CN107326264B - A kind of preparation process of iron silicon phosphorus soft-magnetic composite material - Google Patents

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

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CN107326264B
CN107326264B CN201710543013.7A CN201710543013A CN107326264B CN 107326264 B CN107326264 B CN 107326264B CN 201710543013 A CN201710543013 A CN 201710543013A CN 107326264 B CN107326264 B CN 107326264B
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powder
iron
soft
composite material
magnetic composite
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CN107326264A (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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    • 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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Abstract

The present invention provides a kind of iron silicon phosphorus soft-magnetic composite material preparation process, belongs to soft-magnetic composite material technical field.Process flow are as follows: water atomized iron powder is pre-processed using high-temperature vapor processing first, bipyramid rotary vacuum drying blender is recycled to be sprayed combination drying, lubricant solution atomisation will be bonded, with pretreated water atomized iron powder, superfine silica powder and ultra-fine iron phosphorus powder uniformly mix, obtain segregation-free soft magnetic composite powder, high density green compact is prepared by the warm mould high velocity compacted under die wall lubrication, through sintering densification, improve the strength of materials, eliminate internal stress, improve the magnetic conductivity and resistance rate of material, reduce eddy-current loss, finally obtain iron silicon phosphorus soft-magnetic composite material.This iron silicon phosphorus soft-magnetic composite material has the characteristics that high magnetic permeability, low magnetic loss when medium-high frequency application.The present invention is simple, and manufacturing cost is low.

