CN108097965A - A kind of powder extruding method for making of high silicon steel thin belt material - Google Patents
A kind of powder extruding method for making of high silicon steel thin belt material Download PDFInfo
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- CN108097965A CN108097965A CN201711368375.3A CN201711368375A CN108097965A CN 108097965 A CN108097965 A CN 108097965A CN 201711368375 A CN201711368375 A CN 201711368375A CN 108097965 A CN108097965 A CN 108097965A
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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
- B22F3/20—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
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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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- 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
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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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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- 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 powder extruding method for making of high silicon steel thin belt material, using the reduction Fe powder of irregular pattern, fine Si contents are 70~80% HIGH-PURITY SILICON iron powder, form Fe 4.5~6.7%Si mixed powders.By being molded squarely base; it is heated to 950~1050 DEG C of realization Fe phase austenitizings; slab is hot extruded into the deflection that extrusion ratio is 8~16; then powder is squeezed into slab and carries out vacuum or protection of reducing atmosphere sintering in 1070~1170 DEG C of temperature ranges; it is sintered subsequently through multiple cold rolling, low temperature diffusion; the finally homogeneous alloy of vacuum or the high silicon steel of protection of reducing atmosphere sintering realization in 1275~1335 DEG C of temperature ranges; it is thick to obtain 0.1~0.5mm containing 4.5~6.7%Si, density >=7.38g/cm3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder metallurgy of high silicon steel thin belt material is burnt
The method of knot, hot extrusion and rolling deformation.
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 present invention provides a kind of powder extruding method for making of high silicon steel thin belt material, for 4.5~6.7%Si contents
The problem of Fe-Si alloy thin band materials are difficult to shape, the HIGH-PURITY SILICON iron powder for being 70~80% using reduced iron powder and Si contents as raw material,
Uniformly mixing is molded into extruding green compact after adding binder, then prepares certain thickness slab using powder hot-extrusion method,
It is acted on using the large deformation of hot extrusion and causes the raising of extruded stock density, structure refinement, and the achievement unit division under thermal diffusion effect
Aurification forms the α-Fe crystal grain of the poor Si of plastic deformation ability and the heterogeneous structure of the high Si phases of brittleness.It is subsequently cold by multi-pass
Thin plate is obtained after rolling-being sintered, is finally sintered using High temperature diffusion and obtains the high silicon steel band of homogeneous single phase.
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.It is incited somebody to action by suitable bonding agent, dispersant
Fine HIGH-PURITY SILICON iron powder is adhered in mixed process in the hole of reduced iron powder surface or filling ferrous powder.Due to reducing Fe powder
For the big particle with high-compressibility, larger volume ratio is occupied in mixed powder, is added after fine HIGH-PURITY SILICON iron powder not
Its plastic deformation ability is significantly reduced, it can be by being molded squarely base.It is heated to 950~1050 DEG C of realization Fe phase austenites
Change, slab is hot extruded into the deflection that extrusion ratio is 8~16.Then powder is squeezed into slab in 1070~1170 DEG C of temperature models
It encloses and carries out vacuum or protection of reducing atmosphere sintering, Fe powder particles is made to realize metallurgical binding, and Si and Fe realizes partially-alloyed, shape
Into α-Fe crystal grain fine and close, with the poor Si of plastic deformation ability and the high silicon steel blank of heterogeneous structure of the high Si phases of brittleness.Subsequently
It is sintered by multiple cold rolling, low temperature diffusion, the density rise of slab, plate thickness are reduced, and the alloying level of Si is also continuously improved.
Finally vacuum or protection of reducing atmosphere sintering in 1275~1335 DEG C of temperature ranges, realizes high silicon steel with the help of thermal diffusion
Homogeneous alloy, it is thick to obtain 0.1~0.5mm containing 4.5~6.7%Si, density >=7.38g/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 reduced iron powder, remaining is the impurity such as Si, Mn, P, S, middle grain size
Positioned at 75~106 μm;Use the Si contents of refining for 70~80% HIGH-PURITY SILICON iron powder, with the ferrosilicon powder of grain size≤10 μm, this
Kind of ferrosilicon powder is in addition to containing 70~80%Si, and major impurity is~0.25%Al ,~0.08%Ca ,~0.02%C, remaining
For 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 in follow-up powder extrusion process also being mutually twisted for powder easy to implement and improve the intensity of green compact.
