CN107931612A - A kind of method that high temperature sintering prepares Fe 6.5%Si thin strips with high temperature insostatic pressing (HIP) - Google Patents
A kind of method that high temperature sintering prepares Fe 6.5%Si thin strips with high temperature insostatic pressing (HIP) Download PDFInfo
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- 229910006585 β-FeSi Inorganic materials 0.000 description 1
- 229910006578 β-FeSi2 Inorganic materials 0.000 description 1
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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
-
- 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
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A kind of method that high temperature sintering prepares Fe 6.5%Si thin strips with high temperature insostatic pressing (HIP), chooses reduction Fe powder and water atomization Fe powder, according to 4:6~6:4 ratio mixing, then the HIGH-PURITY SILICON iron powder that Si contents are 50~70% is added, form Fe Si mixed powders.Add bonding agent and dispersant is uniform, using soft iron jacket, in 1050~1150 DEG C, under the high temperature insostatic pressing (HIP) of 100~200MPa, the pressed compact of even compact is obtained, by the high Si phase compositions of the α Fe crystal grain and brittleness of poor Si, with plastic deformation ability, density is up to 6.78~7.02g/cm3.Sintered through multiple cold rolling, low temperature diffusion, density rise, thickness reduction, finally in 1250~1320 DEG C of sintering, alloying is realized under thermal diffusion effect, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.31g/cm3High silicon steel band.
Description
Technical field
The present invention principally falls into preparation and the manufacture field of metal material, and in particular to powder heat of high silicon steel thin belt material etc.
The method of static pressure and rolling deformation.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis curve is very narrow, it and fundamental magnetization curve are almost
Overlap, be mainly used for the iron core of inductance coil, transformer, relay and motor.Fe-Si alloys maximum permeability is sent out with Si contents
Changing, respectively Si mass percent it is (the same below) for 2% and 6.5% nearby there is the peak of two maximum permeabilities
Value, respectively reaches 10000 and 25000.The maximum permeability of Fe-Si alloys does not have absolute predominance, such as slope in soft magnetic materials
The maximum permeability of alloy can not reach 200000.But the Fe-Si lattens of Si ＜ 4.5% manufacture cost is low, therefore
Silicon steel sheet is also known as electrical sheet or silicon steel thin slice, is a kind of very important magnetic material.
And Si>When 4.5%, below 540 DEG C of temperature B can occur for Fe-Si alloys2The eutectoid decomposition reaction of ordered phase, it is raw
Into the unordered phases of α-Fe and DO3Ordered phase so that alloy becomes fragile and is difficult to deform.
For iron Si system alloy of the Si contents between 4.5~6.7%, commonly referred to as high silicon steel, wherein silicone content 6.5%
High silicon steel it is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction is with the increase of Si contents
And reduce, disappear substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increases with Si contents, about
When 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent low in higher frequency operation
Iron loss characteristic.
The transformer of normal operation can occur continuous uniform " drone " sound, this is because alternating current by transformer around
Group when, in the core between generate periodically variable alternating flux, cause iron core magnetostriction and shake the sound sent.Greatly
The sound that amount or large-scale iron core are sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is to play particularly important role in the military aviation such as spacecraft, submarine and guided missile field, Fe-Si systems alloy.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared on No. 11 airships of Apollo as transformer material, are completed the mankind and are landed on the moon first
Heroic undertaking.As it can be seen that high silicon steel is the environment-friendly type soft magnetic materials of a kind of consumption reduction of function admirable, noise reduction.
Compared to other alloys, the research and development process of high silicon steel is relatively very long.Late 1920s
A.Schulze studies discovery first, and the iron Si system alloy of silicone content 6.5% has the almost nil characteristic of magnetostriction coefficient.
