CN107914017A - A kind of powder warm-rolling preparation method of Fe 6.5%Si soft magnetic materials thin strips - Google Patents
A kind of powder warm-rolling preparation method of Fe 6.5%Si soft magnetic materials thin strips Download PDFInfo
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- 239000000696 magnetic material Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 75
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910000976 Electrical steel Inorganic materials 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 15
- 229910052742 iron Inorganic materials 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 14
- 238000009692 water atomization Methods 0.000 claims abstract description 13
- 238000005097 cold rolling Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 3
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- 239000000314 lubricant Substances 0.000 claims description 18
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- 239000011812 mixed powder Substances 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- 238000005238 degreasing Methods 0.000 claims description 10
- 238000009792 diffusion process Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002791 soaking Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 8
- 239000010959 steel Substances 0.000 claims description 8
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 6
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- 238000000265 homogenisation Methods 0.000 claims description 5
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 235000013312 flour Nutrition 0.000 claims description 4
- 239000011733 molybdenum Substances 0.000 claims description 4
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- 238000000713 high-energy ball milling Methods 0.000 claims description 2
- 239000011229 interlayer Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
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- 229910017082 Fe-Si Inorganic materials 0.000 description 7
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- 238000000137 annealing Methods 0.000 description 5
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- 238000005229 chemical vapour deposition Methods 0.000 description 3
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- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
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- 230000008859 change Effects 0.000 description 1
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- 238000007598 dipping method Methods 0.000 description 1
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- 230000005415 magnetization Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
-
- B22F1/0003—
-
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
-
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
-
- 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
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- 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
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
A kind of powder warm-rolling preparation method of Fe 6.5%Si soft magnetic materials thin strips, the present invention use water atomization Fe powder, and Si powder is raw material, and Si powder is adhered to water-atomized iron powder surface in mixed process using compound mixture.Implement the shaping of powder warm-rolling at 125~150 DEG C; prepare that density is higher, the uniform slab of Tissue distribution; powder warm-rolling slab is subjected to vacuum or protection of reducing atmosphere sintering in 1080~1180 DEG C of temperature ranges; Fe powder particles are realized not complete to connect; and Si and Fe realizes partially-alloyed, the high silicon steel blank of porous, the incomplete alloying of formation.Subsequently through multiple cold rolling, sintering, finally sintered in 1280~1350 DEG C of vacuum or protection of reducing atmosphere, realize the homogeneous alloy of high silicon steel, obtain 0.1~0.5mm thickness containing 4.5~6.7%Si, 7.31~7.43g/cm of density3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder metallurgy of Fe-6.5%Si steel bands
The method of sintering and rolling deformation.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis curve is very narrow, it and fundamental magnetization curve are almost
Overlap, be mainly used for the iron core of inductance coil, transformer, relay and motor.Fe-Si alloys maximum permeability is sent out with Si contents
Changing, respectively Si mass percent it is (the same below) for 2% and 6.5% nearby there is the peak of two maximum permeabilities
Value, respectively reaches 10000 and 25000.The maximum permeability of Fe-Si alloys does not have absolute predominance, such as slope in soft magnetic materials
The maximum permeability of alloy can not reach 200000.But the Fe-Si lattens of Si ＜ 4.5% manufacture cost is low, therefore
Silicon steel sheet is also known as electrical sheet or silicon steel thin slice, is a kind of very important magnetic material.
And Si>When 4.5%, below 540 DEG C of temperature B can occur for Fe-Si alloys2The eutectoid decomposition reaction of ordered phase, it is raw
Into the unordered phases of α-Fe and DO3Ordered phase so that alloy becomes fragile and is difficult to deform.
For iron Si system alloy of the Si contents between 4.5~6.7%, commonly referred to as high silicon steel, wherein silicone content 6.5%
High silicon steel it is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction is with the increase of Si contents
And reduce, disappear substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increases with Si contents, about
When 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent low in higher frequency operation
Iron loss characteristic.
