamino)ethanol, diethanolamine, diisopropanolamine, 2-amino-2-methylpropanediol, N-methyldiethanolamine, triisopropylamine At least one of alcoholamine and triethanolamine.
[6]如[3]或[4]之氮化鋁基板用研磨劑組合物，其中該不具有羥基之脂肪族胺化合物係選自乙胺、正丙胺、異丙胺、正丁胺、異丁胺、二級丁胺、三級丁胺、環己胺、哌嗪(piperazine)、二乙胺、甲基丙胺、乙基丙胺、三乙胺、乙二胺、1,2-丙二胺、三亞甲二胺、四亞甲二胺、五亞甲基二胺、六亞甲基二胺、N,N-二甲基乙二胺、N-乙基乙二胺、N,N,N,N-四甲基乙二胺、N-甲基-1,3-丙二胺、1,3-二胺戊烷、二伸乙三胺、雙(六亞甲基) 三胺、三伸乙三胺、三伸乙四胺、四伸乙五胺、五伸乙六胺、四甲基六亞甲基二胺的至少一者。 [6] The abrasive composition for aluminum nitride substrates according to [3] or [4], wherein the aliphatic amine compound without a hydroxyl group is selected from the group consisting of ethylamine, n-propylamine, isopropylamine, n-butylamine, and isobutylamine. Amine, secondary butylamine, tertiary butylamine, cyclohexylamine, piperazine, diethylamine, methylpropylamine, ethylpropylamine, triethylamine, ethylenediamine, 1,2-propanediamine, Trimethylenediamine, tetramethylenediamine, pentamethylenediamine, hexamethylenediamine, N,N-dimethylethylenediamine, N-ethylethylenediamine, N,N,N, N-tetramethylethylenediamine, N-methyl-1,3-propanediamine, 1,3-diaminepentane, diethylenetriamine, bis(hexamethylene) At least one of triamine, triethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, and tetramethylhexamethylenediamine.
[7]如[1]至[6]中任一項之氮化鋁基板用研磨劑組合物，其中該酸及/或其鹽係選自無機酸及/或其鹽、有機酸及/或其鹽之中的至少1種。 [7] The abrasive composition for aluminum nitride substrates according to any one of [1] to [6], wherein the acid and/or its salt is selected from the group consisting of inorganic acid and/or its salt, organic acid and/or At least 1 of its salts.
[8]如[7]之氮化鋁基板用研磨劑組合物，其中該酸及/或其鹽為無機酸及/或其鹽，其係選自由硝酸、硫酸、鹽酸、磷酸及/或其鹽所構成之群組的至少一者。 [8] The abrasive composition for aluminum nitride substrates according to [7], wherein the acid and/or its salt is an inorganic acid and/or its salt, which is selected from the group consisting of nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid and/or its salts. At least one member of the group consisting of salt.
[9]如該[7]之氮化鋁基板用研磨劑組合物，其中該酸及/或其鹽為有機酸及/或其鹽，其係選自由草酸、蘋果酸、檸檬酸、甲酸、乙酸、琥珀酸、丙二酸、己二酸、癸二酸、富馬酸、馬來酸、酒石酸、丙酸、乳酸及/或其鹽所構成之群組的至少一者。 [9] The abrasive composition for aluminum nitride substrates of [7], wherein the acid and/or its salt is an organic acid and/or its salt, which is selected from the group consisting of oxalic acid, malic acid, citric acid, formic acid, At least one of the group consisting of acetic acid, succinic acid, malonic acid, adipic acid, sebacic acid, fumaric acid, maleic acid, tartaric acid, propionic acid, lactic acid and/or salts thereof.
[10]如[1]至[9]中任一項之氮化鋁基板用研磨劑組合物，其中該研磨劑組合物的pH值(25℃)為8.5以上且小於10.5。 [10] The abrasive composition for aluminum nitride substrates according to any one of [1] to [9], wherein the pH value (25° C.) of the abrasive composition is 8.5 or more and less than 10.5.
[11]如[1]至[10]中任一項之氮化鋁基板用研磨劑組合物，其係氮化鋁多晶基板用研磨劑組合物。 [11] The abrasive composition for aluminum nitride substrates according to any one of [1] to [10], which is an abrasive composition for aluminum nitride polycrystalline substrates.
