CN108796568A - The method and device of high-silicon steel thin strip is prepared under a kind of low-intensity magnetic fields - Google Patents
The method and device of high-silicon steel thin strip is prepared under a kind of low-intensity magnetic fields Download PDFInfo
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- CN108796568A CN108796568A CN201710300505.3A CN201710300505A CN108796568A CN 108796568 A CN108796568 A CN 108796568A CN 201710300505 A CN201710300505 A CN 201710300505A CN 108796568 A CN108796568 A CN 108796568A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C25D5/006—
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
- C25D5/50—After-treatment of electroplated surfaces by heat-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0614—Strips or foils
Abstract
The invention discloses a this method to obtain high silicon cladding using magnetostatic field pulse composite plating technology on low-silicon steel piece surface, then the high-silicon steel thin strip that silicone content is 6.5wt%Si is obtained by heat treatment process, the present invention is easy to operate, silicon operation can be increased to be realized under room temperature, it is of low cost, and near-net-shape high-silicon steel band can be prepared.
Description
Technical field
The present invention relates to the method and devices that high-silicon steel thin strip is prepared under a kind of magnetic field.Belong to soft magnetic material prepare,
Electroplating technology.
Background technology
Silicon steel thin belt is widely used in electric power, electric appliance, electronics and state as a kind of very important energy conversion material
Anti- war industry, silicon steel are currently yield and a kind of maximum soft magnetic materials of dosage in electricity, magnetic fields.With silicone content
Increase, the enhancing of the soft magnet performance of silicon steel thin belt, after the silicone content in silicon steel is increased to 6.5wt%, silicon-steel magnetic can reach most
Good, the magnetostriction coefficient of silicon steel thin belt drops significantly to almost zero at this time.But with the increase of silicone content, the brittleness of silicon steel is aobvious
It writes and increases, after silicone content is more than 5wt%, the elongation percentage reduction of silicon steel is almost equal to zero.Therefore, very using conventional milling method
It is 6.5wt%S silicon steel thin belts that difficulty, which prepares high silicon especially silicone content,.
Currently, domestic and foreign scholars to the preparation method of the high silicon especially silicon steel thin belt of 6.5wt%Si largely grind
Study carefully, it is proposed that a variety of preparation processes, such as multiple tracks rolling, fused salt electrodeposition process, laser cladding, powqder rolling process, electro-deposition-
Diffusion method, CVD method and PCVD methods etc..But using these complex process, high energy consumption, and in element silicon distributing homogeneity
Difference limits its application.When using electro-deposition-diffusion the preparation method, it is electroplated under normal condition, the coating silicone content of acquisition
It is small, sufficient silicon source can not be provided for low silicon substrate, coating silicone content is significantly improved using magnetic field energy is applied, but coating table
Face is very coarse, and the magnetic field intensity applied is relatively high, no matter using being electroplated under normal condition or magnetic field, using water system electricity
For evolving hydrogen reaction than more serious, the coating of acquisition is low with the bond strength of matrix, limits the technique in electroplating process when plating solution
Further apply；Therefore, the high-silicon steel preparation method for developing Cheap highly effective is still critical issue urgently to be resolved hurrily.
Invention content
The purpose of the present invention is：It provides and prepares silicone content about 6.5wt%Si high-silicon steel steel under a kind of low-intensity magnetic fields auxiliary
The method and equipment of strip obtain high silicon cladding on low-silicon steel piece surface using magnetostatic field pulse composite plating technology, then pass through
Overheating Treatment technique come obtain with excellent magnetic can high-silicon steel thin strip, can be to be operated under room temperature, and can prepare close
The strip of whole type, easy to operate, manufacturing cost is low, with overcome the deficiencies in the prior art.