The transformer of normal operation can occur continuous uniform " drone " sound, this is because alternating current by transformer around
Group when, in the core between generate periodically variable alternating flux, cause iron core magnetostriction and shake the sound sent.Greatly
The sound that amount or large-scale iron core are sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is to play particularly important role in the military aviation such as spacecraft, submarine and guided missile field, Fe-Si systems alloy.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared on No. 11 airships of Apollo as transformer material, are completed the mankind and are landed on the moon first
Heroic undertaking.As it can be seen that high silicon steel is the environment-friendly type soft magnetic materials of a kind of consumption reduction of function admirable, noise reduction.
Compared to other alloys, the research and development process of high silicon steel is relatively very long.Late 1920s
A.Schulze studies discovery first, and the iron Si system alloy of silicone content 6.5% has the almost nil characteristic of magnetostriction coefficient.
In the 1980s, professor K.I.Arail etc. has found the high silicon steel alloy low compared to traditional Si content in exchange dynamic magnetic field
In there is the magnetic conductivity of lower iron loss and higher.Hereafter between many decades, in order to overcome the brittleness of high silicon steel, in technology of preparing side
There are many trials in face.As the special rolled method of jacket or temperature control, rapid solidification method, chemical vapour deposition technique (CVD method),
Plasma chemical vapor deposition (PCVD methods), hot dipping ooze a diffusion annealing method, powder metallurgic method, microalloying and are modified
Etc. various methods.
Wherein CVD is the successful example of comparison.NKK companies of Japan in 1988 have produced thickness for the first time using CVD technology
It is the No yield point 6.5%Si steel discs of 400mm to spend for 0.1~0.5mm, width.Phase early 1990s, global first commercialization
Can realize that the CVD production lines of continuous siliconising are developed, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is：Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and alloy is reached required content to alloy diffusion inside by elevated furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
Ask, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", its technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, its excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production, is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just produce huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip, for
The Fe-Si alloy thin band materials of 4.5~6.7%Si contents are difficult to the problem of shaping, with water-atomized iron powder and fine simple substance silica flour
Uniformly mixing, adds compound mixture, forms the powder mixture for being adapted to warm-rolling deformation, then prepare using powder warm rolling method
Certain thickness slab, forms porous, heterogeneous blank after degreasing, sintering, is obtained after multi-pass cold rolling-sintering thin
Plate, is finally sintered using High temperature diffusion and obtains the high silicon steel band of homogeneous.
The present invention is achieved by the following technical solutions：Using subsphaeroidal water atomization Fe powder, fine Si powder is original
Material, forms Fe-4.5~6.7%Si mixed powders.Si powder is adhered into water atomization iron in mixed process using compound mixture
Powder surface.Since water atomization Fe powder is the big particle with high-compressibility, larger volume ratio is occupied in mixed powder, is added
Its deformability is not significantly reduced after Si powder.Play warm-rolling shaping technological merit, 125~150 DEG C implement powder warm-rollings into
Shape, prepares that density is higher, the uniform slab of Tissue distribution.Powder warm-rolling slab is carried out in 1080~1180 DEG C of temperature ranges
Vacuum or protection of reducing atmosphere sintering, make Fe powder particles realize do not complete to connect, and Si and Fe realize it is partially-alloyed, formation it is more
Hole, have compressibility incomplete alloying high silicon steel blank.Subsequently through multiple cold rolling, not exclusively sintering, slab
Density rise, plate thickness are reduced, and the alloying level of Si is also continuously improved.The finally vacuum in 1280~1350 DEG C of temperature ranges
Or protection of reducing atmosphere sintering, the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, obtains and contains 4.5~6.7%Si
0.1~0.5mm it is thick, 7.31~7.43g/cm of density3High silicon steel band.
The present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh water-atomized iron powders, Fe >=99.0% in water-atomized iron powder, remaining for Si, Mn, P, S and other can not
The impurity avoided, with the simple substance Si powder of particle diameter≤3 μm, purity is more than 97%, mainly containing Fe, Al and Ca and other are inevitable
Impurity.
