CN107900350A - A kind of method that powder rolling prepares high silicon steel thin belt material - Google Patents
A kind of method that powder rolling prepares high silicon steel thin belt material Download PDFInfo
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- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000009703 powder rolling Methods 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 88
- 238000005245 sintering Methods 0.000 claims abstract description 86
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 39
- 230000009467 reduction Effects 0.000 claims abstract description 32
- XWHPIFXRKKHEKR-UHFFFAOYSA-N iron silicon Chemical compound [Si].[Fe] XWHPIFXRKKHEKR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims description 18
- 238000005096 rolling process Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- 238000009792 diffusion process Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 11
- 229910017082 Fe-Si Inorganic materials 0.000 claims description 10
- 229910017133 Fe—Si Inorganic materials 0.000 claims description 10
- 238000005238 degreasing Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 7
- 238000000265 homogenisation Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000280 densification Methods 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 6
- 239000011230 binding agent Substances 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 239000010431 corundum Substances 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- 239000012188 paraffin wax Substances 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 238000009825 accumulation Methods 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 239000011863 silicon-based powder Substances 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 229920002678 cellulose Polymers 0.000 claims description 2
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- 238000002161 passivation Methods 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 230000002708 enhancing effect Effects 0.000 claims 1
- 239000000956 alloy Substances 0.000 abstract description 18
- 229910045601 alloy Inorganic materials 0.000 abstract description 17
- 238000005097 cold rolling Methods 0.000 abstract description 11
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- 238000005275 alloying Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 description 16
- 230000008569 process Effects 0.000 description 11
- 238000004321 preservation Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910000831 Steel Inorganic materials 0.000 description 5
- 238000000137 annealing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
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- 239000000696 magnetic material Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 229910005347 FeSi Inorganic materials 0.000 description 4
- 229910000519 Ferrosilicon Inorganic materials 0.000 description 4
- 239000010721 machine oil Substances 0.000 description 4
- 230000035699 permeability Effects 0.000 description 4
- 229910005331 FeSi2 Inorganic materials 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910000676 Si alloy Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
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- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000005389 magnetism Effects 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
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- 238000011049 filling Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
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- 230000005415 magnetization Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004801 process automation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- -1 using Si contents Substances 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
- 229910006585 β-FeSi Inorganic materials 0.000 description 1
- 229910006578 β-FeSi2 Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
A kind of method that powder rolling prepares high silicon steel thin belt material, for the present invention using reduction Fe powder, Si contents are the HIGH-PURITY SILICON iron powder of Fe 50~70%, form 4.5~6.7%Si mixed powders.Porous slab is formed by powder rolling; powder rolling slab is subjected to vacuum or protection of reducing atmosphere sintering in 1060~1160 DEG C of temperature ranges; Fe powder particles are made to realize not exclusively connection, and Si and Fe realizes partially-alloyed, the high silicon steel blank of the incomplete alloying of formation.Again by multiple cold rolling, not exclusively sintering, finally sintered in 1265~1335 DEG C of vacuum or protection of reducing atmosphere, realize the homogeneous alloy of high silicon steel, 0.1~0.5mm of the acquisition containing 4.5~6.7%Si is thick, 7.37~7.50g/cm of density3High silicon steel band.
Description
Technical field
Preparation and manufacture field the invention belongs to metal material, and in particular to the powder of the high silicon steel soft magnetism band of high-performance
The metallurgy sintered and method of rolling deformation.
Technical background
Remanent magnetism and coercive force all very littles of soft magnetic material, i.e. hysteresis curve is very narrow, it and fundamental magnetization curve are almost
Overlap, be mainly used for the iron core of inductance coil, transformer, relay and motor.Fe-Si alloys maximum permeability is sent out with Si contents
Changing, respectively Si mass percent it is (the same below) for 2% and 6.5% nearby there is the peak of two maximum permeabilities
Value, respectively reaches 10000 and 25000.The maximum permeability of Fe-Si alloys does not have absolute predominance, such as slope in soft magnetic materials
The maximum permeability of alloy can not reach 200000.But the Fe-Si lattens of Si ＜ 4.5% manufacture cost is low, therefore
Silicon steel sheet is also known as electrical sheet or silicon steel thin slice, is a kind of very important magnetic material.
And Si>When 4.5%, below 540 DEG C of temperature B can occur for Fe-Si alloys2The eutectoid decomposition reaction of ordered phase, it is raw
Into the unordered phases of α-Fe and DO3Ordered phase so that alloy becomes fragile and is difficult to deform.
