JP2008260105A - Composition for polishing and polishing method - Google Patents
Composition for polishing and polishing method Download PDFInfo
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- JP2008260105A JP2008260105A JP2007105830A JP2007105830A JP2008260105A JP 2008260105 A JP2008260105 A JP 2008260105A JP 2007105830 A JP2007105830 A JP 2007105830A JP 2007105830 A JP2007105830 A JP 2007105830A JP 2008260105 A JP2008260105 A JP 2008260105A
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- 238000005498 polishing Methods 0.000 title claims abstract description 224
- 239000000203 mixture Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title claims abstract description 7
- -1 alkali metal salts Chemical class 0.000 claims abstract description 24
- 239000003112 inhibitor Substances 0.000 claims abstract description 24
- 239000007800 oxidant agent Substances 0.000 claims abstract description 24
- 239000006061 abrasive grain Substances 0.000 claims abstract description 21
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 17
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 17
- 239000010452 phosphate Substances 0.000 claims abstract description 16
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 12
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 11
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 claims abstract description 8
- 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 abstract description 8
- WDJHALXBUFZDSR-UHFFFAOYSA-N acetoacetic acid Chemical compound CC(=O)CC(O)=O WDJHALXBUFZDSR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000013922 glutamic acid Nutrition 0.000 claims abstract description 8
- 239000004220 glutamic acid Substances 0.000 claims abstract description 8
- 229960003330 pentetic acid Drugs 0.000 claims abstract description 8
- URDCARMUOSMFFI-UHFFFAOYSA-N 2-[2-[bis(carboxymethyl)amino]ethyl-(2-hydroxyethyl)amino]acetic acid Chemical compound OCCN(CC(O)=O)CCN(CC(O)=O)CC(O)=O URDCARMUOSMFFI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000006866 deterioration Effects 0.000 claims description 33
- 239000002253 acid Substances 0.000 claims description 24
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 claims description 3
- 239000000758 substrate Substances 0.000 abstract description 62
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract 2
- RUSUZAGBORAKPY-UHFFFAOYSA-N acetic acid;n'-[2-(2-aminoethylamino)ethyl]ethane-1,2-diamine Chemical compound CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.CC(O)=O.NCCNCCNCCN RUSUZAGBORAKPY-UHFFFAOYSA-N 0.000 abstract 1
- 230000000593 degrading effect Effects 0.000 abstract 1
- 229910052759 nickel Inorganic materials 0.000 abstract 1
- 229910018104 Ni-P Inorganic materials 0.000 description 51
- 229910018536 Ni—P Inorganic materials 0.000 description 51
- 235000021317 phosphate Nutrition 0.000 description 15
- 230000003746 surface roughness Effects 0.000 description 14
- 230000002829 reductive effect Effects 0.000 description 12
- 230000007423 decrease Effects 0.000 description 9
- 239000011164 primary particle Substances 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 8
- 239000010410 layer Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 229910001868 water Inorganic materials 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 239000008119 colloidal silica Substances 0.000 description 5
- 230000002950 deficient Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 229920005862 polyol Polymers 0.000 description 5
- 150000003077 polyols Chemical class 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 150000002989 phenols Chemical group 0.000 description 3
- 235000011007 phosphoric acid Nutrition 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920005906 polyester polyol Polymers 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- JVXHQHGWBAHSSF-UHFFFAOYSA-L 2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate;hydron;iron(2+) Chemical compound [H+].[H+].[Fe+2].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O JVXHQHGWBAHSSF-UHFFFAOYSA-L 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N Phosphorous acid Chemical compound OP(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].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-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].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-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 1
- 235000019838 diammonium phosphate Nutrition 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000010097 foam moulding Methods 0.000 description 1
- 230000000855 fungicidal effect Effects 0.000 description 1
- 239000000417 fungicide Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 239000005056 polyisocyanate Substances 0.000 description 1
- 229920001228 polyisocyanate Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 230000003678 scratch resistant effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- 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
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
Description
本発明は、ニッケルリンメッキディスク基板（Ｎｉ−Ｐディスク基板）を研磨する用途、特にＮｉ−Ｐディスク基板を仕上げ研磨する用途で主に使用される研磨用組成物及びその研磨用組成物を用いた研磨方法に関する。 The present invention uses a polishing composition and a polishing composition mainly used in applications for polishing a nickel phosphorus plated disk substrate (Ni-P disk substrate), in particular, for finishing polishing a Ni-P disk substrate. Related to the polishing method.
Ｎｉ−Ｐディスク基板を研磨する用途に使用可能な研磨用組成物として例えば、水、酸化剤、約０．０４Ｍ以上のリン酸イオン又はホスホン酸イオン、及び砥粒を含有する研磨用組成物が特許文献１に開示されている。また、特許文献２には水、酸化ケイ素、エチレンジアミン四酢酸鉄を始めとする金属配位化合物、酸化剤、及びｐＨ調整剤を含有する研磨用組成物が開示されている。しかしながら、特許文献１，２の研磨用組成物を含む従来の研磨用組成物を用いて研磨を行った場合には、研磨用組成物による腐食のために研磨パッドの劣化が経時的に起こる虞があり、その結果、実用上許容できないレベルの微小うねりが生じるなど、Ｎｉ−Ｐディスク基板の表面の仕上がりに悪影響が及ぶことがあった。
本発明はこのような実情に鑑みてなされたものであり、その目的は、Ｎｉ−Ｐディスク基板の研磨をより好適に行うことが可能な研磨用組成物及び研磨方法を提供することにある。 The present invention has been made in view of such circumstances, and an object thereof is to provide a polishing composition and a polishing method capable of more suitably polishing a Ni-P disk substrate.
上記の目的を達成するために、請求項１に記載の発明は、ジエチレントリアミン五酢酸、ヒドロキシエチルエチレンジアミン三酢酸、トリエチレンテトラミン六酢酸及びグルタミン酸二酢酸並びにそれらのアルカリ金属塩及びアンモニウム塩から選ばれるパッド劣化抑制剤と、酸化剤とを含有する研磨用組成物を提供する。 To achieve the above object, the invention according to claim 1 is a pad selected from diethylenetriaminepentaacetic acid, hydroxyethylethylenediaminetriacetic acid, triethylenetetraminehexaacetic acid and glutamic acid diacetic acid, and alkali metal salts and ammonium salts thereof. Provided is a polishing composition containing a deterioration inhibitor and an oxidizing agent.
請求項２に記載の発明は、前記パッド劣化抑制剤は、ジエチレントリアミン五酢酸若しくはグルタミン酸二酢酸又はそれらのアルカリ金属塩若しくはアンモニウム塩である請求項１に記載の研磨用組成物を提供する。 The invention according to claim 2 provides the polishing composition according to claim 1, wherein the pad deterioration inhibitor is diethylenetriaminepentaacetic acid, glutamic acid diacetic acid, or an alkali metal salt or ammonium salt thereof.
