JPH04228502A - Acicular metallic iron fine particle containing carbon, its production and magnetic paint composition and magnetic recording medium containing the particle - Google Patents
Acicular metallic iron fine particle containing carbon, its production and magnetic paint composition and magnetic recording medium containing the particleInfo
- Publication number
- JPH04228502A JPH04228502A JP3140817A JP14081791A JPH04228502A JP H04228502 A JPH04228502 A JP H04228502A JP 3140817 A JP3140817 A JP 3140817A JP 14081791 A JP14081791 A JP 14081791A JP H04228502 A JPH04228502 A JP H04228502A
- Authority
- JP
- Japan
- Prior art keywords
- acicular
- fine particles
- metallic iron
- carbon
- magnetic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 239000010419 fine particle Substances 0.000 title claims abstract description 61
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 53
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 42
- 239000002245 particle Substances 0.000 title claims description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000000203 mixture Substances 0.000 title abstract description 19
- 239000003973 paint Substances 0.000 title abstract description 7
- 229910001567 cementite Inorganic materials 0.000 claims abstract description 34
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 22
- 125000004432 carbon atom Chemical group C* 0.000 claims description 22
- 239000008199 coating composition Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000696 magnetic material Substances 0.000 claims description 5
- 229910001111 Fine metal Inorganic materials 0.000 claims 2
- 230000007797 corrosion Effects 0.000 abstract description 16
- 238000005260 corrosion Methods 0.000 abstract description 16
- 150000001721 carbon Chemical group 0.000 abstract description 5
- 239000000843 powder Substances 0.000 description 35
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- -1 γ-Fe2O3 Chemical compound 0.000 description 19
- 235000013980 iron oxide Nutrition 0.000 description 18
- 239000007789 gas Substances 0.000 description 17
- 230000005415 magnetization Effects 0.000 description 17
- 238000000034 method Methods 0.000 description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 15
- CUPCBVUMRUSXIU-UHFFFAOYSA-N [Fe].OOO Chemical compound [Fe].OOO CUPCBVUMRUSXIU-UHFFFAOYSA-N 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 15
- 239000002184 metal Substances 0.000 description 15
- 238000006243 chemical reaction Methods 0.000 description 14
- 239000011248 coating agent Substances 0.000 description 13
- 238000000576 coating method Methods 0.000 description 13
- 229910021519 iron(III) oxide-hydroxide Inorganic materials 0.000 description 13
- 238000005245 sintering Methods 0.000 description 12
- 229920001577 copolymer Polymers 0.000 description 11
- 229910052757 nitrogen Inorganic materials 0.000 description 11
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- 229910003145 α-Fe2O3 Inorganic materials 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- 239000011230 binding agent Substances 0.000 description 9
- 229910052739 hydrogen Inorganic materials 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 239000003085 diluting agent Substances 0.000 description 8
- 239000010439 graphite Substances 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 238000011282 treatment Methods 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 235000014113 dietary fatty acids Nutrition 0.000 description 7
- 150000002148 esters Chemical class 0.000 description 7
- 229930195729 fatty acid Natural products 0.000 description 7
- 239000000194 fatty acid Substances 0.000 description 7
- AEIXRCIKZIZYPM-UHFFFAOYSA-M hydroxy(oxo)iron Chemical compound [O][Fe]O AEIXRCIKZIZYPM-UHFFFAOYSA-M 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 229910052598 goethite Inorganic materials 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 239000002216 antistatic agent Substances 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- 150000004665 fatty acids Chemical class 0.000 description 5
- 230000004907 flux Effects 0.000 description 5
- 239000003112 inhibitor Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 235000019353 potassium silicate Nutrition 0.000 description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- TZIHFWKZFHZASV-UHFFFAOYSA-N methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 229910006540 α-FeOOH Inorganic materials 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 3
- 239000003082 abrasive agent Substances 0.000 description 3
- 125000005396 acrylic acid ester group Chemical group 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 3
- 229920002678 cellulose Chemical class 0.000 description 3
- 239000001913 cellulose Chemical class 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- ZQPPMHVWECSIRJ-MDZDMXLPSA-N elaidic acid Chemical compound CCCCCCCC\C=C\CCCCCCCC(O)=O ZQPPMHVWECSIRJ-MDZDMXLPSA-N 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 125000005397 methacrylic acid ester group Chemical group 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 150000003377 silicon compounds Chemical class 0.000 description 3
- 229910001388 sodium aluminate Inorganic materials 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 2
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001639 boron compounds Chemical class 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- UCNNJGDEJXIUCC-UHFFFAOYSA-L hydroxy(oxo)iron;iron Chemical compound [Fe].O[Fe]=O.O[Fe]=O UCNNJGDEJXIUCC-UHFFFAOYSA-L 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 150000002506 iron compounds Chemical class 0.000 description 2
- VBMVTYDPPZVILR-UHFFFAOYSA-N iron(2+);oxygen(2-) Chemical class [O-2].[Fe+2] VBMVTYDPPZVILR-UHFFFAOYSA-N 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 235000011007 phosphoric acid Nutrition 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 150000003016 phosphoric acids Chemical group 0.000 description 2
- 150000003018 phosphorus compounds Chemical class 0.000 description 2
- 229920006122 polyamide resin Chemical class 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- RGTIBVZDHOMOKC-UHFFFAOYSA-N stearolic acid Chemical compound CCCCCCCCC#CCCCCCCCC(O)=O RGTIBVZDHOMOKC-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 150000003609 titanium compounds Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 229910006299 γ-FeOOH Inorganic materials 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- HMUNWXXNJPVALC-UHFFFAOYSA-N 1-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)C(CN1CC2=C(CC1)NN=N2)=O HMUNWXXNJPVALC-UHFFFAOYSA-N 0.000 description 1
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- YJLUBHOZZTYQIP-UHFFFAOYSA-N 2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CC2=C(CC1)NN=N2 YJLUBHOZZTYQIP-UHFFFAOYSA-N 0.000 description 1
- SZIFAVKTNFCBPC-UHFFFAOYSA-N 2-chloroethanol Chemical compound OCCCl SZIFAVKTNFCBPC-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- CSKRBHOAJUMOKJ-UHFFFAOYSA-N 3,4-diacetylhexane-2,5-dione Chemical compound CC(=O)C(C(C)=O)C(C(C)=O)C(C)=O CSKRBHOAJUMOKJ-UHFFFAOYSA-N 0.000 description 1
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical compound C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
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- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
【０００１】0001
【産業上の利用分野】本発明は炭素を含有する針状金属
鉄微粒子、その製法、それを含有する磁性塗料組成物及
び磁気記録媒体に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to carbon-containing acicular metallic iron particles, a method for producing the same, a magnetic coating composition containing the same, and a magnetic recording medium.
【０００２】0002
【従来の技術】従来の針状金属鉄微粒子は、酸化鉄、例
えばγ−Ｆｅ２Ｏ３の針状微粒子より遥かに良好な磁気
特性を有して、磁気記録テープなど磁気記録媒体用の磁
性材料として使用されている。[Prior Art] Conventional acicular metallic iron fine particles have much better magnetic properties than acicular fine particles of iron oxide, such as γ-Fe2O3, and are used as magnetic materials for magnetic recording media such as magnetic recording tapes. has been done.
【０００３】しかし針状金属鉄微粒子はその表面が金属
であるので耐食性が低いという欠点がある。耐食性を改
善するため金属鉄微粒子表面を酸素もしくは空気で処理
して、その表面に非磁性の又は磁気特性の低い酸化物層
を形成させる方法により耐食性を改善し、磁気特性の経
時劣化を防いでいる。しかし、この方法では金属鉄を非
磁性酸化物で被覆した分の磁化量が犠牲にされるので、
製造工程中に添加される他の焼結防止剤等の重量も合わ
せると、金属鉄単独で本来有する重量当たりの飽和磁化
量の通常２０〜３０％が犠牲となつている。[0003] However, since the surface of acicular metallic iron particles is metal, they have a drawback of low corrosion resistance. To improve corrosion resistance, the surface of metallic iron particles is treated with oxygen or air to form a non-magnetic or low magnetic oxide layer on the surface, which improves corrosion resistance and prevents deterioration of magnetic properties over time. There is. However, with this method, the amount of magnetization of metal iron coated with non-magnetic oxide is sacrificed.
When the weight of other sintering inhibitors added during the manufacturing process is included, usually 20 to 30% of the saturation magnetization per weight that metal iron alone inherently has is sacrificed.
【０００４】耐食性を向上させるその他の方法として、
磁性金属粉末の表面に黒鉛被膜を形成させる方法も提案
されている（特開平２−６９９０４）。これは金属粉末
表面の触媒作用により緻密な黒鉛皮膜を得たものである
が、黒鉛が非磁性物であること、および金属粉末を得る
ため多量の焼結防止剤を必要とするのでやはり飽和磁化
量を犠牲にしている。[0004] As another method for improving corrosion resistance,
A method of forming a graphite film on the surface of magnetic metal powder has also been proposed (Japanese Patent Laid-Open No. 2-69904). This method obtains a dense graphite film through the catalytic action of the metal powder surface, but since graphite is non-magnetic and a large amount of anti-sintering agent is required to obtain the metal powder, saturation magnetization still occurs. sacrificing quantity.
【０００５】また、遷移金属カルボニル化合物から得ら
れ、炭素を実質的に炭化金属の形で含む金属磁性粉（特
開平２−６９９０３）も提案されているが、これは原料
が高価である点が不利である。さらに一次粒子が針状で
はないので、磁場をかけて針状を得ているがその形状は
一般に粗大であり、塗工、および配向が困難であり、磁
気記録媒体に用いるのは不適当である。[0005] Metal magnetic powder obtained from a transition metal carbonyl compound and containing carbon substantially in the form of metal carbide has also been proposed (Japanese Patent Application Laid-Open No. 2-69903), but this has the disadvantage that the raw materials are expensive. It is disadvantageous. Furthermore, since the primary particles are not acicular, they are obtained by applying a magnetic field, but their shape is generally coarse, making coating and orientation difficult, making them unsuitable for use in magnetic recording media. .
【０００６】一方、耐食性に優れた磁性材料として針状
炭化鉄微粒子が知られている。これは化学的に安定で高
保磁力を有し磁気記録媒体用の磁性材料として有用であ
る（例えば特開昭６０−７１５０９号、同６０−１０８
３０９号、同６０−１２７２１２号、同６０−１５５５
２２号）。しかし重量当たりの飽和磁化量の点において
針状金属鉄微粒子に劣る。On the other hand, acicular iron carbide fine particles are known as a magnetic material with excellent corrosion resistance. It is chemically stable and has a high coercive force, and is useful as a magnetic material for magnetic recording media (for example, JP-A-60-71509, JP-A-60-108).
No. 309, No. 60-127212, No. 60-1555
No. 22). However, they are inferior to needle-shaped metal iron fine particles in terms of the amount of saturation magnetization per weight.