For iron Si system alloy of the Si contents between 4.5~6.7%, commonly referred to as high silicon steel, wherein silicone content 6.5%
High silicon steel it is mostly important.Its reason is Fe-Si alloy grains edge<100>The magnetostriction coefficient in direction is with the increase of Si contents
And reduce, disappear substantially at about 6.3%, and<111>The magnetostriction coefficient in direction increases and increases with Si contents, about
When 6.1% with<100>The magnetostriction coefficient in direction is equal so that high silicon steel shows excellent low in higher frequency operation
Iron loss characteristic.
The transformer of normal operation can occur continuous uniform " drone " sound, this is because alternating current by transformer around
Group when, in the core between generate periodically variable alternating flux, cause iron core magnetostriction and shake the sound sent.Greatly
The sound that amount or large-scale iron core are sent in vibrations not only causes the loss of energy, also creates noise pollution.Especially
It is to play particularly important role in the military aviation such as spacecraft, submarine and guided missile field, Fe-Si systems alloy.20th century 60
Age Mo, the alloy of Si contents 6.5% are appeared on No. 11 airships of Apollo as transformer material, are completed the mankind and are landed on the moon first
Heroic undertaking.As it can be seen that high silicon steel is the environment-friendly type soft magnetic materials of a kind of consumption reduction of function admirable, noise reduction.
Compared to other alloys, the research and development process of high silicon steel is relatively very long.Late 1920s
A.Schulze studies discovery first, and the iron Si system alloy of silicone content 6.5% has the almost nil characteristic of magnetostriction coefficient.
In the 1980s, professor K.I.Arail etc. has found the high silicon steel alloy low compared to traditional Si content in exchange dynamic magnetic field
In there is the magnetic conductivity of lower iron loss and higher.Hereafter between many decades, in order to overcome the brittleness of high silicon steel, in technology of preparing side
There are many trials in face.As the special rolled method of jacket or temperature control, rapid solidification method, chemical vapour deposition technique (CVD method),
Plasma chemical vapor deposition (PCVD methods), hot dipping ooze a diffusion annealing method, powder metallurgic method, microalloying and are modified
Etc. various methods.
Wherein CVD is the successful example of comparison.NKK companies of Japan in 1988 have produced thickness for the first time using CVD technology
It is the No yield point 6.5%Si steel discs of 400mm to spend for 0.1~0.5mm, width.Phase early 1990s, global first commercialization
Can realize that the CVD production lines of continuous siliconising are developed, the product size of production can reach 0.1~0.3mm ×
600mm。
The principle of CVD is：Under specific temperature conditions, silicon-containing gas (SiCl4) can react generation Fe- with silicon strip
Si compounds, and alloy is reached required content to alloy diffusion inside by elevated furnace temperature.Although oneself uses this
Technology realizes small-scale industrialized production, but its scale and yield all can not much meet the need in international soft magnetic materials market
Ask, and this preparation method technical process is sufficiently complex, energy consumption and of high cost, operating environment and its severe, it is impossible to meet ring
Guaranteed request.
High silicon steel is " the steel art work ", its technology of preparing is all always and everywhere state-of-the-art steel and iron manufacturing technology, and
It is the hot spot of development and exploitation.For 6.5%Si high silicon steel, its excellent magnetic performance and wide application prospect are even more to inhale
Draw scientific worker and carry out substantial amounts of research-and-development activity.The development of preparation process and ripe and can be cost-effectively
Production, is that 6.5%Si high silicon steel move towards to be commercialized widely applied key, also the always emphasis of research work.Once grope
Go out simple, economic, effective, ripe preparation process, will just produce huge economic benefit and social benefit.
The content of the invention
The object of the present invention is to provide a kind of powder rolling manufacture method of high silicon steel thin belt material, for 4.5~6.7%Si
The Fe-Si alloy thin band materials of content are difficult to the problem of shaping, using reduced iron powder and Si contents as 50~70% HIGH-PURITY SILICON iron powder
For raw material, formation has compressibility powder mixture after adding binder, then prepares certain thickness using powder rolling method
Slab, degreasing, sintering after form porous, heterogeneous blank, obtain thin plate after multi-pass cold rolling-sintering, finally
Sintered using High temperature diffusion and obtain the high silicon steel band of homogeneous.