請求項３に記載の発明は、フェノール化合物をさらに含有する請求項１又は２に記載の研磨用組成物を提供する。 Invention of Claim 3 provides the polishing composition of Claim 1 or 2 which further contains a phenol compound.
請求項４に記載の発明は、リン酸塩をさらに含有する請求項１〜３のいずれか一項に記載の研磨用組成物を提供する。 Invention of Claim 4 provides the polishing composition as described in any one of Claims 1-3 which further contains a phosphate.
請求項５に記載の発明は、砥粒をさらに含有する請求項１〜４のいずれか一項に記載の研磨用組成物を提供する。 Invention of Claim 5 provides the polishing composition as described in any one of Claims 1-4 which further contains an abrasive grain.
請求項６に記載の発明は、請求項１〜５のいずれか一項に記載の研磨用組成物をスエードタイプの研磨パッドと併せて使用して研磨対象物を研磨する研磨方法を提供する。 Invention of Claim 6 provides the grinding | polishing method which grind | polishes a grinding | polishing target object using the polishing composition as described in any one of Claims 1-5 together with a suede type polishing pad.
本発明によれば、Ｎｉ−Ｐディスク基板の研磨をより好適に行うことが可能な研磨用組成物及び研磨方法が提供される。 According to the present invention, a polishing composition and a polishing method capable of more suitably polishing a Ni-P disk substrate are provided.
以下、本発明の一実施形態を説明する。 Hereinafter, an embodiment of the present invention will be described.
本実施形態の研磨用組成物は、パッド劣化抑制剤及び酸化剤を、好ましくはフェノール化合物、リン酸塩、砥粒及び酸の少なくとも一種とともに、水に混合することにより製造される。従って、研磨用組成物は、パッド劣化抑制剤、酸化剤及び水を含有し、好ましくはフェノール化合物、リン酸塩、砥粒及び酸の少なくとも一種をさらに含有する。 The polishing composition of the present embodiment is produced by mixing a pad deterioration inhibitor and an oxidizing agent with water, preferably together with at least one of a phenol compound, a phosphate, abrasive grains, and an acid. Therefore, the polishing composition contains a pad deterioration inhibitor, an oxidizing agent, and water, and preferably further contains at least one of a phenol compound, a phosphate, abrasive grains, and an acid.
本実施形態の研磨用組成物は、Ｎｉ−Ｐディスク基板を研磨する用途、特にＮｉ−Ｐディスク基板を仕上げ研磨する用途で使用される。仕上げ研磨とは、予備研磨された後のＮｉ−Ｐディスク基板を最終研磨することをいう。仕上げ研磨に供される予備研磨後のＮｉ−Ｐディスク基板の表面粗さＲａは１０ｎｍ以下であることが好ましく、より好ましくは５ｎｍ、さらに好ましくは３ｎｍ以下である。また、仕上げ研磨後のＮｉ−Ｐディスク基板の表面粗さＲａは０．２ｎｍ以下であることが好ましく、より好ましくは０．１５ｎｍ以下である。なお、上記の表面粗さＲａの値は、原子間力顕微鏡（ＡＦＭ）などの走査型プローブ顕微鏡を用いて測定されるものである。
本実施形態の研磨用組成物と併せて使用される研磨パッドは、不織布タイプのものよりはスエードタイプのものであることが好ましい。スエードタイプの研磨パッドは特に限定されるものでなく、例えば特開平１１−３３５９７９号公報に記載のものや特開２００１−６２７０４号公報に記載のものを使用することもできる。スエードタイプの研磨パッドを使用した場合には、不織布タイプの研磨パッドを使用した場合に比べて、研磨後のＮｉ−Ｐディスク基板の表面で測定される微小うねりのレベルがもともと小さく、かつ同じく研磨後のＮｉ−Ｐディスク基板の表面で測定されるスクラッチの数も少なくできる。なお、スエードタイプの研磨パッドでは、ポリエステル系ポリウレタンなどの高分子材料の発泡成形によるナップ層がベース層の上に設けられており、ベース層側の表面で研磨機の定盤に固定され、ナップ層側の表面で研磨対象物を研磨する。ポリエステル系ポリウレタンとは、トリレンジイソシアネート、ジフェニルメタンジイソシアネート、ヘキサメチレンジイソシアネートなどのポリイソシアネート成分との反応に供されるポリオール成分の少なくとも一部がポリエステルポリオールであるポリウレタンである。ポリオール成分の一部がポリエステルポリオールである場合、それ以外のポリオール成分は、例えばポリエーテルポリオール、ポリカーボネートポリオールである。
前記パッド劣化抑制剤は、研磨パッド、特にスエードタイプの研磨パッドの劣化を抑制する働きをする。研磨パッドの劣化が起こる要因として、研磨用組成物中の酸化剤が研磨パッドの研磨面に対して何らかの化学的作用をすることにより研磨面の弾力性が低下することがある。研磨面の弾力性が低くなると、研磨中の機械的な力によって研磨面のナップ層が表層から容易に擦り切れることになる。パッド劣化抑制剤は、この酸化剤の化学的作用を阻害することにより研磨パッドの劣化を抑制するものと考えられる。
The polishing composition of the present embodiment is used for polishing a Ni-P disk substrate, particularly for polishing a Ni-P disk substrate. Final polishing refers to final polishing of the Ni-P disk substrate after preliminary polishing. The surface roughness Ra of the Ni-P disk substrate after pre-polishing used for finish polishing is preferably 10 nm or less, more preferably 5 nm, and further preferably 3 nm or less. Further, the surface roughness Ra of the Ni-P disk substrate after finish polishing is preferably 0.2 nm or less, more preferably 0.15 nm or less. The value of the surface roughness Ra is measured using a scanning probe microscope such as an atomic force microscope (AFM).
The polishing pad used in combination with the polishing composition of the present embodiment is preferably a suede type rather than a nonwoven type. The suede type polishing pad is not particularly limited, and for example, the one described in JP-A-11-335979 or the one described in JP-A-2001-62704 can be used. When a suede type polishing pad is used, the level of microwaviness measured on the surface of the Ni-P disk substrate after polishing is originally smaller than that when a non-woven type polishing pad is used, and the polishing is similarly performed. The number of scratches measured on the surface of the Ni-P disk substrate later can also be reduced. A suede type polishing pad has a nap layer formed by foam molding of a polymer material such as polyester polyurethane on the base layer, and is fixed to the surface plate of the polishing machine on the surface of the base layer. The object to be polished is polished on the surface on the layer side. The polyester-based polyurethane is a polyurethane in which at least a part of a polyol component subjected to a reaction with a polyisocyanate component such as tolylene diisocyanate, diphenylmethane diisocyanate, and hexamethylene diisocyanate is a polyester polyol. When a part of the polyol component is a polyester polyol, the other polyol component is, for example, a polyether polyol or a polycarbonate polyol.