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 follow-up batch mixing, hot extrusion, rolling
Inert gas shielding should be used in the process, and used instrument must also take dehydration, drying process in advance.
On the premise of oxygen content is controlled, influence of the impurity such as other Al, Ca, Mn to alloy magnetic property is little, in the process
The possibility for introducing other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and fine Fe-70~80%Si HIGH-PURITY SILICONs iron powder are weighed;
It is mixed under inert protective atmosphere using low energy mixer, mixing velocity and time depending on mixing uniformity, should try one's best and subtract
Processing hardening occurs in mixed process for light Fe powder.
(3) powder squeezes
Square green compact is prepared using compression-moulding methods, green density is 6.36~6.53g/cm3, using square extruding
Cylinder, extrusion ratio are 8~16, using sintered-carbide die, lubricant are done with machine oil and glass dust, by molding square billet in nitrogen before squeezing
Be heated to 950~1050 DEG C under gas shielded effect, keep the temperature 2~4h, extrusion cylinder and extrusion die 400~600 DEG C of preheating insulations 1~
2h implements hot extrusion, and the density of slab is 6.80~7.12g/cm after hot extrusion3;
(4) it is sintered
Hot extrusion pressing plate is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into sintering furnace.Using 2~5 DEG C/
The heating rate of min is warming up to 1070~1170 DEG C of 2~4h of heat preservation sintering.Sintered blank density is 7.37~7.49g/cm3.With
Extruded stock density is compared, and density slightly reduces.
Sintering temperature is too low, is unfavorable for the metallurgical binding of Fe powder particles and Si element thermal diffusions;And sintering temperature is excessively high then
Si elements can be caused quickly to spread, cause crystal grain excessive high hardness, embrittlement, follow-up rolling deformation is difficult to realize.
Take reproducibility, inert gas shielding sintering.Can be used during sintering W, Mo, heat resisting steel etc. as support plate (or
Burn boat), the ceramic wafers such as corundum, zirconium oxide can also be used, but metallic plate thermal conductivity is good, and beneficial to Even Sintering.
The texture of coarse crystal containing the second phase is formed after sintering.X-ray diffraction Discriminating materials are heterogeneous Fe (Si)
Phase, body-centred cubic several characteristic peaks have apparent separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, wherein must
Have that the Si contents in a kind of Fe phases are low, there is plastic deformation ability.
(5) cold rolling-sintering densification
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1070~1170 DEG C of 0.5~2h of heat preservation sintering in sintering furnace.After multiple cold rolling-sintering,
The thickness of plate reaches 0.1~0.5mm, and density reaches 7.38~7.50g/cm3。
Cold-rolling deformation can be born since there are deformable Fe phases, slab in blank.But there is also more in slab
High Si phases, performance is more crisp, therefore for amount not above 8%, accumulation total reduction reaches 30~45%, about needs under every time rolling
Want 8~20 passages.
Due to existing hard crisp phase, it is necessary to take and keep the temperature vacuum-sintering or restitutive protection's gas again at 1070~1170 DEG C
Atmosphere is sintered, to realize that the closing of pores and the reparation of crackle and a degree of Si elements homogenization are generated in cold-rolled process expands
It dissipates., it is necessary to be sintered 1 time again, from the hot extrusion of 2.5~5.0mm after sintered accumulation drafts reaches 30~45% every time
Plate is rolled down to 0.1~0.5mm, takes around and is sintered 6~10 times again.
