CN108097964A - A kind of powder warm-rolling manufacture method of high silicon steel thin belt material - Google Patents
A kind of powder warm-rolling manufacture method of high silicon steel thin belt material Download PDFInfo
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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
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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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
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Abstract
A kind of powder warm-rolling manufacture method of high silicon steel thin belt material, the present invention is using reduction Fe powder, Si contents are 70~80% HIGH-PURITY SILICON iron powder, form Fe 4.5~6.7%Si mixed powders, HIGH-PURITY SILICON iron powder is adhered in the hole of reduced iron powder surface or filling ferrous powder in mixed process using compound mixture, implement the shaping of powder warm-rolling at 125~150 DEG C, prepare slab, powder warm-rolling slab is carried out to vacuum or protection of reducing atmosphere sintering at 1070~1170 DEG C, realize Fe and Si partially-alloyed, it is formed porous, the high silicon steel blank of incomplete alloying with compressibility.It subsequently through multiple cold rolling, sintering, is finally sintered in 1260~1340 DEG C of vacuum or protection of reducing atmosphere, realizes the homogeneous alloy of high silicon steel, obtain 0.1~0.5mm thickness containing 4.5~6.7%Si, 7.32~7.42g/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
Metallurgy sintered and rolling deformation method.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis loop is very narrow, it and fundamental magnetization curve are almost
It overlaps, is 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.There is no absolute predominances, such as slope in soft magnetic materials for the maximum permeability of Fe-Si alloys
The maximum permeability of alloy can not reach 200000.However the manufacture of the Fe-Si lattens of Si ＜ 4.5% is at low cost, 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 increases with Si contents
And reduce, it disappears substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases with Si contents and is increased, 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 the iron core of amount or large size is sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is in the military aviations such as spacecraft, submarine and guided missile field, Fe-Si systems alloy plays particularly important role.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared in as transformer material on No. 11 airships of Apollo, are completed the mankind and are landed on the moon for the first time
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 is for the first time the study found that 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 have lower iron loss and higher magnetic conductivity.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 spends for 0.1~0.5mm, width is the No yield point 6.5%Si steel discs of 400mm.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 to alloy diffusion inside alloy is finally made to reach required content by raised 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
It asks, 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 ", and 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, 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 generate 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 manufacture method of high silicon steel thin belt material, for 4.5~6.7%Si
The problem of Fe-Si alloy thin band materials of content are difficult to shape, using reduced iron powder and Si contents as 70~80% HIGH-PURITY SILICON iron powder
For raw material, compound mixture is added, the powder mixture for being suitble to warm-rolling deformation is formed, then one is prepared using powder warm rolling method
Determine the slab of thickness, form porous, heterogeneous blank after degreasing, sintering, 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 the reduction Fe powder of irregular pattern, fine Si contents
For 70~80% HIGH-PURITY SILICON iron powder, Fe-4.5~6.7%Si mixed powders are formed.Using compound mixture in mixed process
HIGH-PURITY SILICON iron powder is adhered in the hole of reduced iron powder surface or filling ferrous powder.Since reduction Fe powder is with high-compressibility
Big particle occupies larger volume ratio in mixed powder, after adding the HIGH-PURITY SILICON iron powder that fine Si contents are 70~80%
Its deformability will not be significantly reduced.The technological merit of warm-rolling shaping is played, implements the shaping of powder warm-rolling, system at 125~150 DEG C
It is standby go out density is higher, the uniform slab of Tissue distribution.Powder warm-rolling slab is subjected to vacuum in 1070~1170 DEG C of temperature ranges
Or protection of reducing atmosphere sintering, make Fe powder particles realize not exclusively sintering, and Si and Fe realize it is partially-alloyed, formation it is porous,
The high silicon steel blank of incomplete alloying with compressibility.Subsequently through multiple cold rolling, not exclusively sintering, the density of slab
Rise, plate thickness are reduced, and the alloying level of Si is also continuously improved.Finally in 1260~1340 DEG C of temperature ranges vacuum or also
Former gas-protecting sintering realizes the homogeneous alloy of high silicon steel with the help of thermal diffusion, obtains 0.1 containing 4.5~6.7%Si
~0.5mm is thick, 7.32~7.42g/cm of density3High silicon steel band.
The method specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in reduced iron powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, using the Si contents of refining, grain size≤10 μm, this ferrosilicon powder is except containing 70 for 70~80% HIGH-PURITY SILICON iron powder
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
Thin and tall pure silicon iron powder, and during follow-up powder warm-rolling also being mutually twisted for powder easy to implement and improve the intensity of green compact,
Be conducive to the stabilization of powder warm-rolling technique.
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 eutectics
Reaction, forms the β-FeSi with tP3 structures2With Si phase eutectic structures, it is this tissue it is very crisp, 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, Si phases, FeSi in actual tissue2
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 grain size≤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 subsequent blank toughness, cracking is not easily caused in densification process is rolled.But Fe-70~
There are still more Si phases, Si in 80%Si high purity ferrosilicons to be 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, introduces in the process
The possibility of other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed；Lazy
Property protective atmosphere under using low energy mixer mix.During mixing, the lubricant of addition powder gross mass 0.4~0.6%.
