CN101056729A - Method for producing soft magnetic metal powder coated with Mg-containing oxide film and method for producing composite soft magnetic material from the powder - Google Patents
Method for producing soft magnetic metal powder coated with Mg-containing oxide film and method for producing composite soft magnetic material from the powder Download PDFInfo
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Abstract
The invention provides a manufacturing method of a composite soft magnetic metal powder which is coated with a magnesium-containing oxide film and a method which adopts the composite soft magnetic metal powder which is coated with a magnesium-containing oxide film for manufacturing a composite soft magnetic material. In the atmosphere of oxidation, the Mg powder is added in the soft magnetic metal powder which is the heat processed under the temperature of 40 to 500 DEG C for mixing; the mixed powder is heated in the atmosphere of inert gas or the vacuum atmosphere at the temperature of 150 to 1100 DEG C and the pressure of 1 multiplied by 10 <minus 12> to 1 multiplied by 10 <minus 1> MPa, or the mixed powder is heated and rotated simultaneously, then the composite soft magnetic metal powder which is coated with the magnesium-containing oxide film is manufactured, and the composite soft magnetic material is manufactured by using the composite soft magnetic metal powder which is coated with the magnesium-containing oxide film.
Description
Technical field
The present invention relates to contain the manufacture method of Mg oxide-film lining soft magnetic metal powder and adopt the method that Mg oxide-film lining soft magnetic metal powder is made the composite soft magnetic material that contains that method in view of the above makes, this composite soft magnetic material is as for example magnetic core, electric core, the generator magnetic core, solenoid core (solenoid core), ignition coil iron core (ignition core), reactor core (reactor core), transformer core (transformer core), the former material of choke coil iron core (choke coil core) or Magnetic Sensor magnetic core various electromagnetic circuit elements such as (sensor core) uses.
In addition, the invention still further relates to and be used to make the material powder that contains Mg oxide-film lining soft magnetic metal powder.
Background technology
It is generally acknowledged, because the employed soft magnetism material of various electromagnetic circuit elements such as magnetic core, electric core, generator magnetic core, solenoid core, ignition coil iron core, reactor core, transformer core, choking-winding iron core or Magnetic Sensor magnetic core requires iron loss little, therefore require the electrical impedance height, coercive force is little.In addition, owing to pursue miniaturization, the replying of height of electromagnetic circuit in recent years, therefore higher magnetic flux density comes into one's own.
As an example of the magnetic core material that is made of this soft magnetism material, known have the insulating barrier that is made of MgO in the coating of the surface of soft magnetic metal plate and the lamination steel plate (with reference to patent documentation 1) of lamination.But, though this lamination steel plate magnetic flux density and electrical impedance are all good, be difficult to make the electromagnetic component of complicated shape.In order to make the electromagnetic component of complicated shape, think just like inferior method: the damp process by chemical plating and coating etc. is at the surface-coated MgO insulation tunicle of soft magnetic metal powder, make the composite soft magnetic metal dust thus, again this composite soft magnetic metal dust extrusion molding and calcining are made; Perhaps soft magnetic metal powder and Mg ferrite powder are mixed together, extrusion molding and calcining, making thus with MgO is the composite soft magnetic material of insulating barrier.
So, as above-mentioned metal soft magnetic powder, general known iron powder, insulation processing iron powder, Fe-Al are arranged is that iron-base soft magnetic alloy powder, Fe-Ni are that iron-base soft magnetic alloy powder, Fe-Cr are that iron-base soft magnetic alloy powder, Fe-Si are that iron-base soft magnetic alloy powder, Fe-Si-Al are that iron-base soft magnetic alloy powder, Fe-Co are that iron-base soft magnetic alloy powder, Fe-Co-V are that iron-base soft magnetic alloy powder or Fe-P are iron-base soft magnetic alloy powder etc.
Patent documentation 1: the spy opens clear 63-226011 communique
In addition, as one of employed soft magnetism material of various electromagnetic circuit elements, propose to have the composite magnetic that is mingled with the high resistivity material between the particle of the iron powder of making.As an example, known have compression molding by iron powder, generation SiO
2Compound and MgO
3Or the mixture of the powder of MgO formation, be made into body, this formed body is remained on 500～1100 ℃, between the particle of iron powder, form thus with SiO
2With MgO be the glassy phase of main component, guarantee the interparticle insulation of iron powder, carry out the method (with reference to patent documentation 1) that compressed-core is made thus.
Patent documentation 1: the spy opens the 2003-217919 communique
Damp process by chemical plating and coating etc. forms MgO insulation tunicle on described soft magnetic metal powder, to make the method for composite soft magnetic metal dust, because cost is high and be difficult to volume production, therefore the method composite soft magnetic metal dust costliness of making in view of the above, and the composite soft magnetic material that uses this expensive composite soft magnetic alloy powder to make has so-called expensive such shortcoming.In addition, its MgO insulation tunicle of the composite soft magnetic metal dust of method making is more stable than soft magnetic metal powder in view of the above, therefore between MgO insulation tunicle and soft magnetic metal powder surface, be difficult to take place diffusion reaction, close property deficiency between formed for this reason MgO insulation tunicle and the soft magnetic metal powder surface, if the composite soft magnetic metal dust that extrusion molding is made by this damp process, then MgO insulation tunicle can not be brought into play sufficient insulation effect because of breaking etc. when extrusion molding, use the composite soft magnetic metal dust of damp process making in view of the above, exist by its composite soft magnetic material that is made to can not get the such shortcoming of sufficient high impedance.
On the other hand, in soft magnetic metal powder, be added with certain Mg ferrite powder of insulating properties, mixed and pushed calcining method, though it is because cheap for manufacturing cost and can improve cheap composite soft magnetic material, but the composite soft magnetic material made of method can have the tissue that MgO concentrates on 3 crystal boundary points of metal soft magnetic grain in view of the above, MgO disperses few equably at crystal boundary, so the ratio that resulting composite soft magnetic material is deposited resists low such shortcoming.
In addition, the described existing composite soft magnetic sintering material that adds the high resistivity material in iron powder sintering and obtain, within its density, rupture strength, resistivity and magnetic flux density, resistivity is especially insufficient, also requires to have the more composite soft magnetic sintering material of high resistivity.
Summary of the invention
Therefore, present inventors study in order to solve this problem, obtain as inferior result of study:
(A), be that 150～1100 ℃, pressure are 1 * 10 in temperature with the mixed-powder that obtains if the soft magnetic metal powder that will carry out oxidation processes, adds the Mg powder as material powder in this material powder mix
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere, again as required in oxidizing atmosphere, temperature heating with 50～400 ℃, then can access and contain Mg oxide-film lining soft magnetic metal powder, it has the oxide isolated tunicle that contains Mg on the soft magnetic metal powder surface, this contains Mg oxide-film lining soft magnetic metal powder and compares with the Mg oxide-film lining soft magnetic metal powder that contains of the existing Mg of being formed with ferrite membrane, close property is especially excellent, even this contains extrusion molding Mg oxide-film lining soft magnetic metal powder and makes the press-powder body, the situation that insulation is peeled off by film destroy also seldom, in addition, calcine the resulting composite soft magnetic material of press-powder body that this contains Mg oxide-film lining soft magnetic metal powder with 400～1300 ℃ temperature, contain the Mg oxide-film and disperse equably, obtain containing the Mg oxide-film and can not concentrate the tissue that disperses at 3 crystal boundary points at crystal boundary;
(B) soft magnetic metal powder that will carry out oxidation processes is as material powder, adds the Mg powder and mix in this material powder, for the mixed-powder that will obtain is that 150～1100 ℃, pressure are 1 * 10 in temperature
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere, heat while preferably rotate described mixed-powder;
(C) as described soft magnetic metal powder, iron powder, insulation processing iron powder, Fe-Al known to can using usually are that iron-base soft magnetic alloy powder, Fe-Ni are that iron-base soft magnetic alloy powder, Fe-Cr are that iron-base soft magnetic alloy powder, Fe-Si are that iron-base soft magnetic alloy powder, Fe-Si-Al are that iron-base soft magnetic alloy powder, Fe-Co are that iron-base soft magnetic alloy powder, Fe-Co-V are that iron-base soft magnetic alloy powder or Fe-P are the iron-base soft magnetic alloy powder.
(D) by in oxidizing atmosphere, soft magnetic powder being remained on room temperature～500 ℃, thereby heating after in the oxide lining soft magnetic powder of the surface of soft magnetic powder formation oxide, adding silicon monoxide powder and mixing, perhaps while mixing in vacuum atmosphere, the condition that remains on 600～1200 ℃ with temperature heats, moreover add the Mg powder and mix the back heating, or remain on 400～800 ℃ condition with temperature and heat while mixing in vacuum atmosphere, then can access be formed with on the surface of soft magnetic powder contain the Mg-Si oxidation film contain Mg-Si oxide lining soft magnetic powder, use the composite soft magnetic sintering material that Mg-Si oxide lining soft magnetic powder is made that contains that method in view of the above makes, compared with existing to by having generated SiO
2Compound and MgO
3Or the mixture that the powder of MgO constituted carries out compression molding and sintering and the composite soft magnetic sintering material that obtains, and its density, rupture strength, resistivity and magnetic flux density are all excellent.
(E) if by in oxidizing atmosphere, soft magnetic powder being remained on room temperature～500 ℃, thereby form the oxide of iron on the surface of soft magnetic powder, in this oxide lining soft magnetic powder, add silicon monoxide powder and Mg powder simultaneously and mix the back heating, perhaps while mixing in vacuum atmosphere, the condition that remains on 400～1200 ℃ with temperature heats, then can access be formed with on the surface of soft magnetic powder contain the Mg-Si oxidation film contain Mg-Si oxide lining soft magnetic powder, use the composite soft magnetic sintering material that Mg-Si oxide lining soft magnetic powder is made that contains that method in view of the above makes, compared with existing to by having generated SiO
2Compound and MgO
3Or the mixture that the powder of MgO constituted carries out compression molding and sintering and the composite soft magnetic sintering material that obtains, and its density, rupture strength, resistivity and magnetic flux density are all excellent.
(F) if by in oxidizing atmosphere, soft magnetic powder being remained on room temperature～500 ℃, thereby form the oxide of iron on the surface of soft magnetic powder, in this oxide lining soft magnetic powder, add the Mg powder and mix the back heating, perhaps while mixing in vacuum atmosphere, the condition that remains on 400～800 ℃ with temperature heats, then can access be formed with on the surface of soft magnetic powder contain the Mg oxidation film contain Mg oxide lining soft magnetic powder, heat after the silicon monoxide powder also mixes as if containing at this to add again in Mg oxide lining soft magnetic powder, or while mixing in vacuum atmosphere, the condition that remains on 600～1200 ℃ with temperature heats, then can access be formed with on the surface of soft magnetic powder contain the Mg-Si oxidation film contain Mg-Si oxide lining soft magnetic powder, use the composite soft magnetic sintering material that Mg-Si oxide lining soft magnetic powder is made that contains that method in view of the above makes, compared with existing to by having generated SiO
2Compound and MgO
3Or the mixture that the powder of MgO constituted carries out compression molding and sintering and the composite soft magnetic sintering material that obtains, and its density, rupture strength, resistivity and magnetic flux density are all excellent.
(G) addition of preferred described silicon monoxide powder is in the scope of 0.01～1 quality %, and the addition of preferred described Mg powder is in the scope of 0.05～1 quality %.
(H) described vacuum atmosphere is preferably, pressure: 1 * 10
-12～1 * 10
-1The vacuum atmosphere of MPa.
The present invention is based on such result of study and carry out,
(1) contains Mg oxide-film lining composite soft magnetic manufacturing method of power, wherein, the soft magnetic metal powder that will carry out oxidation processes is as material powder, and in this material powder, add the Mg powder and mix, be that 150～1100 ℃, pressure are 1 * 10 with the mixed-powder that obtains in temperature
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere,
(2) contain the manufacture method of Mg oxide-film lining soft magnetic powder, wherein, again in oxidizing atmosphere,, the Mg oxide-film lining soft magnetic powder that contains according to the method manufacturing of described (1) record heated with 50～400 ℃ temperature,
(3) contain Mg oxide-film lining composite soft magnetic manufacturing method of power, wherein, the oxidation processes of the soft magnetic metal powder of described (1) record is in oxidizing atmosphere, carries out heat treated with 50～500 ℃ temperature,
(4) a kind ofly contain Mg oxide-film lining soft magnetic metal powder production of raw material for use powder with what soft magnetic metal powder carried out that oxidation processes forms,
(5) containing Mg oxide-film lining composite soft magnetic manufacturing method of power, wherein, add the Mg powder and mixed in soft magnetic metal powder, is that 150～1100 ℃, pressure are 1 * 10 with the mixed-powder that obtains thus in temperature
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere, then in oxidizing atmosphere, implement oxidation processes with 50～400 ℃ temperature heating,
(6) contain the manufacture method of Mg-Si oxide lining soft magnetic powder, wherein, in the surface of soft magnetic powder is formed with the oxide lining soft magnetic powder of oxide-film of iron, add the silicon monoxide powder and is mixed the back and heat, perhaps while mixing in vacuum atmosphere, the condition that remains on 600～1200 ℃ with temperature heats, add the Mg powder again and mix the back heating, or while mixing in vacuum atmosphere, the condition that remains on 400～800 ℃ with temperature heats.
(7) contain the manufacture method of Mg-Si oxide lining soft magnetic powder, wherein, in the surface of soft magnetic powder is formed with the oxide lining soft magnetic powder of oxide-film of iron, add silicon monoxide powder and MgO powder and is mixed the back and heat, perhaps while mixing in vacuum atmosphere, the condition that remains on 400～1200 ℃ with temperature heats
(8) contain the manufacture method of Mg-Si oxide lining soft magnetic powder, wherein, in the surface of soft magnetic powder is formed with the oxide lining soft magnetic powder of oxide-film of iron, add the Mg powder and is mixed the back and heat, perhaps while mixing in vacuum atmosphere, the condition that remains on 400～800 ℃ with temperature heats, and adds the silicon monoxide powder again and mixes the back heating, while perhaps mix in vacuum atmosphere, the condition that remains on 600～1200 ℃ with temperature heats
(9) manufacture method that contains Mg-Si oxide lining soft magnetic powder of described (6), (7) or (8) record, wherein, be formed with the making of oxide lining soft magnetic powder of the oxide-film of iron on the surface of described soft magnetic powder, be by soft magnetic powder being heated in oxidizing atmosphere and remaining in room temperature～500 ℃
(10) manufacture method that contains Mg-Si oxide lining soft magnetic powder of described (6), (7), (8) or (9) record, wherein, the addition of described silicon monoxide powder is in the scope of 0.01～1 quality %, and the addition of described Mg powder is in the scope of 0.05～1 quality %
(11) manufacture method that contains Mg-Si oxide lining soft magnetic powder of described (6), (7), (8), (9) or (10) record, wherein, described vacuum atmosphere is a pressure: 1 * 10
-12～1 * 10
-1The vacuum atmosphere of MPa.
Because silicon monoxide (SiO) powder also is the highest oxide of vapour pressure within silica, therefore through heating the surperficial evaporation silica composition that makes soft magnetic powder easily, even the silica (SiO that mixed vapour forces down
2) powder heats, and also can't form the silicon oxide film of abundant thickness on the surface of soft magnetic powder, so be not preferred.If after in oxide lining soft magnetic powder, adding silicon monoxide (SiO) powder and being mixed, while perhaps mix in vacuum atmosphere temperature is remained on 600～1200 ℃, thereby the surface that is created on soft magnetic powder is formed with SiO
XThe silicon oxide film lining soft magnetic powder of (wherein x=1～2) film, in this silicon oxide film lining soft magnetic powder, add the Mg powder again, heat while mixing in vacuum atmosphere, then can access and contain Mg-Si oxide lining soft magnetic powder, it is to be coated with by what Mg-Si-Fe-O constituted to contain the Mg-Si oxidation film on soft magnetic powder.
Oxide lining soft magnetic powder, it can be by remaining on soft magnetic powder in (for example in the atmosphere) in the oxidizing atmosphere, and temperature remains on room temperature～500 ℃, makes thereby form ferroelectric oxide film on the surface of soft magnetic powder.And this ferroelectric oxide film has the lining raising effect that makes SiO and/or Mg.When making oxide lining soft magnetic powder, if heating surpasses 500 ℃ in oxidizing atmosphere, then soft magnetic powder aggegation generates the aggregate of soft magnetic powder, through sintering can not homogeneous surface oxidation, so be not preferred.Therefore, oxide lining soft magnetic powder heating-up temperature during fabrication is due to room temperature～500 ℃.Preferred scope is room temperature～300 ℃.Oxidizing atmosphere has more preferably been carried out dry oxidizing atmosphere.