【０００７】[0007]
【発明が解決しようとする課題】本発明の目的は磁気特
性及び耐食性に優れた針状金属鉄微粒子、その製法、そ
れを含有する磁性塗料組成物及び磁気記録媒体を提供す
ることにある。SUMMARY OF THE INVENTION An object of the present invention is to provide acicular metallic iron fine particles having excellent magnetic properties and corrosion resistance, a method for producing the same, a magnetic coating composition containing the same, and a magnetic recording medium.
【０００８】[0008]
【課題を解決するための手段】本発明は炭素を含有する
針状金属鉄微粒子であつて、その平均粒径（長軸）が１
．０μｍ以下、平均軸比が３〜１５であり、前記炭素の
量が前記針状金属鉄微粒子に対して２〜２０重量％であ
る針状金属鉄微粒子に係る。[Means for Solving the Problems] The present invention provides acicular metallic iron fine particles containing carbon, the average particle diameter (long axis) of which is 1.
．． The present invention relates to acicular metal iron fine particles having a diameter of 0 μm or less, an average axial ratio of 3 to 15, and an amount of carbon in the range of 2 to 20% by weight based on the acicular metal iron fine particles.
【０００９】また、本発明は上記針状金属鉄微粒子を含
有する磁性塗料組成物及び磁気記録媒体に係る。The present invention also relates to a magnetic coating composition and a magnetic recording medium containing the above-mentioned acicular metallic iron particles.
【００１０】本発明の針状金属鉄微粒子は針状炭化鉄微
粒子に炭素原子を含有しない還元剤を接触させることに
より製造される。The acicular metallic iron fine particles of the present invention are produced by contacting acicular iron carbide fine particles with a reducing agent containing no carbon atoms.
【００１１】本発明の針状金属鉄微粒子は、従来のオキ
シ水酸化鉄又は酸化鉄を鉄又はこれに近い状態まで水素
で還元して得た針状金属鉄粒子よりも優れた耐食性を有
し、且つ同等又はより優れた保磁力及び飽和磁化量を有
する。更に磁性塗料とした場合、本発明の微粒子は分散
性に優れる。また本発明の磁気記録媒体は従来のものよ
りはるかに優れたシート特性を有する。The acicular metallic iron fine particles of the present invention have better corrosion resistance than the acicular metallic iron particles obtained by reducing conventional iron oxyhydroxide or iron oxide with hydrogen to iron or a state close to iron. , and have equivalent or superior coercive force and saturation magnetization. Furthermore, when used as a magnetic paint, the fine particles of the present invention have excellent dispersibility. Furthermore, the magnetic recording medium of the present invention has sheet properties far superior to those of conventional media.
【００１２】本発明による炭素を含有する針状金属鉄微
粒子が磁気特性に優れている理由は明らかではないが、
従来針状金属鉄微粒子を得る場合、針状酸化鉄微粒子を
直接還元しているので、還元により生成する水のため焼
結、形状の崩れが起こり、高保磁力、高分散性が得られ
ない。その対策として酸化鉄の状態で多量の焼結防止剤
の被着処理を施しているがこれらは非磁性のため金属鉄
微粒子の磁化量の低下の原因になつている。また黒鉛、
炭化鉄で表面被膜処理をしようとする場合金属鉄が触媒
となり炭素が析出しやすくなり磁化量の低下の原因にな
つている。Although it is not clear why the carbon-containing acicular metallic iron fine particles according to the present invention have excellent magnetic properties,
Conventionally, when obtaining acicular metallic iron fine particles, the acicular iron oxide fine particles are directly reduced, which causes sintering and deformation due to water produced by reduction, making it impossible to obtain high coercive force and high dispersibility. As a countermeasure, a large amount of anti-sintering agent is applied to the iron oxide, but since these agents are non-magnetic, they cause a decrease in the amount of magnetization of the metallic iron particles. Also graphite,
When attempting to treat the surface with iron carbide, the metal iron acts as a catalyst and carbon tends to precipitate, causing a decrease in the amount of magnetization.
【００１３】これに対し本発明の針状金属鉄微粒子はそ
の製造時の還元過程において、まず多量の水を生成する
ことがなく、従つて焼結防止剤が少なくても高保磁力、
高分散性を損なうことなく、金属鉄本来の高磁化量を引
き出すことができ、ついで炭化鉄由来の炭素（これはＸ
線回折で黒鉛ではなく、無定形の炭素と推定される）が
活性な還元面を効果的に保護するため前記優れた磁気特
性が長期に亘り劣化することなく維持することができる
。On the other hand, the acicular metallic iron fine particles of the present invention do not generate a large amount of water during the reduction process during production, and therefore have high coercive force and high coercive force even with a small amount of anti-sintering agent.
It is possible to bring out the high magnetization inherent in metallic iron without impairing high dispersibility, and then carbon derived from iron carbide (this is
Since the active reduction surface (presumed to be amorphous carbon rather than graphite by line diffraction) effectively protects the active reduction surface, the excellent magnetic properties can be maintained over a long period of time without deterioration.
【００１４】以上詳述したように本発明の針状金属鉄微
粒子は、焼結防止剤の含有量が従来の針状金属鉄微粒子
の場合に比べて少なく、例えば焼結防止剤がＳｉ成分の
ときその含有量が針状オキシ水酸化鉄の重量を基準にし
て約３重量％以下、約０．０１〜０．５重量％が好まし
く、約０．０１重量％であつても１０００Ｏｅ以上の高
保磁力、高分散性と、１２０ｅｍｕ／ｇ以上の高飽和磁
化量とを示し、且つまた針状金属鉄微粒子に対して２〜
２０重量％の上記炭素によりその活性面が保護されたも
のであるといえる。As detailed above, the acicular metallic iron fine particles of the present invention have a smaller content of the sintering inhibitor than the conventional acicular metallic iron fine particles. When the content is about 3% by weight or less, preferably about 0.01 to 0.5% by weight, based on the weight of the acicular iron oxyhydroxide, even if the content is about 0.01% by weight, it still has a high thermal stability of 1000 Oe or more. It exhibits magnetic force, high dispersibility, and high saturation magnetization of 120 emu/g or more, and also has a
It can be said that the active surface was protected by 20% by weight of the above carbon.
【００１５】本発明の針状金属鉄微粒子の製法において
、出発原料として用いられる針状炭化鉄微粒子としては
例えば特開昭６０−７１５０９号、同６１−１１１９２
１号等に記載された針状炭化鉄微粒子を挙げることがで
きる。かかる微粒子の成分である炭化鉄にはＦｅ５Ｃ２
、Ｆｅ７Ｃ３、ＦｅＣ、Ｆｅ３Ｃがあり、前三者が好ま
しい。[0015] In the method for producing acicular metallic iron fine particles of the present invention, examples of acicular iron carbide fine particles used as a starting material include JP-A-60-71509 and JP-A-61-11192.
Examples include acicular iron carbide fine particles described in No. 1 and the like. Iron carbide, which is a component of such fine particles, contains Fe5C2.
, Fe7C3, FeC, and Fe3C, and the former three are preferred.
【００１６】本発明の出発原料となる針状炭化鉄微粒子
を製造するには、例えば（ａ）針状オキシ水酸化鉄また
は針状酸化鉄に炭素原子を含有しない還元剤を接触させ
た後または接触させずに、（ｂ）炭素原子を含有する還
元剤もしくはこれと炭素原子を含有しない還元剤との混
合物を接触させる方法による。In order to produce the acicular iron carbide fine particles which are the starting material of the present invention, for example, (a) after contacting acicular iron oxyhydroxide or acicular iron oxide with a reducing agent containing no carbon atoms, or (b) A method in which a reducing agent containing a carbon atom or a mixture of this and a reducing agent not containing a carbon atom is brought into contact with the reducing agent without contacting the reducing agent.
【００１７】その方法において針状オキシ水酸化鉄は、
針状α−ＦｅＯＯＨ（ゲーサイト）、β−ＦｅＯＯＨ（
アカガネサイト）又は針状γ−ＦｅＯＯＨ（レピドクロ
サイト）が好ましく、針状酸化鉄は、針状α−Ｆｅ２Ｏ
３（ヘマタイト）、針状γ−Ｆｅ２Ｏ３（マグヘマイト
）又は針状Ｆｅ３Ｏ４（マグネタイト）が好ましい。In the method, the acicular iron oxyhydroxide is
Acicular α-FeOOH (goethite), β-FeOOH (
Akaganesite) or acicular γ-FeOOH (lepidocrocite) is preferable, and acicular iron oxide is acicular α-Fe2O
3 (hematite), acicular γ-Fe2O3 (maghemite), or acicular Fe3O4 (magnetite).
【００１８】上記の針状α−Ｆｅ２Ｏ３又は針状γ−Ｆ
ｅ２Ｏ３としては、例えば針状α−ＦｅＯＯＨ、針状β
−ＦｅＯＯＨ又は針状γ−ＦｅＯＯＨをそれぞれ約２０
０〜３５０℃に加熱及び脱水して得られたもの、あるい
はこれらを更に約３５０〜９００℃に加熱して結晶の緻
密化を図つた針状α−Ｆｅ２Ｏ３、γ−Ｆｅ２Ｏ３等あ
らゆるものが包含される。The above acicular α-Fe2O3 or acicular γ-F
As e2O3, for example, acicular α-FeOOH, acicular β
-FeOOH or acicular γ-FeOOH, each about 20
It includes all kinds of things such as those obtained by heating and dehydrating at 0 to 350°C, or those obtained by further heating these to about 350 to 900°C to make the crystals denser, such as acicular α-Fe2O3 and γ-Fe2O3. Ru.
【００１９】前記の針状Ｆｅ３Ｏ４は、針状Ｆｅ３Ｏ４
以外の針状酸化鉄又は針状オキシ水酸化鉄を炭素原子を
含有する還元剤もしくは炭素原子を含有しない還元剤又
はこれらの混合物と接触させることによつて製造するこ
とができる。炭素原子を含有する還元剤又はこれと炭素
原子を含有しない還元剤との混合物を接触させて針状Ｆ
ｅ３Ｏ４を製造する場合、後述の製法における接触条件
と比較して、時間に関する以外同一の接触条件にするこ
とができる。その場合、針状Ｆｅ３Ｏ４の製造に引き続
き同一条件で接触を継続して目的とする針状炭化鉄粒子
を製造することができる。The above-mentioned acicular Fe3O4 is acicular Fe3O4
The acicular iron oxides or acicular iron oxyhydroxides can be produced by contacting other acicular iron oxides or acicular iron oxyhydroxides with carbon-containing or non-carbon-containing reducing agents or mixtures thereof. Acicular F by contacting a reducing agent containing carbon atoms or a mixture of this and a reducing agent not containing carbon atoms.
When producing e3O4, the contact conditions can be the same except for time as compared to the contact conditions in the production method described below. In that case, the desired acicular iron carbide particles can be produced by continuing contact under the same conditions following the production of acicular Fe3O4.
