CN1863629A - Fe-Ni-Mo flaky metal soft magnetic powder and magnetic composite material containing soft magnetic powder - Google Patents
Fe-Ni-Mo flaky metal soft magnetic powder and magnetic composite material containing soft magnetic powder Download PDFInfo
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Abstract
The invention provides an Fe-Ni-Mo soft magnetic flaky powder having a component composition of, in percent by mass, Ni: 60 to 90%, Mo: 0.05 to 1.95 %, and the balance of Fe and unavoidable impurities, and a flat surface of an average particle size of 30 to 150 m, and an aspect ratio (average particle size /average thickness) of 5 to 500; and having a peak intensity ratio I 200 I 111 within a range between 0.43 and 10, where I 200 is the peak height of the face index (200) and I 111 is the peak height of the face index (111), in an X-ray diffraction pattern measured in such a manner that the plane including the X-ray incident direction and the diffraction direction is perpendicular to the flat surface of the soft magnetic flaky powder, and the angle between the incident direction and the flat surface is equal to the angle between the diffraction direction and the flat surface. Furthermore, the invention provides a soft magnetic flaky powder with oxide layer wherein an oxide layer of a thickness of 50 to 1000 AA is formed on the surface of this soft magnetic flaky powder.
Description
Technical field
The present invention relates to be used for the wave absorber that has excellent electric wave absorption characteristic under tens of MHz～number GHz or the radio communication that under tens of kHz～tens of MHz, has an excellent magnetic characteristic with magnetic material for high frequency wave such as antenna core, Fe-Ni-Mo is the flat metal soft magnetic powder.In addition, the present invention relates in resin directed, to have disperseed above-mentioned Fe-Ni-Mo be the magnetic composite of flat metal soft magnetic powder, particularly magnetic composite sheet.
Japanese Patent Application 2003-358970 number of filing an application of the present patent application, file an application on February 18th, 2004 Japanese Patent Application 2004-41029 number to Japanese Patent Application 2003-205956 number of filing an application, on October 20th, 2003 on August 5th, 2003, and Japanese Patent Application 2004-217371 number of filing an application on July 26th, 2004 require priority, quote its content here.
Background technology
Usually, as the high magnetic permeability soft magnetic material of melting material, agglomerated material, known permalloy A (Fe-70～80%Ni) (% represents quality %, below identical).Slow cooling after this material enforcement heat treatment just generates FeNi
3Ordered phase, crystal magnetic anisotropy constant K
1For negative, its absolute value is big value.Known, at crystal magnetic anisotropy constant K
1Be negative occasion,＜111〉direction become direction of easy axis and＜100〉direction become hard direction, be positive occasion at this constant,＜100〉direction become direction of easy axis and＜111〉direction become hard direction, at this constant is zero occasion, just becomes magnetic isotropy.By generating this FeNi
3Ordered phase produces magnetic anisotropy, its result, and crystal face is not directed, and in the common polycrystal of crystal orientation isotropy, magnetic conductivity reduces.In this material, in order to obtain high magnetic conductivity, chilling after the high-temperature heat treatment perhaps also further needs Ageing Treatment thereafter, but does not industrially use basically.
In addition, also known Mo permalloy (Fe-79%Ni-4%Mo) and the malloy (Fe-79%Ni-5%Mo) that in above-mentioned permalloy, has added Mo.These materials are by adding Mo, even slow cooling after heat treatment has also suppressed FeNi
3The generation of ordered phase is not even implement chilling after the heat treatment, crystal magnetic anisotropy constant K
1Also about vanishing, in the polycrystal of crystal orientation isotropy, also demonstrate excellent magnetic conductivity, therefore be widely used industrial.Also known in addition, outside Mo, also added the high magnetic permeability soft magnetic material of Cu, Cr, Mn in order further to improve magnetic conductivity.
On the other hand, also known powder flattening that will have same composition of people etc. and the flat metal soft magnetic powder that obtains.For example, known composition with Fe-70～83%Ni-2～6%Mo-3～6%Cu-1～2Mo has average grain diameter: 0.1～30 μ m, average thickness: the flat metal soft magnetic powder that 2 μ m are following.This flat metal soft magnetic powder for example uses (opening flat 3-223401 communique with reference to the spy) as magnetic card with the flat metal soft magnetic powder.
In addition, also known flat flakey soft magnetic powder with composition of Fe-40～80%Ni-2～6%Mo.This flat flakey soft magnetic powder for example uses (opening flat 3-232574 communique with reference to the spy) as the magnetic mark with soft magnetic powder.
Known flat metal soft magnetic powder with composition of Fe-60～80%Ni or the following Mo of Fe-60～80%Ni-5% is arranged again.This flat metal soft magnetic powder for example uses (opening flat 4-78112 communique with reference to the spy) as high frequency with magnetic core.
These existing Fe-Ni-Mo are the flat metal soft magnetic powder, all be to make common pulverizing or atomizing and the Fe-Ni-Mo that obtains is the flat that is shaped as of powder, make it to embody the shape magnetic anisotropy of counter magnetic field, make to be the easy magnetization face in the flat horizontal surface, further improve the interior magnetic characteristics such as magnetic conductivity of flat horizontal surface of powder thus.
