CN108103390A - A kind of method that Powder hot isostatic pressure prepares single-phase Fe-6.5%Si silicon steel - Google Patents
A kind of method that Powder hot isostatic pressure prepares single-phase Fe-6.5%Si silicon steel Download PDFInfo
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- CN108103390A CN108103390A CN201711368390.8A CN201711368390A CN108103390A CN 108103390 A CN108103390 A CN 108103390A CN 201711368390 A CN201711368390 A CN 201711368390A CN 108103390 A CN108103390 A CN 108103390A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
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- 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
-
- 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 Powder hot isostatic pressure prepares single-phase Fe 6.5%Si silicon steel, for the present invention using reduction Fe powder, Si powder is raw material, forms Fe Si mixed powders.It adds bonding agent and dispersant is uniform, then soft iron jacket is used, in 1080~1180 DEG C of temperature ranges, under the hot isostatic pressing effect of 100~200MPa, obtain the green compact of even compact, by the high Si phase compositions of the α Fe crystal grain and brittleness of poor Si, there is plastic deformation ability, green density reaches 6.72~7.04g/cm3.It is sintered by multiple cold rolling, low temperature diffusion, density rise, thickness are reduced；It is finally sintered in 1280~1350 DEG C of temperature ranges, the homogeneous alloy of high silicon steel is realized with the help of thermal diffusion, obtain 0.1~0.5mm thickness containing 4.5~6.7%Si, density >=7.29g/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 it is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction increases with Si contents
And reduce, it disappears substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases with Si contents and is increased, about
When 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent low in higher frequency operation
Iron loss characteristic.
The transformer of normal operation can occur continuous uniform " drone " sound, this is because alternating current by transformer around
Group when, in the core between generate periodically variable alternating flux, cause iron core magnetostriction and shake the sound sent.Greatly
The sound that the iron core of amount or large size is sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is in the military aviations such as spacecraft, submarine and guided missile field, Fe-Si systems alloy plays particularly important role.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared in as transformer material on No. 11 airships of Apollo, are completed the mankind and are landed on the moon for the first time
Heroic undertaking.As it can be seen that high silicon steel is the environment-friendly type soft magnetic materials of a kind of consumption reduction of function admirable, noise reduction.
Compared to other alloys, the research and development process of high silicon steel is relatively very long.Late 1920s
A.Schulze is for the first time the study found that the iron Si system alloy of silicone content 6.5% has the almost nil characteristic of magnetostriction coefficient.
In the 1980s, professor K.I.Arail etc. has found the high silicon steel alloy low compared to traditional Si content in exchange dynamic magnetic field
In have lower iron loss and higher magnetic conductivity.Hereafter between many decades, in order to overcome the brittleness of high silicon steel, in technology of preparing side
There are many trials in face.As the special rolled method of jacket or temperature control, rapid solidification method, chemical vapour deposition technique (CVD method),
Plasma chemical vapor deposition (PCVD methods), hot dipping ooze a diffusion annealing method, powder metallurgic method, microalloying and are modified
Etc. various methods.
Wherein CVD is the successful example of comparison.NKK companies of Japan in 1988 have produced thickness for the first time using CVD technology
It spends for 0.1~0.5mm, width is the No yield point 6.5%Si steel discs of 400mm.Phase early 1990s, global first commercialization
Can realize that the CVD production lines of continuous siliconising are developed, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is：Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and to alloy diffusion inside alloy is finally made to reach required content by raised furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
It asks, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", and technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just generate huge economic benefit and social benefit.