【００２０】針状オキシ水酸化鉄又は針状酸化鉄は平均
軸比が３以上のものが通常であり、５〜１５のものが好
適であり、平均粒径（長軸）は、通常１．０μｍ以下、
好適には０．１〜１．０μｍである。これにより製造さ
れた針状炭化鉄微粒子は、原料の平均軸比及び平均粒径
と比較して若干小さくなるが殆ど変らない。The acicular iron oxyhydroxide or acicular iron oxide usually has an average axial ratio of 3 or more, preferably 5 to 15, and the average particle diameter (long axis) is usually 1. 0μm or less,
It is preferably 0.1 to 1.0 μm. The acicular iron carbide fine particles thus produced are slightly smaller than the average axial ratio and average particle diameter of the raw material, but hardly changed.
【００２１】また、針状炭化鉄微粒子の製法における針
状オキシ水酸化鉄又は針状酸化鉄は、形状が針状であり
、主成分がオキシ水酸化鉄又は酸化鉄である限り、少量
の銅、マグネシウム、マンガン、ニツケルの酸化物、炭
酸塩； 珪素の酸化物； カリウム塩、ナトリウム塩等
を添加して成るものであつてもよい。[0021] In addition, as long as the acicular iron oxyhydroxide or acicular iron oxide used in the method for producing acicular iron carbide fine particles has an acicular shape and the main component is iron oxyhydroxide or iron oxide, a small amount of copper may be added. , magnesium, manganese, nickel oxides, carbonates; silicon oxides; potassium salts, sodium salts, etc. may be added.
【００２２】上記針状オキシ水酸化鉄は、特開昭６０−
１０８３０９号にあるように、その表面のｐＨが５以上
の場合は、より高保磁力を有する針状粒子が得られ、好
ましい。ｐＨが５未満の場合は、アルカリ（例えば水酸
化ナトリウム、水酸化カリウム、水酸化アンモニウム）
水溶液と接触させてｐＨを５以上とするのがよい。また
アルカリ処理した針状酸化鉄を用いることもできる。ア
ルカリ処理は、例えば被処理物を水酸化ナトリウム、水
酸化カリウム、水酸化アンモニウムのようなアルカリの
水溶液（例えば、ｐＨ８以上、好ましくは１０以上の水
溶液）と接触させて、必要ならば３０分〜１時間撹拌し
て、ロ別、乾燥することにより行なうことができる。[0022] The above-mentioned acicular iron oxyhydroxide is disclosed in Japanese Patent Application Laid-open No. 1986-
As described in No. 108309, when the pH of the surface is 5 or more, acicular particles having a higher coercive force can be obtained, which is preferable. If the pH is less than 5, use an alkali (e.g. sodium hydroxide, potassium hydroxide, ammonium hydroxide)
It is preferable to bring the pH to 5 or more by contacting with an aqueous solution. It is also possible to use acicular iron oxide treated with alkali. The alkaline treatment is carried out, for example, by bringing the object to be treated into contact with an alkaline aqueous solution (for example, an aqueous solution with a pH of 8 or more, preferably 10 or more) such as sodium hydroxide, potassium hydroxide, or ammonium hydroxide for 30 minutes or more if necessary. This can be done by stirring for 1 hour, filtering, and drying.
【００２３】なお、Ｃｏを被着した針状オキシ水酸化鉄
又は酸化鉄を用いることもできる。Ｃｏを被着するには
、Ｃｏ塩の水溶液（例えば、０．１〜１０重量％の稀薄
溶液）に針状オキシ水酸化鉄又は酸化鉄を投入して室温
ないし加温下に撹拌しアルカリ水溶液でアルカリ性とし
、必要ならば３０分〜１時間撹拌してロ別乾燥するのが
好ましい。[0023] It is also possible to use acicular iron oxyhydroxide or iron oxide coated with Co. To deposit Co, acicular iron oxyhydroxide or iron oxide is added to an aqueous solution of Co salt (for example, a dilute solution of 0.1 to 10% by weight) and stirred at room temperature or under heating to form an alkaline aqueous solution. It is preferable to make the mixture alkaline and, if necessary, stir it for 30 minutes to 1 hour and dry it separately.
【００２４】なお、原料は特開昭６０−１４１６１１号
に記載されるように、珪素化合物、ホウ素化合物、アル
ミニウム化合物、脂肪族カルボン酸もしくはその塩、リ
ン化合物又はチタン化合物などの焼結防止剤を被着して
用いることもできる。As described in JP-A-60-141611, the raw materials contain sintering inhibitors such as silicon compounds, boron compounds, aluminum compounds, aliphatic carboxylic acids or salts thereof, phosphorus compounds, or titanium compounds. It can also be used by being attached.
【００２５】好適な珪素化合物としては、水ガラスやシ
ランカツプリング剤等を挙げることができる。[0025] Suitable silicon compounds include water glass and silane coupling agents.
【００２６】好適に用いられる珪素化合物の具体例を挙
げれば、次のとおりである：γ−アミノプロピルトリエ
トキシシラン、Ｎ−（β−アミノエチル）−γ−アミノ
プロピルトリメトキシシラン、γ−ウレイドプロピルト
リエトキシシラン、γ−グリシドキシプロピルトリメト
キシシラン、β−（３，４−エポキシシクロヘキシル）
エチルトリメチルシラン、γ−メタクリロイルオキシプ
ロピルトリメトキシシラン、γ−メルカプトプロピルト
リメトキシシラン、γ−クロロプロピルトリメトキシシ
ラン、ビニルトリ（β−メトキシエトキシ）シラン、ビ
ニルトリエトキシシラン、ビニルトリクロロシラン、ビ
ニルトリアセトオキシシランなど。Specific examples of silicon compounds that are preferably used are as follows: γ-aminopropyltriethoxysilane, N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, γ-ureido. Propyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, β-(3,4-epoxycyclohexyl)
Ethyltrimethylsilane, γ-methacryloyloxypropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, γ-chloropropyltrimethoxysilane, vinyltri(β-methoxyethoxy)silane, vinyltriethoxysilane, vinyltrichlorosilane, vinyltriacetate such as oxysilane.
【００２７】また好ましいホウ素化合物としては、ホウ
酸とグリセリンのような隣接水酸基を有する多価アルコ
ールを反応させて、分子中に特異な形でホウ素を含む化
学構造を有する化合物、たとえばポリオキシエチレング
リセロールボレート・ラウレート、ポリオキシエチレン
グリセロールボレート・パルミテート、ポリオキシエチ
レングリセロールボレート・ステアレートなどから適宜
に選択したものが使用される。Preferred boron compounds include compounds having a chemical structure containing boron in a unique form in the molecule, such as polyoxyethylene glycerol, which is obtained by reacting boric acid with a polyhydric alcohol having adjacent hydroxyl groups such as glycerin. A material appropriately selected from borate/laurate, polyoxyethylene glycerol borate/palmitate, polyoxyethylene glycerol borate/stearate, etc. is used.
【００２８】更に好適なアルミニウム化合物としては、
アルミン酸カリ、アルミン酸ソーダなどが用いられる。[0028] More suitable aluminum compounds include:
Potassium aluminate, sodium aluminate, etc. are used.
【００２９】好適な脂肪族カルボン酸またはその塩とし
ては、例えばオレイン酸、 ヤシ油脂肪酸、オレイン酸
ナトリウムなどの炭素数１２〜２０の脂肪酸またはその
アルカリ金属（Ｎａ、Ｋなど）塩もしくはアルカリ土類
金属（カルシウム、マグネシウムなど）塩、アンモニウ
ム塩等を例示できる。Suitable aliphatic carboxylic acids or salts thereof include fatty acids having 12 to 20 carbon atoms such as oleic acid, coconut oil fatty acid, and sodium oleate, or their alkali metal (Na, K, etc.) salts or alkaline earth salts. Examples include metal (calcium, magnesium, etc.) salts, ammonium salts, and the like.
【００３０】好適なリン化合物としては、リン酸エステ
ル、リン酸塩等を挙げることができる。リン酸エステル
の具体例としては、アルキルフエノール型リン酸エステ
ル、アルキルリン酸エステル〔東邦化学（製）ＧＡＦＡ
Ｋシリーズ〕など、またリン酸塩の具体例としては例え
ば、ヘキサメタリン酸ナトリウム、ピロリン酸ナトリウ
ム、メタリン酸ナトリウム等を例示できる。[0030] Suitable phosphorus compounds include phosphoric acid esters and phosphates. Specific examples of phosphoric esters include alkylphenol type phosphoric esters, alkyl phosphoric esters [GAFA manufactured by Toho Chemical Co., Ltd.]
K series], and specific examples of phosphates include sodium hexametaphosphate, sodium pyrophosphate, and sodium metaphosphate.
【００３１】好ましいチタン化合物としては分子中に無
機物と結合する部分と有機物と結合する部分を持つチタ
ン有機化合物、たとえばジイソプロポキシ・ビス（アセ
チルアセトン）チタネート、ジ−ｎ−ブトキシ・ビス（
トリエタノールアミン）チタネート、ジヒドロキシ・ビ
ス（ラクテイツクアミド）チタネート、テトラオクチレ
ングリコールチタネートなどを挙げることができる。Preferred titanium compounds include titanium organic compounds having a moiety that binds to inorganic matter and a moiety that binds to organic matter in the molecule, such as diisopropoxy bis(acetylacetone) titanate, di-n-butoxy bis(
Examples include triethanolamine) titanate, dihydroxy bis(lactacamide) titanate, and tetraoctylene glycol titanate.
【００３２】これら焼結防止剤は１種又は２種以上併用
して用いることができる。その被着量はその種類にもよ
るが、ＳｉおよびＡｌ等の場合、一般に針状オキシ水酸
化鉄の重量を基準にして約３％以下を使用するが約０．
０１〜０．５重量％が好ましい。被着量が３％を越える
と炭化反応時に炭素析出触媒として作用し、非磁性物で
ある析出炭素量も増加し、磁化量低下の原因となるので
好ましくない。被着量が少なすぎると焼結が生じこれか
ら得られる磁性塗料組成物の分散性、充填性が悪くなり
、シート特性が劣る。被着処理は公知の方法によればよ
く、通常は上記焼結防止剤の適宜の濃度を有する水溶液
に針状オキシ水酸化鉄の粒子を分散させた後、又はその
後ｐＨを変化させた後、この粒子を濾取し乾燥する方法
が好ましい。These sintering inhibitors can be used alone or in combination of two or more. The amount of the deposit depends on the type, but in the case of Si, Al, etc., it is generally used in an amount of about 3% or less based on the weight of the acicular iron oxyhydroxide, but about 0.