Water atomization Fe powder is a kind of widely used Industrial iron powder, has subsphaeroidal pattern, impurity content is less than reduction Fe
Powder, has the compressibility and mobility of higher, is conducive to the Uniform Flow of powder warm-rolling technical process powder.Water atomization Fe powder
In low impurity content it is favourable to the soft magnetic characteristic of high silicon steel.
The property of simple substance Si is very crisp, it is easy to is refined by Mechanical Crushing technique.The simple substance silica flour for choosing particle diameter≤3 μm has
Beneficial to the realization of follow-up homogenization diffusion-sintering；And hole that tiny Si is formed in blank, brittle interface are also tiny, rise
Strengthening and Toughening to structure refinement acts on, and is conducive to improve follow-up blank toughness, is not easily caused out in densification process is rolled
Split.But Si is easily absorbing oxygen, SiO is formed on powder surface2Film, therefore in the preparation, storage and transfer process of Si powder,
And inert gas shielding should be used in follow-up batch mixing, the operation of rolling, used instrument must also take dehydration, drying in advance
Processing.
On the premise of oxygen content is controlled, influence of the impurity such as other Al, Ca, Mn to alloy magnetic property is little, during
The possibility for introducing other alloying elements is also little.
(2) powder mixes：
According to the ratio of Fe-4.5~6.7%Si, water atomization Fe powder and Si powder are weighed；Using low under inert protective atmosphere
Energy hybrid machine mixes.The compounded lubricant of powder total amount 0.4~0.6% is added during mixing.
Powder warm-rolling technique can reduce the interior friction in powder deformation process, improve powder compact density and density, group
Uniformity is knitted, reduces the fretting wear to tool and mould.Lubricant is the key of technique success or not, and the selection principle of lubricant should
When meeting glass transition temperature at 120~150 DEG C or so, the condition such as low friction factor.Common powder warm deformation binder has
Very much.
(3) powder warm-rolling
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
It is 1.1~2.4mm to roll out thickness, and width is 100~200mm, and density is 5.9~6.4g/cm3Powder warm-rolling slab.Roll
Mixed-powder is heated to 125~150 DEG C using powder heating unit before system, and roll is preheating to same temperature.
Go out the difference in roller direction by band, powder warm-rolling can be divided into vertical, horizontal and tilt 3 kinds of forms, and feeding manner has
Dead weight feeding, forced feed, pre-glued feeding etc..The width of blank is related with the width of feeding trough, and the length of blank regards production
Depending on condition is permitted and is actually needed.
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated with the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace,
2h~4h is kept the temperature respectively using the programming rate of 2~5 DEG C/min, and in 200 DEG C, 400 DEG C, then will heat up to 1080~1180
DEG C 2~4h of heat preservation sintering, sintered blank density is 6.0~6.5g/cm3。
Sintering temperature is too low, the connection and the diffusion of Si being unfavorable between Fe powder particles, and sintering temperature is excessive then can be due to
, there is thick hole in the diffusion into the surface of Fe, Si element, is subsequently difficult to press, and rolling densification is difficult to realize.
During sintering can powder warm-rolling blank can be placed with multilayer, but must separate between layers, to avoid plate during sintering
Base, which is shunk, to be caused to crack.Programming rate should not be too fast during sintering, and multistage insulation can be set in temperature-rise period, to realize degassing, take off
The effect of fat.Reproducibility or inert gas shielding degreasing, sintering can also be taken.W, Mo, heat resisting steel etc. can be used during sintering
As support plate (or burn boat), the ceramic wafers such as corundum, zirconium oxide can also be used, but metallic plate thermal conductivity it is good and beneficial to uniformly
Sintering shrinkage.
Uniformly tiny porous organization is formed after sintering.X-ray diffraction Discriminating materials are heterogeneous Fe (Si) phase, are had
Body-centred cubic several characteristic peaks, but several diffraction maximums have obvious separating phenomenon, illustrate that there are different 2 kinds of Si solid solubility
Fe phases, wherein must have the Si contents in a kind of Fe phases low, have plastic deformation ability.