These existing Fe-Ni-Mo are the flat metal soft magnetic powder, all be that the Fe-Ni-Mo that obtains in common pulverizing or atomizing is ethanol or the water that adds in the powder as solvent, add grinding aid more as required, create thereby use vertical ball mill or ball mill to carry out the flattening processing it.
By the Fe-Ni-Mo that makes such manufacturing is that the flat metal soft magnetic powder is scattered in the resin, and makes the flat horizontal surface orientation, thereby makes magnetic composite.This magnetic composite is the occasion of magnetic composite sheet, and above-mentioned Fe-Ni-Mo is that the flat horizontal surface of flat metal soft magnetic powder is in the direction orientation vertical with magnetic composite sheet thickness direction.
; these existing Fe-Ni-Mo are the flat metal soft magnetic powder, as can not get enough characteristics at wave absorber that has the electric wave absorption characteristic under tens of MHz～number GHz or the radio communication that has magnetic characteristic under tens of kHz～tens of MHz with magnetic material for high frequency wave such as antenna cores.In addition, the more excellent flat metal soft magnetic powder of magnetic conductivity in the demand flat horizontal surface.
Summary of the invention
The inventor is that the Fe-Ni-Mo of the more excellent characteristic of flat metal soft magnetic powder is a flat metal soft magnetic powder and studying in order to obtain having than existing Fe-Ni-Mo as wave absorber or magnetic material for high frequency wave, and the result obtains following knowledge opinion.
(a) to contain Fe-Ni-Mo that one-tenth that Ni:60～90%, Mo:0.05～1.95%, surplus comprises Fe and unavoidable impurities is grouped into be that metal soft magnetic powder is when using vertical ball mill or ball mill flattening to handle with the higher solvent of viscosity when having, the impact that powder is applied is relaxed, the effect of the pulverizing of carrying out simultaneously with flattening is suppressed, in view of the above, obtaining thin thickness and big Fe-Ni-Mo is the flat metal soft magnetic powder.In addition, the Fe-Ni-Mo that obtains like this is the flat metal soft magnetic powder, so that comprise the flat horizontal surface of the plane of the incident direction of X ray and diffraction direction perpendicular to above-mentioned flat metal soft magnetic powder, and in the X-ray diffractogram that the mode that angle that incident direction and flat horizontal surface constitute and diffraction direction are equated with the angle of flat horizontal surface formation is measured, the peak height of the indices of crystallographic plane (200) is designated as I
200, the peak height of the indices of crystallographic plane (111) is designated as I
111The time, peak intensity compares I
200/ I
111In 0.43～10 scope.In addition, peak intensity compares I
200/ I
111Fe-Ni-Mo in 0.43～10 scope is the flat metal soft magnetic powder, the imaginary part of complex permeability demonstrates high value under tens of MHz～number GHz, therefore demonstrate excellent characteristic as the wave absorber that under this frequency band, has the electric wave absorption characteristic with powder, in addition, the real part of complex permeability demonstrates high value under tens of kHz～tens of MHz, therefore demonstrates excellent characteristic as the radio communication that has soft magnetic characteristic under this frequency band with magnetic material for high frequency wave such as antenna cores.
(b) be in the flat metal soft magnetic powder at this Fe-Ni-Mo, by average grain diameter is defined as 30～150 μ m, aspect ratio (average grain diameter/average thickness) is defined as 5～500, the magnetic conductivity in the flat horizontal surface further improves.
The present invention is based on that these knowledge opinions finish, and it relates to following content:
(1) a kind of Fe-Ni-Mo is the flat metal soft magnetic powder, it is to have the Ni:60 of containing～90%, Mo:0.05～1.95%, the one-tenth that surplus comprises Fe and unavoidable impurities is grouped into, and the flat metal soft magnetic powder of the size and dimension of average grain diameter 30～150 μ m and aspect ratio 5～500, it is characterized in that, so that comprise the flat horizontal surface of the plane of the incident direction of X ray and diffraction direction perpendicular to above-mentioned flat metal soft magnetic powder, and in the X-ray diffractogram that the mode that angle that incident direction and flat horizontal surface constitute and diffraction direction are equated with the angle of flat horizontal surface formation is measured, the peak height of the indices of crystallographic plane (200) is designated as I
200, the peak height of the indices of crystallographic plane (111) is designated as I
111The time, peak intensity compares I
200/ I
111In 0.43～10 scope.
Fe-Ni-Mo of the present invention is the flat metal soft magnetic powder, mainly makes it to disperse and make the flat horizontal surface orientation in resin, to use as magnetic composite, particularly magnetic composite sheet.Under the situation of magnetic composite sheet, above-mentioned Fe-Ni-Mo is that the flat horizontal surface of flat metal soft magnetic powder is in the direction orientation vertical with magnetic composite sheet thickness direction.Therefore, the present invention is:
(2) a kind of magnetic composite, wherein, above-mentioned (1) described Fe-Ni-Mo is that the flat horizontal surface of flat metal soft magnetic powder is directed and be scattered here and there in resin.
(3) a kind of magnetic composite sheet, its (2) described magnetic composite that is above-mentioned, above-mentioned Fe-Ni-Mo are that the flat horizontal surface of flat metal soft magnetic powder is directed and be scattered here and there in the direction vertical with magnetic composite sheet thickness direction.
