CN107999766A - A kind of method that powder warm-rolling prepares Fe-6.5%Si bands with diffusion-sintering - Google Patents
A kind of method that powder warm-rolling prepares Fe-6.5%Si bands with diffusion-sintering Download PDFInfo
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
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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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
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- 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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- 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
- H01F1/14775—Fe-Si based alloys in the form of sheets
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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Abstract
A kind of method that powder warm-rolling prepares Fe 6.5%Si bands with diffusion-sintering, the present invention chooses reduction Fe powder and water atomization Fe powder, according to 4:6~6:4 ratio mixing, then the HIGH-PURITY SILICON iron powder that Si contents are 70~80% is added, form Fe 4.5~6.7%Si mixed powders.Implement the shaping of powder warm-rolling at 125~150 DEG C; slab is prepared, slab is subjected to vacuum at 1070~1170 DEG C or protection of reducing atmosphere sinters, Fe powder particles is realized not exclusively sintering; and Si and Fe realizes partially-alloyed, the high silicon steel blank of porous, the incomplete alloying of formation.Multiple cold rolling, sintering again, finally sinter in 1260~1330 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, 7.35~7.49g/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 of the high silicon steel soft magnetism band of high-performance
The metallurgy sintered and method of 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 the side that a kind of powder warm-rolling and High temperature diffusion sintering prepare Fe-6.5%Si thin strips
Method, the problem of being difficult to shaping for the Fe-Si alloy thin band materials of 4.5~6.7%Si contents, using technical pure Fe powder and Si contents as
70~80% HIGH-PURITY SILICON iron powder is raw material, adds compound mixture, forms the powder mixture for being adapted to warm-rolling deformation, then use
Powder warm rolling method prepares certain thickness slab, porous, heterogeneous blank is formed after degreasing, sintering, by multiple tracks
Thin plate is obtained after secondary cold rolling-sintering, 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：Reduction Fe powder and two kinds of Industrial iron powders of water atomization Fe powder are chosen,
According to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, then it is 70~80% to add fine Si contents
HIGH-PURITY SILICON iron powder, forms Fe-4.5~6.7%Si mixed powders.Using compound mixture in mixed process by HIGH-PURITY SILICON iron powder
Adhere in the hole of iron powder surface or filling ferrous powder.Since technical pure Fe powder is the big particle with high-compressibility, mixed
Close in powder and occupy larger volume ratio, it will not be significantly reduced after adding the HIGH-PURITY SILICON iron powder that fine Si contents are 70~80%
Deformability.Play the technological merit of warm-rolling shaping, implement the shaping of powder warm-rollings at 125~150 DEG C, prepare density it is higher,
The uniform slab of Tissue distribution.Powder warm-rolling slab is subjected to vacuum or protection of reducing atmosphere in 1070~1170 DEG C of temperature ranges
Sintering, makes Fe powder particles realize not exclusively sintering, and Si and Fe realizes partially-alloyed, is formed porous, with compressibility
The high silicon steel blank of incomplete alloying.Subsequently through multiple cold rolling, not exclusively sintering, the density rise of slab, plate thickness subtract
Few, the alloying level of Si is also continuously improved.Finally vacuum or protection of reducing atmosphere are burnt in 1260~1330 DEG C of temperature ranges
Knot, realizes the homogeneous alloy of high silicon steel with the help of thermal diffusion, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, close
Spend 7.35~7.49g/cm3High silicon steel band.
The method of the present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitable
Impurity, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining for Si, Mn, P, S and other can not
The impurity avoided, by reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, and is mixed using conical mixer, V-arrangement
Material machine or drum mixer are mixed to form technical pure Fe powder basic materials, and incorporation time is 2~6h.
Si contents are used as 70~80% HIGH-PURITY SILICON iron powder, particle diameter≤10 μm, this ferrosilicon powder except containing 70~
Beyond 80%Si, major impurity is~0.25%Al ,~0.08%Ca and~0.02%C, remaining is Fe.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to
Fine silica powder, and during follow-up powder warm-rolling also being mutually twisted for powder easy to implement and improve the intensity of pressed compact, be conducive to
The stabilization of powder warm-rolling technique.Water atomization Fe powder is also a kind of widely used Industrial iron powder, has subsphaeroidal pattern, and impurity contains
Amount is less than reduction Fe powder, compressibility and mobility with higher, is conducive to the uniform flow of powder warm-rolling technical process powder
Dynamic, low impurity content is favourable to the soft magnetic characteristic of high silicon steel in water atomization Fe powder.Will two kinds of reduction Fe powder and water atomization Fe powder
Industrial iron powder, according to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, and it is each to be conducive to two kinds of straight iron powders of performance
From advantage, be also relatively common method in industrial production iron-base part.
