CN107256752B - A kind of preparation method being sintered iron powder base soft-magnetic composite material - Google Patents
A kind of preparation method being sintered iron powder base soft-magnetic composite material Download PDFInfo
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- CN107256752B CN107256752B CN201710542594.2A CN201710542594A CN107256752B CN 107256752 B CN107256752 B CN 107256752B CN 201710542594 A CN201710542594 A CN 201710542594A CN 107256752 B CN107256752 B CN 107256752B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 239000007921 spray Substances 0.000 claims abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 12
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- SHXJBKVHXUNDLB-UHFFFAOYSA-N [Si].[P].[Fe] Chemical compound [Si].[P].[Fe] SHXJBKVHXUNDLB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005461 lubrication Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 22
- 239000011812 mixed powder Substances 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 13
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- 238000000889 atomisation Methods 0.000 claims description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- HGPXWXLYXNVULB-UHFFFAOYSA-M lithium stearate Chemical compound [Li+].CCCCCCCCCCCCCCCCCC([O-])=O HGPXWXLYXNVULB-UHFFFAOYSA-M 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 6
- 239000011574 phosphorus Substances 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000000741 silica gel Substances 0.000 claims description 6
- 229910002027 silica gel Inorganic materials 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 5
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 5
- 239000000725 suspension Substances 0.000 claims description 5
- 239000001993 wax Substances 0.000 claims description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 4
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyethylene Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical compound C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims description 3
- 239000004200 microcrystalline wax Substances 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims description 3
- 230000035939 shock Effects 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 229920001084 poly(chloroprene) Polymers 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims 1
- 229920002647 polyamide Polymers 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 5
- 239000008187 granular material Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 230000005291 magnetic effect Effects 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 6
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 0.000 description 3
- 229910001096 P alloy Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000009766 low-temperature sintering Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- NJPPVKZQTLUDBO-UHFFFAOYSA-N novaluron Chemical group C1=C(Cl)C(OC(F)(F)C(OC(F)(F)F)F)=CC=C1NC(=O)NC(=O)C1=C(F)C=CC=C1F NJPPVKZQTLUDBO-UHFFFAOYSA-N 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- H01F1/20—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 in the form of particles, e.g. powder
- H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention provides a kind of preparation method for being sintered iron powder base soft-magnetic composite material, 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, Double cone spray blender is recycled to carry out cohesion processing, binder solution is atomized under the action of high pressure gas and is uniformly sprayed on the material constantly to roll, by ultra-fine pure silicon powder and ultra-fine ferrophosphor(us) powder uniform adhesion on ferrous powder granules surface, bonded iron-based powder is obtained.High density green compact is prepared by the warm mould high velocity compacted under die wall lubrication, is densified through low temperature Fast Sintering, finally obtains iron silicon phosphorus soft-magnetic composite material.Resulting sintering iron powder base soft-magnetic composite material had not only had the characteristics that soft-magnetic composite material magnetic conductivity was high, eddy-current loss is low, but also had the advantages that sintering soft-magnetic composite material intensity is high, was suitble to frequency applications.
Description
Technical field
The invention belongs to soft-magnetic composite material technical fields, are related to a kind of with iron powder steam treatment, Double cone spray formula bonding
The method that change processing, warm mold high speed compacting and low-temperature sintering combine preparation sintering soft-magnetic composite material.
Background technique
Iron powder base soft-magnetic composite material by powder particle surface carry out insulating processing, then use powder metallurgical technique
A kind of electromagnetic application material of preparation.The resistivity of soft-magnetic composite material is high, and eddy-current loss is low in alternating magnetic field, be suitable for compared with
It is used under high-frequency, in electrician, electric power and electronic equipment, as electromagnet core, breaker iron core, transformer core, motor are fixed
There is important application in the fields such as the iron core of son and rotor.Traditional iron powder base soft-magnetic composite material passes through organic and inorganic materials
Cladding obtain insulating layer, then use compression moulding, be not necessarily to high temperature sintering, since the intensity of material is low, it is multiple to limit soft magnetism
The popularization and application of condensation material.
