WO2006028185A1 - 酸化物磁性材料および焼結磁石 - Google Patents
酸化物磁性材料および焼結磁石 Download PDFInfo
- Publication number
- WO2006028185A1 WO2006028185A1 PCT/JP2005/016548 JP2005016548W WO2006028185A1 WO 2006028185 A1 WO2006028185 A1 WO 2006028185A1 JP 2005016548 W JP2005016548 W JP 2005016548W WO 2006028185 A1 WO2006028185 A1 WO 2006028185A1
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- WIPO (PCT)
- Prior art keywords
- sintered magnet
- hcj
- magnetic material
- mass
- ferrite
- Prior art date
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 31
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 54
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 14
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 7
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 7
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 4
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 230000004907 flux Effects 0.000 claims description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 19
- 238000004519 manufacturing process Methods 0.000 claims description 19
- 239000001301 oxygen Substances 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 18
- 238000010298 pulverizing process Methods 0.000 claims description 12
- 239000012298 atmosphere Substances 0.000 claims description 11
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 44
- 239000012071 phase Substances 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 15
- 239000011575 calcium Substances 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 238000000465 moulding Methods 0.000 description 13
- 230000007423 decrease Effects 0.000 description 12
- 239000013078 crystal Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000004453 electron probe microanalysis Methods 0.000 description 8
- 239000002245 particle Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 239000006247 magnetic powder Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 229910052761 rare earth metal Inorganic materials 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- 229910017061 Fe Co Inorganic materials 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000005347 demagnetization Effects 0.000 description 3
- 239000002270 dispersing agent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229940038504 oxygen 100 % Drugs 0.000 description 3
- 238000003746 solid phase reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003125 aqueous solvent Substances 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- -1 cationic metal oxides Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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- C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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- H01F41/0273—Imparting anisotropy
Definitions
- the present invention relates to an oxide magnetic material and a sintered magnet containing a ferrite having an M-type magnetoplumbite structure as a main phase, and methods for producing them.
- Ferrite is a general term for compounds formed by divalent cationic metal oxides and trivalent iron, and ferrite magnets are used in various applications such as various rotating machines and speakers.
- ferrite magnets Sr ferrite (SrFe 2 O 3) and Ba ferrite (BaFe 2 O 3) having a hexagonal magnetoplumbite structure are widely used.
- Patent Document 1 Patent Document 2
- Patent Document 1 Japanese Patent Laid-Open No. 10-149910
- Patent Document 2 Japanese Patent Laid-Open No. 11-154604
- Patent Document 3 Japanese Patent Laid-Open No. 2000-223307
- Patent Document 3 describes the improvement of residual magnetic flux density Br, coercive force HcJ, and coercivity.
- CaLaCo ferrite Ca ferrite containing La and Co simultaneously (hereinafter referred to as “CaLaCo ferrite”) is disclosed.
- a value of at least 10% higher and a value of 20 kOe or higher can be obtained.
- CaLaCo ferrite disclosed in Patent Document 3 is Ca La (l-xl xl
- Sr ferrite in which a part of Sr is replaced with a rare earth element such as La and a part of Fe is replaced with Co or the like (hereinafter referred to as "SrLaCo ferrite" t) is Due to its excellent magnetic properties, it is widely used in various applications in place of conventional Sr ferrite and Ba ferrite.
- the application in which the ferrite magnet is most used is a motor. If the magnetic properties of ferrite magnets improve, the motor output can be improved or the motor can be downsized. Therefore, the improvement of residual magnetic flux density Br, coercive force HcJ, and maximum energy product (BH) max is very effective. Along with their properties, the squareness ratio (HkZHcJ) must also be high. If the squareness ratio is low, the limit demagnetizing field strength becomes small, which causes the problem of easy demagnetization.
- Hk which is a parameter to be measured, is the position where 4 ⁇ ⁇ becomes 0.995Br in the second quadrant of the 4 ⁇ I (Magnetic field strength) H (Magnetic field strength) curve. This is the reading of the ⁇ axis.
- the value obtained by dividing Hk by HcJ of the demagnetization curve (Hk / Hcj) is defined as the squareness ratio.