The content of the invention
A kind of method that Powder hot isostatic pressure prepares single-phase Fe-6.5%Si silicon steel, for Fe-4.5~6.7%Si alloys
The problem of thin strip is difficult to shape uniformly is mixed with reducing Fe powder with fine simple substance Si powder, soft using the high temperature of hot isostatic pressing
The characteristics of change effect and uniform pressure, prepares highdensity uniformity slab, and realizes alloy part under thermal diffusion effect
Change, being formed has the α-Fe crystal grain of poor Si of plastic deformation ability and the heterogeneous structure of the high Si phases of brittleness.Subsequently pass through multi-pass
It is further thinned after cold rolling-sintering, 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
Raw material powder forms Fe-4.5~6.7%Si mixed powders.It is uniformly mixed after adding a small amount of bonding agent, dispersant, then uses
Soft iron jacket in 1080~1180 DEG C of temperature ranges, under the hot isostatic pressing effect of 100~200MPa, obtains uniform, densification
Green compact, green density reach 6.72~7.04g/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 forms α-Fe that are fine and close, having plastic deformation ability poor Si
The heterogeneous structure of crystal grain and the high Si phases of brittleness.It is sintered subsequently through multiple cold rolling, low temperature diffusion, the density rise of slab, thickness of slab
Degree is reduced, and the alloying level of Si is also continuously improved.Finally vacuum or reducing atmosphere are protected in 1280~1350 DEG C of temperature ranges
Shield sintering realizes the homogeneous alloy of high silicon steel with the help of thermal diffusion, obtains 0.1~0.5mm containing 4.5~6.7%Si
Thickness, density >=7.29g/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 reduced iron powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, with the simple substance Si of grain size≤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 hot isostatic pressure also being mutually twisted for powder easy to implement and improve the intensity of green compact.
The property of simple substance Si is very crisp, it is easy to be refined by Mechanical Crushing technique.The elemental silicon for choosing 3 μm of grain size ＜ 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 subsequent blank toughness, does not easily cause cracking in densification process.But Si
Oxygen is easily absorbing, SiO is formed on powder surface2Film, therefore in the preparation, storage and transfer process of Si powder, Yi Jihou
Inert gas shielding should be used during continuous batch mixing, heating, Powder hot isostatic pressure, used instrument must also be taken de- in advance
Water, 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, in the process
The possibility for introducing other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Si powder are weighed, is sufficiently mixed under inert protective atmosphere
Uniformly.
(3) Powder hot isostatic pressure
Using soft iron jacket, in 1080~1180 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 6.72~7.04g/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 1080~1180 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 7.27~7.40g/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.
Used sintering range is the sintering process of current powder metallurgical ferrous alloy, has obtained extensive reality
Trample verification.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 can
Si elements is 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 1280~1350 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 reaches 7.29~7.43g/cm3。
The simple substance silica flour of grain size≤3 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.
Blank is processed into 100~300mm of length and width in step (3), thickness is 36~54mm squares；Hot isostatic pressing blank
Three point bending test show plasticity, bending strength is 106~196MPa.
Add cellulose, paraffin micro mist or zinc stearate water-insoluble binder during mixing, the additive amount total amount of binder is not
It more than the 0.8% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays passivation Si powder, bonding Fe-Si
The effect of powder, enhancing powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed-powder gross mass
2%.
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 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 mixed powders.High density, height are obtained uniformly by hot isostatic pressing.
Occur incomplete alloying under the heat effect of hot isostatic pressing, obtain a kind of by plasticity Fe crystal grain and the high Si phase compositions of brittleness
Composite material.Subsequently through multi-pass cold rolling and sintering, structural homogenity and compactness are improved, then is sintered by High temperature diffusion,
The homogenization of Si is realized, so as to obtain the single-phase high silicon steel band of high quality.This method realizes work by technique and equipment Design
Skill process automation, continuous production, can be mass-produced 0.1~0.5mm thickness, density >=7.29g/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 reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤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 0.3%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol according to
200ml/ tons of amount addition.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1080 DEG C of temperature ranges, the hot isostatic pressing of 200MPa
Under effect, dwell time 0.5h obtains green compact uniformly, fine and close.Jacket is removed with machine-tooled method, and blank is processed into
36 × 100 × 100mm squares.Green density reaches 6.72g/cm3.Three point bending test test bending strength reaches 430MPa,
See Fig. 1, show 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 1080 DEG C of heat preservation sintering 2h in vacuum sintering furnace, plate is thick
Degree is thinned to 0.49mm, and density reaches 7.29g/cm3。
4h is sintered in 1280 DEG C of Temperature Vacuums, realizes the full alloyings of Si, forms single-phase alloy, thickness 0.5mm, density reaches
7.29g/cm3, Si contents are 6.7%.