Technical scheme of the present invention
A kind of method that high-silicon steel thin strip is prepared under low-intensity magnetic fields, this method are existed using magnetostatic field pulse composite plating technology
Low-silicon steel piece surface obtains high silicon cladding, then obtains the high-silicon steel thin that silicone content is 6.5wt%Si by heat treatment process
Band.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, the design of this method is：Using having
Machine system modified magnetic silicon-iron particle is added in organic solvent electrolyte, as solvent using pure iron plate or low-silicon steel plate
As anode, the thickness of pure iron plate or low-silicon steel plate using pure iron plate or low-silicon steel plate as cathode, and at cathode is than sun
Very thin, using pulse composite plating method, Silicon-rich of the one layer of silicone content of plating more than 6.5wt%Si plates on low silicon steel thin band
Layer.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, the organic solvent electrolyte is plating
Iron organic solvent electrolyte, the organic solvent are to increase the binding force of coating and matrix in order to reduce evolving hydrogen reaction, specifically match
Fang Shi uses alcohol for solvent, is added 0.01~10mol/L Na2SO4,0.01~10mol/L FeSO4,0.01~
The modified of 0.1~200g/L is added in 10mol/L FeCl2,0.01~10mol/LNH4Cl, 0.1~10g/L of reduced iron powder
Silicon-ferromagnetic particle.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, in the compound electroplating process of pulse,
Coating granule content can be significantly improved by applying one constant external magnetic field, and the magnetic field size is 0.001~0.2T.
It is described to prepare modified magnetism in the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned
Silicon-iron particle is that pure silicon granules are used chemical reduction method plating last layer pure iron, increases its soft magnetic property.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, the pure silicon granules refer to granularity model
It encloses for 0-10 μm of pure silicon powder.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, the chemical reduction method refers to will be pure
Silicon particle injects in iron reducing solution, the FeCl3 solution added with the speed of 5-10ml per minute, by solution after strong mixing 2-5min
It filters and repeatedly washs, obtain modified silicon-iron particle after one layer of iron of reduction deposition on silicon particle, dramatically increase its magnetization
Rate and conductivity.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, the iron reducing solution preparation process
It is that the PAA high molecular surfactants of a concentration of 20wt% and deionized water are added to deionized water by 1 to 4~10 ratio row
In, 100~500g/L of silicon particle is added in water bath condition in guiding humid medium 0.2g/L, dispersant 5g/L, catalyst activator 2g/L
Then the reducing agent of the NaBH4 of 10~50g/L is added in lower strong mixing 60min；The capacity of the FeCl3 solution and iron reducing solution
Capacity ratio be 1:1 and FeCl3 solution concentrations are 0.1~1mol/L.
In the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, specific preparation process is：
Step 1: the preparation of modified silicon-iron particle
1）, prepared sizes ranging from 0-10 μm of pure silicon powder；
2）The preparation and electronation of iron reducing solution, by the PAA high molecular surfactants and deionized water of a concentration of 20wt%
It is add to deionized water by 1 to 4~10 ratio row, guiding humid medium（Ten diamino sulfonic acid sodium）0.2g/L, dispersant（Hexadecane
Base trimethylammonium bromide）5g/L, catalyst activator (palladium bichloride）100~500g/L of silicon particle is added in water bath condition in 2g/L
Then the reducing agent of the NaBH4 of 10~50g/L is added in lower strong mixing 60min, by pure silicon powder to entering in original solution, then press and
Original solution 1:1 ratio adds the FeCl3 solution of 0.1~1mol/L with the speed of 5-10ml per minute, will after strong mixing 2-5min
Solution is filtered and is repeatedly washed, and is obtained modified silicon-iron particle after one layer of iron of reduction deposition on silicon particle, is dramatically increased it
Magnetic susceptibility and conductivity；
Step 2: electro-deposition under magnetic field
The magnetic field intensity of application be 0.001~0.2T, use 0.05~0.5mm thickness pure iron strip or low silicon steel thin piece for
The silicone content of cathode, width 10-2000mm, low-silicon steel strip is 0.1-3wt%, using pure iron piece or low-silicon steel plate as anode,
The thickness of pure iron piece either low-silicon steel plate is less than at anode at the cathode and pure iron piece or low-silicon steel plate use sand paper at cathode
