CN108057884A - A kind of method that High temperature diffusion sintering prepares high silicon steel band with powder rolling - Google Patents
A kind of method that High temperature diffusion sintering prepares high silicon steel band with powder rolling Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 100
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- 239000011863 silicon-based powder Substances 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 15
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- 238000009692 water atomization Methods 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 88
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—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
-
- 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
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1021—Removal of binder or filler
-
- 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
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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)
- Soft Magnetic Materials (AREA)
Abstract
A kind of method that High temperature diffusion sintering prepares high silicon steel band with powder rolling, the present invention chooses reduction Fe powder and water atomization Fe powder, according to 4:6~6:4 ratio mixing, then Si powder is added, form Fe 4.5~6.7%Si mixed powders.Porous slab is formed by powder rolling; slab is carried out to vacuum or protection of reducing atmosphere sintering at 1060~1160 DEG C; Fe powder particles is made to realize not exclusively connection; and Si and Fe realizes partially-alloyed, the high silicon steel blank of the porous incomplete alloying of formation, through multiple cold rolling, not exclusively sintering; finally it is sintered in 1260~1320 DEG C of vacuum or protection of reducing atmosphere; it realizes the homogeneous alloy of high silicon steel, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, 7.32~7.48g/cm of density3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to functional metal material, and in particular to the powder smelting of high silicon steel thin belt material
Gold sintering and 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 method for preparing high silicon steel band with powder rolling is sintered the object of the present invention is to provide a kind of High temperature diffusion, for
The problem of Fe-Si alloy thin band materials of 4.5~6.7%Si contents are difficult to shape, with technical pure Fe powder and fine simple substance Si powder
For raw material, formed after adding binder with compressibility powder mixture, then certain thickness is prepared using powder rolling method
Slab, degreasing, sintering after form porous, heterogeneous blank, obtain thin plate after multi-pass cold rolling-sintering, finally
It is sintered using High temperature diffusion and obtains the high silicon steel band of homogeneous.
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 adds fine Si powder as raw material powder, shape
Into Fe-4.5~6.7%Si mixed powders.Fine Si powder is adhered in mixed process by suitable bonding agent, dispersant
Into the hole of iron powder surface or filling ferrous powder.Since technical pure Fe powder is the big particle with high-compressibility, in mixed powder
In occupy larger volume ratio, do not significantly reduce its deformability after adding Si powder, can porous plate be formed by powder rolling
Base.Powder rolling slab is subjected to vacuum or protection of reducing atmosphere sintering in 1060~1160 DEG C of temperature ranges, makes Fe powder particles
Realize not exclusively connection, and Si and Fe realizations are partially-alloyed, form the height of incomplete alloying that is porous, having compressibility
Silicon steel blank.Subsequently through multiple cold rolling, not exclusively sintering, the density rise of slab, plate thickness are reduced, the alloying level of Si
Also it is continuously improved.Finally vacuum or protection of reducing atmosphere sintering in 1260~1320 DEG C of temperature ranges, in the help of thermal diffusion
The lower homogeneous alloy for realizing high silicon steel obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, 7.32~7.48g/ of density
cm3High silicon steel band.
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.
With the simple substance Si powder of grain size≤3 μm, purity is more than 97%, mainly containing Fe, Al and Ca 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 rolling also being mutually twisted for powder easy to implement and improve the intensity of green compact, be conducive to
The stabilization of powder rolling process.Water atomization Fe powder is also a kind of widely used Industrial iron powder, has subsphaeroidal pattern, and impurity contains
Amount has higher compressibility and mobility, is conducive to the uniform flow of powder rolling process course powder less than reduction Fe powder
Dynamic, low impurity content is favourable to the soft magnetic characteristic of high silicon steel in water atomization Fe powder.It will two kinds of reduction Fe powder and water atomization Fe powder
Industrial iron powder, according to 4:6~6:4 ratio mixing, forms technical pure Fe powder basic materials, is conducive to play two kinds of straight iron powders
Respective advantage is also relatively common method in industrial production iron-base part.
