CN103219120A - Method for manufacturing dust core and dust core obtained by the method - Google Patents
Method for manufacturing dust core and dust core obtained by the method Download PDFInfo
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- CN103219120A CN103219120A CN2012105670299A CN201210567029A CN103219120A CN 103219120 A CN103219120 A CN 103219120A CN 2012105670299 A CN2012105670299 A CN 2012105670299A CN 201210567029 A CN201210567029 A CN 201210567029A CN 103219120 A CN103219120 A CN 103219120A
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- epithelium
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B23/00—Uppers; Boot legs; Stiffeners; Other single parts of footwear
- A43B23/24—Ornamental buckles; Other ornaments for shoes without fastening function
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- A—HUMAN NECESSITIES
- A43—FOOTWEAR
- A43B—CHARACTERISTIC FEATURES OF FOOTWEAR; PARTS OF FOOTWEAR
- A43B23/00—Uppers; Boot legs; Stiffeners; Other single parts of footwear
- A43B23/02—Uppers; Boot legs
- A43B23/0205—Uppers; Boot legs characterised by the material
- A43B23/0225—Composite materials, e.g. material with a matrix
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Abstract
The invention provides a manufacturing method of dust core whose density is not reduced substantially and whose strength is improved, and the dust core. The key points of the manufacturing method of the dust core is that the method includes a forming procedure of obtaining dust core body through compressing a mixture of iron-based soft magnetic powder and lubricating agent; a heat treatment procedure 1 of heating the dust core body in a temperature range of 300 DEG C to 500 DEG C; a heat treatment procedure 2 of heating the dust core body in a temperature range of 500 DEG C to 700 DEG C in an oxidizing atmosphere; and a heat treatment procedure 3 of heating under a temperature in a range of 300 DEG C to 450 DEG C for more than 30 minutes and less than 120 minutes.
Description
Technical field
The compressed-core that the present invention relates to the manufacture method of compressed-core and get by this manufacture method.
Background technology
For compressed-core, importantly the operability in manufacturing process is good and have not damaged so abundant mechanical strength when making the coil spiral for electromagnetic component.Consider that from these aspects known useful electric insulation covers the technology of iron particles in the compressed-core field.Make between iron particles and be engaged by cover iron particles with electric insulation via electric insulation, therefore, use itself and the mechanical strength of compressed-core be improved.
So far, disclose and utilized by the glassy compound of gained such as the high silicone resin of thermal endurance, phosphoric acid the technology that forms material (patent documentation 1) as above-mentioned electric insulation.
In addition, the applicant changes into epithelium and silicone resin epithelium by form the phosphoric acid system of containing element-specific successively on the iron-based soft magnetic powder surface, thereby high magnetic flux density successfully is provided, has hanged down the compressed-core of iron loss, high mechanical properties, and be awarded patent right (patent documentation 2).
Yet, the requirement of the high performance of compressed-core is more improved during than patent documentation 2 applications, and more in the past than the compressed-core that needed high mechanical properties more.
The prior art document
Patent documentation
Patent documentation 1: No. 2710152 communique of Japan Patent
Patent documentation 2: No. 4044591 communique of Japan Patent
Summary of the invention
The present invention is conceived to above-mentioned situation and finishes, and its purpose is to provide manufacture method and the compressed-core that density is declined to a great extent and can make the compressed-core of intensity raising.
The manufacture method that can solve the compressed-core of the present invention of above-mentioned problem has following main idea, promptly comprises: will be mixed with and have press-powder formed body that phosphoric acid system changes into epithelium obtains the press-powder formed body with the mixture compression molding of iron-based soft magnetic powder and lubricant forming process on the iron-based soft magnetic powder surface; With above-mentioned press-powder formed body more than 300 ℃ and the heat treatment step 1 that heats of the temperature below 500 ℃; Then, the heat treatment step 2 that heats in oxidizing atmosphere, in the temperature that surpasses below 500 ℃ and 700 ℃; Again in more than 300 ℃ and the temperature below the 450 ℃ heating heat treatment step 3 more than 30 minutes and below 120 minutes.
Among the present invention, said mixture also contains at least a kind of oxygen source release compound that is selected from sugar alcohol, metal hydroxides, metal peroxides, percarbonate and the oxidant and also is preferred implementation.
In addition, above-mentioned press-powder formed body changes in above-mentioned phosphoric acid system with iron-based soft magnetic powder and has the silicone resin epithelium on the epithelium and also be preferred implementation.
Moreover above-mentioned lubricant is that multi-hydroxy carboxy acid's acid amides (polyhydroxy carboxylic acid) also is preferred implementation.
Also comprise the compressed-core that gets by above-mentioned manufacture method among the present invention.
In addition, the present invention also comprise the iron-based soft magnetic powder compression molding and compressed-core, preferably, for compressed-core, when measuring the plane of disruption with X-ray diffraction method, magnetic iron ore (magnetite) is that 5.0～15 volume %, wustite (wustite) are 3.0 volume % following (comprising 0 volume %).
Manufacturing method according to the invention can provide the compressed-core that density descends not significantly and mechanical strength is high.
Embodiment
Though it is known as mentioned above by the mixture that gets with electric insulation covering iron powder being heat-treated the manufacture method of the mechanical strength raising that makes compressed-core, but in order further to improve the mechanical strength of compressed-core, the inventor has carried out deep research repeatedly.The result is clear and definite in the ferriferous oxide that generates by heat treatment, and magnetic iron ore helps high strength and wustite becomes the principal element that intensity is reduced.Thereby so found wustite to be transformed into magnetic iron ore and can further to improve mechanical strength, thereby finished the present invention by suitable control heat-treat condition.