The present invention is using iron powder steam treatment, the processing of Double cone spray formula cohesion, warm mold high speed compacting and low-temperature sintering
The technique preparation sintering iron powder base soft-magnetic composite material combined.Steam treated is carried out to ferrous powder granules first, in particle surface
Form one layer of very thin Fe3O4Oxidation film is coated, plays the role of interface diffusion barrier layer and hinders counterdiffusion between matrix and Si.
Then fine silicon powder and ferrophosphor(us) powder are evenly coated at by ferrous powder granules surface using cohesion technique.Finally using temperature
The forming of mould high velocity compacting technique, obtains highdensity green compact, promotes the diffusion of element.Powder high velocity compacted is to utilize weight high speed
The enormous impact wave energy that impact generates densifies metal powder in a short period of time, has pressing speed height, green compact close
The advantage that degree is high and Density Distribution is uniform, elastic after effect and knockout press are low, and repeat impact compacting can be carried out, further mention
High green density.By adding ferrophosphor(us), low melting point eutectic phase, the liquid formed in sintering process are formed at a lower temperature
Phase acceleration of sintering process, solve under high temperature sintering Si element in the base quick diffusion-homogenization and cannot be formed has high electricity
The interface iron silicon phase of resistance rate, the problem of increasing eddy-current loss.It is equal to be sintered ferrous powder granules surface in iron powder base soft-magnetic composite material
The iron silicon phase of even one layer thin of cladding, has ferromagnetic atomic ordered structure and high resistivity, reduces the vortex damage of composite material
Consumption, the presence of oxide layer hinder in sintering process Si atom to the diffusion inside iron particle.Resulting sintering iron powder base soft magnetism
Composite material had not only had the characteristics that soft-magnetic composite material eddy-current loss was low, but also had high excellent of sintering soft-magnetic composite material intensity
Point.
Summary of the invention
The purpose of the present invention is to provide a kind of methods for preparing sintering iron powder base soft-magnetic composite material, it is intended to improve iron powder
Consistency, magnetic conductivity and the intensity of base soft-magnetic composite material.
A kind of preparation process being sintered iron powder base soft-magnetic composite material, specific process step have:
1, iron powder steam treatment: using 80-180 μm of water atomized iron powder as raw material, powder is at 570~1150 DEG C, Yu Shui
1~6h of surface oxidation treatment is carried out in vapor atmosphere, the iron powder after steam treatment is 1-5 hours dry at 80-120 DEG C, obtains pre-
Handle iron powder.
2, mixed-powder cohesion is handled: by pretreatment powder and 0.1-5 μm of ultra-fine pure silicon powder and 1-5 μm of ultra-fine iron
Phosphorus alloy powder premixing uniformly, obtains mixed-powder.Mixed-powder carries out cohesion processing in Double cone spray blender, first
First by binder 60~100 DEG C at a temperature of be dissolved in solvent, form binder solution, binder solution is heated to 80-
100 DEG C, then enter in Double cone spray blender under the carrying of high pressure gas, binder solution is atomized and is uniformly sprayed at
On the material constantly to roll, 1-5h is mixed, obtains cohesion processing powder.
Wherein the phosphorus content in ferrophosphor(us) is 15-23%.
The binder is butadiene-styrene rubber, neoprene or polyethylene wax, ethylene bis stearic acid amide, stearic acid, gathers
One or more of amide waxe, microwax.
The solvent be one of gasoline, toluene, dimethylbenzene, chloroform, methylene chloride, normal heptane and alcohol or
It is several.
The content of binder is 0.05wt%~10wt% in the binder solution, and the solution temperature of binder is
60-90℃。
The Double cone spray blender band heating jacket, is heated, heating temperature is 80 DEG C~180 using conduction oil
DEG C, pressure is (0.8-0.9) × 10 in blender-5Pa.The rotational speed of mixing machine is 100-200 revs/min, the center of blender
Atomizer is arranged in position, and high pressure gas carries binder solution and is atomized at nozzle, atomization pressure 0.1-0.5MPa,
The flow of atomization binder is 0.1-0.5 ls/h.The heating temperature of binder is 100-200 DEG C, incorporation time 1-5
Hour.