The property of simple substance Si is very crisp, it is easy to be refined by Mechanical Crushing technique.The elemental silicon for choosing grain size≤3 μm 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, cracking is not easily caused in densification process is rolled.
But Si is easily absorbing oxygen, and SiO is formed on powder surface2Film, therefore in the preparation, storage and transfer process of Si powder, with
And inert gas shielding should be used in follow-up batch mixing, the operation of rolling, used instrument must also take in advance dehydration, it is dry at
Reason.
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, pre- mixed Fe powder and Si powder are weighed；It is used under inert protective atmosphere
Low energy mixer mixes, and mixing velocity and time, the mitigation Fe powder that should try one's best was sent out in mixed process depending on mixing uniformity
Raw processing hardening.
(3) powder rolling
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
Thickness is rolled out as 1.0~2.5mm, width is 100~240mm, and density is 5.9~6.4g/cm3Powder strip plate.
Go out the difference in roller direction by band, powder rolling can be divided into vertical, horizontal and tilt 3 kinds of forms, and feeding manner has
Dead weight feeding, forced feed, pre-glued feeding etc..The width of blank is related with the width of feeding trough, and the length of blank regards production
Depending on condition is permitted and is actually needed.
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace,
2h~4h is kept the temperature respectively using the heating rate of 2~5 DEG C/min, and in 200 DEG C, 400 DEG C, then will heat up to 1060~1160
DEG C 2~4h of heat preservation sintering, sintered blank density are 6.0~6.5g/cm3。
Sintering temperature is too low, the connection and the diffusion of Si being unfavorable between Fe powder particles, and sintering temperature is excessively high then can be due to
, there is coarse hole in the diffusion into the surface of Fe, Si element, is subsequently difficult to press, and rolling densification is difficult to realize.
During sintering can powder rolling blank can be placed with multilayer, but must separate between layers, to avoid plate during sintering
Base contraction causes to crack.Heating rate should not be too fast during sintering, and multistage heat preservation can be set in temperature-rise period, to realize degassing, take off
The effect of fat.Reproducibility or inert gas shielding degreasing, sintering can also be taken.W, Mo, heat resisting steel etc. may be employed during sintering
As support plate (or burn boat), the ceramic wafers such as corundum, zirconium oxide can also be used, but metallic plate thermal conductivity it is good and beneficial to uniformly
Sintering shrinkage.
By 2 cold rollings-sintered metallographic structure.Matrix is about 100 μm of grain structure, there is a small amount of tiny hole
Gap.Uniformly tiny porous organization is formed after sintering.X-ray diffraction Discriminating materials be heterogeneous Fe (Si) phase, body-centered cubic
Several characteristic peaks have apparent separating phenomenon, illustrate there are 2 kinds of different Fe phases of Si solid solubility, wherein must have a kind of Fe phases
In Si contents it is low, have plastic deformation ability.
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, in sintering furnace, 0.5~2h is re-sintered in 1060~1160 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
To 0.1~0.5mm, density reaches 7.31~7.47g/cm3。
Since powder batch is porous organization, and there are deformable Fe phases, slab can bear cold-rolling deformation.Palette
There is also more high Si phases in base, performance is more crisp, therefore not above 8%, accumulation total reduction reaches amount under every time rolling
8~20 passages are taken around to 30~45%.
Since there are a large amount of holes and hard crisp phase, it is necessary to take and keep the temperature vacuum-sintering again at 1060 DEG C~1160 DEG C or go back
Originality protective atmosphere is sintered, to realize the reparation of the closing of pores and crackle and the homogenization diffusion of a degree of Si elements.