Above-mentioned (1) described Fe-Ni-Mo is that the flat metal soft magnetic powder disperses and make above-mentioned (2) described magnetic composite or above-mentioned (3) described magnetic composite sheet of its flat horizontal surface orientation to have excellent characteristic as wave absorber or radio communication with magnetic material for high frequency wave such as antenna cores in resin.; Fe-Ni-Mo is the flat metal soft magnetic powder; because having the one-tenth that is difficult to generate oxide-film on the surface is grouped into; even therefore be that the flat metal soft magnetic powder is placed in atmosphere for a long time with this Fe-Ni-Mo; Fe-Ni-Mo is that the thickness of the oxide-film that forms from the teeth outwards of flat metal soft magnetic powder is also less than 50 ; when making this Fe-Ni-Mo with thin oxide-film is that the flat metal soft magnetic powder is when disperseing with high density in resin; Fe-Ni-Mo is that the flat metal soft magnetic powder adjoins each other; its result; Fe-Ni-Mo is the dispersion amount high density of flat metal soft magnetic powder, and the resistivity of magnetic composite that obtains or magnetic composite sheet descends more.
Therefore, the resistivity deficiency of magnetic composite or magnetic composite sheet needs to have the magnetic composite or the magnetic composite sheet of higher resistivity sometimes.In order to satisfy this requirement, be that the surface of flat metal soft magnetic powder forms thicker oxide-film (50～1000 ) and necessitates at above-mentioned (1) described Fe-Ni-Mo.The oxide-film that this thickness is thicker, can by with above-mentioned (1) described Fe-Ni-Mo be the flat metal soft magnetic powder in oxidizing atmosphere, heat or in warm water heating back drying make.Therefore, the present invention is:
(4) a kind of Fe-Ni-Mo is the flat metal soft magnetic powder of lining oxide-film, it is to have the Ni:60 of containing～90%, Mo:0.05～1.95%, the one-tenth that surplus comprises Fe and unavoidable impurities is grouped into, and the surface of the flat metal soft magnetic powder of the flat horizontal surface of average grain diameter 30～150 μ m and aspect ratio (average grain diameter/average thickness) 5～500, formed the flat metal soft magnetic powder of lining oxide-film of the oxide-film of thickness 50～1000 , so that comprise the flat horizontal surface of the plane of the incident direction of X ray and diffraction direction perpendicular to the flat metal soft magnetic powder of above-mentioned lining oxide-film, and in the X-ray diffractogram that the mode that angle that incident direction and flat horizontal surface constitute and diffraction direction are equated with the angle of flat horizontal surface formation is measured, the peak height of the indices of crystallographic plane (200) is designated as I
200, the peak height of the indices of crystallographic plane (111) is designated as I
111The time, peak intensity compares I
200/ I
111In 0.43～10 scope.
(5) a kind of magnetic composite, wherein, the flat horizontal surface of the flat metal soft magnetic powder of above-mentioned (4) described Fe-Ni-Mo system lining oxide-film is directed and be scattered here and there in resin.
(6) a kind of magnetic composite sheet, its (5) described magnetic composite that is above-mentioned, the flat horizontal surface of the flat metal soft magnetic powder of above-mentioned Fe-Ni-Mo system lining oxide-film are directed and be scattered here and there in the direction vertical with magnetic composite sheet thickness direction.
The flat metal soft magnetic powder of above-mentioned in order to make (4) described Fe-Ni-Mo system lining oxide-film, with above-mentioned (1) described Fe-Ni-Mo is that the flat metal soft magnetic powder heats under the following conditions and gets final product: in atmosphere or contain in the medium oxidizing atmosphere of oxygen gas mixture atmosphere, kept 1 minute～24 hours under 300～600 ℃ temperature.Perhaps, heating is after 1 minute～96 hours in 50～100 ℃ warm water, and drying gets final product under 50～200 ℃.
The oxide thickness of the flat metal soft magnetic powder of above-mentioned (4) of the present invention described Fe-Ni-Mo system lining oxide-film is during less than 50 , as the composite magnetic sheet, the resistivity deficiency, so it is not preferred, when surpassing 1000 , because coercive force increases, so as the composite magnetic sheet, the electric wave absorption characteristic reduces, so not preferred.Therefore, the lower thickness limit of this oxide-film is decided to be 50 , on be defined as 1000 .
In addition, the resin that uses in magnetic composite of the present invention and magnetic composite sheet is that haloflex, polysiloxanes, polyurethane, vinyl acetate, vinyl-vinyl acetate copolymer, ABS resin, vinyl chloride, polyvinyl butyral resin, thermoplastic elastomer (TPE), EM-PM-BD copolymer rubber, styrene-butadiene are that rubber, acrylonitrile-butadiene are rubber etc.In addition, the material of these resins that can be fusion also or with these resin fusion modifications material.
Fe-Ni-Mo of the present invention is the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film, because the maximum of the real part of the complex permeability under 30kHz～30MHz is big, the high-frequency magnetic material that therefore excellence can be provided is to use as antenna, inductor.Have again,, therefore can provide wave absorber with excellent electric wave absorption characteristic because the maximum of the imaginary part of the complex permeability under 30MHz～3GHz is big.Its result brings excellent effect on the Electrical and Electronic industry.
