CN1757078A - Process for producing oxide magnetic material based permanent magnet - Google Patents
Process for producing oxide magnetic material based permanent magnet Download PDFInfo
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- CN1757078A CN1757078A CNA2003801101137A CN200380110113A CN1757078A CN 1757078 A CN1757078 A CN 1757078A CN A2003801101137 A CNA2003801101137 A CN A2003801101137A CN 200380110113 A CN200380110113 A CN 200380110113A CN 1757078 A CN1757078 A CN 1757078A
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- adhesive
- magnetic material
- permanent magnet
- shaping
- wax
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- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000000696 magnetic material Substances 0.000 title claims abstract description 33
- 230000008569 process Effects 0.000 title abstract description 9
- 230000005291 magnetic effect Effects 0.000 claims abstract description 46
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 34
- 239000000194 fatty acid Substances 0.000 claims abstract description 34
- 229930195729 fatty acid Natural products 0.000 claims abstract description 34
- -1 fatty acid ester Chemical class 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 33
- 239000000203 mixture Substances 0.000 claims abstract description 24
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical class CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003825 pressing Methods 0.000 claims abstract description 19
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 230000001070 adhesive effect Effects 0.000 claims description 65
- 239000000853 adhesive Substances 0.000 claims description 61
- 238000007493 shaping process Methods 0.000 claims description 52
- 239000001993 wax Substances 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 29
- 239000000654 additive Substances 0.000 claims description 27
- 230000000996 additive effect Effects 0.000 claims description 27
- 238000005245 sintering Methods 0.000 claims description 26
- 238000004090 dissolution Methods 0.000 claims description 21
- 238000004519 manufacturing process Methods 0.000 claims description 13
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 8
- 239000008116 calcium stearate Substances 0.000 claims description 8
- 235000013539 calcium stearate Nutrition 0.000 claims description 8
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 5
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 4
- 229940063655 aluminum stearate Drugs 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000012178 vegetable wax Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 7
- 238000000465 moulding Methods 0.000 abstract description 7
- 230000033228 biological regulation Effects 0.000 abstract description 5
- 230000005415 magnetization Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 238000010304 firing Methods 0.000 abstract 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000839 emulsion Substances 0.000 description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 239000007859 condensation product Substances 0.000 description 7
- 229910000859 α-Fe Inorganic materials 0.000 description 6
- 208000037656 Respiratory Sounds Diseases 0.000 description 5
- 238000005336 cracking Methods 0.000 description 5
- 238000004080 punching Methods 0.000 description 5
- 238000001354 calcination Methods 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 3
- 241000723346 Cinnamomum camphora Species 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 229960000846 camphor Drugs 0.000 description 3
- 229930008380 camphor Natural products 0.000 description 3
- 239000011812 mixed powder Substances 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 239000012188 paraffin wax Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- IATRAKWUXMZMIY-UHFFFAOYSA-N strontium oxide Chemical compound [O-2].[Sr+2] IATRAKWUXMZMIY-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241000221079 Euphorbia <genus> Species 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- CSSYLTMKCUORDA-UHFFFAOYSA-N barium(2+);oxygen(2-) Chemical compound [O-2].[Ba+2] CSSYLTMKCUORDA-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000004203 carnauba wax Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000003302 ferromagnetic material Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000012168 ouricury wax Substances 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012165 plant wax Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- 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
- H01F41/0253—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 for manufacturing permanent magnets
- H01F41/0273—Imparting anisotropy
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- 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
- C04B35/2683—Other ferrites containing alkaline earth metals or lead
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Hard Magnetic Materials (AREA)
- Magnetic Ceramics (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Powder Metallurgy (AREA)
Abstract
A process for producing an oxide magnetic material based permanent magnet, comprising a binder addition step of adding a binder and a molding auxiliary to raw material powder containing an oxide magnetic material and mixing the same; a moisture regulation step of regulating the moisture of the resultant molding mixture containing the raw material powder, binder and molding auxiliary; an in-magnetic-field dry molding step of charging the molding mixture after moisture regulation into a metal mold and pressing the mold in an applied magnetic field so as to align the easy magnetization directions of the oxide magnetic material powder; and a firing step of firing the thus molded item, wherein the binder added in the binder addition step is a fatty acid ester wax, while the molding auxiliary added in the binder addition step is a stearic acid salt having such a property that it is melted at 90 DEG C or below in relation to the fatty acid ester wax as the binder (90 DEG C melting characteristic). By this process, at low cost, there can be obtained an oxide magnetic material based permanent magnet of enhanced alignment and sintered body density excelling in magnetic characteristics.