3, warm mould high velocity compacted: bonded iron-based powder is suppressed on high-rate forming press, press strokes 30-
70mm, corresponding rate of suppressing is 6.2-9.4m/s, and compacting energy is 795-1855J.Use lithium stearate alcohol suspension as
Die wall lubricant, is applied to high speed press upper punch surface and die cavity inner surface carries out die wall lubrication.Former uses digital temperature control
Silica gel piece is heated, and heating temperature is 60 DEG C -150 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating is carried out Wen Mogao
Ram compression system can carry out repeat impact compacting, and point 2~3 Secondary Shocks obtain soft-magnetic composite material green body.
4, sintering densification: soft-magnetic composite material green body carries out low-temperature short-time sintering, sintering temperature in flowing hydrogen atmosphere
Degree is 900 DEG C -1200 DEG C, soaking time 10-30min.It is cooling with the speed of 1-3 DEG C/min after heat preservation, obtain iron powder
Base soft-magnetic composite material.
The present invention has the advantages that water atomized iron powder forms Fe after vapor high-temperature process3O4Film can prevent
Water atomized iron powder end surface continues to aoxidize, while being able to maintain certain magnetism；Cohesion is carried out using Double cone spray blender
Processing, binder is atomized under the action of high pressure gas, comes into full contact with the material stirred, by ultra-fine pure silicon powder and ultra-fine iron
Phosphorus alloy powder uniform adhesion obtains bonded iron-based powder on ferrous powder granules surface.From iron powder is during heating mixing
To processing hardening is reduced, soft annealing effect effectively improves compressibility.It is in negative pressure, easy volatile solvent and barrel in blender
Steam is formed after contact, steam is extracted out by vacuum pump, improves rate of drying.Warm mould high velocity compacting technique can effectively improve pressure
Base density reduces intergranular air gap distribution, improves the magnetic conductivity and saturation induction density of material；What is uniformly coated is ultra-fine pure
Silicon powder and ultra-fine iron phosphorus powder form low melting point eutectic phase under lower sintering temperature, reduce sintering temperature, obtain one layer high electricity
The clad of resistance rate, clad is complete, reduces eddy-current loss, improves the consistency and intensity of composite material.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Fig. 2 is the schematic diagram of Double cone spray blender.
The names of the parts are as follows in figure:
1 is support shaft, and 2 be mixing tank, and 3 be interlayer, and 4 be vacuum tube, and 5 be nozzle, and 6 be discharge port, and 7 be high pressure gas, 8
It is pedestal for motor, 9,10 be conduction oil.
Specific embodiment
Embodiment 1:Fe-3.5%Si-1.5%P soft-magnetic composite material preparation process
Using 150 μm of water atomized iron powder, 3 μm of ultra-fine pure silicon powder and 5 μm of ultra-fine ferrophosphor(us) powder as raw material,
Phosphorus content in middle ferrophosphor(us) is 23%.Water atomized iron powder end carries out at surface oxidation in water vapour atmosphere at 950 DEG C
3h is managed, the iron powder after steam treatment is 1 hour dry at 110 DEG C, obtains pretreatment iron powder；Will pretreatment iron powder and pure silicon powder and
The premixing of ferrophosphor(us) powder uniformly, obtains mixed-powder.Mixed-powder carries out cohesion processing in Double cone spray blender.