The pad deterioration inhibitor functions to suppress deterioration of a polishing pad, particularly a suede type polishing pad. As a factor that causes the deterioration of the polishing pad, the elasticity of the polishing surface may be lowered by some chemical action of the oxidizing agent in the polishing composition on the polishing surface of the polishing pad. When the elasticity of the polished surface is lowered, the nap layer on the polished surface is easily rubbed off from the surface layer by mechanical force during polishing. The pad deterioration suppressor is considered to suppress the deterioration of the polishing pad by inhibiting the chemical action of the oxidizing agent.
研磨用組成物に含まれるパッド劣化抑制剤は具体的には、ジエチレントリアミン五酢酸、ヒドロキシエチルエチレンジアミン三酢酸、トリエチレンテトラミン六酢酸及びグルタミン酸二酢酸、並びにそのアルカリ金属塩及びアンモニウム塩から選ばれる。その中でも好ましくはジエチレントリアミン五酢酸若しくはグルタミン酸二酢酸、又はそのアルカリ金属塩若しくはアンモニウム塩である。グルタミン酸二酢酸並びにそのアルカリ金属塩及びアンモニウム塩は、研磨用組成物中の酸化剤、特に過酸化水素に対する安定性が高い点で有利である。ジエチレントリアミン五酢酸並びにそのアルカリ金属塩及びアンモニウム塩は、他のパッド劣化抑制剤に比べて研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を向上させることができる点で有利である。なお、上記の各酸の溶解性に比べて同じ酸のアルカリ金属塩及びアンモニウム塩の溶解性の方が高いことから、パッド劣化抑制剤は上記の酸であるよりは上記の酸のアルカリ金属塩又はアンモニウム塩であることが好ましい。 Specifically, the pad deterioration inhibitor contained in the polishing composition is selected from diethylenetriaminepentaacetic acid, hydroxyethylethylenediaminetriacetic acid, triethylenetetraminehexaacetic acid and glutamic acid diacetic acid, and alkali metal salts and ammonium salts thereof. Among them, diethylenetriaminepentaacetic acid or glutamic acid diacetic acid, or an alkali metal salt or ammonium salt thereof is preferable. Glutamic acid diacetic acid and its alkali metal salts and ammonium salts are advantageous in that they are highly stable against oxidizing agents, particularly hydrogen peroxide, in the polishing composition. Diethylenetriaminepentaacetic acid and alkali metal salts and ammonium salts thereof are advantageous in that the polishing rate of the Ni-P disk substrate by the polishing composition can be improved as compared with other pad deterioration inhibitors. Since the solubility of the alkali metal salt and ammonium salt of the same acid is higher than the solubility of each acid, the pad deterioration inhibitor is an alkali metal salt of the above acid rather than the above acid. Or it is preferable that it is an ammonium salt.
研磨用組成物中のパッド劣化抑制剤の含有量の好ましい範囲は一般的には以下の通りである。 The preferred range of the content of the pad deterioration inhibitor in the polishing composition is generally as follows.
すなわち、研磨用組成物中のパッド劣化抑制剤の含有量は０．００１ｍｏｌ／Ｌ以上であることが好ましく、より好ましくは０．００３ｍｏｌ／Ｌ以上、さらに好ましくは０．００５ｍｏｌ／Ｌ以上である。パッド劣化抑制剤の含有量が多くになるにつれて、研磨パッドの劣化はより強く抑制される。この点、研磨用組成物中のパッド劣化抑制剤の含有量が０．００１ｍｏｌ／Ｌ以上、さらに言えば０．００３ｍｏｌ／Ｌ以上、もっと言えば０．００５ｍｏｌ／Ｌ以上であれば、研磨パッドの劣化を実用上特に好適なレベルにまで抑制することができる点で有利である。 That is, the content of the pad deterioration inhibitor in the polishing composition is preferably 0.001 mol / L or more, more preferably 0.003 mol / L or more, and further preferably 0.005 mol / L or more. As the pad deterioration inhibitor content increases, the deterioration of the polishing pad is more strongly suppressed. In this regard, if the content of the pad deterioration inhibitor in the polishing composition is 0.001 mol / L or more, more specifically 0.003 mol / L or more, more specifically 0.005 mol / L or more, This is advantageous in that the deterioration can be suppressed to a particularly suitable level for practical use.
研磨用組成物中のパッド劣化抑制剤の含有量はまた０．２０ｍｏｌ／Ｌ以下であることが好ましく、より好ましくは０．１５ｍｏｌ／Ｌ以下、さらに好ましくは０．１０ｍｏｌ／Ｌ以下である。パッド劣化抑制剤の含有量が少なくなるにつれて、研磨用組成物の材料コストが抑えられることに加え、研磨用組成物中に不溶解分が生じる虞が小さくなる。この点、研磨用組成物中のパッド劣化抑制剤の含有量が０．２０ｍｏｌ／Ｌ以下、さらに言えば０．１５ｍｏｌ／Ｌ以下、もっと言えば０．１０ｍｏｌ／Ｌ以下であれば、費用対効果の点だけでなく、不溶解分の生成を十分に抑えることができる点でも有利である。 The content of the pad deterioration inhibitor in the polishing composition is preferably 0.20 mol / L or less, more preferably 0.15 mol / L or less, and still more preferably 0.10 mol / L or less. As the content of the pad deterioration inhibitor decreases, the material cost of the polishing composition is reduced, and the risk of insoluble matter in the polishing composition is reduced. In this respect, if the content of the pad deterioration inhibitor in the polishing composition is 0.20 mol / L or less, more specifically 0.15 mol / L or less, and more specifically 0.10 mol / L or less, cost effectiveness is achieved. In addition to this point, it is advantageous in that the generation of insoluble matter can be sufficiently suppressed.
前記酸化剤は、Ｎｉ−Ｐディスク基板の表面を酸化する作用を有し、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を向上させる働きをする。 The oxidizing agent has an action of oxidizing the surface of the Ni-P disk substrate, and functions to improve the polishing rate of the Ni-P disk substrate by the polishing composition.
研磨用組成物に含まれる酸化剤は、好ましくは過酸化水素、過硫酸塩、過酢酸などの過酸化物であり、中でも好ましいのは過酸化水素である。 The oxidizing agent contained in the polishing composition is preferably a peroxide such as hydrogen peroxide, persulfate or peracetic acid, and hydrogen peroxide is particularly preferable.
