CN102360672A - Novel composite magnetically soft material and preparation method thereof - Google Patents
Novel composite magnetically soft material and preparation method thereof Download PDFInfo
- Publication number
- CN102360672A CN102360672A CN2011101525412A CN201110152541A CN102360672A CN 102360672 A CN102360672 A CN 102360672A CN 2011101525412 A CN2011101525412 A CN 2011101525412A CN 201110152541 A CN201110152541 A CN 201110152541A CN 102360672 A CN102360672 A CN 102360672A
- Authority
- CN
- China
- Prior art keywords
- powder
- lubricant
- iron
- atomizing
- particle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention belongs to the field of powder metallurgy and particularly relates to a composite magnetically soft material of a magnetically soft magnetic part with a complicated shape, and a preparation method for the composite magnetically soft material. The composite magnetically soft material comprises atomized iron-based powder, nano aluminum oxide powder and a lubricant, wherein the nano aluminum oxide powder is 0.01 to 2 percent based on the mass of the atomized iron-based powder; the lubricant is 0.01 to 2 percent based on the mass of the atomized iron-based powder; the lubricant is a solid lubricant, namely talcpowder, a liquid lubricant, namely vegetable oil, or the combined lubricant of the solid lubricant and the liquid lubricant; and the nano aluminum oxide powder and the lubricant uniformly coat the surface of the atomized iron-based powder. The preparation process is simple, and the material is low in cost and high in density and magnetic induction strength.
Description
Technical field
The invention belongs to field of powder metallurgy, be specifically related to compound soft magnetic material of a kind of soft magnetic property parts with complicated shape and preparation method thereof.
Background technology
Soft magnetic material is used for the stator of motor and the iron core of rotor, transformer and inductor etc.Have the soft magnetic property parts of complicated shape through the stack technology manufacturing, obviously can run into very big difficulty.A kind of solution route is to utilize PM technique that iron-based powder is pressed knot together with lubricant and/or binding agent, then heat treatment at a certain temperature or sintering.Selecting examples of suitable lubricants and/or binding agent is considerable for the high density and the pressed part demoulding that realize material.In fact; The lubricant that is used for this PM technique can have multiple choices; Sweden Huo Jianasi company discloses a series of relevant Chinese patent/applications; Wherein, " iron-based powder combination that comprises the silane lubricant " (application number 200380101930.6) provides alkyl alkoxy or polyethers alkoxy silane as lubricant; " lubricant of insulated soft magnetic iron-based powder compositions " (application number 200580020774.X) provides mineral oil, plant or animal base aliphatic acid, polyethylene glycol, polypropylene glycol, glycerine and esterification derivative thereof as lubricant; " containing the metal-powder compositions of bonding lubricant and contain the bonding lubricant of tristerin " (application number 03813809.3) provides serial tristerin as lubricant; (application number 200580031161.6) provides secondary amide to press knot technological as the soft magnetic powder of lubricant and/adhesive " to comprise the powder metal composition of secondary amide as lubricant and/or binding agent "; " metal-powder compositions that comprises drying oil binder " (application number 200680007914.6) provides with graphite and tall oil and pressed the knot technology as the soft magnetic powder of adhesive; (application number 200380107358.4) discloses with organosilan, titanate esters, aluminic acid ester and the zirconate soft magnetic powder pressure knot technology as lubricant " to comprise insulated particle and the soft magnetic powder composition and method of making the same that is selected from the lubricant of organosilan, titanate esters, aluminic acid ester and zirconate "; " lubricant for powder metallurgy powder " (application number 02820207.4) discloses with polyvinylether and oligoamide and pressed the knot technology as the soft magnetic powder of lubricant.
When the preparation compound soft magnetic material, can carry out insulating to the ferrous powder granules of being selected for use and handle, also can not carry out insulating and handle.The ferrous powder granules insulating can reduce eddy current loss.The technology that at present the ferrous powder granules insulating is commonly used is ferrous powder granules to be carried out phosphorylation handle, for example more than the patented technology of several Sweden Huo Jianasi company all adopt the iron-based powder after this kind PROCESS FOR TREATMENT.But we find to contain phosphatization protective layer parcel and are prone to make the iron-based powder surface hardening, can cause particle deformation difficulty, are difficult to obtain higher density iron powder composite material in the practice under the lower pressure, and this proposes very high request to actual production.
Summary of the invention
The object of the present invention is to provide a kind of novel compound soft magnetic material and preparation method.The additive raw material of this compound soft magnetic material source is abundant, low price, in that to obtain composite density than following of pressure of low pressure knot higher.