01 to 0.5% by weight is preferred. If the amount of deposit exceeds 3%, it is not preferable because it acts as a carbon deposition catalyst during the carbonization reaction, and the amount of deposited carbon, which is a non-magnetic substance, increases, causing a decrease in the amount of magnetization. If the amount of coating is too small, sintering will occur and the resulting magnetic coating composition will have poor dispersibility and filling properties, resulting in poor sheet properties. The adhesion treatment may be carried out by a known method, usually after dispersing acicular iron oxyhydroxide particles in an aqueous solution having an appropriate concentration of the above-mentioned sintering inhibitor, or after changing the pH. A method in which the particles are filtered and dried is preferred.
【００３３】本発明の出発原料として用いる針状炭化鉄
微粒子の製法（ａ）及び（ｂ）において用いられる炭素
原子を含有しない還元剤の代表例としてはＨ２、ＮＨ２
ＮＨ２等を挙げることができる。Typical examples of reducing agents that do not contain carbon atoms used in the methods (a) and (b) for producing acicular iron carbide fine particles used as starting materials in the present invention include H2 and NH2.
Examples include NH2.
【００３４】また（ｂ）における炭素原子を含有する還
元剤としては下記化合物の少なくとも１種以上を使用で
きる。As the reducing agent containing carbon atoms in (b), at least one of the following compounds can be used.
【００３５】■ ＣＯ
■ 脂肪族、鎖状もしくは環状の、飽和もしくは不飽和
炭化水素、例えばメタン、プロパン、ブタン、シクロヘ
キサン、メチルシクロヘキサン、アセチレン、エチレン
、プロピレン、ブタジエン、イソプレン、タウンガスな
ど。■ 芳香族炭化水素、例えばベンゼン、トルエン、
キシレン、沸点１５０℃以下のこれらのアルキル、アル
ケニル誘導体。■ 脂肪族アルコール、例えばメタノー
ル、エタノール、プロパノール、シクロヘキサノール。
■ エステル、例えばギ酸メチル、酢酸エチル等の沸点
１５０℃以下のエステル。■ エーテル、例えば低級ア
ルキルエーテル、ビニルエーテル等の沸点１５０℃以下
のエーテル。■ アルデヒド、例えばホルムアルデヒド
、アセトアルデヒド等の沸点１５０℃以下のアルデヒド
。■ ケトン、例えばアセトン、メチルエチルケトン、
メチルイソブチルケトン等の沸点１５０℃以下のケトン
。■ CO ■ Aliphatic, linear or cyclic, saturated or unsaturated hydrocarbons, such as methane, propane, butane, cyclohexane, methylcyclohexane, acetylene, ethylene, propylene, butadiene, isoprene, town gas and the like. ■ Aromatic hydrocarbons, such as benzene, toluene,
xylene, these alkyl and alkenyl derivatives having a boiling point of 150°C or less. ■ Aliphatic alcohols such as methanol, ethanol, propanol, cyclohexanol. (2) Esters, such as methyl formate and ethyl acetate, having a boiling point of 150°C or less. (2) Ethers, such as lower alkyl ethers and vinyl ethers, having a boiling point of 150°C or less. (2) Aldehydes, such as formaldehyde and acetaldehyde, which have a boiling point of 150°C or less. ■ Ketones, such as acetone, methyl ethyl ketone,
Ketones with a boiling point of 150°C or less, such as methyl isobutyl ketone.
【００３６】特に好ましい炭素原子を含有する還元剤は
ＣＯ、ＣＨ３ＯＨ、ＨＣＯＯＣＨ３、炭素数１〜５の飽
和または不飽和の脂肪族炭化水素である。Particularly preferred reducing agents containing carbon atoms are CO, CH3OH, HCOOCH3, and saturated or unsaturated aliphatic hydrocarbons having 1 to 5 carbon atoms.
【００３７】前記（ａ）工程において、炭素原子を含有
しない還元剤は希釈して使用してもよい。希釈剤として
は、例えばＮ２、アルゴン、ヘリウム等を挙げることが
できる。また希釈率は任意に選択でき、例えば約１．１
〜１０倍（容量比）に希釈するのが好ましい。接触温度
、接触時間、流速等の接触条件は、例えば針状オキシ水
酸化鉄又は針状酸化鉄の製造履歴、平均軸比、平均粒径
、比表面積、及び所望とする特性に応じ変動するため、
適宜選択するのがよい。好ましい接触温度は、約２００
〜７００℃、より好ましくは約３００〜４００℃、好ま
しい接触時間は約０．５〜６時間である。好ましい流速
は、原料の鉄化合物１ｇ当り希釈剤を除いて約１〜１０
００ｍｌＳ．Ｔ．Ｐ／分、好ましくは約５〜５００ｍｌ
Ｓ．Ｔ．Ｐ／分である。なお、接触圧力は、希釈剤を
も含めて、１〜２気圧が常用されるが、特に制限はない
。In the step (a), the reducing agent containing no carbon atoms may be used diluted. Examples of the diluent include N2, argon, helium, and the like. Further, the dilution rate can be selected arbitrarily, for example, about 1.1
It is preferable to dilute to 10 times (volume ratio). Contact conditions such as contact temperature, contact time, and flow rate vary depending on, for example, the manufacturing history of acicular iron oxyhydroxide or acicular iron oxide, average axial ratio, average particle diameter, specific surface area, and desired properties. ,
It is best to choose as appropriate. The preferred contact temperature is about 200
~700°C, more preferably about 300-400°C, and the preferred contact time is about 0.5-6 hours. The preferred flow rate is about 1 to 10% per gram of raw iron compound, excluding diluent.
00mlS. T. P/min, preferably about 5-500ml
S. T. P/min. The contact pressure, including the diluent, is usually 1 to 2 atmospheres, but is not particularly limited.
【００３８】前記（ｂ）工程においても炭素原子を含有
する還元剤もしくはこれと炭素原子を含有しない還元剤
との混合物を希釈してあるいは希釈せずに使用できる。
混合物を用いる場合、その混合比は適宜に選択すること
ができるが、通常は炭素原子を含有する還元剤と炭素原
子を含有しない還元剤の容量比が１／０．０５〜１／５
とするのが好ましい。接触条件も同様に適宜選択するこ
とができるが、好ましい接触温度は約２５０〜４００℃
、より好ましくは約３００〜４００℃、好ましい接触時
間は、（ａ）工程を行つた場合は約０．５〜６時間、（
ａ）工程のない場合は約１〜１２時間である。好ましい
流速は、原料の鉄化合物１ｇ当り希釈剤を除いて約１〜
１０００ｍｌ Ｓ．Ｔ．Ｐ／分、好ましくは５〜５００
ｍｌ Ｓ．Ｔ．Ｐ／分である。なお、接触圧力は、希釈
剤をも含めて、１〜２気圧が常用されるが、特に制限は
ない。Also in the step (b), a reducing agent containing a carbon atom or a mixture of this and a reducing agent not containing a carbon atom can be used diluted or undiluted. When using a mixture, the mixing ratio can be selected as appropriate, but usually the volume ratio of the reducing agent containing carbon atoms and the reducing agent containing no carbon atoms is 1/0.05 to 1/5.
It is preferable that The contact conditions can be similarly selected as appropriate, but the preferred contact temperature is about 250 to 400°C.
, more preferably about 300 to 400°C, and the preferable contact time is about 0.5 to 6 hours when step (a) is carried out, (
a) If there is no step, it is about 1 to 12 hours. The preferred flow rate is about 1 to 1 g per gram of raw iron compound, excluding diluent.
1000ml S. T. P/min, preferably 5-500
ml S. T. P/min. The contact pressure, including the diluent, is usually 1 to 2 atmospheres, but is not particularly limited.
【００３９】上記で得られる生成物は炭化鉄であるが若
干の析出炭素及び酸化鉄も存在し得る。そして炭化鉄の
主成分はＦｅ５Ｃ２であり、Ｆｅ７Ｃ３、ＦｅＣ、Ｆｅ
３Ｃが含まれ得る。The product obtained above is iron carbide, but some precipitated carbon and iron oxide may also be present. The main component of iron carbide is Fe5C2, Fe7C3, FeC, Fe
3C may be included.
【００４０】本発明の炭素を含有する針状金属鉄微粒子
は前記針状炭化鉄微粒子に炭素原子を含有しない還元剤
を接触させることにより得ることができる。炭素原子を
含有しない還元剤としては前述と同様、Ｈ２、ＮＨ２Ｎ
Ｈ２等を例示することができる。好ましい接触温度は約
３００〜５００℃、好ましい接触時間は約０．５〜６時
間である。必要により前述と同様の希釈剤を使用できる
。好ましい流速は針状炭化鉄微粒子１ｇ当り希釈剤を除
いて約１〜１０００ｍｌ Ｓ．Ｔ．Ｐ／分である。尚、
接触圧力は希釈剤をも含めて１〜２気圧が常用されるが
特に制限はない。The carbon-containing acicular metallic iron fine particles of the present invention can be obtained by contacting the acicular iron carbide fine particles with a reducing agent that does not contain carbon atoms. As mentioned above, H2, NH2N are used as reducing agents that do not contain carbon atoms.
H2 etc. can be exemplified. The preferred contact temperature is about 300-500°C, and the preferred contact time is about 0.5-6 hours. Diluents similar to those mentioned above can be used if necessary. A preferred flow rate is about 1 to 1000 ml S.C. per 1 g of acicular iron carbide fine particles, excluding diluent. T. P/min. still,
The contact pressure, including the diluent, is usually 1 to 2 atmospheres, but is not particularly limited.
【００４１】本発明の炭素を含有する針状金属鉄微粒子
は、炭素を針状金属鉄微粒子に対して通常２〜２０重量
％、好ましくは５〜１５重量％含有する。炭素含有量が
これより多いと磁化量の向上が少なく、これより少ない
と耐食性が劣る。炭素含有量は出発原料である炭化鉄中
の炭素及び析出した炭素の合計の全炭素量で表される。
本発明の好ましい範囲において存在する炭素は元素分析
により含有量が確かめられるのみで、Ｘ線では炭化鉄と
しても黒鉛としても検出されず、その形態は無定形とも
推定されるが詳細は不明である。本発明の針状金属鉄微
粒子は平均軸比が３〜１５、平均粒径（長軸）は通常１
．０μｍ以下、好適には０．１〜１．０μｍである。The carbon-containing acicular metallic iron fine particles of the present invention usually contain carbon in an amount of 2 to 20% by weight, preferably 5 to 15% by weight, based on the acicular metallic iron fine particles. If the carbon content is more than this, the improvement in the amount of magnetization will be small, and if it is less than this, the corrosion resistance will be poor. The carbon content is expressed as the total amount of carbon, which is the sum of carbon in iron carbide, which is a starting material, and precipitated carbon. The content of carbon present in the preferred range of the present invention can only be confirmed by elemental analysis, and it is not detected as iron carbide or graphite by X-rays, and its form is presumed to be amorphous, but the details are unknown. . The acicular metallic iron fine particles of the present invention have an average axial ratio of 3 to 15 and an average particle diameter (long axis) of usually 1.
