CN107900348A - A kind of method that powder hotforging prepares single-phase Fe 6.5%Si silicon steel - Google Patents
A kind of method that powder hotforging prepares single-phase Fe 6.5%Si silicon steel Download PDFInfo
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- CN107900348A CN107900348A CN201711367240.5A CN201711367240A CN107900348A CN 107900348 A CN107900348 A CN 107900348A CN 201711367240 A CN201711367240 A CN 201711367240A CN 107900348 A CN107900348 A CN 107900348A
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- 229910017133 Fe—Si Inorganic materials 0.000 claims description 8
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- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
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- 229910000859 α-Fe Inorganic materials 0.000 description 3
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
- B22F2003/175—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging by hot forging, below sintering temperature
-
- 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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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
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- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of method that powder hotforging prepares single-phase Fe 6.5%Si silicon steel, the present invention uses reduction Fe powder and fine Si powder as raw material, form Fe Si mixed powders, Si powder is adhered in the hole of reduced iron powder surface or filling ferrous powder by bonding agent and dispersant, squarely base is molded again, it is heated to 1020~1090 DEG C and realizes Fe phase austenitizings, final forging temperature is 920~990 DEG C after multiple hot forging, and density is up to 6.78~7.10g/cm3.Powder hotforging base is subjected to vacuum or protection of reducing atmosphere sintering in 1080~1180 DEG C of temperature ranges; by multiple cold rolling, low-temperature sintering, finally sintered in 1280~1350 DEG C of High temperature diffusions, realize homogeneous alloy; it is thick to obtain 0.1~0.5mm containing 4.5~6.7%Si, density >=7.34g/cm3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder hotforging of high silicon steel thin belt material and roll
The method for making deformation.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis curve is very narrow, it and fundamental magnetization curve are almost
Overlap, be mainly used for the iron core of inductance coil, transformer, relay and motor.Fe-Si alloys maximum permeability is sent out with Si contents
Changing, respectively Si mass percent it is (the same below) for 2% and 6.5% nearby there is the peak of two maximum permeabilities
Value, respectively reaches 10000 and 25000.The maximum permeability of Fe-Si alloys does not have absolute predominance, such as slope in soft magnetic materials
The maximum permeability of alloy can not reach 200000.But the Fe-Si lattens of Si < 4.5% manufacture cost is low, therefore
Silicon steel sheet is also known as electrical sheet or silicon steel thin slice, is a kind of very important magnetic material.
And Si>When 4.5%, below 540 DEG C of temperature B can occur for Fe-Si alloys2The eutectoid decomposition reaction of ordered phase, it is raw
Into the unordered phases of α-Fe and DO3Ordered phase so that alloy becomes fragile and is difficult to deform.
For iron Si system alloy of the Si contents between 4.5~6.7%, commonly referred to as high silicon steel, wherein silicone content 6.5%
High silicon steel it is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction is with the increase of Si contents
And reduce, disappear substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increases with Si contents, about
When 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent low in higher frequency operation
Iron loss characteristic.
The transformer of normal operation can occur continuous uniform " drone " sound, this is because alternating current by transformer around
Group when, in the core between generate periodically variable alternating flux, cause iron core magnetostriction and shake the sound sent.Greatly
The sound that amount or large-scale iron core are sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is to play particularly important role in the military aviation such as spacecraft, submarine and guided missile field, Fe-Si systems alloy.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared on No. 11 airships of Apollo as transformer material, are completed the mankind and are landed on the moon first
Heroic undertaking.As it can be seen that high silicon steel is the environment-friendly type soft magnetic materials of a kind of consumption reduction of function admirable, noise reduction.
Compared to other alloys, the research and development process of high silicon steel is relatively very long.Late 1920s
A.Schulze studies discovery first, and the iron Si system alloy of silicone content 6.5% has the almost nil characteristic of magnetostriction coefficient.
In the 1980s, professor K.I.Arail etc. has found the high silicon steel alloy low compared to traditional Si content in exchange dynamic magnetic field
In there is the magnetic conductivity of lower iron loss and higher.Hereafter between many decades, in order to overcome the brittleness of high silicon steel, in technology of preparing side
There are many trials in face.As the special rolled method of jacket or temperature control, rapid solidification method, chemical vapour deposition technique (CVD method),
Plasma chemical vapor deposition (PCVD methods), hot dipping ooze a diffusion annealing method, powder metallurgic method, microalloying and are modified
Etc. various methods.