Heating rate can be very fast at this time, in 5~10 DEG C/min, can continuous warming, soaking time determines depending on thickness of slab, during thickness of slab >=1mm,
Soaking time is 1~2h；Thickness of slab is reduced to 0.5~1h in 0.1~1mm, soaking time.Sintered accumulation drafts reaches every time
, it is necessary to be sintered 1 time again after to 30~45%, 0.1~0.5mm is rolled down to from the powder base of 1.0~2.5mm, is taken around again
Sintering 4~8 times.In addition, in order to which the density of plate is made to reach 7.2g/cm3More than (about the 95% of theoretical density), it is also desirable to 4
Secondary above re-sinters.
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1320 DEG C of temperature ranges, in the effect of thermal diffusion
Under, it realizes the homogenization 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 7.32~7.48g/cm3。
The absolute ethyl alcohol of 200~500ml is added in step (1) mixed process according to mixed-powder per ton.
With high-energy ball milling or rush rotation method obtain grain size≤3 μm simple substance Si powder.
Low energy mixer described in step (2) is conical mixer, V-arrangement batch mixer or drum mixer.
Step (2) adds that cellulose, paraffin micro mist or zinc stearate are water-insoluble as binder, and binder adds when mixing
Dosage total amount is no more than the 0.8% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays passivation Si
Powder, bonding Fe-Si powder, the effect for enhancing powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed powder
The 2% of last gross mass.
Step (5) is sintered when re-sintering for 1060~1160 DEG C under vacuum-sintering or restitutive protection's atmosphere, by 5~
10 DEG C/min continuous warmings, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab is reduced to 0.5 in 0.1~1mm, soaking time
~1h after sintered accumulation drafts reaches 30~45% every time, is sintered 1 time, is rolled from the powder base of 1.0~2.5mm again
To 0.1~0.5mm, it is necessary to be sintered 4~8 times again.
Placement sintering plate can be overlapped during high temperature sintering, but interlayer must be laid with MgO powder, and W, Mo can be used and ceramics are burnt
Boat.But plate must tile placement, and tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of elements such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel
Large effect can subsequently be annealed by wet hydrogen, the technological means such as normalizing treatment are controlled by.
Essence of the invention is a small amount of by being with the addition of in the technical pure Fe powder of the big volumetric portion with good plasticity
The fine Si powder of simple substance, forms Fe-4.5~6.7%Si alloy mixtures, and powder rolling is into carrying out incomplete alloying after slab
Sintering makes Fe powder particles realization not exclusively sintering, and Si and Fe realizations are partially-alloyed, formed porous, with compressibility
The high silicon steel blank of incomplete alloying.Subsequently through multi-pass cold rolling and sintering, structural homogenity and compactness are improved, then is led to
High-temperature diffusion process is crossed, realizes the homogenization of Si, so as to obtain the single-phase high silicon steel band of complete alloying.This method passes through work
Skill and equipment Design realize Technics Process Automation, continuous production, and can be mass-produced 0.1~0.5mm thickness, density 7.32
~7.48g/cm3High silicon steel band.
Description of the drawings
Fig. 1 is metallographic structure after the powder rolling base of the embodiment of the present invention 2 is sintered；
Fig. 2 is XRD diffraction curves after the powder rolling base of the embodiment of the present invention 2 is sintered；
Fig. 3 is XRD diffraction curves after the powder rolling base 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 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 simple substance Si powder of grain size≤3 μm according to 93.3:6.7 ratio mixing, shape
Into the mixed-powder of Fe-6.7%Si.The paraffin micro mist of raw material total amount 0.6%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol
It is added according to 200ml/ tons of amounts.Using V-arrangement batch mixer by above-mentioned powder mixing 4h.