Description

A kind of preparation process 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 combines.
Background technique
Si fe alloy is a kind of power electronics and the indispensable important soft magnetic alloy of war industry, be mainly used for motor, The iron core of generator and transformer has 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, needs to use after insulation processing by laminating technology, compares powder metallurgical technique For, the latter is more for advantage, with the mixture of iron silicon powder, iron powder, silicon powder and iron phosphorus powder, the height through high velocity compacted sintering preparation Density core material has three-dimensional magnetic isotropy, low-down eddy-current loss, relatively low total magnetic loss (medium-high frequency), height Saturation magnetic sense intensity, meanwhile, heat treatment temperature reduce, scantling and cost is greatly reduced.It has broad application prospects.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing iron silicon phosphorus soft-magnetic composite material, it is intended to it is compound to improve soft magnetism The magnetic conductivity of material, intensity reduce magnetic loss.
1, a kind of preparation process 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 pretreatment straight iron powder；
Step 2: being dried in vacuo blender using a kind of bipyramid rotary, a kind of bonding lubricant is dissolved by heating organic In solvent, it is sprayed in mixing machine by the spraying mode of high pressure gas by lubricant solution is bonded, makes water atomized iron powder, surpasses Thin pure silicon powder and ultra-fine iron phosphorus powder uniformly mix, and pure silicon powder and iron phosphorus powder can be allowed uniformly to bond and 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 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 It hits, each stroke selects within the scope of 0~70mm, and relaxation ancillary measure can also be used, and obtains soft-magnetic composite material green body；
Step 4: be sintered in 900 DEG C~1200 DEG C tube furnaces by the soft-magnetic composite material green body that finishing is handled, In sintering process iron silicon phosphorus formed low melting point eutectic phase, reduce sintering temperature, protective atmosphere be hydrogen, nitrogen or inert gas, With 5 DEG C/s speed furnace cooling, iron silicon phosphorus soft-magnetic composite material is finally obtained.
Further, water atomized iron powder described in step 1, partial size≤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 blender, in cylinder under vacuum conditions, hot oil It is imported in mixing machine interlayer by pump and heats barrel, temperature is between 80 DEG C~150 DEG C.Meanwhile mixing machine constantly turns round makes material It stirs, for high-pressure gas pressure between 0.01MPa~1MPa, the bonding lubricant solution ejected forms mist, and stirs Material comes into full contact with, and alloying element powder is effectively adhered on matrix powder surface, and easy volatile solvent connects with barrel Steam is formed after touch, is drained by vacuum pump extraction, rate of drying can be improved, form uniform soft-magnetic alloy powder.Solution line There are certain gaps between vacuum tube and drive shaft cavity, are sealed against by vacuum mud, and three does not rotate simultaneously.
Further, bonding lubricant solution described in step 2 is the solution dissolved with bonding lubricant, and solution temperature exists Between 60~100 DEG C, solvent can be the mixing of gasoline, toluene, dimethylbenzene, chloroform, methylene chloride, normal heptane, alcohol Solvent or in which single solvent, and it is volatile；Solute bonding lubricant can be butadiene-styrene rubber, neoprene or polyethylene The blend of the polymer such as wax, ethylene bis stearic acid amide, stearic acid, polyamide wax, microwax or in which single solute.Bonding Lubricant additive amount controls between 0.01wt%~10wt%.
Superfine silica powder described in step 2 and ultra-fine iron phosphorus powder partial size are within 1 μm~5 μ ms, iron phosphorus phosphorus content 22- 24%, the two additional amount is within the scope of 0.05wt%~50wt%.
Further, high velocity compacted described in step 3 is a kind of high density parts forming new technology, it is high using weight The shock wave that speed impact stamping generates reaches densification in a very short period of time, and can carry out repeat impact compacting, into one Step improves green density, the relaxation ancillary measure installs cushion block additional in upper punch lower part or bottom punch top, base can be improved Body surface quality, using digital temperature control silica gel heating sheet, maximum heating temperature is 200 DEG C for former heating.
The present invention has the advantages 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 being able to maintain certain magnetism；(2) mixed through the mixed iron silicon phosphorus of spraying bonding Powder is closed, without being dried, it is i.e. usable not need to be blended into lubricant yet；(3) the warm mould high velocity compacting technique used can To improve green density, intergranular air gap distribution is reduced, improves the magnetic conductivity and saturation induction density of material, bonding lubrication The addition of agent can protect the integrality of insulating coating, improve resistivity, reduce loss；(4) the mixed ultra-fine pure silicon powder of institute The higher clad of a layer resistivity can be formed during the sintering process with ultra-fine iron phosphorus powder, reduces eddy-current loss, reduce material Internal stress, while the two is sintered to form low-melting compound, can reduce sintering temperature, further increase consistency.It is one The technique that kind high efficiency prepares iron silicon phosphorus soft-magnetic composite material.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment 1:Fe-3.5%Si-1.5%P soft-magnetic composite material preparation process