[12]一種氮化鋁基板之研磨方法，其係以循環供給方式使用如[1]至[10]中任一項之研磨劑組合物來研磨氮化鋁基板。 [12] A method for polishing an aluminum nitride substrate, which uses the abrasive composition according to any one of [1] to [10] in a circulating supply manner to polish the aluminum nitride substrate.
[13]一種氮化鋁多晶基板之研磨方法，其係以循環供給方式使用如[11]之研磨劑組合物來研磨氮化鋁多晶基板。 [13] A method for polishing an aluminum nitride polycrystalline substrate, which uses the abrasive composition of [11] in a circulating supply manner to polish the aluminum nitride polycrystalline substrate.
本發明之氮化鋁基板用研磨劑組合物可提升研磨速度，且提升研磨後的表面平滑性。 The abrasive composition for aluminum nitride substrates of the present invention can increase the polishing speed and improve the surface smoothness after polishing.
以下，對本發明之實施形態進行說明。本發明並不限定於以下實施形態，在不脫離申請專利範圍的範圍內，可加以變更、修正、改良。 Hereinafter, embodiments of the present invention will be described. The present invention is not limited to the following embodiments, and changes, corrections, and improvements can be made without departing from the scope of the patent application.
1.研磨劑組合物 1. Abrasive composition
本發明之氮化鋁基板用研磨劑組合物包含氧化鋁粒子、脂肪族胺化合物、酸及/或其鹽以及水。又，pH值(25℃)為7.5以上且小於11.5。 The abrasive composition for aluminum nitride substrates of the present invention contains aluminum oxide particles, an aliphatic amine compound, an acid and/or its salt, and water. Moreover, the pH value (25°C) is 7.5 or more and less than 11.5.
(1)氧化鋁粒子 (1)Alumina particles
本發明所使用之氧化鋁粒子可為α-氧化鋁，亦可為中間氧化鋁，亦可為α-氧化鋁與中間氧化鋁的混合物。作為中間氧化鋁，可列舉：γ-氧化鋁、δ-氧化鋁、θ-氧化鋁等。在研磨氮化鋁基板時，從盡量提高研磨速度的觀點來看，較佳為使用α-氧化鋁。 The alumina particles used in the present invention may be α-alumina, intermediate alumina, or a mixture of α-alumina and intermediate alumina. Examples of intermediate alumina include γ-alumina, δ-alumina, θ-alumina, and the like. When polishing an aluminum nitride substrate, it is preferable to use α-alumina from the viewpoint of increasing the polishing speed as much as possible.
作為製造氧化鋁時的原料，可列舉：三水鋁石：Al2O3．3H2O、水鋁石：Al2O3．H2O、擬水鋁石：Al2O3．nH2O(n=1~2)等。該等氧化鋁原料例如係用以下方法製備。 Examples of raw materials for producing alumina include: gibbsite: Al 2 O 3 . 3H 2 O, diaspore: Al 2 O 3 ． H 2 O, pseudodiaspore: Al 2 O 3 . nH 2 O(n=1~2) etc. These alumina raw materials are prepared by the following method, for example.
三水鋁石：Al2O3．3H2O Gibbsite: Al 2 O 3 . 3H 2 O
藉由使鋁礬土在氫氧化鈉的熱溶液中溶解，將利用過濾去除雜質成分而得的溶液進行冷卻，並將結果所得之沉澱物進行乾燥而得。 It is obtained by dissolving bauxite in a hot solution of sodium hydroxide, cooling the solution obtained by removing impurity components by filtration, and drying the resulting precipitate.
水鋁石：Al2O3．H2O Diaspore: Al 2 O 3 . H 2 O
藉由將由金屬鋁與醇的反應而得的烷氧化鋁：Al(OR)3進行水解而得。 It is obtained by hydrolyzing aluminum alkoxide: Al(OR) 3 , which is obtained by the reaction of metallic aluminum and alcohol.
擬水鋁石：Al2O3．nH2O(n=1~2) Pseudodiaspore: Al 2 O 3 . nH 2 O(n=1~2)
將三水鋁石在鹼性氣體環境下、水蒸氣下進行處理而得。 It is obtained by treating gibbsite in an alkaline gas environment and water vapor.
藉由將該等氧化鋁原料進行燒製，而得到α-氧化鋁、γ-氧化鋁、δ-氧化鋁、θ-氧化鋁等。 By firing these alumina raw materials, α-alumina, γ-alumina, δ-alumina, θ-alumina, etc. are obtained.