In order to achieve the above object, the invention provides following technical scheme:
A kind of NEW TYPE OF COMPOSITE soft magnetic material; Form by atomizing iron-based powder, nano-aluminium oxide powder and lubricant; Wherein the quality of nano-aluminium oxide powder is the 0.01-2% of atomizing iron-based powder quality, and the quality of lubricant is the 0.01-2% of atomizing iron-based powder quality; Said nano-aluminium oxide powder and lubricant evenly are coated on atomizing iron-based powder surface.
Said atomizing iron-based powder is the atomizing straight iron powder, or the mixed powder of atomizing straight iron powder and atomizing iron nickel powder.
In the mixed powder of said atomizing straight iron powder and atomizing iron nickel powder, atomizing iron nickel powder quality accounts for ratio≤5% of atomizing ferrous alloy powder quality.
The particle size range of said atomizing straight iron powder satisfies: at least 30%, preferred at least 60% iron powder is made up of the particle that particle diameter surpasses 20 μ m, and particle diameter is greater than particle≤5% of 40 μ m, powder particle≤10% of particle diameter below 1 μ m.
Said lubricant is the solid phase lubricant, or the liquid phase lubricant, or the combined lubrication agent of solid phase lubricant and liquid phase lubricant.
Said solid phase lubricant is the talcum powder powder, granularity 10nm-1 μ m, preferred nanoscale.
Said talcous quality is the 0.01-2% of atomizing ferrous alloy powder quality, preferred 0.03-1%.
Said liquid phase lubricant is a kind of or its combination in the following vegetable oil: castor oil, palm oil, soya-bean oil, rapeseed oil, peanut oil, sesame oil.
The quality of said liquid phase lubricant is the 0.01-2% of atomizing ferrous alloy powder quality, preferred 0.05-1%.
When lubricant was the combined lubrication agent of solid phase lubricant and liquid phase lubricant, solid phase lubricant quality accounted for the 10-90% of lubricant gross mass, and all the other are the liquid phase lubricant.
Said nano-aluminium oxide powder quality is the 0.1-0.5% of atomizing iron-based powder quality.
A kind of method for preparing the NEW TYPE OF COMPOSITE soft magnetic material comprises the steps:
To atomize iron-based powder and nano-aluminium oxide and lubricant fully dissolves and is scattered in the organic solvent; Alundum (Al and lubricant evenly are coated on the ferrous alloy powder particle surface; Be coated with of the pressure pressed moulding of the ferrous alloy powder particle of alundum (Al and lubricant at 550-750MPa; The parts that suppress were at 120-200 ℃ of following vacuum annealing 10-60 minute; Under 500-600 ℃ argon gas, nitrogen or vacuum condition, annealed 30-180 minute again, obtain required compound iron based soft magnetic materials parts.
Starting powder said atomizing iron-based powder was water atomization or aerosolization before coating after.
Said atomizing iron-based powder carried out hydrogenation treatment or phosphorylation and handles before encapsulation steps.
Said encapsulation steps is that mechanical agitation is mixed coating or sonic oscillation coats, and places until organic solvent evaporation then.
Said pressing step is in 50-60 ℃ of pressed or normal temperature pressed.
Said organic solvent is a kind of in ethanol, isopropyl alcohol, acetone, the butanone, preferred alcohol.
The compound soft magnetic material that the present invention proposes, its additive comprises lubricant and nano-aluminium oxide; Wherein make the solid phase lubricant with talcum powder, it has insulation property, is different from graphite.In order to obtain insulation property better, can suitably add nano-aluminium oxide, the ferrous powder granules surface is wrapped up, simultaneously, talcum powder is cheap, be easy to get, and high lubricating effect; The present invention also proposes to choose vegetable oil as the liquid phase lubricant, and with suitable the cooperating of talcum powder, lubricant effect is superior to single use talcum powder or vegetable oil.
Preparation process mainly comprises: with lubricator with nano-aluminium oxide atomizing ferrous alloy powder particle is coated, then the ferrous alloy powder particle after coating is pressed knot, the soft magnetic part behind the pressure knot is carried out vacuum or protective atmosphere (for example, nitrogen or argon gas) annealing down.
The atomizing ferrous alloy powder can be the atomizing straight iron powder, can be atomizing straight iron powder and atomizing iron nickel powder mixed powder.Select atomizing straight iron powder and atomizing iron nickel powder mixed powder mainly to consider the factor of magnetic permeability.But iron nickel powder content accounts for the ratio of ferrous alloy powder preferably is not higher than 5%, and main what consider is that the saturation magnetization of iron nickel powder is lower than straight iron powder.