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1275~1335 DEG C of temperature ranges, in thermal diffusion
Under effect, the homogenization of Si is realized, form 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 slightly reduces, and reaches 7.42~7.46g/cm3。
Using the square extrusion cylinder of 40 × 120mm in step (3), extrusion die is 5~2.5mm × 120mm, corresponding to squeeze
Than being respectively 8~16;Using sintered-carbide die, lubricant is done with machine oil and glass dust, square billet will be molded before squeezing in nitrogen
It is heated to 950~1050 DEG C under protective effect, 2~4h, extrusion cylinder and extrusion die is kept the temperature in 600 DEG C of preheating insulation 2h, using 300
Ton press implements hot extrusion, and the density of slab is 7.37~7.49g/cm after hot extrusion3, three point bending test shows plasticity,
Bending strength is 63~189MPa.
The ferrosilicon powder of grain size≤10 μm described in step (1) is using high-energy ball milling or rushes the acquisition of rotation method.
The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
Add cellulose, paraffin micro mist or zinc stearate water-insoluble binder during mixing, the additive amount total amount of binder is not
It more than the 0.8% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays passivation Si powder, bonding Fe-Si
The effect of powder, enhancing powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed-powder gross mass
2%.
Using the square extrusion cylinder of 40 × 120mm in step (3), extrusion die is 5~2.5mm × 120mm, corresponding extrusion ratio
Respectively 8~16;Using sintered-carbide die, lubricant is done with machine oil and glass dust, implements hot extrusion using 300 tons of press,
Three point bending test shows plasticity, and bending strength is 63~189MPa.
Step (4) described support plate 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 low volume ratio in the reduction Fe powder of the big volumetric portion with good plasticity
The fine Si powder of simple substance of example forms Fe-4.5~6.7%Si mixed powders.High density, high uniformity plate are obtained using hot extrusion
Base.The element alloyed degree of slab Si is low, and microscopic structure is had high by high-ductility Fe phases and brittleness richness Si phase compositions
Cold deformation ability can be improved structural homogenity and compactness, then High temperature diffusion sintering, realized by multi-pass cold rolling and sintering
The homogenization of Si, so as to obtain the high silicon steel band of high quality.This method realizes technical process certainly by technique and equipment Design
Dynamicization, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.4g/cm3High silicon steel band.
Description of the drawings
Fig. 1 is the three-point bending graph of blank after the powder of the embodiment of the present invention 1 squeezes;
Fig. 2 is metallographic structure figure after powder extruding-cold rolling-sintering of the embodiment of the present invention 2;
Fig. 3 is XRD diffraction curve figures after powder extruding-cold rolling-sintering of the embodiment of the present invention 2;
Fig. 4 is XRD diffraction curve figures after powder extruding-cold rolling-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 forms the mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine are added during mixing
Oil.Absolute ethyl alcohol is added according to 200ml/ tons of amount.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly
40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.32g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 5 × 120mm, and corresponding extrusion ratio is 8.It will before squeezing
Molding square billet is heated to 950 DEG C under nitrogen protective effect, keeps the temperature 4h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.It adopts
Implement hot extrusion with 300 tons of press, the density of slab is 6.80g/cm after hot extrusion3, three point bending test shows plasticity, such as
Fig. 1, bending strength 63MPa.
Using the heating rate of 2 DEG C/min, 1070 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.23g/cm3.It burns
The texture of coarse crystal containing the second phase is formed after knot.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1070 DEG C of heat preservation sintering 2h in sintering furnace.Specifically pressure-annealing schedule is:5mm→
3.5mm → 2.4mm → 1.6mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate
Reach 0.49mm, density reaches 7.37g/cm3。
1h finally is sintered in 1335 DEG C of Temperature Vacuums, under the action of thermal diffusion, the homogenization of Si is realized, forms single-phase conjunction
Gold obtains the high silicon steel of homogeneous.The thickness of plate is almost unchanged after densification sintering, is 0.49mm, and density reaches 7.38g/cm3。
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 the mixed-powder of Fe-4.5%Si.The zinc stearate of raw material total amount 0.7%, 0.1% machine oil are added during mixing.
Absolute ethyl alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder mixing 6h.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly
40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.53g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is 2.5 × 120mm, and corresponding extrusion ratio is 16.It will before squeezing
Molding square billet is heated to 1050 DEG C under nitrogen protective effect, keeps the temperature 2h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.