氧化鋁粒子的平均粒徑(D50)較佳為0.1~10.0μm，更佳為 0.1~5.0μm，再佳為0.2~2.0μm。藉由使平均粒徑為0.1μm以上，可抑制研磨速度降低。藉由使平均粒徑為10.0μm以下，可抑制研磨後的基板表面平滑性變差。 The average particle size (D50) of the alumina particles is preferably 0.1~10.0μm, more preferably 0.1~5.0μm, preferably 0.2~2.0μm. By setting the average particle diameter to 0.1 μm or more, a decrease in the polishing speed can be suppressed. By setting the average particle diameter to 10.0 μm or less, deterioration in smoothness of the substrate surface after polishing can be suppressed.
研磨劑組合物中的氧化鋁粒子的濃度較佳為1~50質量%，更佳為2~45質量%，再佳為3~40質量%。若氧化鋁粒子的濃度少於1質量%，則無法得到充分的研磨速度，即使多於50質量%也未觀察到研磨速度更高，而不經濟。 The concentration of alumina particles in the abrasive composition is preferably 1 to 50 mass%, more preferably 2 to 45 mass%, and still more preferably 3 to 40 mass%. If the concentration of alumina particles is less than 1% by mass, a sufficient polishing speed cannot be obtained, and even if it exceeds 50% by mass, a higher polishing speed is not observed, which is uneconomical.
又，作為氧化鋁粒子的分散劑，可列舉：氧化鋁溶膠、纖維素類、多羧酸(鹽)、包含多羧酸之重複單元的共聚物及縮合磷酸鹽等。 Examples of dispersants for alumina particles include alumina sol, cellulose, polycarboxylic acid (salt), copolymers containing repeating units of polycarboxylic acid, condensed phosphates, and the like.
(2)脂肪族胺化合物 (2) Aliphatic amine compounds
本發明之研磨劑組合物含有脂肪族胺化合物。具體而言，可列舉具有羥基之脂肪族胺化合物及不具有羥基之脂肪族胺化合物。 The abrasive composition of the present invention contains an aliphatic amine compound. Specific examples include aliphatic amine compounds having a hydroxyl group and aliphatic amine compounds not having a hydroxyl group.
作為具有羥基之脂肪族胺化合物的具體例，可列舉：單乙醇胺、1-胺基丙醇、3-胺基丙醇、2-甲胺基乙醇、2-胺基-1-丁醇、2-胺基-2-甲基-1-丙醇、N,N-二乙基羥基胺、N,N-二甲基乙醇胺、2-乙基胺基乙醇、2-(丁基胺基)乙醇、二乙醇胺、二異丙醇胺、2-胺基-2-甲基丙二醇、N-甲基二乙醇胺、三異丙醇胺、三乙醇胺等。 Specific examples of the aliphatic amine compound having a hydroxyl group include monoethanolamine, 1-aminopropanol, 3-aminopropanol, 2-methylaminoethanol, 2-amino-1-butanol, 2 -Amino-2-methyl-1-propanol, N,N-diethylhydroxylamine, N,N-dimethylethanolamine, 2-ethylaminoethanol, 2-(butylamino)ethanol , diethanolamine, diisopropanolamine, 2-amino-2-methylpropanediol, N-methyldiethanolamine, triisopropanolamine, triethanolamine, etc.
作為不具有羥基之脂肪族胺化合物的具體例，可列舉：乙胺、正丙胺、異丙胺、正丁胺、異丁胺、二級丁胺、三級丁胺、環己胺、哌嗪、二乙胺、甲基丙胺、乙基丙胺、三乙胺、乙二胺、1,2-丙二胺、三亞甲二胺、四亞甲二胺、五亞甲基二胺、六亞甲基二胺、N,N-二甲基乙二胺、N-乙基乙二胺、N,N,N,N-四甲基乙二胺、N-甲基-1,3-丙二胺、1,3-二胺戊烷、二伸乙三胺、雙(六亞甲基)三胺、三伸乙三胺、三伸乙四胺、四伸乙五胺、五伸乙六胺、四甲基六亞甲基二胺等。 Specific examples of the aliphatic amine compound having no hydroxyl group include: ethylamine, n-propylamine, isopropylamine, n-butylamine, isobutylamine, secondary butylamine, tertiary butylamine, cyclohexylamine, piperazine, Diethylamine, methylpropylamine, ethylpropylamine, triethylamine, ethylenediamine, 1,2-propanediamine, trimethylenediamine, tetramethylenediamine, pentamethylenediamine, hexamethylenediamine Diamine, N,N-dimethylethylenediamine, N-ethylethylenediamine, N,N,N,N-tetramethylethylenediamine, N-methyl-1,3-propanediamine, 1,3-diaminepentane, diethylenetriamine, bis(hexamethylene)triamine, triethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, tetraethylene Methylhexamethylenediamine, etc.