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~45%, in sintering furnace, 0.5~2h is re-sintered in 1080~1180 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
To 0.1~0.5mm, density reaches 7.30~7.42g/cm3。
Since powder batch is porous organization, and there are deformable Fe phases, slab can bear cold-rolling deformation.Palette
There is also more high Si phases in base, its performance is more crisp, therefore not above 8%, accumulation total reduction reaches amount under every time rolling
8~20 passages are taken around to 30~45%.
Due to there are a large amount of holes and hard crisp phase, taking when re-sintering for 1080 DEG C~1180 DEG C, in vacuum or reproducibility
Sintered under protective atmosphere, to realize the reparation of the closing of pores and crackle, and the homogenization diffusion of a degree of Si elements.At this time
Programming rate can be very fast, in 5~10 DEG C/min, can continuous warming, soaking time determines depending on thickness of slab, during thickness of slab >=1mm, insulation
Time is 1~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time.The accumulation drafts after sintering reaches 30 every time
, it is necessary to sinter 1 time again after~45%, 0.1~0.5mm is rolled down to from the powder base of 1.1~2.4mm, takes around and sinters 4 again
~8 times.In addition, in order to make the density of plate reach 7.2g/cm3More than (about the 95% of solid density), it is also desirable to more than 4 times
Re-sinter.
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, in thermal diffusion
Under effect, the homogenization of Si being realized, forming single-phase alloy, obtain the high silicon steel of homogeneous, the thickness of plate is almost after densification sintering
It is constant, it is 0.1~0.5mm, density reaches 7.31~7.43g/cm3。
The silica flour high-energy ball milling of particle diameter≤3 μm rushes the acquisition of rotation method.
The low energy batch mixer is conical mixer, V-arrangement batch mixer or drum mixer.
The lubricant of powder gross mass 0.4~0.6% is added when step (2) mixes, while adds powder gross mass 0.1%
Glycerine, the lubricant is compounded lubricant, is made of zinc stearate and vinyl bis-stearamides, zinc stearate:EBS
For 4:6~2:8, using absolute ethyl alcohol as solvent, added according to 400~600ml of powder per ton.
Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
Placement sintering plate can be overlapped during high temperature sintering, but interlayer must be laid with MgO powder, and W, Mo and ceramics can be used to burn
Boat.But plate must tile placement, tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of element such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel
Large effect, can subsequently be annealed, the technological means such as normalizing treatment is controlled by by wet hydrogen.
Essence of the invention is a small amount of by with the addition of in the water atomization Fe powder of the big volumetric portion with good plasticity
The fine Si powder of simple substance, forms a kind of composite material of achievable powder warm-rolling；Prepare that density is higher, group using warm-rolling shaping
Knit the slab being evenly distributed；By not exclusively sintering, Fe powder particles are made to realize not exclusively connection, and Si and Fe realizes alloy part
Change, form the high silicon steel blank of incomplete alloying porous, that there is compressibility；Subsequently through multi-pass cold rolling and sintering,
Improve structural homogenity and compactness；Again by high-temperature diffusion process, the homogenization of Si is realized, so as to obtain the high silicon of high quality
Steel band.This method realizes Technics Process Automation, continuous production by technique and equipment Design, can be mass-produced 0.1
~0.5mm is thick, 7.31~7.43g/cm of density3High silicon steel band.