Below, the manufacture method of compressed-core of the present invention and the compressed-core that gets by this manufacture method are illustrated.
[forming process]
Compressed-core of the present invention makes by the press-powder formed body is carried out suitable heat treated.The press-powder formed body can have press-powder formed body that phosphoric acid system changes into epithelium and gets with the mixture compression molding of iron-based soft magnetic powder and lubricant by being mixed with on the iron-based soft magnetic powder surface.
[iron-based soft magnetic powder]
Iron-based soft magnetic powder is the iron-based powder of ferromagnetism body, particularly, can enumerate straight iron powder, iron(-)base powder (Fe-Al alloy, Fe-Si alloy, Sendust (sendust), permalloy (permalloy) etc.), Fe-based amorphous powder etc.These iron-based soft magnetic powders for example can make in the following manner, that is, reduce after utilizing atomization to make molten iron (or molten iron alloy) form particulate, pulverize afterwards etc. again.It is that 50% o'clock particle diameter (median particle diameter) is the iron-based soft magnetic powder about 20 μ m～250 μ m that this method for making can obtain in the particle size distribution cumulative particle size distribution of utilizing sieve method to estimate, but used iron-based soft magnetic powder preferable particle size (median particle diameter) is about 50 μ m～150 μ m among the present invention.
[phosphoric acid system changes into epithelium]
The press-powder formed body has phosphoric acid with iron-based soft magnetic powder (below, be sometimes referred to as " press-powder formed body iron powder ") on the surface of iron-based soft magnetic powder be to change into epithelium.Can give the press-powder formed body thus uses iron powder with electrical insulating property.
Phosphoric acid system changes into epithelium and is meant and uses the glass epithelium that contains the compound of P and form.Its composition is not particularly limited, preferably uses and except that containing P, also contain the compound of Co, Na, S or except that containing P, also contain the compound of Cs and/or Al and the glass epithelium that forms.This is because these elements suppress to descend because of oxygen and Fe form the ratio resistance that semiconductor causes when heat treatment step 2 described later.
In the above-mentioned element, P forms chemical bond by oxygen and iron-based soft magnetic powder surface.If P content is few, then the iron-based soft magnetic powder surface is insufficient with the chemical bond resultant that phosphoric acid system changes into epithelium, might not can form firm epithelium.On the other hand, if P content is too much, the P that does not then participate in chemical bond is residual with unreacted state, and bond strength is reduced.
Co, Na, S, Cs, Al hinder Fe and oxygen formation semiconductor when heat-treating operation 2, have the effect that rejection ratio resistance descends.By compound interpolation Co, Na and S, thereby can make its maximum effect.In addition, can add among Cs and the Al any.If excessive interpolation Co, Na, S, Cs, Al, the relative equilibrium in the time of then not only can not maintaining compound interpolation, and hinder the generation of the chemical bond that P forms by oxygen and iron-based soft magnetic powder surface sometimes.
When phosphoric acid system changes into epithelium for the glass epithelium that uses the compound that also contains above-mentioned Co etc. except that containing P and form, the containing ratio of these elements preferably, the press-powder formed body with iron powder (phosphoric acid system changes into the summation of epithelium and iron-based soft magnetic powder) 100 quality % in, P is that 0.005 quality %～1 quality %, Co is that 0.005 quality %～0.1 quality %, Na is that 0.002 quality %～0.6 quality %, S is 0.001 quality %～0.2 quality %.In addition, preferably Cs is that 0.002 quality %～0.6 quality %, Al is 0.001 quality %～0.1 quality %.Also with Cs and Al the time, also preferably make these elements respectively in above-mentioned scope.
Phosphoric acid system changes into epithelium and also can further contain Mg, B.The containing ratio of these elements be preferably the press-powder formed body with iron powder 100 quality % in Mg, B be 0.001 quality %～0.5 quality %.
The thickness that phosphoric acid system changes into epithelium is not particularly limited, if thickness is thin excessively, then insulation effect can not manifest sometimes.In addition, if thickness is blocked up, then insulation effect is saturated, and the densification of press-powder formed body, considers not preferred from these aspects.Preferred thickness be 1nm above, more preferably more than the 10nm, and be preferably 250nm following, more preferably below the 50nm.
[phosphoric acid system changes into the formation method of epithelium]
To form phosphoric acid on the iron-based soft magnetic powder surface is that the method that changes into epithelium is not particularly limited.For example can obtain in the following manner, that is, in the solvent that constitutes by water and/or organic solvent, mix making solution and the iron-based soft magnetic powder that contains the P-compound dissolving and get, make above-mentioned solvent evaporation afterwards as required.
As above-mentioned solvent, can enumerate hydrophilic organic solvent and their mixtures such as water, alcohol, ketone.Also can add known surfactant in the solvent.
As the above-mentioned P-compound that contains, can enumerate orthophosphoric acid (H
3PO
4).In addition, as making phosphoric acid system change into the compound that epithelium becomes above-mentioned composition, can use for example Co
3(PO
4)
2(Co and P source), Co
3(PO
4)
28H
2O (Co and P source), Na
2HPO
4(P and Na source), NaH
2PO
4(P and Na source), NaH
2PO
4NH
2O (P and Na source), Al (H
2PO
4)
3(P and Al source), Cs
2SO
4(Cs and S source), H
2SO
4(S source), MgO (Mg source), H
3BO
3(B source) etc.Wherein, if use biphosphate sodium salt (NaH
2PO
4) as P source, Na source, then can obtain density, intensity, than the compressed-core of resistance balance.