具有羥基之脂肪族胺化合物及不具有羥基之脂肪族胺化合物可分別單獨使用，亦可併用具有羥基之脂肪族胺化合物與不具有羥基之脂肪族胺化合物。若包含具有羥基之脂肪族胺化合物或不具有羥基之脂肪族胺化合物，則基板的表面粗糙度改善。若併用具有羥基之脂肪族胺化合物與不具有羥基之脂肪族胺化合物，則除了基板的表面粗糙度改善以外，研磨速度也會提升。亦即，較佳為研磨劑組合物中包含各一種以上的具有羥基之脂肪族胺化合物與不具有羥基之脂肪族胺化合物。作為併用具有羥基之脂肪族胺化合物與不具有羥基之脂肪族胺化合物時的具體例，可舉例如：併用二乙醇胺與二乙胺、併用三乙醇胺與二乙胺等。 The aliphatic amine compound having a hydroxyl group and the aliphatic amine compound not having a hydroxyl group may be used alone, or the aliphatic amine compound having a hydroxyl group and the aliphatic amine compound not having a hydroxyl group may be used in combination. If an aliphatic amine compound having a hydroxyl group or an aliphatic amine compound having no hydroxyl group is included, the surface roughness of the substrate will be improved. When an aliphatic amine compound having a hydroxyl group and an aliphatic amine compound not having a hydroxyl group are used together, the surface roughness of the substrate is improved and the polishing speed is also increased. That is, it is preferable that the abrasive composition contains at least one aliphatic amine compound having a hydroxyl group and an aliphatic amine compound not having a hydroxyl group. Specific examples of the combined use of an aliphatic amine compound having a hydroxyl group and an aliphatic amine compound not having a hydroxyl group include the combined use of diethanolamine and diethylamine, the combined use of triethanolamine and diethylamine, and the like.
併用具有羥基之脂肪族胺化合物與不具有羥基之脂肪族胺化合物時，相對於全部脂肪族胺化合物的添加量，具有羥基之脂肪族胺化合物的比例較佳為10~90質量%，不具有羥基之脂肪族胺化合物的比例較佳為10~90質量%。 When an aliphatic amine compound having a hydroxyl group and an aliphatic amine compound not having a hydroxyl group are used in combination, the proportion of the aliphatic amine compound having a hydroxyl group is preferably 10 to 90% by mass relative to the added amount of the entire aliphatic amine compound. The ratio of the hydroxyl group to the aliphatic amine compound is preferably 10 to 90% by mass.
研磨劑組合物中的脂肪族胺化合物的含量通常為0.00001~4.0質量%，較佳為0.0001~2.0質量%。 The content of the aliphatic amine compound in the abrasive composition is usually 0.00001 to 4.0 mass%, preferably 0.0001 to 2.0 mass%.
(3)酸及/或其鹽 (3)Acid and/or its salt
本發明所使用之酸及/或其鹽係選自無機酸及/或其鹽、有機酸及/或其鹽之中的至少一者。 The acid and/or its salt used in the present invention is at least one selected from the group consisting of inorganic acid and/or its salt, organic acid and/or its salt.
作為無機酸及/或其鹽，可列舉：硝酸、硫酸、鹽酸、氫氟酸、磷酸、膦酸、碳酸及/或其鹽等，但其中較佳為硝酸、硫酸、鹽酸、磷酸及/或其鹽。作為鹽的種類，可列舉：銨鹽、鈉鹽、鉀鹽等。 Examples of inorganic acids and/or salts thereof include nitric acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, phosphoric acid, phosphonic acid, carbonic acid and/or salts thereof, and among them, nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid and/or salts thereof are preferred. Its salt. Examples of the salt include ammonium salt, sodium salt, potassium salt, and the like.