Brief description of the drawings
Fig. 1 is that the powder warm-rolling base of the embodiment of the present invention 2 sinters the porous shape appearance figure of rear surface polishing；
Fig. 2 is XRD diffraction curve figures after the powder warm-rolling base of the embodiment of the present invention 2 sinters；
Fig. 3 is XRD diffraction curve figures after the powder warm-rolling base high temperature sintering of the embodiment of the present invention 4.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 93.3:6.7 ratio mixing, forms
The mixed-powder of Fe-6.7%Si.During mixing total amount of adding be 0.4% compounded lubricant, and 0.1% glycerine mitigate powder
The oxidation of last heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant is by stearic acid
Zinc and EBS compositions, zinc stearate:EBS is 2:8.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Mixed-powder is heated to 130 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 2.4mm
Last warm-rolling slab, the width of slab is 100mm.The density of pressed compact is 5.9g/cm3。
Powder strip plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.Adopt
With the programming rate of 2 DEG C/min, and 4h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1080 DEG C of heat preservation sintering 4h.Burn
It is 6.0g/cm to tie base density3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~45%, then in vacuum sintering furnace, in 1080 DEG C of heat preservation sinterings.With 5 DEG C/min speed continuous warmings, soaking time regards plate
Thickness determines, during thickness of slab >=1mm, soaking time 2h；Thickness of slab is in 0.1~1mm, soaking time 1h.Specific pressure-annealing schedule
For：2.4mm → 1.76mm → 1.22mm → 0.81mm → 0.49mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches
To 0.49mm, density reaches 7.30g/cm3。
For above-mentioned cold rolling made-up belt in 1350 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.31g/cm to obtain thickness3, Si
Content is the 6.7% high silicon steel of single-phase homogeneous.
Embodiment 2
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 95.5:4.5 ratio mixing, forms
The mixed-powder of Fe-4.5%Si.During mixing total amount of adding be 0.6% compounded lubricant, and 0.1% glycerine mitigate powder
The oxidation of last heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant is by stearic acid
Zinc and EBS compositions, zinc stearate:EBS is 4:6.Using drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 140 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 1.1mm
Last warm-rolling slab, the width of slab is 200mm.The density of pressed compact is 6.4g/cm3。
Powder strip plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.Adopt
With the programming rate of 5 DEG C/min, and 2h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1180 DEG C of heat preservation sintering 2h.Burn
It is 6.5g/cm to tie base density3.Surface after sintering polishes porous pattern, sees Fig. 1.X-ray diffraction Discriminating materials are heterogeneous
Fe (Si) phase, is shown in Fig. 2, is body-centred cubic several characteristic peaks, has obvious separating phenomenon, illustrate that there are Si solid solubility is different
2 kinds of Fe phases, wherein must have the Si contents in a kind of Fe phases low, have plastic deformation ability.
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~45%, then in vacuum sintering furnace, in 1180 DEG C of heat preservation sinterings.With 10 DEG C/min speed continuous warmings, soaking time is
1h.Specifically pressure-annealing schedule is：1.1mm → 0.75mm → 0.45mm → 0.29mm → 0.19mm → 0.14mm → 0.10mm,
I.e. after 6 cold rollings and 5 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.42g/cm3。
For above-mentioned cold rolling made-up belt in 1280 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.43g/cm to obtain thickness3, Si
Content is the 4.5% high silicon steel of single-phase homogeneous.
Embodiment 3
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 93.5:6.5 ratio is mixed to form
The mixed-powder of Fe-6.5%Si.During mixing total amount of adding be 0.5% compounded lubricant, and 0.1% glycerine mitigate powder
The oxidation of last heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant is by stearic acid
Zinc and EBS compositions, zinc stearate:EBS is 3:7.Using drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 120 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 1.6mm
Last warm-rolling slab, the width of slab is 150mm.The density of pressed compact is 6.0g/cm3。
Powder strip plate is placed on surface to be coated with the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the programming rate of 3 DEG C/min, and 2h, 400 DEG C of insulation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1150 DEG C of insulations and burn
Tie 3h.Sintered blank density is 6.05g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~45%, then in hydrogen tube furnace, in 1150 DEG C of heat preservation sintering 1h.With 6 DEG C/min speed continuous warmings.Specific pressure-
Annealing schedule is：1.6mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 4 cold rollings and 3 sintering, plate
Thickness reach 0.27mm, density reaches 7.36g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.37g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous.
Embodiment 4
By the water atomization Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 94.2:5.8 ratio mixing, forms
The mixed-powder of Fe-5.8%Si.During mixing total amount of adding be 0.5% compounded lubricant, and 0.1% glycerine mitigate powder
The oxidation of last heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant is by stearic acid
Zinc and EBS compositions, zinc stearate:EBS is 3:7.Using drum mixer by above-mentioned powder mixing 3h.