In the manufacture method that contains Mg-Si oxide lining soft magnetic powder of the present invention, why the SiO amount of powder of adding in the oxide lining soft magnetic powder is defined as 0.01～1 quality %, be because the addition of SiO powder when being lower than 0.01 quality %, the thickness deficiency of the surperficial formed silicon oxide film of oxide lining soft magnetic powder, so contain the quantity not sufficient of the contained Si of Mg-Si oxidation film, therefore can not get resistivity high contain the Mg-Si oxidation film and for preferred, on the other hand, surpass 1 quality %, then formed SiO if add
XThe thickness of (wherein x=1～2) silicon oxide film becomes blocked up, and the density that contains the composite soft magnetic material that Mg-Si oxide lining soft magnetic powder obtains through the press-powder calcining that obtains is reduced, and is not preferred therefore.
In addition, in the manufacture method that contains Mg-Si oxide lining soft magnetic powder of the present invention, why the addition of Mg powder is defined as 0.05～1 quality %, be because the addition of Mg powder when being lower than 0.05 quality %, thickness deficiency at the surperficial formed Mg film of oxide lining soft magnetic powder, the quantity not sufficient that contains the contained Mg of Mg-Si oxidation film, therefore can not get the Mg-Si oxidation film of abundant thickness, so be not preferred, on the other hand, surpass 1 quality % if add, the thickness that then forms the Mg film becomes blocked up, the density that contains the composite soft magnetic material that Mg-Si oxide lining soft magnetic powder obtains through the press-powder calcining that obtains is reduced, and is not preferred therefore.
In the manufacture method that contains Mg-Si oxide lining soft magnetic powder of the present invention, in oxide lining soft magnetic powder, add the SiO powder, the mixed-powder of Mg powder or SiO powder and Mg powder and the condition of being mixed, why be in 600～1200 ℃ vacuum atmosphere as temperature, be because to be lower than 600 ℃ of heating, because the vapour pressure of SiO is little, so can not get fully thick SiO film or contain Mg-Si oxide tunicle, on the other hand, if surpassing 1200 ℃ mixes, then can make the soft magnetic powder sintering, what can not get expecting contains Mg-Si oxide lining soft magnetic powder, is not preferred therefore.In addition, heating atmosphere at this moment is 1 * 10 at pressure preferably
-12～1 * 10
-1In the vacuum atmosphere of MPa, heat while further preferably rotate in addition.
The soft magnetic powder that uses when making oxide lining soft magnetic powder preferably uses average grain diameter to be in the interior soft magnetic powder of scope of 5～500 μ m.Its reason is, if average grain diameter is also littler than 5 μ m, then the compressibility of powder reduces, the volume ratio step-down of soft magnetic powder so the value of magnetic flux density reduces, is not preferred therefore, on the other hand, if average grain diameter is also bigger than 500 μ m, then the vortex flow of soft magnetic powder inside increases, and the permeability under the high frequency reduces.
As described above, in the manufacturing that contains Mg-Si oxide lining soft magnetic powder of the present invention, the oxide lining soft magnetic powder that the surface of soft magnetic powder need be formed with the oxide-film of iron uses as material powder.Therefore, the present invention
(12) be that soft magnetic powder constituted contains Mg-Si oxide lining soft magnetic powder production of raw material for use powder for the oxide lining of a kind of surface at soft magnetic powder oxide-film of being formed with iron.
(13) be the manufacture method that contains Mg oxide-film lining soft magnetic metal powder, wherein, heat, so carry out described (1), (5), (7), the vacuum of (8) or (9) record or the heating in the inert gas atmosphere while rotate,
The material powder that uses in the manufacture method of the Mg of containing oxide-film lining soft magnetic metal powder of the present invention, what use is the soft magnetic metal powder that has carried out oxidation processes, and the present invention uses the soft magnetic metal powder that this has carried out oxidation processes as containing Mg oxide-film lining soft magnetic metal powder production of raw material for use powder.Therefore, the present invention
(14) be described (6) record contain Mg oxide-film lining soft magnetic metal powder production of raw material for use powder, wherein, described soft magnetic metal powder is that iron powder, insulation processing iron powder, Fe-Al are that iron-base soft magnetic alloy powder, Fe-Ni are that iron-base soft magnetic alloy powder, Fe-Cr are that iron-base soft magnetic alloy powder, Fe-Si are that iron-base soft magnetic alloy powder, Fe-Si-Al are that iron-base soft magnetic alloy powder, Fe-Co are that iron-base soft magnetic alloy powder, Fe-Co-V are that iron-base soft magnetic alloy powder or Fe-P are the iron-base soft magnetic alloy powder.
(15) be the manufacture method of material powder as the soft magnetic metal powder that has carried out oxidation processes, wherein, Fe-Si be add the Si powder in iron-base soft magnetic alloy powder or the Fe powder and mix after, by in nonoxidizing atmosphere, heating, the Fe-Si that the surface that is produced on described Fe-Si in advance and is iron-base soft magnetic alloy powder or Fe powder has high concentration Si diffusion layer is the iron-base soft magnetic alloy powder, the described Fe-Si of concentration ratio of the Si that this high concentration Si diffusion layer contains is the concentration height of the contained Si of iron-base soft magnetic alloy powder or Fe powder, with the Fe-Si with high concentration Si diffusion layer that obtains is that the iron-base soft magnetic alloy powder carries out oxidation processes, and becoming the surface oxidation high concentration Fe-Si that has oxide layer on high concentration Si diffusion layer thus is the iron-base soft magnetic alloy powder.
Use contains Mg oxide-film lining soft magnetic metal powder according to the method manufacturing of described (1), (5), (7), (8) or (9) record, just can produce the composite soft magnetic material of resistivity and mechanical strength excellence according to usual way.Therefore, the present invention
(16) be the manufacture method of the composite soft magnetic material of resistivity and mechanical strength excellence, wherein, will according to the method manufacturing of described (1), (5), (7), (8) or (9) record contain Mg oxide-film lining soft magnetic metal powder extrusion molding after, with 400～1300 ℃ temperature calcining
(17) be the manufacture method of the composite soft magnetic material of resistivity and mechanical strength excellence, wherein, in containing in the Mg oxide-film lining soft magnetic metal powder of the method manufacturing of putting down in writing according to described (1), (5), (7), (8) or (9), the composite material that mixes organic insulation, inorganic insulating material or organic insulation and inorganic insulating material carries out press-powder afterwards and is shaped, with 500～1000 ℃ of calcinings.
In the manufacture method that contains Mg oxide-film lining soft magnetic metal powder of the present invention, in order in the soft magnetic metal powder that has carried out oxidation processes, to add the Mg powder and to mix, preferably in the soft magnetic metal powder that has carried out oxidation processes, add the Mg powder of 0.05～2 quality % and make mixed-powder to make mixed-powder.This be because, with respect to the soft magnetic metal powder that has carried out oxidation processes, when the addition of Mg powder was lower than 0.05 quality %, the amount of formed Mg tunicle was insufficient, therefore, can not get the fully thick Mg oxide-film that contains, on the other hand, surpass 2 quality % if add, then the thickness of Mg tunicle becomes blocked up, the thickness that contains the Mg oxide-film becomes blocked up, and this contains Mg oxide-film lining soft magnetic metal powder and the magnetic flux density of the composite soft magnetic material that obtains reduces to make calcining, is not preferred therefore.
The oxidation processes of soft magnetic metal powder has the effect of the lining raising that makes Mg, and its mode of carrying out is in oxidizing atmosphere, remains in 50～500 ℃ temperature, perhaps remains in 50～100 ℃ temperature in distilled water or pure water.Under this situation, it all is inefficent being lower than 50 ℃, on the other hand, if the maintenance above 500 ℃ in oxidizing atmosphere is then calcined, is not preferred therefore.Oxidizing atmosphere has more preferably been carried out dry oxidizing atmosphere.
The ideograph of the pairing variations in temperature of time when showing the oxidation processes soft magnetic metal powder is illustrated among Fig. 1.Common pattern shown in Fig. 1 (a), by heating in oxidizing atmosphere, oxidation processes is carried out, but shown in Fig. 1 (b), can be also with after being warming up to low temperature and keeping, the pattern that is warming up to high temperature again and keeps is carried out, in addition as Fig. 1 (c) shown in, and can be to be warming up to after high temperature and the maintenance, the pattern that is cooled to low temperature again and keeps is carried out, pattern shown in Fig. 1 (d) also can be with along with heating up and cooling, and the pattern that is not kept is in fact carried out.In addition, in distilled water or pure water, the temperature of Fig. 1 (a)～(d) is made as 100 ℃ of the upper limits, following 50 ℃ of limits, can carries out with same pattern.In the manufacture method that contains Mg oxide-film lining soft magnetic metal powder of the present invention, the pattern of the pairing variations in temperature of time during expression oxidation processes soft magnetic metal powder is not limited to Fig. 1, but can freely change in 50～500 ℃ scope.
In the soft magnetic metal powder that has carried out oxidation processes, add the Mg powder and mix and obtain be mixed into powder, be 150～1100 ℃ with it in temperature, pressure is 1 * 10
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere, while or rotate and heat.At this, heating atmosphere is why as pressure: 1 * 10
-12～1 * 10
-1The inert gas atmosphere of MPa or vacuum atmosphere are owing to be 1 * 10 as pressure
-12～1 * 10
-1The inert gas atmosphere of MPa comprises so-called high vacuum atmosphere.
In addition, the reason that makes heating-up temperature be in 150～1100 ℃ be because, need make pressure be lower than 1 * 10 when temperature is lower than 150 ℃
-12MPa industrially is difficulty or does not have effect that on the other hand, if temperature surpasses 1100 ℃, then the loss of Mg is many, therefore be preferred, in addition if pressure above 1 * 10
-1MPa, then the lining efficient of Mg tunicle reduces, and therefore the uneven thickness one of formed in addition Mg tunicle is not preferred.The preferred scope of the heating-up temperature of the mixed-powder of soft magnetic metal powder and Mg powder is 300～900 ℃, and the preferred scope of atmosphere pressures is 1 * 10
-10～1 * 10
-2MPa.
Demonstration is heated the soft magnetic metal powder that has carried out oxidation processes, is illustrated among Fig. 2 while perhaps rotate the ideograph of the pairing variations in temperature of time when it is heated.Common pattern as Fig. 2 (a), be to be undertaken by remaining on to heat under the steady temperature, but also can shown in Fig. 2 (b), make it like that to change, in addition as the pattern of Fig. 2 (c), can be with after being warming up to low temperature and keeping, be warming up to high temperature again and the pattern that keeps is carried out, in addition the pattern shown in Fig. 1 (d), also can be with after being warming up to high temperature and keeping, be cooled to low temperature again and the pattern that keeps is carried out.Pattern shown in Fig. 1 (e) also can repeat the pattern of Fig. 1 (a) for several times in addition.In addition, the pattern shown in Fig. 1 (f) also can be to remain on low temperature in the way after remaining in high temperature, remains in the pattern of high temperature again.
In the manufacture method that contains Mg oxide-film lining soft magnetic metal powder of the present invention, expression is heated the soft magnetic metal powder that has carried out oxidation processes or is not limited to Fig. 2 while the pattern of rotating the pairing variations in temperature of time when heating, but can freely change in 150～1100 ℃ scope.
In addition, as with above-mentioned different embodiment, if in soft magnetic metal powder, add the Mg powder and mix and obtain be mixed into powder, be 150～1100 ℃ with it in temperature, pressure is 1 * 10
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere, or while rotate heat after, the oxidation processes that heats with 50～400 ℃ temperature is implemented in continuation in oxidizing atmosphere, then contain the Mg oxide-film, can produce the Mg of containing oxide-film lining soft magnetic metal powder of the present invention in the formation of the surface of soft magnetic metal powder.At this moment heating-up temperature be lower than 50 ℃ then inefficent, if in oxidizing atmosphere, remain on and surpass 400 ℃, then can cause calcining on the other hand, be not preferred therefore.Oxidizing atmosphere has more preferably been carried out dry oxidizing atmosphere.
The ideograph of the pairing variations in temperature of time when described oxidation processes is implemented in expression is illustrated in Fig. 3.Common pattern shown in Fig. 3 (a), can carry out the heating in the oxidizing atmosphere, but also can be shown in Fig. 3 (b) like that with after being warming up to low temperature and keeping, the pattern that is warming up to high temperature again and keeps is carried out, and the pattern as Fig. 3 (c) shown in addition also can be to be warming up to after high temperature and the maintenance, the pattern that is cooled to low temperature again and keeps is carried out, pattern that also can be shown in Fig. 3 (d), with along with heating up and cooling, and the pattern that is not kept is in fact carried out.The pattern of the pairing variations in temperature of time when described oxidation processes is implemented in expression is not limited to Fig. 3, but can freely change in 50～400 ℃ scope.
If carried out the soft magnetic metal powder of oxidation processes and the mixed-powder of Mg powder while rotating to heat with such condition, then can form the oxide-film that contains Mg on the surface of soft magnetic metal powder, contain Mg oxide-film lining soft magnetic metal powder thereby form, but have the inadequate situation of oxidation of Mg.For fear of this situation, the described Mg of the containing oxide-film lining soft magnetic metal powder that further preferably rotation is obtained carries out heat treated with 50～400 ℃ temperature in oxidizing atmosphere, this temperature is preferably more than 50 ℃, but if heating surpasses 400 ℃, then beginning sintering, is not preferred therefore.Therefore this temperature is decided to be 50～400 ℃.
The soft magnetic metal powder that in the manufacture method that contains Mg oxide-film lining soft magnetic metal powder of the present invention, uses as material powder, the always general known iron powder that has, the insulation processing iron powder, Fe-Al is the iron-base soft magnetic alloy powder, Fe-Ni is the iron-base soft magnetic alloy powder, Fe-Cr is the iron-base soft magnetic alloy powder, Fe-Si is the iron-base soft magnetic alloy powder, Fe-Si-Al is the iron-base soft magnetic alloy powder, Fe-Co is the iron-base soft magnetic alloy powder, Fe-Co-V is that iron-base soft magnetic alloy powder or Fe-P are the iron-base soft magnetic alloy powder, more particularly, iron powder is a pure iron powder, the insulation processing iron powder is a phosphate lining iron powder, the wet type solution that perhaps adds collosol and gel (silicate silicate) solution of silicon or the sol gel solution of aluminium oxide etc. is also mixed, be coated on after the iron powder surface, carry out the silica or the aluminium oxide lining iron powder of drying and calcining.
Fe-Al is that the iron-base soft magnetic alloy powder preferably contains Al:0.1～20%, and the Fe-Al that surplus is made of Fe and unavoidable impurities is iron-base soft magnetic alloy powder (for example, having this ア Le パ one system powder formed that is made of Fe-15%Al),
Fe-Ni is that the iron-base soft magnetic alloy powder preferably contains Ni:35～85%, contain below the Mo:5% as required, below the Cu:5%, below the Cr:2%, within Mn:0.5% is following more than a kind or 2 kinds, the Ni-based soft magnetic alloy powder that surplus is made of Fe and unavoidable impurities (for example Fe-49%Ni powder), Fe-Cr is that the iron-base soft magnetic alloy powder preferably contains Cr:1～20%, contain below the Al:5% as required, within Ni:5% is following 1 or 2 kind, the Fe-Cr that surplus is made of Fe and evitable impurity is the iron-base soft magnetic alloy powder
Fe-Si is that the iron-base soft magnetic alloy powder preferably contains Si:0.1～10%, and the Fe-Si that surplus is made of Fe and evitable impurity is the iron-base soft magnetic alloy powder,
Fe-Si-Al is that the iron-base soft magnetic alloy powder preferably contains Si:0.1～10%, Al:0.1～20%, and the Fe-Si-Al that surplus is made of Fe and evitable impurity is the iron-base soft magnetic alloy powder,
Fe-Co-V is that the iron-base soft magnetic alloy powder preferably contains Co:0.1～52%, V:0.1～3%, and the Fe-Co-V that surplus is made of Fe and evitable impurity is the iron-base soft magnetic alloy powder,
Fe-Co is that the iron-base soft magnetic alloy powder preferably contains Co:0.1～52%, and the Fe-Co that surplus is made of Fe and evitable impurity is the iron-base soft magnetic alloy powder,
Fe-P is that the iron-base soft magnetic alloy powder preferably contains P:0.5～1%, and the Fe-P that surplus is made of Fe and evitable impurity is iron-base soft magnetic alloy powder (above % represents quality %).