作為有機酸及/或其鹽，可列舉：草酸、蘋果酸、檸檬酸、甲酸、乙酸、琥珀酸、丙二酸、己二酸、癸二酸、富馬酸、馬來酸、酒石酸、丙酸、乳酸及/或其鹽等。作為鹽的種類，可列舉：銨鹽、鈉鹽、鉀鹽等。 多酸(polyacid)的情況下，亦可為部分鹽。 Examples of organic acids and/or salts thereof include: oxalic acid, malic acid, citric acid, formic acid, acetic acid, succinic acid, malonic acid, adipic acid, sebacic acid, fumaric acid, maleic acid, tartaric acid, and propionic acid. Acid, lactic acid and/or its salts, etc. Examples of the salt include ammonium salt, sodium salt, potassium salt, and the like. In the case of polyacid, it may be a partial salt.
研磨劑組合物中的酸及/或其鹽的含量，可因應pH值(25℃)的設定而適當決定。 The content of the acid and/or its salt in the abrasive composition can be appropriately determined according to the setting of the pH value (25°C).
(4)氧化劑 (4) Oxidizing agent
本發明之研磨劑組合物可包含氧化劑作為任意成分。作為氧化劑，可列舉：過氧化氫、過碘酸系氧化劑、過錳酸系氧化劑、過金屬酸系氧化劑等。作為具體例，可列舉：過氧化氫、正過碘酸、正過碘酸鹽、偏過碘酸、偏過碘酸鹽、過錳酸、過錳酸鹽、過金屬酸、過金屬酸鹽等。作為更具體的例子，可列舉：過氧化氫、正過碘酸、偏過碘酸鈉、過錳酸鉀、過鉬酸、過鉬酸鈉等。 The abrasive composition of the present invention may contain an oxidizing agent as an optional ingredient. Examples of the oxidizing agent include hydrogen peroxide, periodic acid-based oxidizing agent, permanganic acid-based oxidizing agent, permetallic acid-based oxidizing agent, and the like. Specific examples include hydrogen peroxide, orthoperiodic acid, orthoperiodate, metaperiodic acid, metaperiodate, permanganic acid, permanganate, permetallic acid, and permetallate. wait. More specific examples include hydrogen peroxide, orthoperiodic acid, sodium metaperiodate, potassium permanganate, permolybdic acid, sodium permolybdate, and the like.
研磨劑組合物中的氧化劑的含量，較佳在0.1~10.0質量%的範圍，再佳在0.2~8.0質量%的範圍。 The content of the oxidizing agent in the abrasive composition is preferably in the range of 0.1 to 10.0 mass%, and more preferably in the range of 0.2 to 8.0 mass%.
(5)水 (5)Water
本發明所使用的水，較佳為使用蒸餾水、離子交換水等去除雜質的水。若考量研磨後的清洗性，較佳為離子交換水。水具有控制研磨劑之流動性的功能，故其含量可對應研磨速度等的目標研磨特性而適當設定。例如，水的含有比例較佳為研磨劑組合物的40~90質量%。若水的含量少於研磨劑組合物的40質量%，則研磨劑的黏性變高，而可能損及流動性。另一方面，若水的含量超過90質量%，則研磨粒濃度變低，而可能無法得到充分的研磨速度。 The water used in the present invention is preferably water from which impurities have been removed using distilled water, ion-exchanged water, or the like. If cleaning ability after grinding is considered, ion-exchange water is preferred. Water has the function of controlling the fluidity of the abrasive, so its content can be appropriately set according to the target polishing characteristics such as polishing speed. For example, the content ratio of water is preferably 40 to 90% by mass of the abrasive composition. If the water content is less than 40% by mass of the abrasive composition, the viscosity of the abrasive becomes high, which may impair fluidity. On the other hand, if the water content exceeds 90 mass %, the abrasive grain concentration becomes low, and a sufficient polishing speed may not be obtained.