The present invention is achieved by the following technical solutions：Using the reduction Fe powder of irregular pattern, fine Si contents
For the HIGH-PURITY SILICON iron powder of Fe-50~70%, 4.5~6.7%Si mixed powders are formed.Be tod by suitable bonding agent, dispersant
Fine HIGH-PURITY SILICON iron powder is adhered in mixed process in the hole of reduced iron powder surface or filling ferrous powder.Due to reducing Fe powder
For the big particle with high-compressibility, larger volume ratio is occupied in mixed powder, add fine Si contents for 50~
Its deformability will not be significantly reduced after 70% HIGH-PURITY SILICON iron powder, porous slab can be formed by powder rolling.By powder
Rolled slab carries out vacuum or protection of reducing atmosphere sintering in 1060~1160 DEG C of temperature ranges, realizes Fe powder particles incomplete
Connection, and Si and Fe realizes partially-alloyed, the high silicon steel blank of porous, with compressibility the incomplete alloying of formation.
Subsequently through multiple cold rolling, not exclusively sintering, the density rise of slab, plate thickness are reduced, and the alloying level of Si also constantly carries
It is high.Finally vacuum or protection of reducing atmosphere sintering in 1265~1335 DEG C of temperature ranges, are realized high with the help of thermal diffusion
The homogeneous alloy of silicon steel, obtains 0.1~0.5mm thickness containing 4.5~6.7%Si, 7.37~7.50g/cm of density3High silicon steel
Band.
The method of the present invention specifically comprises the following steps：
(1) raw material powder prepares
Using -100 mesh reduced iron powders, Fe >=98.5% in reduced iron powder, remaining is Si, Mn, P, S and other are inevitable
Impurity, using Si contents, particle diameter≤6 μm, this ferrosilicon powder is except containing 50~70% for 50~70% HIGH-PURITY SILICON iron powder
Beyond Si, major impurity is~0.24%Al ,~0.07%Ca and~0.02%C, remaining is Fe.
Reduced iron powder is a kind of widely used Industrial iron powder, has irregular porous pattern, micro- beneficial to storing, adhering to
Thin and tall pure silicon iron powder, and during follow-up powder rolling also being mutually twisted for powder easy to implement and improve the intensity of pressed compact,
Be conducive to the stabilization of powder rolling process.
Fe-50~70%Si high purity ferrosilicons in process of setting there are two eutectic reactions, when rich Si sides are at 1207 DEG C
Form the β-FeSi with tP3 structures2With Si phase eutectic structures, form when rich Fe sides are at 1212 DEG C and tied with tP3
β-the FeSi of structure2With the FeSi eutectic structures of cP8 structures；At 982 DEG C and 937 DEG C, also there are β-FeSi2Decomposition and oC48-
FeSi2Two solid-state phase changes processes of formation of phase.Therefore it is easy in process of setting of the Fe-50~70%Si after refining crisp
Change, form trickle Fe-Si or Si heterogeneous structures, it is easy to refine by Mechanical Crushing technique.Fe-50~70%Si is high-purity
Ferrosilicon is crushed to≤6 μm of ferrosilicon powder, the Si phases in its actual tissue, FeSi2, FeSi phases it is more tiny, be conducive to subsequent high temperature
The thermal diffusion homogenization of Si elements, forms homogeneous Fe-6.5%Si single-phase alloys during sintering.Meanwhile exist in high purity ferrosilicon powder
30~50%Fe can effectively reduce the degree of oxidation of Si, be conducive to improve the product quality of high silicon steel.
By Fe-50~70%Si high purity ferrosilicons Mechanical Crushing to particle diameter≤6 μm, be conducive to it and be adhered to the table of reduction Fe powder
Face is filled in the hole of reduction Fe powder, tiny Si, FeSi2, FeSi phases Dispersed precipitate in blank, play structure refinement
Strengthening and Toughening effect, be conducive to improve follow-up blank toughness, cracking do not easily caused in densification process is rolled.But Fe-50
Still contain a small amount of Si phases in~70%Si high purity ferrosilicons, Si is easily absorbing oxygen, and SiO is formed in exposed Si phase surfaces2Film,
Therefore in the preparation, storage and transfer process of Fe-50~70%Si HIGH-PURITY SILICON iron powders, and in follow-up batch mixing, the operation of rolling
Inert gas shielding should be used, used instrument must also take dehydration, drying process in advance.
On the premise of oxygen content is controlled, influence of the impurity such as Al, Ca, Mn to alloy magnetic property is little, during introduce
The possibility of other alloying elements is also little.