Atomizing straight iron powder particle size range should satisfy: at least 30%, preferred at least 60% iron powder is made up of the particle that particle diameter surpasses 20 μ m, and particle diameter accounts for 5% at most greater than the particle of 40 μ m, and the powder particle of particle diameter below 1 μ m is less than 10%.Selecting the iron powder of appropriate particle size, is the prerequisite that can obtain high density material.
Lubricant in the inventive method can only select the solid phase talcum powder lubricated, also can only select for use one or more vegetable oil lubricated, can also be that talcum powder is deployed into the combined lubrication agent as solid phase lubricant and one or more vegetable oil as the liquid phase lubricant.We find that the type of lubricant is directly connected to the density and the magnetic property of the compound soft magnetic material that makes.
The solid phase talcum powder has better lubricant effect with the mixed lubricant compositions of one or more vegetable fat, can obtain the more soft magnetic material of high density, high magnetic strength.We find that also the consumption of lubricant also is directly connected to the density and the magnetic property of the compound soft magnetic material that makes simultaneously.
Solid phase lubricant talcum powder powder in the inventive method, granularity 10nm-1 μ m, preferred nanoscale, nano level talcum powder particle can be dispersed in the ferrous powder granules surface, increases the flowability of ferrous powder granules, has improved the insulating properties on ferrous powder granules surface simultaneously.Solid phase lubricant talcum powder is wide, the inexpensive material in source, can directly reduce the cost of compound soft magnetic material.
Liquid phase lubricant in the inventive method is a kind of common vegetable oil or the composition of several plant oils.For example castor oil, palm oil, soya-bean oil, vegetable seed wet goods, this quasi-grease economy is easy to get high lubricating effect.During use,, stir solid phase lubricant talcum powder powder and the two the fully mixing by a certain percentage of liquid phase lubricant.And the selected lubricant ability while of the present invention is as the release agent of profiled part.
Atomizing ferrous alloy powder in the inventive method can directly adopt former powder of iron powder and talcum powder lubricant directly to coat before coating, and mixed with nano-aluminium oxide more afterwards; Can directly coat with the combined lubrication agent that talcum powder and vegetable oil are deployed into, mix with nano-aluminium oxide more afterwards.Because talcum powder is the good insulation performance material, therefore, can obtain the soft magnetic material of high density, high magnetic strength, good insulating after the compacting.We are also unexpected to find, content is lower than 0.5% nano-aluminium oxide and also has certain lubrication simultaneously.
Iron powder in the inventive method also can carry out hydrogenation process to the atomizing ferrous alloy powder and handle before coating.This method can effectively be removed the oxide layer on atomized iron powder surface; Make that the ferrous powder granules surface is softening; Select examples of suitable lubricants to coat again, selected lubricant can be a solid phase talcum powder lubricant, can be that one or more vegetable oil are deployed into vegetable fat; Can also be the combined lubrication agent that talcum powder and vegetable fat are deployed into, can both obtain the compound soft magnetic material of high density, high magnetic strength.
Iron powder in the inventive method also can carry out the phosphorylation PROCESS FOR TREATMENT to the former powder of atomized iron powder (the original iron-based powder after water atomization or the aerosolization) before coating, this technology can effectively improve the insulating properties of material.This also is the main means that present said material realizes insulation, but increases through the atomized iron powder case hardness after the phosphorylation PROCESS FOR TREATMENT, during compacting, must suitably improve pressing pressure to obtain highdensity soft magnetic material.
The cladding process on atomized iron powder surface comprises in the inventive method: mechanical agitation is mixed coating, and sonic oscillation coats, and can also be that fluidized-bed process coats in principle.The advantage of mechanical agitation hybrid packet coating process is can be quick, large batch of coating.The sonic oscillation cladding process can guarantee that the iron powder powder surface coats the combined lubrication agent uniformly.Fluidized-bed process coats can be wrapped in the iron powder powder surface with the combined lubrication agent in enormous quantities, evenly and apace.
Pressing process in the inventive method can be 50-60 ℃ of pressed, also normal temperature pressed.
Organic solvent in the inventive method is selected ethanol, isopropyl alcohol, acetone or butanone for use.The effect of organic solvent is the even coating that can better help the combined lubrication agent.
Be coated with the pressure pressed of the ferrous powder granules of combined lubrication agent at 550-750MPa, can be at normal temperatures, also can be 50-60 ℃ of pressed.
The parts that suppress are at 120-200 ℃ of following vacuum annealing 10-60 minute, again under argon gas, nitrogen or vacuum protection condition, 550-600 ℃ of annealing 30-180 minute down, obtain having high density, the compound iron-based soft magnetic parts of high magnetic strength.