- CaLaCo ferrite according to Patent Document 3 shows excellent magnetic properties comparable to SrLaCo ferrite, and is expected to be applied in the future, but has a problem that the squareness ratio (HkZHcJ) is very low.
- HkZHcJ squareness ratio
- xl 0.8
- the squareness ratio exceeds 85%, but the coercive force HcJ decreases rapidly.
- the CaLaCo ferrite according to Patent Document 3 is SrLaCo ferrite in the anisotropic magnetic field H.
- Br and HcJ have characteristics comparable to SrLaCo ferrite, but they cannot satisfy both the high coercive force and the high squareness ratio. Until it is applied to various applications such as
- An object of the present invention is to provide an oxide magnetic material and a sintered magnet that solve the problems in the conventional CaLaCo ferrite, improve Br and HcJ, and exhibit a high depression angle ratio.
- R is at least one element selected from La, Nd, and Pr and must contain La
- M is at least one element selected from Co, Zn, Ni, and Mn, and must contain Co
- molar ratio x, y, and n are respectively
- An acidic magnetic material mainly composed of ferrite with hexagonal M-type magnetoplumbite structure.
- an oxide magnetic material having high Br, high HcJ, and a high squareness ratio. Fees can be provided.
- the coercive force HcJ obtained when the sintered magnet is produced from the oxide magnetic material according to the present invention achieves a value of 370 kAZm or more in the preferred configuration, and the residual magnetic flux density Br is 0.45 T in the preferred configuration.
- the above values can be achieved.
- the squareness ratio when a sintered magnet is formed using an oxide magnetic material can be 85% or more in a preferred configuration, and 90% or more in a more preferred configuration.
- HcJ can be achieved.
- CaLaCo ferrite according to Patent Document 3 is calcined in oxygen (oxygen 100%
- the sintered magnet according to the present invention has high Br, high HcJ, and a high squareness ratio, and is therefore optimal for applications such as motors.
- the ratio xZy between La substitution amount X and Co substitution amount y was changed to 1.0 force to 5.0, and the composition ratio xZy and the residual magnetic flux density Br and coercivity of the sintered magnet were changed. It is a graph which shows the relationship with HcJ and HkZHcJ.
- n is changed from 3.6 force to 6.0, and the yield is n, the residual magnetic flux density Br of the sintered magnet, the coercive force HcJ and HkZHcJ. It is a graph which shows the relationship.
- FIG. 10 is a graph showing a relationship between y ′ (NiO amount) and residual magnetic flux density Br, coercive force HcJ, and squareness ratio Hk ZHcJ of a sintered magnet.
- the oxide magnetic material according to the present invention is represented by the following formula.
- CaLaCo ferrite has an anisotropic magnetic field H greater than SrLaCo ferrite.
- Patent Document 3 the preferred range of the forces x and y in which CaLaCo ferrite is described is 0.4 to 0.6 from the description of the examples.
- the amounts of Fe and Co in the composition formula are expressed by z. Therefore, there is no description about the n value.
- the present invention relates to an improvement of CaLaCo ferrite, and Ca is an essential element.
- R is at least one element selected from La, Nd, and Pr, and must contain La.
- elements having an ion radius close to that of Sr 2+ such as Ce, Sm, Eu, and Gd, is acceptable.
- M is at least one element selected from Co, Zn, Ni, and Mn, and must contain Co. Even elements other than the above can be allowed to be mixed as inevitable impurities.
- Co can be substituted with Zn, Ni, and Mn as described above, and even if any of Zn, Ni, and Mn is substituted, Patent Document 1 and Patent Document 2 Br and HcJ exceeding the Sr LaCo ferrite disclosed in (1) can be achieved.
- Patent Document 1 and Patent Document 2 Br and HcJ exceeding the Sr LaCo ferrite disclosed in (1) can be achieved.
- the manufacturing cost can be reduced without degrading the magnetic properties.
- HcJ can improve the force Br, which decreases slightly.
- the substitution amount of Zn, Ni and Mn is 50% or less of Co in molar ratio.
- X represents the content of R, and is preferably 0.4 ⁇ x ⁇ 0.6. This is because Br and the squareness ratio decrease when the x force is less than 0.4 and exceeds 0.6.