And what these soft magnetic metal powders preferably used is the interior soft magnetic metal powder of scope that average grain diameter is in 5～500 μ m.Its reason is, if average grain diameter is also littler than 5 μ m, then the compressibility of powder reduces, the volume ratio step-down of soft magnetic powder so the value of magnetic flux density reduces, is not preferred therefore, on the other hand, if average grain diameter is also bigger than 500 μ m, then the vortex flow of soft magnetic powder inside increases, and the permeability under the high frequency reduces.
In order to use the Mg oxide-film lining soft magnetic metal powder of making according to method of the present invention that contains to carry out the manufacturing of composite soft magnetic material, the Mg oxide-film lining soft magnetic metal powder that contains that the method according to this invention can be made is shaped by the usual way press-powder and carries out sintering and make, but, its making also can be carried out by the following method: containing average grain diameter is the following silica of 0.5 μ m, 1 kind or 2 kind of 0.05～1 quality % among the aluminium oxide, the Mg oxide-film lining soft magnetic metal powder that contains that remainder is made by the method according to this invention constitutes, allocate the mixed mixed-powder that makes in this way, this mixed-powder is shaped with the usual way press-powder, and carries out sintering.
The folding method is made according to the present invention contains Mg oxide-film lining soft magnetic metal powder, be formed with on its surface and contain the Mg oxide-film, this contains Mg oxide-film and silica and aluminium oxide reaction and forms composite oxides, thereby obtain being mingled with the composite soft magnetic material that high resistivity is arranged of composite oxides with high impedance at the crystal boundary of soft magnetic powder, simultaneously because be mingled with silica and alumina sintering, so composite soft magnetic material that can the manufacturing machine excellent strength.At this moment, because silica and aluminium oxide become main body and be sintered,, therefore can make the few composite soft magnetic material of magnetic hysteresis loss so can guarantee that coercive force is little, described calcining preferably in inert gas atmosphere or oxidizing gas atmosphere, is carried out with 400～1300 ℃ temperature.
In addition, carry out drying after the wet type solution of collosol and gel (silicate) solution of interpolation silicon and the sol gel solution of aluminium oxide etc. is also mixed in the Mg of containing oxide-film lining iron powder of the present invention, with this drying the mixture compression molding after, in inert gas atmosphere or oxidizing gas atmosphere, with 400～1300 ℃ temperature calcining, can make the composite soft magnetic material thus.
In addition, in containing in the Mg oxide-film lining soft magnetic metal powder that the method according to this invention is made, mix organic insulation and inorganic insulating material, perhaps the composite material of organic insulation and inorganic insulating material can be made the composite soft magnetic material that resistivity and intensity further improve.Under this situation, organic insulation can adopt following material: epoxy resin, fluororesin, phenolic resins, polyurethane resin, silicones, alkyd resin, phenoxy resin, Lauxite, isocyanate resin, allyl resin, polyimide resin, PPS resin etc.In addition, inorganic insulating material can adopt following material: the phosphate of ferric phosphate etc., various glassy insulant, be waterglass, insulating properties oxide of principal component etc. with the sodium metasilicate.
In addition, in containing in the Mg oxide-film lining soft magnetic metal powder that the method according to this invention is made, within allotment boron oxide, vanadium oxide, bismuth oxide, antimony oxide and the molybdenum oxide more than a kind or 2 kinds, with B
2O
3, V
2O
5, Bi
2O
3, Sb
2O
3, MoO
3Be scaled 0.05～1 quality %, carry out press-powder after being mixed and be shaped,, can make the composite soft magnetic material thus the press-powder formed body that obtains temperature sintering with 500～1000 ℃.So the composite soft magnetic material of making has following composition: contain within boron oxide, vanadium oxide, bismuth oxide, antimony oxide and the molybdenum oxide more than a kind or 2 kinds, with B
2O
3, V
2O
5, Bi
2O
3, Sb
2O
3, MoO
3Be scaled 0.05～1 quality %, remainder is to be made of the Mg oxide-film lining soft magnetic metal powder that contains that the method according to this invention is made.Under this situation, what form on the surface that contains Mg oxide-film lining soft magnetic metal powder that the method according to this invention is made contains the Mg oxide-film, and the reaction more than a kind or 2 kinds with within boron oxide, vanadium oxide, bismuth oxide, antimony oxide and the molybdenum oxide forms epithelium.
In addition, this composite soft magnetic material can obtain by the following method: within the sol solution of the sol solution of the sol solution of the sol solution of the sol solution of boron oxide or powder, vanadium oxide or powder, bismuth oxide or powder, antimony oxide or powder and molybdenum oxide or the powder more than a kind or 2 kinds, with B
2O
3, V
2O
5, Bi
2O
3, Sb
2O
3, MoO
3Be scaled 0.05～1 quality %, surplus is made of the described Mg of containing oxide-film lining iron powder of the present invention, allocate, mix in the mode that becomes this composition, after the mixed oxide that obtains is carried out press-powder, is shaped, with 500～1000 ℃ temperature sintering.
The composite soft magnetic material that uses the Mg of containing oxide-film lining soft magnetic metal powder of the present invention to make has high density, high strength, high resistivity and high magnetic flux density, this composite soft magnetic material has the feature of high magnetic flux density, the low iron loss of high frequency, can use as the material of the various electromagnetic circuit elements that produce this feature thus.
In addition, make the composite soft magnetic material in order to use the Mg-Si oxide-film lining soft magnetic powder of making according to method of the present invention that contains, can contain Mg-Si oxide-film lining soft magnetic powder by after the usual way compression molding by what the method according to this invention was made, in inert gas atmosphere or oxidizing gas atmosphere, with 400～1300 ℃ temperature calcining.
In addition, in containing in the Mg-Si oxide-film lining soft magnetic powder that the method according to this invention is made, mix organic insulation and inorganic insulating material, perhaps the composite material of organic insulation and inorganic insulating material can be made the composite soft magnetic material that resistivity and intensity further improve.Under this situation, organic insulation can adopt following material: epoxy resin, fluororesin, phenolic resins, polyurethane resin, silicones, alkyd resin, phenoxy resin, Lauxite, isocyanate resin, allyl resin, polyimide resin, PPS resin etc.In addition, inorganic insulating material can adopt following material: the phosphate of ferric phosphate etc., various glassy insulant, be waterglass, insulating properties oxide of principal component etc. with the sodium metasilicate.
In addition, in containing in the Mg-Si oxide-film lining soft magnetic metal powder that the method according to this invention is made, within allotment boron oxide, vanadium oxide, bismuth oxide, antimony oxide and the molybdenum oxide more than a kind or 2 kinds, with B
2O
3, V
2O
5, Bi
2O
3, Sb
2O
3, MoO
3Be scaled 0.05～1 quality %, carry out press-powder after being mixed and be shaped,, can make the composite soft magnetic material thus the press-powder formed body that obtains temperature sintering with 500～1000 ℃.So the composite soft magnetic material of making has following composition: contain within boron oxide, vanadium oxide, bismuth oxide, antimony oxide and the molybdenum oxide more than a kind or 2 kinds, with B
2O
3, V
2O
5, Bi
2O
3, Sb
2O
3, MoO
3Be scaled 0.05～1 quality %, remainder is to be made of the Mg oxide-film lining soft magnetic metal powder that contains that the method according to this invention is made.Under this situation, what form on the surface that contains Mg oxide-film lining soft magnetic metal powder that the method according to this invention is made contains the Mg oxide-film, and the reaction more than a kind or 2 kinds with within boron oxide, vanadium oxide, bismuth oxide, antimony oxide and the molybdenum oxide forms epithelium.
In addition, this composite soft magnetic material can obtain by the following method: within the sol solution of the sol solution of the sol solution of the sol solution of the sol solution of boron oxide or powder, vanadium oxide or powder, bismuth oxide or powder, antimony oxide or powder and molybdenum oxide or the powder more than a kind or 2 kinds, with B
2O
3, V
2O
5, Bi
2O
3, Sb
2O
3, MoO
3Be scaled 0.05～1 quality %, surplus is made of the described Mg of containing oxide-film lining iron powder of the present invention, allocate, mix in the mode that becomes this composition, after the mixed oxide that obtains is carried out press-powder, is shaped, with 500～1000 ℃ temperature sintering.
In addition, at the wet type solution that adds collosol and gel (silicate) solution of silicon and the sol gel solution of aluminium oxide etc. in the Mg-Si oxide-film lining soft magnetic powder that contains of the present invention, and carry out drying after being mixed, with this drying the mixture compression molding after, in inert gas atmosphere or oxidizing gas atmosphere, with 500～1000 ℃ temperature calcining, can make the composite soft magnetic material thus.
The composite soft magnetic material that uses the Mg-Si of containing oxide-film lining soft magnetic powder of the present invention to make has high density, high strength, high resistivity and high magnetic flux density, this composite soft magnetic material has the feature of high magnetic flux density, the low iron loss of high frequency, can use as the material of the various electromagnetic circuit elements that produce this feature thus.
Description of drawings
The ideograph of the pairing variations in temperature of time when Fig. 1 is expression oxidation processes soft magnetic metal powder.
Fig. 2 shows the soft magnetic metal powder that has carried out oxidation processes heated, while perhaps rotate the ideograph of the pairing variations in temperature of time when it is heated.
Fig. 3 is expression heating or while the ideograph that rotates the pairing variations in temperature of time when carrying out oxidation processes after heating.
The specific embodiment
As soft magnetic metal powder, prepare all to have the pure iron powder that average grain diameter is 70 μ m (is soft magnetic powder A to call this pure iron powder in the following text),
Preparing Al is that efflorescence (atomize) Fe-Al that 10 quality %, surplus are made of Fe is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder B to call this Fe-Al in the following text),
Preparing Ni is that the efflorescence Fe-Ni that 49 quality %, surplus are made of Fe is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder C to call this Fe-Ni in the following text),
Preparing Cr is that the efflorescence Fe-Cr that 10 quality %, surplus are made of Fe is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder D to call this Fe-Cr in the following text),
Preparing Si is that 3 quality %, surplus Fe are iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder E to call this efflorescence Fe-Si in the following text) by the efflorescence Fe-Si that constitutes,
It is that 3 quality %, Al are that the efflorescence Fe-Si-Al that 3 quality %, surplus are made of Fe is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder F to call this Fe-Si-Al in the following text) that preparation contains Si,
The Fe-Co-V that preparation contains that Co is 30%, V is 2%, surplus is made of Fe and unavoidable impurities is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder G to call this Fe-Co-V in the following text),
It is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder H to call this Fe-P in the following text) that preparation contains the Fe-P that P is 0.6%, surplus is made of Fe and unavoidable impurities,
As the insulation processing iron powder, prepare the phosphate lining iron powder (is soft magnetic powder I to call this phosphate lining iron powder in the following text) of market sale,
It is iron-base soft magnetic alloy powder (is that the iron-base soft magnetic alloy powder is soft magnetic powder J to call this Fe-Co in the following text) that preparation contains the Fe-Co that Co is 30%, surplus is made of Fe and unavoidable impurities.
In addition, the preparation average grain diameter is that Mg powder and the average grain diameter of 30 μ m are the Mg ferrite powder of 3 μ m.
Embodiment 1
In the allotment ratio shown in the table 1, for soft magnetic powder A (pure iron powder) the allotment Mg powder of having implemented the oxidation processes under the condition shown in the table 1, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 1 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 1, making is implemented the inventive method 1～7 and comparative approach 1～3 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 1～7 and comparative approach 1～3 constitutes, its result is presented in the table 1, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results show at table 1.
(conventional example 1)
In the allotment ratio shown in the table 1, for the soft magnetic powder A allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 1, making is implemented existing method 1 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 1 of mensuration obtains constitutes, its result is presented in the table 1, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 1.
[table 1]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | Form the condition that contains the Mg oxide-film by rotating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 1 | A | 200 ℃ in atmosphere | Mg：0.2 | Vacuum | 150 | 1×10 -12 | 500 | 98.2 | 170 | 1.65 | 65 |
| 2 | 300 | 1×10 -8 | 500 | 98.4 | 180 | 1.68 | 120 | |||||
| 3 | Argon | 400 | 1×10 -6 | 500 | 98.5 | 190 | 1.69 | 150 | ||||
| 4 | 500 | 1×10 -5 | 500 | 98.5 | 195 | 1.69 | 160 | |||||
| 5 | 700 | 1×10 -2 | 500 | 98.5 | 180 | 1.68 | 150 | |||||
| 6 | 900 | 1×10 -1 | 500 | 98.4 | 170 | 1.67 | 130 | |||||
| 7 | 1100 | 1×10 -1 | 500 | 98.3 | 170 | 1.66 | 105 | |||||
| Comparison method | 1 | Vacuum | 120 * | 1×10 -12 | 500 | 98.3 | 150 | 1.66 | 8 | |||
| 2 | Argon | 1150 * | 1×10 -1 | 500 | 98.3 | 165 | 1.66 | 12 | ||||
| 3 | 1100 | 1×10 0* | 500 | 98.4 | 80 | 1.66 | 1 | |||||
| Existing method 1 | - | Mg ferrite: 0.33 | - | - | - | 500 | 97.9 | 25 | 1.60 | 0.2 | ||
*Value outside the expression scope of the invention.
(embodiment 1 other embodiment)
With with the embodiment 1 shown in the table 2 be the mode of same allotment ratio, for material powder A (pure iron powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 2 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 2 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 1 '～7 ' and comparative approach 1 '～3 ' and existing method 1 ' is presented in the table 2.
[table 2]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 1′ | A | Mg：0.2 | Vacuum | 150 | 1×10 -12 | 200 ℃ in atmosphere | 500 | 98.3 | 175 | 1.65 | 65 |
| 2′ | 300 | 1×10 -8 | 500 | 98.4 | 180 | 1.68 | 125 | |||||
| 3′ | Argon | 400 | 1×10 -6 | 500 | 98.5 | 185 | 1.69 | 155 | ||||
| 4′ | 500 | 1×10 -5 | 500 | 98.5 | 195 | 1.69 | 165 | |||||
| 5′ | 700 | 1×10 -2 | 500 | 98.5 | 175 | 1.69 | 150 | |||||
| 6′ | 900 | 1×10 -1 | 500 | 98.4 | 170 | 1.67 | 135 | |||||
| 7′ | 1100 | 1×10 -1 | 500 | 98.3 | 165 | 1.66 | 110 | |||||
| Comparison method | 1′ | Vacuum | 120 * | 1×10 -12 | 500 | 98.3 | 150 | 1.66 | 8 | |||
| 2′ | Argon | 1150 * | 1×10 -1 | 500 | 98.3 | 165 | 1.66 | 13 | ||||
| 3′ | 1100 | 1×10 0* | 500 | 98.4 | 85 | 1.66 | 1 | |||||
| Existing method 1 ' | Mg ferrite: 0.33 | - | - | - | - | 500 | 97.9 | 25 | 1.60 | 0.2 | ||
*Value outside the expression scope of the invention.
By the result shown in table 1 and the table 2 as can be known, composite soft magnetic material according to the inventive method 1～7 and the inventive method 1 '～7 ' making, compare with the composite soft magnetic material that existing method 1 of basis and present method 1 ' are made, rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 1～3 and comparative approach 1 '～3 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 2
In the allotment ratio shown in the table 3, for the soft magnetic powder B that has implemented the oxidation processes under the condition shown in the table 3 (Fe-Al is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 3 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 3, making is implemented the inventive method 8～14 and comparative approach 4～6 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 8～14 and comparative approach 4～6 constitutes, its result is presented in the table 3, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results show at table 3.
(conventional example 2)
In the allotment ratio shown in the table 3, for the soft magnetic powder B allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 3, making is implemented existing method 2 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 2 of mensuration obtains constitutes, its result is presented in the table 3, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 3.
[table 3]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 8 | B | O 2：5 ％， N 2：95 ％ 500 ℃ | Mg：0.1 | Vacuum | 150 | 1×10 -12 | 800 | 98.3 | 180 | 1.53 | 70 |
| 9 | 300 | 1×10 -8 | 800 | 98.4 | 190 | 1.55 | 140 | |||||
| 10 | Argon | 400 | 1×10 -6 | 800 | 98.5 | 205 | 1.55 | 180 | ||||
| 11 | 500 | 1×10 -5 | 800 | 98.6 | 220 | 1.56 | 200 | |||||
| 12 | 700 | 1×10 -2 | 800 | 98.5 | 210 | 1.55 | 215 | |||||
| 13 | 900 | 1×10 -1 | 800 | 98.3 | 210 | 1.55 | 210 | |||||
| 14 | 1100 | 1×10 -1 | 800 | 98.3 | 200 | 1.53 | 100 | |||||
| Comparison method | 4 | Vacuum | 120 * | 1×10 -12 | 800 | 98.3 | 170 | 1.51 | 9 | |||
| 5 | Argon | 1150 * | 1×10 -1 | 800 | 98.2 | 185 | 1.52 | 12 | ||||
| 6 | 1100 | 1×10 0* | 800 | 98.4 | 70 | 1.55 | 2 | |||||
| Existing method 2 | Mg ferrite: 0.17 | - | - | - | 800 | 97.4 | 30 | 1.47 | 1 | |||
*Value outside the expression scope of the invention.