It polishes bright and clean, then with being put into electroplate liquid after pickling, acetone grease removal；To ensure that electroplate liquid silicon-ferromagnetic particle is uniformly suspended in
In electroplate liquid, mechanical agitation may be used or stir electroplate liquid by the way of acid solution pump circulation；It puts the electrodes into electrolytic cell,
It is that 0.01A~100A/dm2 pulse currents carry out composite plating to be passed through mean value current density；
Step 3: the preparation of electroplating solution
Use alcohol for solvent, 0.01~10mol/L Na2SO4,0.01~10mol/L FeSO4,0.01~10mol/L
Then silicon-ferromagnetism of 0.1~200g/L is added in FeCl2,0.01~10mol/LNH4Cl, 0.1~10g/L of reduced iron powder
Particle；
Step 4: to ensure to obtain continuous high silicon composite deposite, cathode and anode spacing are maintained at 0.2-20cm；Pass through control
The Multiple factors such as silicon-iron particle concentration, modified silicon-iron particle surface layer pure iron layer thickness, magnetic field intensity in current density, electroplate liquid
To control the silicone content in composite deposite.To prepare the high-silicon steel thin strip of overall silicone content about 6.5wt%Si, in composite deposite
Silicone content can be controlled between 6.5-50wt%, the thickness of composite deposite is 5-500 microns；
Step 5: homogenization diffusion annealing：Iron-the Antaciron for being about 6.5Wt% by the average silicon content that above-mentioned steps obtain
Particles dispersed coated steel strips are put into band inert gas after dry dry, or are reducing gas or are inert gas and reduction
Heat treatment DIFFUSION TREATMENT is carried out in the tubular electric furnace of gas mixing gas shielded, is obtained average silicone content and is 6.5Wt% and is distributed equal
Even orientation or non-oriented silicon steel sheet, at 900-1300 DEG C, heat treatment time is 0.25-10 hours for heat treatment temperature control.
The device of high-silicon steel thin strip, including Stationary Magnetic Field Generator for Magnetic, protective device, electricity are prepared under a kind of low-intensity magnetic fields
Coating bath, plating tank cover plate, polytetrafluoroethylene (PTFE) bottom, electroplate liquid, modified silicon-iron particle, pure iron piece anode, low-silicon steel band cathode, arteries and veins
Rush power supply, mechanical agitation paddle, mechanical agitation control device, with meshed grid baffle, the heatproof electroplating bath is placed in poly- four
On vinyl fluoride bottom plate, and periphery is followed successively by electroplating bath, protection materials and Stationary Magnetic Field Generator for Magnetic from inside to outside；In the electroplating bath
Storage electroplate liquid and modified silicon-iron particle are contained, interior bottom is provided with the mechanical agitation paddle of externally continuous mechanical mixing control device, impregnates
In there is the pure iron piece anode plate to be connected on the pulse power with low-silicon steel band cathode in electroplate liquid, tank cover plate and electroplating bath is electroplated
Upper end face paste is neat and is held out against with protective device inside, with meshed grid baffle plate setting to separate mechanical agitation in electroplating bath
Paddle and the pulse power.
In the device for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, which is duty ratio and frequency
The adjustable pulse power of rate or duty ratio, frequency and period can be reversed DC power supply, or constant amplitude it is straight
Galvanic electricity source provides the electric current of different characteristics for electroplating process.
In the device for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields above-mentioned, magnetic field generator can be electromagnet
The magnetic field of generation, or the magnetic field that permanent magnet provides, the magnetic induction intensity provided are 0.001-0.2T
Compared with prior art, the present invention has obvious prominent substantive distinguishing features and marked improvement：
（1）It is electroplated under conditions of applying stationary magnetic field, the magnetization of modified silicon-iron particle is inhaled using magnetic field force
Cathode surface is guided to improve the silicone content of coating.The magnetic field intensity of application is smaller, 0-0.2T.
（2）Since electrodeposition process is carried out under conditions of magnetic field, due to magnetocrystalline anisotropy and induced anisotropy
Effect, by adjusting current density, the parameters such as magnetic field intensity can make tissue orientating（Magnetic field can promote silicon steel thin belt along
(110)[001]）, improve magnetic property.
（3）Whole preparation process be not present pressure processing or its property deformation process, can fundamentally avoid it is any due to
Processing difficulties caused by the inductile of 6.5wt%Si high-silicon steels.