Beneficial effect of the present invention is: preparation technology of the present invention is simple, the cost of material is low, and density is high, magnetic flux density is big.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further set forth:
Embodiment 1:
The straight iron powder powder that will atomize is as raw material, and the granularity of iron powder accounts for 50% between 20-30 μ m, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 10%.This iron powder has the particle mean size between the 8-20 μ m, and the powder particle of granularity below 1 μ m is less than 10%.With etc. the talcum powder and the castor oil of quality fully mix, stirred 20 minutes, obtain the combined lubrication agent.With accounting for the iron powder quality is 0.2% combined lubrication agent and 0.1% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.With the pressure single shaft of 650MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 600 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.6g/cm
3, magnetic strength B
8000Be 1.262T, maximum permeability μ
mBe 0.3mH/m.
Embodiment 2:
To atomize straight iron powder and iron nickel powder mixed powder as the iron-based powder raw material; Wherein the iron nickel powder accounts for 2% of total ferrous alloy powder quality; The straight iron powder particle mean size accounts for 45% between 10-30 μ m, granularity accounts for 3% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 1%.With etc. the talcum powder and the soybean oil of quality fully mix, stirred 20 minutes, obtain the combined lubrication agent.With accounting for the iron powder quality is 0.2% combined lubrication agent and 0.3% nanometer Al
2O
3Join in the iron-based powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress were 200 ℃ of following vacuum annealings 30 minutes, and 500 ℃ of following heat treatment elements obtained composite soft-magnetic ring-type sample in 30 minutes in a vacuum again, and its density is 7.47g/cm
3, magnetic strength B
8000Be 1.25T, maximum permeability μ
mBe 0.3mH/m.
Embodiment 3:
As raw material, the iron powder particle mean size accounts for 50% between 20-30 μ m with the atomized iron powder powder, and granularity accounts for 2.5% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 3%.With accounting for the iron powder quality is 0.2% talcum powder and 0.1% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.To being squeezed into the ring-type sample, behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 40 minutes with the pressure single shaft of 600MPa, and 600 ℃ of following heat treatment elements are 60 minutes in a vacuum, obtain composite soft-magnetic ring-type sample, and its density is 7.55g/cm
3, magnetic strength B
8000Be 1.186T, maximum permeability μ
mBe 0.3mH/m.
Embodiment 4:
To atomize straight iron powder and iron nickel powder mixed powder as raw material; Wherein the iron nickel powder accounts for 5% of total ferrous alloy powder weight; The straight iron powder particle mean size accounts for 30% between 20-30 μ m, granularity accounts for 4% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 9%.With accounting for the iron powder quality is 0.1% rapeseed oil and 0.2% nanometer Al
2O
3Join in the iron-based powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 180 ℃ of following vacuum annealings 25 minutes, and 500 ℃ of following heat treatment elements 40 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.45g/cm
3, magnetic strength B
8000Be 1.02T, maximum permeability μ
mBe 0.2mH/m.
Embodiment 5:
To atomize straight iron powder and iron nickel powder mixed powder as raw material, and wherein the iron nickel powder accounts for 1% of iron powder quality, and the straight iron powder particle mean size accounts for 40% between 20-40 μ m, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 6%.With etc. the talcum powder and the rapeseed oil of quality fully mix, stirred 20 minutes, obtain the combined lubrication agent.With accounting for the iron powder quality is 0.2% combined lubrication agent and 0.3% nanometer Al
2O
3Join in the iron-based powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 6000MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 600 minutes, and 500 ℃ of following heat treatment elements 90 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.52g/cm
3, magnetic strength B
8000Be 1.221T, maximum permeability μ
mBe 0.3mH/m.
Embodiment 6:
As raw material, the iron powder particle mean size accounts for 60% between 20-40 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 8%.With mass ratio is that 1: 1 talcum powder and palm oil fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 0.4% combined lubrication agent and 0.5% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 550MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 160 ℃ of following vacuum annealings 40 minutes, and 500 ℃ of following heat treatment elements 160 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.02g/cm
3, magnetic strength B
8000Be 0.82T, maximum permeability μ
mBe 0.1mH/m.
Embodiment 7:
As raw material, the iron powder particle mean size accounts for 40% between 20-40 μ m with the atomized iron powder powder, and granularity accounts for 5% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 7%.With mass ratio is that 4: 1 talcum powder and palm oil fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 0.2% combined lubrication agent and 0.3% nanometer Al
2O
3Join in the iron powder powder, add organic solvent and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 180 ℃ of following vacuum annealings 30 minutes, and 500 ℃ of following heat treatment elements 120 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.45g/cm
3, magnetic strength B
8000Be 1.245T, maximum permeability μ
mBe 0.3mH/m.