(embodiment 2 other embodiment)
With with the embodiment 2 shown in the table 2 be the mode of same allotment ratio, for material powder B (Fe-Al is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 4 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 4 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 8 '～14 ' and comparative approach 4 '～6 ' and existing method 2 ' is presented in the table 4.
[table 4]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 8′ | B | Mg：0.1 | Vacuum | 150 | 1×10 -12 | O 2：5％， N 2：95％ 400℃ | 800 | 98.3 | 180 | 1.53 | 70 |
| 9′ | 300 | 1×10 -8 | 800 | 98 | 185 | 1.55 | 145 | |||||
| 10′ | Argon | 400 | 1×10 -6 | 800 | 99 | 210 | 1.55 | 180 | ||||
| 11′ | 500 | 1×10 -5 | 800 | 98.6 | 220 | 1.56 | 200 | |||||
| 12′ | 700 | 1×10 -2 | 800 | 98.5 | 210 | 1.55 | 215 | |||||
| 13′ | 900 | 1×10 -1 | 800 | 98.4 | 205 | 1.54 | 200 | |||||
| 14′ | 1100 | 1×10 -1 | 800 | 98 | 200 | 1.53 | 100 | |||||
| Comparison method | 4′ | Vacuum | 120 * | 1×10 -12 | 800 | 98.2 | 170 | 1.51 | 9 | |||
| 5′ | Argon | 1150 * | 1×10 -1 | 800 | 98 | 185 | 1.52 | 11 | ||||
| 6′ | 1100 | 1×10 0* | 800 | 98.4 | 70 | 1.55 | 2 | |||||
| Existing method 2 ' | Mg ferrite: 0.17 | - | - | - | - | 800 | 97.4 | 30 | 1.47 | 1 | ||
*Value outside the expression scope of the invention.
By the result shown in table 3 and the table 4 as can be known, composite soft magnetic material according to the inventive method 8～14 and the inventive method 8 '～14 ' making, compare with the composite soft magnetic material that existing method 2 of basis and present method 2 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 4～6 and comparative approach 4 '～6 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 3
In the allotment ratio shown in the table 5, for the soft magnetic powder C that has implemented the oxidation processes under the condition shown in the table 5 (Fe-Ni is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 5 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 5, making is implemented the inventive method 15～21 and comparative approach 7～9 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 15～21 and comparative approach 7～9 constitutes, its result is presented in the table 5, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results show at table 5.
(conventional example 3)
In the allotment ratio shown in the table 5, for the soft magnetic powder C allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 5, making is implemented existing method 3 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 3 of mensuration obtains constitutes, its result is presented in the table 5, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 5.
[table 5]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 15 | C | O 2：70 ％， N 2：30％ 500℃ | Mg：0.05 | Vacuum | 150 | 1×10 -12 | 1000 | 98.4 | 185 | 1.48 | 70 |
| 16 | 300 | 1×10 -8 | 1000 | 98.5 | 190 | 1.50 | 135 | |||||
| 17 | Argon | 400 | 1×10 -6 | 1000 | 98.5 | 210 | 1.51 | 160 | ||||
| 18 | 500 | 1×10 -5 | 1000 | 98.5 | 220 | 1.51 | 175 | |||||
| 19 | 700 | 1×10 -2 | 1000 | 98.5 | 220 | 1.50 | 160 | |||||
| 20 | 900 | 1×10 -1 | 1000 | 98.4 | 205 | 1.49 | 150 | |||||
| 21 | 1100 | 1×10 -1 | 1000 | 98.3 | 180 | 1.46 | 80 | |||||
| Comparison method | 7 | Vacuum | 120 * | 1×10 -12 | 1000 | 98.4 | 170 | 1.47 | 12 | |||
| 8 | Argon | 1150 * | 1×10 -1 | 1000 | 98.2 | 165 | 1.44 | 15 | ||||
| 9 | 1100 | 1×10 0* | 1000 | 98.5 | 60 | 1.50 | 3 | |||||
| Existing method 3 | - | Mg ferrite: 0.08 | - | - | - | 1000 | 97.9 | 25 | 1.44 | 0.7 | ||
*Value outside the expression scope of the invention.
(embodiment 3 other embodiment)
With with the embodiment 3 shown in the table 6 be the mode of same allotment ratio, for material powder C (Fe-Ni is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 6 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 6 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 15 '～21 ' and comparative approach 7 '～9 ' and existing method 3 ' is presented in the table 6.
[table 6]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 15′ | C | Mg：0.05 | Vacuum | 150 | 1×10 -12 | O 2：70 ％， N 2：30％ 500℃ | 1000 | 98 | 185 | 1.48 | 70 |
| 16′ | 300 | 1×10 -8 | 1000 | 99 | 190 | 1.50 | 135 | |||||
| 17′ | Argon | 400 | 1×10 -6 | 1000 | 99 | 210 | 1.50 | 160 | ||||
| 18′ | 500 | 1×10 -5 | 1000 | 99 | 215 | 1.50 | 175 | |||||
| 19′ | 700 | 1×10 -2 | 1000 | 98.5 | 220 | 1.51 | 155 | |||||
| 20′ | 900 | 1×10 -1 | 1000 | 98.4 | 210 | 1.49 | 150 | |||||
| 21′ | 1100 | 1×10 -1 | 1000 | 98 | 180 | 1.46 | 80 | |||||
| Comparison method | 7′ | Vacuum | 120 * | 1×10 -12 | 1000 | 98 | 170 | 1.47 | 12 | |||
| 8′ | Argon | 1150 * | 1×10 -1 | 1000 | 98 | 160 | 1.44 | 15 | ||||
| 9′ | 1100 | 1×10 0* | 1000 | 98.4 | 55 | 1.49 | 4 | |||||
| Existing method 3 ' | Mg ferrite: 0.08 | - | - | - | - | - | 98 | 25 | 1.44 | 0.7 | ||
*Value outside the expression scope of the invention.
By the result shown in table 5 and the table 6 as can be known, composite soft magnetic material according to the inventive method 15～21 and the inventive method 15 '～21 ' making, compare with the composite soft magnetic material that existing method 3 of basis and present method 3 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 7～9 and comparative approach 7 '～9 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 4
In the allotment ratio shown in the table 7, for the soft magnetic powder D that has implemented the oxidation processes under the condition shown in the table 7 (Fe-Cr is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 7 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 7, making is implemented the inventive method 22～28 and comparative approach 10～12 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 22～28 and comparative approach 10～12 constitutes, its result is presented in the table 7, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 7.
(conventional example 4)
In the allotment ratio shown in the table 7, for the soft magnetic powder D allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 7, making is implemented existing method 4 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 4 of mensuration obtains constitutes, its result is presented in the table 7, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 7.
[table 7]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 22 | D | 500 ℃ in atmosphere | Mg：0.08 | Vacuum | 150 | 1×10 -12 | 1200 | 98.2 | 250 | 1.55 | 85 |
| 23 | 300 | 1×10 -8 | 1200 | 98.3 | 275 | 1.56 | 140 | |||||
| 24 | Argon | 400 | 1×10 -6 | 1200 | 98.4 | 310 | 1.57 | 170 | ||||
| 25 | 500 | 1×10 -5 | 1200 | 98.4 | 330 | 1.58 | 210 | |||||
| 26 | 700 | 1×10 -2 | 1200 | 98.4 | 320 | 1.58 | 205 | |||||
| 27 | 900 | 1×10 -1 | 1200 | 98.4 | 305 | 1.57 | 170 | |||||
| 28 | 1100 | 1×10 -1 | 1200 | 98.4 | 290 | 1.56 | 115 | |||||
| Comparison method | 10 | Vacuum | 120 * | 1×10 -12 | 1200 | 98.0 | 130 | 1.52 | 14 | |||
| 11 | Argon | 1150 * | 1×10 -1 | 1200 | 98.1 | 160 | 1.53 | 19 | ||||
| 12 | 1100 | 1×10 0* | 1200 | 98.3 | 120 | 1.56 | 5 | |||||
| Existing method 4 | - | Mg ferrite: 0.14 | - | - | - | 1200 | 97.7 | 50 | 1.40 | 0.5 | ||
*Value outside the expression scope of the invention.
(embodiment 4 other embodiment)
With with the embodiment 4 shown in the table 8 be the mode of same allotment ratio, for material powder D (Fe-Cr is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 8 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 8 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 22 '～35 ' and comparative approach 10 '～15 ' and existing method 4 ' is presented in the table 8.
[table 8]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 22′ | D | Mg：0.08 | Vacuum | 150 | 1×10 -12 | 400 ℃ in atmosphere | 1200 | 98.2 | 250 | 1.55 | 85 |
| 23′ | 300 | 1×10 -8 | 1200 | 98.3 | 275 | 1.56 | 140 | |||||
| 24′ | Argon | 400 | 1×10 -6 | 1200 | 98.4 | 310 | 1.57 | 170 | ||||
| 25′ | 500 | 1×10 -5 | 1200 | 98.5 | 335 | 1.59 | 205 | |||||
| 26′ | 700 | 1×10 -2 | 1200 | 98.4 | 320 | 1.58 | 205 | |||||
| 27′ | 900 | 1×10 -1 | 1200 | 98.4 | 305 | 1.57 | 170 | |||||
| 28′ | 1100 | 1×10 -1 | 1200 | 98.4 | 290 | 1.56 | 115 | |||||
| 29′ | Vacuum | 150 | 1×10 -12 | 1150 | 98.1 | 240 | 1.54 | 90 | ||||
| 30′ | 300 | 1×10 -8 | 1150 | 98.2 | 270 | 1.55 | 141 | |||||
| 31′ | Argon | 400 | 1×10 -6 | 1150 | 98.2 | 300 | 1.56 | 175 | ||||
| 32 | 500 | 1×10 -5 | 1150 | 98.4 | 320 | 1.58 | 212 | |||||
| 33′ | 700 | 1×10 -2 | 1150 | 98.3 | 300 | 1.57 | 210 | |||||
| 34′ | 900 | 1×10 -1 | 1150 | 98.3 | 290 | 1.56 | 185 | |||||
| 35′ | 1100 | 1×10 -1 | 1150 | 98.2 | 275 | 1.54 | 120 | |||||
| Comparison method | 10′ | Vacuum | 120 * | 1×10 -12 | 1200 | 98.0 | 130 | 1.52 | 14 | |||
| 11′ | Argon | 1150 * | 1×10 -1 | 1200 | 98.1 | 160 | 1.53 | 19 | ||||
| 12′ | 1100 | 1×10 -0* | 1200 | 98.3 | 120 | 1.56 | 5 | |||||
| 13′ | Vacuum | 120 * | 1×10 -12 | 1150 | 97.9 | 120 | 1.51 | 19 | ||||
| 14′ | Argon | 1150 * | 1×10 -1 | 1150 | 98.0 | 150 | 1.52 | 25 | ||||
| 15′ | 1100 | 1×10 -0* | 1150 | 98.1 | 110 | 1.53 | 8 | |||||
| Existing method | 4′ | Mg ferrite: 0.14 | - | - | - | - | 1200 | 97.7 | 50 | 1.40 | 0.5 | |
*Value outside the expression scope of the invention.
By the result shown in table 7 and the table 8 as can be known, composite soft magnetic material according to the inventive method 22～28 and the inventive method 22 '～35 ' making, compare with the composite soft magnetic material that existing method 4 of basis and present method 4 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 10～12 and comparative approach 10 '～15 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 5
In the allotment ratio shown in the table 9, for the soft magnetic powder E that has implemented the oxidation processes under the condition shown in the table 9 (Fe-Si is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 9 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 9, making is implemented the inventive method 29～35 and comparative approach 13～15 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 29～35 and comparative approach 13～15 constitutes, its result is presented in the table 9, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 9.
(conventional example 5)
In the allotment ratio shown in the table 9, for the soft magnetic powder E allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 9, making is implemented existing method 5 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 5 of mensuration obtains constitutes, its result is presented in the table 9, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 9.
[table 9]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 29 | E | 150 ℃ in atmosphere | Mg：1 | Vacuum | 150 | 1×10 -12 | 1000 | 96.3 | 145 | 1.47 | 90 |
| 30 | 300 | 1×10 -8 | 1000 | 96.4 | 160 | 1.48 | 155 | |||||
| 31 | Argon | 400 | 1×10 -6 | 1000 | 96.6 | 180 | 1.50 | 170 | ||||
| 32 | 500 | 1×10 -5 | 1000 | 96.6 | 195 | 1.51 | 180 | |||||
| 33 | 700 | 1×10 -2 | 1000 | 96.5 | 190 | 1.50 | 175 | |||||
| 34 | 900 | 1×10 -1 | 1000 | 96.5 | 180 | 1.50 | 160 | |||||
| 35 | 1100 | 1×10 -1 | 1000 | 96.3 | 180 | 1.48 | 85 | |||||
| Comparison method | 13 | Vacuum | 120 * | 1×10 -12 | 1000 | 96.2 | 120 | 1.46 | 10 | |||
| 14 | Argon | 1150 * | 1×10 -1 | 1000 | 96.1 | 165 | 1.45 | 17 | ||||
| 15 | 1100 | 1×10 0* | 1000 | 96.3 | 70 | 1.47 | 1.5 | |||||
| Existing method 5 | - | Mg ferrite: 1.7 | - | - | - | 1000 | 94.0 | 20 | 1.38 | 0.6 | ||
*Value outside the expression scope of the invention.
(embodiment 5 other embodiment)
With with the embodiment 5 shown in the table 10 be the mode of same allotment ratio, for material powder E (Fe-Si is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 10 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 10 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 36 '～49 ' and comparative approach 16 '～21 ' and existing method 5 ' is presented in the table 10.
[table 10]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 36′ | E | Mg：1 | Vacuum | 150 | 1×10 -12 | 150 ℃ in atmosphere | 1000 | 96.3 | 145 | 1.47 | 90 |
| 37′ | 300 | 1×10 -8 | 1000 | 96.4 | 160 | 1.48 | 155 | |||||
| 38′ | Argon | 400 | 1×10 -6 | 1000 | 96.5 | 175 | 1.49 | 175 | ||||
| 39′ | 500 | 1×10 -5 | 1000 | 96.6 | 195 | 1.51 | 180 | |||||
| 40′ | 700 | 1×10 -2 | 1000 | 96.5 | 190 | 1.50 | 175 | |||||
| 41′ | 900 | 1×10 -1 | 1000 | 96.5 | 180 | 1.50 | 160 | |||||
| 42′ | 1100 | 1×10 -1 | 1000 | 96.3 | 180 | 1.48 | 85 | |||||
| 43′ | Vacuum | 150 | 1×10 -12 | 950 | 96.1 | 138 | 1.45 | 95 | ||||
| 44′ | 300 | 1×10 -8 | 950 | 96.3 | 150 | 1.46 | 160 | |||||
| 45′ | Argon | 400 | 1×10 -6 | 950 | 96.4 | 165 | 1.47 | 185 | ||||
| 46′ | 500 | 1×10 -5 | 950 | 96.5 | 190 | 1.50 | 190 | |||||
| 47′ | 700 | 1×10 -2 | 950 | 96.4 | 180 | 1.49 | 185 | |||||
| 48′ | 900 | 1×10 -1 | 950 | 96.3 | 190 | 1.48 | 170 | |||||
| 49′ | 1100 | 1×10 -1 | 950 | 96.2 | 165 | 1.47 | 90 | |||||
| Comparison method | 16′ | Vacuum | 120 * | 1×10 -12 | 1000 | 96.2 | 120 | 1.46 | 10 | |||
| 17′ | Argon | 1150 * | 1×10 -1 | 1000 | 96.0 | 160 | 1.44 | 19 | ||||
| 18′ | 1100 | 1×10 0* | 1000 | 96.3 | 70 | 1.47 | 1.5 | |||||
| 19′ | Vacuum | 120 * | 1×10 -12 | 950 | 96.0 | 105 | 1.44 | 15 | ||||
| 20′ | Argon | 1150 * | 1×10 -1 | 950 | 95.8 | 140 | 1.42 | 23 | ||||
| 21′ | 1100 | 1×10 0* | 950 | 96.1 | 80 | 1.45 | 1.7 | |||||
| Existing method | 5′ | Mg ferrite: 1.7 | - | - | - | - | 1000 | 94.0 | 20 | 1.38 | 0.6 | |
*Value outside the expression scope of the invention.