- y indicates the content of M, and 0.2 ⁇ y ⁇ 0.35. As described above, in the CaLaCo ferrite, a preferred range of y is a force crystal structure that is considered to be 0.4 to 0.6. A heterogeneous phase containing a large amount of Co is generated in the crystal structure. The present invention is characterized in that the range of y is 0.2 ⁇ y ⁇ 0.35, and X and y described later are specified ratios. If y is less than 0.2, Br and HcJ decrease, and if it exceeds 0.35, a heterogeneous phase containing a large amount of Co is generated, and HcJ decreases.
- n value that defines the ratio of CaO, R 2 O and Fe 2 O, MO is within this range where 4 ⁇ n ⁇ 6 is preferred.
- a squareness ratio (HkZHcJ) of 85% or more is obtained. Furthermore, it is preferably 4.8 ⁇ n ⁇ 5.8, and a squareness ratio of 90% or more is obtained.
- the squareness ratio is a value when a sintered magnet is used because it is difficult to measure with a calcined body after calcining.
- raw material powders such as CaCO, Fe 2 O, La 2 O, and Co 2 O are prepared. Prepared powder
- x, y, and n are blended so as to be in preferable ranges.
- the raw material powder may be in the form of a solution, such as hydroxide, nitrate, or chloride, in addition to the oxide or carbonate.
- Raw material powders other than 2 may be added with the raw material mixing force, or may be added after calcination described later. For example, after blending, mixing and calcining CaCO, Fe 2 O and La 2 O, Co
- O and the like can be added and pulverized before molding and sintering. Also promotes reactivity during calcination
- the addition of HBO is effective in improving HcJ and Br.
- the amount of H BO added is 0.2
- H BO also has the effect of controlling the crystal grains during sintering, so after calcination (before pulverization or
- the raw material powder may be wet, dry, or misaligned! /.
- a medium such as a steel ball
- it can be mixed more uniformly. If wet, use water as the solvent.
- a known dispersing agent such as polycarboxylic acid ammonium or dalconic acid calcium may be used.
- the mixed raw material slurry is dehydrated to become a mixed raw material powder.
- the mixed raw material powder is heated using an electric furnace, a gas furnace or the like, and forms a magnetoplumbite type ferrite compound by a solid phase reaction. This process is called “calcination”, and the resulting composite is called “calcination”.
- the calcination step is preferably performed in an atmosphere having an oxygen concentration of 5% or more. Oxygen concentration is 5
- a more preferable oxygen concentration is 20% or more.
- a ferrite phase is formed by a solid phase reaction with an increase in temperature, and is completed at about 1100 ° C. Below this temperature, unreacted hematite (iron oxide) remains. Low magnetic properties.
- the temperature exceeds 1100 ° C, the effect of the present invention occurs.
- the calcining temperature exceeds 1450 ° C., crystal grains grow too much, which may cause inconveniences such as a long time for the grinding process. Therefore, the calcination temperature is preferably 1100 ° C to 1450 ° C. More preferably, it is 1200 ° C to 1350 ° C.
- the calcining time is preferably 0.5 to 5 hours.
- Calcination can be performed at ° C.
- the calcined body obtained by the calcining step has a main phase of hexagonal M-type magnetoplumbite type ferrite represented by the following chemical formula, and the oxide magnetic material of the present invention When Become.
- a magnetic powder By pulverizing and / or crushing such a calcined body, a magnetic powder can be obtained, which can be applied to a bond magnet or a magnetic recording medium.
- the above calcined body can be produced by a known production technique such as a spray pyrolysis method or a coprecipitation method.
- the magnetic powder When the magnetic powder is applied to a bonded magnet, the magnetic powder is mixed with a flexible rubber, hard light plastic, or the like and then molded.
- the molding process may be performed by methods such as injection molding, extrusion molding, and roll molding.
- the magnetic powder when it is applied to a bonded magnet, it is preferably heat-treated at a temperature range of 700 ° C. to 1100 ° C. for about 0.1 to 3 hours in order to relax the crystal distortion of the magnetic powder.
- a more preferable temperature range is 900 ° C to 1000 ° C.
- a coating type magnetic recording medium is prepared. can do.