．． It is 0 μm or less, preferably 0.1 to 1.0 μm.
【００４２】本発明の磁性塗料組成物は上記本発明の針
状鉄微粒子を結合剤と共に有機溶媒に分散することによ
り得られる。尚、磁性塗料組成物には分散剤、潤滑剤、
研磨剤、帯電防止剤等を必要に応じ加えることができる
。The magnetic coating composition of the present invention can be obtained by dispersing the acicular iron fine particles of the present invention together with a binder in an organic solvent. In addition, the magnetic coating composition contains a dispersant, a lubricant,
Abrasives, antistatic agents, etc. can be added as necessary.
【００４３】本発明において使用される結合剤としては
、従来公知の熱可塑性樹脂、熱硬化性樹脂又は反応型樹
脂やこれらの混合物が使用される。As the binder used in the present invention, conventionally known thermoplastic resins, thermosetting resins, reactive resins, and mixtures thereof are used.
【００４４】熱可塑性樹脂として、軟化温度が１５０℃
以下、平均分子量が １００００〜２０００００、重合
度が約２００〜２０００程度のもので、例えば塩化ビニ
ル酢酸ビニル共重合体、塩化ビニル塩化ビニリデン共重
合体、塩化ビニルアクリロニトリル共重合体、アクリル
酸エステルアクリロニトリル共重合体、アクリル酸エス
テル塩化ビニリデン共重合体、アクリル酸エステルスチ
レン共重合体、メタクリル酸エステルアクリロニトリル
共重合体、メタクリル酸エステル塩化ビニリデン共重合
体、メタクリル酸エステルスチレン共重合体、ウレタン
エラストマー、ポリ弗化ビニル、塩化ビニリデンアクリ
ロニトリル共重合体、ブタジエンアクリロニトリル共重
合体、ポリアミド樹脂、ポリビニルブチラール、セルロ
ース誘導体（セルロースアセテートブチレート、セルロ
ースダイアセテート、セルローストリアセテート、セル
ロースプロピオネート、ニトロセルロース等）、スチレ
ンブタジエン共重合体、ポリエステル樹脂、クロロビニ
ルエーテルアクリル酸エステル共重合体、アミノ樹脂、
各種の合成ゴム系の熱可塑性樹脂及びこれらの混合物等
が使用される。[0044] As a thermoplastic resin, the softening temperature is 150°C.
Below, the average molecular weight is 10,000 to 200,000 and the degree of polymerization is about 200 to 2,000, such as vinyl chloride vinyl acetate copolymer, vinyl chloride vinylidene chloride copolymer, vinyl chloride acrylonitrile copolymer, acrylic acid ester acrylonitrile copolymer, etc. Polymer, acrylic acid ester vinylidene chloride copolymer, acrylic acid ester styrene copolymer, methacrylic acid ester acrylonitrile copolymer, methacrylic acid ester vinylidene chloride copolymer, methacrylic acid ester styrene copolymer, urethane elastomer, polyfluoride Vinyl chloride, vinylidene chloride acrylonitrile copolymer, butadiene acrylonitrile copolymer, polyamide resin, polyvinyl butyral, cellulose derivatives (cellulose acetate butyrate, cellulose diacetate, cellulose triacetate, cellulose propionate, nitrocellulose, etc.), styrene butadiene copolymer Polymer, polyester resin, chlorovinyl ether acrylate copolymer, amino resin,
Various synthetic rubber-based thermoplastic resins and mixtures thereof are used.
【００４５】熱硬化性樹脂又は反応型樹脂としては、塗
布液の状態では２０００００以下の分子量であり、塗布
、乾燥後に加熱することにより、縮合、付加等の反応に
より分子量は無限大のものとなる。又、これらの樹脂の
なかで、樹脂が熱分解するまでの間に軟化又は溶融しな
いものが好ましい。具体的には例えばフエノール樹脂、
エポキシ樹脂、ポリウレタン硬化型樹脂、尿素樹脂、メ
ラミン樹脂、アルキツド樹脂、シリコン樹脂、アクリル
系反応樹脂、エポキシーポリアミド樹脂、高分子量ポリ
エステル樹脂とイソシアネートプレポリマーの混合物、
メタクリル酸塩共重合体とジイソシアネートプレポリマ
ーの混合物、ポリエステルポリオールとポリイソシアネ
ートの混合物、尿素ホルムアルデヒド樹脂、低分子量グ
リコール／高分子量ジオール／トリフエニルメタントリ
イソシアネートの混合物、ポリアミン樹脂及びこれらの
混合物等である。The thermosetting resin or reactive resin has a molecular weight of 200,000 or less in the state of a coating solution, and when heated after coating and drying, the molecular weight becomes infinite due to reactions such as condensation and addition. . Also, among these resins, those that do not soften or melt before the resin is thermally decomposed are preferred. Specifically, for example, phenolic resin,
Epoxy resin, polyurethane curable resin, urea resin, melamine resin, alkyd resin, silicone resin, acrylic reaction resin, epoxy polyamide resin, mixture of high molecular weight polyester resin and isocyanate prepolymer,
Mixtures of methacrylate copolymers and diisocyanate prepolymers, mixtures of polyester polyols and polyisocyanates, urea formaldehyde resins, mixtures of low molecular weight glycols/high molecular weight diols/triphenylmethane triisocyanates, polyamine resins, and mixtures thereof, etc. .
【００４６】これらの結合剤の単独又は組合わされたも
のが使われ、他に添加剤が加えられる。針状粒子と結合
剤との混合割合は、重量比で針状粒子１００重量部に対
して結合剤１０〜４００重量部、好ましくは３０〜２０
０重量部の範囲で使用される。These binders may be used alone or in combination, and other additives may be added. The mixing ratio of the acicular particles and the binder is 10 to 400 parts by weight, preferably 30 to 20 parts by weight of the binder to 100 parts by weight of the acicular particles.
It is used in a range of 0 parts by weight.
【００４７】有機溶媒としては、アセトン、メチルエチ
ルケトン、メチルイソブチルケトン、シクロヘキサノン
等のケトン系 ； メタノール、エタノール、プロパノ
ール、ブタノール等のアルコール系 ； 酢酸メチル、
酢酸エチル、酢酸ブチル、乳酸エチル、酢酸グリコール
、モノエチルエーテル等のエステル系 ； エーテル、
グリコールジメチルエーテル、グリコールモノエチルエ
ーテル、ジオキサン等のグリコールエーテル系 ； ベ
ンゼン、トルエン、キシレン等のタール系（芳香族炭化
水素） ； メチレンクロライド、エチレンクロライド
、四塩化炭素、クロロホルム、エチレンクロルヒドリン
、ジクロルベンゼン等の塩素化炭化水素等が使用できる
。Examples of organic solvents include ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, and cyclohexanone; alcohols such as methanol, ethanol, propanol, and butanol; methyl acetate;
Ester systems such as ethyl acetate, butyl acetate, ethyl lactate, glycol acetate, monoethyl ether; ether,
Glycol ethers such as glycol dimethyl ether, glycol monoethyl ether, and dioxane; Tars (aromatic hydrocarbons) such as benzene, toluene, and xylene; Methylene chloride, ethylene chloride, carbon tetrachloride, chloroform, ethylene chlorohydrin, and dichlor Chlorinated hydrocarbons such as benzene can be used.
【００４８】分散剤としては、カプリル酸、カプリン酸
、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリ
ン酸、オレイン酸、エライジン酸、リノール酸、リノレ
ン酸、ステアロール酸等の炭素数１２〜１８個の脂肪酸
（Ｒ１ＣＯＯＨ、Ｒ１は炭素数１１〜１７のアルキル基
） ； 前記の脂肪酸のアルカリ金属（Ｌｉ、Ｎａ、Ｋ
等）またはアルカリ土類金属（Ｍｇ、Ｃａ、Ｂａ等）か
ら成る金属石鹸 ； レシチン等が使用される。この他
に炭素数１２以上の高級アルコール、及びこれらの他に
硫酸エステル等も使用可能である。これらの分散剤は、
結合剤１００重量部に対して１〜２０重量部の範囲で添
加される。Examples of dispersants include those having 12 to 18 carbon atoms, such as caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, and stearolic acid. Fatty acid (R1COOH, R1 is an alkyl group having 11 to 17 carbon atoms); Alkali metals (Li, Na, K
etc.) or metal soaps made of alkaline earth metals (Mg, Ca, Ba, etc.); lecithin, etc. are used. In addition to these, higher alcohols having 12 or more carbon atoms and sulfuric esters can also be used. These dispersants are
It is added in an amount of 1 to 20 parts by weight per 100 parts by weight of the binder.
【００４９】潤滑剤としては、シリコンオイル、グラフ
アイト、二硫化モリブデン、二硫化タングステン、炭素
数１２〜１６の一塩基性脂肪酸と炭素数３〜１２の一価
のアルコールから成る脂肪酸エステル類、炭素数１７以
上の一塩基性脂肪酸と該脂肪酸の炭素数と合計して炭素
数が２１〜２３と成る一価のアルコールから成る脂肪酸
エステル等が使用できる。これらの潤滑剤は、結合剤１
００重量部に対して０．２〜２０重量部の範囲で添加さ
れる。As the lubricant, silicone oil, graphite, molybdenum disulfide, tungsten disulfide, fatty acid esters consisting of a monobasic fatty acid with 12 to 16 carbon atoms and a monohydric alcohol with 3 to 12 carbon atoms, carbon A fatty acid ester consisting of a monobasic fatty acid having a number of 17 or more and a monohydric alcohol having 21 to 23 carbon atoms in total can be used. These lubricants are binder 1
It is added in an amount of 0.2 to 20 parts by weight per 00 parts by weight.
【００５０】研磨剤としては、一般に使用される材料で
溶融アルミナ、炭化ケイ素、酸化クロム、コランダム、
人造コランダム、ダイアモンド、人造ダイアモンド、ザ
クロ石、エメリー（主成分：コランダムと磁鉄鉱）等が
使用される。これらの研磨剤は平均粒子径が０．０５〜
５μｍの大きさのものが使用され、特に好ましくは０．
１〜２μｍである。これらの研磨剤は、結合剤１００重
量部に対して７〜２０重量部の範囲で添加される。As the abrasive, commonly used materials include fused alumina, silicon carbide, chromium oxide, corundum,
Artificial corundum, diamond, artificial diamond, garnet, emery (main ingredients: corundum and magnetite), etc. are used. These abrasives have an average particle size of 0.05~
A size of 5 μm is used, particularly preferably a size of 0.5 μm.
It is 1 to 2 μm. These abrasives are added in an amount of 7 to 20 parts by weight based on 100 parts by weight of the binder.