By the result shown in table 9 and the table 10 as can be known, composite soft magnetic material according to the inventive method 29～35 and the inventive method 36 '～49 ' making, compare with the composite soft magnetic material that existing method 5 of basis and present method 5 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 13～15 and comparative approach 16 '～21 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 6
In the allotment ratio shown in the table 11, for the soft magnetic powder F that has implemented the oxidation processes under the condition shown in the table 11 (Fe-Si-Al is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 11 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 11, making is implemented the inventive method 36～42 and comparative approach 16～18 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 36～42 and comparative approach 16～18 constitutes, its result is presented in the table 11, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 11.
(conventional example 6)
In the allotment ratio shown in the table 11, for the soft magnetic powder F allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 11, making is implemented existing method 6 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 6 of mensuration obtains constitutes, its result is presented in the table 11, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 11.
[table 11]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 36 | F | O 2：30％， Ar：70％ 100℃ | Mg：0.7 | Vacuum | 150 | 1×10 -12 | 900 | 98.1 | 160 | 1.48 | 90 |
| 37 | 300 | 1×10 -8 | 900 | 98.2 | 175 | 1.50 | 165 | |||||
| 38 | Argon | 400 | 1×10 -6 | 900 | 98.3 | 185 | 1.51 | 170 | ||||
| 39 | 500 | 1×10 -5 | 900 | 98.3 | 190 | 1.51 | 180 | |||||
| 40 | 700 | 1×10 -2 | 900 | 98.1 | 180 | 1.48 | 185 | |||||
| 41 | 900 | 1×10 -1 | 900 | 98.1 | 175 | 1.48 | 170 | |||||
| 42 | 1100 | 1×10 -1 | 900 | 98.0 | 160 | 1.46 | 105 | |||||
| Comparison method | 16 | Vacuum | 120 * | 1×10 -12 | 900 | 98.0 | 155 | 1.45 | 12 | |||
| 17 | Argon | 1150 * | 1×10 -1 | 900 | 97.9 | 150 | 1.42 | 15 | ||||
| 18 | 1100 | 1×10 0* | 900 | 98.3 | 55 | 1.50 | 4 | |||||
| Existing method 6 | - | Mg ferrite: 1.2 | - | - | - | 900 | 97.3 | 18 | 1.36 | 0.8 | ||
*Value outside the expression scope of the invention.
(embodiment 6 other embodiment)
With with the embodiment 6 shown in the table 12 be the mode of same allotment ratio, for material powder F (Fe-Si-Al is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 12 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 12 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 50 '～56 ' and comparative approach 22 '～24 ' and existing method 6 ' is presented in the table 12.
[table 12]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 50′ | F | Mg：0.7 | Vacuum | 150 | 1×10 -12 | O 2：30％， N 2：70％ 100℃ | 900 | 98.2 | 165 | 1.49 | 80 |
| 51′ | 300 | 1×10 -8 | 900 | 98.2 | 175 | 1.50 | 165 | |||||
| 52′ | Argon | 400 | 1×10 -6 | 900 | 98.3 | 185 | 1.51 | 170 | ||||
| 53′ | 500 | 1×10 -5 | 900 | 98.3 | 190 | 1.51 | 180 | |||||
| 54′ | 700 | 1×10 -2 | 900 | 98.1 | 180 | 1.48 | 185 | |||||
| 55′ | 900 | 1×10 -1 | 900 | 98.1 | 175 | 1.48 | 170 | |||||
| 56′ | 1100 | 1×10 -1 | 900 | 98.0 | 160 | 1.46 | 105 | |||||
| Comparison method | 22′ | Vacuum | 120 * | 1×10 -12 | 900 | 98.0 | 155 | 1.45 | 12 | |||
| 23′ | Argon | 1150 * | 1×10 -1 | 900 | 97.9 | 150 | 1.42 | 15 | ||||
| 24′ | 1100 | 1×10 0* | 900 | 98.3 | 55 | 1.50 | 4 | |||||
| Existing method 6 ' | Mg ferrite: 1.2 | - | - | - | - | 900 | 97.3 | 18 | 1.36 | 0.8 | ||
*Value outside the expression scope of the invention.
By the result shown in table 11 and the table 12 as can be known, composite soft magnetic material according to the inventive method 36～42 and the inventive method 50 '～56 ' making, compare with the composite soft magnetic material that existing method 6 of basis and present method 6 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 16～18 and comparative approach 22 '～24 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 7
In the allotment ratio shown in the table 13, for the soft magnetic powder G that has implemented the oxidation processes under the condition shown in the table 13 (Fe-Co-V is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 13 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 13, making is implemented the inventive method 43～49 and comparative approach 19～21 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 43～49 and comparative approach 19～21 constitutes, its result is presented in the table 13, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 13.
(conventional example 7)
In the allotment ratio shown in the table 13, for the soft magnetic powder G allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 13, making is implemented existing method 7 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 7 of mensuration obtains constitutes, its result is presented in the table 13, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 13.
[table 13]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 43 | G | 150 ℃ in atmosphere | Mg：2 | Vacuum | 150 | 1×10 -12 | 1300 | 94.8 | 180 | 1.68 | 80 |
| 44 | 300 | 1×10 -8 | 1300 | 95.2 | 205 | 1.70 | 115 | |||||
| 45 | Argon | 400 | 1×10 -6 | 1300 | 95.1 | 210 | 1.69 | 120 | ||||
| 46 | 500 | 1×10 -5 | 1300 | 95.0 | 200 | 1.69 | 130 | |||||
| 47 | 700 | 1×10 -2 | 1300 | 94.9 | 190 | 1.68 | 115 | |||||
| 48 | 900 | 1×10 -1 | 1300 | 94.8 | 185 | 1.65 | 115 | |||||
| 49 | 1100 | 1×10 -1 | 1300 | 94.5 | 160 | 1.67 | 90 | |||||
| Comparison method | 19 | Vacuum | 120 * | 1×10 -12 | 1300 | 94.8 | 110 | 1.65 | 10 | |||
| 20 | Argon | 1150 * | 1×10 -1 | 1300 | 94.0 | 125 | 1.60 | 15 | ||||
| 21 | 1100 | 1×10 0* | 1300 | 94.5 | 170 | 1.62 | 3 | |||||
| Existing method 7 | - | Mg ferrite: 3.33 | - | - | - | 1300 | 95.0 | 175 | 1.65 | 0.3 | ||
*Value outside the expression scope of the invention.
(embodiment 7 other embodiment)
With with the embodiment 7 shown in the table 14 be the mode of same allotment ratio, for material powder G (Fe-Co-V is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 14 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 14 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 57 '～70 ' and comparative approach 25 '～30 ' and existing method 7 ' is presented in the table 14.
[table 14]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 57′ | G | Mg：2 | Vacuum | 150 | 1×10 -12 | 150 ℃ in atmosphere | 1300 | 94.8 | 180 | 1.68 | 80 |
| 58′ | 300 | 1×10 -8 | 1300 | 95.2 | 205 | 1.70 | 115 | |||||
| 59′ | Argon | 400 | 1×10 -6 | 1300 | 95.2 | 215 | 1.70 | 110 | ||||
| 60′ | 500 | 1×10 -5 | 1300 | 95.0 | 200 | 1.69 | 130 | |||||
| 61′ | 700 | 1×10 -2 | 1300 | 94.9 | 190 | 1.68 | 115 | |||||
| 62′ | 900 | 1×10 -1 | 1300 | 94.8 | 185 | 1.67 | 115 | |||||
| 63′ | 1100 | 1×10 -1 | 1300 | 94.5 | 160 | 1.65 | 90 | |||||
| 64′ | Vacuum | 150 | 1×10 -12 | 1250 | 94.5 | 170 | 1.67 | 100 | ||||
| 65′ | 300 | 1×10 -8 | 1250 | 94.7 | 190 | 1.67 | 110 | |||||
| 66′ | Argon | 400 | 1×10 -6 | 1250 | 95.0 | 210 | 1.68 | 100 | ||||
| 67′ | 500 | 1×10 -5 | 1250 | 95.2 | 210 | 1.70 | 150 | |||||
| 68′ | 700 | 1×10 -2 | 1250 | 95.1 | 180 | 1.69 | 120 | |||||
| 69′ | 900 | 1×10 -1 | 1250 | 95.0 | 180 | 1.69 | 150 | |||||
| 70′ | 1100 | 1×10 -1 | 1250 | 94.6 | 170 | 1.66 | 120 | |||||
| Comparison method | 25′ | Vacuum | 120 * | 1×10 -12 | 1300 | 94.8 | 110 | 1.67 | 10 | |||
| 26′ | Argon | 1150 * | 1×10 -1 | 1300 | 94.0 | 125 | 1.60 | 15 | ||||
| 27′ | 1100 | 1×10 0* | 1300 | 94.5 | 170 | 1.62 | 3 | |||||
| 28′ | Vacuum | 120 * | 1×10 -12 | 1250 | 94.6 | 120 | 1.65 | 10 | ||||
| 29′ | Argon | 1150 * | 1×10 -1 | 1250 | 93.8 | 135 | 1.58 | 10 | ||||
| 30′ | 1100 | 1×10 0* | 1250 | 98.3 | 180 | 1.59 | 5 | |||||
| Existing method | 7′ | Mg ferrite: 3.33 | - | - | - | - | 1300 | 95.0 | 175 | 1.65 | 0.3 | |
*Value outside the expression scope of the invention.
By the result shown in table 13 and the table 14 as can be known, composite soft magnetic material according to the inventive method 43～49 and the inventive method 57 '～70 ' making, compare with the composite soft magnetic material that existing method 7 of basis and present method 7 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 19～21 and comparative approach 25 '～30 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 8
In the allotment ratio shown in the table 15, for the soft magnetic powder H that has implemented the oxidation processes under the condition shown in the table 15 (Fe-P is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 15 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 15, making is implemented the inventive method 50～56 and comparative approach 22～24 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 22～28 and comparative approach 10～12 constitutes, its result is presented in the table 15, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 15.
(conventional example 8)
In the allotment ratio shown in the table 15, for the soft magnetic powder H allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 15, making is implemented existing method 8 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 8 of mensuration obtains constitutes, its result is presented in the table 15, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 15.
[table 15]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 50 | H | O 2： 10 ％， Ar： 90 ％ 100 ℃ | Mg：0.5 | Vacuum | 150 | 1×10 -12 | 400 | 98.3 | 165 | 1.65 | 70 |
| 51 | 300 | 1×10 -8 | 400 | 98.5 | 170 | 1.68 | 125 | |||||
| 52 | Argon | 400 | 1×10 -6 | 400 | 98.5 | 185 | 1.68 | 160 | ||||
| 53 | 500 | 1×10 -5 | 400 | 98.6 | 185 | 1.69 | 175 | |||||
| 54 | 700 | 1×10 -2 | 400 | 98.6 | 180 | 1.69 | 165 | |||||
| 55 | 900 | 1×10 -1 | 400 | 98.7 | 170 | 1.70 | 140 | |||||
| 56 | 1100 | 1×10 -1 | 400 | 98.4 | 160 | 1.66 | 110 | |||||
| Comparison method | 22 | Vacuum | 120 * | 1×10 -12 | 400 | 98.2 | 155 | 1.62 | 12 | |||
| 23 | Argon | 1150 * | 1×10 -1 | 400 | 98.4 | 170 | 1.66 | 15 | ||||
| 24 | 1100 | 1×10 0* | 400 | 98.5 | 90 | 1.67 | 2 | |||||
| Existing method 8 | - | Mg ferrite: 0.85 | - | - | - | 400 | 98.1 | 27 | 1.61 | 0.25 | ||
*Value outside the expression scope of the invention.
(embodiment 8 other embodiment)
With with the embodiment shown in the table 16 be the mode of same allotment ratio, for material powder H (Fe-P is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 16 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 16 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 71 '～84 ' and comparative approach 31 '～36 ' and existing method 8 ' is presented in the table 16.
[table 16]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 71′ | H | Mg：0.5 | Vacuum | 150 | 1×10 -12 | O 2：10％， Ar：90％ 100℃ | 400 | 98.3 | 165 | 1.65 | 70 |
| 72′ | 300 | 1×10 -8 | 400 | 98.5 | 170 | 1.68 | 125 | |||||
| 73′ | Argon | 400 | 1×10 -6 | 400 | 98.5 | 185 | 1.68 | 160 | ||||
| 74′ | 500 | 1×10 -5 | 400 | 98.6 | 185 | 1.69 | 175 | |||||
| 75′ | 700 | 1×10 -2 | 400 | 98.6 | 180 | 1.69 | 165 | |||||
| 76′ | 900 | 1×10 -1 | 400 | 98.7 | 170 | 1.70 | 140 | |||||
| 77′ | 1100 | 1×10 -1 | 400 | 98.4 | 160 | 1.66 | 110 | |||||
| 78′ | Vacuum | 150 | 1×10 -12 | 450 | 98.4 | 170 | 1.66 | 68 | ||||
| 79′ | 300 | 1×10 -8 | 450 | 98.6 | 175 | 1.68 | 120 | |||||
| 80′ | Argon | 400 | 1×10 -6 | 450 | 98.6 | 190 | 1.68 | 155 | ||||
| 81′ | 500 | 1×10 -5 | 450 | 98.7 | 190 | 1.70 | 170 | |||||
| 82′ | 700 | 1×10 -2 | 450 | 98.7 | 185 | 1.69 | 160 | |||||
| 83′ | 900 | 1×10 -1 | 450 | 98.7 | 173 | 1.70 | 137 | |||||
| 84′ | 1100 | 1×10 -1 | 450 | 98.5 | 165 | 1.67 | 105 | |||||
| Comparison method | 31′ | Vacuum | 120 * | 1×10 -12 | 400 | 98.2 | 155 | 1.62 | 12 | |||
| 32′ | Argon | 1150 * | 1×10 -1 | 400 | 98.4 | 170 | 1.66 | 15 | ||||
| 33′ | 1100 | 1×10 -0* | 400 | 98.5 | 90 | 1.67 | 2 | |||||
| 34′ | Vacuum | 120 * | 1×10 -12 | 450 | 98.3 | 160 | 1.63 | 10 | ||||
| 35′ | Argon | 1150 * | 1×10 -1 | 450 | 98.5 | 180 | 1.66 | 12 | ||||
| 36′ | 1100 | 1×10 -0* | 450 | 98.6 | 95 | 1.68 | 1.7 | |||||
| Existing method | 8′ | Mg ferrite: 0.85 | - | - | - | - | 400 | 98.1 | 27 | 1.61 | 0.25 | |
*Value outside the expression scope of the invention.
By the result shown in table 15 and the table 16 as can be known, composite soft magnetic material according to the inventive method 50～56 and the inventive method 71 '～84 ' making, compare with the composite soft magnetic material that existing method 8 of basis and present method 8 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 22～24 and comparative approach 31 '～36 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 9
In the allotment ratio shown in the table 17, for the soft magnetic powder I that has implemented the oxidation processes under the condition shown in the table 17 (phosphate lining iron powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 17 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 17, making is implemented the inventive method 57～63 and comparative approach 25～27 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 57～63 and comparative approach 25～27 constitutes, its result is presented in the table 17, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 17.
(conventional example 9)
In the allotment ratio shown in the table 17, for the soft magnetic powder I allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 17, making is implemented existing method 9 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 9 of mensuration obtains constitutes, its result is presented in the table 17, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 17.
[table 17]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic interpolation of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m(T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 57 | I | O 2： 10 ％， Ar： 90 ％ 100 ℃ | Mg：0.5 | Vacuum | 150 | 1×10 -12 | 600 | 98.3 | 165 | 1.65 | 70 |
| 58 | 300 | 1×10 -8 | 600 | 98.5 | 170 | 1.68 | 125 | |||||
| 59 | Argon | 400 | 1×10 -6 | 600 | 98.5 | 180 | 1.68 | 180 | ||||
| 60 | 500 | 1×10 -5 | 600 | 98.6 | 180 | 1.69 | 185 | |||||
| 61 | 700 | 1×10 -2 | 600 | 98.6 | 185 | 1.69 | 180 | |||||
| 62 | 900 | 1×10 -1 | 600 | 98.7 | 170 | 1.70 | 160 | |||||
| 63 | 1100 | 1×10 -1 | 600 | 98.4 | 160 | 1.66 | 130 | |||||
| Comparison method | 25 | Vacuum | 120 * | 1×10 -12 | 600 | 98.2 | 110 | 1.62 | 120 | |||
| 26 | Argon | 1150 * | 1×10 -1 | 600 | 98.4 | 150 | 1.66 | 14 | ||||
| 27 | 1100 | 1×10 0* | 600 | 98.5 | 160 | 1.67 | 20 | |||||
| Existing method 9 | - | Mg ferrite: 0.85 | - | - | - | 60 | 98.1 | 20 | 1.61 | 0.3 | ||
*Value outside the expression scope of the invention.