- a thin film magnetic layer used for a magnetic recording medium can be formed by a sputtering method or the like using the oxide magnetic material of the present invention and a sintered magnet using the same as a target.
- the calcined body is finely pulverized into a fine particle by a vibration mill, a ball mill and Z or an attritor.
- the average particle size of the fine particles is preferably about 0.4 to 0.8 m (air permeation method).
- the fine pulverization step may be either dry pulverization or wet pulverization, but is preferably performed in combination.
- an aqueous solvent such as water and various non-aqueous solvents (for example, organic solvents such as acetone, ethanol, xylene) can be used.
- a slurry in which the solvent and the calcined body are mixed is generated. It is preferable to add 0.2% by mass to 2.0% by mass or less of various known dispersants and surface active agents in a solid content ratio to the slurry.
- the slurry is preferably concentrated and kneaded.
- SiO has effects such as control of crystal grains during calcination.
- press molding is performed in a magnetic field or in a non-magnetic field while removing the solvent in the slurry.
- the crystal orientation of the powder particles can be aligned. Magnetic properties can be dramatically improved by press molding in a magnetic field.
- a dispersant and a lubricant may be added from 0.01 to L: 0% by mass.
- the molded body obtained by press molding is subjected to a degreasing process as necessary, followed by a sintering process.
- the sintering process is performed using an electric furnace, a gas furnace, or the like.
- the sintering step is preferably performed in an atmosphere having an oxygen concentration of 10% or more.
- a more preferable oxygen concentration is 20% or more, and most preferable is an oxygen concentration of 100%.
- the oxide magnetic material of the present invention has magnetic properties equivalent to or better than those obtained by firing CaLaCo ferrite in oxygen (100% oxygen) according to Patent Document 3 even in the atmosphere, as in the examples described later. Indicates. Therefore, further superior magnetic properties can be obtained by performing baking in oxygen similar to the baking in oxygen disclosed in Patent Document 3.
- the sintering temperature is preferably 1150 ° C to 1250 ° C.
- the sintering time is preferably 0.5 to 2 hours.
- the average crystal grain size of the sintered magnet obtained by the sintering process is about 0.5-2 / ⁇ ⁇ .
- a ferrite sintered magnet product is finally completed through known manufacturing processes such as a processing step, a cleaning step, and an inspection step.
- the mixture was mixed with a ball mill for 4 hours, dried and sized. Subsequently, it was calcined at 1300 ° C. for 3 hours in the air to obtain a powdery calcined body.
- the CaCO powder is 0.6% by mass in terms of CaO, and the SiO powder is 0%.
- Figure 1 shows the measurement results of residual magnetic flux density Br, coercivity HcJ, and squareness ratio HkZHcJ, with the relative ratio xZy of X and y (La and Co) as the horizontal axis.
- Figure 2 shows the measurement results for Br, HcJ, and HkZHcJ, where the amount of applied force on y is plotted on the horizontal axis.
- xZy is approximately 1.25 or less, HcJ is below 340 kAZm (4.27 kOe), and 1.4. Below, HkZHcJ fell below 85%. When xZy was too large, Br and HcJ decreased. When xZy was about 2.5 or more, Br was 0.44T and HcJ was below 340kAZm (4.27kOe). Conventionally, xZy is best around 1 because of the charge correction of La and Co. However, CaLaCo ferrite according to the present invention has high magnetic properties around 1.4 ⁇ x / y ⁇ 2.5. What is obtained is ⁇ .
- Figure 3 shows the measurement results of residual magnetic flux density Br, coercivity HcJ, and squareness ratio HkZHcJ, with the value of n on the horizontal axis.
- the magnetic properties of the obtained sintered magnet were measured.
- Figure 4 shows the measurement results of residual magnetic flux density Br, coercive force HcJ, and squareness ratio HkZHcJ, with the added amount of X on the horizontal axis.
- the EPMA analysis was performed using an EPMA device (EPMA1610 manufactured by SHIMADZU) under the conditions of an acceleration voltage of 15 kV, a sample current of 0.1 lA, and an irradiation range of ⁇ 100 m (electron beam diameter).
- the sintered magnet according to the present invention does not show a heterogeneous phase containing a large amount of Co. Therefore, high magnetic properties as shown in the above-described Examples 1 to 4 can be obtained.