研磨用組成物中の酸化剤の含有量は０．０１質量％以上であることが好ましく、より好ましくは０．０３質量％以上、さらに好ましくは０．０５質量％以上である。酸化剤の含有量が多くになるにつれて、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度は向上する。この点、研磨用組成物中の酸化剤の含有量が０．０１質量％以上、さらに言えば０．０３質量％以上、もっと言えば０．０５質量％以上であれば、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を実用上特に好適なレベルまで向上させることができる点で有利である。 The content of the oxidizing agent in the polishing composition is preferably 0.01% by mass or more, more preferably 0.03% by mass or more, and further preferably 0.05% by mass or more. As the content of the oxidizing agent increases, the polishing rate of the Ni-P disk substrate with the polishing composition increases. In this respect, if the content of the oxidizing agent in the polishing composition is 0.01% by mass or more, more specifically 0.03% by mass or more, and more specifically 0.05% by mass or more, depending on the polishing composition This is advantageous in that the polishing rate of the Ni-P disk substrate can be improved to a practically suitable level.
研磨用組成物中の酸化剤の含有量はまた１．５質量％以下であることが好ましく、より好ましくは１．２質量％以下、さらに好ましくは１．０質量％以下である。酸化剤の含有量が少なくなるにつれて、研磨用組成物の材料コストが抑えられることに加え、研磨使用後の研磨用組成物の処理、すなわち廃液処理の負荷が軽減する。この点、研磨用組成物中の酸化剤の含有量が１．５質量％以下、さらに言えば１．２質量％以下、もっと言えば１．０質量％以下であれば、費用対効果の点だけでなく、廃液処理の負荷を大きく軽減することができる点でも有利である。 The content of the oxidizing agent in the polishing composition is also preferably 1.5% by mass or less, more preferably 1.2% by mass or less, and still more preferably 1.0% by mass or less. As the content of the oxidizing agent decreases, the material cost of the polishing composition can be reduced, and the load of the treatment of the polishing composition after polishing, that is, the waste liquid treatment is reduced. In this respect, if the content of the oxidizing agent in the polishing composition is 1.5% by mass or less, more specifically 1.2% by mass or less, and more specifically 1.0% by mass or less, cost effectiveness is achieved. In addition, it is advantageous in that the load of waste liquid treatment can be greatly reduced.
前記フェノール化合物は、研磨用組成物を用いて研磨後のＮｉ−Ｐディスク基板の表面で測定されるスクラッチ及び微小うねりを低減させる働きをする。フェノール化合物のこの働きは、研磨用組成物中の酸化剤による研磨パッドの研磨面に対する化学的作用をフェノール化合物が阻害することに基づくものと考えられる。 The phenolic compound functions to reduce scratches and micro-waviness measured on the surface of the Ni-P disk substrate after polishing using the polishing composition. This function of the phenol compound is considered to be based on the fact that the phenol compound inhibits the chemical action on the polishing surface of the polishing pad by the oxidizing agent in the polishing composition.
研磨用組成物に含まれるフェノール化合物は、例えばアルコキシフェノールであり、好ましくはｐ−メトキシフェノールなどのｐ−アルコキシフェノールである。 The phenol compound contained in the polishing composition is, for example, alkoxyphenol, preferably p-alkoxyphenol such as p-methoxyphenol.
研磨用組成物中のフェノール化合物の含有量は５質量％以下であることが好ましく、より好ましくは３質量％以下、さらに好ましくは１質量％以下である。フェノール化合物の含有量が少なくなるにつれて、研磨用組成物の材料コストが抑えられることに加え、研磨用組成物中に不溶解分が生じる虞が小さくなる。この点、研磨用組成物中のフェノール化合物の含有量が５質量％以下、さらに言えば３質量％以下、もっと言えば１質量％以下であれば、費用対効果の点だけでなく、不溶解分の生成を十分に抑えることができる点でも有利である。 It is preferable that content of the phenolic compound in polishing composition is 5 mass% or less, More preferably, it is 3 mass% or less, More preferably, it is 1 mass% or less. As the content of the phenol compound decreases, the material cost of the polishing composition can be reduced, and the possibility that an insoluble matter is generated in the polishing composition is reduced. In this respect, if the content of the phenol compound in the polishing composition is 5% by mass or less, more specifically 3% by mass or less, and more specifically 1% by mass or less, it is not only cost effective but also insoluble. It is also advantageous in that generation of minutes can be sufficiently suppressed.
前記リン酸塩は、研磨用組成物を用いて研磨後のＮｉ−Ｐディスク基板の表面で測定されるスクラッチを低減させる働きをする。リン酸塩のこの働きは、Ｎｉ−Ｐディスク基板の表面に耐スクラッチ性を有する不動態膜が形成されることによると考えられる。 The phosphate serves to reduce scratches measured on the surface of the Ni-P disk substrate after polishing using the polishing composition. This action of phosphate is considered to be due to the formation of a scratch-resistant passive film on the surface of the Ni-P disk substrate.
研磨用組成物に含まれるリン酸塩は、例えば、オルトリン酸、メタリン酸、ポリリン酸、メチルアシッドホスフェート、エチルアシッドホスフェート、エチルグリコールアシッドホスフェート又はフィチン酸のナトリウム塩、カリウム塩、リチウム塩又はアンモニウム塩である。その中でも好ましくは、リン酸水素二アンモニウム又はリン酸水素二カリウムである。 Phosphate contained in the polishing composition is, for example, orthophosphoric acid, metaphosphoric acid, polyphosphoric acid, methyl acid phosphate, ethyl acid phosphate, ethyl glycol acid phosphate or phytic acid sodium salt, potassium salt, lithium salt or ammonium salt It is. Among them, diammonium hydrogen phosphate or dipotassium hydrogen phosphate is preferable.
研磨用組成物中のリン酸塩の含有量は３質量％以下であることが好ましく、より好ましくは２質量％以下、さらに好ましくは１質量％以下である。リン酸塩の含有量が少なくなるにつれて、研磨用組成物の材料コストが抑えられる。この点、研磨用組成物中のリン酸塩の含有量が３質量％以下、さらに言えば２質量％以下、もっと言えば１質量％以下であれば、費用対効果の点で有利である。 The content of phosphate in the polishing composition is preferably 3% by mass or less, more preferably 2% by mass or less, and still more preferably 1% by mass or less. As the phosphate content decreases, the material cost of the polishing composition is reduced. In this respect, if the content of the phosphate in the polishing composition is 3% by mass or less, more specifically 2% by mass or less, and more specifically 1% by mass or less, it is advantageous in terms of cost effectiveness.
