CN107256752A - A kind of preparation method for sintering iron powder base soft-magnetic composite material - Google Patents
A kind of preparation method for sintering iron powder base soft-magnetic composite material Download PDFInfo
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- CN107256752A CN107256752A CN201710542594.2A CN201710542594A CN107256752A CN 107256752 A CN107256752 A CN 107256752A CN 201710542594 A CN201710542594 A CN 201710542594A CN 107256752 A CN107256752 A CN 107256752A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000005245 sintering Methods 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011230 binding agent Substances 0.000 claims abstract description 60
- 239000000843 powder Substances 0.000 claims abstract description 40
- 239000007921 spray Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 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
- 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
- 239000012298 atmosphere Substances 0.000 claims description 12
- 238000000889 atomisation Methods 0.000 claims description 12
- 239000000758 substrate Substances 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
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 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
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 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
- 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
- 238000007781 pre-processing Methods 0.000 claims description 5
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 5
- 239000000725 suspension 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
- ZJOLCKGSXLIVAA-UHFFFAOYSA-N ethene;octadecanamide Chemical compound C=C.CCCCCCCCCCCCCCCCCC(N)=O.CCCCCCCCCCCCCCCCCC(N)=O ZJOLCKGSXLIVAA-UHFFFAOYSA-N 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
- 238000001816 cooling Methods 0.000 claims 1
- -1 or Tissuemat E Chemical compound 0.000 claims 1
- 229920002647 polyamide Polymers 0.000 claims 1
- 239000001993 wax Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 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
- 230000005291 magnetic effect Effects 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 7
- 238000009413 insulation Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 4
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910001096 P alloy Inorganic materials 0.000 description 2
- 230000004888 barrier function Effects 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
- 235000013312 flour Nutrition 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
- 230000005389 magnetism Effects 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
- DPTATFGPDCLUTF-UHFFFAOYSA-N phosphanylidyneiron Chemical compound [Fe]#P DPTATFGPDCLUTF-UHFFFAOYSA-N 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
- 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
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 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
- 239000011368 organic material Substances 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
- 230000009467 reduction Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 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 sintering iron powder base soft-magnetic composite material, belongs to soft-magnetic composite material technical field.Technological process is：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 in the presence of gases at high pressure and is uniformly sprayed on the material constantly rolled, 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 pressed compact is prepared by the warm mould high velocity compacted under die wall lubrication, is densified through low temperature Fast Sintering, finally gives iron silicon phosphorus soft-magnetic composite material.The sintering iron powder base soft-magnetic composite material of gained both has the characteristics of soft-magnetic composite material magnetic conductivity is high, eddy-current loss is low, has the advantages that sintering soft-magnetic composite material intensity is high again, is adapted to frequency applications.
Description
Technical field
The invention belongs to soft-magnetic composite material technical field, it is related to a kind of with iron powder steam treatment, Double cone spray formula bonding
Change processing, warm mold high speed compacting and low-temperature sintering are combined the method for preparing sintering soft-magnetic composite material.
Background technology
Iron powder base soft-magnetic composite material to powder particle surface by carrying out insulating processing, then using powder metallurgical technique
The class electromagnetic application material prepared.The resistivity of soft-magnetic composite material is high, and eddy-current loss is low in alternating magnetic field, be suitable for compared with
Used under high-frequency, in electrician, electric power and electronic equipment, such 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 barrier, then using compressing, without high temperature sintering, due to the low intensity of material, limit soft magnetism answer
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 being combined prepares sintering iron powder base soft-magnetic composite material.Steam treated is carried out to ferrous powder granules first, in particle surface
Form one layer of very thin Fe3O4Oxide-film is coated, plays a part of interface diffusion barrier layer and hinders counterdiffusion between matrix and Si.
Then fine silica flour and ferrophosphor(us) powder are evenly coated at by ferrous powder granules surface using cohesion technique.Finally using temperature
Mould high velocity compacting technique shapes, and obtains highdensity pressed compact, promotes the diffusion of element.Powder high velocity compacted is to utilize weight high speed
The enormous impact wave energy that impact is produced makes metal dust be densified in a short period of time, close with pressing speed height, pressed compact
Uniform high and Density Distribution, elastic after effect and the low advantage of knockout press are spent, and repeat impact compacting can be carried out, is further carried
High green density.By adding ferrophosphor(us), the liquid formed in low melting point eutectic phase, sintering process is formed at a lower temperature
Phase acceleration of sintering process, solve under high temperature sintering Si elements in the base quick diffusion-homogenization and can not be formed with high electricity
The interface iron silicon phase of resistance rate, makes the problem of eddy-current loss increases.Sinter ferrous powder granules surface in iron powder base soft-magnetic composite material equal
Even cladding iron silicon phase one layer thin, with ferromagnetic atomic ordered structure and high resistivity, the vortex for reducing composite is damaged
Consumption, the presence of oxide layer hinders in sintering process Si atoms to the diffusion inside iron particle.The sintering iron powder base soft magnetism of gained
Composite both has the characteristics of soft-magnetic composite material eddy-current loss is low, has high excellent of sintering soft-magnetic composite material intensity again
Point.