As long as containing P-compound is adjusted into respect to the addition of iron-based soft magnetic powder and makes formed phosphoric acid system change into the composition of epithelium in above-mentioned scope.For example, with respect to iron-based soft magnetic powder 100 mass parts, add being used for about 1～10 mass parts solid component content is adjusted into containing P-compound, contain the solution of the compound of the element that is included in epithelium as required about 0.01 quality %～10 quality %.And, utilize mixers such as known blender, ball mill, kneading machine, V-Mixer, comminutor to mix, be to change into the composition of epithelium in above-mentioned scope thereby can make formed phosphoric acid.
In addition, also can be as required after above-mentioned mixed processes, in atmosphere, decompression is down or under the vacuum, carries out drying at 150 ℃～250 ℃.Also can make it after drying by mesh is that sieve about 200 μ m～500 μ m is adjusted particle size distribution.Through above-mentioned operation, be the press-powder formed body iron powder that changes into epithelium thereby can obtain being formed with phosphoric acid on the iron-based soft magnetic powder surface.
[silicone resin epithelium]
Press-powder formed body of the present invention can be to change into further to have the silicone resin epithelium on the epithelium at above-mentioned phosphoric acid also with iron powder.Thus, (during compression) powder strong bonded each other when crosslinked, the curing reaction of silicone resin finishes.In addition, form the Si-O key of excellent heat resistance, can improve the thermal stability of insulating coating.
As silicone resin, just be not particularly limited as long as can obtain above-mentioned effect, if the curing of silicone resin is slow, then owing to powder the operability variation of remaining adhesiveness after epithelium is formed.Therefore, preferably has D unit (R than two functionalities
2SiX
2: X is a hydrolization group) the T unit (RSiX of more trifunctional
3: X is same as described above).In addition, if contain the Q unit (SiX of a large amount of four functionalities
4: X is same as described above), then powder secure bond each other when precuring can't be carried out follow-up forming process, and is therefore not preferred.Therefore, it is desirable to, silicone resin preferably contains the above T unit of 60 moles of %, more preferably contains the above T unit of 80 moles of %, further preferably contains the T unit of 100 moles of %.
As silicone resin, the Methylphenylsilanone resin that normally above-mentioned R is a methyl or phenyl has more phenyl person thermal endurance height.Yet under the heat-treat condition of the high temperature that the present invention will adopt, the existence of phenyl is but ineffective like this.Its reason infers it is because the large volume of phenyl has been upset fine and close glassy reticulate structure, can reduce the obstruction effect that thermal stability, reduction and iron form compound on the contrary.Therefore, in the present invention, preferred use methyl be the above Methylphenylsilanone resin of 50 moles of % (for example, KR255, the KR311 etc. of chemical industrial company of SHIN-ETSU HANTOTAI system), more preferably 70 moles of % are above (for example, the KR300 of chemical industrial company of SHIN-ETSU HANTOTAI system etc.), most preferably use do not contain phenyl fully the methyl silicone resin (for example, KR251, the KR400 of chemical industrial company of SHIN-ETSU HANTOTAI system, KR220L, KR242A, KR240, KR500, KC89 etc., the SR2400 of Dong Li Dow Corning Corporation system etc.).In addition, can wait by FT-IR and analyze for the methyl of silicone resin (epithelium) and ratio, the functionality of phenyl.
To change into the press-powder formed body that is formed with the silicone resin epithelium on the epithelium in phosphoric acid system and use iron powder (promptly, iron-based soft magnetic powder, phosphoric acid system change into the summation of epithelium and silicone resin epithelium) when being made as 100 quality %, preferably the adhesion amount with the silicone resin epithelium is adjusted into 0.05 quality %～0.3 quality %.If the silicone resin epithelium is less than 0.05 quality %, then the press-powder formed body is with the poor insulativity of iron powder, and resistance reduces.In addition, during more than 0.3 quality %, be difficult to reach the densification of gained press-powder formed body at the silicone resin epithelium.
The thickness of silicone resin epithelium is not particularly limited, from obtaining the viewpoint of above-mentioned effect, be preferably 1nm above, more preferably more than the 20nm, and be preferably 200nm following, more preferably below the 150nm.In addition, phosphoric acid system changes into the gross thickness of epithelium and silicone resin epithelium as long as determine suitably that in the scope of above-mentioned each thickness if thickness is blocked up, then the decline of magnetic flux density is excessive sometimes, so gross thickness is preferably below the 250nm.
[the formation method of silicone resin epithelium]
Be not particularly limited changing into the method that forms the silicone resin epithelium on the epithelium in phosphoric acid system.For example, with make silicone resin be dissolved into oil such as alcohols or toluene, dimethylbenzene be organic solvent etc. and silicone resin solution with have the iron-based soft magnetic powder (below, be sometimes referred to as " phosphoric acid is that epithelium forms iron powder ") that phosphoric acid system changes into epithelium and mix.Then, make above-mentioned organic solvent evaporation as required, thereby can form the silicone resin epithelium.
As long as silicone resin is that the addition that epithelium forms iron powder makes the adhesion amount of formed silicone resin epithelium in above-mentioned scope with respect to phosphoric acid.For example, change into epithelium with respect to above-mentioned phosphoric acid system and form iron powder 100 mass parts, add so that solid constituent for silicone resin solution 0.5～10 mass parts that roughly mode of 2 quality %～10 quality % prepares about, and mixed, dry getting final product.If the addition of silicone resin solution is less than 0.5 mass parts, then may makes to mix and expend time in or epithelium becomes inhomogeneous.On the other hand, if the addition of silicone resin solution above 10 mass parts, then may make drying expend time in or drying becomes insufficient.Silicone resin solution also can suitably heat in advance.Mixer can use mixer same as described above.
