CN108080640A - A kind of method that hot isostatic pressing prepares Fe-6.5%Si thin strips with high temperature sintering - Google Patents
A kind of method that hot isostatic pressing prepares Fe-6.5%Si thin strips with high temperature sintering Download PDFInfo
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
-
- B22F1/0003—
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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
- 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
-
- 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
Abstract
A kind of method that hot isostatic pressing prepares Fe 6.5%Si thin strips with high temperature sintering, the present invention chooses reduction Fe powder and water atomization Fe powder, according to 4:6~6:4 ratio mixing, then with Fe 70~80%Si HIGH-PURITY SILICON iron powders, formed Fe Si mixed powders.It is uniformly mixed after adding bonding agent and dispersant, using soft iron jacket, 1060~1160 DEG C, 100~200MPa hot isostatic pressings obtain even compact green compact, by the high Si phase compositions of the α Fe crystal grain and brittleness of poor Si, with plastic deformation ability, green density reaches 6.73~7.06g/cm3.It is sintered through multiple cold rolling, low temperature diffusion, density rise, thickness reduction, last 1260~1330 DEG C of sintering realize alloying under thermal diffusion effect, obtain 0.1~0.5mm thickness 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 hot isostatic pressure of high silicon steel thin belt material
With the method for 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 is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction contains with Si
Amount increases and reduces, and disappears substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases with Si contents and is increased,
At about 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent in higher frequency operation
Low 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 are oozed a diffusion annealing method, powder metallurgic method, microalloying and are changed
The various methods such as property.
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 business
Be developed with the CVD production lines that can realize continuous siliconising, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is：Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and to alloy diffusion inside alloy is finally made to reach required content by raised furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
It asks, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", and technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just generate huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of Powder hot isostatic pressures and High temperature diffusion sintering to prepare Fe-6.5%Si thin strips
Method, for Fe-4.5~6.7%Si alloy thin bands material difficult the problem of shaping, with industrial Fe powder with Si contents 70~
80% HIGH-PURITY SILICON iron powder mixing, using hot isostatic pressing hot mastication effect and pressure it is uniform the characteristics of, prepare high density
Uniformity slab, and realize partially-alloyed under thermal diffusion effect, form the α-Fe crystal grain of poor Si and the high Si phases group of brittleness
Into heterogeneous structure, have plastic deformation ability.Subsequently by multi-pass cold rolling-sintering, further it is thinned, finally using high temperature
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 70~80% 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 using soft iron jacket, in 1060~1160 DEG C of temperature ranges, under the hot isostatic pressing effect of 100~200MPa, obtain equal
Even, fine and close green compact.Green density reaches 6.73~7.06g/cm3.Under the heat effect of hot isostatic pressing and pressure effect, Fe
Powder particles obtain metallurgical binding, and incomplete diffusion has occurred in Si elements, formed it is fine and close, there is plastic deformation ability
The heterogeneous structure of the high Si phases of α-Fe crystal grain and brittleness of poor Si.Subsequently through multiple cold rolling, low temperature diffusion be sintered, slab it is close
Degree rise, plate thickness are reduced, and the alloying level of Si is also continuously improved.Finally in 1260~1330 DEG C of temperature ranges vacuum or
Protection of reducing atmosphere is sintered, and the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, is obtained containing 4.5~6.7%Si
0.1~0.5mm is thick, density >=7.34g/cm3High silicon steel band.
The method specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in 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 the Si contents of refining, grain size≤10 μm, this ferrosilicon powder is except containing for 70~80% HIGH-PURITY SILICON iron powder
Beyond 70~80%Si, major impurity is~0.25%Al ,~0.08%Ca and~0.02%C, remaining is Fe.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to
Fine silica powder, also being mutually twisted for powder easy to implement and improve the intensity of green compact.Water atomization Fe powder is also a kind of widely used
Industrial iron powder, has subsphaeroidal pattern, and impurity content has higher compressibility and mobility, water mist less than reduction Fe powder
It is favourable to the soft magnetic characteristic of high silicon steel to change impurity content low in Fe powder.It 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-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, it is single-phase to form homogeneous Fe-4.5~6.7%Si
Alloy.Meanwhile 20~30%Fe present in powder can effectively reduce the degree of oxidation of Si, be conducive to improve high silicon steel
Product quality.