（4）The deposition velocity and diffusion velocity of silicon-iron modified particles can be strong by the current density of adjusting deposition, magnetic field
Degree and mechanical agitation speed, avoid silicon steel thin belt surface silicon too high levels.
（5）When being heat-treated, due to fine silicon-ferromagnetic particle using 0.1-10um, not only grain size is thin
It is small, there is larger contact area with iron plating matrix, be conducive to the uniform diffusion of element silicon, element silicon distribution ratio can be obtained
More uniform 6.5wt%Si high-silicon steel thin strips.
（6）By the way of Composite Coatings under room temperature, the energy can be greatlyd save；Stable processing technique is controllable.
（7）The original structure of matrix is influenced small.
（8）The medicament used is cheap, easily obtains, and consumes few.
Description of the drawings
Attached drawing 1 is the structural schematic diagram of the dedicated unit used in the present invention.
Specific implementation mode
Below in conjunction with the accompanying drawings to further detailed description of the invention, but not as any limitation of the invention.
Embodiment one：
1）The preparation of modified silicon-iron particle：It is 0-10 μm of pure silicon powder by particle size range, silicon particle is added to reproducibility ring first
Chemical plating reduction is carried out in the ferrous iron solution of border so that silicon particle coating surface last layer pure iron layer obtains modified silicon-iron particle,
What pure silicon granules is compared, and the magnetic susceptibility of particle what conductivity is significantly improved.Then it is dried in vacuum environment after filtering standby
With.
2）The preparation of iron reducing solution：The PAA high molecular surfactants and deionized water of a concentration of 20wt% are pressed 1 to 4
~10 ratio row are add to deionized water, guiding humid medium（Ten diamino sulfonic acid sodium）0.2g/L, dispersant（Cetyl front three
Base ammonium bromide）5g/L, catalyst activator (palladium bichloride）2g/L is added 100~500g/L of silicon particle and is stirred by force under water bath condition
60min is mixed, the reducing agent of the NaBH4 of 10~50g/L is then added, is pressed and original solution 1:1 ratio is with the speed of 7.5ml per minute
Degree adds the FeCl3 solution of 0.1~1mol/L, filters solution after strong mixing 2-5min and repeatedly washs.
3）Electro-deposition under magnetic field：The magnetic field intensity of application is 0.001~0.2T, and the pure iron using 0.05~0.5mm thickness is thin
Band or low silicon steel thin piece are cathode, and the silicone content of width 10-2000mm, low-silicon steel strip are 0.1-3wt%, with pure iron
Piece or low-silicon steel plate are anode；To ensure that electroplate liquid silicon-ferromagnetic particle is uniformly suspended in electroplate liquid, machinery may be used
Stirring stirs electroplate liquid by the way of acid solution pump circulation；It puts the electrodes into electrolytic cell, being passed through mean value current density is
0.01A~100A/dm2 pulse currents carry out composite plating；
4）The preparation of electroplating solution：Use alcohol for solvent, 0.01~10mol/L Na2SO4,0.01~10mol/L FeSO4,
0.01~10mol/L FeCl2,0.01~10mol/LNH4Cl, 0.1~10g/L of reduced iron powder, then be added 0.1~
Modified silicon-iron particle of 200g/L.
5）To ensure to obtain continuous high silicon composite deposite, cathode and anode spacing are maintained at 0.2-20cm；Pass through control
Surface layer pure iron layer thickness, magnetic field intensity etc. are more in modified silicon-iron particle concentration, modified silicon-iron particle in current density, electroplate liquid
It is a because usually controlling the silicone content in composite deposite.It is compound to prepare the high-silicon steel thin strip of overall silicone content about 6.5wt%Si
Silicone content in coating is can be controlled between 6.5-50wt%；The thickness of composite deposite is 5-500 microns.
6）Homogenize diffusion annealing：The composite deposite for being about 6.5Wt% by the ensemble average silicon content that above-mentioned steps obtain
Steel band is put into band inert gas after dry dry, or is reducing gas（Carbon monoxide, hydrogen etc.）Or for inert gas with
Heat treatment DIFFUSION TREATMENT is carried out in the tubular electric furnace of reducing gas mixing gas shielded, average silicone content is obtained and is 6.5Wt% and divides
Cloth is uniformly orientated or non-oriented silicon steel sheet.At 900-1300 DEG C, heat treatment time is that 0.25-10 is small for heat treatment temperature control
When.