Description
Technical field
The present invention relates to the manufacture method of oxide magnetic material based permanent magnet, particularly use the manufacture method of the oxide magnetic material based permanent magnet of so-called dry pressing method shaping.
Background technology
The anisotropy oxide permanent magnet of magnet lead ores such as Sr ferrite and Ba ferrite is made through sintering after being shaped in magnetic field again.Shaping in magnetic field roughly is divided into dry pressing method and wet forming method according to its method.The wet forming method is because the permanent magnet material particle easily rotates, so the orientation of magnetic material becomes well, can obtain good magnetic properties., owing in press molding, need decentralized medium is discharged to (outside the mold cavity) outside the formingspace, so the productivity variation.And it is large-scale that mould structure becomes, and equipment cost also uprises.
Its on the other hand, the dry pressing method is that the permanent magnet material with drying regime is filled in the formingspace (chamber) method that is shaped in magnetic field.Therefore, with wet forming method ratio, the orientation of magnetic material is bad, but the productivity height, the installation cost cheapness has this very excellent advantage.
In the dry pressing method, contain adhesive among the permanent magnet material in being filled to mould.As the desired ideal characterisitics of adhesive, can list the adhesive effect excellence of material particle, and not damage the permutation of material particle on the direction of principal axis of easy magnetization on the magnetic.Reason as the directionality variation lists: the magnetic loss of (1) material particle is harmful, promptly the adhesive effect owing to material particle and adhesive is too strong, therefore damages the permutation of particle on the direction of principal axis of easy magnetization on the magnetic; Friction when (2) being shaped, particle each other contact friction caused, in addition and since between particle and the mould also the effect friction therefore the pressure that brings of pressurization pass on insufficiently, formability is step-down also, or the like.In order to improve the deterioration of such orientation, the adhesive that in the dry pressing method, attempting selected low friction, does not carry out magnetic loss evil adds among the permanent magnet material.
That is, when the shaping of dry pressing method,, use paraffin, stearic acid, camphor etc. as the adhesive that contains in the ferromagnetic material.
, though paraffin and stearic acid adhesive effect excellence because adhesive effect is too strong, are therefore damaged the permutation of particle on the direction of the axle of easy magnetization on the magnetic easily.In addition, though camphor is effective as the adhesive in the shaping when externally-applied magnetic field, because distillation, the blending ratio of itself and ferrite powder can change along with the variation of time.Therefore, have following shortcoming,, perhaps cause the intensity of formed body to reduce as bringing fault to forming operation.
In order to solve such problem, as the adhesive of dry type magnetic forming with ferrite magnet powder, proposed to use the scheme of the adhesive (special public clear 47-21197 communique) of stearic slaine (as metal M, M=Ca, Ba, Sr, Pb), the adhesive (special public clear 60-22484 communique) of use dolomol etc.
, the adhesive of so stearic slaine is difficult to make it therefore, have to increase the addition of adhesive in each evenly lining of surface of particle.Therefore, the carbon quantitative change in the magnet behind the sintering is many, causes magnetic characteristic and reduces, or a little less than guarantor's type power, becomes the reason that crackle takes place in the sintered body behind the sintering.
In addition, as the mixed method of adhesive, list the method that applies the adhesive of gas phase shape on the surface of particle by heating or decompression., this method equipment become large-scale in, it is many that the number of working processes number also becomes, and the problem that can not seek cost degradation is arranged.
And, in order to improve formability, to improve mobile, friction when reducing punch die etc., in adhesive, add shaping additive usually.
Such shaping additive becomes the root that generates carbide when sintering, becomes the reason that makes sintered density reduce, make magnetic characteristic (Br) deterioration, therefore wishes to reduce its addition as much as possible.
,, guarantee good formability in order to reduce the punch die pressure of shaping thing and mould, have to increasing to a certain degree of the addition of shaping additive, this is a present situation.
The present invention is the innovation case under such actual state, its purpose is, when utilizing dry pressing to make oxide magnetic material based permanent magnet, use a small amount of interpolation promptly to obtain sufficient formability and help the novel shaping additive of cost degradation, the oxide magnetic material based permanent magnet of be improved orientation and sintered density, magnetic characteristic excellence.