(6)pH (6)pH
本發明之研磨劑組合物的pH值(25℃)為7.5以上小於11.5，較佳為8.5以上且小於10.5。若pH值(25℃)小於7.5，則研磨速度變得不充分，而生產性降低。若pH值(25℃)為11.5以上，則研磨後的氮化鋁基板表面的平滑性 變差。研磨劑組合物的pH值(25℃)可藉由調整脂肪族胺化合物的含量、酸及/或其鹽的含量而適當設定。 The pH value (25°C) of the abrasive composition of the present invention is 7.5 or more and less than 11.5, preferably 8.5 or more and less than 10.5. If the pH value (25° C.) is less than 7.5, the polishing speed becomes insufficient and productivity decreases. If the pH value (25°C) is above 11.5, the smoothness of the surface of the polished aluminum nitride substrate will get worse. The pH value (25° C.) of the abrasive composition can be appropriately set by adjusting the content of the aliphatic amine compound, the acid and/or its salt.
(7)研磨劑組合物的製備方法 (7) Preparation method of abrasive composition
本發明之研磨劑組合物可藉由以習知的方法將各成分混合而製備。從經濟性的觀點來看，研磨劑組合物通常係作為濃縮液而製造，使用其時大多進行稀釋。研磨劑組合物可直接使用，若為濃縮液，只要稀釋使用即可。稀釋濃縮液時，其稀釋倍率並無特別限制，可因應濃縮液中各成分的濃度及研磨條件而適當決定。此外，上述各成分的含量係使用時的含量。 The abrasive composition of the present invention can be prepared by mixing the ingredients by a conventional method. From an economical point of view, abrasive compositions are usually produced as concentrated solutions, and are often diluted when used. The abrasive composition can be used directly. If it is a concentrated solution, it can be used as long as it is diluted. When diluting the concentrated solution, the dilution ratio is not particularly limited and can be appropriately determined according to the concentration of each component in the concentrated solution and the grinding conditions. In addition, the content of each component mentioned above is the content at the time of use.
2.氮化鋁基板之研磨方法 2. Polishing method of aluminum nitride substrate
使用本發明之研磨劑組合物來研磨氮化鋁基板的裝置並無特別限制，可使用具備保持氮化鋁基板之夾具(載具)及研磨墊的研磨機，亦可為雙面研磨機及單面研磨機的任一者。 The device for polishing the aluminum nitride substrate using the abrasive composition of the present invention is not particularly limited. A polishing machine equipped with a fixture (carrier) for holding the aluminum nitride substrate and a polishing pad can be used, or a double-sided polisher and a polishing pad can be used. Either single side grinder.
研磨墊並無特別限制，可使用以往習知者。作為研磨墊的材質，可舉例如聚胺基甲酸酯等。研磨墊的形狀較佳為使用例如不織布狀者、麂皮絨狀者等。 The polishing pad is not particularly limited, and those known in the art can be used. Examples of the material of the polishing pad include polyurethane. As the shape of the polishing pad, it is preferable to use, for example, a non-woven fabric shape, a suede shape, etc.
將本發明之研磨劑組合物供給至研磨機的方法，可使用在預先將研磨劑組合物的構成成分充分混合的狀態下以泵等供給至研磨墊與氮化鋁基板之間的方法；在即將研磨前的供給線內等將構成成分混合而供給的方法等。從提升研磨速度的觀點及減輕研磨機負載的觀點來看，較佳為使用在預先將研磨劑組合物的構成成分充分混合的狀態下，利用泵等以循環供給方式將研磨劑組合物供給至研磨墊與氮化鋁基板之間的方法。此外，上述研磨方法中，作為氮化鋁基板，氮化鋁單晶基板、氮化鋁多晶基板之任一者皆可研磨。 The method of supplying the polishing compound composition of the present invention to the polishing machine can be a method of supplying the polishing compound composition between the polishing pad and the aluminum nitride substrate with a pump or the like in a state where the components of the polishing compound composition are thoroughly mixed in advance; Methods such as mixing and supplying the constituent components in a supply line immediately before grinding. From the viewpoint of increasing the polishing speed and reducing the load on the grinder, it is preferable to use a state where the constituent components of the polishing composition are thoroughly mixed in advance, and the polishing composition is supplied in a circulating supply manner using a pump or the like. Method between polishing pad and aluminum nitride substrate. In addition, in the above polishing method, as the aluminum nitride substrate, any one of an aluminum nitride single crystal substrate and an aluminum nitride polycrystalline substrate can be polished.
[實施例] [Example]
以下，根據實施例進一步詳細說明本發明，但本發明並不限定於該等實施例。 Hereinafter, the present invention will be described in further detail based on examples, but the present invention is not limited to these examples.