Below be the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film to Fe-Ni-Mo of the present invention, determinant composition, average grain diameter, the reason of peak intensity ratio when in length and breadth are described as described above.
One-tenth is grouped into:
At Fe-Ni-Mo of the present invention is in the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film, and it is because no matter less than 60% still greater than 90%, magnetic characteristic all reduces that Ni content is defined as 60～90% reason.This scope is usually known scope, but is Ni content in the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film at Fe-Ni-Mo of the present invention, and is further preferred in 70～85% scope.
In addition, with Mo content be defined as 0.05～1.95% reason be because: when Mo less than 0.05% the time, by the slow cooling after the heat treatment, the FeNi of generation
3The ordered phase surplus, crystal magnetic anisotropy constant K
1For negative, its absolute value is excessive, and magnetic characteristic reduces, thus not preferred, when content greater than 1.95% the time, the FeNi of generation
3Ordered phase is not enough, crystal magnetic anisotropy constant K
1For negative and its absolute value is too small, or just become, because the crystal magnetic anisotropy, make in the flat horizontal surface to the effect of easy magnetization face more insufficiently, the magnetic characteristic in the flat horizontal surface reduces, so not preferred.At Fe-Ni-Mo of the present invention is in the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film, and the further preferred range of Mo content is 0.5～1.95% (most preferably 0.8～1.9%).
Average grain diameter:
At Fe-Ni-Mo of the present invention is in the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film, when average grain diameter during less than 30 μ m, the importing of the strain when flattening is handled becomes remarkable, even implement heat treatment in the temperature more than 500 ℃, also can not get enough magnetic characteristics, so not preferred.On the other hand, when average grain diameter surpasses 150 μ m, when making sheet, with mixing process such as resin in, powder warpage, or broken, magnetic characteristic reduces, so not preferred.Therefore, the average grain diameter of the flat metal soft magnetic powder of flat metal soft magnetic powder of the present invention and Fe-Ni-Mo system lining oxide-film is defined as 30～150 μ m.The further preferred range of average grain diameter is 35～140 μ m.
Aspect ratio:
At Fe-Ni-Mo of the present invention is in the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film, when aspect ratio less than 5 the time, it is big that the demagnetized field of powder becomes, the magnetic conductivity in the flat horizontal surface reduces, so not preferred.On the other hand, when aspect ratio greater than 500 the time, the importing of the strain when flattening is handled becomes significantly, even in the enforcement of the temperature more than 500 ℃ heat treatment, also can not get enough magnetic characteristics, so not preferred.Therefore, Fe-Ni-Mo of the present invention is that the aspect ratio of the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film is defined as 5～500.
The peak intensity ratio:
When to be metal soft magnetic powder with Fe-Ni-Mo with the higher solvent of viscosity used vertical ball mill or ball mill flattening to handle, (100) crystal face of face-centered cubic (fcc) lattice and the flat horizontal surface of powder be orientation abreast.; so that comprise the flat horizontal surface of the plane of the incident direction of X ray and diffraction direction perpendicular to above-mentioned flat metal soft magnetic powder; and in the X-ray diffractogram that the mode that angle that incident direction and flat horizontal surface constitute and diffraction direction are equated with the angle of flat horizontal surface formation is measured; the peak of the indices of crystallographic plane (100); decay rule according to the diffraction maximum of face-centered cubic (fcc) lattice only observes by FeNi
3Ordered phase generates and the small peak of generation, and in addition, the height at this peak is subjected to FeNi
3The influence of the growing amount of ordered phase.Therefore, in the present invention,, be the secondary diffraction maximum of (100) crystal face, and measure and be not subjected to FeNi as the directed abreast index of the flat horizontal surface of (100) crystal face of fcc lattice and powder
3Ordered phase generates the peak height I of the indices of crystallographic plane (200) of influence
200, obtain peak height I with the indices of crystallographic plane (111) of expression maximum peak under the unoriented situation of crystal orientation
111Peak intensity compare I
200/ I
111At Fe-Ni-Mo of the present invention is in the flat metal soft magnetic powder, I
200/ I
111Determine that in 0.43～10 scope, its reason is: when less than 0.43 the time, because the crystal magnetic anisotropy, make in the flat horizontal surface to the effect of easy magnetization face more insufficiently, the magnetic characteristic in the flat horizontal surface reduces, so not preferred.When greater than 10 the time, make in industrial being difficult to.The further preferred range of peak intensity is 0.50～10, and most preferred scope is 0.60～10.
In addition, the coefficient of viscosity of solvent that use, that viscosity is higher when to make Fe-Ni-Mo of the present invention be the flat metal soft magnetic powder of flat metal soft magnetic powder and Fe-Ni-Mo system lining oxide-film, under 20 ℃ preferably in 2～5mPas[milli handkerchief second] scope in.When the coefficient of viscosity of the solvent that adds when adopting vertical ball mill or ball mill to carry out the flattening processing is lower than 2mPas, mitigation is little to the effect of the impact that the material powder soft magnetic powder applies, when handling, flattening pulverizes, can not get thin thickness and big powder, in addition, (100) the directed abreast effect of the flat horizontal surface of crystal face and powder is insufficient, and the magnetic conductivity of powder reduces as a result, so not preferred.On the other hand, when the coefficient of viscosity of solvent is higher than 5mPas, the efficient that flattening is handled significantly reduces, or after flattening is handled, take out when having mixed the slurry of powder and solvent, the valve of conveying end stops up, or stop up for further improving the slurry EGR that uniformity that flattening handles is provided with, so not preferred.