The content of the invention
It is an object of the invention to provide a kind of method for preparing sintering iron powder base soft-magnetic composite material, it is intended to improves iron powder
Consistency, magnetic conductivity and the intensity of base soft-magnetic composite material.
A kind of preparation technology for sintering iron powder base soft-magnetic composite material, concrete technology step has：
1st, iron powder steam treatment：Using 80-180 μm of water atomized iron powder as raw material, powder is in 570~1150 DEG C, Yu Shui
The iron powder carried out in vapor atmosphere after 1~6h of surface oxidation treatment, steam treatment is dry 1-5 hours at 80-120 DEG C, obtains pre-
Handle iron powder.
2nd, mixed-powder cohesion is handled：Powder and 0.1-5 μm of ultra-fine pure silicon powder and 1-5 μm of ultra-fine iron will be pre-processed
Phosphorus alloy powder premixing is uniform, obtains mixed-powder.Mixed-powder carries out cohesion processing in Double cone spray blender, first
First binding agent is dissolved in solvent at a temperature of 60~100 DEG C, binder solution is formed, binder solution is heated to 80-
100 DEG C, then enter under the carrying of gases at high pressure in Double cone spray blender, binder solution is atomized and is uniformly sprayed at
On the material constantly rolled, 1-5h is mixed, cohesion processing powder is obtained.
Phosphorus content wherein in ferrophosphor(us) is 15-23%.
Described binding agent is butadiene-styrene rubber, neoprene, or Tissuemat E, ethylene bis stearic acid amide, stearic acid, poly-
One or more in amide waxe, microwax.
Described solvent be gasoline, toluene, dimethylbenzene, chloroform, dichloromethane, normal heptane and alcohol in one kind or
It is several.
The content of binding agent is 0.05wt%~10wt% in described binder solution, and the solution temperature of binding agent is
60-90℃。
Described Double cone spray blender band heating jacket, is heated, heating-up 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
Position sets atomizer, and gases at high pressure carry binder solution and are atomized at nozzle, and atomization pressure is 0.1-0.5MPa,
Atomization is 0.1-0.5 ls/h with the flow of binding agent.The heating-up temperature of binding agent is 100-200 DEG C, and incorporation time is 1-5
Hour.
3rd, warm mould high velocity compacted：Bonded iron-based powder is suppressed on high-rate forming press, and press strokes are 30-
70mm, corresponding compacting speed is 6.2-9.4m/s, and compacting energy is 795-1855J.With lithium stearate alcohol suspension conduct
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-up temperature is 60 DEG C -150 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating carries out Wen Mogao
Ram compression system, can carry out repeat impact compacting, point 2~3 Secondary Shocks, obtain soft-magnetic composite material base substrate.
4th, sintering densification：Soft-magnetic composite material base substrate carries out low-temperature short-time sintering, sintering temperature in flowing hydrogen atmosphere
Spend for 900 DEG C -1200 DEG C, soaking time is 10-30min.Insulation is cooled down after terminating with 1-3 DEG C/min speed, obtains iron powder
Base soft-magnetic composite material.
The advantage of the invention is that：Water atomized iron powder forms Fe after vapor high-temperature process3O4Film, can be prevented
Water atomized iron powder end surface continues to aoxidize, while certain magnetic can be kept；Cohesion is carried out using Double cone spray blender
Processing, binding agent is atomized in the presence of gases at high pressure, fully contacted 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.Iron powder rises during mixing is heated
To reduction processing hardening, soft annealing effect effectively improves compressibility.It is in negative pressure, easy volatile solvent and barrel in blender
Steam is formed after contact, steam improves rate of drying by vacuum pumped.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
Silica flour and ultra-fine iron phosphorus powder form low melting point eutectic phase under lower sintering temperature, reduce sintering temperature, obtain floor height electricity
The clad of resistance rate, clad is complete, reduces eddy-current loss, improves the consistency and intensity of composite.
Brief description of the drawings
Fig. 1 is process chart of the invention.
Fig. 2 is the schematic diagram of Double cone spray blender.