【００５１】帯電防止剤として、サポニンなどの天然界
面活性剤 ； アルキレンオキサイド系、グリセリン系
、グリシドール系などのノニオン界面活性剤 ； 高級
アルキルアミン類、第４級アンモニウム塩類、ピリジン
その他の複素環類、ホスホニウム又はスルホニウム類な
どのカチオン界面活性剤 ； カルボン酸、スルホン酸
、燐酸、硫酸エステル基、燐酸エステル基等の酸性基を
含むアニオン界面活性剤 ； アミノ酸類、アミノスル
ホン酸類、アミノアルコールの硫酸または燐酸エステル
類等の両性活性剤などが使用される。これらの帯電防止
剤は、単独または混合して添加してもよい。これらは帯
電防止剤として用いられるものであるが、時としてその
他の目的、たとえば分散、磁気特性の改良、潤滑性の改
良、塗布助剤として適用される場合もある。これらの帯
電防止剤は、結合剤１００重量部に対して１〜２重量部
の範囲で添加される。As antistatic agents, natural surfactants such as saponin; nonionic surfactants such as alkylene oxide type, glycerin type, and glycidol type; higher alkylamines, quaternary ammonium salts, pyridine and other heterocycles, Cationic surfactants such as phosphonium or sulfoniums; Anionic surfactants containing acidic groups such as carboxylic acids, sulfonic acids, phosphoric acids, sulfuric ester groups, and phosphoric ester groups; Sulfuric or phosphoric acids of amino acids, aminosulfonic acids, and amino alcohols Ampholytic activators such as esters are used. These antistatic agents may be added alone or in combination. Although these are used as antistatic agents, they are sometimes applied for other purposes, such as dispersion, improving magnetic properties, improving lubricity, and as coating aids. These antistatic agents are added in an amount of 1 to 2 parts by weight per 100 parts by weight of the binder.
【００５２】本発明の磁気記録媒体は、上記磁性塗料組
成物を基体（支持体）上に塗布することにより得られる
。The magnetic recording medium of the present invention can be obtained by coating the above magnetic coating composition on a substrate (support).
【００５３】支持体の厚みは５〜５０μｍ程度、好まし
くは１０〜４０μｍ程度が良く、素材としてはポリエチ
レンテレフタレート、ポリエチレン−２，６−ナフタレ
ート等のポリエステル類、ポリプロピレン等のポリオレ
フイン類、セルローストリアセテート、セルロースダイ
アセテート等のセルロース誘導体、ポリカーボネート等
が使用される。The thickness of the support is preferably about 5 to 50 μm, preferably about 10 to 40 μm, and materials include polyesters such as polyethylene terephthalate and polyethylene-2,6-naphthalate, polyolefins such as polypropylene, cellulose triacetate, and cellulose. Cellulose derivatives such as diacetate, polycarbonate, etc. are used.
【００５４】上記の支持体は、帯電防止、転写防止等の
目的で、磁性層を設けた側の反対の面がいわゆるバツク
コート（ｂａｃｋｃｏａｔ）されてもよい。The above-mentioned support may be coated with a so-called backcoat on the surface opposite to the side on which the magnetic layer is provided for the purpose of preventing static electricity, preventing transfer, and the like.
【００５５】又、支持体の形態は、テープ、シート、カ
ード、デイスク、ドラム等のいずれでも良く、形態に応
じて種々の材料が必要に応じて選択される。The support may be in the form of a tape, sheet, card, disk, drum, etc., and various materials may be selected as necessary depending on the form.
【００５６】支持体上へ前記の磁性塗料組成物を塗布す
る方法としては、エアードクターコート、ブレードコー
ト、エアナイフコート、スクイズコート、含浸コート、
リバースロールコート、トランスフアーロールコート、
グラビアコート、キスコート、キヤストコート、スプレ
ーコート等が利用でき、その他の方法も可能である。Methods for applying the above-mentioned magnetic coating composition onto the support include air doctor coating, blade coating, air knife coating, squeeze coating, impregnation coating,
reverse roll coat, transfer roll coat,
Gravure coating, kiss coating, cast coating, spray coating, etc. can be used, and other methods are also possible.
【００５７】この様な方法により、支持体上に塗布され
た磁性層は、必要により層中の磁性粉末を配向させる処
理を施したのち、形成した磁性層を乾燥する。又必要に
より表面平滑化加工を施したり、所望の形状に裁断した
りして、本発明の磁気記録媒体を製造する。この場合、
配向磁場は、交流または直流で約５００〜５０００ガウ
ス程度であり、乾燥温度は約５０〜１００℃程度、乾燥
時間は約３〜１０分間程度である。By such a method, the magnetic layer coated on the support is subjected to a treatment for orienting the magnetic powder in the layer, if necessary, and then the formed magnetic layer is dried. Further, the magnetic recording medium of the present invention is manufactured by subjecting it to surface smoothing processing and cutting it into a desired shape, if necessary. in this case,
The orientation magnetic field is about 500 to 5000 Gauss in alternating current or direct current, the drying temperature is about 50 to 100° C., and the drying time is about 3 to 10 minutes.
【００５８】[0058]
【実施例】以下に実施例及び比較例を挙げて詳しく説明
する。実施例において、各種特性等はそれぞれ次の方法
によつて求めた。
（１） 磁気特性
実施例１〜２及び比較例１〜３は次の方法によつて求め
る。ホール素子を用いたガウスメーターにより試料充填
率０．２で、測定磁場５ｋＯｅで、保磁力（Ｈｃ、充填
率０．２で、測定磁場５ｋＯｅで、保磁力（Ｈｃ、Ｏｅ
）、飽和磁化量（σｓ、ｅｍｕ／ｇ）及び角型比（Ｓｑ
）を測定する。また実施例３，４，５，６、比較例４は
ガウスメーターにかえて振動試料型磁化特性測定装置を
用いて粉体は測定磁場１０ｋＯｅで、シートは５ｋＯｅ
で特性を測定する。
（２） Ｃ， Ｈ及びＮの元素分析
元素分析は（株）柳本製作所製のＭＴ２ ＣＨＮ ＣＯ
ＲＤＥＲ Ｙａｎａｃｏを使用し、９００℃で酸素（ヘ
リウムキヤリヤ）を通じることにより常法に従つて行う
。
（３） 比表面積 窒素吸着法によるＢＥＴ比表面積
（４） 耐食性（耐酸化性） （１−Ｂ／Ａ）×１
００ （％）
Ａ： 飽和磁化量 σｓ（ｅｍｕ／ｇ）Ｂ： １００
℃の空気中で８時間放置後のσｓ[Examples] A detailed explanation will be given below with reference to Examples and Comparative Examples. In the Examples, various characteristics etc. were determined by the following methods. (1) Magnetic properties Examples 1 to 2 and Comparative Examples 1 to 3 are determined by the following method. With a sample filling factor of 0.2 and a measuring magnetic field of 5 kOe using a Gauss meter using a Hall element, the coercive force (Hc, Oe) is measured.
), saturation magnetization (σs, emu/g) and squareness ratio (Sq
) to measure. Furthermore, in Examples 3, 4, 5, 6, and Comparative Example 4, a vibrating sample type magnetization characteristic measuring device was used instead of the Gaussmeter, and the powder was measured in a magnetic field of 10 kOe and the sheet was measured at 5 kOe.
to measure the characteristics. (2) Elemental analysis of C, H and N Elemental analysis was performed using MT2 CHN CO manufactured by Yanagimoto Seisakusho Co., Ltd.
This is carried out in a conventional manner using an RDER Yanaco at 900° C. by passing oxygen (helium carrier) through. (3) Specific surface area BET specific surface area by nitrogen adsorption method (4) Corrosion resistance (oxidation resistance) (1-B/A) x 1
00 (%) A: Saturation magnetization σs (emu/g) B: 100
σs after being left in air at ℃ for 8 hours
【００５９】実施例１
平均粒径 ０．７μｍ（長軸）、平均軸比１０の針状ゲ
ーサイト粒子 ６ｋｇを水 １９４ｌ中に分散させ、少
量のアルカリ溶液（ＮａＯＨ２０％ｓｏｌｎ）を添加し
ｐＨ１３以上に調整した後、水ガラス３号（Ｎａ２Ｏ・
３ＳｉＯ２）１ｋｇ（α−ＦｅＯＯＨに対しＳｉ分約２
．６％）を添加し、撹拌する。この水溶液に１Ｎ−ＨＣ
ｌを添加し、ｐＨ５に調整し、１時間後に濾過を行い乾
燥した。この処理した粒子粉末をマツフル炉に入れ、６
００℃で１時間加熱してα−Ｆｅ２Ｏ３粉末を得た。Example 1 6 kg of acicular goethite particles with an average particle diameter of 0.7 μm (long axis) and an average axial ratio of 10 were dispersed in 194 liters of water, and a small amount of alkaline solution (NaOH 20% soln) was added to adjust the pH to 13 or higher. After adjusting to water glass No. 3 (Na2O・
3SiO2) 1kg (Si content approximately 2 for α-FeOOH
．． 6%) and stir. Add 1N-HC to this aqueous solution.
1 was added to adjust the pH to 5, and after 1 hour, it was filtered and dried. This treated particle powder was put into a Matsufuru furnace, and 6
The mixture was heated at 00°C for 1 hour to obtain α-Fe2O3 powder.
【００６０】このα−Ｆｅ２Ｏ３粉末３ｋｇを反応管に
入れ、ＣＯを９０ｌ／ｍｉｎの流速で流しながら３６５
℃で８時間処理した。ガスを窒素にかえ、室温付近まで
冷却した後、徐々にガスを空気にかえ、炭化鉄粉体を得
た。生成物のＸ線回折パターン（Ｃｕ Ｋα線）はＡＳ
ＴＭのＸ−ｒａｙ Ｐｏｗｄｅｒ Ｄａｔａ Ｆｉｌｅ
２０−５０９のＦｅ５Ｃ２と一致した。この粉末４
０ｇを取り反応管に入れ、水素を５ｌ／ｍｉｎ流しなが
ら３２０℃で３時間処理した。ガスを窒素にかえ、室温
付近まで冷却した後徐々にガスを空気にかえて本発明の
粉体を得た。生成物のＸ線回折パターンはＡＳＴＭのＸ
−ｒａｙ Ｐｏｗｄｅｒ Ｄａｔａ Ｆｉｌｅの６−６
９６ α−Ｆｅと一致した。透過型電子顕微鏡観察によ
り針状の形状が良好に保たれていることを確認した。こ
の本発明の粉体の磁気特性は保磁力Ｈｃ＝１２４０Ｏｅ
、飽和磁化量σｓは１４６ｅｍｕ／ｇであり、全炭素量
は１２％、窒素吸着法によるＢＥＴ比表面積は５４ｍ２
／ｇであつた。耐食試験の結果、この本発明の粉体のσ
ｓは１３％低下した。又、この粉体 ２０ｇ、変性ポリ
ウレタン ５ｇを溶剤 ６０ｇ中で混合、分散させて磁
性塗料を調製しポリエチレンテレフタレート（ＰＥＴ）
フイルム上に厚み約５μに塗布して磁気シートを製作し
た。このシートの保磁力は１２８０Ｏｅ、飽和磁束密度
は２４００Ｇ、角型比は０．７６であつた。[0060] 3 kg of this α-Fe2O3 powder was put into a reaction tube, and while CO was flowing at a flow rate of 90 l/min, 365
It was treated at ℃ for 8 hours. After changing the gas to nitrogen and cooling it to around room temperature, the gas was gradually changed to air to obtain iron carbide powder. The X-ray diffraction pattern (Cu Kα radiation) of the product is AS
TM's X-ray Powder Data File
It matched with Fe5C2 of 20-509. This powder 4
0 g was taken and put into a reaction tube, and treated at 320°C for 3 hours while flowing hydrogen at 5 l/min. The gas was changed to nitrogen, and after cooling to around room temperature, the gas was gradually changed to air to obtain a powder of the present invention. The X-ray diffraction pattern of the product is ASTM
-ray Powder Data File 6-6
96 α-Fe. It was confirmed by transmission electron microscopy that the needle-like shape was well maintained. The magnetic properties of the powder of the present invention are coercive force Hc=1240Oe
, the saturation magnetization σs is 146 emu/g, the total carbon content is 12%, and the BET specific surface area by nitrogen adsorption method is 54 m2.