Summary of the invention
In order to solve above-mentioned problem, following formation the present invention, the present invention is a kind of manufacture method of oxide magnetic material based permanent magnet, comprises following operation: the adhesive of adding and mixed adhesive and shaping additive adds operation in containing the material powder of oxidate magnetic material; Adjustment contains the moisture adjustment operation of the shaping of material powder, adhesive and shaping additive with the moisture in the mixture; To carry out the above-mentioned shaping of moisture adjustment and put into mould with mixture, pressurization makes dry pressing operation in the magnetic field of direction of easy axis unanimity of oxidate magnetic material powder in externally-applied magnetic field; Sintering circuit with the formed body of sintering formed thereby, wherein, adding the adhesive that uses in the operation at above-mentioned adhesive is that fatty acid ester is a wax, adding the shaping additive that uses in the operation at above-mentioned adhesive is stearate, and itself and above-mentioned fatty acid ester as adhesive are that the pass of wax is fastened and had at the soluble characteristic of the temperature below 90 ℃ (90 ℃ of dissolution characteristics).
In addition, as preferred scheme of the present invention, above-mentioned stearate is at least one that select among calcium stearate, zinc stearate, dolomol and aluminum stearate and constituting.
In addition, as preferred scheme of the present invention, on constituting, make the addition of above-mentioned stearate reach the scope of 0.1-0.45wt%.
In addition, as preferred scheme of the present invention, above-mentioned fatty acid ester is that wax constitutes as vegetable wax.
In addition, as preferred scheme of the present invention, making on constituting is shaped reaches 0.2-1.5wt% with the binder content in the mixture.
The preferred plan that carries out an invention
Below describe the manufacture method of oxide magnetic material based permanent magnet of the present invention in detail.
The manufacture method of oxide magnetic material based permanent magnet of the present invention, as master operation, be included in the material powder that contains oxidate magnetic material and add and the adhesive of mixed adhesive adds operation, adjust the moisture adjustment operation of the moisture of mixture to the shaping that contains above-mentioned raw materials powder and adhesive with adding moisture in the mixture, to carry out the above-mentioned shaping of moisture adjustment and put into mould makes the direction of easy axis unanimity of oxidate magnetic material powder in the externally-applied magnetic field pressurization magnetic field dry pressing operation with mixture, sintering circuit with the formed body of sintering formed thereby.
The material powder of the oxidate magnetic material of preparing before above-mentioned adhesive adds operation adopts following main points to make usually.
[making of material powder]
For example, barium ferrite is generally with iron oxide (Fe
2O
3) and brium carbonate (BaCO
3) powder be main material, in addition, strontium ferrite is generally with iron oxide (Fe
2O
3) and strontium carbonate (SrCO
3) powder be main material, those powder of weighing make it to reach predetermined component, add again, cooperate the regulation additive, with mixing such as ball mills.
As additive, for example use oxide, chloride of Bi, As, B, Si, Ge, Na, Al, Cr, Ti, W, Mo etc. etc.Such additive for acceleration of sintering, prevent excessive the growing up of crystal grain and use.The temperature calcining of such mixture about 1000 ℃.By this calcining, make the carbon dioxide composition decompose, distribute, and make barium monoxide and iron oxide or strontium oxide strontia and iron oxide carry out chemical combination.
Burnt like this material is fully pulverized with ball mill etc.Also can further add additive as required after the pulverizing.
[adhesive interpolation operation]
Add adhesive and mixing to the material powder that contains oxidate magnetic material that adopts above-mentioned main points to prepare.As the adhesive that adds, be that wax, the particularly fatty acid ester of molecular weight 300-800 are that wax is after emulsification and use to well with fatty acid ester.In the present invention, when using such fatty acid ester to be wax, further add the salt shaping additive that constitutes by the stearic acid of regulation rerum natura described later as adhesive.
Among fatty acid ester is wax, special preferred plant wax (Brazil wax, the cured root of Beijing euphorbia is cured, Japan is cured, ouricury wax etc.).
The preferred 0.2-1.5wt% of adhesive addition, preferred especially 0.25-1.2wt%, further preferred 0.3-0.9wt%.When addition is very few, can not embody as the effect of adhesive, guarantor's type power dies down.In addition, when addition is too much, thereby because the organic carbonization during sintering causes the density of sintered body to reduce the magnetic characteristic deterioration of Br etc.
And, add the shaping additive that adds the present application regulation in the operation at this adhesive.Promptly, add in the operation at adhesive of the present invention, use stearate as shaping additive, and this stearate the characteristic (following only be called " 90 ℃ of dissolution characteristics ") that has in the dissolving of the temperature below 90 ℃ is fastened in the pass being wax with above-mentioned fatty acid ester as adhesive, this is decided to be necessary important document.