(embodiment 9 other embodiment)
With with the embodiment 9 shown in the table 18 be the mode of same allotment ratio, for material powder I (phosphate lining iron powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 18 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 18 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 85 '～91 ' and comparative approach 37 '～39 ' and existing method 9 ' is presented in the table 18.
[table 18]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 85′ | I | Mg：0.5 | Vacuum | 150 | 1×10 -12 | O 2：10％， Ar：90％ 100℃ | 600 | 98.2 | 160 | 1.66 | 70 |
| 86′ | 300 | 1×10 -8 | 600 | 98.3 | 175 | 1.64 | 125 | |||||
| 87′ | Argon | 400 | 1×10 -6 | 600 | 98.3 | 170 | 1.64 | 160 | ||||
| 88′ | 500 | 1×10 -5 | 600 | 98.4 | 165 | 1.65 | 170 | |||||
| 89′ | 700 | 1×10 -2 | 600 | 98.4 | 160 | 1.65 | 160 | |||||
| 90′ | 900 | 1×10 -1 | 600 | 98.5 | 160 | 1.66 | 150 | |||||
| 91′ | 1100 | 1×10 -1 | 600 | 98.6 | 170 | 1.66 | 110 | |||||
| Comparison method | 37′ | Vacuum | 120 * | 1×10 -12 | 600 | 98.2 | 160 | 1.64 | 12 | |||
| 38′ | Argon | 1150 * | 1×10 -1 | 600 | 98.0 | 150 | 1.60 | 15 | ||||
| 39′ | 1100 | 1×10 0* | 600 | 98.2 | 95 | 1.64 | 2 | |||||
| Existing method d 9 ' | Mg ferrite: 0.85 | - | - | - | - | 60 | 98.1 | 20 | 1.61 | 0.3 | ||
*Value outside the expression scope of the invention.
By the result shown in table 17 and the table 18 as can be known, composite soft magnetic material according to the inventive method 57～63 and the inventive method 85 '～91 ' making, compare with the composite soft magnetic material that existing method 9 of basis and present method 9 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 25～27 and comparative approach 37 '～39 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Embodiment 10
In the allotment ratio shown in the table 19, for the soft magnetic powder J that has implemented the oxidation processes under the condition shown in the table 19 (Fe-Co is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 19 and the temperature and rotate, make thus and contain Mg oxide-film lining soft magnetic metal powder.
The Mg oxide-film lining soft magnetic metal powder that contains that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 19, making is implemented the inventive method 64～70 and comparative approach 28～30 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that mensuration obtains according to the inventive method 57～63 and comparative approach 25～27 constitutes, its result is presented in the table 19, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 19.
(conventional example 10)
In the allotment ratio shown in the table 19, for the soft magnetic powder J allotment Mg ferrite powder of preparing among the embodiment, should allocate powder and in atmosphere, stir while rotating, be made into mixed-powder.The mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, height: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, the calcining that keeps 30 minutes with the temperature shown in the table 19, making is implemented existing method 10 by composite soft magnetic material tabular and that the ring-type calcined body constitutes.Relative density, resistivity and the fracture resistence force of the composite soft magnetic material that the tabular calcined body that the existing in view of the above method 10 of mensuration obtains constitutes, its result is presented in the table 19, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density by BH tracing instrument, these results are displayed in Table 19.
[table 19]
| Species | Soft magnetic powder | The oxidation processes condition | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 64 | J | O 2： 10％， Ar： 90％ 100 ℃ | Mg：0.5 | Vacuum | 150 | 1×10 -12 | 1300 | 94.7 | 160 | 1.65 | 70 |
| 65 | 300 | 1×10 -8 | 1300 | 94.9 | 180 | 1.66 | 100 | |||||
| 66 | Argon | 400 | 1×10 -6 | 1300 | 94.9 | 190 | 1.67 | 115 | ||||
| 67 | 500 | 1×10 -5 | 1300 | 95.0 | 195 | 1.67 | 120 | |||||
| 68 | 700 | 1×10 -2 | 1300 | 95.0 | 190 | 1.67 | 115 | |||||
| 69 | 900 | 1×10 -1 | 1300 | 95.0 | 180 | 1.67 | 110 | |||||
| 70 | 1100 | 1×10 -1 | 1300 | 94.9 | 170 | 1.65 | 85 | |||||
| Comparison method | 28 | Vacuum | 120 * | 1×10 -12 | 1300 | 94.6 | 110 | 1.63 | 10 | |||
| 29 | Argon | 1150 * | 1×10 -1 | 1300 | 94.2 | 120 | 1.60 | 12 | ||||
| 30 | 1100 | 1×10 0* | 1300 | 94.2 | 160 | 1.60 | 3 | |||||
| Existing method 10 | - | Mg ferrite: 0.85 | - | - | - | 1300 | 92.0 | 150 | 1.55 | 0.3 | ||
*Value outside the expression scope of the invention.
(embodiment 10 other embodiment)
With with the embodiment 10 shown in the table 20 be the mode of same allotment ratio, for material powder J (Fe-Co is the iron-base soft magnetic alloy powder) allotment Mg powder, should allocate powder in argon gas or vacuum atmosphere, remain under pressure shown in the table 20 and the temperature and rotate, implement the oxidation processes under the condition shown in the table 20 afterwards, be made into thus and contain Mg oxide-film lining soft magnetic metal powder.
The result who has implemented the inventive method 92 '～98 ' and comparative approach 40 '～42 ' and existing method 10 ' is presented in the table 20.
[table 20]
| Species | Material powder | The ferritic addition of Mg or Mg (quality %) | The condition of material powder and Mg powder is rotated in heating | The oxidation processes condition | Calcining heat (℃) | The characteristic of composite soft magnetic material | ||||||
| Atmosphere | Temperature (℃) | Pressure (MPa) | Relative density (%) | Rupture strength (MPa) | Magnetic flux density B 10KA/m (T) | Resistivity (μ Ω m) | ||||||
| Method of the present invention | 92′ | J | Mg：0.5 | Vacuum | 150 | 1×10 -12 | O 2：10％， Ar：90％ 100℃ | 1300 | 94.9 | 190 | 1.70 | 70 |
| 93′ | 300 | 1×10 -8 | 1300 | 95.3 | 210 | 1.72 | 105 | |||||
| 94′ | Argon | 400 | 1×10 -6 | 1300 | 95.3 | 220 | 1.72 | 100 | ||||
| 95′ | 500 | 1×10 -5 | 1300 | 95.1 | 210 | 1.71 | 100 | |||||
| 96′ | 700 | 1×10 -2 | 1300 | 95.0 | 200 | 1.70 | 105 | |||||
| 97′ | 900 | 1×10 -1 | 1300 | 94.9 | 190 | 1.69 | 100 | |||||
| 98′ | 1100 | 1×10 -1 | 1300 | 94.6 | 170 | 1.68 | 80 | |||||
| Comparison method | 40′ | Vacuum | 120 * | 1×10 -12 | 1300 | 94.9 | 100 | 1.67 | 8 | |||
| 41′ | Argon | 1150 * | 1×10 -1 | 1300 | 94.1 | 110 | 1.60 | 13 | ||||
| 42′ | 1100 | 1×10 0* | 1300 | 94.6 | 175 | 1.63 | 2 | |||||
| Existing method 10 ' | Mg ferrite: 0.85 | - | - | - | - | 1300 | 92.0 | 150 | 1.55 | 0.3 | ||
*Value outside the expression scope of the invention.
By the result shown in table 19 and the table 20 as can be known, composite soft magnetic material according to the inventive method 64～70 and the inventive method 92 '～98 ' making, compare with the composite soft magnetic material that existing method 10 of basis and present method 10 ' are made, its rupture strength, magnetic flux density and resistivity are all excellent.But according to the composite soft magnetic material of comparative approach 28～30 and comparative approach 40 '～42 ' making, the characteristic of its relative density, magnetic flux density is poor, is not preferred therefore.
Next, just describe again based on other the embodiment of mode.
As the soft magnetism material powder, prepare all to have the pure iron powder that average grain diameter is 70 μ m,
Preparing Al is that the efflorescence Fe-Al that 10 quality %, surplus are made of Fe is the iron-base soft magnetic alloy powder,
Preparing Ni is that the efflorescence Fe-Ni that 49 quality %, surplus are made of Fe is the iron-base soft magnetic alloy powder,
Preparing Cr is that the efflorescence Fe-Cr that 10 quality %, surplus are made of Fe is the iron-base soft magnetic alloy powder,
Preparing Si is that 3 quality %, surplus Fe are the iron-base soft magnetic alloy powder by the efflorescence Fe-Si that constitutes,
It is that 3 quality %, Al are that the efflorescence Fe-Si-Al that 3 quality %, surplus are made of Fe is the iron-base soft magnetic alloy powder that preparation contains Si,
The Fe-Co-V that preparation contains that Co is 30%, V is 2%, surplus is made of Fe and unavoidable impurities is the iron-base soft magnetic alloy powder.These soft magnetic powders in atmosphere, were kept 1 hour with 220 ℃ temperature, make the oxide lining soft magnetic powder that the surface has ferroelectric oxide film thus, prepare as material powder.In addition, to prepare to have average grain diameter be the SiO powder of 10 μ m and have the Mg powder that average grain diameter is 50 μ m.
Embodiment 11
First-selected, in ready oxide lining soft magnetic powder as material powder, with oxide lining soft magnetic powder: SiO powder=99.9 quality %: the mode of 0.1 quality % is added the SiO powder respectively and is mixed, be made into mixed-powder, with the mixed-powder that obtains temperature, 2.7 * 10 at 650 ℃
-4The pressure of MPa kept 3 hours down, was produced on the silica lining soft magnetic powder that the surface has silicon oxide film thus.The surperficial formed silicon oxide film of confirming these silica lining soft magnetic powders is to contain SiO
X(wherein x=1～2) film.Secondly, in this silica lining soft magnetic powder, with silica lining soft magnetic powder: Mg powder=99.8 quality %: the mode of 0.2 quality % is added the Mg powder respectively and is mixed, and makes mixed-powder, with the mixed-powder that the obtains temperature, 2.7 * 10 at 650 ℃
-4The pressure of MPa kept 1 hour down, and what the surface that is produced on soft magnetic powder thus was formed with the oxidation film that contains Mg and Si contains Mg-Si oxide lining soft magnetic powder.
These are contained Mg-Si oxide lining soft magnetic powder put into the metal pattern extrusion molding respectively, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, calcine with the condition that 600 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of these tabular calcined bodies formations, its result is presented in the table 21, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 1.5T, iron loss during frequency 50Hz, and magnetic flux density 1.0T, the magnetic characteristic of the iron loss during frequency 400Hz etc., these results are presented in the table 21.
First-selected, in ready oxide lining soft magnetic powder as material powder, in oxide lining soft magnetic powder: SiO powder: Mg powder=99.7 quality %: 0.1 quality %: the ratio of 0.2 quality %, adding SiO powder and Mg powder is respectively simultaneously also mixed, be made into mixed-powder, with the mixed-powder that obtains temperature, 2.7 * 10 at 650 ℃
-4The pressure of MPa kept 3 hours down, and what the surface that is produced on soft magnetic powder thus was formed with the oxidation film that contains Mg and Si contains Mg-Si oxide lining soft magnetic powder.
These are contained Mg-Si oxide lining soft magnetic powder put into the metal pattern extrusion molding respectively, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, calcine with the condition that 600 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of these tabular calcined bodies formations, its result is presented in the table 21, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 1.5T, iron loss during frequency 50Hz, and magnetic flux density 1.0T, the magnetic characteristic of the iron loss during frequency 400Hz etc., these results are presented in the table 22.
Embodiment 13
First-selected, in ready oxide lining soft magnetic powder as material powder, with oxide lining soft magnetic powder: Mg powder=99.8 quality %: the mode of 0.2 quality % is added the Mg powder respectively and is mixed, be made into mixed-powder, with the mixed-powder that obtains temperature, 2.7 * 10 at 650 ℃
-4The pressure of MPa kept 2 hours down, was made into the magnesia lining soft magnetic powder that has the MgO film on the surface thus.Again in this silica lining soft magnetic powder, with magnesia lining soft magnetic powder: SiO powder=99.9 quality %: the mode of 0.1 quality % is added the SiO powder respectively and is mixed, making mixed-powder, with the mixed-powder that obtains temperature, 2.7 * 10 at 650 ℃
-4The pressure of MPa kept 3 hours down, and what the surface that is produced on soft magnetic powder thus was formed with the oxidation film that contains Mg and Si contains Mg-Si oxide lining soft magnetic powder.
These are contained Mg-Si oxide lining soft magnetic powder put into the metal pattern extrusion molding respectively, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, calcine with the condition that 600 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of these tabular calcined bodies formations, its result is presented in the table 21, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 1.5T, iron loss during frequency 50Hz, and magnetic flux density 1.0T, the magnetic characteristic of the iron loss during frequency 400Hz etc., these results are presented in the table 23.
(conventional example 11)
At first, connect according to water atomization pure soft magnetic powder: silicones: the ratio of Mg powder=99.8: 14: 0.06, distinguish hybrid silicone and MgO powder for ready as the pure soft magnetic powder of water atomization, make existing mixed-powder, the mixed-powder that obtains is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, 30 minutes condition sintering of temperature maintenance with 600 ℃, make thus by composite soft magnetic sintering material tabular and that the ring-type sintered body constitutes, measure the resistivity of the composite soft magnetic material of tabular sintered body formation, its result is presented in the table 21, the composite soft magnetic material that the ring-type sintered body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 1.5T, iron loss during frequency 50Hz, and magnetic flux density 1.0T, the magnetic characteristic of the iron loss during frequency 400Hz etc., these results are presented in table 21～23.
[21]
| Species | The one-tenth of oxide lining soft magnetic metal powder is grouped into (quality %) | Use the characteristic of the composite soft magnetic sintering material of oxide lining soft magnetic metal powder making | |||||||
| Oxide | Surplus | Density (g/cm3) | Magnetic flux density B10KA/m (T) | Coercive force (A/m) | Iron loss *4 (W/kg) | Iron loss *5 (W/kg) | Resistivity (μ Ω m) | ||
| The present invention | 1 | 0.1%SiO steaming-＞0.2%Mg steaming ( *1) | Straight iron powder | 7.65 | 1.68 | 180 | 8.1 | 55 | 100 |
| Existing method | Silicones n 0.14 %, the MgO powder | Pure is an iron powder | 7.65 | 1.59 | 220 | 60 | 800 | 0.4 | |
| The present invention | 2 | *1 | Fe-Al is an iron powder | 7.18 | 1.58 | 110 | 4.2 | 35 | 120 |
| Existing method | * | Fe-Al is an iron powder | 7.15 | 1.56 | 100 | 30 | 420 | 15 | |
| The present invention | 3 | *1 | Fe-Ni is an iron powder | 7.91 | 1.15 | 120 | --- | 40 | 130 |
| Existing method | * | Fe-Ni is an iron powder | 7.86 | 1.1 | 140 | --- | 480 | 20 | |
| The present invention | 4 | *1 | Fe-Cr is an iron powder | 7.64 | 1.25 | 180 | --- | 48 | 110 |
| Existing method | * | Fe-Cr is an iron powder | 7.64 | 1.2 | 200 | --- | 720 | 12 | |
| The present invention | 5 | *1 | Fe-Si is an iron powder | 7.62 | 1.55 | 100 | 3.8 | 30 | 200 |
| Existing method | * | Fe-Si is an iron powder | 7.63 | 1.53 | 120 | 30 | 400 | 15 | |
| The present invention | 6 | *1 | Fe-Si-Al is an iron powder | 7.64 | 1.05 | 110 | --- | 40 | 100 |
| Existing method | * | Fe-Si-Al is an iron powder | 7.63 | 1.01 | 140 | --- | 500 | 20 | |
| The present invention | 7 | *1 | Fe-Co-V is an iron powder | 7.65 | 1.95 | 180 | 6.2 | 50 | 100 |
| Existing method | * | Fe-Co-V is an iron powder | 7.65 | 1.92 | 220 | 60 | 780 | 12 | |
Iron loss when ※ 4 iron loss are represented magnetic flux density 1.5T, frequency 50Hz.