It is desirable to, in above-mentioned interpolation, after mixing drying process is set, described drying process heats making under used organic solvent volatilization and the temperature less than the curing temperature of silicone resin, and organic solvent is fully volatilized.As concrete baking temperature, be to be about 60 ℃～80 ℃ under the situation of organic solvent at above-mentioned alcohols, oil.After the drying,, preferably make it in advance by the sieve about mesh 300 μ m～500 μ m in order to remove the cohesion agglomerate.
In addition, recommendation be, heat with iron powder (below, be sometimes referred to as " the silicone resin epithelium forms iron powder ") change into the press-powder formed body that is formed with the silicone resin epithelium on the epithelium in phosphoric acid system, make the precuring of silicone resin epithelium.So-called precuring is the processing of instigating the softening process of silicone resin epithelium when solidifying to finish with pulverulence.Handle by this precuring, can when warm forming, (about 100～250 ℃) guarantee that the silicone resin epithelium forms the flowability of iron powder.As concrete method, easy having forms near the iron powder method that the short time heats the curing temperature of this silicone resin with the silicone resin epithelium, also can utilize the method for using reagent (curing agent).Difference between precuring and curing (being not that preparation is solidified but full solidification) are handled is, during precuring is handled, powder each other can complete bonding curing, can easily decompose fragmentation, relative therewith, in the heat cured of after the shaping of powder, carrying out, the curing that is bonded to each other of resin solidification, powder.Handle the formed body intensity enhancing by full solidification.
As mentioned above, make and it is decomposed after the silicone resin precuring brokenly, can obtain mobile excellent powder thus, when compression molding, can put in the finishing die like that by astigmatism sand.If do not make it precuring, for example occur sometimes then that powder is attached to each other when warm forming, be difficult to put in the finishing die at short notice.In practical operation, the raising of operability is very significant.In addition, find the ratio resistance of gained compressed-core to be significantly improved by making it precuring.Its reason is still indeterminate, but think perhaps be since when solidifying the press-powder formed body with the cause of iron powder connecting airtight property raising each other.
When utilizing the short time heating to carry out precuring, the heat treated of carrying out under 100～200 ℃ 5～100 minutes gets final product.More preferably carried out 10～30 minutes at 130～170 ℃.Preferably after precuring, also sieve as described above.
[lubricant]
Among the present invention, be that epithelium forms iron powder (or the silicone resin epithelium forms iron powder) and mix lubricant and forms mixture with phosphoric acid.By the effect of this lubricant, between the iron powder in the time of can being reduced in the mixture compression molding or the frictional resistance between iron powder and finishing die inwall, and can prevent that formed body from clinging mould, heating when preventing to be shaped.For effective this effect of performance, be that epithelium forms the lubricant that contains in the amount of the mixture of iron powder (or the silicone resin epithelium forms iron powder) and lubricant (adding when containing oxygen source release compound) more than the 0.2 quality % preferably at phosphoric acid.But, if the amount of lubricant is too much, then be unfavorable for the densification of press-powder formed body, therefore preferably be limited to below the 0.8 quality %.In addition, when compression molding, behind finishing die internal face application of lubricating, filling mixture forms (mould is lubricated to be shaped), in this case, even the amount of lubricant also can obtain above-mentioned effect less than 0.2 quality %.
As lubricant, can use known in the past lubricant.Particularly, can enumerate stearic metal salt powders such as zinc stearate, lithium stearate, calcium stearate, fatty acid amides such as multi-hydroxy carboxy acid's acid amides, ethylenebis stearic amide, (N-octadecylene base) palmitic amide, paraffin, wax, natural or synthetic resin derivative etc.Wherein, preferred multi-hydroxy carboxy acid's acid amides, fatty acid amide.These lubricants can use separately, also can be used in combination of two or more.
As multi-hydroxy carboxy acid's acid amides, can enumerate the C that puts down in writing in the WO2005/068588 communique for example
mH
M+1(OH)
m-CONH-C
nH
2n+1(m is 2 or 5, n is 6～24 integer).
More specifically, can enumerate following multi-hydroxy carboxy acid's acid amides.
(1)n-C
2H
3(OH)
2-CONH-n-C
6H
13
(N-hexyl) glyceric acid acid amides
(2)n-C
2H
3(OH)
2-CONH-n-C
8H
17
(N-octyl group) glyceric acid acid amides
(3)n-C
2H
3(OH)
2-CONH-n-C
18H
37
(N-octadecyl) glyceric acid acid amides
(4)n-C
2H
3(OH)
2-CONH-n-C
18H
35
(N-octadecylene base) glyceric acid acid amides
(5)n-C
2H
3(OH)
2-CONH-n-C
22H
45
(N-docosyl) glyceric acid acid amides
(6)n-C
2H
3(OH)
2-CONH-n-C
24H
49
(N-tetracosyl) glyceric acid acid amides
(7)n-C
5H
6(OH)
5-CONH-n-C
6H
13
(N-hexyl) gluconic acid acid amides
(8)n-C
5H
6(OH)
5-CONH-n-C
8H
17
(N-octyl group) gluconic acid acid amides
(9)n-C
5H
6(OH)
5-CONH-n-C
18H
37
(N-octadecyl) gluconic acid acid amides
(10)n-C
5H
6(OH)
5-CONH-n-C
18H
35
(N-octadecylene base) gluconic acid acid amides
(11)n-C
5H
6(OH)
5-CONH-n-C
22H
45
(N-docosyl) gluconic acid acid amides
(12)n-C
5H
6(OH)
5-CONH-n-C
24H
49
(N-tetracosyl) gluconic acid acid amides
[oxygen source release compound]
Said mixture preferably also contains oxygen source and discharges compound.During heating press-powder formed body, discharge compound from oxygen source and discharge oxygen sources such as oxygen, water, hydrogen peroxide, further promote of the oxidation of press-powder formed body with the iron powder surface.Particularly, by so that this oxygen source discharges the mode that compound also is configured in the inside of press-powder formed body mixes, thereby when heat treatment step, also carry out of the oxidation of press-powder formed body with the iron powder surface in press-powder formed body inside.