Embodiment two：
Referring to Fig. 1, the device of high silicon steel thin belt is prepared under this low-intensity magnetic fields, is applied to the above method, including stationary magnetic field is sent out
Raw device 1, protective device 2, electroplating bath 3, plating tank cover plate 4, polytetrafluoroethylene (PTFE) bottom 5, electroplate liquid 6, modified silicon-iron particle 7, pure iron
Piece anode 8, low-silicon steel with cathode 9, the pulse power 10, mechanical agitation paddle 11, mechanical agitation control device 12, with mesh 13
Grid baffles 14 etc. form.The heatproof electroplating bath 3 is placed on polytetrafluoroethylene (PTFE) bottom plate 5, and periphery is followed successively by electricity from inside to outside
Coating bath 3, protection materials 2 and Stationary Magnetic Field Generator for Magnetic 1；Storage electroplate liquid 6 and modified silicon-iron particle 7 are contained in the electroplating bath 3, it is interior
Bottom is provided with the mechanical agitation paddle 11 of externally continuous mechanical mixing control device 12, and being soaked in electroplate liquid 6 has the pure iron
Piece anode plate 8 and low-silicon steel band cathode 9 connect on the pulse power 10.
Embodiment three：
A kind of method that high-silicon steel thin strip is prepared under low-intensity magnetic fields, the specific operation of the present embodiment are as described below：
Filling plating of the peak diameter for 0.1-0.5um iron layer acquisition modified silicon-iron particle 7 on 2 μm, silicon particle coating surface
Liquid 6 is placed in the heatproof electroplating bath 3 that capacity is 50 L, and the ingredient of electroplate liquid is：Alcohol is solvent, 0.5mol/L Na2SO4,
Modified silicon-iron particle 7 of 20g/L is added in 0.90mol/L FeSO4,0.15mol/L FeCl2,0.43mol/LNH4Cl.
It is the low silicon steel thin strip cathodes of 3wt%Si 9 that pure iron piece anode 8 and silicone content are equipped in electroplating bath 3.Meanwhile to ensure electroplate liquid 6
In modified silicon-iron particle 7 be distributed it is relatively uniform, using mechanical agitation paddle 11 and mechanical agitation control device 12 come stir electrolysis
Liquid, rotating speed are 80 r/min.
Use thickness for 0.2mm, width 500mm, silicon content be 3wt% low silicon silicon strip as silicon strip cathode 9,
Pure iron piece anode 8 is immersed in electroplate liquid 6, and pure iron piece anode 8 and cathode 9 are connected with the anode and cathode of the pulse power 10
It connects；Mechanical agitation paddle 12 and mechanical agitation control device 11 are opened simultaneously, control mixing speed is 80 revs/min, is then turned on
The composite plating pulse power 10, adjustment pulse current pulsewidth are 0.5ms, and duty ratio 40%, the flat width of pulse is the arteries and veins of 1A/dm2
Electric current is rushed,；The magnetic field of Stationary Magnetic Field Generator for Magnetic 1 is provided by electromagnet, and magnetic induction intensity remains 0.1T.The direction of the magnetic line of force 15
It is horizontal direction on cathode surface.
It is 2 μm of modified silicon-iron particles due to containing peak diameter in electroplate liquid 6, utilizes composite plating effect and magnetic field pair
Modified silicon-iron particle is adsorbed on surface of the 3wt%Si low-silicon steels with cathode by magnetization effect of the low-silicon steel with cathode, and multiple with iron
Electro-deposition is closed, the composite deposite of Silicon-rich is obtained, is measured through energy spectrum analysis (EDS), which is 28.56wt%,
The thickness of composite deposite is about 50 microns, and the composite deposite and 3wt%Si low-silicon steels band cathode are final through subsequent heat treatment
Silicone content reaches 6.45wt%, this ingredient has basically reached the component target of optimum magnetic energy 6.5wt%Si silicon steel thin belts.
In conclusion the basic principles, main features and advantages of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Effect object defines.
