CN102129908A - Novel composite soft magnetic material and preparation method thereof - Google Patents
Novel composite soft magnetic material and preparation method thereof Download PDFInfo
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- CN102129908A CN102129908A CN2011100821796A CN201110082179A CN102129908A CN 102129908 A CN102129908 A CN 102129908A CN 2011100821796 A CN2011100821796 A CN 2011100821796A CN 201110082179 A CN201110082179 A CN 201110082179A CN 102129908 A CN102129908 A CN 102129908A
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Abstract
The invention belongs to the field of powder metallurgy and particularly relates to a composite soft magnetic material with a soft magnetic component with a complex shape and a preparation method thereof. The composite soft magnetic material comprises atomized iron-based powder, nano aluminium oxide powder and a lubricant, wherein the mass of the nano aluminium oxide powder is 0.01 to 2 percent of the mass of the atomized iron-based powder; the mass of the lubricant is 0.01 to 2 percent of the mass of the atomized iron-based powder; the lubricant is a solid-phase lubricant, or a liquid-phase lubricant, or a mixed lubricant of the solid-phase lubricant and the liquid-phase lubricant; the solid-phase lubricant is talcpowder; the liquid-phase lubricant is vegetable oil; and the nano aluminium oxide powder and the lubricant are uniformly coated on the surface of the atomized iron-based powder. The composite soft magnetic material has simple preparation process, low material cost, high density and high magnetic induction intensity.
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 by the stack technology manufacturing, obviously can run into very big difficulty.A kind of solution route is to utilize powder metallurgy technology 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 powder metallurgy technology 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; " comprise the powder metal composition of secondary amide " as lubricant and/or binding agent (application number 200580031161.6) provide secondary amide as lubricant and/soft magnetic powder of adhesive presses the knot technology; " 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 selected ferrous powder granules and handle, also can not carry out insulating and handle.The ferrous powder granules insulating can reduce eddy current loss.At present the technology that the ferrous powder granules insulating is commonly used is ferrous powder granules to be carried out phosphorylation handle, and for example the patented technology of above several Sweden Huo Jianasi company all adopts the iron-based powder after this kind PROCESS FOR TREATMENT.But we find to contain phosphatization protective layer parcel and easily 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; Described nano-aluminium oxide powder and lubricant evenly are coated on atomizing iron-based powder surface.
Described atomizing iron-based powder is the atomizing straight iron powder, or the mixed powder of atomizing straight iron powder and atomizing iron nickel powder.Wherein atomize in the mixed powder of 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 described atomizing straight iron powder satisfies: at least 30%, preferred at least 60% iron powder is made up of the particle that particle diameter surpasses 200 μ m, and particle diameter is greater than particle≤5% of 400 μ m, powder particle≤10% of particle diameter below 10 μ m.
Described lubricant is the solid phase lubricant, or the liquid phase lubricant, or the combined lubrication agent of solid phase lubricant and liquid phase lubricant, and wherein the solid phase lubricant is the talcum powder powder, granularity 10nm-1 μ m, preferred nanoscale.
Described talcous quality is the 0.01-2% of atomizing ferrous alloy powder quality, preferred 0.03-1%.
Described 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 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.
Described nano-aluminium oxide powder quality is the 0.1-0.5% of atomizing iron-based powder quality.
A kind of method for preparing above-mentioned 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 ferrous alloy powder particle compression moulding under the pressure of 550-750MPa of alundum (Al and lubricant, 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 described atomizing iron-based powder was water atomization or aerosolization before coating after.
Described atomizing iron-based powder carried out hydrogenation treatment or phosphorylation and handles before encapsulation steps.
Described encapsulation steps is that mechanical agitation is mixed coating or sonic oscillation coats, and places until organic solvent evaporation then.
Described pressing step is to suppress under compacting or the normal temperature under 50-60 ℃.
Described 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 better than 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 200 μ m, and particle diameter accounts for 5% at most greater than the particle of 400 μ m, and the powder particle of particle diameter below 10 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.
Solid phase talcum powder and the mixed lubricant compositions of one or more vegetable fat have better lubricant effect, 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 energy 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 that such material is realized the main means of insulation at present, 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 compacting down, also normal temperature compacting down.
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.
The ferrous powder granules that is coated with the combined lubrication agent is suppressed under the pressure of 550-750MPa, can also can suppress down at 50-60 ℃ at normal temperatures.