前記砥粒は、Ｎｉ−Ｐディスク基板を機械的に研磨する作用を有し、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を向上させる働きをする。 The abrasive grains have a function of mechanically polishing the Ni-P disk substrate and serve to improve the polishing rate of the Ni-P disk substrate by the polishing composition.
研磨用組成物に含まれる砥粒は、好ましくはシリカ、より好ましくはコロイダルシリカである。 The abrasive contained in the polishing composition is preferably silica, more preferably colloidal silica.
研磨用組成物中の砥粒の含有量は３０質量％以下であることが好ましく、より好ましくは２０質量％以下、さらに好ましくは１０質量％以下である。砥粒の含有量が少なくなるにつれて、研磨用組成物の材料コストが抑えられる。この点、研磨用組成物中の砥粒の含有量が３０質量％以下、さらに言えば２０質量％以下、もっと言えば１０質量％以下であれば、費用対効果の点で有利である。 The content of abrasive grains in the polishing composition is preferably 30% by mass or less, more preferably 20% by mass or less, and still more preferably 10% by mass or less. As the content of abrasive grains decreases, the material cost of the polishing composition is reduced. In this respect, if the content of the abrasive grains in the polishing composition is 30% by mass or less, more specifically 20% by mass or less, and more specifically 10% by mass or less, it is advantageous in terms of cost effectiveness.
研磨用組成物に含まれる砥粒の平均一次粒子径は１ｎｍ以上であることが好ましく、より好ましくは３ｎｍ以上、さらに好ましくは５ｎｍ以上、最も好ましくは１０ｎｍ以上である。平均一次粒子径が大きくなるにつれて、Ｎｉ−Ｐディスク基板を機械的に研磨する砥粒の作用が強まるため、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度は向上する。この点、砥粒の平均一次粒子径が１ｎｍ以上、さらに言えば３ｎｍ以上、もっと言えば５ｎｍ以上、さらにもっと言えば１０ｎｍ以上であれば、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を実用上特に好適なレベルにまで向上させることができる点で有利である。 The average primary particle diameter of the abrasive grains contained in the polishing composition is preferably 1 nm or more, more preferably 3 nm or more, still more preferably 5 nm or more, and most preferably 10 nm or more. As the average primary particle size increases, the action of abrasive grains that mechanically polish the Ni-P disk substrate increases, so that the polishing rate of the Ni-P disk substrate by the polishing composition increases. In this respect, if the average primary particle diameter of the abrasive grains is 1 nm or more, more specifically 3 nm or more, more specifically 5 nm or more, and even more preferably 10 nm or more, the polishing rate of the Ni-P disk substrate by the polishing composition is increased. This is advantageous in that it can be improved to a level that is particularly suitable for practical use.
研磨用組成物に含まれる砥粒の平均一次粒子径はまた１００ｎｍ以下であることが好ましく、より好ましくは６０ｎｍ以下、さらに好ましくは５０ｎｍ以下、最も好ましくは３０ｎｍ以下である。平均一次粒子径が小さくなるにつれて、研磨用組成物を用いて研磨後のＮｉ−Ｐディスク基板の微小うねりを含む表面品質が良好になる。この点、砥粒の平均一次粒子径が１００ｎｍ以下、さらに言えば６０ｎｍ以下、もっと言えば５０ｎｍ以下、さらにもっと言えば３０ｎｍ以下であれば、研磨後のＮｉ−Ｐディスク基板の表面品質を実用上特に好適なレベルにまで向上させることができる。なお、以上で説明した平均一次粒子径の値は、ＢＥＴ法で測定される砥粒の比表面積に基づいて算出されるものである。 The average primary particle diameter of the abrasive grains contained in the polishing composition is also preferably 100 nm or less, more preferably 60 nm or less, still more preferably 50 nm or less, and most preferably 30 nm or less. As the average primary particle diameter decreases, the surface quality including fine waviness of the Ni-P disk substrate after polishing using the polishing composition becomes better. In this respect, if the average primary particle diameter of the abrasive grains is 100 nm or less, more specifically 60 nm or less, more specifically 50 nm or less, and even more specifically 30 nm or less, the surface quality of the Ni-P disk substrate after polishing is practically used. It can be improved to a particularly suitable level. In addition, the value of the average primary particle diameter demonstrated above is computed based on the specific surface area of the abrasive grain measured by BET method.
前記酸は、Ｎｉ−Ｐディスク基板を化学的に研磨する作用を有し、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を向上させる働きをする。 The acid has a function of chemically polishing the Ni-P disk substrate and functions to improve the polishing rate of the Ni-P disk substrate by the polishing composition.
研磨用組成物に含まれる酸は、塩酸、硫酸、硝酸、リン酸、ホスホン酸、スルファミン酸などの無機酸であってもよいし、リンゴ酸、コハク酸、クエン酸、マレイン酸などの有機酸であってもよい。好ましい無機酸は硫酸及びリン酸である。 The acid contained in the polishing composition may be an inorganic acid such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, phosphonic acid or sulfamic acid, or an organic acid such as malic acid, succinic acid, citric acid or maleic acid. It may be. Preferred inorganic acids are sulfuric acid and phosphoric acid.
研磨用組成物中の酸の含有量は１０質量％以下であることが好ましく、より好ましくは８質量％以下、さらに好ましくは５質量％以下である。酸の含有量が少なくなるにつれて、研磨用組成物の材料コストが抑えられる。この点、研磨用組成物中の酸の含有量が１０質量％以下、さらに言えば８質量％以下、もっと言えば５質量％以下であれば、費用対効果の点で有利である。 It is preferable that content of the acid in polishing composition is 10 mass% or less, More preferably, it is 8 mass% or less, More preferably, it is 5 mass% or less. As the acid content decreases, the material cost of the polishing composition is reduced. In this respect, if the content of the acid in the polishing composition is 10% by mass or less, more specifically 8% by mass or less, and more specifically 5% by mass or less, it is advantageous in terms of cost effectiveness.
研磨用組成物のｐＨは４以下であることが好ましく、より好ましくは３以下である。ｐＨが小さくなるにつれて、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度が向上することに加え、研磨用組成物を用いて研磨後のＮｉ−Ｐディスク基板の表面で測定される微小うねりが低減する。この点、研磨用組成物のｐＨが４以下、さらに言えば３以下であれば、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度を実用上特に好適なレベルまで向上させることができるだけでなく、研磨用組成物を用いて研磨後のＮｉ−Ｐディスク基板における微小うねりを実用上特に好適なレベルにまで低減させることができる点でも有利である。 The pH of the polishing composition is preferably 4 or less, more preferably 3 or less. As the pH decreases, the polishing rate of the Ni-P disk substrate with the polishing composition increases, and in addition, micro-waviness measured on the surface of the Ni-P disk substrate after polishing with the polishing composition is present. To reduce. In this respect, if the polishing composition has a pH of 4 or less, more specifically 3 or less, it is possible not only to improve the polishing rate of the Ni-P disk substrate with the polishing composition to a particularly suitable level for practical use. Also, it is advantageous in that the fine waviness in the Ni-P disk substrate after polishing can be reduced to a particularly suitable level for practical use by using the polishing composition.