These 90 ℃ of dissolution characteristics make it possible to verify having or not of its characteristic with following mensuration main points definition.Promptly; getting by the fatty acid ester of emulsification is basic emulsion solution (trade name: Serozoru 524 (Zhong jing grease Co., Ltd. system)) 10ml of wax; 90 ℃ solution is made in heating; in this solution, drop into (solution temperature remains on 90 ℃) behind the stearate 1.5g; carry out common manual stirring, by whether judging 90 ℃ of dissolvings.If 90 ℃ of dissolvings then be judged to be the stearate of 90 ℃ of dissolution characteristics.Whether becoming dissolved state can fully judge through visual.If dissolving then become roughly solution uniformly is not if dissolve then the powder of stearate is cotton-shaped residual in solution.Also can judge the state of dissolving by the viscosimetric analysis of solution.If dissolve then viscosity especially reduces (for example under the Shear Rate 8/sec for about 1-20).
As stearate, can exemplify calcium stearate, zinc stearate, dolomol, aluminum stearate etc. as preference, but these materials must satisfy 90 ℃ of above-mentioned dissolution characteristics.
The method for making of stearate generally has (1) to be called as the method for making of wet type double decomposition and the method for making that (2) are called as the dry type direct method.In order to possess 90 ℃ of dissolution characteristics, have various tricks of the trade on the method for making, but the former method for making of (1) can be described as the method for making that is suitable for obtaining possessing the stearate of 90 ℃ of dissolution characteristics.
Always the general grade of the stearate that uses in the technical field of the present application is near the material (not possessing 90 ℃ of dissolution characteristics in the present application) that fusing point is arranged 120 ℃, in the time of near binder solution rises to 120 ℃, these stearate just possess the characteristic of basic dissolving.
The degree that the stearate with 90 ℃ of dissolution characteristics in the present application, its addition can not propose to the past is less promptly brought into play effect of sufficient.In the present invention promptly, the stearate with 90 ℃ of dissolution characteristics is decided to be 0.1-0.45wt%, preferably is decided to be 0.1-0.4wt%, more preferably is decided to be 0.15-0.30wt%.When addition was very few, the effect that can not show that formability improves, mobilely improves, friction reduces etc. had served as for a long time on the contrary, thereby because the carbonization of the organic substance during sintering causes the density of sintered body to reduce, the unfavorable condition of magnetic characteristic Br deterioration.
In adhesive adds operation, when mixing the material powder that contains Magnaglo and adhesive, can take the method for under liquid condition or solid state, mixing.In the occasion of using liquid adhesive, easily produce cohesion, there is the tendency of the degree of orientation reduction of Magnaglo.In addition, in the occasion of the adhesive that uses solid, shaped, can see difficult mixed uniformly this problem.When mixing, use mixers such as Henschel blender, plunger fully to stir adhesive.
This adhesive adds the adding method and the order of shaping additive in the operation, that possess the afore mentioned rules rerum natura and wishes following carrying out.That is, preferably after mixed adhesive and Magnaglo, add shaping additive.Its reason be when the shaping auxiliary agent be present in adhesive and Magnaglo mixed powder around when being shaped, the effect of shaping additive promptly reduces friction, it is big to improve effect mobile, the raising formability.In addition, side by side add before adhesive adds or with adhesive and also obtain same effect.
[moisture adjustment operation]
Adjust in operation at this moisture, add moisture in mixture, perhaps reduce the moisture of moisture adjustment mixture to the shaping that contains above-mentioned raw materials powder, adhesive and shaping additive.
Mixed shaping causes very big influence for formability, magnetic characteristic with the amount of moisture of mixture.The preferred 0.20-0.80wt% of amount of moisture, preferred especially 0.25-0.35wt%.When amount of moisture during, during the shaping of next process, keep the desired form difficulty that becomes less than 0.20wt%.When amount of moisture surpasses 0.80wt%, cause the cohesion of Magnaglo, the permutation of infringement magnetic powder particles on the direction of principal axis of easy magnetization on the magnetic, magnetic characteristic (Br) reduces.The tendency of sintered density reduction, crackle, aperture takes place to produce in addition.
The moisture adjustment can make it to be amount of moisture arbitrarily by the management temperature and humidity.Preferred moisture adjustment of adopting room temperature to place to carry out or the tiny steam (about several microns to tens microns) by manufacturings such as constant temperature and humidity cabinet and sprayers carry out the interpolation of moisture.For example, when using atomizer etc. to make water particle become big, easily condense, the tendency of the orientation when upsetting shaping is arranged.