In the 1980s, professor K.I.Arail etc. has found the high silicon steel alloy low compared to traditional Si content in exchange dynamic magnetic field
In there is the magnetic conductivity of lower iron loss and higher.Hereafter between many decades, in order to overcome the brittleness of high silicon steel, in technology of preparing side
There are many trials in face.As the special rolled method of jacket or temperature control, rapid solidification method, chemical vapour deposition technique (CVD method),
Plasma chemical vapor deposition (PCVD methods), hot dipping ooze a diffusion annealing method, powder metallurgic method, microalloying and are modified
Etc. various methods.
Wherein CVD is the successful example of comparison.NKK companies of Japan in 1988 have produced thickness for the first time using CVD technology
It is the No yield point 6.5%Si steel discs of 400mm to spend for 0.1~0.5mm, width.Phase early 1990s, global first commercialization
Can realize that the CVD production lines of continuous siliconising are developed, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is：Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and alloy is reached required content to alloy diffusion inside by elevated furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
Ask, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", its technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, its excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production, is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just produce huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of Powder hot isostatic pressure and High temperature diffusion sintering to prepare Fe-6.5%Si thin strips
Method, the problem of being difficult to shaping for Fe-4.5~6.7%Si alloy thin band materials, using technical pure Fe powder and Si contents as 50~
70% HIGH-PURITY SILICON iron powder is raw material, using high temperature insostatic pressing (HIP) hot mastication effect and pressure it is uniform the characteristics of, prepare highly dense
The uniformity slab of degree, and thermal diffusion effect under realize it is partially-alloyed, formed with plastic deformation ability poor Si α-
The heterogeneous structure of Fe crystal grain and the high Si phases of brittleness.Subsequently further it is thinned after multi-pass cold rolling-sintering, finally using high temperature
Diffusion-sintering obtains the high silicon steel band of homogeneous single phase.
The present invention is achieved by the following technical solutions：Reduction Fe powder and two kinds of Industrial iron powders of water atomization Fe powder are chosen,
According to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, then it is 50~70% to add fine Si contents
HIGH-PURITY SILICON iron powder is raw material, forms Fe-4.5~6.7%Si mixed powders.It is uniformly mixed after adding a small amount of bonding agent, dispersant,
Then soft iron jacket is used, in 1050~1150 DEG C of temperature ranges, under the high temperature insostatic pressing (HIP) effect of 100~200MPa, is obtained equal
Even, fine and close pressed compact.Green density reaches 6.78~7.02g/cm3.Under the heat effect of high temperature insostatic pressing (HIP) and pressure effect, Fe powder
Particle obtains metallurgical binding, and Si elements are there occurs incomplete diffusion, formed densification, have the plastic deformation ability poor
The heterogeneous structure of the high Si phases of α-Fe crystal grain and brittleness of Si.Sintered subsequently through multiple cold rolling, low temperature diffusion, the density liter of slab
High, plate thickness is reduced, and the alloying level of Si is also continuously improved.Finally vacuum or reduction in 1250~1320 DEG C of temperature ranges
Gas-protecting sintering, realizes the homogeneous alloy of high silicon steel with the help of thermal diffusion, obtain containing 4.5~6.7%Si 0.1~
0.5mm is thick, density >=7.31g/cm3High silicon steel band.
The method of the present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitable
Impurity, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining for Si, Mn, P, S and other can not
The impurity avoided, by reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, and is mixed using conical mixer, V-arrangement
Material machine or drum mixer are mixed to form technical pure Fe powder basic materials, and incorporation time is 2~6h.
Using Si contents, particle diameter≤6 μm, this ferrosilicon powder is except containing 50~70% for 50~70% HIGH-PURITY SILICON iron powder
Beyond Si, major impurity is~0.24%Al ,~0.07%Ca and~0.02%C, remaining is Fe.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to
Fine silica powder, also being mutually twisted for powder easy to implement and improve the intensity of pressed compact.Water atomization Fe powder is also a kind of widely used
Industrial iron powder, has subsphaeroidal pattern, impurity content is less than reduction Fe powder, compressibility and mobility with higher, water mist
It is favourable to the soft magnetic characteristic of high silicon steel to change impurity content low in Fe powder.Will reduction Fe powder and two kinds of irons of water atomization Fe powder
Powder, according to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, and it is respective excellent to be conducive to two kinds of straight iron powders of performance
Gesture, is also relatively common method in industrial production iron-base part.