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 that technique success or not, and the selection principle of lubricant should
When meeting glass transition temperature at 120~150 DEG C or so, the conditions 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,
Thickness is rolled out as 1.2~2.4mm, width is 100~200mm, and density is 6.05~6.55g/cm3Powder warm-rolling slab.
Mixed-powder is heated to 125~150 DEG C using powder heating unit before rolling, and roll is preheating to similary 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 in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace,
2h~4h is kept the temperature respectively using the heating 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 are 6.1~6.6g/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, subsequent rolling and sintering can be closed.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 with matrix group
It knits 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 excessively high then can be by
In the diffusion into the surface of Fe, Si element, there is coarse 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 contraction causes to crack.Heating rate should not be too fast during sintering, and multistage heat preservation 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. may be employed 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 7.31~7.41g/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, 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
Originality protective atmosphere is sintered, to realize the reparation of the closing of pores and crackle and the homogenization diffusion of a degree of Si elements.This
When heating 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, protects
The warm time is 1~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time.Sintered accumulation drafts reaches every time
, it is necessary to be sintered 1 time again after 30~45%, 0.1~0.5mm is rolled down to from the powder base of 1.2~2.4mm, takes around and burns again
Knot 4~8 times.In addition, in order to which the density of plate is made to reach 7.2g/cm3More than (about the 95% of theoretical density), it is also desirable to 4 times
Above re-sinters.
By about 100 μm of grain structure of 2 cold rollings-sintered metallographic structure, there is a small amount of tiny hole.Matrix
Crystal grain is there are two types of different contrasts, this is because Si contents are different and cause to corrode difference, low Si crystal grain is favourable in this kind tissue
In 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 1260~1340 DEG C of temperature ranges, in the effect of thermal diffusion
Under, it realizes the homogenization of Si, forms 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, reach 7.32~7.42g/cm3。
The HIGH-PURITY SILICON iron powder high-energy ball milling of grain size≤10 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 be compounded lubricant, be 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 can be used and ceramics are burnt
Boat.But plate must tile placement, and tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of elements such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel
Large effect can subsequently be annealed by wet hydrogen, the technological means such as normalizing treatment are controlled by.
Essence of the invention is by being with the addition of the μ of granularity≤10 in the reduction Fe powder of the big volumetric portion with good plasticity
Fe-70~80%Si high-purity powders of m form a kind of composite material of achievable powder warm-rolling；It is shaped and prepared using warm-rolling
Go out that density is higher, the uniform slab of Tissue distribution；By being not exclusively sintered, Fe powder particles is made to realize not exclusively connection, and Si with
Fe realizes partially-alloyed, the high silicon steel blank of porous, with compressibility the incomplete alloying of formation；Subsequently through multiple tracks
Secondary 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
Obtain the high silicon steel band of high quality.This method realizes Technics Process Automation, continuous production by technique and equipment Design,
Can be mass-produced 0.1~0.5mm thickness, 7.32~7.42g/cm of density3High silicon steel band.
Description of the drawings
Fig. 1 is the sintered metallograph of powder warm-rolling base of the embodiment of the present invention 2；
Fig. 2 is that the plate of the embodiment of the present invention 3 passes through 2 cold rollings-sintered metallograph；
Fig. 3 is XRD diffraction curve figures after the powder warm-rolling base high temperature sintering of the embodiment of the present invention 4.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the reduction Fe powder of -100 mesh and the Fe-80%Si high-purity powders of granularity≤10 μm according to 91.625:8.375 ratio
Example mixing.Form Fe-6.7Si alloys.The compounded lubricant and 0.1% glycerine that total amount of adding is 0.4% during mixing mitigate
The oxidation of powder heating process using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant is by tristearin
Sour 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 150 DEG C using powder heating unit, and roll is preheating to similary 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 green compact is 6.05g/cm3。
Powder strip plate is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts
With the heating 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.It burns
It is 6.1g/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：2.4mm → 1.59mm → 1.03mm → 0.71mm → 0.49mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches
To 0.49mm, density reaches 7.31g/cm3。
For above-mentioned cold rolling made-up belt in 1340 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.32g/cm to obtain thickness3, Si
Content is the 6.7% high silicon steel of single-phase homogeneous.
Embodiment 2
By the reduction Fe powder of -100 mesh and the Fe-70%Si high-purity powders of granularity≤10 μm according to 93.57:6.42 ratio
Mixing forms Fe-4.5Si alloys.The compounded lubricant and 0.1% glycerine that total amount of adding is 0.6% during mixing 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 drum mixer by above-mentioned powder mixing 6h.
Mixed-powder is heated to 125 DEG C using powder heating unit, and roll is preheating to similary 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 1.0mm
Last warm-rolling slab, the width of slab is 200mm.The density of green compact is 6.55g/cm3。
Powder strip plate is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts
With the heating 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.It burns
It is 6.6g/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, subsequent rolling and sintering can be closed.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 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：1.0mm → 0.65mm → 0.39mm → 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 7.41g/cm3。
For above-mentioned cold rolling made-up belt in 1260 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.42g/cm to obtain thickness3, Si
Content is the 4.5% high silicon steel of single-phase homogeneous.