本実施形態によれば以下の利点が得られる。 According to the present embodiment, the following advantages can be obtained.
本実施形態の研磨用組成物によれば、パッド劣化抑制剤が研磨用組成物に含まれているために、研磨パッドの劣化を抑制することができ、研磨後のＮｉ−Ｐディスク基板における微小うねりのレベルが研磨パッドの劣化により増大することを抑制することができる。従って、研磨パッドを長時間交換しなくてもＮｉ−Ｐディスク基板の表面を良好に仕上げることができる。よって、本実施形態の研磨用組成物は、Ｎｉ−Ｐディスク基板を研磨する用途、特にＮｉ−Ｐディスク基板を仕上げ研磨する用途で好適に使用することができる。 According to the polishing composition of this embodiment, since the pad deterioration inhibitor is contained in the polishing composition, it is possible to suppress the deterioration of the polishing pad, and the minuteness in the polished Ni-P disk substrate can be suppressed. An increase in the level of waviness due to deterioration of the polishing pad can be suppressed. Therefore, the surface of the Ni-P disk substrate can be satisfactorily finished without changing the polishing pad for a long time. Therefore, the polishing composition of the present embodiment can be suitably used in applications for polishing Ni-P disk substrates, particularly in applications for final polishing Ni-P disk substrates.
前記実施形態は次のように変更されてもよい。 The embodiment may be modified as follows.
・ 前記実施形態の研磨用組成物には二種類以上のパッド劣化抑制剤が含有されてもよい。 -Two or more types of pad deterioration inhibitors may be contained in the polishing composition of the embodiment.
・ 前記実施形態の研磨用組成物には二種類以上の酸化剤が含有されてもよい。 -Two or more types of oxidizing agents may contain in the polishing composition of the said embodiment.
・ 前記実施形態の研磨用組成物には二種類以上のフェノール化合物が含有されてもよい。 -Two or more types of phenol compounds may contain in the polishing composition of the said embodiment.
・ 前記実施形態の研磨用組成物には二種類以上のリン酸塩が含有されてもよい。 -Two or more types of phosphates may be contained in the polishing composition of the embodiment.
・ 前記実施形態の研磨用組成物には二種類以上の砥粒、例えば平均一次粒子径が異なる二種類以上の砥粒が含有されてもよい。 -The polishing composition of the embodiment may contain two or more kinds of abrasive grains, for example, two or more kinds of abrasive grains having different average primary particle diameters.
・ 前記実施形態の研磨用組成物には二種類以上の酸が含有されてもよい。 -Two or more types of acids may contain in the polishing composition of the said embodiment.
・ 前記実施形態の研磨用組成物が酸を含有する場合には、ｐＨ緩衝作用を研磨用組成物に持たせるために塩を添加してもよい。 -When the polishing composition of the said embodiment contains an acid, you may add a salt in order to give a polishing composition the pH buffering effect.
・ 前記実施形態の研磨用組成物には必要に応じて防腐剤や防カビ剤のような公知の添加剤を添加してもよい。 -You may add well-known additives like antiseptic | preservative and a fungicide to the polishing composition of the said embodiment as needed.
・ 前記実施形態の研磨用組成物は一剤型であってもよいし、二剤型を始めとする多剤型であってもよい。多剤型とする場合、コロイダルシリカを含む剤のｐＨは６〜１２であることが好ましく、より好ましくは６．５〜１１である。このｐＨが低すぎる場合には、コロイダルシリカの分散安定性が良くないため、ゲル化が起こりやすい。逆にｐＨが高すぎる場合には、コロイダルシリカの溶解が起こる虞がある。 The polishing composition of the above embodiment may be a one-part type or a multi-part type including a two-part type. When setting it as a multi-drug type, it is preferable that pH of the agent containing colloidal silica is 6-12, More preferably, it is 6.5-11. When this pH is too low, the dispersion stability of colloidal silica is not good and gelation is likely to occur. Conversely, if the pH is too high, the colloidal silica may be dissolved.
・ 前記実施形態の研磨用組成物は、研磨用組成物の原液を水で希釈することによって調製されてもよい。 -The polishing composition of the said embodiment may be prepared by diluting the undiluted | stock solution of polishing composition with water.
・ 前記実施形態の研磨用組成物は、Ｎｉ−Ｐディスク基板以外の研磨対象物を研磨する用途で使用されてもよい。 -The polishing composition of the said embodiment may be used for the use which grind | polishes a grinding | polishing target object other than a Ni-P disk substrate.
次に、本発明の実施例及び比較例を説明する。 Next, examples and comparative examples of the present invention will be described.
実施例１〜１６では、パッド劣化抑制剤、酸化剤、フェノール化合物、リン酸塩、砥粒及び酸を適宜に水と混合することにより研磨用組成物を調製した。比較例１〜１０では、パッド劣化抑制剤又はそれに代わる化合物、酸化剤、砥粒及び酸を適宜に水と混合することにより研磨用組成物を調製した。各例の研磨用組成物中のパッド劣化抑制剤又はそれに代わる化合物、酸化剤、フェノール化合物、リン酸塩及び酸の詳細、並びに研磨用組成物のｐＨを測定した結果を表１，２に示す。なお、表１，２には示さないが、各例の研磨用組成物は砥粒としていずれも平均一次粒子径が２５ｎｍのコロイダルシリカを８質量％含有している。 In Examples 1-16, the polishing composition was prepared by mixing a pad deterioration inhibitor, an oxidizing agent, a phenol compound, a phosphate, an abrasive grain, and an acid with water suitably. In Comparative Examples 1 to 10, polishing compositions were prepared by appropriately mixing a pad deterioration inhibitor or a compound in place thereof, an oxidizing agent, abrasive grains and an acid with water. Tables 1 and 2 show the details of the pad deterioration inhibitor in the polishing composition of each example or a substitute compound, an oxidizing agent, a phenol compound, a phosphate and an acid, and the results of measuring the pH of the polishing composition. . Although not shown in Tables 1 and 2, the polishing composition of each example contains 8% by mass of colloidal silica having an average primary particle diameter of 25 nm as abrasive grains.