/g. As a result of the corrosion resistance test, the σ of the powder of the present invention was
s decreased by 13%. Also, 20g of this powder and 5g of modified polyurethane were mixed and dispersed in 60g of solvent to prepare a magnetic paint, and polyethylene terephthalate (PET) was prepared.
A magnetic sheet was produced by coating a film to a thickness of approximately 5 μm. This sheet had a coercive force of 1280 Oe, a saturation magnetic flux density of 2400 G, and a squareness ratio of 0.76.
【００６１】実施例２
実施例１で得たα−Ｆｅ２Ｏ３ ４０ｇを反応管に入れ
ＣＯを５ｌ／ｍｉｎの流速で流しながら３６５℃で３．
５時間処理した後、ガスを水素に切り替え、更に１時間
処理した。ガスを窒素にかえ、室温付近まで冷却した後
、徐々にガスを空気にかえ粉末を得た。結果を表１に示
す。Example 2 40 g of α-Fe2O3 obtained in Example 1 was placed in a reaction tube and heated at 365°C for 3.5 hours while flowing CO at a flow rate of 5 l/min.
After treatment for 5 hours, the gas was switched to hydrogen and treatment was continued for an additional 1 hour. After changing the gas to nitrogen and cooling it to around room temperature, the gas was gradually changed to air to obtain a powder. The results are shown in Table 1.
【００６２】実施例３
平均粒径 ０．４μｍ（長軸）、平均軸比１０の針状ゲ
ーサイト粒子 １ｋｇを水 ２０ｌ中に分散させ、少量
のアルカリ溶液（ＮａＯＨ２０％ｓｏｌｎ）を添加しｐ
Ｈ１３以上に調整した後、水ガラス３号 ０．０２ｋｇ
（α−ＦｅＯＯＨに対しＳｉ分約０．２７％）を添加し
、ｐＨ５に調整し、１時間後に濾過を行い乾燥した。Example 3 1 kg of acicular goethite particles with an average particle diameter of 0.4 μm (long axis) and an average axial ratio of 10 were dispersed in 20 liters of water, and a small amount of alkaline solution (NaOH 20% soln) was added.
After adjusting to H13 or higher, water glass No. 3 0.02kg
(Si content: about 0.27% based on α-FeOOH) was added, the pH was adjusted to 5, and after 1 hour, the mixture was filtered and dried.
【００６３】この処理した粒子粉末をマツフル炉に入れ
、６００℃で１時間加熱してα−Ｆｅ２Ｏ３粉末を得た
。[0063] The treated powder particles were placed in a Matsufuru furnace and heated at 600°C for 1 hour to obtain α-Fe2O3 powder.
【００６４】この酸化鉄粉末 ０．５ｋｇを反応管に入
れ、ＣＯを９０ｌ／ｍｉｎの流速で流しながら３６５℃
で５時間処理した。ガスを窒素にかえ、室温付近まで冷
却した後、徐々にガスを空気にかえ、炭化鉄粉体を得た
。図１に示す生成物のＸ線回折パターンはＡＳＴＭのＸ
−ｒａｙ Ｐｏｗｄｅｒ Ｄａｔａ Ｆｉｌｅ ２０
−５０９のＦｅ５Ｃ２と一致した。この粉末４０ｇを取
り反応管に入れ、水素を５ｌ／ｍｉｎの流速で流しなが
ら３２０℃で２時間処理した。ガスを窒素にかえ、室温
付近まで冷却した後徐々にガスを空気にかえて本発明の
粉体を得た。図２に示す生成物のＸ線回折パターンはＡ
ＳＴＭのＸ−ｒａｙ Ｐｏｗｄｅｒ Ｄａｔａ Ｆｉｌ
ｅの６−６９６ α−Ｆｅと一致し、黒鉛、炭化鉄の回
折ピークはみられなかつた。透過型電子顕微鏡観察によ
り針状の形状が良好に保たれていることを確認した。こ
の本発明の粉体の磁気特性は保磁力Ｈｃ＝１５４０Ｏｅ
、飽和磁化量σｓは１５８ｅｍｕ／ｇであり、全炭素量
は１０％、窒素吸着法によるＢＥＴ比表面積は５６ｍ２
／ｇであつた。耐食試験の結果、この本発明の粉体のσ
ｓは１５％低下した。又、この粉体 ２０ｇ、スルホニ
ル基含有の塩化ビニル樹脂ＭＲ−１１０（日本ゼオン社
） ５ｇを溶剤 ６０ｇ中で混合、分散させて磁性塗料
を調製しポリエチレンテレフタレート（ＰＥＴ）フイル
ム上に厚み約５μに塗布して磁気シートを製作した。こ
のシートの保磁力は１５２０Ｏｅ、飽和磁束密度は４９
５０Ｇ、角型比は０．８６であつた。このシートを６０
℃、９０％ＲＨ中に１週間保持し、飽和磁束密度の低下
を測定すると約７％であつた。尚、従来の針状金属鉄微
粒子を用いて得られたシートでは１０〜１３％の飽和磁
束密度の低下が見られた。[0064] 0.5 kg of this iron oxide powder was placed in a reaction tube and heated to 365°C while flowing CO at a flow rate of 90 l/min.
It was treated for 5 hours. After changing the gas to nitrogen and cooling it to around room temperature, the gas was gradually changed to air to obtain iron carbide powder. The X-ray diffraction pattern of the product shown in Figure 1 is ASTM
-ray Powder Data File 20
It matched with Fe5C2 of -509. 40 g of this powder was taken and put into a reaction tube, and treated at 320° C. for 2 hours while flowing hydrogen at a flow rate of 5 l/min. The gas was changed to nitrogen, and after cooling to around room temperature, the gas was gradually changed to air to obtain a powder of the present invention. The X-ray diffraction pattern of the product shown in Figure 2 is A
STM's X-ray Powder Data File
6-696 α-Fe of e, and no diffraction peaks of graphite or iron carbide were observed. It was confirmed by transmission electron microscopy that the needle-like shape was well maintained. The magnetic properties of the powder of the present invention are coercive force Hc=1540Oe
, the saturation magnetization σs is 158 emu/g, the total carbon content is 10%, and the BET specific surface area by nitrogen adsorption method is 56 m2.
/g. As a result of the corrosion resistance test, the σ of the powder of the present invention was
s decreased by 15%. In addition, 20 g of this powder and 5 g of sulfonyl group-containing vinyl chloride resin MR-110 (Nippon Zeon Co., Ltd.) were mixed and dispersed in 60 g of a solvent to prepare a magnetic paint, which was coated on a polyethylene terephthalate (PET) film to a thickness of about 5 μm. A magnetic sheet was produced by coating the material. The coercive force of this sheet is 1520 Oe, and the saturation magnetic flux density is 49
50G, and the squareness ratio was 0.86. This sheet is 60
C. and 90% RH for one week, and the decrease in saturation magnetic flux density was measured to be about 7%. In addition, a decrease in saturation magnetic flux density of 10 to 13% was observed in sheets obtained using conventional acicular metal iron fine particles.
【００６５】実施例４
実施例３における針状ゲーサイトを平均粒径０．２５μ
（長軸）、平均軸比６の形状の異なる針状ゲーサイトに
変更した以外は実施例３と同様の処理、反応を行つた。
結果を表２に示す。Example 4 The acicular goethite in Example 3 had an average particle size of 0.25 μm.
The same treatments and reactions as in Example 3 were carried out except that acicular goethite having a different shape (long axis) and average axial ratio of 6 was used. The results are shown in Table 2.
【００６６】実施例５
表面処理剤の水ガラスをアルミン酸ソーダ（ＮａＡｌＯ
２、純度７５％）に変更し、その量を０．０１ｋｇにし
た以外は実施例３と同様の処理、反応を行つた。結果は
表２に示す。Example 5 Water glass as a surface treatment agent was treated with sodium aluminate (NaAlO
2, purity 75%) and the amount was changed to 0.01 kg, the same treatments and reactions as in Example 3 were performed. The results are shown in Table 2.
【００６７】実施例６
平均粒径 ０．４μｍ（長軸）、平均軸比１０の針状ゲ
ーサイト粒子 １ｋｇを水 ２０ｌ中に分散させ、少量
のアルカリ溶液（ＮａＯＨ２０％ｓｏｌｎ）を添加しｐ
Ｈ１３以上に調整した後、水ガラス３号 ０．０２ｋｇ
とアルミン酸ソーダ ０．０１ｋｇを添加し、ｐＨ５に
調整し、１時間後に濾過を行い乾燥した。Example 6 1 kg of acicular goethite particles with an average particle diameter of 0.4 μm (long axis) and an average axial ratio of 10 was dispersed in 20 liters of water, and a small amount of alkaline solution (NaOH 20% soln) was added.
After adjusting to H13 or higher, water glass No. 3 0.02kg
and 0.01 kg of sodium aluminate were added to adjust the pH to 5, and after 1 hour, it was filtered and dried.
【００６８】この処理した粒子粉末をマツフル炉に入れ
、６００℃で１時間加熱してα−Ｆｅ２Ｏ３粉末を得た
。[0068] The treated powder particles were placed in a Matsufuru furnace and heated at 600°C for 1 hour to obtain α-Fe2O3 powder.
【００６９】この酸化鉄粉末 ０．５ｋｇを反応管に入
れ、ＣＯを９０ｌ／ｍｉｎの流速で流しながら３７０℃
で５時間処理した。ガスを窒素にかえ、室温付近まで冷
却した後、徐々にガスを空気にかえ、炭化鉄粉体を得た
。[0069] 0.5 kg of this iron oxide powder was placed in a reaction tube and heated to 370°C while flowing CO at a flow rate of 90 l/min.