Implement hot extrusion using 300 tons of press, the density of slab is 7.12g/cm after hot extrusion3, three point bending test shows plasticity,
Bending strength is 189MPa.
Using the heating rate of 2 DEG C/min, 1170 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.35g/cm3.It burns
The texture of coarse crystal containing the second phase is formed after knot, sees Fig. 2.X-ray diffraction Discriminating materials are heterogeneous Fe (Si) phase, such as
Fig. 3 findings, body-centred cubic several characteristic peaks have apparent separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility,
In must have that the Si contents in a kind of Fe phases are low, there is plastic deformation ability.
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1170 DEG C of heat preservation sintering 0.5h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate
Degree reaches 0.1mm, and density reaches 7.43g/cm3.Specifically cold rolling-sintering schedule is:2.5mm→1.85mm→1.39mm→
1.15mm → 0.89mm → 0.65mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, i.e., through 10 cold rollings and
After 9 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.49g/cm3。
4h finally is sintered in 1275 DEG C of Temperature Vacuums, forms the high silicon steel of single-phase homogeneous that Si contents are 4.5%, thickness is
0.1mm, density reach 7.50g/cm3。
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.The paraffin micro mist of raw material total amount 0.4% is added during mixing, 0.2% methyl is fine
Dimension element, 0.1% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Above-mentioned powder is mixed using drum mixer
6h。
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly
40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.39g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is 4 × 120mm, and corresponding extrusion ratio is 10.By mould before squeezing
Pressure square billet is heated to 1000 DEG C under nitrogen protective effect, keeps the temperature 3h.Extrusion cylinder and extrusion die are in 600 DEG C of preheating insulation 2h.It adopts
Implement hot extrusion with 300 tons of press, the density of slab is 6.83g/cm after hot extrusion3, bending strength 146MPa.
Using the heating rate of 3 DEG C/min, 1150 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.25g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, and specific cold rolling-sintering schedule is:4.0mm→2.8mm→
2.0mm → 1.40mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 7 cold rollings and 6 sintering, the thickness of plate
Degree reaches 0.27mm, and density reaches 7.38g/cm3。
For above-mentioned cold rolling made-up belt in 1310 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 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.The paraffin micro mist of raw material total amount 0.6%, 0.2% machine oil are added during mixing.
Absolute ethyl alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder mixing 3h.
Square green compact is prepared using compression-moulding methods, the length and width of green compact is respectively 120mm and 80mm, is highly
40mm uses surface pressing to be suppressed for the pressure of 600MPa, and the total output pressure of press is 576 tons.The green density of acquisition is
6.41g/cm3。
Using the square extrusion cylinder of 40 × 120mm, extrusion die is respectively 3.2 × 120mm, and corresponding extrusion ratio is 12.5.It squeezes
Molding square billet under nitrogen protective effect is heated to 1020 DEG C before pressure, keeps the temperature 4h.Extrusion cylinder and extrusion die are protected in 600 DEG C of preheatings
Warm 2h.Implement hot extrusion using 300 tons of press, the density of slab is 6.84g/cm after hot extrusion3, bending strength 140MPa.
Using the heating rate of 4 DEG C/min, 1120 DEG C of heat preservation sintering 2h are warming up to.Sintered blank density is 7.26g/cm3。
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to stagnation pressure
After lower rate reaches 30~45%, then in 1120 DEG C of heat preservation sintering 1h in sintering furnace.After multiple cold rolling-sintering, the thickness of plate
Reach 0.22mm, density reaches 7.43g/cm3.Specifically cold rolling-sintering schedule is:3.2mm→2.4mm→2.0mm→1.3mm→
0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm, i.e., after 9 cold rollings and 8 sintering, the thickness of plate reaches
0.21mm, density reach 7.39g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.40g/cm to obtain thickness3, Si
Content is 5.8%, and the XRD analysis figure of final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.