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 dry, pretreatment straight iron powder is obtained；500g soft magnetism is blended by the formula of Fe-3.5%Si-1.5%P Mixed-powder needs ultra-fine pure silicon powder 17.5g, needs to weigh ultra-fine iron phosphorus powder 32.6g, and water atomized iron powder 450g will be weighed up Water atomized iron powder and alloy powder by hand premix after, pour into bipyramid rotary vacuum drying blender barrel in it is dry-mixed 0.5h opens simultaneously Heat-transfer Oil Pump, and 120 DEG C of temperature of conduction oil is pumped into barrel interlayer, circulating-heating heat preservation；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 methylene chloride and It is spare after dissolved clarification in normal heptane (1:3) solvent；Steps are as follows for sprinkling: (1) in 20min, starting 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 vacuum pump；(3) will 200ml lubricant solution sucks Mono pump under heated condition, through conveyance conduit under stream pressure, is sprayed by the nozzle in barrel It nebulizes, with admixture of powder in barrel；(4) after having sprayed, nitrogen is closed, remixes 0.5h, vacuum pump reruns and closes after 15min It closes, the solvent discharge that will volatilize；(5) shift to an earlier date 10min, then take 200ml solution, with (3) step operation, after the completion, with (4) step Suddenly, 0.5h is remixed；(6) finally that remaining 100ml lubricant solution is sprayed, same to step (3) and (4), after mixing 0.5h, Close barrel switch, co-blended 2h；Lubricant stearic acid lithium is dissolved in acetone, ratio 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 obtains iron silicon phosphorus soft-magnetic composite material green body after compacting demoulding；Through The iron silicon phosphorus soft-magnetic composite material green body for crossing finishing processing in hydrogen atmosphere protection tube furnace, is warming up to 900 with 5 DEG C/s speed DEG C sintering 0.5h with 5 DEG C/s speed furnace cooling finally obtains iron silicon phosphorus soft-magnetic composite material.
Embodiment 2:Fe-6.5%Si-1.0%P soft-magnetic composite material preparation process
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 dry, pretreatment straight iron powder is obtained；500g soft magnetism is blended by the formula of Fe-6.5%Si-1.0%P Mixed-powder needs ultra-fine pure silicon powder 32.5g, needs to weigh ultra-fine iron phosphorus powder 21.7g, and water atomized iron powder 446g will be weighed up Water atomized iron powder and alloy powder by hand premix after, pour into bipyramid rotary vacuum drying blender barrel in it is dry-mixed 0.5h opens simultaneously Heat-transfer Oil Pump, and 120 DEG C of temperature of conduction oil is pumped into barrel interlayer, circulating-heating heat preservation；It is derived from viscous Lubricant polymer blend 0.3wt%, i.e. 1.5g are tied, 500ml chloroform is dissolved in temperature for 80 DEG C and normal heptane (1:3) is molten It is spare after dissolved clarification in agent；Steps are as follows for sprinkling: (1) in 20min, starting 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 vacuum pump；(3) 200ml lubricant is molten Liquid sucks Mono pump under 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, remixes 0.5h, vacuum pump, which reruns, closes after 15min, and what be will volatilize is molten Agent discharge；(5) shift to an earlier date 10min, then take 200ml solution, with (3) step operation, after the completion, with (4) step, remix 0.5h； (6) finally that remaining 100ml lubricant solution is sprayed, barrel switch after mixing 0.5h, is closed in same step (3) and (4), Co-blended 2h；Lubricant stearic acid lithium is dissolved in acetone, ratio 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, by iron silicon phosphorus mixed-powder be sent into the former of heating into Row temperature mould high velocity compacted, stroke 50mm obtain iron silicon phosphorus soft-magnetic composite material green body after compacting demoulding；By finishing processing Iron silicon phosphorus soft-magnetic composite material green body in hydrogen atmosphere protection tube furnace, is warming up to 1050 DEG C of sintering 0.5h with 5 DEG C/s speed, With 5 DEG C/s speed furnace cooling, iron silicon phosphorus soft-magnetic composite material is finally obtained.
Embodiment 3:Fe-10%Si-2.0%P soft-magnetic composite material preparation process
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 dry, pretreatment straight iron powder is obtained；500g soft magnetism is blended by the formula of Fe-10%Si-2.0%P Mixed-powder needs ultra-fine pure silicon powder 50g, needs to weigh ultra-fine iron phosphorus powder 43.5g, and water atomized iron powder 406.5g will be weighed up Water atomized iron powder and alloy powder by hand premix after, pour into bipyramid rotary vacuum drying blender barrel in it is dry-mixed 0.5h opens simultaneously Heat-transfer Oil Pump, and 120 DEG C of temperature of conduction oil is pumped into barrel interlayer, circulating-heating heat preservation；It is derived from viscous Lubricant polymer blend 0.2wt%, i.e. 1.0g are tied, 500ml chloroform is dissolved in temperature for 80 DEG C and normal heptane (1:3) is molten It is spare after dissolved clarification in agent；Steps are as follows for sprinkling: (1) in 20min, starting 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 vacuum pump；(3) 200ml lubricant is molten Liquid sucks Mono pump under 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, remixes 0.5h, vacuum pump, which reruns, closes after 15min, and what be will volatilize is molten Agent discharge；(5) shift to an earlier date 10min, then take 200ml solution, with (3) step operation, after the completion, with (4) step, remix 0.5h； (6) finally that remaining 100ml lubricant solution is sprayed, barrel switch after mixing 0.5h, is closed in same step (3) and (4), Co-blended 2h；Lubricant stearic acid lithium is dissolved in acetone, ratio 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, by iron silicon phosphorus mixed-powder be sent into the former of heating into Row temperature mould high velocity compacted, stroke 30mm, a secondary stroke 40mm obtain iron silicon phosphorus soft-magnetic composite material base after compacting demoulding Body；By the iron silicon phosphorus soft-magnetic composite material green body that finishing is handled, in hydrogen atmosphere protection tube furnace, with the heating of 5 DEG C/s speed Iron silicon phosphorus soft-magnetic composite material is finally obtained with 5 DEG C/s speed furnace cooling to 1110 DEG C of sintering 0.5h.

