CN107326264A - A kind of preparation technology of iron silicon phosphorus soft-magnetic composite material - Google Patents

A kind of preparation technology of iron silicon phosphorus soft-magnetic composite material Download PDF

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CN107326264A
CN107326264A CN201710543013.7A CN201710543013A CN107326264A CN 107326264 A CN107326264 A CN 107326264A CN 201710543013 A CN201710543013 A CN 201710543013A CN 107326264 A CN107326264 A CN 107326264A
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powder
iron
soft
composite material
magnetic composite
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CN107326264B (en
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曲选辉
孙海身
章林
陈彦
秦明礼
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0264—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements the maximum content of each alloying element not exceeding 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C33/00—Making ferrous alloys
    • C22C33/02—Making ferrous alloys by powder metallurgy
    • C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
    • C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C38/00—Ferrous alloys, e.g. steel alloys
    • C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • H01F1/147—Alloys characterised by their composition
    • H01F1/14766—Fe-Si based alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
    • H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
    • H01F41/0266—Moulding; Pressing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B22F2003/026—Mold wall lubrication or article surface lubrication

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  • Chemical & Material Sciences (AREA)
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  • Metallurgy (AREA)
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  • Manufacturing & Machinery (AREA)
  • Electromagnetism (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Soft Magnetic Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention provides a kind of iron silicon phosphorus soft-magnetic composite material preparation technology, belongs to soft-magnetic composite material technical field.Technological process is：Water atomized iron powder is pre-processed using high-temperature vapor processing first, recycle bipyramid rotary vacuum drying blender spraying combination drying, lubricant solution atomisation will be bonded, uniformly mixed with pretreated water atomized iron powder, superfine silica powder and ultra-fine iron phosphorus powder, obtain segregation-free soft magnetic composite powder, high density pressed compact is prepared by the warm mould high velocity compacted under die wall lubrication, sintered densification, improve the strength of materials, eliminate internal stress, the magnetic conductivity and resistivity of material are improved, eddy-current loss is reduced, finally gives iron silicon phosphorus soft-magnetic composite material.When there is this iron silicon phosphorus soft-magnetic composite material medium-high frequency to apply the characteristics of high magnetic permeability, low magnetic loss.The present invention is simple, and manufacturing cost is low.