Claims (7)
1. a kind of powder extruding method for making 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 and S and inevitable impurity,
Middle grain size is located at 75~106 μm;Use the Si contents of refining for 70~80% HIGH-PURITY SILICON iron powder, with the ferrosilicon of grain size≤10 μm
Powder, the impurity of HIGH-PURITY SILICON iron powder is~0.25%Al ,~0.08%Ca ,~0.02%C, remaining is Fe;
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and fine Fe-70~80%Si HIGH-PURITY SILICONs iron powder are weighed;Lazy
Property protective atmosphere under using low energy mixer mix;
(3) powder squeezes
Square green compact is prepared using compression-moulding methods, green density is 6.32~6.53g/cm3;Using square extrusion cylinder, squeeze
Pressure ratio is 8~16, and using sintered-carbide die, lubricant is done with machine oil and glass dust, protects molding square billet in nitrogen before squeezing
950~1050 DEG C are heated under shield effect, keep the temperature 2~4h, extrusion cylinder and extrusion die in 400~600 DEG C of 1~2h of preheating insulation,
Implement hot extrusion, the density of slab is 6.80~7.12g/cm after hot extrusion3;
(4) it is sintered
Hot extrusion pressing plate is placed on the support plate that surface is coated with MgO micro mists, is placed into sintering furnace, using 2~5 DEG C/min's
Heating rate, is warming up to 1070~1170 DEG C of 2~4h of heat preservation sintering, and sintered blank density is 7.23~7.35g/cm3;
(5) cold rolling-sintering densification
By above-mentioned sintering slab, progressively cold rolling-sintering is thinned, single pass rolling reduction≤8%, through multi- pass rolling to total reduction
After reaching 30~45%, then in 1070~1170 DEG C of 0.5~2h of heat preservation sintering, after multiple cold rolling-sintering, plate in sintering furnace
Thickness reach 0.1~0.5mm, density reaches 7.37~7.49g/cm3;
(6) high temperature sintering is homogenized
Finally vacuum or restitutive protection 1~4h of atmosphere sintering in 1275~1335 DEG C of temperature ranges, in the effect of thermal diffusion
Under, realize the homogenization of Si, form single-phase alloy, obtain the high silicon steel of homogeneous, after densification sintering the thickness of plate for 0.1~
0.5mm, density are 7.38~7.50g/cm3。
2. the powder extruding method for making of high silicon steel thin belt material as described in claim 1, it is characterised in that:The low energy
Mixer is conical mixer, V-arrangement batch mixer or drum mixer.
3. the powder extruding method for making of high silicon steel thin belt material as described in claim 1, it is characterised in that:Step (1) is described
Grain size≤10 μm ferrosilicon powder using high-energy ball milling or rush rotation method acquisition.
4. the powder extruding method for making of high silicon steel thin belt material as described in claim 1, it is characterised in that:Step is adopted in (3)
With the square extrusion cylinder of 40 × 120mm, extrusion die is 5~2.5mm × 120mm, and corresponding extrusion ratio is respectively 8~16;Using hard
Matter alloy mold does lubricant with machine oil and glass dust, implements hot extrusion using 300 tons of press, three point bending test is shown
Plasticity, bending strength are 63~189MPa.
5. the powder extruding method for making of high silicon steel thin belt material as described in claim 1, it is characterised in that:Add fiber during mixing
Element, paraffin micro mist or the water-insoluble binder of zinc stearate, the additive amount total amount of binder are no more than mixed-powder gross mass
0.8%, while add grease and absolute ethyl alcohol does passivator, rise passivation Si powder, bonding Fe-Si powder, enhancing powder flowbility and
The effect of compact strength, the additive amount total amount of passivator are no more than the 2% of mixed-powder gross mass.
6. the powder extruding method for making of high silicon steel thin belt material as described in claim 1, it is characterised in that:Step (4) is described
Support plate use molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the powder extruding method for making of high silicon steel thin belt material as described in claim 1, it is characterised in that:Step (6) is described
High temperature sintering when, overlapping place sintering plate, interlayer be laid with MgO powder, plate tiling place, on plate place tablet weight
Object prevents from deforming in sintering process.
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