As the high solvent of this coefficient of viscosity, can use isobutyl alcohol (coefficient of viscosity under 20 ℃: 4.4mPas[milli handkerchief second], below identical, wherein, 1mPas=1cP[centipoise]), isoamyl alcohol (4.4mPas), 1-butanols (3.0mPas), 1-propyl alcohol (2.2mPas), 2-propyl alcohol (2.4mPas) etc., be the higher alcohol of liquid at normal temperatures.In addition, also can be the solvent that in water, ethanol, methyl alcohol, has dissolved at normal temperatures for the higher alcohol of liquid or solid or ethylene glycol, glycerine etc.These have dissolved in water, ethanol, methyl alcohol and have been the solvent of the higher alcohol of liquid or solid or ethylene glycol, glycerine etc. at normal temperatures, and water (1.0mPas), ethanol (1.2mPas), methyl alcohol (0.6mPas) ratio with using in the past demonstrate high coefficient of viscosity.
Description of drawings
Fig. 1 is the X-ray diffractogram of the Cu-K α of flat metal soft magnetic powder 3 of the present invention.
The specific embodiment
Preferred embodiment of the present invention below is described.But the present invention is not limited by each following embodiment, for example can suit to make up the inscape of these embodiment yet.
Embodiment 1
High frequency melted alloy raw material, the fused solution that the one-tenth shown in making table 1～2 is grouped into, these fused solutions of water atomization are made atomized powder, and this atomized powder classification is handled, and have made the atomized feed powder.Have again, as solvent, prepared in ethanol, to have added glycerine: the solvent of the 35 quality % (coefficient of viscosity under 20 ℃: 3.1mPas).
Be added on to this atomized feed powder and contain glycerine in the ethanol: the solvent of 35 quality %, handle with the vertical ball mill flattening, then put it in the heat-treatment furnace, in Ar gas atmosphere, under 500 ℃ of temperature, carried out keeping 2 hours heat treatment.Powder that these are heat treated adopts the air classifier classification, made have that the one-tenth shown in table 1～2 is grouped into, the flat metal soft magnetic powder 1～20 of the present invention of average grain diameter d, average thickness t, aspect ratio (d/t) and flat metal soft magnetic powder 1～8 relatively.
Have again,, prepared the ethanol (coefficient of viscosity under 20 ℃: 1.2mPas) as solvent, add ethanol to above-mentioned atomized feed powder, handle with the vertical ball mill flattening, then put it in the heat-treatment furnace, in Ar gas atmosphere, under 500 ℃ of temperature, carried out keeping 2 hours heat treatment.Powder that these are heat treated adopts the air classifier classification, made have that the one-tenth shown in the table 2 is grouped into, average grain diameter d, average thickness t, aspect ratio (d/t) relatively use flat metal soft magnetic powder (suitable) with goods in the past.
At the flat metal soft magnetic powder 1～20 of the present invention that obtains like this, relatively with flat metal soft magnetic powder 1～8 and mixed chlorinated polyethylene in the flat metal soft magnetic powder in the past: 15 quality % and mixing after, by the roller moulding, made the magnetic composite sheet of flat horizontal surface and the sheet surface thickness that be arranged in parallel, that have 0.5mm of flat metal soft magnetic powder.Then, plane by making the incident direction that comprises X ray and diffraction direction is perpendicular to the sheet surface of this magnetic composite sheet, and the angle that surperficial angle that constitutes of incident direction and sheet and diffraction direction and sheet surface are constituted equates and measures, and obtains the X-ray diffractogram of Cu-K α, calculates peak intensity and compares I
200/ I
111, table 1 and table 2 show its result.
Be reference, Fig. 1 illustrates the X-ray diffractogram of the Cu-K α of flat metal soft magnetic powder 3 of the present invention.As can be known clear and definite by Fig. 1, use vertical ball mill or ball mill flattening to handle and the Fe-Ni-Mo that obtains is in the flat metal soft magnetic powder with the higher solvent of viscosity being metal soft magnetic powder with Fe-Ni-Mo, (100) crystal face of face-centered cubic (fcc) lattice and the flat horizontal surface of powder are directed abreast, but the peak of the indices of crystallographic plane (100) crystal face, decay rule according to the diffraction maximum of face-centered cubic (fcc) lattice, on X-ray diffractogram, almost do not manifest, because FeNi
3The generation of ordered phase only observes a little.The height at this peak is subjected to FeNi
3The influence of the growing amount of ordered phase.Therefore, in the present embodiment, be determined as the secondary diffraction maximum of (100) crystal face and be not subjected to FeNi
3The peak height I of the indices of crystallographic plane of the influence of the generation of ordered phase (200)
200, obtain and the peak height I of the indices of crystallographic plane (111) of expression maximum peak under the unoriented situation of crystal orientation
111Peak intensity compare I
200/ I
111
Have again, cut from these magnetic composite sheet, make sample, utilize impedance measuring device and network analyser to measure the complex permeability of 30kHz～30MHz, 30MHz～3GHz, with the maximum of the real part of the complex permeability of important 30kHz～30MHz, as the maximum of wave absorber with the imaginary part of the complex permeability of important 30MHz～3GHz, table 1 and table 2 show its result to mensuration as antenna, inductor.