It was treated for 5 hours. After changing the gas to nitrogen and cooling it to around room temperature, the gas was gradually changed to air to obtain iron carbide powder.
【００７０】この炭化鉄粉末４０ｇを取り反応管に入れ
、水素を５ｌ／ｍｉｎの流速で流しながら４００℃で１
時間処理した。ガスを窒素にかえ、室温付近まで冷却し
た後徐々にガスを空気にかえて本発明の粉体を得た。結
果を表２に示す。40 g of this iron carbide powder was placed in a reaction tube, and heated at 400°C for 1 hour while flowing hydrogen at a flow rate of 5 l/min.
Time processed. The gas was changed to nitrogen, and after cooling to around room temperature, the gas was gradually changed to air to obtain a powder of the present invention. The results are shown in Table 2.
【００７１】比較例１
比較のために実施例１で得られたＦｅ５Ｃ２に一致する
粉末を得て、還元処理を行わず直接上記と同様に評価を
行つた。結果を表１に示す。Comparative Example 1 For comparison, a powder corresponding to Fe5C2 obtained in Example 1 was obtained and directly evaluated in the same manner as above without performing any reduction treatment. The results are shown in Table 1.
【００７２】比較例２
実施例１で得たα−Ｆｅ２Ｏ３を表に示した条件で水素
のみで反応させて、徐酸化後、金属鉄微粒子を得、同様
の評価を行つた。結果を表１に示す。比表面積が小さく
なつていること及び透過型電子顕微鏡観察により粒子間
に焼結が起こつていることがわかつた。これより得られ
る塗料組成物においては、針状粒子間の焼結により分散
性が劣る。又これより作製したシートの角型比は低く、
又耐食性も低い。実施例１で得たα−Ｆｅ２Ｏ３には被
着剤（Ｓｉ）が添加されているがこの量では不十分であ
ることを示している。Comparative Example 2 α-Fe2O3 obtained in Example 1 was reacted with hydrogen alone under the conditions shown in the table, and after gradual oxidation, metallic iron fine particles were obtained and evaluated in the same way. The results are shown in Table 1. It was found that the specific surface area became smaller and that sintering occurred between particles by observation using a transmission electron microscope. The resulting coating composition has poor dispersibility due to sintering between the acicular particles. Also, the squareness ratio of sheets made from this is low,
It also has low corrosion resistance. Although adhesive (Si) was added to α-Fe2O3 obtained in Example 1, this amount was insufficient.
【００７３】比較例３
実施例１で得たα−Ｆｅ２Ｏ３をまず水素と反応させ金
属鉄まで還元した後、ＣＯ：Ｎ２＝５：９５の混合ガス
で処理を行って表面に炭化鉄を被覆した磁性粉末を得、
同様の評価を行つた。ここで得られる炭化鉄はＦｅ３Ｃ
である。結果を表１に示す。保磁力、磁化量、比表面積
、耐食性、角型比ともに本発明の金属鉄微粒子より低い
。Comparative Example 3 The α-Fe2O3 obtained in Example 1 was first reacted with hydrogen to be reduced to metallic iron, and then treated with a mixed gas of CO:N2=5:95 to coat the surface with iron carbide. obtain magnetic powder,
A similar evaluation was conducted. The iron carbide obtained here is Fe3C
It is. The results are shown in Table 1. Coercive force, magnetization amount, specific surface area, corrosion resistance, and squareness ratio are all lower than those of the metallic iron fine particles of the present invention.
【００７４】比較例４
実施例３で得られた中間体の炭化鉄 ４０ｇを取り反応
管に入れ、水素を５ｌ／ｍｉｎの流速で流しながら３２
０℃で２０ｍｉｎ処理し、粉体を得た。生成物はＸ線回
折パターンでＦｅ５Ｃ２とα−Ｆｅの混合物であり、第
２反応が完全に終了していなかつた。結果を表２に示し
たが、特性はすべてに低く、炭化鉄が残留すると磁気特
性の向上は少ない。Comparative Example 4 40 g of the intermediate iron carbide obtained in Example 3 was taken and put into a reaction tube, and heated for 32 hours while flowing hydrogen at a flow rate of 5 l/min.
A powder was obtained by processing at 0° C. for 20 minutes. The product was a mixture of Fe5C2 and α-Fe in the X-ray diffraction pattern, indicating that the second reaction was not completely completed. The results are shown in Table 2, and the properties are all poor, and if iron carbide remains, the improvement in magnetic properties is small.
【００７５】[0075]
【表１】[Table 1]
【００７６】[0076]
【表２】[Table 2]
【００７７】[0077]
【発明の効果】本発明の炭素を含有する針状金属鉄微粒
子は磁気特性及び耐食性の双方において優れ、例えば磁
気特性では保磁力が１０００Ｏｅ以上、飽和磁化量が１
２０ｅｍｕ／ｇ以上で、従来の針状金属鉄微粒子より優
れ、耐食性が針状炭化鉄微粒子と殆ど等しく、従来の針
状金属鉄微粒子のそれより遥かに優れている。更に磁性
塗料とした場合、本発明の微粒子は分散性に優れる。こ
れより得られる磁気記録媒体は優れた飽和磁束密度を与
え、長期に亘る安定した磁気特性を与える。Effects of the Invention The carbon-containing acicular metallic iron fine particles of the present invention are excellent in both magnetic properties and corrosion resistance.
At 20 emu/g or more, it is superior to conventional acicular metallic iron fine particles, and its corrosion resistance is almost equal to that of acicular iron carbide fine particles, and is far superior to that of conventional acicular metallic iron fine particles. Furthermore, when used as a magnetic paint, the fine particles of the present invention have excellent dispersibility. The magnetic recording medium obtained thereby provides excellent saturation magnetic flux density and stable magnetic properties over a long period of time.
【図１】 実施例３で得られた針状炭化鉄微粒子のＸ
線回折パターンである。[Figure 1] X of acicular iron carbide fine particles obtained in Example 3
This is a line diffraction pattern.
【図２】 実施例３で得られた本発明の針状金属鉄微
粒子のＸ線回折パターンである。FIG. 2 is an X-ray diffraction pattern of acicular metallic iron fine particles of the present invention obtained in Example 3.
Claims (5)
つて、その平均粒径（長軸）が１．０μｍ以下、平均軸
比が３〜１５であり、前記炭素の量が前記針状金属鉄微
粒子に対して２〜２０重量％である針状金属鉄微粒子。1. Acicular metallic iron fine particles containing carbon, the average particle diameter (long axis) of which is 1.0 μm or less, the average axial ratio of 3 to 15, and the amount of carbon Acicular metallic iron fine particles whose content is 2 to 20% by weight based on the metallic iron fine particles.
ない還元剤とを加熱条件下に接触させることにより得ら
れた炭素を含有する針状金属鉄微粒子。2. Acicular metallic iron fine particles containing carbon obtained by bringing acicular iron carbide fine particles into contact with a reducing agent that does not contain carbon atoms under heating conditions.
ない還元剤とを加熱条件下に接触させることを特徴とす
る炭素を含有する針状金属鉄微粒子の製法。3. A method for producing carbon-containing acicular metallic iron fine particles, which comprises bringing acicular iron carbide fine particles into contact with a reducing agent that does not contain carbon atoms under heating conditions.
つて、その平均粒径（長軸）が１．０μｍ以下、平均軸
比が３〜１５であり、前記炭素の量が前記針状金属鉄微
粒子に対して２〜２０重量％である針状金属鉄微粒子を
磁性材料として含有する磁性塗料組成物。4. Acicular metallic iron fine particles containing carbon, the average particle diameter (long axis) of which is 1.0 μm or less, the average axial ratio of 3 to 15, and the amount of carbon A magnetic coating composition containing 2 to 20% by weight of acicular metallic iron fine particles as a magnetic material based on the metallic iron fine particles.
つて、その平均粒径（長軸）が１．０μｍ以下、平均軸
比が３〜１５であり、前記炭素の量が前記針状金属鉄微
粒子に対して２〜２０重量％である針状金属鉄微粒子を
磁性材料として含有する磁気記録媒体。5. Acicular metallic iron fine particles containing carbon, the average particle diameter (long axis) of which is 1.0 μm or less, the average axial ratio of 3 to 15, and the amount of carbon A magnetic recording medium containing acicular fine metal iron particles as a magnetic material in an amount of 2 to 20% by weight based on fine metal iron particles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03140817A JP3087348B2 (en) | 1990-05-15 | 1991-05-15 | Needle-like metallic iron fine particles containing carbon, method for producing the same, magnetic coating composition containing the same, and magnetic recording medium |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12629190 | 1990-05-15 | ||
| JP2-126291 | 1990-05-15 | ||
| JP03140817A JP3087348B2 (en) | 1990-05-15 | 1991-05-15 | Needle-like metallic iron fine particles containing carbon, method for producing the same, magnetic coating composition containing the same, and magnetic recording medium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04228502A true JPH04228502A (en) | 1992-08-18 |
| JP3087348B2 JP3087348B2 (en) | 2000-09-11 |
Family
ID=26462511
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03140817A Expired - Fee Related JP3087348B2 (en) | 1990-05-15 | 1991-05-15 | Needle-like metallic iron fine particles containing carbon, method for producing the same, magnetic coating composition containing the same, and magnetic recording medium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3087348B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001342014A (en) * | 2000-03-31 | 2001-12-11 | Osaka Gas Co Ltd | Method of preparing nano-scale acicular materials |
| JP2010270217A (en) * | 2009-05-21 | 2010-12-02 | Ishihara Sangyo Kaisha Ltd | Infrared reflective material, method for producing the same, and paint and resin composition containing the same |
| CN103409054A (en) * | 2013-08-26 | 2013-11-27 | 昆明梵阗盛科技有限公司 | Magnetic paint |
| JP2015513780A (en) * | 2012-01-04 | 2015-05-14 | ヴァージニア コモンウェルス ユニバーシティ | Non-rare earth magnetic nanoparticles |
| JP2017228747A (en) * | 2016-06-24 | 2017-12-28 | ソマール株式会社 | Communication filter |
-
1991
- 1991-05-15 JP JP03140817A patent/JP3087348B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001342014A (en) * | 2000-03-31 | 2001-12-11 | Osaka Gas Co Ltd | Method of preparing nano-scale acicular materials |
| JP2010270217A (en) * | 2009-05-21 | 2010-12-02 | Ishihara Sangyo Kaisha Ltd | Infrared reflective material, method for producing the same, and paint and resin composition containing the same |
| JP2015513780A (en) * | 2012-01-04 | 2015-05-14 | ヴァージニア コモンウェルス ユニバーシティ | Non-rare earth magnetic nanoparticles |
| CN103409054A (en) * | 2013-08-26 | 2013-11-27 | 昆明梵阗盛科技有限公司 | Magnetic paint |
| JP2017228747A (en) * | 2016-06-24 | 2017-12-28 | ソマール株式会社 | Communication filter |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3087348B2 (en) | 2000-09-11 |
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