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed；Lazy
Property protective atmosphere under using low energy mixer mix, mixing velocity and time regarding mixing uniformity depending on, should try one's best mitigation Fe
Processing hardening occurs in mixed process for powder.
(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,
It is 0.96~2.3mm to roll out thickness, and width is 100~240mm, and density is 6.2~6.7g/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 with the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace,
2h~4h is kept the temperature respectively using the programming 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 is 6.25~6.7g/cm3。
Uniform equiaxed grain structure is formed after sintering.Matrix grain is about 70~100 μm, and crystal boundary has hole about~10 μm
Gap, follow-up rolling and sintering can close.Only a small amount of the second phase about~2 μm is remained in matrix, with matrix
Tissue has good interface cohesion, i.e., the face divided does not occur.These obvious second phases are certain richness Si phases, these richness Si phases
Presence, reduce the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile itself and matrix
Highly organized interface cohesion and Dispersed precipitate are conducive to subsequently homogenization diffusion.
Sintering temperature is too low, the connection being unfavorable between Fe powder particles and Si atoms permeatings, and sintering temperature is excessive then can be by
In the diffusion into the surface of Fe, Si element, there is thick hole, be subsequently difficult to press, 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, which is shunk, to be caused to crack.Programming rate should not be too fast during sintering, and multistage insulation 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. can be used 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.
(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 7.36~7.49g/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, its 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%.
Due to there are a large amount of holes and hard crisp phase, taking when re-sintering for 1060 DEG C~1160 DEG C, in vacuum-sintering or also
Sintered under originality protective atmosphere, to realize the reparation of the closing of pores and crackle, and the homogenization diffusion of a degree of Si elements.
Programming 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.The accumulation drafts after sintering reaches every time
, it is necessary to sinter 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 make the density of plate reach 7.2g/cm3More than (about the 95% of solid density), it is also desirable to 4
Re-sintering more than secondary.
Metallographic structure matrix after cold rolling-sintering is about 100 μm of grain structure, there is a small amount of tiny hole.
Matrix grain has two kinds of different contrasts, this is because Si contents are different and cause to corrode difference, low Si crystal grain in this kind tissue
Be conducive to machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
(6) high temperature sintering is homogenized
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1260~1330 DEG C of temperature ranges, in the effect of thermal diffusion
Under, to realize the homogenization of Si, form single-phase alloy, obtain the high silicon steel of homogeneous, the thickness of plate is almost unchanged after densification sintering,
For 0.1~0.5mm, density reaches 7.37~7.50g/cm3。
With high-energy ball milling or rush rotation method acquisition particle diameter≤6 μm HIGH-PURITY SILICON iron powder.
Low energy mixer described in step (2) is conical mixer, V-arrangement batch mixer or drum mixer.
Step (2) adds cellulose, paraffin micro mist when mixing or zinc stearate is water-insoluble adds as binder, binder
Dosage total amount is no more than the 0.8% of mixed-powder gross mass, while adds grease and absolute ethyl alcohol does passivator, plays passivation Si
Powder, bonding Fe-Si powder, the effect for strengthening powder flowbility and compact strength, the additive amount total amount of passivator are no more than mixed powder
The 2% of last gross mass.
Step (5) sinters, by 5 when re-sintering for 1060 DEG C~1160 DEG C under vacuum-sintering or restitutive protection's atmosphere
~10 DEG C/min continuous warmings, during thickness of slab >=1mm, soaking time is 1~2h；Thickness of slab is reduced in 0.1~1mm, soaking time
0.5~1h, after the accumulation drafts after sintering reaches 30~45% every time, sinters 1 time, from the powder base of 0.96~2.3mm again
0.1~0.5mm is rolled down to, it is necessary to sinter 4~8 times again.
Support plate described in step (4) burns boat using W, Mo, corundum or zirconia ceramics.
Placement sintering plate can be overlapped during high temperature sintering, but interlayer must be laid with MgO powder, and W, Mo and ceramics can be used to burn
Boat.But plate must tile placement, tablet weight can be placed on plate, prevents from deforming in sintering process.
In addition to Si contents, content of element such as grain size, crystal grain orientation, C etc. also has the magnetic behavior of high silicon steel
Large effect, can subsequently be annealed, the technological means such as normalizing treatment is controlled by by wet hydrogen.