Fe-50~70%Si high purity ferrosilicons in process of setting there are two eutectic reactions, when rich Si sides are at 1207 DEG C
Form the β-FeSi with tP3 structures2With Si phase eutectic structures, form when rich Fe sides are at 1212 DEG C and tied with tP3
β-the FeSi of structure2With the FeSi eutectic structures of cP8 structures；At 982 DEG C and 937 DEG C, also there are β-FeSi2Decomposition and oC48-
FeSi2Two solid-state phase changes processes of formation of phase.Therefore it is easy in process of setting of the Fe-50~70%Si after refining crisp
Change, form trickle Fe-Si or Si heterogeneous structures, it is easy to refine by Mechanical Crushing technique.Fe-50~70%Si is high-purity
Ferrosilicon is crushed to≤6 μm of ferrosilicon powder, the Si phases in its actual tissue, FeSi2, FeSi phases it is more tiny, be conducive to subsequent high temperature
The thermal diffusion homogenization of Si elements, forms homogeneous Fe-6.5%Si single-phase alloys during sintering.Meanwhile exist in high purity ferrosilicon powder
30~50%Fe can effectively reduce the degree of oxidation of Si, be conducive to improve the product quality of high silicon steel.
By Fe-50~70%Si high purity ferrosilicons Mechanical Crushing to particle diameter≤6 μm, be conducive to it and be adhered to technical pure Fe powder
Surface is filled in the hole of technical pure Fe powder, tiny Si, FeSi2, FeSi phases Dispersed precipitate in blank, play tissue
The Strengthening and Toughening effect of refinement, is conducive to improve follow-up blank toughness, cracking is not easily caused in densification process is rolled.But
Still contain a small amount of Si phases in Fe-50~70%Si high purity ferrosilicons, Si is easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2
Film, therefore in the preparation, storage and transfer process of Fe-50~70%Si HIGH-PURITY SILICON iron powders, and follow-up batch mixing, heat etc. are quiet
Inert gas shielding should be used in pressure, the operation of rolling, 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, 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, technical pure Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed,
It is sufficiently mixed under inert protective atmosphere uniformly.
(3) Powder hot isostatic pressure
Using soft iron jacket, in 1050~1150 DEG C of temperature ranges, under the high temperature insostatic pressing (HIP) effect of 100~200MPa, protect
The pressure time is 0.5~2h, obtains pressed compact uniformly, fine and close, and green density reaches 6.78~7.02g/cm3。
(4) cold rolling-sintering
By above-mentioned high temperature insostatic pressing (HIP) plate cold rolling-sintering, progressively it is thinned, single pass rolling reduction≤8%, through multi- pass rolling to always
After reduction ratio reaches 30~50%, then in 1050~1150 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering in sintering furnace
Afterwards, the thickness of plate reaches 0.1~0.5mm, and after the completion of Si alloyings, strip density brings up to 7.31~7.43g/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 high temperature insostatic pressing (HIP) 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 1250~1320 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 brings up to 7.31~7.43g/cm3。
Mixing iron powder per ton adds 200~500ml absolute ethyl alcohols in mixed process.
The HIGH-PURITY SILICON iron powder of particle diameter≤6 μm described in step (1) 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.
100~300mm of length and width is processed into step (3) and by blank, thickness is 36~54mm squares；High temperature insostatic pressing (HIP) base
The three point bending test of material shows plasticity, and bending strength reaches 282~480MPa.
It is water-insoluble total as binder, the additive amount of binder to add cellulose, paraffin micro mist or zinc stearate during mixing
0.5% of amount no more than mixed-powder gross mass, while add grease and absolute ethyl alcohol does passivator, play passivation Si powder, bonding
The effect of Fe-Si powder, enhancing powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed-powder gross mass
2%.