Claims (10)
1. a kind of method for preparing high-silicon steel thin strip under low-intensity magnetic fields, it is characterised in that：This method utilizes magnetostatic field pulse
Composite plating technology obtains high silicon cladding on low-silicon steel piece surface, then obtains silicone content by heat treatment process as 6.5wt%
The high-silicon steel thin strip of Si.
2. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 1, it is characterised in that：It should
The design of method is：Using organic system as solvent, modified magnetic silicon-iron particle is added in organic solvent electrolyte,
Using pure iron plate or low-silicon steel plate as anode, pure iron plate using pure iron plate or low-silicon steel plate as cathode, and at cathode or
The thickness of low-silicon steel plate is thinner than anode, using pulse composite plating method, one layer of silicone content of plating on low silicon steel thin band
Silicon-rich coating more than 6.5wt%Si.
3. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 2, it is characterised in that：Institute
It is plating iron organic solvent electrolyte to state organic solvent electrolyte, the organic solvent be in order to reduce evolving hydrogen reaction, increase coating with
The binding force of matrix when specific formula, uses alcohol for solvent, is added 0.01~10mol/L Na2SO4,0.01~
10mol/L FeSO4,0.01~10mol/L FeCl2,0.01~10mol/LNH4Cl, 0.1~10g/L of reduced iron powder add
Enter modified silicon-ferromagnetic particle of 0.1~200g/L.
4. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 2, it is characterised in that：?
In the compound electroplating process of pulse, coating granule content can be significantly improved by applying one constant external magnetic field, and the magnetic field is big
Small is 0.001~0.2T.
5. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 2, it is characterised in that：Institute
It is that pure silicon granules are used chemical reduction method plating last layer pure iron to state and prepare modified magnetic silicon-iron particle, and it is soft to increase its
Magnetic property.
6. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 5, it is characterised in that：Institute
State pure silicon granules refer to particle size range be 0-10 μm of pure silicon powder.
7. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 5, it is characterised in that：Institute
It refers to injecting pure silicon granules in iron reducing solution to state chemical reduction method, the FeCl3 solution added with the speed of 5-10ml per minute,
Solution is filtered after strong mixing 2-5min and is repeatedly washed, modified silicon-is obtained after one layer of iron of reduction deposition on silicon particle
Iron particle dramatically increases its magnetic susceptibility and conductivity.
8. the method for preparing high-silicon steel thin strip under a kind of low-intensity magnetic fields according to claim 7, it is characterised in that：Institute
Stating iron reducing solution preparation process is, the PAA high molecular surfactants and deionized water of a concentration of 20wt% are pressed 1 to 4~10
Ratio row be add to deionized water, guiding humid medium 0.2g/L, dispersant 5g/L, catalyst activator 2g/L, be added silicon particle
Then the reducing agent of the NaBH4 of 10~50g/L is added in 100~500g/L strong mixing 60min under water bath condition；The FeCl3 is molten
The capacity of liquid is 1 with the capacity ratio of iron reducing solution:1 and FeCl3 solution concentrations are 0.1~1mol/L.