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
The powder rolling slab of 2.5mm is rolled out, the width of slab is 100mm.The density of green compact is 5.9g/cm3。
Powder strip plate is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts
With the heating rate of 2 DEG C/min, and 4h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1060 DEG C of heat preservation sintering 4h.It burns
It is 6.0g/cm to tie base density3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in vacuum sintering furnace, in 1060 DEG C of heat preservation sinterings.With 5 DEG C/min speed continuous warmings, soaking time regards plate
Thickness determines, during thickness of slab >=1mm, soaking time 2h；Thickness of slab is in 0.1~1mm, soaking time 1h.Specific pressure-annealing schedule
For：2.5mm → 1.6mm → 1.02mm → 0.71mm → 0.49mm, i.e., after 4 cold rollings and 3 sintering, the thickness of plate reaches
To 0.49mm, density reaches 7.31g/cm3。
For above-mentioned cold rolling made-up belt in 1320 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.32g/cm to obtain thickness3, Si
Content is the 6.7% high silicon steel of single-phase homogeneous.
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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the simple substance Si powder of grain size≤3 μm according to 95.5:4.5 ratio mixing, shape
Into the mixed-powder of Fe-4.5%Si.The zinc stearate of raw material total amount 0.7%, 0.1% machine oil are added during mixing.Absolute ethyl alcohol
It is added according to 400ml/ tons of amounts.Using drum mixer by above-mentioned powder mixing 6h.
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
The powder rolling slab of 1.0mm is rolled out, the width of slab is 240mm.The density of green compact is 6.4g/cm3。
Powder strip plate is placed on surface to be coated on the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.It adopts
With the heating rate of 5 DEG C/min, and 2h is kept the temperature respectively in 200 DEG C, 400 DEG C.Then will heat up to 1160 DEG C of heat preservation sintering 2h.It burns
It is 6.5g/cm to tie base density3.Uniformly tiny porous organization is formed after sintering, sees Fig. 1.X-ray diffraction Discriminating materials are non-
Homogeneous Fe (Si) phase, as seen in Figure 2, body-centred cubic several characteristic peaks have apparent separating phenomenon, illustrate that there are Si solid solubility
2 kinds of different Fe phases, wherein must have, the Si contents in a kind of Fe phases are low, have plastic deformation ability.
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in vacuum sintering furnace, in 1160 DEG C of heat preservation sinterings.With 10 DEG C/min speed continuous warmings, soaking time is
1h.Specifically pressure-annealing schedule is：1.0mm→0.65mm→0.39mm→ 0.25mm→0.17mm→0.13mm→
0.10mm, i.e., after 6 cold rollings and 5 sintering, the thickness of plate reaches 0.10mm, and density reaches 7.47g/cm3。
For above-mentioned cold rolling made-up belt in 1260 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.48g/cm to obtain thickness3, Si
Content is the 4.5% high silicon steel of single-phase homogeneous.
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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the simple substance Si powder of grain size≤3 μm according to 93.5:6.5 ratio mixing, shape
Into the mixed-powder of Fe-6.5%Si.The paraffin micro mist of addition raw material total amount 0.4% during mixing, 0.2% methylcellulose,
0.1% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Using drum mixer by above-mentioned powder mixing 6h.
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
The powder rolling slab of 1.6mm is rolled out, the width of slab is 180mm.The density of green compact is 6.0g/cm3。
Powder strip plate is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the heating rate of 3 DEG C/min, and 2h, 400 DEG C of heat preservation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1120 DEG C of heat preservations and burn
Tie 3h.Sintered blank density is 6.06g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in hydrogen tube furnace, in 1120 DEG C of heat preservation sintering 1h.With 6 DEG C/min speed continuous warmings.Specific pressure-
Annealing schedule is：1.6mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 4 cold rollings and 3 sintering, plate
Thickness reach 0.27mm, density reaches 7.32g/cm3。
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.33g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous.
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
Ethyl alcohol.
By well pre-mixed technical pure Fe powder and the simple substance Si powder of grain size≤3 μm according to 94.2:5.8 ratio mixing, shape
Into the mixed-powder of Fe-5.8%Si.The paraffin micro mist of raw material total amount 0.6%, 0.2% machine oil are added during mixing.Absolute ethyl alcohol
It is added according to 400ml/ tons of amounts.Using drum mixer by above-mentioned powder mixing 3h.