Binder is butadiene-styrene rubber, and solvent is methylene chloride.In binder solution the content of binder be 0.3wt%, binder it is molten
Solving temperature is 80 DEG C.First by binder 80 DEG C at a temperature of be dissolved in solvent, formed binder solution, binder solution quilt
90 DEG C are heated to, is then entered in Double cone spray blender under the carrying of high pressure gas, binder solution is atomized simultaneously uniformly
It is sprayed on the material constantly to roll, mixes 2h, obtain cohesion processing powder.The heating temperature of Double cone spray blender is
120 DEG C, pressure is 0.85 × 10 in blender-5Pa.The rotational speed of mixing machine is 150 revs/min, and atomization pressure is
0.15MPa, the flow of atomization binder are 0.2 l/h.Bonded iron-based powder is pressed on high-rate forming press
System, press strokes 60mm, corresponding rate of suppressing is 8.7m/s, and compacting energy is 1590J.With lithium stearate alcohol suspension
As die wall lubricant, it is applied to high speed press upper punch surface and die cavity inner surface carries out die wall lubrication.Former is using number
Temperature control silica gel piece is heated, and heating temperature is 100 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating is carried out warm mould high speed
Compacting carries out one-shot compacting, obtains soft-magnetic composite material green body.Soft-magnetic composite material green body in flowing hydrogen atmosphere into
Row sintering, sintering temperature are 970 DEG C, soaking time 20min.It is cooling with the speed of 3 DEG C/min after heat preservation, obtain iron powder
Base soft-magnetic composite material.
Embodiment 2:Fe-6.5%Si-2.0%P soft-magnetic composite material preparation process
Using 180 μm of water atomized iron powder, 2 μm of ultra-fine pure silicon powder and 3 μm of ultra-fine ferrophosphor(us) powder as raw material,
Wherein the phosphorus content in ferrophosphor(us) is 21%.Water atomized iron powder end carries out surface oxidation at 900 DEG C in steam atmosphere
1h is handled, the iron powder after steam treatment is 1.5 hours dry at 120 DEG C, obtains pretreatment iron powder；It will pretreatment iron powder and pure silicon powder
End and the premixing of ferrophosphor(us) powder uniformly, obtain mixed-powder.Mixed-powder carries out cohesion in Double cone spray blender
Processing.Binder is polyethylene wax, and solvent is normal heptane.The content of binder is 0.4wt% in binder solution, binder
Solution temperature is 60 DEG C.First by binder 60 DEG C at a temperature of be dissolved in solvent, formed binder solution, binder solution
80 DEG C are heated to, is then entered in Double cone spray blender under the carrying of high pressure gas, binder solution is atomized simultaneously
It is even to be sprayed on the material constantly to roll, 1.5h is mixed, cohesion processing powder is obtained.The heating temperature of Double cone spray blender
It is 130 DEG C, pressure is 0.8 × 10 in blender-5Pa.The rotational speed of mixing machine is 200 revs/min, and atomization pressure is
0.3MPa, the flow of atomization binder are 0.3 l/h.Bonded iron-based powder is suppressed on high-rate forming press,
Press strokes are 70mm, and corresponding rate of suppressing is 9.4m/s, and compacting energy is 1855J.Made with lithium stearate alcohol suspension
For die wall lubricant, it is applied to high speed press upper punch surface and die cavity inner surface carries out die wall lubrication.Former is using number temperature
Control silica gel piece is heated, and heating temperature is 90 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating is carried out Wen Mogao ram compression
System carries out one-shot compacting, obtains soft-magnetic composite material green body.Soft-magnetic composite material green body carries out in flowing hydrogen atmosphere
Sintering, sintering temperature are 1050 DEG C, soaking time 15min.It is cooling with the speed of 3 DEG C/min after heat preservation, obtain iron powder
Base soft-magnetic composite material.