Table 1
| The flat pattern metal soft magnetic powder | Become to be grouped into (quality %) | Average grain diameter d (μ m) | Average thickness t (μ m) | Aspect ratio d/t | I 200/I 111 | The real part maximum of the complex permeability under 30kHz～30MHz | The imaginary part maximum of the complex permeability under 30MHz～3GHz | |||
| Ni | Mo | Fe | ||||||||
| The present invention | 1 | 60.7 | 1.52 | Surplus | 61.9 | 0.3 | 206 | 0.44 | 69 | 20 |
| 2 | 65.2 | 0.61 | Surplus | 43.3 | 1.7 | 25 | 1.97 | 68 | 20 | |
| 3 | 70.1 | 1.16 | Surplus | 31.1 | 0.9 | 35 | 1.77 | 76 | 24 | |
| 4 | 74.8 | 0.77 | Surplus | 56.4 | 3.7 | 15 | 4.22 | 66 | 20 | |
| 5 | 75.0 | 1.63 | Surplus | 41.9 | 2.0 | 21 | 9.62 | 72 | 22 | |
| 6 | 77.9 | 0.08 | Surplus | 35.6 | 4.4 | 8.1 | 2.42 | 64 | 20 | |
| 7 | 78.1 | 1.39 | Surplus | 69.8 | 0.6 | 116 | 0.57 | 74 | 23 | |
| 8 | 78.1 | 1.95 | Surplus | 47.2 | 2.7 | 17 | 6.26 | 67 | 20 | |
| 9 | 80.0 | 0.94 | Surplus | 58.7 | 0.2 | 294 | 0.73 | 81 | 25 | |
| 10 | 80.2 | 1.43 | Surplus | 64.6 | 1.4 | 46 | 2.79 | 74 | 23 | |
| 11 | 79.9 | 1.74 | Surplus | 32.3 | 0.9 | 36 | 1.43 | 65 | 20 | |
| 12 | 81.8 | 0.43 | Surplus | 48.8 | 0.1 | 488 | 0.66 | 62 | 19 | |
| 13 | 82.1 | 1.38 | Surplus | 51.2 | 1.1 | 47 | 3.66 | 71 | 22 | |
| 14 | 82.2 | 1.83 | Surplus | 66.5 | 0.2 | 333 | 0.98 | 80 | 24 | |
| 15 | 85.0 | 0.95 | Surplus | 34.3 | 0.6 | 57 | 1.24 | 77 | 23 | |
Table 2
| The flat pattern metal soft magnetic powder | Become to be grouped into (quality %) | Average grain diameter d (μ m) | Average thickness t (μ m) | Aspect ratio d/t | I 200/I 111 | The real part maximum of the complex permeability under 30kHz～30MHz | The imaginary part maximum of the complex permeability under 30MH2～3GHz | |||
| Ni | Mo | Fe | ||||||||
| The present invention | 16 | 84.9 | 1.72 | Surplus | 40.5 | 7.1 | 5.7 | 1.83 | 73 | 22 |
| 17 | 89.9 | 1.12 | Surplus | 37.6 | 1.7 | 22 | 0.85 | 65 | 20 | |
| 18 | 80.5 | 1.06 | Surplus | 78.4 | 4.3 | 18 | 0.78 | 78 | 24 | |
| 19 | 79.7 | 1.95 | Surplus | 88.7 | 3.6 | 25 | 1.15 | 75 | 22 | |
| 20 | 80.2 | 1.88 | Surplus | 117.5 | 2.5 | 47 | 3.41 | 73 | 22 | |
| Relatively | 1 | 55.3* | 1.23 | Surplus | 44.2 | 0.9 | 49 | 1.64 | 39 | 12 |
| 2 | 94.8* | 1.65 | Surplus | 58.1 | 1.8 | 32 | 1.22 | 41 | 12 | |
| 3 | 80.1 | 0.01* | Surplus | 56.9 | 1.2 | 47 | 0.94 | 33 | 10 | |
| 4 | 78.2 | 1.99* | Surplus | 37.7 | 2.0 | 19 | 0.82 | 45 | 14 | |
| 5 | 80.1 | 1.65 | Surplus | 28.6* | 1.4 | 20 | 1.36 | 36 | 11 | |
| 6 | 77.8 | 1.25 | Surplus | 123.3* | 3.8 | 34 | 1.43 | 30 | 12 | |
| 7 | 80.2 | 1.54 | Surplus | 39.9 | 8.2 | 4.9* | 0.95 | 39 | 12 | |
| 8 | 82.1 | 1.77 | Surplus | 52.7 | 0.1 | 527* | 1.12 | 43 | 13 | |
| In the past | 80.2 | 2.0* | Surplus | 36.1 | 0.9 | 40 | 0.42* | 42 | 12 | |
(the * symbolic representation is the value outside the scope of the invention)
From the result shown in table 1 and the table 2 as can be known, the magnetic composite sheet that adopts flat metal soft magnetic powder 1～20 of the present invention to make, with adopt relatively magnetic composite sheet of making and the magnetic composite sheet ratio that adopts flat metal soft magnetic powder making in the past of flat metal soft magnetic powder 1～8, the maximum of the real part of the complex permeability of 30kHz～30MHz is big, and, the imaginary part maximum height of the complex permeability of 30MHz～3GHz.