By Fe-70~80%Si high purity ferrosilicons Mechanical Crushing to grain size≤10 μm, be conducive to it and be adhered to industrial Fe powder
Surface, tiny Si, FeSi2The mutually Dispersed precipitate in blank plays the role of the Strengthening and Toughening of structure refinement, is conducive to improve follow-up
Blank toughness, do not easily cause cracking in densification process is rolled.But in Fe-70~80%Si high purity ferrosilicons there are still compared with
More Si phases, Si are easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2Film, thus it is high-purity in Fe-70~80%Si
Inert gas should be used in the preparation of ferrosilicon powder, storage and transfer process and in follow-up batch mixing, hot isostatic pressing, the operation of rolling
Protection, 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, industrial Fe powder and Fe-70~80%Si HIGH-PURITY SILICON iron powders are weighed, lazy
Property protective atmosphere under be sufficiently mixed uniformly.
(3) Powder hot isostatic pressure：
Using soft iron jacket, in 1060~1160 DEG C of temperature ranges, under the hot isostatic pressing effect of 100~200MPa, protect
The pressure time is 0.5~2h, obtains green compact uniformly, fine and close, and green density reaches 6.73~7.06g/cm3。
(4) cold rolling-sintering
It by above-mentioned hot isostatic pressing plate cold rolling-sintering, is progressively thinned, single pass rolling reduction≤8%, through multi- pass rolling to always
After reduction ratio reaches 30~50%, then in 1060~1160 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 is increased to 7.33~7.44g/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, 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
It repairs and a degree of Si elements homogenization is spread.Cold rolling reduction accumulation needs to be sintered 1 again to a certain extent afterwards
It is secondary, 0.1~0.5mm is rolled down to from 36~54mm hot isostatic pressing plates, takes around and is sintered 12~20 times again.
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 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 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) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1330 DEG C of temperature ranges, in the effect of thermal diffusion
Under, it realizes the full alloyings of Si, forms single-phase alloy, obtain the high silicon steel of homogeneous, the thickness of plate is almost unchanged after densification sintering,
For 0.1~0.5mm, density is increased to 7.34~7.46g/cm3。
Iron powder per ton adds in 200~500ml absolute ethyl alcohols in mixed process described in step (1).
The HIGH-PURITY SILICON iron powder of grain size≤10 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；Hot isostatic pressing base
The three point bending test of material shows plasticity, and bending strength reaches 280~498MPa.
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 0.4% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays passivation Si powder, bonding Fe-
The effect of 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 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 fine Fe- in the industrial Fe powder of the big volumetric portion with good plasticity
70~80%Si HIGH-PURITY SILICON iron powders, form Fe-4.5~6.7%Si mixed powders.High density, Gao Jun are obtained by hot isostatic pressing
It is even.Incomplete alloying occurs under the heat effect of hot isostatic pressing, obtains one kind by plasticity Fe crystal grain and the high Si phases group of brittleness
Into composite material.Subsequently through multi-pass cold rolling and sintering, structural homogenity and compactness are improved, then is burnt by High temperature diffusion
Knot realizes the homogenization of Si, so as to obtain the single-phase high silicon steel band of high quality.This method is real by technique and equipment Design
Existing Technics Process Automation, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.34g/cm3High silicon steel
Band.
Description of the drawings
Fig. 1 be the embodiment of the present invention 1 Powder hot isostatic pressure after blank three-point bending graph；
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.
Specific 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 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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-80%Si high-purity powders of granularity≤10 μm according to 91.625:
8.375 ratio mixing forms the mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.3% is added during mixing,
0.1% machine oil.Absolute ethyl alcohol is added according to 200ml/ tons of amount.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1060 DEG C of temperature ranges, heat of 200MPa etc. is quiet
Under pressure effect, dwell time 0.5h obtains green 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 6.73g/cm3.Three point bending test test bending strength reaches
280MPa is shown in Fig. 1, and shows plasticity.
By above-mentioned hot isostatic pressing 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 is sintered through 13 cold rollings and 12 times.
For multi-pass cold rolling to after 30~50%, then in 1060 DEG C of heat preservation sintering 2h in vacuum sintering furnace, plate is thick
Degree is thinned to 0.49mm, and density reaches 7.33g/cm3。
4h is sintered in 1260 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 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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-70%Si high-purity powders of granularity≤10 μm according to 93.57:6.42
Ratio mixing, form the mixed-powder of Fe-4.5%Si.The zinc stearate of addition raw material total amount 0.2% during mixing, 0.1%
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 1160 DEG C of temperature ranges, the hot isostatic pressing of 100MPa
Under effect, dwell time 2h obtains green 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 6.73~7.06g/cm3.Three point bending test test bending strength reaches
498MPa。
By above-mentioned hot isostatic pressing 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
With 19 sintering.