Mixed-powder is heated to 125 DEG C using powder heating unit, and roll is preheating to same temperature.Using two rollers
Horizontal mill and inclination feeding trough, are conducted oneself with dignity, the frictional force feeding between roll and powder using powder, roll out the powder of 2.0mm
Last warm-rolling slab, the width of slab is 160mm.The density of pressed compact is 6.18g/cm3。
Powder strip plate is placed on surface to be coated with the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the programming rate of 4 DEG C/min, and 3h, 400 DEG C of insulation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1130 DEG C of insulations and burn
Tie 2h.Sintered blank density is 6.22g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reaches 30 through multi- pass rolling to total reduction
After~45%, then in hydrogen tube furnace, in 1130 DEG C of heat preservation sintering 0.5h.With 8 DEG C/min speed continuous warmings.Specific pressure
Under-annealing schedule is：2.0mm → 1.3mm → 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm is that is, cold through 7 times
Roll with after 6 sintering, the thickness of plate reaches 0.21mm, and density reaches 7.38g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.39g/cm to obtain thickness3, Si
Content is 5.8%, and the XRD analysis figure of its final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.
Claims (7)
1. the powder warm-rolling preparation method of a kind of Fe-6.5%Si soft magnetic materials thin strip, it is characterised in that comprise the following steps：
(1) raw material powder prepares
Using -100 mesh water-atomized iron powders, Fe >=99.0% in water-atomized iron powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, with the simple substance Si powder of particle diameter≤3 μm, purity is more than 97%, mainly containing Fe, Al and Ca and other are inevitably miscellaneous
Matter；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, water atomization Fe powder and Si powder are weighed；Low energy is used under inert protective atmosphere
Mixer mixes, and the compounded lubricant of powder total amount 0.4~0.6% is added during mixing；
(3) powder warm-rolling
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder, rolled
It is 1.1~2.4mm to go out thickness, and width is 100~200mm, and density is 5.9~6.4g/cm3Powder warm-rolling slab.Before rolling
Mixed-powder is heated to 125~150 DEG C using powder heating unit, and roll is preheating to same temperature；
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated with the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2
The programming rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, then it will heat up to 1080~1180 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density is 6.0~6.5g/cm3；
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reach 30 through multi- pass rolling to total reduction~
After 45%, in sintering furnace, 0.5~2h is re-sintered in 1080~1180 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
0.1~0.5mm, density reach 7.30~7.42g/cm3；
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, it is real under the action of thermal diffusion
The homogenization of existing Si, forms single-phase alloy, obtains the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering,
Density reaches 7.31~7.43g/cm3。
2. a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature
It is：The simple substance silica flour high-energy ball milling of particle diameter≤3 μm rushes the acquisition of rotation method.
3. a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature
It is：The low energy batch mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature
It is：The lubricant of powder gross mass 0.4~0.6%, and the glycerine of powder gross mass 0.1% are added when step (2) mixes,
The lubricant is compounded lubricant, is made of zinc stearate and vinyl bis-stearamides, zinc stearate:EBS is 4:6~
2:8, using absolute ethyl alcohol as solvent, added according to 400~600ml of powder per ton.
5. a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature
It is：After step (5) cold rolling when re-sintering for 1080 DEG C~1180 DEG C, burnt using under vacuum-sintering or restitutive protection's atmosphere
Knot, programming rate determines in 5~10 DEG C/min, continuous warming, soaking time depending on thickness of slab, during thickness of slab >=1mm, soaking time 1
~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time, and the accumulation drafts after sintering reaches 30~45% every time
Afterwards, it is necessary to sinter 1 time again, 0.1~0.5mm is rolled down to from the powder base of 1.1~2.4mm, it is necessary to sinter 4~8 times again.
6. a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature
It is：Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. a kind of powder warm-rolling preparation method of Fe-6.5%Si soft magnetic materials thin strip as claimed in claim 1, its feature
It is：Overlapping places sintering plate during high temperature sintering, and interlayer is laid with MgO powder, and plate tiling is placed, and tablet weight is placed on plate
Thing, prevents from deforming in sintering process.
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