Embodiment 2
The table 1 that to make in embodiment 1 and the flat metal soft magnetic powder of the present invention 1～20 shown in the table 2 are as material powder, with they oxidation processes under the condition shown in table 3 and the table 4 respectively, form the oxide-film of the thickness shown in table 3 and the table 4 thus on the surface of flat metal soft magnetic powder of the present invention, made the flat metal soft magnetic powder 1～20 of lining oxide-film of the present invention.
Mixed chlorinated polyethylene in the flat metal soft magnetic powder 1～20 of this lining oxide-film of the present invention: after 15 quality % are also mixing, by the roller moulding, made the magnetic composite sheet of flat horizontal surface and sheet surface thickness that be arranged in parallel, that have 0.5mm of the flat metal soft magnetic powder of lining oxide-film, measure the resistivity of this magnetic composite sheet, table 3 and table 4 show its result.
Table 3
| Kind | Material powder | The oxide-film formation condition | The thickness of oxide-film () | The resistivity of magnetic composite sheet (Ω cm) | |||
| Atmosphere | Heating-up temperature (℃) | Heat time heating time (hour) | |||||
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 1 | The flat metal soft magnetic powder 1 of the present invention of table 1 | Atmosphere | 400 | 0.5 | 1000 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 2 | The flat metal soft magnetic powder 2 of the present invention of table 1 | Atmosphere | 375 | 1 | 500 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 3 | The flat metal soft magnetic powder 3 of the present invention of table 1 | Atmosphere | 350 | 2 | 700 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 4 | The flat metal soft magnetic powder 4 of the present invention of table 1 | Atmosphere | 325 | 4 | 800 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 5 | The flat metal soft magnetic powder 5 of the present invention of table 1 | Atmosphere | 300 | 8 | 500 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 6 | The flat metal soft magnetic powder 6 of the present invention of table 1 | O 2：10％ N 2：90％ | 400 | 0.5 | 600 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 7 | The flat metal soft magnetic powder 7 of the present invention of table 1 | O 2：10％ N 2：90％ | 375 | 1 | 300 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 8 | The flat metal soft magnetic powder 8 of the present invention of table 1 | O 2：10％ N 2：90％ | 350 | 2 | 400 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 9 | The flat metal soft magnetic powder 9 of the present invention of table 1 | O 2：10％ N 2：90％ | 325 | 4 | 450 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 10 | The flat metal soft magnetic powder 10 of the present invention of table 1 | O 2：10％ N 2：90％ | 300 | 8 | 300 | 10 6 |
Table 4
| Kind | Material powder | The oxide-film formation condition | The thickness of oxide-film () | The resistivity of magnetic composite sheet (Ω cm) | |||
| Atmosphere | Heating-up temperature (℃) | Heat time heating time (hour) | |||||
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 11 | The flat metal soft magnetic powder 11 of the present invention of table 1 | Distilled water | 100 | 2 | 100 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 12 | The flat metal soft magnetic powder 12 of the present invention of table 1 | Distilled water | 100 | 1 | 80 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 13 | The flat metal soft magnetic powder 13 of the present invention of table 1 | Distilled water | 100 | 0.5 | 60 | 10 7 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 14 | The flat metal soft magnetic powder 14 of the present invention of table 1 | Distilled water | 100 | 0.2 | 55 | 10 4 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 15 | The flat metal soft magnetic powder 15 of the present invention of table 1 | Distilled water | 100 | 0.1 | 50 | 10 3 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 16 | The flat metal soft magnetic powder 16 of the present invention of table 2 | Distilled water | 90 | 1 | 60 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 17 | The flat metal soft magnetic powder 17 of the present invention of table 2 | Distilled water | 80 | 2 | 60 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 18 | The flat metal soft magnetic powder 18 of the present invention of table 2 | Distilled water | 70 | 6 | 60 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 19 | The flat metal soft magnetic powder 19 of the present invention of table 2 | Distilled water | 60 | 24 | 60 | 10 6 |
| The be covered flat metal soft magnetic powder of oxide-film of the present invention | 20 | The flat metal soft magnetic powder 20 of the present invention of table 2 | Distilled water | 50 | 96 | 60 | 10 6 |
From the result shown in table 3 and the table 4 as can be known, use the flat metal soft magnetic powder 1～20 that has formed the lining oxide-film of the present invention of oxide-film by oxidation in oxidizing atmosphere on the surface, the magnetic composite sheet of making demonstrates high resistivity.