Wherein CVD is the successful example of comparison.NKK companies of Japan in 1988 have produced thickness for the first time using CVD technology
It is the No yield point 6.5%Si steel discs of 400mm to spend for 0.1~0.5mm, width.Phase early 1990s, global first commercialization
Can realize that the CVD production lines of continuous siliconising are developed, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is:Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and alloy is reached required content to alloy diffusion inside by elevated furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
Ask, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", its technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, its excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production, is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just produce huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of method that powder hotforging prepares single-phase Fe-6.5%Si silicon steel, for Fe-4.5
~6.7%Si alloy thin band materials are difficult to the problem of shaping, are uniformly mixed with fine simple substance Si powder with reducing Fe powder, addition shaping
Hot forging green compact are molded into after agent, then certain thickness slab is prepared using powder hotforging method, big using powder hotforging becomes
Shape act on so that green density improve, structure refinement, and thermal diffusion effect under realize it is partially-alloyed, formed have plasticity become
The heterogeneous structure of the high Si phases of α-Fe crystal grain and brittleness of the poor Si of shape ability.Subsequently 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 single phase.
The present invention is achieved by the following technical solutions:Using the reduction Fe powder of irregular pattern, fine Si powder is
Material powder, forms Fe-4.5~6.7%Si mixed powders.By suitable bonding agent, dispersant by fine Si powder mixed
Adhered to during conjunction in the hole of reduced iron powder surface or filling ferrous powder.Since reduction Fe powder is with the thick of high-compressibility
Particle, occupies larger volume ratio in mixed powder, does not significantly reduce its plastic deformation ability after adding Si powder, can pass through mould
It is pressed into square base.It is heated to 1020~1090 DEG C and realizes Fe phase austenitizings, then place into closed mould hot forging, repeatedly forging
Rear final forging temperature is made as 910~980 DEG C so that pressed compact is about 6.78~7.10g/cm close to full densification3.Then by powder heat
Forging stock carries out vacuum or protection of reducing atmosphere sintering in 1080~1180 DEG C of temperature ranges, makes Fe powder particles metallurgical bindings, and Si
Realized with Fe it is partially-alloyed, formed densification, with the poor Si of plastic deformation ability α-Fe crystal grain and the high Si phases of brittleness it is more
The high silicon steel blank of phase constitution.Sintered subsequently through multiple cold rolling, low temperature diffusion, the density rise of slab, plate thickness are reduced, Si's
Alloying level is also continuously improved.Finally vacuum or protection of reducing atmosphere sintering in 1280~1350 DEG C of temperature ranges, in heat
The homogeneous alloy of high silicon steel is realized with the help of diffusion, 0.1~0.5mm of the acquisition containing 4.5~6.7%Si is thick, density >=
7.34g/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 Si, Mn, P, S and other are inevitable
Impurity, with the simple substance Si powder of particle diameter≤3 μm, purity is more than 97%, mainly containing Fe, Al, Ca and other inevitable impurity.
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 hotforging also being mutually twisted for powder easy to implement and improve the intensity of pressed compact.
The property of simple substance Si is very crisp, it is easy to is refined by Mechanical Crushing technique.The elemental silicon for choosing 3 μm of particle diameter < is favourable
In the realization of subsequently homogenization diffusion-sintering;And hole that tiny Si is formed in blank, brittle interface are also tiny, play
The Strengthening and Toughening effect of structure refinement, is conducive to improve follow-up blank toughness, is not easily caused in extruding, rolling densification process
Cracking.But Si is easily absorbing oxygen, SiO is formed on powder surface2Film, therefore in the preparation, storage and transfer process of Si powder
In, and inert gas shielding should be used during follow-up batch mixing, heating, powder hotforging, used instrument also must be in advance
Take dehydration, drying process.
On the premise of oxygen content is controlled, influence of the impurity such as other Al, Ca, Mn to alloy magnetic property is little, during
The possibility for introducing other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and simple substance Si powder are weighed;Used under inert protective atmosphere
Low energy mixer mixes, and mixing velocity and time, the mitigation Fe powder that should try one's best was sent out in mixed process depending on mixing uniformity
Raw processing hardening.
(3) powder hotforging
Square pressed compact is prepared using compression-moulding methods, the green density of acquisition is 6.35~6.52g/cm3;Before hot forging
Molding square billet is heated to 1020~1090 DEG C under nitrogen protective effect, keeps the temperature 2~4h, hot forging is fine and close in square dies
Change, repeatedly final forging temperature is 920~990 DEG C after forging, and pressed compact is close complete fine and close, and density reaches 6.78~7.10g/cm3。
Under impact force action, hot forging pressed compact is close complete fine and close.Make the plasticity of plate after hot forging in order to avoid alloying
Decline, relatively low heating-up temperature is have selected before hot forging.Fe phase and complexity FeSi phase composition of the alloy structure for high-ductility after hot forging
Complex tissue, which possesses the high-ductility characteristic of simple substance Fe.