Essence of the invention is by with the addition of granularity≤6 μm in the reduction Fe powder of the big volumetric portion with good plasticity
Fe-50~70%Si high-purity powders, form Fe-4.5~6.7%Si alloy mixtures, powder rolling is into carrying out after slab
Incomplete alloying sintering, makes Fe powder particles realize not exclusively sintering, and Si and Fe realize it is partially-alloyed, formed it is porous, have
There is the high silicon steel blank of the incomplete alloying of compressibility.Subsequently through multi-pass cold rolling and sintering, structural homogenity is improved
And compactness, then by high-temperature diffusion process, the homogenization of Si is realized, so as to obtain the single-phase high silicon strip of complete alloying
Material.This method realizes Technics Process Automation, continuous production by technique and equipment Design, it can be mass-produced 0.1~
0.5mm is thick, 7.37~7.50g/cm of density3High silicon steel band.
Brief description of the drawings
Fig. 1 is the metallograph after the powder rolling base sintering of the embodiment of the present invention 2；
Fig. 2 is metallograph of the plate of the embodiment of the present invention 3 after 2 cold rolling-sintering；
Fig. 3 is XRD diffraction curve figures after the powder rolling base high temperature sintering of the embodiment of the present invention 4.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Embodiment 1
By the reduction Fe powder of -100 mesh and the Fe-70%Si high-purity powders of granularity≤6 μm according to 90.43:9.57 ratio
Mixing, forms 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 is added according to 200ml/ tons of amount.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 2.3mm is rolled out, the width of slab is 100mm.The density of pressed compact is 6.2g/cm3。
Powder strip plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.Adopt
With the programming 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.Burn
It is 6.25g/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：2.3mm → 1.58mm → 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 7.36g/cm3。
For above-mentioned cold rolling made-up belt in 1335 DEG C of vacuum-sintering 1h, it is about 0.50mm, density 7.37g/cm to obtain thickness3, Si
Content is the 6.7% high silicon steel of single-phase homogeneous.
Embodiment 2
By the reduction Fe powder of -100 mesh and the Fe-50%Si high-purity powders of granularity≤10 μm according to 91:9 ratio mixing,
Form 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.Anhydrous second
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 1.0mm is rolled out, the width of slab is 240mm.The density of pressed compact is 6.70g/cm3。
Powder strip plate is placed on surface to be coated with the molybdenum plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace.Adopt
With the programming 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.Burn
It is 6.70g/cm to tie base density3。
Uniform equiaxed grain structure is formed after sintering, sees Fig. 1.Matrix grain is about 70~100 μm, and crystal boundary exists about~10
μm hole, follow-up rolling and sintering can close.Only a small amount of the second phase about~2 μm is remained in matrix,
There is good interface cohesion with matrix, i.e., the face divided do not occur.These obvious second phases are certain richness Si phases, these
The presence of rich Si phases, reduces the Si contents of matrix so that matrix has high plastic deformation ability；Meanwhile its
Good interface cohesion and Dispersed precipitate are conducive to subsequently homogenization diffusion with matrix.
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：0.96mm→0.64mm→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 7.49g/cm3。
For above-mentioned cold rolling made-up belt in 1265 DEG C of vacuum-sintering 4h, it is about 0.10mm, density 7.50g/cm to obtain thickness3, Si
Content is the 4.5% high silicon steel of single-phase homogeneous.
Embodiment 3
By the reduction Fe powder of -100 mesh and the Fe-60%Si high-purity powders of granularity≤6 μm according to 89.17:10.83 ratio
Mixing, forms the mixed-powder of Fe-6.5%Si.The paraffin micro mist of raw material total amount 0.4% is added during mixing, 0.2% methyl is fine
Dimension element, 0.1% machine oil.Absolute ethyl alcohol is added according to 400ml/ tons of amount.Above-mentioned powder is mixed using drum mixer
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 1.58mm is rolled out, the width of slab is 150mm.The density of pressed compact is 6.25g/cm3。
Powder strip plate is placed on surface to be coated with the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the programming rate of 3 DEG C/min, and 2h, 400 DEG C of insulation 3h are kept the temperature at 200 DEG C.Then it will heat up to 1120 DEG C of insulations and burn
Tie 3h.Sintered blank density is 6.30g/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：1.58mm → 1.08mm → 0.70mm → 0.45mm → 0.27mm, i.e., after 4 cold rollings and 3 sintering, plate
Thickness reach 0.27mm, density reaches 7.38g/cm3。
Fig. 2 is shown in metallographic structure after 2 cold rolling-sintering, and matrix is about 100 μm of grain structure, exists a small amount of thin
Small hole.Matrix grain has two kinds of different contrasts, this is because Si contents are different and cause to corrode difference, in this kind tissue
Low Si crystal grain is conducive to machining deformation so that the thin plate of 0.1~0.5mm of manufacture is possibly realized.