After such moisture is adjusted operation, preferably be provided for pulverizing the broken process that is shaped with the condensation product in the mixture.By broken process is set, for example can eliminate by the dry condensation product that generates (pulverize and form minuteness particle).When condensation product existed, when applying magnetic field in the dry pressing operation in magnetic field described later, the orientation difficulty became the reason that magnetic characteristic reduces.The occasion of additional this broken process after above-mentioned moisture is adjusted operation, preferably the amount of moisture in the mixture in the moment that broken process is over is 0.20-0.80wt%.Its reason is identical with the reason of narrating in above-mentioned moisture adjustment operation.
[dry pressing operation in the magnetic field]
The adjusted above-mentioned shaping of moisture is placed in the mould with mixture, suppresses in externally-applied magnetic field.Can make the direction of easy axis unanimity of material powder (magnetic powder particles) thus, improve magnetic characteristic.
In the present invention, put into shaping in the mould of dry pressing operation in the magnetic field with mixture (input raw material), being present in this shaping exists ratio to wish to be 0.01-0.80wt%, to be preferably 0.01-0.78wt% with the above condensation product of 500 μ m in the mixture.When this value surpassed 0.80wt%, when applying magnetic field in the dry pressing operation in magnetic field, it is difficult that orientation becomes, and the tendency of the reason that becomes the magnetic characteristic reduction is arranged.Lower limit also can be zero, but under the prior art level, thinks that 0.01wt% is suitable.
The condensation product that 500 μ m are above have a ratio, available following main points are obtained.That is, will be shaped with mixture be added to give vibration in 3 minutes on the automatic screen(ing) machine after, measure the ratio of the above condensation product of 500 μ m, the ratio that exists of being calculated the condensation product more than the 500 μ m by its measured value gets final product.
In the magnetic field in the dry pressing operation, alignment magnetic field is decided to be about 3-12kOe (239-955kA/m), forming pressure is decided to be 0.1-5ton/cm
2About.
The shaping thing of Xing Chenging is by ensuing sintering circuit sintering like this.
[sintering circuit]
The shaping thing that forms in the dry pressing operation in above-mentioned magnetic field is by this operation sintering.The preferred 1200-1260 of sintering temperature ℃ scope.When sintering temperature during, obtain the sufficient sintered density difficulty that becomes less than 1200 ℃.On the other hand, when sintering temperature surpasses 1260 ℃, cause that easily unusual grain length is big, the tendency that exists the iHc value to reduce.Be decided to be about 0.5-4.0 hour the stabilization time that is used for sintering.Sintering atmosphere can be in the atmosphere, while but by controlling the partial pressure of oxygen sintering, can obtain high density more, magnet that magnetic characteristic is higher.
Below enumerate specific embodiment and further describe the present invention.
With the Sr ferrite calcining powder of 100 weight portions and the SiO of 0.5 weight portion
2, and the CaCO of 1 weight portion
3It is broken that water carries out the wet type micro mist, and make the specific area of calcining powder reach 7.0m
2/ g.Then, make slurry dry, make the material powder of experiment usefulness.
After the material powder that obtains like this adds the adhesive shown in the following table 1, use the Henschel blender to mix 20 minutes at 90 ℃.Mix the back and add the shaping additive shown in the table 1, mixed again 3 minutes.
Details about shaping additive is as described below.
Sample 1 ... basis is calcium stearate, possesses 90 ℃ of dissolution characteristics (representing with zero in the table).With being dissolved in about 3 minutes in 90 ℃ the basic emulsion solution.
Sample 2 ... basis is calcium stearate, possesses 90 ℃ of dissolution characteristics (representing with zero in the table).With being dissolved in about 3 minutes in 90 ℃ the basic emulsion solution.
Sample 3 ... basis is calcium stearate, possesses 90 ℃ of dissolution characteristics (representing with zero in the table).With being dissolved in about 4 minutes in 90 ℃ the basic emulsion solution.
Sample 4 ... basis is zinc stearate, possesses 90 ℃ of dissolution characteristics (representing with zero in the table).With being dissolved in about 5 minutes in 90 ℃ the basic emulsion solution.
Sample 5 ... basis is dolomol, possesses 90 ℃ of dissolution characteristics (representing with zero in the table).With being dissolved in about 3 minutes in 90 ℃ the basic emulsion solution.
Sample 6 ... basis is aluminum stearate, possesses 90 ℃ of dissolution characteristics (representing with zero in the table).With being dissolved in about 6 minutes in 90 ℃ the basic emulsion solution.