Description

A kind of preparation technology of iron silicon phosphorus soft-magnetic composite material
Technical field
The invention belongs to soft-magnetic composite material technical field, be related to it is a kind of with powder surface modifications, spraying combination drying and The preparation method for the high-performance iron silicon phosphorus soft-magnetic composite material that high velocity compacted is combined.
Background technology
Si fe alloy is a kind of power electronics and the indispensable important soft magnetic alloy of war industry, be mainly used in motor, The iron core of generator and transformer, with high magnetic permeability and low loss characteristic, but it smelts rolling mill practice complexity, production cost It is higher, and its magnetic property has directionality, it is necessary to be used by laminating technology after insulation processing, compared to powder metallurgical technique For, for advantage, with the mixture of iron silica flour, iron powder, silica flour and iron phosphorus powder, the height prepared more is sintered through high velocity compacted by the latter Density core material, with three-dimensional magnetic isotropy, low-down eddy-current loss, relatively low total magnetic loss (medium-high frequency) is high Saturation magnetic sense intensity, meanwhile, heat treatment temperature reduction, scantling and cost is greatly reduced.Have broad application prospects.
The content of the invention
It is an object of the invention to provide a kind of method for preparing iron silicon phosphorus soft-magnetic composite material, it is intended to improves soft magnetism and is combined The magnetic conductivity of material, intensity reduces magnetic loss.
1st, a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material, it is characterised in that complete in the steps below：
Step 1: water atomized iron powder is at a temperature of 570 DEG C~1150 DEG C, surface oxidation treatment 1 in steam atmosphere~ 6h, after the 110 DEG C of dryings of gained iron powder, obtains pre-processing straight iron powder；
Step 2: being dried in vacuo blender using a kind of bipyramid rotary, a kind of cohesive lubricant is dissolved by heating organic In solvent, bonding lubricant solution is sprayed in mixing machine by way of gases at high pressure are sprayed, makes water atomized iron powder, surpass Thin pure silicon powder and ultra-fine iron phosphorus powder are uniformly mixed, and can allow pure silicon powder and iron phosphorus powder are uniformly cohesive to be coated on water atomized iron powder Surface, prevents component segregation, obtains iron silicon phosphorus mixed-powder；
Step 3: lubricant stearic acid lithium is dissolved in acetone, ratio is 100g：1L, is applied to high speed press upper punch Surface and die cavity inner surface, carry out die wall lubrication, and former is previously heated to 60 DEG C~150 DEG C, and iron silicon phosphorus mixed-powder is sent into The former of heating carries out warm mould high velocity compacted, and impact velocity is 1~10m/s, can carry out repeat impact compacting, point 2~3 punchings Hit, each stroke is selected in the range of 0~70mm, can also use relaxation ancillary method, obtain soft-magnetic composite material base substrate；
Step 4: the soft-magnetic composite material base substrate handled by finishing, is sintered in 900 DEG C~1200 DEG C tube furnaces, In sintering process iron silicon phosphorus formation low melting point eutectic phase, reduce sintering temperature, protective atmosphere be hydrogen, nitrogen or inert gas, With 5 DEG C/s speed furnace coolings, iron silicon phosphorus soft-magnetic composite material is finally given.
Further, water atomized iron powder described in step one, particle diameter≤180 μm, after vapor high-temperature process, surface Form one layer of Fe3O4 coating film；
Further, a kind of bipyramid rotary described in step 2 is dried in vacuo in blender, cylinder under vacuum conditions, deep fat Imported by pump in mixing machine interlayer and heat barrel, temperature is between 80 DEG C~150 DEG C.Meanwhile, mixing machine constantly revolution makes material Stir, high-pressure gas pressure is between 0.01MPa~1MPa, and the bonding lubricant solution ejected forms vaporific, with stirring Material is fully contacted, and alloying element powder is effectively sticked on matrix powder surface, and easy volatile solvent connects with barrel Steam is formed after touch, is drained by vacuum pumped, rate of drying can be improved, and forms uniform soft-magnetic alloy powder.Solution line There is certain gap between vacuum tube and drive shaft cavity, be sealed against by vacuum mud, three rotates when different.
Further, it is that, dissolved with the solution for bonding lubricant, solution temperature exists that lubricant solution is bonded described in step 2 Between 60~100 DEG C, solvent can be the mixing of gasoline, toluene, dimethylbenzene, chloroform, dichloromethane, normal heptane, alcohol Solvent or wherein single solvent, and it is volatile；It can be butadiene-styrene rubber, neoprene, or polyethylene that solute, which bonds lubricant, The blend of the polymer such as wax, ethylene bis stearic acid amide, stearic acid, polyamide wax, microwax or wherein single solute.Bond Lubricant addition is controlled between 0.01wt%~10wt%.