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 body in the technical pure Fe powder of the big volumetric portion with good plasticity
Fine Fe-50~70%Si HIGH-PURITY SILICONs iron powder of product ratio, forms Fe-4.5~6.7%Si mixed powders.Pass through high temperature insostatic pressing (HIP)
Obtain high density, height uniformly.Incomplete alloying occurs under the heat effect of high temperature insostatic pressing (HIP), obtains one kind by plasticity Fe crystal grain
With the composite material of the high Si phase compositions of brittleness.Subsequently through multi-pass cold rolling and sintering, structural homogenity and compactness are improved, then
Sintered by High temperature diffusion, realize the homogenization of Si, so as to obtain the single-phase high silicon steel band of high quality.This method passes through technique
And equipment Design, realize Technics Process Automation, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=
7.31g/cm3High silicon steel band.
Brief description of the drawings
Fig. 1 be the embodiment of the present invention 1 Powder hot isostatic pressure after blank three-point bending curve map；
Fig. 2 is metallographic structure figure after Powder hot isostatic pressure-cold rolling-sintering of the embodiment of the present invention 2；
Fig. 3 is XRD diffraction curve figures after Powder hot isostatic pressure-cold rolling-sintering of the embodiment of the present invention 2；
Fig. 4 is XRD diffraction curve figures after Powder hot isostatic pressure-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 water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 4:6 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 2h, is added in mixed process according to 200ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-70%Si high-purity powders of granularity≤6 μm according to 90.43:9.57
Ratio mixes, and forms the mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.4%, 0.1% machine are added during mixing
Oil.Absolute ethyl alcohol is added according to 200ml/ tons of amount.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1050 DEG C of temperature ranges, the high temperature insostatic pressing (HIP) of 200MPa
Under effect, dwell time 0.5h, obtains pressed compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into
The square of 36 × 100 × 100mm.Green density reaches 6.78g/cm3.Three point bending test test bending strength reaches
282MPa, is shown in Fig. 1, and shows plasticity.
By above-mentioned high temperature insostatic pressing (HIP) 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, i.e., sinter through 13 cold rollings and 12 times.
Multi-pass cold rolling is thick in 1050 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 7.31g/cm3。
4h is sintered in 1250 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches
7.31g/cm3, Si contents are 6.7%.
Embodiment 2
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 5:6 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 3h, is added in mixed process according to 400ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-50%Si high-purity powders of granularity≤10 μm according to 91:9 ratio is mixed
Close, form the mixed-powder of Fe-4.5%Si.The zinc stearate of raw material total amount 0.4%, 0.1% machine oil are added during mixing.Nothing
Water-ethanol is added according to 400ml/ tons of amount.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1150 DEG C of temperature ranges, the high temperature insostatic pressing (HIP) of 100MPa
Under effect, dwell time 2h, obtains pressed compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into 54
The square of × 300 × 300mm.Green density reaches 7.02g/cm3.Three point bending test test bending strength reaches 480MPa.
By above-mentioned high temperature insostatic pressing (HIP) 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., through 20 cold rollings and
19 sintering.
Multi-pass cold rolling is to after 30~50% total reductions, then is burnt in hydrogen shield sintering furnace in 1150 DEG C of insulations
0.5h is tied, sheet metal thickness is thinned to 0.10mm, and density reaches 7.43g/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.
1h is sintered in 1320 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches
7.43g/cm3, Si contents are 4.5%.