表１，２の“研磨速度”欄には、各例の研磨用組成物を用いてＮｉ−Ｐディスク基板を表３に示す研磨条件で研磨したときの研磨速度を測定した結果を示す。研磨速度の測定は下記の計算式に従って行った。 The “polishing rate” column in Tables 1 and 2 shows the results of measuring the polishing rate when the Ni-P disk substrate was polished under the polishing conditions shown in Table 3 using the polishing composition of each example. The polishing rate was measured according to the following calculation formula.
研磨速度［μｍ／分］＝（研磨前の基板の重量［ｇ］−研磨後の基板の重量［ｇ］）／（基板表面の面積［ｃｍ２］×ニッケルリンメッキの密度［ｇ／ｃｍ３］×研磨時間［分］）×１０４
表１，２の“パッド表面粗度の変化率”欄には、各例の研磨用組成物を用いてＮｉ−Ｐディスク基板を連続研磨したときの研磨パッドの劣化、すなわち研磨パッドの表面粗度の変化率に関する評価の結果を示す。具体的には、５０時間研磨使用した研磨パッドのナップ層表面で測定される表面粗さＲａの値を、１０時間研磨使用した研磨パッドのナップ層表面で測定される表面粗さＲａの値で除することにより表面粗度の変化率を求めた。そして、表面粗度の変化率が１２０％未満の場合には○（良）、１２０％以上１３０％未満の場合には△（やや不良）、１３０％以上の場合には×（不良）と評価した。なお、表面粗さＲａの測定には東京精密株式会社製の“ハンディサーフE-35A”を使用し、測定条件は測定長：１２．５ｍｍ、カットオフ：２．５ｍｍとした。また、この評価時の研磨条件は、研磨時間を除いては表３に示すのと同じである。
Polishing rate [μm / min] = (Weight of substrate before polishing [g] −Weight of substrate after polishing [g]) / (Area of substrate surface [cm 2 ] × Nickel phosphorus plating density [g / cm 3] ] × Polishing time [min]) × 10 4
In the "pad surface roughness change rate" column of Tables 1 and 2, the deterioration of the polishing pad when the Ni-P disk substrate was continuously polished using the polishing composition of each example, that is, the surface roughness of the polishing pad. The result of the evaluation regarding the rate of change in degree is shown. Specifically, the value of the surface roughness Ra measured on the nap layer surface of the polishing pad used for 50 hours polishing is the value of the surface roughness Ra measured on the nap layer surface of the polishing pad used for 10 hours polishing. The rate of change in surface roughness was determined by dividing the value. When the rate of change in surface roughness is less than 120%, it is evaluated as ◯ (good), when it is 120% or more and less than 130%, Δ (slightly defective), and when it is 130% or more, evaluation is × (defect). did. For measurement of the surface roughness Ra, “Handy Surf E-35A” manufactured by Tokyo Seimitsu Co., Ltd. was used, and the measurement conditions were a measurement length of 12.5 mm and a cut-off of 2.5 mm. The polishing conditions at the time of this evaluation are the same as those shown in Table 3 except for the polishing time.
表１，２の“基板微小うねりの初期値”欄には、１０時間研磨使用することによりナップ層表面の表面粗さＲａの値が安定した研磨パッドを各例の研磨用組成物と併せて用いて、表３に示す研磨条件でＮｉ−Ｐディスク基板を研磨したときに研磨後のＮｉ−Ｐディスク基板の表面で測定される微小うねりに関する評価の結果を示す。具体的には、Candela社製の“OSA6100”を使用して表４に示す測定条件で測定される表面粗さＲａとしての微小うねりの値が０．５Å未満の場合には◎（優）、０．５Å以上０．５８Å未満の場合には○（良）、０．５８Å以上０．６２Å未満の場合には△（やや不良）、０．６２Å以上の場合には×（不良）と評価した。 In the column “Initial value of substrate fine waviness” in Tables 1 and 2, polishing pads in which the value of surface roughness Ra of the nap layer surface is stabilized by polishing for 10 hours are combined with the polishing composition of each example. 1 shows the results of evaluation regarding micro-waviness measured on the surface of the Ni-P disk substrate after polishing when the Ni-P disk substrate is polished under the polishing conditions shown in Table 3. Specifically, when the value of the microwaviness as the surface roughness Ra measured under the measurement conditions shown in Table 4 using “OSA6100” manufactured by Candela is less than 0.5 mm, ◎ (excellent), In the case of 0.5 mm or more and less than 0.58 mm, it was evaluated as ◯ (good), in the case of 0.58 mm or more and less than 0.62 mm, Δ (slightly defective), and in the case of 0.62 mm or more, evaluated as x (defective) .
表１，２の“基板微小うねりの変化率”欄には、各例の研磨用組成物を用いて表３に示す研磨条件で研磨したＮｉ−Ｐディスク基板の表面で測定される微小うねりの値の研磨パッドの使用時間による変化率に関する評価の結果を示す。具体的には、５０時間研磨使用した研磨パッドを用いて研磨したＮｉ−Ｐディスク基板の表面で測定される微小うねりの値を、１０時間研磨使用した研磨パッドを用いて研磨したＮｉ−Ｐディスク基板の表面で測定される微小うねりの値で除することにより微小うねりの変化率を求めた。そして、微小うねりの変化率が１１０％未満の場合には◎（優）、１１０％以上１２０％未満の場合には○（良）、１２０％以上１３０％未満の場合には△（やや不良）、１３０％以上の場合には×（不良）と評価した。なお、微小うねりの測定の詳細は上記に同じである。 In the column “Change rate of substrate microwaviness” in Tables 1 and 2, the microwaviness measured on the surface of the Ni-P disk substrate polished under the polishing conditions shown in Table 3 using the polishing composition of each example. The result of the evaluation regarding the change rate by the usage time of the polishing pad of a value is shown. Specifically, the Ni-P disk polished using the polishing pad used for polishing for 10 hours was measured for the value of microwaviness measured on the surface of the Ni-P disk substrate polished using the polishing pad used for 50 hours. The rate of change of microwaviness was obtained by dividing by the value of microwaviness measured on the surface of the substrate. And, when the change rate of micro swell is less than 110%, ◎ (excellent), when it is 110% or more and less than 120%, ○ (good), and when it is 120% or more and less than 130%, △ (somewhat poor) In the case of 130% or more, it was evaluated as x (defect). The details of the measurement of micro swell are the same as above.