Embodiment 8:
As raw material, the iron powder particle mean size accounts for 50% between 20-40 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 8%.With mass ratio is that 1: 1 talcum powder and palm oil fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 0.4% combined lubrication agent and 0.3% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 160 ℃ of following vacuum annealings 40 minutes, and 500 ℃ of following heat treatment elements 180 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.41g/cm
3
Embodiment 9:
As raw material, the iron powder particle mean size accounts for 45% between 20-30 μ m with the atomized iron powder powder, and granularity accounts for 3% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 8%.To account for the iron powder quality is 0.3% palmitic 0.3% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 700MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 60 minutes, and 550 ℃ of following heat treatment elements 100 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.37g/cm
3
Embodiment 10:
As raw material, the iron powder particle mean size accounts for 40% between 20-40 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 8%.With mass ratio is that 1: 1 talcum powder and palm oil fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 1% combined lubrication agent and 0.4% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent isopropyl alcohol and fully mix, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 160 ℃ of following vacuum annealings 40 minutes, and 500 ℃ of following heat treatment elements 180 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.39g/cm
3
Embodiment 11:
As raw material, the iron powder particle mean size accounts for 50% between 20-40 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 8%.With mass ratio is that 1: 1 talcum powder and palm oil fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 0.4% combined lubrication agent and 0.8% nanometer Al
2O
3Join in the iron powder powder, add a kind of in the organic solvent butanone, fully mix in the preferred alcohol, ultrasonator vibration 25 minutes, treat organic solvent evaporation again.With the pressure single shaft of 750MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 160 ℃ of following vacuum annealings 40 minutes, and 500 ℃ of following heat treatment elements 180 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.51g/cm
3
Embodiment 12:
The straight iron powder powder that will atomize is as raw material, and the granularity of iron powder accounts for 50% between 20-30 μ m, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 10%.This iron powder has the particle mean size between the 8-20 μ m, and the powder particle of granularity below 1 μ m is less than 8%.With accounting for the iron powder quality is 0.2% castor oil and 0.1% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, mechanical agitation is 15 minutes again, treats organic solvent evaporation.Under 50 ℃ of conditions, with the pressure single shaft of 750MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 600 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.3g/cm
3
Embodiment 13:
As raw material, the iron powder particle mean size accounts for 55% between 20-30 μ m with the atomized iron powder powder, and granularity accounts for 1% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 3%.To account for the iron powder quality is 0.05% palmitic 0.3% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.Under 60 ℃ of conditions, with the pressure single shaft of 700MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 120 ℃ of following vacuum annealings 30 minutes, and 550 ℃ of following heat treatment elements 100 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.02g/cm
3
Embodiment 14:
With atomized iron powder phosphorylation PROCESS FOR TREATMENT, the iron powder particle mean size accounts for 50% between 20-40 μ m, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 9%.To account for the iron powder quality is 0.1% palmitic 0.3% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.Under 50 ℃ of conditions, with the pressure single shaft of 500MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 120 ℃ of following vacuum annealings 10 minutes, and 550 ℃ of following heat treatment elements 100 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 6.92g/cm
3
Embodiment 15:
As raw material, the iron powder particle mean size accounts for 60% between 20-30 μ m with the atomized iron powder powder, and granularity accounts for 5% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 5%.With accounting for the iron powder quality is 0.3% talcum powder and 0.2% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 20 minutes, treat organic solvent evaporation again.With the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 20 minutes, and 600 ℃ of following heat treatment elements 150 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.22g/cm
3
Embodiment 16:
The straight iron powder powder that will atomize is as raw material, and the granularity of iron powder accounts for 60% between 10-30 μ m, and granularity accounts for 3% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 10%.This iron powder has the particle mean size between the 8-20 μ m, and the powder particle of granularity below 1 μ m is less than 8%.With accounting for the iron powder quality is 0.2% talcum powder and 0.2% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, mechanical agitation is 20 minutes again, treats organic solvent evaporation afterwards again.Under 60 ℃ of conditions, with the pressure single shaft of 700MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 650 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.12g/cm
3
Embodiment 17:
The straight iron powder powder that will atomize is as raw material, and the granularity of iron powder accounts for 50% between 20-30 μ m, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 10%.This iron powder has the particle mean size between the 8-20 μ m, and the powder particle of granularity below 1 μ m is less than 8%.With accounting for the iron powder quality is 1% castor oil and 0.1% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, mechanical agitation is 15 minutes again, treats organic solvent evaporation.Under 50 ℃ of conditions, with the pressure single shaft of 750MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 600 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.1g/cm
3
Embodiment 18:
As raw material, the iron powder particle mean size accounts for 45% between 25-40 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 5%.To wait mass ratio is that 2: 1 talcum powder and castor oil fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 2% combined lubrication agent and 0.2% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.Under 60 ℃ of conditions, with the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 150 ℃ of following vacuum annealings 45 minutes, and 500 ℃ of following heat treatment elements 40 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.23g/cm
3
Embodiment 19:
Atomized iron powder powder iron powder particle mean size accounts for 35% between 10-30 μ m, granularity accounts for 3% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 6%.The iron powder powder that at first makes water fogging carried out hydrogen treat (being hydrogenation treatment) 30 minutes under 250 ℃.With mass ratio is that talcum powder and the palm oil of 3:1 fully mixes, and stirs 20 minutes, obtains the combined lubrication agent.With accounting for the iron powder quality is 0.2% combined lubrication agent and 2% nanometer Al
2O
3Join in the water-atomized iron powder powder after hydrogen is handled, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 10 minutes, treat organic solvent evaporation again.Under 50 ℃ of conditions, with the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 15 minutes, and 500 ℃ of following heat treatment elements 90 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.42g/cm
3
Embodiment 20:
The pure iron original washing powder powder that will atomize is as raw material, and the granularity of iron powder accounts for 60% between 10-30 μ m, and granularity accounts for 3% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 10%.This ferrous alloy powder has the particle mean size between the 8-20 μ m, and the powder particle of granularity below 1 μ m is less than 8%.With accounting for the iron powder quality is 0.8% talcum powder and 0.01% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, mechanical agitation is 20 minutes again, treats organic solvent evaporation.Under 60 ℃ of conditions, with the pressure single shaft of 700MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 30 minutes, and 650 ℃ of following heat treatment elements 60 minutes in a vacuum obtain composite soft-magnetic ring-type sample again, and its density is 7.02g/cm
3
Embodiment 21:
As raw material, the iron powder particle mean size accounts for 50% between 20-30 μ m with the atomized iron powder powder, and granularity accounts for 2.5% greater than the particle of 40 μ m, and the powder particle of granularity below 1 μ m accounts for 3%.With accounting for the iron powder quality is 0.01% talcum powder and 0.1% nanometer Al
2O
3Join in the iron powder powder, add in the organic solvent absolute ethyl alcohol and fully mix, ultrasonator vibration 15 minutes, treat organic solvent evaporation again.Under 50 ℃ of conditions, with the pressure single shaft of 600MPa to being squeezed into the ring-type sample.Behind the extrusion operation, the parts that suppress are 200 ℃ of following vacuum annealings 40 minutes, and 600 ℃ of following heat treatment elements are 60 minutes in a vacuum, obtain composite soft-magnetic ring-type sample, and its density is 7.55g/cm
3
It should be noted last that; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although with reference to preferred embodiment the present invention is specified, those of ordinary skill in the art should be appreciated that and can make amendment or be equal to replacement technical scheme of the present invention; And not breaking away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed among the claim scope of the present invention.
Claims (17)
1. NEW TYPE OF COMPOSITE soft magnetic material; It is characterized in that: it is made up of atomizing iron-based powder, nano-aluminium oxide powder and lubricant; Wherein the quality of nano-aluminium oxide powder is the 0.01-2% of atomizing iron-based powder quality, and the quality of lubricant is the 0.01-2% of atomizing iron-based powder quality; Said nano-aluminium oxide powder and lubricant evenly are coated on atomizing iron-based powder surface.
2. material as claimed in claim 1 is characterized in that: said atomizing iron-based powder is the atomizing straight iron powder, or the mixed powder of atomizing straight iron powder and atomizing iron nickel powder.
3. material as claimed in claim 2 is characterized in that: in the mixed powder of said atomizing straight iron powder and atomizing iron nickel powder, atomizing iron nickel powder quality accounts for ratio≤5% of atomizing ferrous alloy powder quality.
4. material as claimed in claim 2; It is characterized in that: the particle size range of said atomizing straight iron powder satisfies: at least 30%, preferred at least 60% iron powder is made up of the particle that particle diameter surpasses 20 μ m; Particle diameter is greater than particle≤5% of 40 μ m, powder particle≤10% of particle diameter below 1 μ m.
5. material as claimed in claim 1 is characterized in that: said lubricant is the solid phase lubricant, or the liquid phase lubricant, or the combined lubrication agent of solid phase lubricant and liquid phase lubricant.