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 height, magnetic flux density are 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 200-300 μ m, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 μ m accounts for 10%.This iron powder has the particle mean size between the 80-200 μ m, and the powder particle of granularity below 10 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 100-300 μ m, granularity accounts for 3% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-300 μ m with the atomized iron powder powder, and granularity accounts for 2.5% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-300 μ m, granularity accounts for 4% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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, wherein the iron nickel powder accounts for 1% of iron powder quality, the straight iron powder particle mean size accounts for 40% between 200-400 μ m, granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-400 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-400 μ m with the atomized iron powder powder, and granularity accounts for 5% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-400 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-300 μ m with the atomized iron powder powder, and granularity accounts for 3% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-400 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-400 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-300 μ m, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 μ m accounts for 10%.This iron powder has the particle mean size between the 80-200 μ m, and the powder particle of granularity below 10 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 200-300 μ m with the atomized iron powder powder, and granularity accounts for 1% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-400 μ m, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 200-300 μ m with the atomized iron powder powder, and granularity accounts for 5% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 100-300 μ m, and granularity accounts for 3% greater than the particle of 400 μ m, and the powder particle of granularity below 10 μ m accounts for 10%.This iron powder has the particle mean size between the 80-200 μ m, and the powder particle of granularity below 10 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 200-300 μ m, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 μ m accounts for 10%.This iron powder has the particle mean size between the 80-200 μ m, and the powder particle of granularity below 10 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 250-400 μ m with the atomized iron powder powder, and granularity accounts for 2% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 100-300 μ m, granularity accounts for 3% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 3: 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 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 100-300 μ m, and granularity accounts for 3% greater than the particle of 400 μ m, and the powder particle of granularity below 10 μ m accounts for 10%.This ferrous alloy powder has the particle mean size between the 80-200 μ m, and the powder particle of granularity below 10 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 200-300 μ m with the atomized iron powder powder, and granularity accounts for 2.5% greater than the particle of 400 μ m, and the powder particle of granularity below 10 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 the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from the spirit and scope of technical solution 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; Described 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: described 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 described 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 described atomizing straight iron powder satisfies: at least 30%, preferred at least 60% iron powder is made up of the particle that particle diameter surpasses 200 μ m, particle diameter is greater than particle≤5% of 400 μ m, powder particle≤10% of particle diameter below 10 μ m.
5. material as claimed in claim 1 is characterized in that: described 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: described 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: described 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: described 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 described 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: described 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 ferrous alloy powder particle compression moulding under the pressure of 550-750MPa of alundum (Al and lubricant, 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 described atomizing iron-based powder was water atomization or aerosolization before coating after.
14. method as claimed in claim 12 is characterized in that: described 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: described 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: described pressing step is to suppress under compacting or the normal temperature under 50-60 ℃.
17. method as claimed in claim 12 is characterized in that: described organic solvent is a kind of in ethanol, isopropyl alcohol, acetone, the butanone, preferred alcohol.
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Cited By (5)
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| WO2013159558A1 (en) * | 2012-04-26 | 2013-10-31 | The Hong Kong University Of Science And Technology | Soft magnetic composite materials |
| CN103406533A (en) * | 2013-07-02 | 2013-11-27 | 安徽瑞泰汽车零部件有限责任公司 | Powder metallurgy and manufacturing method thereof |
| WO2014032506A1 (en) | 2012-08-29 | 2014-03-06 | Shenzhen Byd Auto R & D Company Limited | Paste for nfc magnetic sheet and method of preparing the same and nfc magnetic sheet |
| CN106373689A (en) * | 2016-08-30 | 2017-02-01 | 孟永辉 | Magnet composite material based on nanometer Montreal soil and preparation method of magnet composite material |
| CN111009370A (en) * | 2019-12-26 | 2020-04-14 | 东睦新材料集团股份有限公司 | Preparation method of metal magnetic powder core |
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| 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 |
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| JP2004211129A (en) * | 2002-12-27 | 2004-07-29 | Jfe Steel Kk | Metal powder for powder magnetic core, and powder magnetic core using it |
| CN100595850C (en) * | 2007-09-05 | 2010-03-24 | 湖州科达磁电有限公司 | Soft magnetic composite organically/inorganically compound insulation coating powdered iron and preparation method thereof |
| JP5663974B2 (en) * | 2009-06-26 | 2015-02-04 | Ｊｆｅスチール株式会社 | Iron-based mixed powder for powder metallurgy |
| CN101745637B (en) * | 2010-02-11 | 2016-03-09 | 昆山磁通新材料科技有限公司 | A kind of insulating coating method and the metal-powder-core prepared according to the method |
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| WO2013159558A1 (en) * | 2012-04-26 | 2013-10-31 | The Hong Kong University Of Science And Technology | Soft magnetic composite materials |
| CN104321839A (en) * | 2012-04-26 | 2015-01-28 | 香港科技大学 | Soft magnetic composite materials |
| US20150050178A1 (en) * | 2012-04-26 | 2015-02-19 | The Hong Kong University Of Science And Technolog | Soft Magnetic Composite Materials |
| WO2014032506A1 (en) | 2012-08-29 | 2014-03-06 | Shenzhen Byd Auto R & D Company Limited | Paste for nfc magnetic sheet and method of preparing the same and nfc magnetic sheet |
| EP2893541A4 (en) * | 2012-08-29 | 2016-04-27 | Byd Co Ltd | Paste for nfc magnetic sheet and method of preparing the same and nfc magnetic sheet |
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| 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 |
| CN106373689A (en) * | 2016-08-30 | 2017-02-01 | 孟永辉 | Magnet composite material based on nanometer Montreal soil and preparation method of magnet composite material |
| CN111009370A (en) * | 2019-12-26 | 2020-04-14 | 东睦新材料集团股份有限公司 | Preparation method of metal magnetic powder core |
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