[研磨劑組合物的製備方法] [Preparation method of abrasive composition]
實施例1~11及比較例1~3所使用的研磨劑組合物，係以表1所記載之含量包含表1所記載之材料的研磨劑組合物。使用該等研磨劑組合物進行研磨試驗的結果顯示於表2。 The abrasive compositions used in Examples 1 to 11 and Comparative Examples 1 to 3 contain the materials described in Table 1 in the contents described in Table 1. The results of the polishing test using these abrasive compositions are shown in Table 2.
表1
[氧化鋁粒子的平均粒徑] [Average particle size of alumina particles]
本發明所使用之氧化鋁粒子的平均粒徑係使用雷射繞射式粒度分布測量裝置(島津製作所股份有限公司製，SALD2200)所測量。氧化鋁粒子的平均粒徑係以體積為基準而從小粒徑側開始的累積粒徑分布成為50%的平均粒徑(D50)。 The average particle diameter of the alumina particles used in the present invention was measured using a laser diffraction particle size distribution measuring device (manufactured by Shimadzu Corporation, SALD2200). The average particle diameter of the alumina particles is an average particle diameter (D50) at which the cumulative particle diameter distribution from the small particle diameter side becomes 50% based on the volume.
[研磨條件] [Grinding conditions]
進行研磨試驗時的研磨條件顯示如下。 The polishing conditions when performing the polishing test are shown below.
研磨加工機 不二越機械工業股份有限公司製，SLM-100(單面研磨機) Grinding machine Made by Fujikoshi Machinery Co., Ltd., SLM-100 (single-sided grinding machine)
壓板直徑 350mm Pressure plate diameter 350mm
研磨對象物 MARUWA Co.,Ltd.製，多晶氮化鋁2inch基板 Polishing object: Made by MARUWA Co., Ltd., polycrystalline aluminum nitride 2-inch substrate
研磨墊 SUBA800 Polishing pad SUBA800
研磨壓力 350gf/cm2 Grinding pressure 350gf/cm 2
壓板旋轉數 60rpm Pressure plate rotation speed 60rpm
研磨劑供給速度 200ml/min(循環供給方式) Abrasive supply speed 200ml/min (circulation supply method)
研磨時間 2hr Grinding time 2hr
[研磨速度的算出方法] [How to calculate grinding speed]
研磨速度(μm/hr)=[氮化鋁多晶基板的研磨前重量(g)-氮化鋁多晶基板的研磨後重量(g)]÷氮化鋁多晶基板的研磨面積(cm2)÷氮化鋁多晶基板的密度(g/cm3)÷研磨時間(min)×1000(μm/cm)×60(min/hr) Polishing speed (μm/hr) = [weight of aluminum nitride polycrystalline substrate before polishing (g) - weight of aluminum nitride polycrystalline substrate after polishing (g)] ÷ polishing area of aluminum nitride polycrystalline substrate (cm 2 )÷density of aluminum nitride polycrystalline substrate (g/cm 3 )÷polishing time (min) × 1000 (μm/cm) × 60 (min/hr)
[氮化鋁多晶基板的表面粗糙度(Sa)] [Surface roughness (Sa) of aluminum nitride polycrystalline substrate]
表面粗糙度(Sa)係使用OLYMPUS公司製的3D測量雷射顯微鏡所測量。測量條件係使用OLYMPUS公司製的測量裝置(OLS4100(測量倍率2160倍))，無截止值(cutoff)，測量區域為128μm×128μm。 Surface roughness (Sa) was measured using a 3D measurement laser microscope manufactured by OLYMPUS Corporation. The measurement conditions used a measurement device (OLS4100 (measurement magnification: 2160 times)) manufactured by OLYMPUS Corporation, with no cutoff and a measurement area of 128 μm × 128 μm.
表2
[研究] [Research]
實施例1~4係使用含有不具有羥基之脂肪族胺化合物作為脂肪族胺化合物的研磨劑組合物的實驗例，相較於使用不含脂肪族胺化合物之研磨劑組合物的比較例1，其表面粗糙度(Sa)改善。 Examples 1 to 4 are experimental examples using a polishing composition containing an aliphatic amine compound that does not have a hydroxyl group as the aliphatic amine compound. Compared with Comparative Example 1 using a polishing composition that does not contain an aliphatic amine compound, Its surface roughness (Sa) is improved.