As a result, for compressed-core of the present invention, the press-powder formed body becomes firmly with combining of insulating coating (for example phosphoric acid system changes into epithelium) with the iron powder surface, and insulating coating combination each other simultaneously also becomes firmly, so mechanical strength improves.In addition, the ratio resistance (insulating properties) of compressed-core also increases.
In order effectively to bring into play such effect, discharge in the amount of the mixture of compound with iron powder (iron-based soft magnetic powder, phosphoric acid system change into epithelium, silicone resin epithelium), lubricant and oxygen source at the press-powder formed body, the content that oxygen source discharges compound is preferably more than the 0.01 quality %, more preferably more than the 0.05 quality %.Yet, if discharging compound, oxygen source becomes many, be unfavorable for the densification of press-powder formed body, therefore be preferably below the 0.8 quality %, more preferably below the 0.6 quality %.
Discharge compound as oxygen source, just there is no particular limitation so long as discharge the compound of oxygen sources such as oxygen, water, hydrogen peroxide by heating, can enumerate for example antierythrite, glycerine, isomalt (isomalt), lactitol, maltitol, sweet mellow wine, D-sorbite, xylitol etc. discharge water outlet by heating sugar alcohol; Magnesium hydroxide, aluminium hydroxide, calcium hydroxide, manganous hydroxide, iron hydroxide, cobalt hydroxide, nickel hydroxide, Kocide SD etc. discharge the metal hydroxides of water outlet by heating; Lithium peroxide, sodium peroxide, zinc peroxide etc. discharge the metal peroxides of oxygen by heating; SODIUM PERCARBONATEs etc. discharge and will resolve into the percarbonate of the hydrogen peroxide of water and oxygen by heating; Oxidants such as nitric acid anion, nitrous acid anion, salt acid anion.As the anionic counter ion counterionsl gegenions (cation) of oxidant, can lithium ion, sodium ion, potassium ion, ammonium ion, calcium ion, strontium ion, barium ions etc. be shown example.These oxygen sources discharge compound and may be used alone, can also be used in combination two or more.
[compression molding]
The press-powder formed body is by getting the said mixture compression molding.There is no particular limitation for compression forming method, can adopt known method in the past.
The suitable condition of relevant compression molding, in face pressure aspect, be preferably 490MPa above, more preferably above, the further preferred 790MPa of 700MPa above, further more than the preferred 980MPa, and preferred 1960MPa is following, more preferably below the 1180MPa.Particularly, if the condition more than 980MPa is carried out compression molding, then obtaining final densities easily is 7.40g/cm
3Above compressed-core, and can obtain high strength, the good compressed-core of magnetic characteristic (magnetic flux density), therefore preferred.For forming temperature, can be shaped for room temperature, warm forming (100～250 ℃) any.Preferably, the lubricated shaping of above-mentioned mould carried out warm forming,, can obtain more high-intensity compressed-core by such shaping.As the target of compressed-core intensity, the rupture strength that utilizes the assay method in aftermentioned embodiment to record is preferably more than the 70MPa, more preferably more than the 80MPa.
Among the present invention, the press-powder formed body that gets by 1～3 pair of compression molding of following heat treatment step carries out heat treated, thereby can make high-intensity compressed-core.
[heat treatment step 1]
In the manufacture method of the present invention, at first more than 300 ℃ and the press-powder formed body of the temperature below 500 ℃ after to compression molding heat.By this operation, can prevent insulating coating (phosphoric acid system changes into epithelium and/or silicone resin epithelium) breakage, and simultaneously the lubricant thermal decomposition be removed.
In addition, under the situation of adding oxygen source release compound, make oxygen sources such as oxygen, water, hydrogen peroxide discharge compound from oxygen source slowly releases by this heating, therefore can suppress the sealing of the oxygen source path between the iron powder of press-powder formed body inside for a long time, and promote simultaneously lubricant evaporation, disperse.
Heat treatment step 1, particularly, the method that can be listed below: in pressure vessel, drop into after the press-powder formed body, in container, enclose aftermentioned gas make in the container saturated after, in the said temperature scope, heat in to container.
The atmosphere of heat treatment step 1 is not particularly limited, and can be oxidizing atmospheres such as atmosphere, oxygen, ozone, steam, perhaps rare gas such as nitrogen, helium, argon gas, any in the torpescence atmosphere such as vacuum.
In addition, in each atmosphere, in the scope of the purpose that does not hinder heat treatment step 1, also can contain other gases.