9. according to the method for preparing high-silicon steel thin strip under a kind of any low-intensity magnetic fields of claim 1-8, feature
It is：Specifically preparation process is：
Step 1: the preparation of modified silicon-iron particle
1）, prepared sizes ranging from 0-10 μm of pure silicon powder；
2）The preparation and electronation of iron reducing solution, by the PAA high molecular surfactants and deionized water of a concentration of 20wt%
It is add to deionized water by 1 to 4~10 ratio row, guiding humid medium 0.2g/L, dispersant 5g/L, catalyst activator 2g/L,
100~500g/L of silicon particle strong mixing 60min under water bath condition are added, the reduction of the NaBH4 of 10~50g/L is then added
Then agent is pressed and original solution 1 by pure silicon powder to entering in original solution:1 ratio adds 0.1 with the speed of 5-10ml per minute~
Solution is filtered after strong mixing 2-5min and is repeatedly washed by the FeCl3 solution of 1mol/L, on silicon particle reduction deposit one layer of iron
Modified silicon-iron particle is obtained afterwards, dramatically increases its magnetic susceptibility and conductivity；
Step 2: electro-deposition under magnetic field
The magnetic field intensity of application be 0.001~0.2T, use 0.05~0.5mm thickness pure iron strip or low silicon steel thin piece for
The silicone content of cathode, width 10-2000mm, low-silicon steel strip is 0.1-3wt%, using pure iron piece or low-silicon steel plate as anode,
The thickness of pure iron piece either low-silicon steel plate is less than at anode at the cathode and pure iron piece or low-silicon steel plate use sand paper at cathode
It polishes bright and clean, then with being put into electroplate liquid after pickling, acetone grease removal；To ensure that electroplate liquid silicon-ferromagnetic particle is uniformly suspended in
In electroplate liquid, mechanical agitation may be used or stir electroplate liquid by the way of acid solution pump circulation；It puts the electrodes into electrolytic cell,
It is that 0.01A~100A/dm2 pulse currents carry out composite plating to be passed through mean value current density；
Step 3: the preparation of electroplating solution
Use alcohol for solvent, 0.01~10mol/L Na2SO4,0.01~10mol/L FeSO4,0.01~10mol/L
Then silicon-ferromagnetism of 0.1~200g/L is added in FeCl2,0.01~10mol/LNH4Cl, 0.1~10g/L of reduced iron powder
Particle；
Step 4: to ensure to obtain continuous high silicon composite deposite, cathode and anode spacing are maintained at 0.2-20cm；Pass through control
The Multiple factors such as silicon-iron particle concentration, modified silicon-iron particle surface layer pure iron layer thickness, magnetic field intensity in current density, electroplate liquid
The silicone content in composite deposite is controlled, to prepare the high-silicon steel thin strip of overall silicone content about 6.5wt%Si, in composite deposite
Silicone content can be controlled between 6.5-50wt%, the thickness of composite deposite is 5-500 microns；
Step 5: homogenization diffusion annealing：Iron-the Antaciron for being about 6.5Wt% by the average silicon content that above-mentioned steps obtain
Particles dispersed coated steel strips are put into band inert gas after dry dry, or are reducing gas or are inert gas and reduction
Heat treatment DIFFUSION TREATMENT is carried out in the tubular electric furnace of gas mixing gas shielded, is obtained average silicone content and is 6.5Wt% and is distributed equal
Even orientation or non-oriented silicon steel sheet, at 900-1300 DEG C, heat treatment time is 0.25-10 hours for heat treatment temperature control.
10. preparing the device of high-silicon steel thin strip, including Stationary Magnetic Field Generator for Magnetic under a kind of low-intensity magnetic fields（1）, protective device
（2）, electroplating bath（3）, plating tank cover plate（4）, polytetrafluoroethylene (PTFE) bottom（5）, electroplate liquid（6）, modified silicon-iron particle（7）, pure iron piece
Anode（8）, low-silicon steel band cathode（9）, the pulse power（10）, mechanical agitation paddle（11）, mechanical agitation control device（12）, carry
Mesh（13）Grid baffle（14）, it is characterised in that：The heatproof electroplating bath（3）It is placed in polytetrafluoroethylene (PTFE) bottom plate（5）On, and
Periphery is followed successively by electroplating bath from inside to outside（3）, protection materials（2）And Stationary Magnetic Field Generator for Magnetic（1）；The electroplating bath（3）Interior Sheng
Store electroplate liquid（6）With modified silicon-iron particle（7）, interior bottom is provided with externally continuous mechanical mixing control device（12）Machinery stir
Mix paddle（11）, it is soaked in electroplate liquid（6）Inside there is the pure iron piece anode plate（8）With low-silicon steel band cathode（9）Connect pulse electricity
Source（10）On, tank cover plate is electroplated（4）With electroplating bath（3）Upper end face paste is neat and and protective device（2）Inside is held out against, and carries mesh
（13）Grid baffle（14）It is arranged in electroplating bath（3）It is interior to separate mechanical agitation paddle（11）And the pulse power（10）.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115874232A (en) * | 2023-02-27 | 2023-03-31 | 北京科技大学 | Method for preparing gradient high-silicon steel by molten salt electrolysis |
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