(4) cold rolling-sintering
By above-mentioned hot forged plate cold rolling-sintering, progressively it is thinned.
Single pass rolling reduction≤8%, after multi- pass rolling reaches 30~50% to total reduction, then in sintering furnace in
1080~1180 DEG C of 0.5~2h of heat preservation sintering, after multiple cold rolling-sintering, the thickness of plate reaches 0.1~0.5mm, with Si's
Alloying is gradually completing, and strip density improves, and reaches 7.32~7.45g/cm3。
There are a large amount of deformable Fe phases in blank, slab can bear cold-rolling deformation.But there is also more in slab
High Si phases, its performance is more crisp, therefore amount cannot be too high under every time rolling, and accumulation total reduction reaches 30~50%, takes around 8
~25 passages.
Since existing hard crisp phase, cold deformation process can form some micro-cracks.In order to realize the closing of pores and crackle
Repair, and the homogenization diffusion of a degree of Si elements.Cold rolling reduction accumulation needs to sinter 1 again to a certain extent afterwards
It is secondary, 0.1~0.5mm is rolled down to from 36~54mm hot forging plates, takes around and sinters 12~20 times again.
Sintering temperature is too low, is unfavorable for metallurgical binding and the Si element thermal diffusions of Fe powder particles;And sintering temperature is excessive 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 or vacuum-sintering.W, Mo, heat resisting steel etc. can be used during sintering as support
Plate (or burning boat), can also use the ceramic wafers such as corundum, zirconium oxide, but metallic plate thermal conductivity is good, and be 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 obvious separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, wherein must
There are the Si contents in a kind of Fe phases low, there is plastic deformation ability.
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, in the effect of thermal diffusion
Under, to realize the full alloyings 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 reaches 7.34~7.48g/cm3。
The HIGH-PURITY SILICON iron powder of particle diameter≤10 μm is by 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.
The square pressed compact prepared in step (3), length and width are respectively 100~300mm, are highly 40~60mm, using table
The pressure that surface pressure is 400~600MPa is suppressed.The thickness of blank is 36~54mm after hot forging, and three point bending test shows to mould
Property, bending strength reaches 126~210MPa.
Step (2) adds cellulose, paraffin micro mist when mixing or zinc stearate is water-insoluble adds as binder, binder
Dosage total amount is no 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 powder, the effect for strengthening powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed powder
The 2% of last gross mass.
Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
During high temperature sintering described in step (6), overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed,
Tablet weight is placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of element such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel
Large effect, can subsequently be annealed, the technological means such as normalizing treatment is controlled by by wet hydrogen.
Essence of the invention is by with the addition of certain volume in the reduction Fe powder of the big volumetric portion with good plasticity
The fine Si powder of simple substance of ratio, forms Fe-4.5~6.7%Si alloys basis powder.Using powder hotforging into slab, obtain high
Green density.Since hot forging is organized as incomplete alloying tissue, in tissue in addition to small part richness Si phases, main constituent
For yielding Fe phases, therefore subsequently structural homogenity and compactness, then high temperature can be improved by multi-pass cold rolling and sintering
Diffusion technique, realizes the homogenization of Si, so as to obtain the single-phase high silicon steel band of high quality.This method is set by technique and equipment
Meter, realizes Technics Process Automation, continuous production, and can be mass-produced 0.1~0.5mm thickness, density >=7.34g/cm3Height
Silicon steel band.
Brief description of the drawings
Fig. 1 be the embodiment of the present invention 1 powder hotforging after blank three-point bending curve map;
Fig. 2 is metallographic structure figure after powder hotforging-cold rolling-sintering of the embodiment of the present invention 2;
Fig. 3 is XRD diffraction curve figures after powder hotforging-cold rolling-sintering of the embodiment of the present invention 2;
Fig. 4 is XRD diffraction curve figures after powder hotforging-cold rolling-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 reduction Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 93.3:6.7 ratio mixing, forms Fe-
The mixed-powder of 6.7%Si.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol according to
200ml/ tons of amount addition.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Square pressed compact is prepared using compression-moulding methods, and pressed compact size is 100 × 100 × 40mm, surface pressing
600MPa, green density 6.35g/cm3。
Molding square billet is heated to 1020 DEG C under nitrogen protective effect, keeps the temperature 4h.Using power forging machine, in square dies
Middle hot forging densification, repeatedly final forging temperature is 920 DEG C after forging, and the thickness of blank is about 36mm, and density reaches 6.78g/cm3。
Three point bending test shows plasticity, sees Fig. 1, and bending strength reaches 126MPa.