Superfine silica powder described in step 2 and ultra-fine iron phosphorus powder particle diameter are within 1 μm~5 μ ms, iron phosphorus phosphorus content 22- 24%, both additions are in the range of 0.05wt%~50wt%.
Further, high velocity compacted described in step 3 is a kind of high density parts shaping new technology, and it is high using weight The shock wave that speed impact stamping is produced reaches densification within the extremely short time, and can carry out repeat impact compacting, enters one Step improves green density, and the relaxation ancillary method installs cushion block additional in upper punch bottom or bottom punch top, can improve base Body surface quality, former heating uses digital temperature control silica gel heating sheet, and maximum heating temperature is 200 DEG C.
The advantage of the invention is that：(1) water atomized iron powder forms Fe after vapor high-temperature process3O4Film, Neng Goufang Sealing atomization pure iron powder surface continues to aoxidize, while certain magnetic can be kept；(2) the iron silicon phosphorus for bonding mixing through spraying is mixed Powder is closed, without drying process, it is not required that be blended into lubricant and can be used；(3) the warm mould high velocity compacting technique used can To improve green density, intergranular air gap distribution is reduced, the magnetic conductivity and saturation induction density of material is improved, bonds lubrication The addition of agent can protect the integrality of insulating coating, improve resistivity, reduction loss；(4) the ultra-fine pure silicon powder being mixed into The higher clad of a layer resistivity can be formed in sintering process with ultra-fine iron phosphorus powder, eddy-current loss is reduced, material is reduced Internal stress, while the two sintering forms low-melting compound, can reduce sintering temperature, further improve consistency.It is one Plant the technique that high efficiency prepares iron silicon phosphorus soft-magnetic composite material.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Embodiment
Embodiment 1：Fe-3.5%Si-1.5%P soft-magnetic composite material preparation technologies
Straight iron powder 500g make water fogging at a temperature of 950 DEG C, surface oxidation treatment 2h in steam atmosphere, gained iron powder After 110 DEG C of air dry ovens are dried, obtain pre-processing straight iron powder；500g soft magnetisms are blended by Fe-3.5%Si-1.5%P formula Mixed-powder is, it is necessary to which ultra-fine pure silicon powder 17.5g, it is necessary to weigh ultra-fine iron phosphorus powder 32.6g, water atomized iron powder 450g, will be weighed up Water atomized iron powder and alloy powder by hand after premix, pour into dry-mixed in the barrel of bipyramid rotary vacuum drying blender 0.5h, while opening Heat-transfer Oil Pump, 120 DEG C of conduction oil of temperature is pumped into barrel interlayer, circulating-heating insulation；Take neoprene rubber Glue caking agent and ethylene bis stearic acid amide (1:1) 0.3wt%, i.e. 1.5g, temperature be 80 DEG C be dissolved in 500ml dichloromethane and Normal heptane (1:3) it is standby after dissolved clarification in solvent；Spray step as follows：(1) in 20min, start that lubricant solution will be bonded 200ml, 80 DEG C of heating dissolved clarifications are to be sprayed；(2) nitrogen is opened, adjustment pressure is 0.05MPa, while opening vavuum pump；(3) will Mono pump is sucked under 200ml lubricant solutions, heated condition, through conveyance conduit under stream pressure, is sprayed by the nozzle in barrel Nebulize, with admixture of powder in barrel；(4) after having sprayed, nitrogen is closed, 0.5h is remixed, vavuum pump reruns pass after 15min Close, the solvent of volatilization is discharged；(5) shift to an earlier date 10min, then take 200ml solution, with (3) step operation, after the completion of, with (4) step Suddenly, 0.5h is remixed；(6) finally that remaining 100ml lubricant solutions is sprayed, same to step (3) and (4) are mixed after 0.5h, Close barrel switch, co-blended 2h；Lubricant stearic acid lithium is dissolved in acetone, ratio is 100g：1L, is applied to high speed press Upper punch surface and die cavity inner surface, carry out die wall lubrication, and former is previously heated to 120 DEG C, and iron silicon phosphorus mixed-powder is sent into The former of heating carries out warm mould high velocity compacted, and stroke 70mm after the compacting demoulding, obtains iron silicon phosphorus soft-magnetic composite material base substrate；Through Cross in the iron silicon phosphorus soft-magnetic composite material base substrate of finishing processing, hydrogen atmosphere protection tube furnace, 900 are warming up to 5 DEG C/s speed DEG C sintering 0.5h, with 5 DEG C/s speed furnace coolings, finally give iron silicon phosphorus soft-magnetic composite material.
Embodiment 2：Fe-6.5%Si-1.0%P soft-magnetic composite material preparation technologies