Fe-70~80%Si high purity ferrosilicons are in process of setting in addition to primary silicon crystal grain, and at 1207 DEG C, there are eutectic
Reaction, forms the β-FeSi with tP3 structures2It is very crisp with Si phase eutectic structures, this tissue, it is easy to pass through Mechanical Crushing
Technique refines.Fe-70~80%Si high purity ferrosilicons are crushed to≤10 μm of ferrosilicon powder, the Si phases in its actual tissue, FeSi2
It is mutually more tiny, be conducive to the thermal diffusion homogenization of Si elements during subsequent high temperature sintering, form homogeneous Fe-6.5%Si single-phase alloys.
Meanwhile 20~30%Fe present in powder can effectively reduce the degree of oxidation of Si, be conducive to improve the product matter of high silicon steel
Amount.
By Fe-70~80%Si high purity ferrosilicons Mechanical Crushing to particle diameter≤10 μm, be conducive to it and be adhered to reduction Fe powder
Surface is filled in the hole of reduction Fe powder, tiny Si, FeSi2The mutually Dispersed precipitate in blank, plays structure refinement
Strengthening and Toughening acts on, and is conducive to improve follow-up blank toughness, cracking is not easily caused in densification process is rolled.But Fe-70~
More Si phases are still suffered from 80%Si high purity ferrosilicons, Si is easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2Film,
Therefore in the preparation, storage and transfer process of Fe-70~80%Si HIGH-PURITY SILICON iron powders, and in follow-up batch mixing, the operation of rolling
Inert gas shielding should be used, used instrument must also take dehydration, drying process in advance.
On the premise of oxygen content is controlled, influence of the impurity such as Al, Ca, Mn to alloy magnetic property is little, during introduce
The possibility of other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, pre- mixed Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed；
Mixed under inert protective atmosphere using low energy mixer, total amount of adding is 0.4~0.6% compounded lubricant 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,
It is 0.9~1.9mm to roll out thickness, and width is 100~200mm, and density is 6.2~6.65g/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,
2~4h 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 1070~1170
DEG C 2~4h of heat preservation sintering, sintered blank density is 6.0~6.5g/cm3。
Uniform equiaxed grain structure is formed after sintering, matrix grain is about 70~120 μm, and crystal boundary has about 10~20 μm
Hole, follow-up rolling and sintering can close.A large amount of 1~5 μm of the second phase is evenly distributed in matrix, with matrix group
Good interface cohesion is woven with, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these richness Si phases
In the presence of reducing the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile itself and matrix group
Knit good interface cohesion and Dispersed precipitate is conducive to subsequently homogenization diffusion.
Sintering temperature is too low, the connection being unfavorable between Fe powder particles and Si atoms permeatings, and sintering temperature is excessive then can be by
In the diffusion into the surface of Fe, Si element, there is thick hole, be subsequently difficult to press, 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.
(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 1070~1170 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
To 0.1~0.5mm, density reaches 7.34~7.48g/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 1070 DEG C~1170 DEG C, in vacuum-sintering or also
Sintered under originality protective atmosphere, to realize the reparation of the closing of pores and crackle, and the homogenization diffusion of a degree of Si elements.
Programming rate can be very fast at this time, in 5~10 DEG C/min, can continuous warming, soaking time determines depending on thickness of slab, during thickness of slab >=1mm,
Soaking 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 every time
, it is necessary to sinter 1 time again after to 30~45%, 0.1~0.5mm is rolled down to from the powder base of 0.9~1.9mm, is taken around again
Sintering 4~8 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 4
Re-sintering more than secondary.
Matrix after 2 cold rolling-sintering is about 100 μm of grain structure, there is a small amount of tiny hole.Matrix is brilliant
Grain has two kinds of different contrasts, this is because Si contents are different and cause to corrode difference, low Si crystal grain is conducive in this kind tissue
Machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1330 DEG C of temperature ranges, in the effect of thermal diffusion
Under, to realize the homogenization of Si, form single-phase alloy, obtain the high silicon steel of homogeneous, the thickness of plate is almost unchanged after densification sintering,
For 0.1~0.5mm, density slightly reduces, and reaches 7.35~7.49g/cm3。
Mixing iron powder per ton adds the absolute ethyl alcohol of 200~500ml in step (1) mixed process.
Particle size≤10 μm HIGH-PURITY SILICON iron powder the high-energy ball milling rushes the acquisition of rotation method.