Each component names 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 discharging opening, and 7 be gases at high pressure, 8
It is base for motor, 9,10 be conduction oil.
Embodiment
Embodiment 1：Fe-3.5%Si-1.5%P soft-magnetic composite material preparation technologies
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, its
Phosphorus content in middle ferrophosphor(us) is 23%.Water atomized iron powder end is carried out at surface oxidation at 950 DEG C in water vapour atmosphere
Manage the iron powder after 3h, steam treatment to dry 1 hour at 110 DEG C, obtain pre-processing iron powder；Will pretreatment iron powder and pure silicon powder and
The premixing of ferrophosphor(us) powder is uniform, obtains mixed-powder.Mixed-powder carries out cohesion processing in Double cone spray blender.
Binding agent is butadiene-styrene rubber, and solvent is dichloromethane.In binder solution the content of binding agent be 0.3wt%, binding agent it is molten
It is 80 DEG C to solve temperature.Binding agent is dissolved in solvent at a temperature of 80 DEG C first, binder solution, binder solution quilt is formed
90 DEG C are heated to, is then entered under the carrying of gases at high pressure in Double cone spray blender, binder solution is atomized and uniform
It is sprayed on the material constantly rolled, mixes 2h, obtains cohesion processing powder.The heating-up 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 binding agent is 0.2 l/h.Bonded iron-based powder is pressed on high-rate forming press
System, press strokes are 60mm, and corresponding compacting speed 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 numeral
Temperature control silica gel piece is heated, and heating-up temperature is 100 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating carries out warm mould at a high speed
Compacting, carries out one-shot compacting, obtains soft-magnetic composite material base substrate.Soft-magnetic composite material base substrate enters in flowing hydrogen atmosphere
Row sintering, sintering temperature is 970 DEG C, and soaking time is 20min.Insulation is cooled down after terminating with 3 DEG C/min speed, obtains iron powder
Base soft-magnetic composite material.
Embodiment 2：Fe-6.5%Si-2.0%P soft-magnetic composite material preparation technologies
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,
Phosphorus content wherein in ferrophosphor(us) is 21%.Water atomized iron powder end carries out surface oxidation at 900 DEG C in steam atmosphere
Handle the iron powder after 1h, steam treatment to dry 1.5 hours at 120 DEG C, obtain pre-processing iron powder；Will pretreatment iron powder and pure silicon powder
End and the premixing of ferrophosphor(us) powder are uniform, obtain mixed-powder.Mixed-powder carries out cohesion in Double cone spray blender
Processing.Binding agent is Tissuemat E, and solvent is normal heptane.The content of binding agent is 0.4wt% in binder solution, binding agent
Solution temperature is 60 DEG C.Binding agent is dissolved in solvent at a temperature of 60 DEG C first, binder solution, binder solution is formed
80 DEG C are heated to, is then entered under the carrying of gases at high pressure in Double cone spray blender, binder solution is atomized and equal
It is even to be sprayed on the material constantly rolled, 1.5h is mixed, cohesion processing powder is obtained.The heating-up temperature of Double cone spray blender
For 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 binding agent is 0.3 l/h.Bonded iron-based powder is suppressed on high-rate forming press,
Press strokes are 70mm, and corresponding compacting speed 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 numeral temperature
Control silica gel piece is heated, and heating-up temperature is 90 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating carries out Wen Mogao ram compressions
System, carries out one-shot compacting, obtains soft-magnetic composite material base substrate.Soft-magnetic composite material base substrate is carried out in flowing hydrogen atmosphere
Sintering, sintering temperature is 1050 DEG C, and soaking time is 15min.Insulation is cooled down after terminating with 3 DEG C/min speed, obtains iron powder
Base soft-magnetic composite material.