For above-mentioned cold rolling made-up belt in 1300 DEG C of vacuum-sintering 2h, it is about 0.27mm, density 7.39g/cm to obtain thickness3, Si
Content is the 6.5% high silicon steel of single-phase homogeneous.
Embodiment 4
By the reduction Fe powder of -100 mesh and the Fe-62%Si high-purity powders of granularity≤10 μm according to 90.64:9.36 ratio
Mixing, forms 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 is added according to 400ml/ tons of amount.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 180mm.The density of pressed compact is 6.42g/cm3。
Powder strip plate is placed on surface to be coated with the corundum plate of MgO micro mists, the degreasing of hydrogen tube furnace is placed into, burns
Knot.Using the programming rate of 4 DEG C/min, and 3h, 400 DEG C of insulation 2h are kept the temperature at 200 DEG C.Then it will heat up to 1130 DEG C of insulations and burn
Tie 2h.Sintered blank density is 6.46g/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 1130 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 is that is, cold through 7 times
Roll with after 6 sintering, the thickness of plate reaches 0.21mm, and density reaches 7.42g/cm3。
For above-mentioned cold rolling made-up belt in 1315 DEG C of vacuum-sintering 2h, it is about 0.22mm, density 7.43g/cm to obtain thickness3, Si
Content is 5.8%, and the XRD analysis figure of its final plate is shown in Fig. 3, is the high silicon steel of single-phase homogeneous.
Claims (7)
1. a kind of powder rolling manufacture method of high silicon steel thin belt material, 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, uses Si contents as 50~70% HIGH-PURITY SILICON iron powder, particle diameter≤6 μm, and major impurity is~0.24%Al ,~0.07%Ca
With~0.02%C, remaining is Fe；
(2) powder mixes
According to the ratio of Fe-4.5~6.7%Si, reduction Fe powder and Fe-50~70%Si HIGH-PURITY SILICON iron powders are weighed；Protected in inertia
Protect under atmosphere and mixed using low energy mixer；
(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
It is 0.96~2.3mm to go out thickness, and width is 100~240mm, and density is 6.2~6.7g/cm3Powder strip plate；
(4) degreasing, sintering
Powder strip plate is placed on surface to be coated with the support plate of MgO micro mists, is placed into vacuum degreasing, sintering furnace, using 2
The programming rate of~5 DEG C/min, and 2h~4h is kept the temperature respectively in 200 DEG C, 400 DEG C, then it will heat up to 1060~1160 DEG C of guarantors
Temperature 2~4h of sintering, sintered blank density is 6.25~6.7g/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 7.36~7.49g/cm3；
(6) high temperature sintering is homogenized：
Vacuum or restitutive protection 1~4h of atmosphere sintering in 1265~1335 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 7.37~7.50g/cm3。
2. the powder rolling manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：With high-energy ball milling or
Rush rotation method and obtain particle diameter≤6 μm HIGH-PURITY SILICON iron powder.
3. the powder rolling manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (2) is described
Low energy mixer be conical mixer, V-arrangement batch mixer or drum mixer.
4. the powder rolling manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (2) mixes
When add that cellulose, paraffin micro mist or zinc stearate are water-insoluble as binder, the additive amount total amount of binder is no more than mixing
The 0.8% of powder gross mass, while add grease and absolute ethyl alcohol does passivator, play passivation Si powder, bonding Fe-Si powder, enhancing
The effect of powder flowbility and compact strength, the additive amount total amount of passivator are no more than the 2% of mixed-powder gross mass.
5. the powder rolling manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (5) exists
1060~1160 DEG C when re-sintering, sinter 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 0.5~1h in 0.1~1mm, soaking time, every time after sintering
Accumulation drafts reach 30~45% after, again sinter 1 time, be rolled down to 0.1~0.5mm from the powder base of 0.96~2.3mm, it is necessary to
Again sinter 4~8 times.
6. the powder rolling manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Folded during high temperature sintering
Close and place sintering plate, interlayer is laid with MgO powder.
7. the powder rolling manufacture method of high silicon steel thin belt material as claimed in claim 1, it is characterised in that：Step (4) is described
Support plate boat is burnt using W, Mo, corundum or zirconia ceramics.
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