In addition, the temperature of heat treatment step 1 is set at when being lower than 300 ℃ temperature, the decomposition of lubricant is removed effect and is become insufficient.Therefore, the temperature of heat treatment step 1 is more than 300 ℃, is preferably more than 330 ℃.On the other hand, if temperature is too high, then in the decomposition that fully is lubricated agent, carry out the oxidation of press-powder formed body before removing, cause volumetric expansion, the volatilization path of lubricant is blocked, lubricant can not fully be removed.Therefore, the oxygen that supplies to formed body inside is insufficient, and the formed body interior oxidation is suppressed.If above-mentioned situation takes place, the mechanical strength of formed body (losing intensity) deterioration then.Therefore, the temperature of heat treatment step 1 be below 500 ℃, be preferably below 480 ℃, more preferably below 450 ℃.
As long as can reach above-mentioned heat treatment purpose the heating time in the heat treatment step 1, be not particularly limited.Heating time in short-term, can not fully enjoy the above-mentioned effect of bringing by heat treatment step 1 sometimes.Therefore, heating time is preferred more than 10 minutes, more preferably more than 20 minutes, and preferred below 250 minutes, more preferably below 200 minutes, further preferred below 150 minutes.
[heat treatment step 2]
In the manufacture method of the present invention, be included in the operation (heat treatment step 2) that in oxidizing atmosphere, heats after the above-mentioned heat treatment step 1 in the temperature that surpasses below 500 ℃ and 700 ℃.By this operation, the shaping of the press-powder of the inside of press-powder formed body obtains promoting that simultaneously, the iron powder surface changes into combining between the epithelium with phosphoric acid system and becomes firm with the oxidation of iron powder.And then the combination each other of the insulating coating of adjacency also becomes firmly, and the mechanical strength of gained compressed-core is improved.
In addition, when adding oxygen source release compound,, thereby utilize the oxygen source that discharges from oxygen source release compound can further promote press-powder formed body interior oxidation by this heating.
In addition, among the present invention, each heat treatment step can carry out continuously, is heated to the temperature of regulation after also can temporarily cooling off again.During atmosphere in the conversion container, also can for example after finishing, temporarily cool off heat treatment step 1 the press-powder formed body, then with oxidizing gas to replacing in the pressure vessel, with oxidizing gas make in the container saturated after, heat-treat operation 2 with being heated to set point of temperature in the container.In addition, when constant ventilation atmosphere, it is desirable to for example heat-treat continuously operation 1 and heat treatment step 2.That is, also can after heat treatment step 1 finishes, temporarily not cool off and directly be warming up to set point of temperature and heat-treat operation 2.
For the atmosphere in the heat treatment step 2, need under oxidizing atmosphere, carry out for the oxidation that promotes iron powder, if carry out in non-active atmosphere such as nitrogen, then oxidation becomes insufficient, is difficult to obtain high mechanical properties.Heat treatment step 2 is implemented to get final product in above-mentioned oxidizing atmosphere, considers from the manufacturing cost aspect, and also can be air atmosphere.
Heat treatment temperature in heat treatment step 2 is crossed when low, and the inside that the insufficient or oxidation of the oxidation of iron powder sometimes proceeds to the press-powder formed body needs for a long time.In addition, when heat treatment temperature was too high, iron powder and phosphoric acid system changed into the boundary strength decline between the epithelium sometimes, and the mechanical strength of compressed-core descends.In addition, if insulating coating is exposed to high temperature, then because of making insulating properties, thin-walled property descends sometimes.The heating-up temperature of heat treatment step 2 is preferably more than 530 ℃, more preferably more than 550 ℃, and be preferably below 680 ℃, more preferably below 650 ℃.
As long as reach above-mentioned heat treatment purpose the heating time in the heat treatment step 2, there is no particular limitation., when too short, can not fully enjoy the above-mentioned effect of bringing by heat treatment step 2 in heating time sometimes.Therefore, be preferably heating time more than 10 minutes, more preferably more than 15 minutes.In addition, consider that heating time, the elder was preferred from the viewpoint of separating de-stress, still, if carry out high-temperature heat treatment for a long time, then sometimes as described above because the thin-walled property of insulating coating makes insulating properties decline.Therefore, be preferably heating time below 60 minutes, more preferably below 50 minutes, more preferably below 40 minutes.
[heat treatment step 3]
In the manufacture method of the present invention, also be included in after the above-mentioned heat treatment step 2 in more than 300 ℃ and the heating of the temperature below 450 ℃ more than 30 minutes and the operation below 120 minutes (heat treatment step 3).By this operation, wustite is transformed into magnetic iron ore, realized that minimizing causes the low wustite of intensity, increase the magnetic iron ore that helps high strength simultaneously, therefore, the mechanical strength of gained compressed-core is further improved.Particularly, the volume fraction that can obtain magnetic iron ore as described later is 5.0～15%, the volume fraction of wustite is the compressed-core that (comprises 0%) below 3.0%.
By in the temperature range of regulation, heat-treating operation 3, can prevent that the magnetic iron ore that has generated from being encircled by broken, and simultaneously wustite is transformed into magnetic iron ore.When under being lower than 300 ℃ temperature, heat-treating operation 3, wustite magnetic iron ore can not be transformed into, high strength can't be realized.In addition, when under being higher than 450 ℃ temperature, heat-treating operation 3, newly grow wustite sometimes.The heating-up temperature of heat treatment step 3 is preferably more than 320 ℃, more preferably more than 340 ℃, and be preferably below 430 ℃, more preferably below 410 ℃.