Duplicate 1 ... basis is calcium stearate, does not possess 90 ℃ of dissolution characteristics (usefulness * expression in the table).Can not be dissolved in 90 ℃ the basic emulsion solution, residual cotton-shaped powder, the viscosity of solution also increases gradually.Finally dissolve up to about 120 ℃ by the temperature that improves basic emulsion solution.
Duplicate 2 ... basis is calcium stearate, does not possess 90 ℃ of dissolution characteristics (usefulness * expression in the table).Can not be dissolved in 90 ℃ the basic emulsion solution, residual cotton-shaped powder, the viscosity of solution also increases gradually.Finally dissolve up to about 110 ℃ by the temperature that improves basic emulsion solution.
Secondly, the amount of moisture use constant temperature and humidity cabinet of the mixed-powder that will cooperate with said sequence is adjusted to amount of moisture and reaches 0.30wt%.
, this mixed-powder used ultramicro grinding crusher machine, make permanent magnet material thereafter.
Then, with this permanent magnet material dry pressing in the magnetic field of about 7.5kOe.Forming pressure is decided to be 1ton/cm
2In atmosphere, 1240 ℃ of resulting formed bodies of sintering 1 hour, obtain the magnet sample of the about 26mm of diameter, high 10mm.
About the magnet sample that obtains like this, use (the eastern English industry (strain): dc magnetizing characteristic determinator TRF-5BH) carry out the magnetic characteristic evaluation of Br, iHc of B-H follow-up mechanism.
In addition, measure the density (dp) of formed body and the density (df) of sintered body with following main points.
The density of formed body (dp)
When obtaining volume V by the actual size of formed body, the actual measurement weight W is calculated divided by volume by weight.dp＝W/V
The density of sintered body (df)
The density of sintered body (df) is calculated based on the value of utilizing Archimedes's method to obtain.
And, based on following benchmark evaluation when mould is gone out the shaping thing punching press and the cracking frequency that when mould is gone out the shaping thing, takes place sometimes.If usually punching press uprises, then cracking frequency has the tendency that uprises.
Punching press (Kg/cm
2
)
((forming pressure is 1ton/cm to Φ 15.4mm * 5mm) form to use the mould that punch test uses
2), then, working strength testing machine (Instron MODEL-4550) is measured the punching press when mould is gone out the shaping thing.The speed of going out is decided to be 100mm/min.
Cracking frequency
Whether Visual Confirmation cracks when mould is gone out the shaping thing.Crackle takes place to divide in the bottom of shaping thing usually to confirm, the crackle of umbrella takes place to inside from bottom periphery.The bottom branch of shaping thing is the part of going out from mould at last, and when going out, instantaneous crustal stress is by lax, and therefore volumetric expansion sharp is the position of the easiest generation crackle.
The working sample number is 50.
The result is as shown in table 1.
The standard that each mensuration project in the table 1 should satisfy is to be stamped into 0.120 (Kg/cm
2) below, cracking frequency is 0/50, the density of formed body (dp) is 2.880 (Mg/m
3) more than, the density of sintered body (df) is 4.910 (Mg/m
3) more than, sintered body intensity is 16.0 (Kgf/mm
2) more than, Br is more than 3800 (G), iHc is more than 3000 (Oe).