Iron loss when ※ 5 iron loss are represented magnetic flux density 1.0T, frequency 400Hz.
[22]
| Species | The one-tenth of oxide lining soft magnetic metal powder is grouped into (quality %) | Use the characteristic of the composite soft magnetic sintering material of oxide lining soft magnetic metal powder making | |||||||
| Oxide | Surplus | Density (g/cm3) | Magnetic flux density B10KA/m (T) | Coercive force (A/m) | Iron loss *4 (W/kg) | Iron loss *5 (W/kg) | Resistivity (μ Ω m) | ||
| The present invention | 1 | 0.1%SiO and 0.2%Mg steaming simultaneously ( *2) | Straight iron powder | 7.65 | 1.69 | 165 | 7.8 | 49 | 110 |
| Existing method | 0.14% silicones, the 0.06%MgO powder ( *) | Straight iron powder | 7.65 | 1.59 | 220 | 60 | 800 | 0.4 | |
| The present invention | 2 | *2 | Fe-Al is an iron powder | 7.18 | 1.58 | 100 | 3.8 | 31 | 135 |
| Existing method | * | Fe-Al is an iron powder | 7.15 | 1.56 | 100 | 30 | 420 | 15 | |
| The present invention | 3 | *2 | Fe-Ni is an iron powder | 7.91 | 1.15 | 105 | --- | 36 | 140 |
| Existing method | * | Fe-Ni is an iron powder | 7.86 | 1.1 | 140 | --- | 480 | 20 | |
| The present invention | 4 | *2 | Fe-Cr is an iron powder | 7.64 | 1.25 | 162 | --- | 44 | 122 |
| Existing method | * | Fe-Cr is an iron powder | 7.64 | 1.2 | 200 | --- | 720 | 12 | |
| The present invention | 5 | *2 | Fe-Si is an iron powder | 7.62 | 1.55 | 90 | 3.6 | 27 | 220 |
| Existing method | * | Fe-Si is an iron powder | 7.63 | 1.53 | 120 | 30 | 400 | 15 | |
| The present invention | 6 | *2 | Fe-Si-Al is an iron powder | 7.64 | 1.05 | 100 | --- | 36 | 110 |
| Existing method | * | Fe-Si-Al is an iron powder | 7.63 | 1.01 | 140 | --- | 500 | 20 | |
| The present invention | 7 | *2 | Fe-Co-V is an iron powder | 7.65 | 1.95 | 162 | 5.8 | 45 | 108 |
| Existing method | * | Fe-Co-V is an iron powder | 7.65 | 1.92 | 220 | 60 | 780 | 12 | |
[23]
| Species | The one-tenth of oxide lining soft magnetic metal powder is grouped into (quality %) | Use the characteristic of the composite soft magnetic sintering material of oxide lining soft magnetic metal powder making | |||||||
| Oxide | Surplus | Density (g/cm3) | Magnetic flux density B10KA/m (T) | Coercive force (A/m) | Iron loss *4 (W/kg) | Iron loss *5 (W/kg) | Resistivity (μ Ω m) | ||
| The present invention | 1 | 0.2%MgO steaming-＞0.1%SiO steaming ( *3) | Straight iron powder | 7.64 | 1.68 | 170 | 7.9 | 52 | 105 |
| Existing method | 0.14% silicones, the MgO powder | Straight iron powder | 7.65 | 1.59 | 220 | 60 | 800 | 0.4 | |
| The present invention | 2 | *3 | Fe-Al is an iron powder | 7.18 | 1.58 | 105 | 4 | 34 | 128 |
| Existing method | * | Fe-Al is an iron powder | 7.15 | 1.56 | 100 | 30 | 420 | 15 | |
| The present invention | 3 | *3 | Fe-Ni is an iron powder | 7.91 | 1.15 | 113 | --- | 38 | 136 |
| Existing method | * | Fe-Ni is an iron powder | 7.86 | 1.1 | 140 | --- | 480 | 20 | |
| The present invention | 4 | *3 | Fe-Cr is an iron powder | 7.64 | 1.25 | 172 | --- | 46 | 115 |
| Existing method | * | Fe-Cr is an iron powder | 7.64 | 1.2 | 200 | --- | 720 | 12 | |
| The present invention | 5 | *3 | Fe-Si is an iron powder | 7.62 | 1.55 | 95 | 3.6 | 28 | 210 |
| Existing method | * | Fe-Si is an iron powder | 7.63 | 1.53 | 120 | 30 | 400 | 15 | |
| The present invention | 6 | *3 | Fe-Si-Al is an iron powder | 7.64 | 1.05 | 105 | --- | 38 | 105 |
| Existing method | * | Fe-Si-Al is an iron powder | 7.63 | 1.01 | 140 | --- | 500 | 20 | |
| The present invention | 7 | *3 | Fe-Co-V is an iron powder | 7.65 | 1.95 | 173 | 6 | 47 | 108 |
| Existing method | * | Fe-Co-V is an iron powder | 7.65 | 1.92 | 220 | 60 | 780 | 12 | |
By the result shown in table 21～23 as can be known, adopted the composite soft magnetic material of making by embodiment 1～3 that Mg-Si oxide lining soft magnetic powder makes that contains to have as inferior characteristic, it is compared with adopting the composite soft magnetic material of being made by conventional example 1 that Mg-Si oxide lining soft magnetic powder makes that contains, there is not big difference with regard to density, but adopted the composite soft magnetic material that Mg-Si oxide lining soft magnetic powder is made that contains by embodiment 1～3 making, with adopt the composite soft magnetic material of making by conventional example 1 that Mg-Si oxide lining soft magnetic powder makes that contains and compare, its magnetic flux density height, coercive force is little, resistivity is especially high in addition, therefore iron loss is especially little, and particularly the big more iron loss of frequency is more little.
Embodiment 14
As material powder, preparing to have average grain diameter is that 75 μ m, Si are that the Fe-Si that 1 quality %, surplus are made of Fe and unavoidable impurities is an iron-based soft magnetic powder, and preparing average grain diameter in addition is the following pure Si powder of 1 μ m.Preparing average grain diameter again is the Mg powder of 50 μ m.
First-selected, at Fe-Si is in the iron-based soft magnetic powder, with Fe-Si is iron-based soft magnetic powder: pure Si powder=99.5 quality %: the mode of 0.5 quality % is allocated pure Si powder, and the mixed mixed-powder that makes in addition, with the mixed-powder that obtains in nitrogen atmosphere, heat-treat with the condition that 950 ℃ temperature kept 1 hour, be that the iron-based soft magnetic powder surface forms high concentration Si diffusion layer at Fe-Si thus, thereafter in atmosphere, keep under the condition of 250 ℃ temperature, being produced on the surface oxidation Fe-Si that has oxide layer on the high concentration Si diffusion layer thus is the iron-base soft magnetic material powder.
At surface oxidation Fe-Si is in the iron-base soft magnetic material powder, in surface oxidation Fe-Si is the iron-base soft magnetic material powder: Mg powder=99.8 quality %: the ratio of 0.2 quality % is allocated preprepared Mg powder, mixing manufacture mixed-powder in addition is 2.7 * 10 with the mixed-powder that obtains at 650 ℃ temperature, pressure
-4The following limit of rotating of the condition of MPa kept 1 hour, and it is iron-based soft magnetic powder 1 (piling up oxide-film lining powder hereinafter referred to as the present invention) that the present invention that the surface that is produced on Fe-Si thus and is iron-based soft magnetic powder is formed with the accumulation oxide-film that is made of Mg, Si, Fe and O piles up oxide-film lining Fe-Si.
The present invention who so obtains is piled up oxide-film lining powder 1 puts into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, calcine with the condition that 500 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 24, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 1.5T, iron loss during frequency 50Hz, and magnetic flux density 1.0T, the magnetic characteristic of the iron loss during frequency 400Hz etc., these results are presented in the table 1.
Conventional example 12
Making what prepare among the embodiment 14 is that to be formed with the existing Mg of the containing ferrite magnetic oxide lining Fe-Si that contains Mg ferrite magnetic oxide layer be iron-based soft magnetic powder (to call the existing oxide-film lining powder of piling up in the following text) for the surface chemistry ground of iron-based soft magnetic powder at Fe-Si, this existing oxide-film lining powder of piling up is put into the metal pattern extrusion molding, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in blanket of nitrogen, carry out sintering with the condition that 500 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type sintered body constitutes, measure the resistivity of the composite soft magnetic material of tabular sintered body formation, its result is presented in the table 24, the composite soft magnetic material that the ring-type sintered body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 1.5T, iron loss during frequency 50Hz, and magnetic flux density 1.0T, the magnetic characteristic of the iron loss during frequency 400Hz etc., these results are presented in the table 24.
[24]
| Species | The Mg-Si-Fe-O quaternary system is piled up the characteristic of oxide-film | The characteristic of composite soft magnetic material | ||||||
| Thickness (nm) | Maximum crystallization particle diameter (mm) | Density (g/cm 3) | Magnetic flux density B10KA/m (T) | Coercive force (A/m) | Iron loss * (W/kg) | Iron loss ** (W/kg) | Resistivity (μ Ω m) | |
| Embodiment 14 | 100 | 30 | 7.6 | 1.57 | 90 | 23 | 20 | 1200 |
| Conventional example 12 | - | - | 7.4 | 1.50 | 145 | - | 58 | 35 |
Iron loss
*Iron loss during expression magnetic flux density 1.5T frequency 50Hz.
Iron loss
*Iron loss during expression magnetic flux density 1.0T frequency 400Hz.
By the result shown in the table 24 as can be known, having used the present invention who is made by embodiment 14 to pile up the composite soft magnetic material that oxide-film lining powder 1 makes has as inferior characteristic, its with use by conventional example 12 make to contain Mg ferrite magnetic oxide lining Fe-Si be that the composite soft magnetic material that iron-based soft magnetic powder is made is compared, there is not big difference with regard to density, but adopted the present invention who makes by embodiment 14 to pile up the composite soft magnetic material that oxide-film lining powder 1 is made, with adopting this Mg of containing ferrite of the existing accumulation oxide-film lining powder oxide-film lining Fe-Si that is made by conventional example 12 is that the composite soft magnetic material that iron-based soft magnetic powder is made is compared, its magnetic flux density height, coercive force is little, resistivity is especially high in addition, therefore iron loss is especially little, and particularly the big more iron loss of frequency is more little.
Embodiment 15
As material powder, preparing to have granularity shown in the table 25 and contain Si is 1 quality %, and the Fe-Si that surplus is made of Fe and unavoidable impurities is an iron-based soft magnetic powder.Preparing average grain diameter in addition is that 1 μ m following pure Si powder and average grain diameter are the Mg powder of 50 μ m.
Different Fe-Si is in the iron-based soft magnetic powder in these granularities, with Fe-Si is iron-based soft magnetic powder: pure Si powder=97 quality %: the mode of 2 quality % is allocated pure Si powder, and the mixed mixed-powder that makes in addition, with the mixed-powder that obtains in nitrogen atmosphere, heat-treat with the condition that 950 ℃ temperature kept 1 hour, be that the iron-based soft magnetic powder surface forms high concentration Si diffusion layer at Fe-Si thus, thereafter in atmosphere, 220 ℃ temperature conditions keeps down, and being produced on the surface oxidation Fe-Si that has oxide layer on the high concentration Si diffusion layer thus is the iron-base soft magnetic material powder.
For surface oxidation Fe-Si is the iron-base soft magnetic material powder, in surface oxidation Fe-Si is the iron-base soft magnetic material powder: Mg powder=99.8 quality %: the ratio of 0.2 quality % is allocated preprepared Mg powder, mixing manufacture mixed-powder in addition, the temperature, the pressure that the mixed-powder that obtains are implemented in 650 ℃ are 2.7 * 10
-4The condition of MPa is following rotates the processing that the limit kept 1 hour (in surface oxidation Fe-Si is the iron-base soft magnetic material powder: Mg powder=99.8 quality %: the ratio of 0.2 quality % is allocated and mixed and make mixed-powder, is 2.7 * 10 with the mixed-powder that obtains at 650 ℃ temperature, pressure
-4Keep 1 hour while rotating under the condition of MPa, this processing is hereinafter referred to as " Mg be covered processing "), the accumulation oxide-film lining Fe-Si that the surface that is produced on Fe-Si thus and is iron-based soft magnetic powder is formed with the accumulation oxide-film that is made of Mg, Si, Fe and O is an iron-based soft magnetic powder, thereby has implemented the inventive method 71～73.
For the accumulation oxide-film lining Fe-Si that obtains by the inventive method 71～73 is iron-based soft magnetic powder, add silicones and mixing in proportioning 2 quality %, making has been covered by silicones, and to pile up oxide-film lining Fe-Si be the resin-coated composite powder on the surface of iron-based soft magnetic powder, this resin-coated composite powder is put into the metal pattern extrusion molding that is heated to 120 ℃, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in a vacuum, calcine with the condition that 700 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 2, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 0.1T, iron loss during frequency 20Hz, these results are presented in the table 25.
Conventional example 13
As material powder, preparation has granularity shown in the table 25 and contains Si is 1 quality %, the Fe-Si that surplus is made of Fe and unavoidable impurities is an iron-based soft magnetic powder, to this Fe-Si is that iron-based soft magnetic powder does not carry out Mg lining processing, but add silicones and mixing in proportioning 2 quality %, making by silicones lining Fe-Si is the resin-coated composite powder on the surface of iron-based soft magnetic powder.This resin-coated composite powder is put into the metal pattern extrusion molding that is heated to 120 ℃, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in a vacuum, calcine with the condition that 700 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 25, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 0.1T, iron loss during frequency 20Hz, these results are presented in the table 25.
[25]
| Species | The average grain diameter of Fe-1%Si raw material powder (μ m) | The Mg processing that is covered | Magnetic characteristic | ||||
| Magnetic flux density B 10KA/m(T) | Coercive force (A/m) | Iron loss * (W/kg) | Resistivity (μ Ω m) | ||||
| Method of the present invention | 71 | 60 | Have | 1.30 | 95 | 46 | 25000 |
| 72 | 150 | Have | 1.32 | 90 | 41 | 24000 | |
| 73 | 300 | Have | 1.35 | 80 | 39 | 20000 | |
| Existing method 11 | 150 | Do not have | 1.32 | 130 | 9700 | 150 | |
Iron loss
*Iron loss during expression magnetic flux density 1.0T frequency 200Hz.
Make the composite soft magnetic material by the inventive method as can be known and have as inferior characteristic, it compares the magnetic flux density height with the composite soft magnetic material of making according to existing method 11, coercive force is little, resistivity is especially high in addition, so iron loss is especially little, and particularly the big more iron loss of frequency is more little.
Embodiment 16
As material powder, preparing to have granularity shown in the table 26 and contain Si is 3 quality %, and the Fe-Si that surplus is made of Fe and unavoidable impurities is an iron-based soft magnetic powder.Preparing average grain diameter in addition is that 1 μ m following pure Si powder and average grain diameter are the Mg powder of 50 μ m.
Different Fe-Si is in the iron-based soft magnetic powder in these granularities, with Fe-Si is iron-based soft magnetic powder: pure Si powder=99.5 quality %: the mode of 0.5 quality % is allocated pure Si powder, and the mixed mixed-powder that makes in addition, with the mixed-powder that obtains in nitrogen atmosphere, heat-treat with the condition that 950 ℃ temperature kept 1 hour, be that the iron-based soft magnetic powder surface forms high concentration Si diffusion layer at Fe-Si thus, thereafter in atmosphere, 220 ℃ temperature conditions keeps down, and being produced on the surface oxidation Fe-Si that has oxide layer on the high concentration Si diffusion layer thus is the iron-base soft magnetic material powder.
For this surface oxidation Fe-Si is that the iron-base soft magnetic material powder is implemented Mg lining processing, the accumulation oxide-film lining Fe-Si that the surface that is produced on Fe-Si thus and is iron-based soft magnetic powder is formed with the accumulation oxide-film that is made of Mg, Si, Fe and O is an iron-based soft magnetic powder, thereby has implemented the inventive method 74～76.
For the accumulation oxide-film lining Fe-Si that obtains by the inventive method 74～76 is iron-based soft magnetic powder, add silicones and mix in proportioning 2 quality %, make being covered by silicones that to pile up oxide-film lining Fe-Si be the resin-coated composite powder on the surface of iron-based soft magnetic powder.This resin-coated composite powder is put into the metal pattern extrusion molding that is heated to 120 ℃, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in a vacuum, calcine with the condition that 700 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 3, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 0.1T, iron loss during frequency 20Hz, these results are presented in the table 26.