6. material as claimed in claim 5 is characterized in that: said solid phase lubricant is the talcum powder powder, granularity 10nm-1 μ m, preferred nanoscale.
7. material as claimed in claim 6 is characterized in that: said talcous quality is the 0.01-2% of atomizing ferrous alloy powder quality, preferred 0.03-1%.
8. material as claimed in claim 5 is characterized in that: said liquid phase lubricant is a kind of or its combination in the following vegetable oil: castor oil, palm oil, soya-bean oil, rapeseed oil, peanut oil, sesame oil.
9. material as claimed in claim 8 is characterized in that: the quality of said liquid phase lubricant is the 0.01-2% of atomizing ferrous alloy powder quality, preferred 0.05-1%.
10. material as claimed in claim 5 is characterized in that: when lubricant was the combined lubrication agent of solid phase lubricant and liquid phase lubricant, solid phase lubricant quality accounted for the 10-90% of lubricant gross mass, and all the other are the liquid phase lubricant.
11. material as claimed in claim 1 is characterized in that: said nano-aluminium oxide powder quality is the 0.1-0.5% of atomizing iron-based powder quality.
12. a method for preparing NEW TYPE OF COMPOSITE soft magnetic material as claimed in claim 1 is characterized in that: this method comprises the steps:
To atomize iron-based powder and nano-aluminium oxide and lubricant fully dissolves and is scattered in the organic solvent; Alundum (Al and lubricant evenly are coated on the ferrous alloy powder particle surface; Be coated with of the pressure pressed moulding of the ferrous alloy powder particle of alundum (Al and lubricant at 550-750MPa; The parts that suppress were at 120-200 ℃ of following vacuum annealing 10-60 minute; Under 500-600 ℃ argon gas, nitrogen or vacuum condition, annealed 30-180 minute again, obtain required compound iron based soft magnetic materials parts.
13. method as claimed in claim 12 is characterized in that: the starting powder said atomizing iron-based powder was water atomization or aerosolization before coating after.
14. method as claimed in claim 12 is characterized in that: said atomizing iron-based powder carried out hydrogenation treatment or phosphorylation and handles before encapsulation steps.
15. method as claimed in claim 12 is characterized in that: said encapsulation steps is that mechanical agitation is mixed coating or sonic oscillation coats, and places until organic solvent evaporation then.
16. method as claimed in claim 12 is characterized in that: said pressing step is in 50-60 ℃ of pressed or normal temperature pressed.
17. method as claimed in claim 12 is characterized in that: said organic solvent is a kind of in ethanol, isopropyl alcohol, acetone, the butanone, preferred alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101525412A CN102360672A (en) | 2011-04-01 | 2011-06-08 | Novel composite magnetically soft material and preparation method thereof |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110082179.6 | 2011-04-01 | ||
| CN2011100821796A CN102129908A (en) | 2011-04-01 | 2011-04-01 | Novel composite soft magnetic material and preparation method thereof |
| CN2011101525412A CN102360672A (en) | 2011-04-01 | 2011-06-08 | Novel composite magnetically soft material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102360672A true CN102360672A (en) | 2012-02-22 |
Family
ID=44267957
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100821796A Pending CN102129908A (en) | 2011-04-01 | 2011-04-01 | Novel composite soft magnetic material and preparation method thereof |
| CN2011101525412A Pending CN102360672A (en) | 2011-04-01 | 2011-06-08 | Novel composite magnetically soft material and preparation method thereof |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011100821796A Pending CN102129908A (en) | 2011-04-01 | 2011-04-01 | Novel composite soft magnetic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (2) | CN102129908A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103632795A (en) * | 2012-08-29 | 2014-03-12 | 比亚迪股份有限公司 | Sizing agent for NFC magnetic sheet, preparing method of sizing agent and NFC magnetic sheet |
| CN104425093A (en) * | 2013-08-20 | 2015-03-18 | 东睦新材料集团股份有限公司 | Iron-based soft magnetic composite and preparation method thereof |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20150050178A1 (en) * | 2012-04-26 | 2015-02-19 | The Hong Kong University Of Science And Technolog | Soft Magnetic Composite Materials |
| CN103406533B (en) * | 2013-07-02 | 2016-02-10 | 安徽瑞泰汽车零部件有限责任公司 | A kind of powder metallurgy and preparation method thereof |
| CN106373689B (en) * | 2016-08-30 | 2018-07-24 | 海门市彼维知识产权服务有限公司 | A kind of magnet composite material and preparation method for covering special soil based on nanometer |