By above-mentioned hot forged plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is:36mm→24mm→17mm→
12mm → 9.5mm → 7.2mm → 5mm → 3.5mm → 2.4mm → 1.6mm → 1.02mm → 1.02mm → 0.71mm → 0.49mm,
Sintered through 13 cold rollings and 12 times.
Multi-pass cold rolling is thick in 1080 DEG C of heat preservation sintering 2h, plate to after 30~50%, then in vacuum sintering furnace
Degree is thinned to 0.49mm, and density reaches 7.32g/cm3。
1h is sintered in 1350 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches
7.34g/cm3, Si contents are 6.7%.
Embodiment 2
By the reduction Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 95.5:4.5 ratio mixing, forms Fe-
The mixed-powder of 4.5%Si.The zinc stearate of raw material total amount 0.7%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol according to
400ml/ tons of amount addition.Using drum mixer by above-mentioned powder mixing 6h.
Square pressed compact is prepared using compression-moulding methods, and pressed compact size is 300 × 300 × 60mm, surface pressing
600MPa, green density 6.52g/cm3。
Molding square billet is heated to 1090 DEG C under nitrogen protective effect, keeps the temperature 2h.Using power forging machine, in square dies
Middle hot forging densification, repeatedly final forging temperature is 990 DEG C after forging, and the thickness of blank is about 54mm, and density reaches 7.10g/cm3。
Three point bending test shows plasticity, and bending strength reaches 210MPa.
By above-mentioned hot forged plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is:54mm→36mm→36mm→
24mm→17mm→12mm→9.5mm→7.2mm→5mm→3.5mm→2.4mm→1.6mm→1.02mm→1.02mm→
0.71mm → 0.49mm → 0.39mm → 0.25mm → 0.17mm → 0.13mm → 0.10mm, i.e., burn through 20 cold rollings and 19 times
Knot.
Multi-pass cold rolling is to after 30~50% total reductions, then is burnt in hydrogen shield sintering furnace in 1180 DEG C of insulations
0.5h is tied, sheet metal thickness is thinned to 0.10mm, and density reaches 7.45g/cm3。
The texture of coarse crystal containing the second phase is formed after sintering, sees Fig. 2.X-ray diffraction Discriminating materials are heterogeneous Fe
(Si) phase, as seen in Figure 3, body-centred cubic several characteristic peaks have obvious separating phenomenon, illustrate there are Si solid solubility it is different 2
Kind Fe phases, wherein must have the Si contents in a kind of Fe phases low, have plastic deformation ability.
4h is sintered in 1280 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches
7.48g/cm3, Si contents are 4.5%.
Embodiment 3
By the reduction Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 93.5:6.5 ratio mixing, forms Fe-
The mixed-powder of 6.5%Si.The paraffin micro mist of addition raw material total amount 0.4% during mixing, 0.2% methylcellulose, 0.1%
Machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder mixing 6h.
Square pressed compact is prepared using compression-moulding methods, and pressed compact size is 200 × 200 × 50mm, surface pressing
500MPa, green density 6.36g/cm3。
Molding square billet is heated to 1000 DEG C under nitrogen protective effect, keeps the temperature 2h.Using power forging machine, in square dies
Middle hot forging densification, repeatedly final forging temperature is 960 DEG C after forging, and the thickness of blank is about 46mm, and density reaches 6.82g/cm3。
Three point bending test shows plasticity, and bending strength reaches 140MPa.
By above-mentioned hot forged plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is:46mm→36mm→24mm→
17mm→12mm→9.5mm→7.2mm→5mm→3.5mm→2.4mm→1.6mm→1.02mm→1.02mm→0.71mm→
0.49mm → 0.39mm → 0.27mm, i.e., sinter through 16 cold rollings and 15 times.