- Component analysis by EPMA was performed on the obtained sintered magnet.
- Figure 7 shows the analysis results.
- the EPMA conditions are the same as in Example 5.
- the sintered magnet according to the comparative example has a large number of different phases containing a large amount of Co (name spots in the photograph at the right end of the lower stage in FIG. 7).
- Br 0.44 IT
- HcJ 325.5 kA / m (4.09 kOe)
- Hk / HcJ 63%
- HkZHcJ was deteriorated. This is thought to be due to the presence of a heterogeneous phase containing a large amount of Co.
- Fig. 8 shows the measurement results of bundle density Br, coercive force HcJ, and squareness ratio HkZHcJ.
- H BO powder 0.1% by mass of H BO powder, 0.5% to 0.9% by mass of CaCO powder in terms of CaO, SiO powder
- a sintered magnet was produced in the same manner as in Example 6 except that 0.3 to 0.9 mass% of 3 3 3 2 powder was added. The magnetic properties of the obtained sintered magnet were measured. Residual magnetic flux density with the added amount of SiO on the horizontal axis
- Figure 9 shows the measurement results for degree Br, coercivity HcJ, and squareness ratio HkZHcJ.
- the black circle is CaOO. 5 mass%
- the black square is CaOO. 9 mass%.
- FIG. 9 et al. Show that the amount of CaCO added to the CaLaCo ferrite in the present invention is CaO.
- a sintered magnet was produced in the same manner as in Example 1 except that 6% by mass was added, the calcining temperature was 1225 ° C, and the sintering temperature was 1190 ° C and 1200 ° C.
- Table 2 shows the results of measuring the magnetic properties of the obtained sintered magnet. [0094] [Table 2] Sintering temperature Br Hcj (BH) max Hk / Hcj
- the mixture was finely pulverized with a wet ball mill using 6% by mass of water as a solvent until the average particle size by air permeation method became 0.55 / x m. While removing the solvent from the finely pulverized slurry, press molding was performed in a magnetic field. Press molding was performed so that the pressurization direction and the magnetic field direction were parallel, and the magnetic field strength was 13 kOe. The obtained molded body was sintered in the atmosphere at 1190 ° C for 1 hour to obtain a sintered magnet.
- Figure 10 shows the measurement results of residual magnetic flux density Br, coercivity HcJ, and squareness ratio HkZHcJ, with y '(NiO content) on the horizontal axis.
- the oxide magnetic material of the present invention has not only the residual magnetic flux density Br and the coercive force Hcj, but also the corners. Since the mold ratio is high, it is suitable for high-performance motor applications.
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Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
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EP05782321A EP1808422B1 (en) | 2004-09-10 | 2005-09-08 | Oxide magnetic material and sintered magnet |
US10/592,488 US7758767B2 (en) | 2004-09-10 | 2005-09-08 | Oxide magnetic material and sintered magnet |
CN2005800164602A CN1956935B (zh) | 2004-09-10 | 2005-09-08 | 氧化物磁性材料和烧结磁铁 |
MXPA06015044A MXPA06015044A (es) | 2004-09-10 | 2005-09-08 | Material magnetico de oxido e iman sinterizado. |
BRPI0508979A BRPI0508979B1 (pt) | 2004-09-10 | 2005-09-08 | material magnético de óxido e magneto sinterizado |
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JP2004-264568 | 2004-09-10 | ||