In addition, in above-mentioned heat-treatment temperature range, be more than 30 minutes and below 120 minutes heating time.Heating time in short-term, wustite can not be transformed into magnetic iron ore fully sometimes, thereby can not improve mechanical strength.Therefore, be preferably heating time more than 40 minutes, more preferably more than 50 minutes.Consider that from the viewpoint that promotes wustite to generate magnetic iron ore heating time, the elder was preferred, if carry out high-temperature heat treatment for a long time, then newly grew wustite sometimes.Therefore, be preferably heating time below 110 minutes, more preferably below 90 minutes.
[compressed-core]
After the press-powder formed body heat-treated, make it to be back to normal temperature, can obtain compressed-core of the present invention as long as cool off.
In sum, in manufacture method of the present invention,, then can make the compressed-core that has than high in the past mechanical strength if heat-treat operation 1～heat treatment step 3 under these conditions.
Particularly, can obtain magnetic iron ore is that 5.0～15 volume %, wustite are the 3.0 volume % compressed-cores of following (comprising 0 volume %).
If the volume fraction of magnetic iron ore is low excessively, then can not obtain full intensity, in addition, if volume fraction is too high, intensity reduces on the contrary.Therefore, magnetic iron ore be preferably 5.0 volume % above, more preferably 5.2 volume % above, more preferably more than the 5.5 volume %, and be preferably 15 volume % following, more preferably 13 volume % following, more preferably below the 11 volume %.
In addition, if the volume fraction of wustite uprises, the volume fraction of then intensity step-down, so wustite is preferably below the 3.0 volume %, more preferably below the 1.0 volume %, does not further preferably contain (0 volume %) wustite fully.
The volume ratio of magnetic iron ore and wustite (mean value) can get by the plane of disruption (a plurality of arbitrarily position) that utilizes X-ray diffraction method to measure compressed-core.
In addition, the remainder beyond magnetic iron ore and the wustite is organized as bloodstone, iron etc., and from guaranteeing the viewpoint of mechanical strength, suitably the volume fraction of controlling magnet ore deposit and wustite gets final product, and is not particularly limited for the structure of other remainder tissues.
Embodiment
Below, enumerate embodiment and be described more specifically the present invention, but the present invention is not subjected to the restriction of following embodiment, can in the scope that can meet the described purport of context, suitably implement after changing, it also includes in technical scope of the present invention.
(forming process)
As iron-based soft magnetic powder, prepare straight iron powder (refreshing Kobe system steel made " Atomel (ア ト メ Le) (registered trade mark) ML35N ", average grain diameter 100～150 μ m), form ferric phosphate at this powder surface and change into epithelium and obtain press-powder formed body iron-based soft magnetic powder.Particularly, with respect to having passed through mesh is the above-mentioned straight iron powder 1kg of the sieve of 300 μ m, adding also, mixed phosphate iron changes into epithelium treatment fluid 50mL, then, in atmosphere in 200 ℃ of dryings 30 minutes, by the sieve of mesh 300 μ m, obtain press-powder formed body iron-based soft magnetic powder (thickness 20nm).
Change into the epithelium treatment fluid as ferric phosphate, use following and treatment fluid, that is, and with water: 50 parts, NaH
2PO
4: 30 parts, H
3PO
4: 10 parts, (NH
2OH)
2H
28O
4: 10 parts, Co
3(PO
4)
2: 10 parts of mixing, again 10 times of dilute with waters and treatment fluid (phosphoric acid concentration 1.5 quality %).
Then, silicone resin (Dong Li Dow Corning Corporation system " SR2400 ") is dissolved in the toluene, the resin solution of the solid component concentration of preparation 4.8%.Is the mode of 0.05 quality % with the adhesion amount of silicone resin epithelium with respect to being formed with the press-powder formed body iron powder that phosphoric acid system changes into epithelium and silicone resin epithelium, adds and mixes this resin solution.Then, in baking oven, in atmosphere after 75 ℃ of heating were carried out drying in 30 minutes, by the sieve of mesh 300 μ m.Afterwards, carried out precuring 30 minutes, obtain having press-powder formed body iron-based soft magnetic powder (the silicone resin thickness: 100nm) of silicone resin epithelium at 150 ℃.
Then, to be the mode of 0.2 quality % with the amount of the mixture that iron powder, lubricant and oxygen source discharge compound, to add and mix multi-hydroxy carboxy acid's amide lubricant, thereby obtain mixture as lubricant with respect to the press-powder formed body.
In addition, for a part of embodiment, also being the mode of 0.1 quality % with the amount of the mixture that iron powder, lubricant and oxygen source discharge compound with respect to the press-powder formed body that is formed with the silicone resin epithelium, add and mixture table 1 described oxygen source releasing agent (oxygen source release compound), thereby obtain mixture.
This mixture is filled in the mould, presses under 784MPa, the room temperature (25 ℃) at face and carry out compression molding, obtain press-powder formed body (vertical 31.75mm * horizontal 12.7mm * about 5mm of height).
(heat treatment step)
Then, under the condition of table 1 record, the press-powder formed body is implemented heat treatment step 1～3 (in No.11～14, not heat-treating operation 3).After heat treatment step 3 finished, directly cooling (stove is cold) was made compressed-core to room temperature in container.The average heating speed that is warmed up to the set point of temperature of heat treatment step 1 and heat treatment step 2 is controlled in about 10 ℃/minute.In addition, the average cooling rate that cools to the set point of temperature of heat treatment temperature 3 from heat treatment temperature 2 is controlled in about 10 ℃/minute.In addition, each heat treatment step carry out continuously (for example, among the No.1,300 ℃ heat-treat operation 1 after, then be warming up to 550 ℃ and heat-treat operation 2).