Straight iron powder 500g make water fogging at a temperature of 970 DEG C, surface oxidation treatment 1.5h in steam atmosphere, gained iron powder After 100 DEG C of air dry ovens are dried, obtain pre-processing straight iron powder；500g soft magnetisms are blended by Fe-6.5%Si-1.0%P formula Mixed-powder is, it is necessary to which ultra-fine pure silicon powder 32.5g, it is necessary to weigh ultra-fine iron phosphorus powder 21.7g, water atomized iron powder 446g, will be weighed up Water atomized iron powder and alloy powder by hand after premix, pour into dry-mixed in the barrel of bipyramid rotary vacuum drying blender 0.5h, while opening Heat-transfer Oil Pump, 120 DEG C of conduction oil of temperature is pumped into barrel interlayer, circulating-heating insulation；It is derived from viscous Lubricant polymer blend 0.3wt%, i.e. 1.5g are tied, being 80 DEG C in temperature is dissolved in 500ml chloroforms and normal heptane (1:3) it is molten It is standby after dissolved clarification in agent；Spray step as follows：(1) in 20min, start that lubricant solution 200ml, 80 DEG C of heating will be bonded Dissolved clarification, it is to be sprayed；(2) nitrogen is opened, adjustment pressure is 0.05MPa, while opening vavuum pump；(3) it is 200ml lubricants is molten Mono pump is sucked under liquid, heated condition, through conveyance conduit under stream pressure, by the nozzle atomisation in barrel, with barrel Middle admixture of powder；(4) after having sprayed, nitrogen is closed, 0.5h is remixed, vavuum pump reruns closing after 15min, by the molten of volatilization Agent is discharged；(5) shift to an earlier date 10min, then take 200ml solution, with (3) step operation, after the completion of, with (4) step, remix 0.5h； (6) finally that remaining 100ml lubricant solutions is sprayed, same to step (3) and (4) are mixed after 0.5h, close barrel switch, Co-blended 2h；Lubricant stearic acid lithium is dissolved in acetone, ratio is 100g：1L, be applied to high speed press upper punch surface and Die cavity inner surface, carries out die wall lubrication, and former is previously heated to 110 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating enters Row temperature mould high velocity compacted, stroke 50mm after the compacting demoulding, obtains iron silicon phosphorus soft-magnetic composite material base substrate；Handled by finishing In iron silicon phosphorus soft-magnetic composite material base substrate, hydrogen atmosphere protection tube furnace, 1050 DEG C of sintering 0.5h are warming up to 5 DEG C/s speed, With 5 DEG C/s speed furnace coolings, iron silicon phosphorus soft-magnetic composite material is finally given.
Embodiment 3：Fe-10%Si-2.0%P soft-magnetic composite material preparation technologies
Straight iron powder 500g make water fogging at a temperature of 1000 DEG C, surface oxidation treatment 1.0h in steam atmosphere, gained iron After 100 DEG C of air dry ovens of powder are dried, obtain pre-processing straight iron powder；500g soft magnetisms are blended by Fe-10%Si-2.0%P formula Mixed-powder is, it is necessary to which ultra-fine pure silicon powder 50g, it is necessary to weigh ultra-fine iron phosphorus powder 43.5g, water atomized iron powder 406.5g, will be weighed up Water atomized iron powder and alloy powder by hand after premix, pour into dry-mixed in the barrel of bipyramid rotary vacuum drying blender 0.5h, while opening Heat-transfer Oil Pump, 120 DEG C of conduction oil of temperature is pumped into barrel interlayer, circulating-heating insulation；It is derived from viscous Lubricant polymer blend 0.2wt%, i.e. 1.0g are tied, being 80 DEG C in temperature is dissolved in 500ml chloroforms and normal heptane (1:3) it is molten It is standby after dissolved clarification in agent；Spray step as follows：(1) in 20min, start that lubricant solution 200ml, 80 DEG C of heating will be bonded Dissolved clarification, it is to be sprayed；(2) nitrogen is opened, adjustment pressure is 0.05MPa, while opening vavuum pump；(3) it is 200ml lubricants is molten Mono pump is sucked under liquid, heated condition, through conveyance conduit under stream pressure, by the nozzle atomisation in barrel, with barrel Middle admixture of powder；(4) after having sprayed, nitrogen is closed, 0.5h is remixed, vavuum pump reruns closing after 15min, by the molten of volatilization Agent is discharged；(5) shift to an earlier date 10min, then take 200ml solution, with (3) step operation, after the completion of, with (4) step, remix 0.5h； (6) finally that remaining 100ml lubricant solutions is sprayed, same to step (3) and (4) are mixed after 0.5h, close barrel switch, Co-blended 2h；Lubricant stearic acid lithium is dissolved in acetone, ratio is 100g：1L, be applied to high speed press upper punch surface and Die cavity inner surface, carries out die wall lubrication, and former is previously heated to 130 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating enters Row temperature mould high velocity compacted, stroke 30mm, a secondary stroke 40mm after the compacting demoulding, obtain iron silicon phosphorus soft-magnetic composite material base Body；In the iron silicon phosphorus soft-magnetic composite material base substrate handled by finishing, hydrogen atmosphere protection tube furnace, heated up with 5 DEG C/s speed To 1110 DEG C of sintering 0.5h, with 5 DEG C/s speed furnace coolings, iron silicon phosphorus soft-magnetic composite material is finally given.