Multi-pass cold rolling is to after 30~50% total reductions, then is burnt in hydrogen shield sintering furnace in 1160 DEG C of heat preservations
0.5h is tied, sheet metal thickness is thinned to 0.10mm, and density reaches 7.44g/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 apparent 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 are low, have plastic deformation ability.
1h is sintered in 1330 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.1mm, density reaches
7.46g/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 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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-76%Si high-purity powders of granularity≤10 μm according to 91.45:8.55
Ratio mixing, form the mixed-powder of Fe-6.5%Si.The paraffin micro mist of addition raw material total amount 0.2% during mixing, 0.1%
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 hot isostatic pressing of 150MPa
Under effect, dwell time 1.5h obtains green compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into
The square of 46 × 150 × 150mm.Green density reaches 6.89g/cm3.Three point bending test test bending strength reaches
318MPa。
By above-mentioned hot isostatic pressing 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 is sintered 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 heat preservations
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 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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the Fe-72%Si high-purity powders of granularity≤10 μm according to 91.05:8.95
Ratio mixing, form the mixed-powder of Fe-5.8%Si.The paraffin micro mist of addition raw material total amount 0.6% during mixing, 0.2%
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 hot isostatic pressing of 150MPa
Under effect, dwell time 1h obtains green compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into 52
The square of × 240 × 240mm.Green density reaches 6.99g/cm3.Three point bending test test bending strength reaches 381MPa.
By above-mentioned hot isostatic pressing 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.It is 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 heat preservations
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 final plate is shown in Fig. 4, are the high silicon steel of single-phase homogeneous.
Claims (8)
1. a kind of method that hot isostatic pressing prepares Fe-6.5%Si thin strips with high temperature sintering, it is characterised in that including following mistake
Journey：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in Fe powder is reduced, remaining is Si, Mn, P, S and other are inevitably miscellaneous
Matter, using -100 mesh water-atomized iron powders, Fe >=99.0% in water atomization Fe powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, will reduction Fe powder and water atomization Fe powder according to 4:6~6:4 ratio is prepared, using conical mixer, V-arrangement batch mixer
Or drum mixer is mixed to form technical pure Fe powder basic materials, incorporation time is 2~6h；
Si contents are used as 70~80% HIGH-PURITY SILICON iron powder, grain size≤10 μm, major impurity is~0.25%Al ,~0.08%
Ca and~0.02%C, remaining is Fe；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, Fe powder and Fe-70~80%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 1060~1160 DEG C of temperature ranges, under the hot isostatic pressing effect of 100~200MPa, during pressurize
Between for 0.5~2h, obtain green compact uniformly, fine and close, green density reaches 6.73~7.06g/cm3；
(4) cold rolling-sintering
It is progressively thinned, single pass rolling reduction≤8%, above-mentioned hot isostatic pressing plate cold rolling-sintering through under multi- pass rolling to stagnation pressure
After rate reaches 30~50%, then in 1060~1160 DEG C of 0.5~2h of heat preservation sintering, after multiple cold rolling-sintering, plate in sintering furnace
The thickness of material reaches 0.1~0.5mm, and after the completion of Si alloyings, strip density is increased to 7.33~7.44g/cm3；
(5) full alloying high temperature sintering
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1330 DEG C of temperature ranges, it is real under the action of thermal diffusion
The 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 is increased to 7.34~7.46g/cm3。
2. the method that hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, feature exist
In：Iron powder per ton adds 200~500ml absolute ethyl alcohols in mixed process.
3. the method that hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, feature exist
In：The HIGH-PURITY SILICON iron powder of grain size≤10 μm described in step (1) is by high-energy ball milling or rushes the acquisition of rotation method.
4. the method that hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, feature exist
In：The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
5. the method that hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, 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 hot isostatic pressing blank
Point bend test shows plasticity, and bending strength is 280~498MP.
6. the method that hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, 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 0.4% 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 hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, 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 hot isostatic pressing as described in claim 1 prepares Fe-6.5%Si thin strips with high temperature sintering, 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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