Embodiment 3:Fe-4.0%Si-2.5%P soft-magnetic composite material preparation process
Using 100 μm of water atomized iron powder, 5 μm of ultra-fine pure silicon powder and 1 μm of ultra-fine ferrophosphor(us) powder as raw material,
Wherein the phosphorus content in ferrophosphor(us) is 22%.Water atomized iron powder end carries out Surface Oxygen at 1050 DEG C in steam atmosphere
Change processing 1h, the iron powder after steam treatment is 1 hour dry at 100 DEG C, obtains pretreatment iron powder；It will pretreatment iron powder and pure silicon powder
End and the premixing of ferrophosphor(us) powder uniformly, obtain mixed-powder.Mixed-powder carries out cohesion in Double cone spray blender
Processing.Binder is polyethylene wax, ethylene bis stearic acid amide and stearic blend.Solvent is chloroform, normal heptane
With the mixed solvent of alcohol.The content of binder is 0.2wt% in binder solution, and the solution temperature of binder is 85 DEG C.It is first
First by binder 85 DEG C at a temperature of be dissolved in solvent, form binder solution, binder solution is heated to 95 DEG C, then
Enter in Double cone spray blender under the carrying of high pressure gas, binder solution, which is atomized and is uniformly sprayed at, constantly to roll
On material, 2h is mixed, obtains cohesion processing powder.The heating temperature of Double cone spray blender is 140 DEG C, pressure in blender
It is 0.9 × 10-5Pa.The rotational speed of mixing machine is 140 revs/min, atomization pressure 0.25MPa, atomization binder
Flow is 0.4 l/h.Bonded iron-based powder is suppressed on high-rate forming press, and press strokes are 30mm and 40mm,
Corresponding compacting rate is respectively 6.2m/s and 7.1m/s, and compacting energy is respectively 795J and 1060J.It is outstanding with lithium stearate alcohol
Supernatant liquid is applied to high speed press upper punch surface and die cavity inner surface carries out die wall lubrication as die wall lubricant.Former uses
Digital temperature control silica gel piece is heated, and heating temperature is 110 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating is carried out Wen Mo
High velocity compacted carries out secondary pulse compacting, obtains soft-magnetic composite material green body.Soft-magnetic composite material green body is in flowing hydrogen atmosphere
In be sintered, sintering temperature be 1070 DEG C, soaking time 30min.It is cooling with the speed of 1 DEG C/min after heat preservation, it obtains
To iron powder base soft-magnetic composite material.
Embodiment 4:Fe-10%Si-3.0%P soft-magnetic composite material preparation process
Using 75 μm of water atomized iron powder, 5 μm of ultra-fine pure silicon powder and 5 μm of ultra-fine ferrophosphor(us) powder as raw material,
Phosphorus content in middle ferrophosphor(us) is 23%.Water atomized iron powder end carries out surface oxidation at 1100 DEG C in steam atmosphere
1h is handled, the iron powder after steam treatment is 1 hour dry at 120 DEG C, obtains pretreatment iron powder；It will pretreatment iron powder and pure silicon powder
Uniformly with the premixing of ferrophosphor(us) powder, mixed-powder is obtained.Mixed-powder carries out at cohesion in Double cone spray blender
Reason.Binder is the blend of ethylene bis stearic acid amide, stearic acid and microwax.Solvent is methylene chloride, normal heptane and wine
The mixed solvent of essence.The content of binder is 0.3wt% in binder solution, and the solution temperature of binder is 90 DEG C.First will
Binder 90 DEG C at a temperature of be dissolved in solvent, formed binder solution, binder solution is heated to 95 DEG C, then in height
Calm the anger body carrying under enter in Double cone spray blender, binder solution is atomized and is uniformly sprayed at the material constantly to roll
On, 2h is mixed, cohesion processing powder is obtained.The heating temperature of Double cone spray blender is 110 DEG C, and pressure is in blender
0.8×10-5Pa.The rotational speed of mixing machine is 180 revs/min, atomization pressure 0.1MPa, the atomization flow of binder
It is 0.25 l/h.Bonded iron-based powder is suppressed on high-rate forming press, press strokes 65mm, corresponding to press
Rate processed is 9.1m/s, and compacting energy is 1722.5J.It uses lithium stearate alcohol suspension as die wall lubricant, is applied to height
Ram compression machine upper punch surface and die cavity inner surface carry out die wall lubrication.Former is heated using digital temperature control silica gel piece, is heated
Temperature is 100 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating is carried out warm mould high velocity compacted, carries out one-shot compacting,
Obtain soft-magnetic composite material green body.Soft-magnetic composite material green body is sintered in flowing hydrogen atmosphere, sintering temperature 1110
DEG C, soaking time 10min.It is cooling with the speed of 2 DEG C/min after heat preservation, obtain iron powder base soft-magnetic composite material.