Table 1
| Sample No. | Adhesive | Shaping additive | Punching press (Kg/cm2) | Cracking frequency | Formed body density d p (Mg/m3) | Sintered density df (Mg/m3) | Sintered body intensity (Kgf/mm2) | Br (G) | iHc (Oe) | ||||
| Kind | Molecular weight | Content (wt%) | Kind | 90 ℃ of dissolution characteristics | Content (wt%) | ||||||||
| Embodiment 1 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 1 | ○ | 0.10 | 0.105 | 0/50 | 2.915 | 4.938 | 18.1 | 3917 | 3085 |
| Embodiment 2 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 1 | ○ | 0.15 | 0.102 | 0/50 | 2.916 | 4.939 | 19.1 | 3913 | 3091 |
| Embodiment 3 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 1 | ○ | 0.20 | 0.091 | 0/50 | 2.912 | 4.937 | 17.6 | 3878 | 3093 |
| Embodiment 4 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 1 | ○ | 0.30 | 0.091 | 0/50 | 2.905 | 4.939 | 17.3 | 3805 | 3125 |
| Embodiment 5 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 1 | ○ | 0.40 | 0.085 | 0/50 | 2.903 | 4.937 | 17.0 | 3801 | 3128 |
| Embodiment 6 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 2 | ○ | 0.20 | 0.092 | 0/50 | 2.901 | 4.935 | 17.9 | 3811 | 3089 |
| Embodiment 7 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 3 | ○ | 0.20 | 0.088 | 0/50 | 2.900 | 4.929 | 17.3 | 3856 | 3003 |
| Embodiment 8 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 4 | ○ | 0.20 | 0.080 | 0/50 | 2.884 | 4.926 | 17.0 | 3817 | 3081 |
| Embodiment 9 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 5 | ○ | 0.20 | 0.110 | 0/50 | 2.895 | 4.916 | 16.2 | 3838 | 3092 |
| Embodiment 10 | Fatty acid ester is a wax | 400～600 | 0.36 | Sample 6 | ○ | 0.20 | 0.113 | 0/50 | 2.904 | 4.919 | 16.7 | 3826 | 3121 |
| Comparative example 1 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 1 | × | 0.10 | 0.167 | 12/50 | 2.908 | 4.935 | 15.7 | 3853 | 3092 |
| Comparative example 2 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 1 | × | 0.15 | 0.162 | 10/50 | 2.908 | 4.933 | 16.8 | 3852 | 3088 |
| Comparative example 3 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 1 | × | 0.20 | 0.158 | 7/50 | 2.909 | 4.930 | 15.3 | 3789 | 3112 |
| Comparative example 4 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 1 | × | 0.30 | 0.145 | 4/50 | 2.898 | 4.924 | 15.0 | 3691 | 3133 |
| Comparative example 5 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 1 | × | 0.50 | 0.117 | 2/50 | 2.896 | 4.917 | 14.4 | 3572 | 3206 |
| Comparative example 6 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 1 | × | 0.70 | 0.096 | 0/50 | 2.872 | 4.871 | 14.1 | 3523 | 3230 |
| Comparative example 7 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 2 | × | 0.40 | 0.137 | 5/50 | 2.885 | 4.920 | 15.7 | 3770 | 3170 |
| Comparative example 8 | Fatty acid ester is a wax | 400～600 | 0.36 | Duplicate 2 | × | 0.70 | 0.124 | 2/50 | 2.864 | 4.865 | 13.4 | 3732 | 3118 |
| Comparative example 9 | Camphor | 152 | 1.2 | Sample 1 | ○ | 0.20 | 0.131 | 2/50 | 2.903 | 4.904 | 16.3 | 3778 | 3191 |
| Comparative example 10 | microstaclean wax | 800 | 0.60 | Sample 1 | ○ | 0.20 | 0.189 | 12/50 | 2.906 | 4.910 | 16.0 | 2969 | 3341 |
| Comparative example 11 | Paraffin | 300～500 | 0.60 | Sample 1 | ○ | 0.20 | 0.157 | 7/50 | 2.925 | 4.930 | 17.1 | 3315 | 3195 |
| Comparative example 12 | Tissuemat E | 2000 | 0.60 | Sample 1 | ○ | 0.20 | 0.179 | 12/50 | 2.891 | 4.900 | 15.1 | 3361 | 3107 |
See that by The above results effect of the present invention is clear and definite.That is, of the present invention being constructed as follows is a kind of manufacture method of oxide magnetic material based permanent magnet, comprises following operation: the adhesive of adding and mixed adhesive and shaping additive adds operation in containing the material powder of oxidate magnetic material; Adjustment contains the moisture adjustment operation of the shaping of material powder, adhesive and shaping additive with the moisture in the mixture; To carry out the shaping of moisture adjustment and put into mould makes the direction of easy axis unanimity of oxidate magnetic material powder in the externally-applied magnetic field pressurization magnetic field dry pressing operation with mixture; Sintering circuit with the formed body of sintering formed thereby, wherein, adding the adhesive that uses in the operation at above-mentioned adhesive is that fatty acid ester is a wax, adding the shaping additive that uses in the operation at above-mentioned adhesive is stearate, and it is that wax is fastened in the pass and had the characteristic (90 ℃ of dissolution characteristics) of dissolving in the temperature below 90 ℃ with above-mentioned fatty acid ester as adhesive.Therefore, can seek low cost, the oxide magnetic material based permanent magnet of be improved simultaneously orientation and sintered density, magnetic characteristic excellence.
Industrial applicibility
The present invention can utilize when making oxide magnetic material based permanent magnet.