Claims (6)
1. a Fe-Ni-Mo is the flat metal soft magnetic powder, it is to have Ni:60～90% that contains in mass, Mo:0.05～1.95%, the one-tenth that surplus comprises Fe and unavoidable impurities is grouped into, and the flat metal soft magnetic powder of the flat horizontal surface of average grain diameter 30～150 μ m and aspect ratio (average grain diameter/average thickness) 5～500, so that comprise the flat horizontal surface of the plane of the incident direction of X ray and diffraction direction perpendicular to above-mentioned flat metal soft magnetic powder, and in the X-ray diffractogram that the mode that angle that incident direction and flat horizontal surface constitute and diffraction direction are equated with the angle of flat horizontal surface formation is measured, the peak height of the indices of crystallographic plane (200) is designated as I
200, the peak height of the indices of crystallographic plane (111) is designated as I
111The time, peak intensity compares I
200/ I
111In 0.43～10 scope.
2. magnetic composite, wherein, the described Fe-Ni-Mo of claim 1 is that the flat horizontal surface of flat metal soft magnetic powder is directed and be scattered here and there in resin.
3. magnetic composite sheet, it is the described magnetic composite of claim 2, above-mentioned Fe-Ni-Mo is that the flat horizontal surface of flat metal soft magnetic powder is directed and be scattered here and there in the direction vertical with magnetic composite sheet thickness direction.
4. the flat metal soft magnetic powder of Fe-Ni-Mo system lining oxide-film, it is that one-tenth that Ni:60～90%, Mo:0.05～1.95%, the surplus that contain in mass comprise Fe and unavoidable impurities is grouped into and the surface of the flat metal soft magnetic powder of the flat horizontal surface of average grain diameter 30～150 μ m and aspect ratio (average grain diameter/average thickness) 5～500 having, formed the flat metal soft magnetic powder of lining oxide-film of the oxide-film of thickness 50～1000
So that comprise the flat horizontal surface of the plane of the incident direction of X ray and diffraction direction perpendicular to the flat metal soft magnetic powder of above-mentioned lining oxide-film, and in the X-ray diffractogram that the mode that angle that incident direction and flat horizontal surface constitute and diffraction direction are equated with the angle of flat horizontal surface formation is measured, the peak height of the indices of crystallographic plane (200) is designated as I
200, the peak height of the indices of crystallographic plane (111) is designated as I
111The time, peak intensity compares I
200/ I
111In 0.43～10 scope.
5. magnetic composite, wherein, the flat horizontal surface of the flat metal soft magnetic powder of the described Fe-Ni-Mo of claim 4 system lining oxide-film is directed and be scattered here and there in resin.
6. magnetic composite sheet, it is the described magnetic composite of claim 5, the flat horizontal surface of the flat metal soft magnetic powder of above-mentioned Fe-Ni-Mo system lining oxide-film is directed and be scattered here and there in the direction vertical with magnetic composite sheet thickness direction.
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| JP2003205956 | 2003-08-05 | ||
| JP205956/2003 | 2003-08-05 | ||
| JP358970/2003 | 2003-10-20 | ||
| JP041029/2004 | 2004-02-18 | ||
| JP217371/2004 | 2004-07-26 |
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| CN100471600C CN100471600C (en) | 2009-03-25 |
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|---|---|---|---|---|
| CN100566891C (en) * | 2007-03-14 | 2009-12-09 | 中国原子能科学研究院 | Preparation of147Powder metallurgy process of Pm high-activity source |
| CN101246773B (en) * | 2007-02-12 | 2010-05-19 | 北京有色金属研究总院 | High-efficiency soft magnetic material and method for producing the same |
| CN101616764B (en) * | 2007-04-13 | 2012-06-06 | 住友大阪水泥股份有限公司 | Nickel-iron-zinc alloy nanoparticle |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101246773B (en) * | 2007-02-12 | 2010-05-19 | 北京有色金属研究总院 | High-efficiency soft magnetic material and method for producing the same |
| CN100566891C (en) * | 2007-03-14 | 2009-12-09 | 中国原子能科学研究院 | Preparation of147Powder metallurgy process of Pm high-activity source |
| CN101616764B (en) * | 2007-04-13 | 2012-06-06 | 住友大阪水泥股份有限公司 | Nickel-iron-zinc alloy nanoparticle |
| CN102933335A (en) * | 2010-06-09 | 2013-02-13 | 新东工业株式会社 | Iron group-based soft magnetic powder |
| CN102933335B (en) * | 2010-06-09 | 2015-01-14 | 新东工业株式会社 | Iron group-based soft magnetic powder |
| CN106876078A (en) * | 2011-04-27 | 2017-06-20 | 太阳诱电株式会社 | Magnetic material and use its coil component |
| CN106876078B (en) * | 2011-04-27 | 2019-09-06 | 太阳诱电株式会社 | Magnetic material and the coil component for using it |
| CN104008844A (en) * | 2014-01-20 | 2014-08-27 | 横店集团东磁股份有限公司 | Fabrication method of soft magnetic alloy materials |
| CN104008844B (en) * | 2014-01-20 | 2017-05-10 | 横店集团东磁股份有限公司 | Fabrication method of soft magnetic alloy materials |
| CN109545493A (en) * | 2017-09-22 | 2019-03-29 | 株式会社村田制作所 | Composite magnetic and the coil component for having used the composite magnetic |
| CN109545493B (en) * | 2017-09-22 | 2020-11-24 | 株式会社村田制作所 | Composite magnetic material and coil component using same |
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| CN100471600C (en) | 2009-03-25 |
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