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder,
The powder rolling slab of 1.96mm is rolled out, the width of slab is 200mm.The density of green compact is 6.2g/cm3。
Powder strip plate is placed on surface to be coated on the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the heating rate of 4 DEG C/min, and 3h, 400 DEG C of heat preservation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1120 DEG C of heat preservations and burn
Tie 2h.Sintered blank density is 6.26g/cm3。
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8% reaches 30 through multi- pass rolling to total reduction
After~45%, then in hydrogen tube furnace, in 1120 DEG C of heat preservation sintering 0.5h.With 8 DEG C/min speed continuous warmings.Specific pressure
Under-annealing schedule is：1.96mm → 1.3mm → 0.96mm → 0.72mm → 0.46mm → 0.32mm → 0.21mm, i.e., through 7 times
After cold rolling and 6 sintering, the thickness of plate reaches 0.21mm, and density reaches 7.35g/cm3。
For above-mentioned cold rolling made-up belt in 1310 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.36g/cm to obtain thickness3, Si
Content is 5.8%, and the XRD analysis figure of final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.
Claims (8)
1. a kind of method that High temperature diffusion sintering prepares high silicon steel band with powder rolling, it is characterised in that comprise 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 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；With the simple substance Si of grain size≤3 μm
Powder, purity is more than 97%, mainly containing Fe, Al and Ca impurity；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, pre- mixed Fe powder and Si powder are weighed；Low energy is used under inert protective atmosphere
Measure mixer mixing；
(3) powder rolling
Using two roller horizontal mills and feeding trough is tilted, is conducted oneself with dignity using powder, the frictional force feeding between roll and powder, rolled
Go out thickness for 1.0~2.5mm, width is 100~240mm, and density is 5.9~6.4g/cm3Powder strip plate；
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated in the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2
The heating rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, it then will heat up to 1060~1160 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density are 6.0~6.5g/cm3；
(5) cold rolling-sintering densification
By above-mentioned sintering slab rolled thickness reduction, single pass rolling reduction≤8%, reach 30 through multi- pass rolling to total reduction~
After 45%, in sintering furnace, 0.5~2h is re-sintered in 1060~1160 DEG C, after multiple cold rolling-sintering, the thickness of plate reaches
0.1~0.5mm, density reach 7.31~7.47g/cm3；
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1320 DEG C of temperature ranges, it is real under the action of thermal diffusion
The homogenization of existing Si forms single-phase alloy, obtains the high silicon steel of homogeneous, and the thickness of plate is 0.1~0.5mm after densification sintering,
Density reaches 7.32~7.48g/cm3。
2. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
The absolute ethyl alcohol of 200~500ml is added in step (1) mixed process according to mixed-powder per ton.
3. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
With high-energy ball milling or rush rotation method obtain grain size≤3 μm simple substance Si powder.
4. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
Low energy mixer described in step (2) is conical mixer, V-arrangement batch mixer or drum mixer.
5. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
It is water-insoluble as binder, the additive amount total amount of binder that step (2) adds cellulose, paraffin micro mist or zinc stearate when mixing
It no more than the 0.8% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays passivation Si powder, bonding Fe-
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%.
6. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
Step (5) is sintered, by 5~10 DEG C/min when re-sintering for 1060~1160 DEG C under vacuum-sintering or restitutive protection's atmosphere
Continuous warming, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab is in 0.1~1mm, and soaking time is reduced to 0.5~1h, often
After secondary sintered accumulation drafts reaches 30~45%, it is sintered 1 time again, 0.1 is rolled down to from the powder base of 1.0~2.5mm~
0.5mm, it is necessary to be sintered 4~8 times again.
7. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
Overlapping places sintering plate during high temperature sintering, and interlayer is laid with MgO powder.
8. the method that High temperature diffusion sintering as described in claim 1 prepares high silicon steel band with powder rolling, it is characterised in that：
Support plate described in step (4) burns boat using W, Mo, corundum or zirconia ceramics.
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