Claims (3)

1. a kind of preparation process 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, and 1~6h of surface oxidation treatment in steam atmosphere, institute After obtaining 110 DEG C of dryings of iron powder, pretreatment straight iron powder is obtained；
Step 2: being dried in vacuo blender using bipyramid rotary, bonding lubricant is dissolved by heating in organic solvent, height is passed through 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 uniformly mixes, and pure silicon powder and iron phosphorus powder can be allowed uniformly to bond and be coated on water atomized iron powder surface, prevented into Divide segregation, obtains iron silicon phosphorus mixed-powder；
Step 3: lubricant stearic acid lithium is dissolved in acetone, ratio 100g:1L, it 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, and iron silicon phosphorus mixed-powder is sent into and is heated Former carry out warm mould high velocity compacted, impact velocity is 1~10m/s, carry out repeat impact compacting, point 2~3 Secondary Shocks, every time Stroke selects within the scope of 0~70mm, or uses relaxation ancillary measure, obtains soft-magnetic composite material green body；
Step 4: being sintered, being sintered in 900 DEG C~1200 DEG C tube furnaces by the soft-magnetic composite material green body that finishing is handled Iron silicon phosphorus forms low melting point eutectic phase in the process, reduces sintering temperature, protective atmosphere is hydrogen, nitrogen or inert gas, with 5 DEG C/s speed furnace cooling, finally obtain iron silicon phosphorus soft-magnetic composite material；
Water atomized iron powder described in step 1, partial size≤180 μm, after vapor high-temperature process, surface forms one layer of Fe3O4 Coating film；
Within 1 μm~5 μ ms, iron phosphorus phosphorus content is 22- for superfine silica powder described in step 2 and ultra-fine iron phosphorus powder partial size 24%, superfine silica powder and ultra-fine iron phosphorus powder additional amount are within the scope of 0.05wt%~50wt%；
High velocity compacted described in step 3 is that the shock wave generated using weight high speed impact stamping is reached in a very short period of time Densification, and can be carried out repeat impact compacting, further increase green density, the relaxation ancillary measure, i.e., in upper punch Lower part or bottom punch top install cushion block additional, improve billet surface quality, and former is heated using digital temperature control silica gel heating sheet, Maximum heating temperature is 200 DEG C.
2. a kind of preparation process of iron silicon phosphorus soft-magnetic composite material according to claim 1, it is characterised in that: institute in step 2 Bipyramid rotary vacuum drying blender is stated, in cylinder under vacuum conditions, hot oil 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 turns round makes material turning, high-pressure gas pressure is in 0.01MPa~1MPa Between, the bonding lubricant solution ejected forms mist, comes into full contact with the material stirred, and alloying element powder is effective Be adhered on matrix powder surface, and easy volatile solvent contacted with barrel after form steam, by vacuum pump extraction drain, can mention High rate of drying forms uniform soft-magnetic alloy powder；There are certain gap between solution line and vacuum tube and drive shaft cavity, It is sealed against by vacuum mud, three does not rotate simultaneously.
3. a kind of preparation process of iron silicon phosphorus soft-magnetic composite material according to claim 1 or claim 2, it is characterised in that: step 2 Described in bonding lubricant solution be dissolved with bonding lubricant solution, for solution temperature between 60~100 DEG C, solvent is vapour Oil, toluene, dimethylbenzene, chloroform, methylene chloride, normal heptane, alcohol mixed solvent or in which single solvent, and easily wave Hair；Bonding lubricant solute is butadiene-styrene rubber, neoprene or polyethylene wax, ethylene bis stearic acid amide, stearic acid, polyamides The blend or in which single solute of amine wax, microwax polymer；Bond lubricant additive amount control 0.01wt%~ Between 10wt%.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1580770A2 (en) * 2004-03-22 2005-09-28 Aisin Seiki Kabushiki Kaisha Soft magnetic powder and a method of manufacturing a soft magnetic powder compact
CN102306525A (en) * 2011-05-19 2012-01-04 浙江科达磁电有限公司 Fe-Si alloy soft magnetic material with magnetic permeability mu of 26 and manufacturing method for Fe-Si alloy soft magnetic material
CN103305743A (en) * 2013-06-18 2013-09-18 北京科技大学 Method for preparing pure iron and iron-phosphorus magnetically soft alloy product through powder metallurgy process
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1580770A2 (en) * 2004-03-22 2005-09-28 Aisin Seiki Kabushiki Kaisha Soft magnetic powder and a method of manufacturing a soft magnetic powder compact
CN102306525A (en) * 2011-05-19 2012-01-04 浙江科达磁电有限公司 Fe-Si alloy soft magnetic material with magnetic permeability mu of 26 and manufacturing method for Fe-Si alloy soft magnetic material
CN103305743A (en) * 2013-06-18 2013-09-18 北京科技大学 Method for preparing pure iron and iron-phosphorus magnetically soft alloy product through powder metallurgy process
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

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