Embodiment 2
By the reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤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 0.2%, 0.5% machine oil are added during mixing.Absolute ethyl alcohol according to
400ml/ tons of amount addition.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1180 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 7.04g/cm3.Three point bending test test bending strength reaches 869MPa.
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 and
19 sintering.
Multi-pass cold rolling is to after 30~50% total reductions, then is burnt in hydrogen shield sintering furnace in 1180 DEG C of heat preservations
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 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 1350 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 reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤3 μm according to 93.5:6.5 ratio mixing, forms Fe-
The mixed-powder of 6.5%Si.The methylcellulose of raw material total amount 0.2%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol is pressed
It is added according to 400ml/ tons of amounts.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1150 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 × 200 × 200mm.Green density reaches 6.85g/cm3.Three point bending test test bending strength reaches
458MPa。
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 reduction Fe powder of -100 mesh and the simple substance Si powder of grain size≤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 0.3%, 0.02% machine oil are added during mixing.Absolute ethyl alcohol according to
400ml/ tons of amount addition.
After above-mentioned powder is sufficiently mixed, using soft iron jacket, in 1120 DEG C of temperature ranges, the hot isostatic pressing of 120MPa
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 52 × 180 × 180mm.Green density reaches 6.93g/cm3.Three point bending test test bending strength reaches
540MPa。
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 7.38g/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 7.39g/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 (7)
1. a kind of method that Powder hot isostatic pressure 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 of grain size≤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, is sufficiently mixed under inert protective atmosphere
It is even；
(3) Powder hot isostatic pressure
Using soft iron jacket, in 1080~1180 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 6.72~7.04g/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 1080~1180 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 7.27~7.40g/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 almost unchanged after densification sintering, is 0.1
~0.5mm, density reach 7.29~7.43g/cm3。
2. the method that Powder hot isostatic pressure as is described in the claims prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：
The simple substance silica flour of grain size≤3 μm described in step (1) is by high-energy ball milling or rushes the acquisition of rotation method.
3. the method that Powder hot isostatic pressure as is described in the claims prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：
The low energy mixer is conical mixer, V-arrangement batch mixer or drum mixer.
4. the method that Powder hot isostatic pressure as is described in the claims prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：
100~300mm of length and width is processed into step (3) and by blank, thickness is 36~54mm squares；3 points of hot isostatic pressing blank
Bend test shows plasticity, and bending strength is 106~196MPa.
5. the method that Powder hot isostatic pressure as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：It is mixed
Add cellulose, paraffin micro mist or zinc stearate water-insoluble binder during conjunction, the additive amount total amount of binder is no more than mixed powder
The 0.3% of last gross mass, while add grease and absolute ethyl alcohol does passivator, play passivation Si powder, bonding Fe-Si powder, enhancing powder
The effect of last mobility 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 hot isostatic pressure as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：Step
Suddenly the support plate described in (4) uses molybdenum plate, W plates, heat resisting steel, corundum or zirconia ceramics plate.
7. the method that Powder hot isostatic pressure as described in claim 1 prepares single-phase Fe-6.5%Si silicon steel, it is characterised in that：Step
Suddenly during high temperature sintering described in (6), overlapping places sintering plate, and interlayer is laid with MgO powder, and plate tiling is placed, put on plate
Horizontalization plate weight prevents from deforming in sintering process.
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| CN (1) | CN108103390A (en) |
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| CN109849385A (en) * | 2018-12-20 | 2019-06-07 | 赣州海盛硬质合金有限公司 | A method of increasing slab and is densified in pressing process |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109849385A (en) * | 2018-12-20 | 2019-06-07 | 赣州海盛硬质合金有限公司 | A method of increasing slab and is densified in pressing process |
| CN114686745A (en) * | 2022-01-05 | 2022-07-01 | 中南大学 | Powder metallurgy modified low-alloy ultrahigh-strength steel and preparation method thereof |
| CN114686745B (en) * | 2022-01-05 | 2022-11-01 | 中南大学 | Powder metallurgy modified low-alloy ultrahigh-strength steel and preparation method thereof |
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