Claims (5)
1. the manufacture method of an oxide magnetic material based permanent magnet comprises following operation:
The adhesive of adding and mixed adhesive and shaping additive adds operation in the material powder that contains oxidate magnetic material,
Adjustment contains the moisture adjustment operation of the shaping of material powder, adhesive and shaping additive with the moisture in the mixture,
The above-mentioned shaping that to carry out the moisture adjustment is with the mixture mould of packing into, in externally-applied magnetic field pressurization make in the magnetic field of direction of easy axis unanimity of oxidate magnetic material powder the dry pressing operation and
The sintering circuit of the formed body of sintering formed thereby; It is characterized in that,
Adding the adhesive that uses in the operation at above-mentioned adhesive is that fatty acid ester is a wax,
Adding the shaping additive that uses in the operation at above-mentioned adhesive is stearate, and it is that wax is fastened in the pass and had the characteristic (90 ℃ of dissolution characteristics) of dissolving in the temperature below 90 ℃ with above-mentioned fatty acid ester as adhesive.
2. the manufacture method of oxide magnetic material based permanent magnet according to claim 1, above-mentioned stearate is select among calcium stearate, zinc stearate, dolomol and aluminum stearate at least a.
3. the manufacture method of oxide magnetic material based permanent magnet according to claim 1, the addition of above-mentioned stearate is 0.1-0.45wt%.
4. the manufacture method of oxide magnetic material based permanent magnet according to claim 1, above-mentioned fatty acid ester is that wax is vegetable wax.
5. the manufacture method of oxide magnetic material based permanent magnet according to claim 1, being shaped with the binder content in the mixture is 0.2-1.5wt%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003056893A JP2004266196A (en) | 2003-03-04 | 2003-03-04 | Manufacturing method of oxide magnetic material based permanent magnet |
| JP56893/2003 | 2003-03-04 |
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|---|---|
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| CN100538923C CN100538923C (en) | 2009-09-09 |
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|---|---|---|---|
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| Country | Link |
|---|---|
| JP (1) | JP2004266196A (en) |
| KR (1) | KR100656962B1 (en) |
| CN (1) | CN100538923C (en) |
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|---|---|---|---|---|
| CN109081690A (en) * | 2018-08-15 | 2018-12-25 | 横店集团东磁股份有限公司 | A kind of preparation method of the high two polar diameter anisotropy magnet ring of table magnetic dry-pressing of big height |
| TWI728913B (en) * | 2020-09-09 | 2021-05-21 | 中國鋼鐵股份有限公司 | Method of fabricating modified ferrite magnetic powder and method of fabricating modified ferrite magnet |
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| CN105384433B (en) * | 2015-10-27 | 2017-08-01 | 横店集团东磁股份有限公司 | A kind of manufacture method of permanent-magnet ferrite |
| CN110715836A (en) * | 2019-10-09 | 2020-01-21 | 国合通用测试评价认证股份公司 | Preparation method of magnetic material detection sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0497957A (en) * | 1990-08-10 | 1992-03-30 | Daido Steel Co Ltd | Method for removing binder in molded body of powder |
| JPH04137704A (en) * | 1990-09-28 | 1992-05-12 | Tokin Corp | Manufacture of oxide magnetic material |
| JPH05247297A (en) * | 1992-03-05 | 1993-09-24 | Mizusawa Ind Chem Ltd | Chlorinated resin composition |
| JPH0794312A (en) * | 1993-04-28 | 1995-04-07 | Kawasaki Steel Corp | Manufacture of ferrite magnet |
-
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- 2003-12-22 WO PCT/JP2003/016414 patent/WO2004079756A1/en active Application Filing
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Cited By (2)
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| CN109081690A (en) * | 2018-08-15 | 2018-12-25 | 横店集团东磁股份有限公司 | A kind of preparation method of the high two polar diameter anisotropy magnet ring of table magnetic dry-pressing of big height |
| TWI728913B (en) * | 2020-09-09 | 2021-05-21 | 中國鋼鐵股份有限公司 | Method of fabricating modified ferrite magnetic powder and method of fabricating modified ferrite magnet |
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| Publication number | Publication date |
|---|---|
| JP2004266196A (en) | 2004-09-24 |
| CN100538923C (en) | 2009-09-09 |
| WO2004079756A1 (en) | 2004-09-16 |
| TW200421359A (en) | 2004-10-16 |
| TWI267096B (en) | 2006-11-21 |
| KR100656962B1 (en) | 2006-12-13 |
| KR20050095764A (en) | 2005-09-30 |
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