表１，２の“スクラッチ”欄には、各例の研磨用組成物を用いて表３に示す研磨条件で研磨したＮｉ−Ｐディスク基板の表面で測定されるスクラッチの本数に関する評価の結果を示す。具体的には、Ｎｉ−Ｐディスク基板の表面のうち基板の外周縁から中心に向かって０〜１５ｍｍの間の部分で測定されるスクラッチの本数が１２未満の場合には◎（優）、１２以上１８未満の場合には○（良）、１８以上２３未満の場合には△（やや不良）、２３以上の場合には×（不良）と評価した。なお、スクラッチの計数にはVISION PSYTEC社製の“MicroMax VMX2100”を使用した。 In the “scratch” column of Tables 1 and 2, the evaluation results regarding the number of scratches measured on the surface of the Ni-P disk substrate polished using the polishing composition of each example under the polishing conditions shown in Table 3 are shown. Show. Specifically, when the number of scratches measured at a portion between 0 to 15 mm from the outer peripheral edge of the surface of the Ni-P disk substrate toward the center is less than 12, ◎ (excellent), 12 When it was less than 18, it was evaluated as ◯ (good), when it was 18 or more and less than 23, Δ (slightly defective), and when it was 23 or more, it was evaluated as x (defective). In addition, “MicroMax VMX2100” manufactured by VISION PSYTEC was used for counting scratches.
表１，２の“スラリー安定性”欄には、各例の研磨用組成物の研磨性能上の安定性に関する評価の結果を示す。具体的には、各例の研磨用組成物を調整後に常温保存したとき、保存後の研磨用組成物を用いてＮｉ−Ｐディスク基板を研磨したときに測定される研磨速度の値が、調整直後の研磨用組成物を用いてＮｉ−Ｐディスク基板を研磨したときに測定される研磨速度の値の８５％にまで低下するのに要する日数を調べた。そして、その日数が調整後１４日以上の場合には◎（優）、７日以上１４日未満の場合には○（良）、３日以上７日未満の場合には△（やや不良）、３日未満の場合には×（不良）と評価した。 In the “Slurry Stability” column of Tables 1 and 2, the results of evaluation on the stability of the polishing composition of each example regarding the polishing performance are shown. Specifically, when the polishing composition of each example was stored at room temperature after adjustment, the value of the polishing rate measured when the Ni-P disk substrate was polished using the polishing composition after storage was adjusted. The number of days required to decrease to 85% of the value of the polishing rate measured when the Ni-P disk substrate was polished using the polishing composition immediately after the polishing was examined. And, if the number of days is 14 days or more after adjustment, ◎ (excellent), if it is 7 days or more and less than 14 days, ○ (good), if it is 3 days or more and less than 7 days, △ (somewhat bad), In the case of less than 3 days, it was evaluated as x (defect).
これに対し、パッド劣化抑制剤を含まない研磨用組成物を用いた比較例２〜１０では、パッド表面粗度の変化率と基板微小うねりの変化率がいずれも１３０％以上であり、パッド表面粗度の変化率及び基板微小うねりの変化率に関して実用に足るレベルの値が得られなかった。また、酸化剤を含まない研磨用組成物を用いた比較例１では、研磨速度が０．０４μｍ／分であり、研磨速度に関して実用に足るレベルの値が得られなかった。 On the other hand, in Comparative Examples 2 to 10 using the polishing composition not containing the pad deterioration inhibitor, the change rate of the pad surface roughness and the change rate of the substrate microwaviness are both 130% or more, and the pad surface A practically satisfactory value was not obtained for the rate of change in roughness and the rate of change in substrate microwaviness. Further, in Comparative Example 1 using the polishing composition containing no oxidizing agent, the polishing rate was 0.04 μm / min, and a practically sufficient value for the polishing rate could not be obtained.
前記実施形態より把握できる技術的思想について以下に記載する。 The technical idea that can be grasped from the embodiment will be described below.
酸をさらに含有することを特徴とする請求項１〜５のいずれか一項に記載の研磨用組成物。この場合、酸の化学的研磨作用のために、研磨用組成物によるＮｉ−Ｐディスク基板の研磨速度が向上する。 The polishing composition according to claim 1, further comprising an acid. In this case, the polishing rate of the Ni-P disk substrate by the polishing composition is improved due to the chemical polishing action of the acid.
Claims (6)
酸化剤と
を含有することを特徴とする研磨用組成物。 A pad deterioration inhibitor that suppresses deterioration of a polishing pad selected from diethylenetriaminepentaacetic acid, hydroxyethylethylenediaminetriacetic acid, triethylenetetraminehexaacetic acid and glutamic acid diacetic acid, and alkali metal salts and ammonium salts thereof;
A polishing composition comprising an oxidizing agent.
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| JP2007105830A JP5259975B2 (en) | 2007-04-13 | 2007-04-13 | Polishing composition and polishing method |
| MYPI20094266 MY152929A (en) | 2007-04-13 | 2008-04-10 | Polishing composition and polishing method |
| PCT/JP2008/057099 WO2008133023A1 (en) | 2007-04-13 | 2008-04-10 | Polishing composition and polishing method |
| MYPI2013000694A MY160635A (en) | 2007-04-13 | 2013-02-28 | Polishing composition and polishing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04363385A (en) * | 1990-08-29 | 1992-12-16 | Mitsubishi Kasei Corp | Abradant composition |
| JPH1121545A (en) * | 1997-06-30 | 1999-01-26 | Fujimi Inkooporeetetsudo:Kk | Polishing composition |
| JP2005243673A (en) * | 2004-02-24 | 2005-09-08 | Toshiro Doi | Chemical mechanical polishing method and polishing body |
| JP2006049912A (en) * | 2004-08-03 | 2006-02-16 | Samsung Electronics Co Ltd | Cmp slurry, chemical mechanical polishing method using the cmp slurry, and method of forming metal wiring using the cmp slurry |
| JP2007067089A (en) * | 2005-08-30 | 2007-03-15 | Fujifilm Holdings Corp | Polishing solution and semiconductor device manufacturing method using the solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04363385A (en) * | 1990-08-29 | 1992-12-16 | Mitsubishi Kasei Corp | Abradant composition |
| JPH1121545A (en) * | 1997-06-30 | 1999-01-26 | Fujimi Inkooporeetetsudo:Kk | Polishing composition |
| JP2005243673A (en) * | 2004-02-24 | 2005-09-08 | Toshiro Doi | Chemical mechanical polishing method and polishing body |
| JP2006049912A (en) * | 2004-08-03 | 2006-02-16 | Samsung Electronics Co Ltd | Cmp slurry, chemical mechanical polishing method using the cmp slurry, and method of forming metal wiring using the cmp slurry |
| JP2007067089A (en) * | 2005-08-30 | 2007-03-15 | Fujifilm Holdings Corp | Polishing solution and semiconductor device manufacturing method using the solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010260121A (en) * | 2009-04-30 | 2010-11-18 | Kao Corp | Method of manufacturing abrasive slurry |
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| MY152929A (en) | 2014-12-15 |
| MY160635A (en) | 2017-03-15 |
| WO2008133023A1 (en) | 2008-11-06 |
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