(evaluation)
Will be to density, rupture strength and the magnetic iron ore (Fe of each compressed-core of making
3O
4) and the volume ratio of wustite (FeO) measure the results are shown in table 2.
(density)
Calculate density from the quality of compressed-core and the measured value of size.Among the present invention, be 7.40g/cm with density
3Above average evaluation is qualified.
(rupture strength)
To the rupture strength of compressed-core carry out 3 bend tests (with Japanese powder metallurgy industry can JPMA M 09-1992 be benchmark) estimate mechanical strength.Measure and use cupping machine (Shimadzu Seisakusho Ltd.'s system " AUTOGRAPH AG-5000E "), length of support is from being set at 25mm.With rupture strength is that average evaluation more than the 70MPa is qualified, will be defective less than the average evaluation of 70MPa.
(volume ratio)
The magnetic iron ore that contains in the compressed-core and the volume ratio of wustite use the test film after the above-mentioned bending test to measure.Particularly, the face irradiation X ray that exposes rupturing because of bending test is implemented X-ray diffraction and is measured, and obtains the volume ratio of magnetic iron ore and wustite.Determinator uses the system X-ray diffraction device RAD-RU300 of Co., Ltd. of science.The K alpha ray that use is produced by Co target and monochromator, (2 θ) measures with 15～110 ° mensuration angles.The irradiated area of the X ray in the mensuration face is horizontal approximately 10mm * vertical 15mm, amounts to 3 positions as evaluation object with central portion, the two ends of the plane of disruption.To from Fe
3O
4The peak, from the peak of FeO with from the peak of Fe carrying out peak fitting, obtain magnetic iron ore (Fe
3O
4), the volume ratio of wustite (FeO).
[table 1]
[table 2]
In No.1～10 of satisfying of the present invention creating conditions (heat treatment step 1～3), oxidation proceeds to the inside of compressed-core, obtains the high compressed-core of mechanical strength.Particularly in No.6～10 of having added oxygen source releasing agent (oxygen source release compound), compare with the No.1 that does not add the oxygen source releasing agent～5, oxidation obtains promoting, therefore can obtain having the more compressed-core of high mechanical properties.
On the other hand, in the No.11 that creates conditions～24 of discontented unabridged version invention, can not improve the mechanical strength of compressed-core.
Particularly, in the No.11 that does not heat-treat operation 3～14, can not reduce wustite, the mechanical strength of compressed-core reduces.
Among the No.15 that heating-up temperature in heat treatment step 1 is low, 16, can not fully decompose lubricant, after heat treatment step in oxidation fully do not carry out, so magnetic iron ore reduces, the mechanical strength of compressed-core reduces.
On the other hand, among the No.17 that the heating-up temperature in heat treatment step 1 is high, 18, owing to carried out the oxidation of formed body before fully removing at lubricant, so the oxidation of formed body is suppressed, and can not guarantee sufficient magnetic iron ore, and mechanical strength reduces.
Among the low No.19 of heating-up temperature in heat treatment step 2, oxidation is not fully carried out, and therefore can not guarantee sufficient magnetic iron ore, and mechanical strength is low.
On the other hand, among the No.20 that the heating-up temperature in heat treatment step 2 is high, 21, hyperoxidation carries out, and mechanical strength reduces.
Atmosphere at heat treatment step 2 is that oxidation is not fully carried out among the No.22,23 of nitrogen, can not guarantee sufficient magnetic iron ore, and mechanical strength reduces.
In the No.24 of the weak point heating time of heat treatment step 3, can not reduce FeO, mechanical strength reduces.
Claims (6)
1. the manufacture method of a compressed-core, it comprises:
Has press-powder formed body that phosphoric acid system changes into epithelium obtains the press-powder formed body with the mixture compression molding of iron-based soft magnetic powder and lubricant forming process on the iron-based soft magnetic powder surface with being mixed with;
With described press-powder formed body more than 300 ℃ and the heat treatment step 1 that heats of the temperature below 500 ℃;
Then, the heat treatment step 2 that heats in oxidizing atmosphere, in the temperature that surpasses below 500 ℃ and 700 ℃;
Again in more than 300 ℃ and the temperature below the 450 ℃ heating heat treatment step 3 more than 30 minutes and below 120 minutes.
2. the manufacture method of compressed-core according to claim 1, wherein, described mixture also contains at least a kind of oxygen source that is selected from sugar alcohol, metal hydroxides, metal peroxides, percarbonate and the oxidant and discharges compound.
3. the manufacture method of compressed-core according to claim 1, wherein, described press-powder formed body changes in described phosphoric acid system with iron-based soft magnetic powder has the silicone resin epithelium on the epithelium.
4. the manufacture method of compressed-core according to claim 1, wherein, described lubricant is multi-hydroxy carboxy acid's acid amides.
5. compressed-core, it gets by the described manufacture method of claim 1.
6. compressed-core, it is characterized in that, it is with the iron-based soft magnetic powder compression molding and the compressed-core that gets, and when utilizing X-ray diffraction method to measure the plane of disruption of described compressed-core, magnetic iron ore is that 5.0～15 volume %, wustite are below the 3.0 volume % and comprise 0 volume %.
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| JP (1) | JP6159531B2 (en) |
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| JP6159531B2 (en) | 2017-07-05 |
| KR20130085007A (en) | 2013-07-26 |
| KR101420562B1 (en) | 2014-07-16 |
| CN103219120B (en) | 2016-02-10 |
| MY156645A (en) | 2016-03-15 |
| JP2013168648A (en) | 2013-08-29 |
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