Claims (5)
1. a kind of preparation method for being sintered iron powder base soft-magnetic composite material, it is characterised in that:
Step 1: using 80-180 μm of water atomized iron powder as raw material, powder at 570~1150 DEG C, in steam atmosphere into
Row 1~6h of surface oxidation treatment, the iron powder after steam treatment is 1-5 hours dry at 80-120 DEG C, obtains pretreatment iron powder；
It is pre-mixed Step 2: powder will be pre-processed with 0.1-5 μm of ultra-fine pure silicon powder and 1-5 μm of ultra-fine ferrophosphor(us) powder
It is even, obtain mixed-powder；Mixed-powder carries out cohesion processing in Double cone spray blender, first by binder 60~
It is dissolved in solvent at a temperature of 100 DEG C, forms binder solution, binder solution is heated to 80-100 DEG C, then in high pressure
Enter in Double cone spray blender under the carrying of gas, binder solution is atomized and is uniformly sprayed at the material constantly to roll
On, 1-5h is mixed, cohesion processing powder is obtained；
Step 3: the described Double cone spray blender band heating jacket, is heated using conduction oil, heating temperature is 80 DEG C~
180 DEG C, pressure is (0.8-0.9) × 10 in blender-5Pa；The rotational speed of mixing machine is 100-200 revs/min, blender
Atomizer is arranged in centre, and high pressure gas carries binder solution and is atomized at nozzle, atomization pressure 0.1-
The flow of 0.5MPa, atomization binder are 0.1-0.5 ls/h；The heating temperature of binder is 100-200 DEG C, when mixing
Between be 1-5 hours；
Step 4: bonded iron-based powder is suppressed on high-rate forming press, press strokes 30-70mm is corresponding to press
Rate processed is 6.2-9.4m/s, and compacting energy is 795-1855J；It uses lithium stearate alcohol suspension as die wall lubricant, applies
It is put on high speed press upper punch surface and die cavity inner surface carries out die wall lubrication；Former is added using digital temperature control silica gel piece
Heat, heating temperature are 60 DEG C -150 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating is carried out warm mould high velocity compacted, is carried out more
Secondary Shocks compacting, point 2~3 Secondary Shocks obtain soft-magnetic composite material green body；
Step 5: soft-magnetic composite material green body carries out low-temperature short-time sintering in flowing hydrogen atmosphere, with 1-3 after heat preservation
DEG C/speed of min is cooling, obtain iron powder base soft-magnetic composite material；
Low-temperature short-time sintering temperature described in step 5 is 900 DEG C -1200 DEG C, soaking time 10-30min.
2. a kind of preparation method for being sintered iron powder base soft-magnetic composite material according to claim 1, it is characterised in that: step 1
Described in phosphorus content in ferrophosphor(us) be 15-23%.
3. a kind of preparation method for being sintered iron powder base soft-magnetic composite material according to claim 1, it is characterised in that: step 1
Described in binder be butadiene-styrene rubber, neoprene or polyethylene wax, ethylene bis stearic acid amide, stearic acid, polyamide
One or more of wax, microwax.
4. a kind of preparation method for being sintered iron powder base soft-magnetic composite material according to claim 1, it is characterised in that: step 1
Described in solvent be one or more of gasoline, toluene, dimethylbenzene, chloroform, methylene chloride, normal heptane and alcohol.
5. a kind of preparation method for being sintered iron powder base soft-magnetic composite material according to claim 1, it is characterised in that: step 1
Described in binder solution in the content of binder be 0.05wt%~10wt%, the solution temperature of binder is 60-90 DEG C.
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