Conventional example 14
As material powder, preparation has granularity shown in the table 26 and contains Si is 1 quality %, the Fe-Si that surplus is made of Fe and unavoidable impurities is an iron-based soft magnetic powder, to this Fe-Si is that iron-based soft magnetic powder does not carry out Mg lining processing, but add silicones and mixing in proportioning 2 quality %, making by silicones lining Fe-Si is the resin-coated composite powder on the surface of iron-based soft magnetic powder.This resin-coated composite powder is put into the metal pattern extrusion molding that is heated to 120 ℃, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, with the press-powder body that obtains in a vacuum, calcine with the condition that 700 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 25, the composite soft magnetic material that the ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 0.1T, iron loss during frequency 20Hz, these results are presented in the table 26.
[26]
| Species | The average grain diameter of Fe-1%Si raw material powder (μ m) | The Mg processing that is covered | Magnetic characteristic | ||||
| Magnetic flux density B 10KA/m(T) | Coercive force (A/m) | Iron loss * (W/kg) | Resistivity (μ Ω m) | ||||
| Method of the present invention | 74 | 60 | Have | 1.42 | 100 | 55 | 21000 |
| 75 | 150 | Have | 1.43 | 97 | 52 | 20000 | |
| 76 | 300 | Have | 1.47 | 83 | 47 | 17000 | |
| Existing | 150 | Do not have | 1.43 | 140 | 9900 | 150 | |
Iron loss
*Iron loss during expression magnetic flux density 1.0T frequency 200Hz.
Make the composite soft magnetic material according to the inventive method 74～76 as can be known and have as inferior characteristic, it compares the magnetic flux density height with the composite soft magnetic material of making according to existing method 12, coercive force is little, resistivity is especially high in addition, so iron loss is especially little, and particularly the big more iron loss of frequency is more little.
Embodiment 17
As material powder, prepare to have the Fe of granularity shown in the table 27 powder.Preparing average grain diameter in addition is that 1 μ m following pure Si powder and average grain diameter are the Mg powder of 50 μ m.
In the different Fe powder of these granularities, with the Fe powder: pure Si powder=97 quality %: the mode of 3 quality % is allocated pure Si powder, and the mixed mixed-powder that makes in addition, with the mixed-powder that obtains in nitrogen atmosphere, heat-treat with the condition that 950 ℃ temperature kept 1 hour, be that the iron-based soft magnetic powder surface forms high concentration Si diffusion layer at Fe-Si thus, thereafter in atmosphere, temperature is to keep under 220 ℃ the condition, being produced on the surface oxidation Fe-Si that has oxide layer on the high concentration Si diffusion layer thus is the iron-base soft magnetic material powder.
For this surface oxidation Fe-Si is that the iron-base soft magnetic material powder is implemented Mg lining processing, the accumulation oxide-film lining Fe-Si that the surface that is produced on Fe-Si thus and is iron-based soft magnetic powder is formed with the accumulation oxide-film that is made of Mg, Si, Fe and O is an iron-based soft magnetic powder, thereby has implemented the inventive method 77～79.
For the accumulation oxide-film lining Fe-Si that obtains by the inventive method 77～79 is iron-based soft magnetic powder, add silicones and mix in proportioning 2 quality %, make being covered by silicones that to pile up oxide-film lining Fe-Si be the resin-coated composite powder on the surface of iron-based soft magnetic powder.This resin-coated composite powder is put into the metal pattern extrusion molding that is heated to 120 ℃, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, has external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, and has external diameter a: 50mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 25mm, with the press-powder body that obtains in a vacuum, calcine with the condition that 700 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 27, in addition the composite soft magnetic material that is made of path ring-type calcined body is implemented coiling, measure magnetic flux density, coercive force, with magnetic flux density 0.1T, iron loss during frequency 20Hz, these results are presented in the table 27.
This path ring-type press-powder calcined body is measured inductance (inductance) under the 20kHz of 20A direct current when overlapping, try to achieve the permeability of interchange, its result is presented in the table 28.Then, big external diameter ring-type press-powder calcined body is implemented coiling, make inductance and be roughly constant reactor (reactor).Connect this reactor on the Switching Power Supply of subsidiary general active filter (active filter), measure the efficient (%) of input electric power 1000W and the pairing output power of 1500W, its result is presented in the table 28.
Conventional example 15
As material powder, prepare to have the Fe of granularity shown in the table 4 powder, this Fe powder is not carried out the Mg lining handle, also mix but add silicones in proportioning 2 quality %, make resin-coated composite powder by the surface of silicones lining Fe powder.This resin-coated composite powder is put into the metal pattern extrusion molding that is heated to 120 ℃, be configured as have vertical: 55mm; Horizontal: 10mm, thick: the tabular press-powder body of the such size of 5mm, with have external diameter: 35mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 5mm, and has external diameter a: 50mm, internal diameter: 25mm, high: the annular press-powder body of the such size of 25mm, with the press-powder body that obtains in a vacuum, calcine with the condition that 700 ℃ temperature kept 30 minutes, making is by composite soft magnetic material tabular and that the ring-type calcined body constitutes, measure the resistivity of the composite soft magnetic material of tabular thus calcined body formation, its result is presented in the table 27, the composite soft magnetic material that path ring-type calcined body is constituted is implemented coiling in addition, measure magnetic flux density, coercive force, with magnetic flux density 0.1T, iron loss during frequency 20Hz, these results are presented in the table 27.
This path ring-type press-powder calcined body is measured inductance (inductance) under the 20kHz of 20A direct current when overlapping, try to achieve the permeability of interchange, its result is presented in the table 28.Then, big external diameter ring-type press-powder calcined body is implemented coiling, make inductance and be roughly constant reactor (reactor).Connect this reactor on the Switching Power Supply of subsidiary general active filter (active filter), measure the efficient (%) of input electric power 1000W and the pairing output power of 1500W, its result is presented in the table 28.
[27]
| Species | The average grain diameter of Fe raw material powder (μ m) | The Mg processing that is covered | Magnetic characteristic | ||||
| Magnetic flux density B 10KA/m(T) | Coercive force (A/m) | Iron loss * (W/kg) | Resistivity (μ Ω m) | ||||
| Method of the present invention | 77 | 80 | Have | 1.50 | 115 | 62 | 18000 |
| 78 | 150 | Have | 1.52 | 100 | 68 | 15000 | |
| 79 | 300 | Have | 1.55 | 90 | 75 | 12000 | |
| Conventional example 13 | 150 | Do not have | 1.51 | 150 | 1000 | 80 | |
Iron loss
*Iron loss during expression magnetic flux density 1.0T frequency 200Hz.
[28]
| Species | Magnetic flux density B10K (T) | Coercive force (A/m) | Iron loss W1/10k (W/kg) | Permeability 20A 20kHz | Switching Power Supply | |
| Input electric power (W) | Efficient (%) | |||||
| Embodiment 18 | 1.55 | 90 | 17 | 32 | 1000 | 92.7 |
| 1500 | 91.9 | |||||
| Conventional example 16 | 1.51 | 150 | 30 | 28 | 1000 | 89.0 |
| 1500 | 88.0 | |||||
Make the composite soft magnetic material according to the inventive method 77～79 as can be known and have as inferior characteristic, it compares the magnetic flux density height with the composite soft magnetic material of making according to existing method 13, coercive force is little, resistivity is especially high in addition, so iron loss is especially little, and particularly the big more iron loss of frequency is more little.
The industrial possibility of utilizing
Adopted the composite soft magnetic material with high impedance that contains Mg oxide-film coating soft magnetic metal powder made from method of the present invention, feature with high magnetic flux density, the low iron loss of high frequency thus can be as the materials'use of the various electromagnetic circuit elements that produce this feature. Described electromagnetic circuit element has such as magnetic core, electric core, generator magnetic core, solenoid core, ignition coil iron core, reactor core, transformer core, choking-winding iron core or Magnetic Sensor magnetic core etc. And, in the electrical equipment of having assembled these electromagnetic circuit elements, motor, generator, solenoid, injector (injector), Electromagnetically driven valve, inverter, current transformer, relay, magnetic sensor-based system etc. are arranged, can carry out high efficiency high performance and the miniaturization and of electrical equipment.
As aforementioned, make the composite soft magnetic material if use the Mg oxide-film coating soft magnetic metal powder that contains made from method of the present invention, then can obtain with low cost the composite soft magnetic material of resistivity and mechanicalness excellent strength, have excellent effect in electric and electronic industry direction.
If follow the present invention who uses take the SiO powder as material powder, then can easily contain Mg-Si oxide coating soft magnetic powder with low cost fabrication, therefore use this to contain Mg-Si oxide coating soft magnetic powder, can obtain with low cost the composite soft magnetic material of resistivity height and mechanicalness excellent strength, in addition, this composite soft magnetic material has the feature of high magnetic flux density, the low iron loss of high frequency, thus can be as the materials'use of the various electromagnetic circuit elements that produce this feature. As described various electromagnetic circuit elements, such as magnetic core, electric core, generator magnetic core, solenoid core, ignition coil iron core, reactor core, transformer core, choking-winding iron core or Magnetic Sensor magnetic core etc. are arranged, in the electrical equipment of having assembled these electromagnetic circuit elements, motor, generator, solenoid, injector (injector), Electromagnetically driven valve, inverter, current transformer, relay, magnetic sensor-based system etc. are arranged, thereby can carry out high efficiency high performance and the miniaturization and of electrical equipment.
Claims (21)
1. manufacture method that contains Mg oxide-film lining soft magnetic powder, it is characterized in that, to carry out the soft magnetic metal powder of oxidation processes as material powder, adding the Mg powder and mix in this material powder, is that 150～1100 ℃, pressure are 1 * 10 with the mixed-powder that obtains thus in temperature
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere.
2. a manufacture method that contains Mg oxide-film lining soft magnetic powder is characterized in that, further in oxidizing atmosphere, with 50～400 ℃ temperature, the Mg oxide-film lining soft magnetic powder that contains by the described method manufacturing of claim 1 is heated.
3. a manufacture method that contains Mg oxide-film lining soft magnetic powder is characterized in that the oxidation processes of the described soft magnetic metal powder of claim 1 is in oxidizing atmosphere, with 50～500 ℃ temperature soft magnetic metal powder is carried out heat treated.
4. one kind contains Mg oxide-film lining soft magnetic metal powder production of raw material for use powder, it is characterized in that, soft magnetic metal powder is carried out oxidation processes form.
5. a manufacture method that contains Mg oxide-film lining soft magnetic powder is characterized in that, in soft magnetic metal powder, add the Mg powder and mixed, and be that 150～1100 ℃, pressure are 1 * 10 with the mixed-powder that obtains thus in temperature
-12～1 * 10
-1Heat in the inert gas atmosphere of MPa or the vacuum atmosphere, then in oxidizing atmosphere, implement the oxidation processes that heats with 50～400 ℃ temperature.
6. manufacture method that contains Mg-Si oxide lining soft magnetic powder, it is characterized in that, be formed with in the oxide lining soft magnetic powder of oxide-film on the surface of soft magnetic powder, add the silicon monoxide powder and mix the back heating, perhaps while mixing in vacuum atmosphere being that the condition of 600～1200 ℃ of maintenances heats in temperature, further add the Mg powder and mix the back heating, while or mix in vacuum atmosphere being that the condition of 400～800 ℃ of maintenances heats in temperature.
7. manufacture method that contains Mg-Si oxide lining soft magnetic powder, it is characterized in that, be formed with in the oxide lining soft magnetic powder of oxide-film on the surface of soft magnetic powder, add silicon monoxide powder and Mg powder and mix the back heating, while perhaps mix in vacuum atmosphere being that the condition of 400～1200 ℃ of maintenances heats in temperature.
8. manufacture method that contains Mg-Si oxide lining soft magnetic powder, it is characterized in that, in the surface of soft magnetic powder is formed with the oxide lining soft magnetic powder of oxide-film, adds the Mg powder and mix the back heating, perhaps while mixing in vacuum atmosphere serving as to keep the condition of 400～800 ℃ of maintenances to heat in temperature, further add the silicon monoxide powder and mix the back heating, while perhaps mix in vacuum atmosphere being to heat under the condition of 600～1200 ℃ of maintenances in temperature.
9. according to claim 6,7, the 8 described manufacture methods that contain Mg--Si oxide lining soft magnetic powder, it is characterized in that the oxide lining soft magnetic powder that the surface of described soft magnetic powder is formed with oxide is to remain in room temperature～500 and ℃ make by soft magnetic powder is heated in oxidizing atmosphere.
10. according to claim 6,7,8, the 9 described manufacture methods that contain Mg-Si oxide lining soft magnetic powder, it is characterized in that, the addition of described silicon monoxide powder is in the scope of 0.01～1 quality %, and the addition of described Mg powder is in the scope of 0.05～1 quality %.
11., it is characterized in that described vacuum atmosphere is a pressure: 1 * 10 according to claim 6,7,8,9, the 10 described manufacture methods that contain Mg-Si oxide lining soft magnetic powder
-12～1 * 10
-1The vacuum atmosphere of MPa.
12. one kind contains Mg-Si oxide lining soft magnetic powder production of raw material for use powder, it is characterized in that the oxide lining soft magnetic powder that is formed with oxide-film by the surface at soft magnetic powder constitutes.
13. a manufacture method that contains Mg oxide-film lining soft magnetic metal powder is characterized in that, while the heating in claim 1,5,6,7,8 described vacuum or the inert gas atmosphere is to rotate to heat.
14. according to claim 1,5,6,7, the 8 described manufacture methods that contain Mg oxide-film lining soft magnetic metal powder, it is characterized in that described soft magnetic metal powder is that iron powder, insulation processing iron powder, Fe-Al are that iron-base soft magnetic alloy powder, Fe-Ni are that iron-base soft magnetic alloy powder, Fe-Cr are that iron-base soft magnetic alloy powder, Fe-Si are that iron-base soft magnetic alloy powder, Fe-Si-Al are that iron-base soft magnetic alloy powder, Fe-Co are that iron-base soft magnetic alloy powder, Fe-Co-V are that iron-base soft magnetic alloy powder or Fe-P are the iron-base soft magnetic alloy powder.
15. according to claim 1,5,6,7, the manufacture method of material powder of the soft magnetic metal powder of oxidation processes has been carried out in 8 described conducts, it is characterized in that, Fe-Si be add the Si powder in iron-base soft magnetic alloy powder or the Fe powder and mix after, by in nonoxidizing atmosphere, heating, the Fe-Si that the surface that is produced on Fe-Si thus and is iron-base soft magnetic alloy powder or Fe powder has high concentration Si diffusion layer is the iron-base soft magnetic alloy powder, the described Fe-Si of concentration ratio of the Si that this high concentration Si diffusion layer contains is the concentration height of the contained Si of iron-base soft magnetic alloy powder or Fe powder, to resulting Fe-Si with high concentration Si diffusion layer is that the iron-base soft magnetic alloy powder carries out oxidation processes, and becoming the surface oxidation Fe-Si that has oxide layer on high concentration Si diffusion layer thus is the iron-base soft magnetic material powder.
16. the manufacture method of the composite soft magnetic material of resistivity and mechanicalness excellent strength, it is characterized in that, will according to claim 1,5,6,7,8 described method manufacturings contain Mg oxide-film lining soft magnetic metal powder extrusion molding after, with 400～1300 ℃ temperature calcining.
17. the manufacture method of the composite soft magnetic material of resistivity and mechanicalness excellent strength, it is characterized in that, asking the containing in the Mg oxide-film lining soft magnetic metal powder of 1,5,6,7,8 described method manufacturings according to right, the composite material that mixes organic insulation, inorganic insulating material or organic insulation and inorganic insulating material carries out press-powder afterwards and is shaped, and calcines at 500～1000 ℃.
18. the soft magnetism material of resistivity and mechanicalness excellent strength is characterized in that, according to claim 16,17 described method manufacturings.
19. an electromagnetic circuit element is characterized in that, is made of the described composite soft magnetic material of claim 18.
20. described electromagnetic circuit element of claim 19, it is characterized in that described electromagnetic circuit element is magnetic core, electric core, generator magnetic core, solenoid core, ignition coil iron core, reactor core, transformer core, choke coil iron core or Magnetic Sensor magnetic core.
21. an electrical equipment is characterized in that, is assembled with the described electromagnetic circuit element of claim 20.
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| JP2004257841 | 2004-09-06 | ||
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| JP158894/2005 | 2005-05-31 | ||
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