| CN111009370B (en) * | 2019-12-26 | 2021-07-16 | 东睦新材料集团股份有限公司 | Preparation method of metal magnetic powder core |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004211129A (en) * | 2002-12-27 | 2004-07-29 | Jfe Steel Kk | Metal powder for powder magnetic core, and powder magnetic core using it |
| CN101226807A (en) * | 2007-09-05 | 2008-07-23 | 湖州科达磁电有限公司 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
| CN101745637A (en) * | 2010-02-11 | 2010-06-23 | 柴秀兰 | Insulating coating method and metal powder core prepared with same |
| WO2010150920A1 (en) * | 2009-06-26 | 2010-12-29 | Ｊｆｅスチール株式会社 | Iron-based mixed powder for powder metallurgy |
-
2011
- 2011-04-01 CN CN2011100821796A patent/CN102129908A/en active Pending
- 2011-06-08 CN CN2011101525412A patent/CN102360672A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004211129A (en) * | 2002-12-27 | 2004-07-29 | Jfe Steel Kk | Metal powder for powder magnetic core, and powder magnetic core using it |
| CN101226807A (en) * | 2007-09-05 | 2008-07-23 | 湖州科达磁电有限公司 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
| WO2010150920A1 (en) * | 2009-06-26 | 2010-12-29 | Ｊｆｅスチール株式会社 | Iron-based mixed powder for powder metallurgy |
| CN101745637A (en) * | 2010-02-11 | 2010-06-23 | 柴秀兰 | Insulating coating method and metal powder core prepared with same |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103632795A (en) * | 2012-08-29 | 2014-03-12 | 比亚迪股份有限公司 | Sizing agent for NFC magnetic sheet, preparing method of sizing agent and NFC magnetic sheet |
| US9570218B2 (en) | 2012-08-29 | 2017-02-14 | Byd Company Limited | Paste for NFC magnetic sheet, method of preparing the same, and NFC magnetic sheet |
| CN104425093A (en) * | 2013-08-20 | 2015-03-18 | 东睦新材料集团股份有限公司 | Iron-based soft magnetic composite and preparation method thereof |
| CN104425093B (en) * | 2013-08-20 | 2017-05-03 | 东睦新材料集团股份有限公司 | Iron-based soft magnetic composite and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102129908A (en) | 2011-07-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6662436B2 (en) | Manufacturing method of dust core | |
| CN102360672A (en) | Novel composite magnetically soft material and preparation method thereof | |
| KR101302921B1 (en) | Soft magnetic material, shaped body, compressed powder magnetic core, electromagnetic component, process for production of soft magnetic material, and process for production of compressed powder magnetic core | |
| CN101681709B (en) | Soft magnetic powder | |
| CN102360671B (en) | Preparation method for mu75 magnetic powder core of ferrosilicon aluminum | |
| KR20070027758A (en) | Powder metallurgical composition comprising carbon black as flow enhancing agent | |
| CN102744403A (en) | Preparation method of nanocrystalline magnetic powder cores | |
| US8911663B2 (en) | Insulated iron-base powder for soft magnetic applications | |
| CN109590460B (en) | Soft magnetic composite material and preparation method thereof | |
| CN102360662A (en) | Iron-based composite soft magnetic material and preparation method thereof | |
| CN104575913A (en) | Preparation method of low-loss amorphous magnetic powder core | |
| CN103270559A (en) | Soft magnetic powder | |
| CN103107014A (en) | Preparing method for alloy soft magnetism powder core | |
| JP2009266973A (en) | Soft magnetic metal particle powder and method of manufacturing the same, and magnetic core formed of pressed powder containing the same | |
| JP6043275B2 (en) | Soft magnetic powder | |
| PL209529B1 (en) | Soft magnetic powder composition comprising insulated particles and a lubricant selected from organo-silanes, -titanates, -aluminates and zirconates and a process for their preparation | |
| US7718082B2 (en) | Lubricants for insulated soft magnetic iron-based powder compositions | |
| JP2011171346A (en) | Iron-based soft magnetic powder for dust core, method of manufacturing the same, and dust core | |
| CN107256752B (en) | A kind of preparation method being sintered iron powder base soft-magnetic composite material | |
| CN102360663B (en) | Composite soft magnetic material and preparation method thereof | |
| CN104036903B (en) | A kind of preparation method of ferrum tantnickel powder core | |
| CN103811143B (en) | Pcrmeability is Fe-based amorphous powder core of 60 and preparation method thereof | |
| CN109599240B (en) | Ferrite soft magnetic powder core and preparation method thereof | |
| KR101202371B1 (en) | Powder metallurgical composition comprising carbon black as flow enhancing agent | |
| CN114147219B (en) | Amorphous nanocrystalline insulating finished powder and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120222 |