Claims (6)

1. a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material, it is characterised in that complete in the steps below：
Step 1: water atomized iron powder is at a temperature of 570 DEG C~1150 DEG C, 1~6h of surface oxidation treatment in steam atmosphere, institute Obtain after 110 DEG C of dryings of iron powder, obtain pre-processing straight iron powder；
Step 2: being dried in vacuo blender using bipyramid rotary, lubricant will be bonded and dissolved by heating in organic solvent, pass through height The mode of spray body of calming the anger is sprayed at lubricant solution is bonded in mixing machine, and makes water atomized iron powder, ultra-fine pure silicon powder and super Thin iron phosphorus powder is uniformly mixed, and can be allowed pure silicon powder and iron phosphorus powder are uniformly cohesive to be coated on water atomized iron powder surface, be prevented into Divide segregation, obtain iron silicon phosphorus mixed-powder；
Step 3: lubricant stearic acid lithium is dissolved in acetone, ratio is 100g：1L, is applied to high speed press upper punch surface With die cavity inner surface, die wall lubrication is carried out, former is previously heated to 60 DEG C~150 DEG C, iron silicon phosphorus mixed-powder is sent into and heated Former carry out warm mould high velocity compacted, impact velocity is 1~10m/s, carries out repeat impact compacting, point 2~3 Secondary Shocks, every time Stroke is selected in the range of 0~70mm, or uses relaxation ancillary method, obtains soft-magnetic composite material base substrate；
Step 4: the soft-magnetic composite material base substrate handled by finishing, is sintered in 900 DEG C~1200 DEG C tube furnaces, in sintering During iron silicon phosphorus formation low melting point eutectic phase, reduce sintering temperature, protective atmosphere be hydrogen, nitrogen or inert gas, with 5 DEG C/s speed furnace coolings, finally give iron silicon phosphorus soft-magnetic composite material.
2. a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material according to claim 1, it is characterised in that：Institute in step one State water atomized iron powder, particle diameter≤180 μm, after vapor high-temperature process, surface forms one layer of Fe3O4Coating film.
3. a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material according to claim 1, it is characterised in that：Institute in step 2 State in bipyramid rotary vacuum drying blender, cylinder under vacuum conditions, deep fat is imported in mixing machine interlayer by pump and heats barrel, temperature Degree is between 80 DEG C~150 DEG C；Meanwhile, mixing machine constantly revolution makes material turning, and high-pressure gas pressure is in 0.01MPa~1MPa Between, the bonding lubricant solution ejected forms vaporific, is fully contacted with the material stirred, and alloying element powder is effective Stick on matrix powder surface, and easy volatile solvent contacted with barrel after form steam, drained by vacuum pumped, can carried High rate of drying, forms uniform soft-magnetic alloy powder；There is certain gap between solution line and vacuum tube and drive shaft cavity, It is sealed against by vacuum mud, three rotates when different.
4. a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material according to claim 1 or 3, it is characterised in that：Step 2 Described in bond lubricant solution be dissolved with bond lubricant solution, solution temperature is between 60~100 DEG C, and solvent is vapour Oil, toluene, dimethylbenzene, chloroform, dichloromethane, normal heptane, the mixed solvent of alcohol or wherein single solvent, and easily waving Hair；Lubricant solute is bonded for butadiene-styrene rubber, neoprene, or Tissuemat E, ethylene bis stearic acid amide, stearic acid, polyamides Amine wax, the blend of microwax polymer or wherein single solute；Bond the control of lubricant addition 0.01wt%~ Between 10wt%.
5. a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material according to claim 1, it is characterised in that：Institute in step 2 Superfine silica powder and ultra-fine iron phosphorus powder particle diameter are stated within 1 μm~5 μ ms, iron phosphorus phosphorus content is 22-24%, superfine silica powder and super Thin iron phosphorus powder addition is in the range of 0.05wt%~50wt%.
6. a kind of preparation technology of iron silicon phosphorus soft-magnetic composite material according to claim 1, it is characterised in that：Institute in step 3 It is that the shock wave produced using weight high speed impact stamping reaches densification within the extremely short time to state high velocity compacted, and can be entered Row repeat impact is suppressed, and further improves green density, the relaxation ancillary method, i.e., on upper punch bottom or bottom punch top Install cushion block additional, improve billet surface quality, former heating uses digital temperature control silica gel heating sheet, and maximum heating temperature is 200℃。
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CN109093125A (en) * 2018-09-26 2018-12-28 海安县鹰球粉末冶金有限公司 Magnetic pole shoe material and sintering method for braking
CN112176240A (en) * 2020-09-11 2021-01-05 北京科技大学 Preparation method of high-performance high-aluminum silicon steel
CN114582616A (en) * 2022-01-27 2022-06-03 武汉科技大学 Fe/FeSi composite iron powder core with layered structure and preparation method thereof

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CN109093125A (en) * 2018-09-26 2018-12-28 海安县鹰球粉末冶金有限公司 Magnetic pole shoe material and sintering method for braking
CN109093125B (en) * 2018-09-26 2020-09-29 海安县鹰球粉末冶金有限公司 Magnetic pole shoe material for braking and sintering method
CN112176240A (en) * 2020-09-11 2021-01-05 北京科技大学 Preparation method of high-performance high-aluminum silicon steel
CN112176240B (en) * 2020-09-11 2021-11-26 北京科技大学 Preparation method of high-performance high-aluminum silicon steel
CN114582616A (en) * 2022-01-27 2022-06-03 武汉科技大学 Fe/FeSi composite iron powder core with layered structure and preparation method thereof

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