Multi-pass cold rolling is to after 30~50% total deformations, then is burnt in nitrogen protective sintering stove in 1120 DEG C of insulations
1h is tied, sheet metal thickness is thinned to 0.27mm, and density reaches 7.36g/cm3。
2h is sintered in 1320 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.27mm, density reaches
To 7.38g/cm3, Si contents are 6.5%,
Embodiment 4
By the reduction Fe powder of -100 mesh and the simple substance Si powder of particle diameter≤3 μm according to 94.2:5.8 ratio mixing, forms Fe-
The mixed-powder of 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 according to
400ml/ tons of amount addition.Using drum mixer by above-mentioned powder mixing 3h.
Square pressed compact is prepared using compression-moulding methods, and pressed compact size is 220 × 220 × 55mm, surface pressing
450MPa, green density 6.40g/cm3。
Molding square billet is heated to 1020 DEG C under nitrogen protective effect, keeps the temperature 2h.Using power forging machine, in square dies
Middle hot forging densification, repeatedly final forging temperature is 980 DEG C after forging, and the thickness of blank is about 52mm, and density reaches 6.86g/cm3。
Three point bending test shows plasticity, and bending strength reaches 160MPa.
By above-mentioned hot forged plate cold rolling-sintering, progressively it is thinned.Specifically pressure-annealing schedule is:52mm→39mm→26mm→
18mm→13mm→10.5mm→8.2mm→5mm→3.2mm→2.4mm→2.0mm→1.3mm→0.90mm→0.63→
0.43mm→0.32mm→0.21mm.Sintered through 17 cold rollings and 16 times.
Multi-pass cold rolling is to after 30~50% total deformations, then is burnt in hydrogen shield sintering furnace in 1150 DEG C of insulations
1h is tied, sheet metal thickness is thinned to 0.21mm, and density reaches 7.40g/cm3。
2h is sintered in 1300 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.21mm, density reaches
To 7.41g/cm3, Si contents are 5.8%, and the XRD analysis figure of its final plate is shown in Fig. 4, is the high silicon steel of single-phase homogeneous.
Claims (7)
1. a kind of method that powder hotforging prepares single-phase Fe-6.5%Si silicon steel, 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, with the simple substance Si powder of particle diameter≤3 μm, purity is more than 97%, mainly containing Fe, Al, Ca and other inevitable impurity;
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Si powder are weighed;Mixed under inert protective atmosphere using low energy
Conjunction machine mixes;
(3) powder hotforging
Square pressed compact is prepared using compression-moulding methods, green density is 6.35~6.52g/cm3;Square billet will be molded before hot forging
1020~1090 DEG C are heated under nitrogen protective effect, keeps the temperature 2~4h, repeatedly final forging temperature is 920~990 DEG C after forging,
Pressed compact reaches 6.78~7.10g/cm close to full densification, density3;
(4) cold rolling-sintering
By above-mentioned hot forged plate cold rolling-sintering, progressively it is thinned, single pass rolling reduction≤8%, is reached through multi- pass rolling to total reduction
To after 30~50%, 0.5~2h is re-sintered in 1080~1180 DEG C in sintering furnace, after multiple cold rolling-sintering, the thickness of plate
Reach 0.1~0.5mm, strip density reaches 7.32~7.45g/cm3;
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1280~1350 DEG C of temperature ranges, it is real under the action of thermal diffusion
The existing full alloyings of Si, form single-phase alloy, obtain the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering,
Density reaches 7.34~7.48g/cm3。
2. the method that powder hotforging as claimed in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that:Particle diameter≤
3 μm of simple substance Si powder is by high-energy ball milling or rushes the acquisition of rotation method.
3. the method that powder hotforging as claimed in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that described
Low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the method that powder hotforging as claimed in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that:Step
(3) the square pressed compact prepared in, length and width are respectively 100~300mm, are highly 40~60mm, use surface pressing as 400
The pressure compacting of~600MPa;The thickness of blank is 36~54mm after hot forging, and three point bending test shows plasticity, bending strength
Reach 126~210MPa.
5. the method that powder hotforging as claimed in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that:Step
(2) cellulose, paraffin micro mist or zinc stearate water-insoluble binder are added when mixing, the additive amount total amount of binder, which is no more than, mixes
The 0.8% of powder gross mass is closed, while adds grease and absolute ethyl alcohol does passivator, passivation Si powder, bonding Fe-Si powder is played, increases
The effect of strong powder flowbility and compact strength, the additive amount total amount of passivator are no more than the 2% of mixed-powder gross mass.
6. the method that powder hotforging as claimed in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that:Step
(4) support plate described in uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the method that powder hotforging as claimed in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that:Step
(6) during high temperature sintering described in, overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed, placed on plate
Tablet weight, prevents from deforming in sintering process.
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