Embodiment 3
By the reduction Fe powder of -100 mesh and the Fe-76%Si high-purity powders of granularity≤10 μm according to 91.45:8.55 ratio
Mixing forms the mixed-powder of Fe-6.5%Si.During mixing total amount of adding be 0.6% compounded lubricant and 0.1% it is sweet
Oil mitigates the oxidation of powder heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant
It 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 140 DEG C using powder heating unit, and roll is preheating to similary 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 green compact is 6.1g/cm3。
Powder strip plate is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the heating rate of 3 DEG C/min, and 2h, 400 DEG C of heat preservation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1150 DEG C of heat preservations and burn
Tie 3h.Sintered blank density is 6.15g/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 1160 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 7.32g/cm3。
See Fig. 2 by 2 cold rollings-sintered metallographic structure, matrix is about 100 μm of grain structure, is existed a small amount of thin
Small hole.Matrix grain is there are two types 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 7.33g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous.
Embodiment 4
By the reduction Fe powder of -100 mesh and the Fe-72%Si high-purity powders of granularity≤10 μm according to 91.05:8.95 ratio
Mixing forms the mixed-powder of Fe-5.8%Si.During mixing total amount of adding be 0.6% compounded lubricant and 0.1% it is sweet
Oil mitigates the oxidation of powder heating process, using absolute ethyl alcohol as solvent, is added according to 500ml/ tons of amounts.Compounded lubricant
It 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 130 DEG C using powder heating unit, and roll is preheating to similary 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 green compact is 6.14g/cm3。
Powder strip plate is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the heating rate of 4 DEG C/min, and 3h, 400 DEG C of heat preservation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1130 DEG C of heat preservations and burn
Tie 2h.Sintered blank density is 6.18g/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.2.0mm→
1.3mm → 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm, i.e., after 7 cold rollings and 6 sintering, the thickness of plate
Degree reaches 0.21mm, and density reaches 7.36g/cm3.In 1320 DEG C of vacuum-sintering 2h, obtain thickness is about above-mentioned cold rolling made-up belt
0.22mm, density 7.37g/cm3, Si contents are 5.8%, and the XRD analysis figure of final plate is shown in Fig. 3, are that single-phase homogeneous is high
Silicon steel.
Claims (7)
1. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material, it is characterised in that comprise the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in reduced iron powder, remaining is Si, Mn, P, S and other are inevitably miscellaneous
Matter uses the Si contents of refining as 70~80% HIGH-PURITY SILICON iron powder, grain size≤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, reduction Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed；It is protected in inertia
It protects under atmosphere and is mixed using low energy mixer, during mixing, the lubricant of addition powder gross mass 0.4~0.6%；
(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
Go out thickness for 1.2~2.4mm, width is 100~200mm, and density is 6.05~6.55g/cm3Powder warm-rolling slab.Rolling
It is preceding that mixed-powder is heated to 125~150 DEG C using powder heating unit, and roll is preheating to similary temperature；
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2
The heating rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, it then will heat up to 1070~1170 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density are 6.1~6.6g/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 7.31~7.41g/cm3；
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1340 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 almost unchanged after densification sintering, is 0.1
~0.5mm, reaches 7.32~7.42g/cm3。
2. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material as described in claim 1, it is characterised in that：The grain
The HIGH-PURITY SILICON iron powder high-energy ball milling of footpath≤10 μm rushes the acquisition of rotation method.
3. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material as described in claim 1, it is characterised in that：Described is low
Energy batch mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material as described in claim 1, it is characterised in that：Step (2)
The lubricant of powder gross mass 0.4~0.6% is added during mixing, while adds the glycerine of powder gross mass 0.1%, the profit
Lubrication prescription is compounded lubricant, is made of zinc stearate and vinyl bis-stearamides, zinc stearate:EBS is 4:6~2:8, it uses
Absolute ethyl alcohol is added as solvent according to 400~600ml of powder per ton.
5. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material as described in claim 1, it is characterised in that：Step (5)
After cold rolling when re-sintering for 1070 DEG C~1170 DEG C, it is sintered using under vacuum-sintering or restitutive protection's atmosphere, heating rate
In 5~10 DEG C/min, continuous warming, soaking time is determined depending on thickness of slab, and during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab exists
0.1~1mm, soaking time are reduced to 0.5~1h, it is necessary to again after sintered accumulation drafts reaches 30~45% every time
Sintering 1 time is rolled down to 0.1~0.5mm, it is necessary to be sintered 4~8 times again from the powder base of 1.2~2.4mm.
6. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material as described in claim 1, it is characterised in that：Step (4)
The support plate uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. a kind of powder warm-rolling manufacture method of high silicon steel thin belt material as described in claim 1, it is characterised in that：High temperature sintering
When overlapping place sintering plate, interlayer be laid with MgO powder, plate tiling place, on plate place tablet weight, prevent sintered
It is deformed in journey.
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