JP2004264568 | 2004-09-10 |
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US (2) | US7758767B2 (ja) |
EP (1) | EP1808422B1 (ja) |
KR (1) | KR100910048B1 (ja) |
CN (1) | CN1956935B (ja) |
BR (1) | BRPI0508979B1 (ja) |
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WO2007105398A1 (ja) | 2006-03-10 | 2007-09-20 | Hitachi Metals, Ltd. | 回転機、ボンド磁石、マグネットロール、及びフェライト焼結磁石の製造方法 |
WO2014050433A1 (ja) * | 2012-09-28 | 2014-04-03 | 日立金属株式会社 | フェライト焼結磁石及びその製造方法 |
WO2014084059A1 (ja) * | 2012-11-30 | 2014-06-05 | 日立金属株式会社 | フェライト化合物 |
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CN102089835A (zh) * | 2008-07-08 | 2011-06-08 | 丹麦理工大学 | 磁致热致冷器 |
SI2450922T1 (sl) * | 2009-06-30 | 2018-11-30 | Hitachi Metals, Ltd. | Postopek izdelave feritnega sintranega magneta in feritni sintrani magnet |
EP2452928B1 (en) * | 2009-07-08 | 2016-09-07 | TDK Corporation | Ferrite magnetic material |
US8506838B2 (en) | 2010-03-10 | 2013-08-13 | Hitachi Metals, Ltd. | Sintered ferrite magnet and its production method |
CN103282977B (zh) * | 2010-12-28 | 2016-06-08 | 日立金属株式会社 | 铁氧体烧结磁体及其制造方法 |
EP2881956B1 (en) | 2012-07-31 | 2017-07-05 | Hitachi Metals, Ltd. | Sintered ferrite magnet and its production method |
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KR102258552B1 (ko) | 2017-03-31 | 2021-06-01 | 유니온머티리얼 주식회사 | 페라이트 자성재료 및 페라이트 소결자석 |
US11289250B2 (en) | 2017-05-24 | 2022-03-29 | Hitachi Metals, Ltd. | Sintered ferrite magnet |
EP3633697A4 (en) * | 2017-05-24 | 2021-03-10 | Hitachi Metals, Ltd. | SINTERED FERRITE MAGNET |
CN110323025B (zh) * | 2018-03-28 | 2021-12-10 | Tdk株式会社 | 铁氧体烧结磁铁 |
JP7000954B2 (ja) * | 2018-03-28 | 2022-01-19 | Tdk株式会社 | フェライト焼結磁石 |
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JP7347296B2 (ja) * | 2020-03-30 | 2023-09-20 | Tdk株式会社 | フェライト焼結磁石および回転電気機械 |
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2007105398A1 (ja) | 2006-03-10 | 2007-09-20 | Hitachi Metals, Ltd. | 回転機、ボンド磁石、マグネットロール、及びフェライト焼結磁石の製造方法 |
EP2244269A1 (en) | 2006-03-10 | 2010-10-27 | Hitachi Metals, Ltd. | Method for producing sintered ferrite magnet |
US8303837B2 (en) | 2006-03-10 | 2012-11-06 | Hitachi Metals, Ltd. | Rotating machine, bonded magnet, magnet roll, and method for producing sintered ferrite magnet |
US8512590B2 (en) | 2006-03-10 | 2013-08-20 | Hitachi Metals, Ltd. | Rotating machine, bonded magnet, magnet roll, and method for producing sintered ferrite magnet |
TWI456870B (zh) * | 2006-03-10 | 2014-10-11 | Hitachi Metals Ltd | 肥粒鐵燒結磁鐵之製造方法 |
WO2014050433A1 (ja) * | 2012-09-28 | 2014-04-03 | 日立金属株式会社 | フェライト焼結磁石及びその製造方法 |
US9536646B2 (en) | 2012-09-28 | 2017-01-03 | Hitachi Metals, Ltd. | Sintered ferrite magnet and its production method |
WO2014084059A1 (ja) * | 2012-11-30 | 2014-06-05 | 日立金属株式会社 | フェライト化合物 |
JPWO2014084059A1 (ja) * | 2012-11-30 | 2017-01-05 | 日立金属株式会社 | フェライト化合物 |
Also Published As
Publication number | Publication date |
---|---|
CN1956935A (zh) | 2007-05-02 |
BRPI0508979B1 (pt) | 2016-07-12 |
CN1956935B (zh) | 2010-05-05 |
KR20060132917A (ko) | 2006-12-22 |
BRPI0508979A (pt) | 2007-08-28 |
US7758767B2 (en) | 2010-07-20 |
EP1808422B1 (en) | 2012-06-06 |
US20100237273A1 (en) | 2010-09-23 |
EP1808422A4 (en) | 2011-04-13 |
US20070194269A1 (en) | 2007-08-23 |
MXPA06015044A (es) | 2007-04-25 |
EP1808422A1 (en) | 2007-07-18 |
KR100910048B1 (ko) | 2009-07-30 |
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