Embodiment 3
By the water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 6:4 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 4h, is added in mixed process according to 500ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-60%Si high-purity powders of granularity≤6 μm according to 89.17:10.83
Ratio mixes, and forms the mixed-powder of Fe-6.5%Si.The paraffin micro mist of raw material total amount 0.2%, 0.2% first are added during mixing
Base cellulose, 0.05% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1120 DEG C of temperature ranges, the high temperature insostatic pressing (HIP) of 160MPa
Under effect, dwell time 1.2h, obtains pressed compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into
The square of 46 × 160 × 160mm.Green density reaches 6.98g/cm3.Three point bending test test bending strength reaches
328MPa。
By above-mentioned high temperature insostatic pressing (HIP) 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 7.37g/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 water atomization Fe powder of the reduction Fe powder of -100 mesh and -100 mesh according to 5:5 ratio is prepared, and is mixed using drum-type
Material machine is mixed to form technical pure Fe powder raw materials, incorporation time 6h, is added in mixed process according to 500ml/ tons of ratio anhydrous
Ethanol.
By well pre-mixed technical pure Fe powder and the Fe-62%Si high-purity powders of granularity≤10 μm according to 90.64:9.36
Ratio mixes, and forms the mixed-powder of Fe-5.8%Si.The paraffin micro mist of addition raw material total amount 0.3% during mixing, 0.02%
Machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1120 DEG C of temperature ranges, the high temperature insostatic pressing (HIP) of 120MPa
Under effect, dwell time 1.6h, obtains pressed compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into
The square of 52 × 250 × 250mm.Green density reaches 6.92g/cm3.Three point bending test test bending strength reaches
382MPa。
By above-mentioned high temperature insostatic pressing (HIP) 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 7.39g/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 7.40g/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 (8)
1. a kind of method that high temperature sintering prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), it is characterised in that including following step
Suddenly：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitably miscellaneous
Matter, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, will reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, using conical mixer, V-arrangement batch mixer
Or drum mixer is mixed to form technical pure Fe powder basic materials, incorporation time is 2~6h；
Si contents are used as 50~70% HIGH-PURITY SILICON iron powder, particle diameter≤6 μm, major impurity is~0.24%Al ,~0.07%
Ca and~0.02%C, remaining is Fe；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed, gas is protected in inertia
It is sufficiently mixed under atmosphere uniformly；
(3) Powder hot isostatic pressure
Using soft iron jacket, in 1050~1150 DEG C of temperature ranges, under the high temperature insostatic pressing (HIP) effect of 100~200MPa, during pressurize
Between be 0.5~2h, obtain pressed compact uniformly, fine and close, green density reaches 6.78~7.02g/cm3；
(4) cold rolling-sintering
Progressively it is thinned, single pass rolling reduction≤8%, above-mentioned high temperature insostatic pressing (HIP) plate cold rolling-sintering through under multi- pass rolling to stagnation pressure
After rate reaches 30~50%, then in sintering furnace after 1050~1150 DEG C of 0.5~2h of heat preservation sintering, multiple cold rolling-sintering, plate
The thickness of material reaches 0.1~0.5mm, and after the completion of Si alloyings, strip density brings up to 7.31~7.43g/cm3；
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1250~1320 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 almost unchanged after densification sintering, is 0.1
~0.5mm, density bring up to 7.31~7.43g/cm3。
2. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：Iron powder per ton adds 200~500ml absolute ethyl alcohols in mixed process.
3. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：The HIGH-PURITY SILICON iron powder of particle diameter≤6 μm described in step (1) is by high-energy ball milling or rushes the acquisition of rotation method.
4. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
5. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：100~300mm of length and width is processed into step (3) and by blank, thickness is 36~54mm squares；The three of high temperature insostatic pressing (HIP) blank
Point bend test shows plasticity, and bending strength is 282~480MPa.
6. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：Add cellulose, paraffin micro mist or zinc stearate water-insoluble binder during mixing, the additive amount total amount of binder, which is no more than, mixes
The 0.3% 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.
7. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：Support plate described in step (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
8. the method that high temperature sintering as claimed in claim 1 prepares Fe-6.5%Si thin strips with high temperature insostatic pressing (HIP), its feature exist
In：During high temperature sintering described in step (6), overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed, in plate
Upper placement tablet weight, prevents from deforming in sintering process.
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