實施例5與6係使用含有具有羥基之脂肪族胺化合物作為脂肪族胺化合物的研磨劑組合物的實驗例，相較於比較例1，其表面粗糙度(Sa)改善。 Examples 5 and 6 are experimental examples using a polishing composition containing an aliphatic amine compound having a hydroxyl group as the aliphatic amine compound. Compared with Comparative Example 1, the surface roughness (Sa) was improved.
實施例7~9係併用不具有羥基之脂肪族胺化合物與具有羥基之脂肪族胺化合物的實驗例，相較於僅使用不具有羥基之脂肪族胺化合物的實施例1，其研磨速度提升。 Examples 7 to 9 are experimental examples in which an aliphatic amine compound without a hydroxyl group and an aliphatic amine compound with a hydroxyl group are used in combination. Compared with Example 1 in which only an aliphatic amine compound without a hydroxyl group is used, the grinding speed is increased.
由實施例10與比較例2的對比可知，藉由使研磨劑組合物的pH(25℃)為7.5以上，研磨速度變高。由實施例11與比較例3的對比可知，藉由使研磨劑組合物的pH(25℃)小於11.5，表面粗糙度(Sa)降低。 From the comparison between Example 10 and Comparative Example 2, it can be seen that by setting the pH (25° C.) of the polishing composition to 7.5 or more, the polishing rate becomes higher. From the comparison between Example 11 and Comparative Example 3, it can be seen that the surface roughness (Sa) is reduced by making the pH (25° C.) of the abrasive composition less than 11.5.
由以上明確可知，藉由使用本申請發明的研磨劑組合物，研磨速度、研磨後的多晶基板表面粗糙度(Sa)的平衡提升。 From the above, it is clear that by using the abrasive composition of the present invention, the balance between the polishing speed and the surface roughness (Sa) of the polycrystalline substrate after polishing is improved.
[產業上的可利用性] [Industrial availability]
本申請案發明的研磨劑組合物，可用於製造作為以積體電路或積體電路封裝體為代表之各種電子材料的散熱基板使用的氮化鋁多晶基板。又，亦可將作為用以製造半導體元件之基板材料使用的氮化鋁單晶基板用於表面處理，以形成適合磊晶成長之基板表面。 The abrasive composition of the present invention can be used to produce aluminum nitride polycrystalline substrates used as heat dissipation substrates for various electronic materials represented by integrated circuits or integrated circuit packages. In addition, an aluminum nitride single crystal substrate used as a substrate material for manufacturing semiconductor elements can also be used for surface treatment to form a substrate surface suitable for epitaxial growth.
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| CN101454121A (en) * | 2006-05-31 | 2009-06-10 | 旭硝子株式会社 | Polishing composition and polishing method |
| TW201704442A (en) * | 2015-05-19 | 2017-02-01 | Showa Denko Kk | Polishing composition and polishing method using the same which is excellent in dissolution stability and capable of polishing at a high polishing rate and aplied to especially a high hardened and high brittle substrate |
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| US5962343A (en) * | 1996-07-30 | 1999-10-05 | Nissan Chemical Industries, Ltd. | Process for producing crystalline ceric oxide particles and abrasive |
| JP2002020732A (en) * | 2000-07-05 | 2002-01-23 | Showa Denko Kk | Polishing composition |
| JP5657247B2 (en) * | 2009-12-25 | 2015-01-21 | 花王株式会社 | Polishing liquid composition |
| JP6756460B2 (en) | 2014-12-26 | 2020-09-16 | 株式会社フジミインコーポレーテッド | Polishing method and manufacturing method of ceramic parts |
| WO2018123875A1 (en) | 2016-12-26 | 2018-07-05 | 株式会社フジミインコーポレーテッド | Polishing composition and polishing method |
| JP6861063B2 (en) * | 2017-03-23 | 2021-04-21 | 山口精研工業株式会社 | Abrasive composition for aluminum nitride polycrystalline substrate and method for polishing aluminum nitride polycrystalline substrate |
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| CN101454121A (en) * | 2006-05-31 | 2009-06-10 | 旭硝子株式会社 | Polishing composition and polishing method |
| TW201704442A (en) * | 2015-05-19 | 2017-02-01 | Showa Denko Kk | Polishing composition and polishing method using the same which is excellent in dissolution stability and capable of polishing at a high polishing rate and aplied to especially a high hardened and high brittle substrate |
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| CN111793467B (en) | 2022-07-12 |
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