Low energy batch mixer described in step (2) is conical mixer, V-arrangement batch mixer or drum mixer.
The lubricant of addition powder gross mass 0.4~0.6% when step (2) mixes, and powder gross mass 0.1% are sweet
Oil, the lubricant are compounded lubricant, are 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.
Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
After step (5) cold rolling when re-sintering for 1070~1170 DEG C, using under vacuum-sintering or restitutive protection's atmosphere
Sintering, programming rate determines in 5~10 DEG C/min, continuous warming, soaking time depending on thickness of slab, and during thickness of slab >=1mm, soaking time is
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 0.9~1.9mm, it is necessary to sinter 4~8 times again.
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 be by with the addition of in the technical pure Fe powder of the big volumetric portion with good plasticity granularity≤
10 μm of Fe-70~80%Si high-purity powders, form a kind of composite material of achievable powder warm-rolling；Using warm-rolling into shape
It is standby go out density is higher, the uniform slab of Tissue distribution；By not exclusively sintering, Fe powder particles is realized not exclusively and connect, and Si
Partially-alloyed, the high silicon steel blank of porous, with compressibility the incomplete alloying of formation is realized with Fe；Subsequently through more
Passage cold rolling and sintering, improve structural homogenity and compactness；Again by high-temperature diffusion process, the homogenization of Si is realized, so that
Obtain the high silicon steel band of high quality.This method realizes Technics Process Automation, continuous metaplasia by technique and equipment Design
Production, can be mass-produced 0.1~0.5mm thickness, 7.35~7.49g/cm of density3High silicon steel band.
Brief description of the drawings
Fig. 1 is the metallograph after the powder warm-rolling base sintering of the embodiment of the present invention 2；
Fig. 2 is metallograph of the plate of the embodiment of the present invention 3 after 2 cold rolling-sintering；
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 the reduction Fe powder of -100 mesh and -100 mesh according to 4:6 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 2h, is added in mixed process according to 200ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-80%Si high-purity powders of granularity≤10 μm according to 91.625:8.375
Ratio mixing, form the mixed-powder of Fe-6.7%Si.Total amount of adding is 0.6% compounded lubricant during mixing, and
0.1% glycerine mitigates the oxidation of powder heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.
Compounded lubricant is made of zinc stearate and EBS, zinc stearate:EBS is 2:8.Above-mentioned powder is mixed using V-arrangement batch mixer
4h。
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 1.9mm
Last warm-rolling slab, the width of slab is 100mm.The density of pressed compact is 6.2g/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 1070 DEG C of heat preservation sintering 4h.Burn
It is 6.25g/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 1070 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：1.9mm → 1.38mm → 1.00mm → 0.71mm → 0.50mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches
To 0.50mm, density reaches 7.34g/cm3。
For above-mentioned cold rolling made-up belt in 1330 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.35cm to obtain thickness3, Si contains
Measure the high silicon steel of single-phase homogeneous for 6.7%.
Embodiment 2
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 6:4 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 3h, is added in mixed process according to 400ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-70%Si high-purity powders of granularity≤10 μm according to 93.57:6.42
Ratio mixes, and forms the mixed-powder of Fe-4.5%Si.Total amount of adding is 0.6% compounded lubricant during mixing, and 0.1%
Glycerine mitigate powder heating process oxidation, using absolute ethyl alcohol be used as solvent, according to 500ml/ tons amounts addition.Compound profit
Lubrication prescription is made of zinc stearate and EBS, zinc stearate:EBS is 4:6.Using drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 135 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 0.9mm
Last warm-rolling slab, the width of slab is 200mm.The density of pressed compact is 6.65g/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 1170 DEG C of heat preservation sintering 2h.Burn
It is 6.70g/cm to tie base density3。
Uniform equiaxed grain structure is formed after sintering, sees Fig. 1.Matrix grain is about 70~120 μm, and crystal boundary presence about 10~
20 μm of hole, follow-up rolling and sintering can close.A large amount of 1~5 μm of the second phase is evenly distributed in matrix, with
Matrix has good interface cohesion, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these are rich
The presence of Si phases, reduces the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile its with
The good interface cohesion of matrix and Dispersed precipitate are conducive to subsequently homogenization diffusion.