Embodiment 3：Fe-4.0%Si-2.5%P soft-magnetic composite material preparation technologies
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,
Phosphorus content wherein in ferrophosphor(us) is 22%.Water atomized iron powder end carries out Surface Oxygen at 1050 DEG C in steam atmosphere
Change the iron powder after processing 1h, steam treatment to dry 1 hour at 100 DEG C, obtain pre-processing iron powder；Will pretreatment iron powder and pure silicon powder
End and the premixing of ferrophosphor(us) powder are uniform, obtain mixed-powder.Mixed-powder carries out cohesion in Double cone spray blender
Processing.Binding agent is Tissuemat E, ethylene bis stearic acid amide and stearic blend.Solvent is chloroform, normal heptane
With the mixed solvent of alcohol.The content of binding agent is 0.2wt% in binder solution, and the solution temperature of binding agent is 85 DEG C.It is first
First binding agent is dissolved in solvent at a temperature of 85 DEG C, binder solution is formed, binder solution is heated to 95 DEG C, then
Enter under the carrying of gases at high pressure in Double cone spray blender, binder solution is atomized and is uniformly sprayed at what is constantly rolled
On material, 2h is mixed, cohesion processing powder is obtained.The heating-up temperature of Double cone spray blender is 140 DEG C, pressure in blender
For 0.9 × 10-5Pa.The rotational speed of mixing machine is 140 revs/min, and atomization pressure is 0.25MPa, atomization binding agent
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 speed 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 is used
Digital temperature control silica gel piece is heated, and heating-up temperature is 110 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating carries out Wen Mo
High velocity compacted, carries out secondary pulse compacting, obtains soft-magnetic composite material base substrate.Soft-magnetic composite material base substrate is in flowing hydrogen atmosphere
In be sintered, sintering temperature be 1070 DEG C, soaking time is 30min.Insulation is cooled down after terminating with 1 DEG C/min speed, is obtained
To iron powder base soft-magnetic composite material.
Embodiment 4：Fe-10%Si-3.0%P soft-magnetic composite material preparation technologies
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, its
Phosphorus content in middle ferrophosphor(us) is 23%.Water atomized iron powder end carries out surface oxidation at 1100 DEG C in steam atmosphere
Handle the iron powder after 1h, steam treatment to dry 1 hour at 120 DEG C, obtain pre-processing iron powder；Will pretreatment iron powder and pure silicon powder
It is uniform with the premixing of ferrophosphor(us) powder, obtain mixed-powder.Mixed-powder is carried out at cohesion in Double cone spray blender
Reason.Binding agent is the blend of ethylene bis stearic acid amide, stearic acid and microwax.Solvent is dichloromethane, normal heptane and wine
The mixed solvent of essence.The content of binding agent is 0.3wt% in binder solution, and the solution temperature of binding agent is 90 DEG C.First will
Binding agent is dissolved in solvent at a temperature of 90 DEG C, forms binder solution, binder solution is heated to 95 DEG C, then in height
Calm the anger and enter in Double cone spray blender under the carrying of body, binder solution is atomized and be uniformly sprayed at the material constantly rolled
On, 2h is mixed, cohesion processing powder is obtained.The heating-up 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, and atomization pressure is 0.1MPa, the flow of atomization binding agent
For 0.25 l/h.Bonded iron-based powder is suppressed on high-rate forming press, and press strokes are 65mm, corresponding pressure
Speed processed is 9.1m/s, and compacting energy is 1722.5J.With lithium stearate alcohol suspension as die wall lubricant, height is applied to
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, heating
Temperature is 100 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating carries out warm mould high velocity compacted, carries out one-shot compacting,
Obtain soft-magnetic composite material base substrate.Soft-magnetic composite material base substrate is sintered in flowing hydrogen atmosphere, and sintering temperature is 1110
DEG C, soaking time is 10min.Insulation is cooled down after terminating with 2 DEG C/min speed, obtains iron powder base soft-magnetic composite material.
Claims (6)
1. a kind of preparation method for sintering 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 enters at 570~1150 DEG C in steam atmosphere
Iron powder after row 1~6h of surface oxidation treatment, steam treatment is dry 1-5 hours at 80-120 DEG C, obtains pre-processing iron powder；
It is pre-mixed with 0.1-5 μm of ultra-fine pure silicon powder and 1-5 μm of ultra-fine ferrophosphor(us) powder Step 2: powder will be pre-processed
It is even, obtain mixed-powder；Mixed-powder carries out cohesion processing in Double cone spray blender, first by binding agent 60~
It is dissolved at a temperature of 100 DEG C in solvent, forms binder solution, binder solution is heated to 80-100 DEG C, then in high pressure
Enter under the carrying of gas in Double cone spray blender, binder solution is atomized and be uniformly sprayed at the material constantly rolled
On, 1-5h is mixed, cohesion processing powder is obtained；
Step 3: described Double cone spray blender band heating jacket, is heated using conduction oil, heating-up temperature for 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
Centre sets atomizer, and gases at high pressure carry binder solution and are atomized at nozzle, and atomization pressure is 0.1-
0.5MPa, atomization is 0.1-0.5 ls/h with the flow of binding agent；The heating-up temperature of binding agent is 100-200 DEG C, during mixing
Between be 1-5 hours；
Step 4: bonded iron-based powder is suppressed on high-rate forming press, press strokes are 30-70mm, corresponding pressure
Speed processed is 6.2-9.4m/s, and compacting energy is 795-1855J；With lithium stearate alcohol suspension as die wall lubricant, apply
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-up temperature is 60 DEG C -150 DEG C, and the former that iron silicon phosphorus mixed-powder is sent into heating carries out warm mould high velocity compacted, carries out many
Secondary Shocks are suppressed, point 2~3 Secondary Shocks, obtain soft-magnetic composite material base substrate；
Step 5: soft-magnetic composite material base substrate carries out low-temperature short-time sintering in flowing hydrogen atmosphere, it is incubated after terminating with 1-3
DEG C/cooling of min speed, obtain iron powder base soft-magnetic composite material.