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 1170 DEG C of heat preservation sinterings.With 10 DEG C/min speed continuous warmings, soaking time is
1h.Specifically pressure-annealing schedule is：0.9mm → 0.63mm → 0.38mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm,
I.e. after 6 cold rollings and 5 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.46g/cm3。
For above-mentioned cold rolling made-up belt in 1260 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.49g/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 the reduction Fe powder of -100 mesh and -100 mesh according to 6:4 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 4h, is added in mixed process according to 500ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-76%Si high-purity powders of granularity≤10 μm according to 91.45:8.55
Ratio mixes, and forms the mixed-powder of Fe-6.5%Si.Total amount of adding is 0.6% compounded lubricant during mixing, and 0.1%
Glycerine mitigate powder heating process oxidation, using absolute ethyl alcohol be used as solvent, according to 500ml/ tons amounts addition.Compound profit
Lubrication prescription is made of zinc stearate and EBS, zinc stearate:EBS is 3:7.Using drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 145 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 120mm.The density of pressed compact is 6.25g/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 1130 DEG C of insulations and burn
Tie 3h.Sintered blank density is 6.30g/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 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 7.38g/cm3。
Fig. 2 is shown in metallographic structure after 2 cold rolling-sintering, and matrix is about 100 μm of grain structure, exists a small amount of thin
Small hole.Matrix grain has two kinds of different contrasts, this is because Si contents are different and cause to corrode difference, in this kind tissue
Low Si crystal grain is conducive to machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.39g/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 the reduction Fe powder of -100 mesh and -100 mesh according to 5:5 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 6h, is added in mixed process according to 500ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-72%Si high-purity powders of granularity≤10 μm according to 91.05:8.95
Ratio mixes, and forms the mixed-powder of Fe-5.8%Si.Total amount of adding is 0.6% compounded lubricant during mixing, and 0.1%
Glycerine mitigate powder heating process oxidation, using absolute ethyl alcohol be used as solvent, according to 500ml/ tons amounts addition.Compound profit
Lubrication prescription is made of zinc stearate and EBS, zinc stearate:EBS is 3:7.Using drum mixer by above-mentioned powder mixing 3h.
Mixed-powder is heated to 150 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 1.7mm
Last warm-rolling slab, the width of slab is 160mm.The density of pressed compact is 6.35g/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 6.40g/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：1.7mm → 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 7.41g/cm3。
For above-mentioned cold rolling made-up belt in 1290 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.42g/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 (8)
1. a kind of method that powder warm-rolling prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that comprise the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitably miscellaneous
Matter, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, will reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, using conical mixer, V-arrangement batch mixer
Or drum mixer is mixed to form technical pure Fe powder basic materials, incorporation time is 2~6h；
Si contents are used as 70~80% HIGH-PURITY SILICON iron powder, particle diameter≤10 μm, major impurity is~0.25%Al ,~0.08%
Ca and~0.02%C, remaining is Fe；
(2) powder mixes：
According to the ratio of Fe-4.5~6.7%Si, pre- mixed Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed；Lazy
Property protective atmosphere under mixed using low energy mixer, total amount of adding is 0.4~0.6% compounded lubricant 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 0.9~1.9mm to go out thickness, and width is 100~200mm, and density is 6.2~6.65g/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 1070~1170 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density is 6.25~6.7g/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 1070~1170 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
0.1~0.5mm, density reach 7.34~7.48g/cm3。
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1330 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 7.35~7.49g/cm3。
2. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that：
Mixing iron powder per ton adds 200~500ml absolute ethyl alcohols in step (1) mixed process.
3. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si thin strips with High temperature diffusion sintering, it is special
Sign is：The HIGH-PURITY SILICON iron powder high-energy ball milling of particle diameter≤10 μm rushes the acquisition of rotation method.
4. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that：
Low energy batch mixer described in step (2) is conical mixer, V-arrangement batch mixer or drum mixer.
5. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that：
The lubricant of powder gross mass 0.4~0.6% is added when step (2) mixes, then adds the glycerine of powder gross mass 0.1%, institute
The lubricant stated 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.
6. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that：
After step (5) cold rolling when re-sintering for 1070~1170 DEG C, sinter, heat up using under vacuum-sintering or restitutive protection's atmosphere
Speed determines in 5~10 DEG C/min, continuous warming, soaking time depending on thickness of slab, and during thickness of slab >=1mm, soaking time is 1~2h；Plate
Thickness in 0.1~1mm, soaking time is reduced to 0.5~1h, after the accumulation drafts after sintering reaches 30~45% every time, it is necessary to
Again sinter 1 time, be rolled down to 0.1~0.5mm from the powder base of 0.9~1.9mm, it is necessary to sinter 4~8 times again.
7. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that：
Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
8. the method that powder warm-rolling as claimed in claim 1 prepares Fe-6.5%Si bands with diffusion-sintering, it is characterised in that：
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, is prevented
Only deformed in sintering process.
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