2. according to claim 1 it is a kind of sinter iron powder base soft-magnetic composite material preparation method, it is characterised in that：Step one
Described in phosphorus content in ferrophosphor(us) be 15-23%.
3. according to claim 1 it is a kind of sinter iron powder base soft-magnetic composite material preparation method, it is characterised in that：Step one
Described in binding agent be butadiene-styrene rubber, neoprene, or Tissuemat E, ethylene bis stearic acid amide, stearic acid, polyamide
One or more in wax, microwax.
4. according to claim 1 it is a kind of sinter iron powder base soft-magnetic composite material preparation method, it is characterised in that：Step one
Described in solvent be gasoline, toluene, dimethylbenzene, chloroform, dichloromethane, normal heptane and alcohol in one or more.
5. according to claim 1 it is a kind of sinter iron powder base soft-magnetic composite material preparation method, it is characterised in that：Step one
Described in binder solution in the content of binding agent be 0.05wt%~10wt%, the solution temperature of binding agent is 60-90 DEG C.
6. according to claim 1 it is a kind of sinter iron powder base soft-magnetic composite material preparation method, it is characterised in that：Step 5
Described in low-temperature short-time sintering temperature be 900 DEG C -1200 DEG C, soaking time is 10-30min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107900361A (en) * | 2017-11-23 | 2018-04-13 | 北京科技大学 | A kind of method that high pass quantity research prepares iron-base powder metallurgical product |
| 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 |
| CN111883328A (en) * | 2020-06-09 | 2020-11-03 | 山东精创磁电产业技术研究院有限公司 | Modified binder and method for preparing soft magnetic composite material by using same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000087117A (en) * | 1998-09-16 | 2000-03-28 | Hitachi Powdered Metals Co Ltd | Method for joining valve shaft of solenoid valve to sintered movable iron core |
| CN1731542A (en) * | 2004-08-05 | 2006-02-08 | 株式会社电装 | Method for manufacturing soft magnetic material |
| CN102560223A (en) * | 2012-02-29 | 2012-07-11 | 北京科技大学 | Method for forming bonded iron-based powder by high velocity compaction technology |
| CN105665715A (en) * | 2016-04-15 | 2016-06-15 | 厦门理工学院 | Iron-silicon series magnetically soft alloy prepared through powder metallurgy process and method |
| CN106782982A (en) * | 2016-12-31 | 2017-05-31 | 浙江工业大学 | A kind of soft-magnetic composite material and preparation method thereof |
-
2017
- 2017-07-05 CN CN201710542594.2A patent/CN107256752B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000087117A (en) * | 1998-09-16 | 2000-03-28 | Hitachi Powdered Metals Co Ltd | Method for joining valve shaft of solenoid valve to sintered movable iron core |
| CN1731542A (en) * | 2004-08-05 | 2006-02-08 | 株式会社电装 | Method for manufacturing soft magnetic material |
| CN102560223A (en) * | 2012-02-29 | 2012-07-11 | 北京科技大学 | Method for forming bonded iron-based powder by high velocity compaction technology |
| CN105665715A (en) * | 2016-04-15 | 2016-06-15 | 厦门理工学院 | Iron-silicon series magnetically soft alloy prepared through powder metallurgy process and method |
| CN106782982A (en) * | 2016-12-31 | 2017-05-31 | 浙江工业大学 | A kind of soft-magnetic composite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 蔡飞虎等: "6.3 坯料的混合", 《陶瓷墙地砖生产技术》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107900361A (en) * | 2017-11-23 | 2018-04-13 | 北京科技大学 | A kind of method that high pass quantity research prepares iron-base powder metallurgical product |
| 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 |
| CN111883328A (en) * | 2020-06-09 | 2020-11-03 | 山东精创磁电产业技术研究院有限公司 | Modified binder and method for preparing soft magnetic composite material by using same |
| CN111883328B (en) * | 2020-06-09 | 2021-06-18 | 山东精创磁电产业技术研究院有限公司 | Modified binder and method for preparing soft magnetic composite material by using same |
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