CN110218853A - Prepare the process of low temperature high magnetic induction grain-oriented silicon steel - Google Patents
Prepare the process of low temperature high magnetic induction grain-oriented silicon steel Download PDFInfo
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- CN110218853A CN110218853A CN201910563069.8A CN201910563069A CN110218853A CN 110218853 A CN110218853 A CN 110218853A CN 201910563069 A CN201910563069 A CN 201910563069A CN 110218853 A CN110218853 A CN 110218853A
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- nitriding
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D3/00—Diffusion processes for extraction of non-metals; Furnaces therefor
- C21D3/02—Extraction of non-metals
- C21D3/04—Decarburising
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
- C23C8/24—Nitriding
- C23C8/26—Nitriding of ferrous surfaces
Abstract
The invention discloses a kind of processes for preparing low temperature high magnetic induction grain-oriented silicon steel, belong to steelmaking technical field.The process is different from nitridation technique after traditional cold-reduced sheet decarburizing annealing, and nitriding is carried out within the temperature range of cold-reduced sheet decarburizing annealing initial stage starts primary recrystallization, and reduce the escape of nitrogen by being formed to internal oxidation layer in different strip thickness control nitrogen contents and decarbonizing process and contribute to form stable nitride precipitated phase.And this method control nitriding decarburization after primary recrystallization Grain Surface it is smaller and with central core crystallite dimension ratio within OK range, increase Gauss nucleus quantity, reducing finished product crystallite dimension reduces iron loss purpose to reach, and reaching improves product iron loss and ensure the stable dual purpose of performance.Obtaining improves product iron loss, improves magnetic temperature stability and energy-saving beneficial effect.
Description
Technical field
The present invention relates to the technology controlling and process of high magnetic induction grain-oriented silicon steel, belong to steelmaking technical field, more particularly to a kind of system
The process of standby low temperature high magnetic induction grain-oriented silicon steel.
Background technique
There is silicon steel low-loss, low magnetostriction etc. to have excellent magnetic characteristic, be electric power, magnetic mostly important in electronics industry
Property material.Silicon steel is generally divided into orientation silicon steel and non-orientation silicon steel.Wherein, orientation silicon steel is that secondary recrystallization occurs using crystal grain
Abnormal growth, so that finished product tissue is in the preferred orientation of goss texture { 111 }<001>.Due to the orientation characteristic of its finished product crystal grain,
<001>axis of internal crystal framework is as parallel with rolling direction as possible, this kind of material has good magnetic conductivity in rolling direction, can obtain
High magnetic induction, therefore it is widely used in transformer core manufacture.As main electromagnetic conversion carrier body, iron core is set
Meter and manufacture are one of mostly important links during transformer manufacturing.If iron core selection is excessive, volume of transformer will lead to
Increase, cost increases, and selects smaller iron core, then the value that must give one's hand to silicon steel sheet magnetic strength limits.In general, transformer industry
With magnetic induction B of silicon steel sheet under the conditions of 800A/m, 50Hz alternating magnetic field800As the reference number under iron core operating condition
According to, at the same with silicon steel sheet under the conditions of 50Hz alternating magnetic field magnetic strength be 1.7T when iron loss P17/50Grading parameter is lost for it.B800
In the referred to as high magnetic induction grain-oriented silicon steel, and its B of 1.89T or more800Higher, iron loss P17/50More low then product hierarchy is higher, more
It can satisfy the production of miniaturization low cost, high energy efficiency transformer.Preparing high-grade oriented silicon steel is manufacturing enterprise, electric power
Industry bring added value also correspondinglys increase.
The production method of current manufacture high magnetic induction grain-oriented silicon steel mainly includes three kinds, is that hot rolling slab heating temperature exists respectively
Medium temperature heating of plate blank system of 1300 DEG C or more of the high temperature heating of plate blank the preparation method, heating temperature between 1200 DEG C to 1300 DEG C
Standby method and slab heating temperature are lower than 1200 DEG C of low temperature heating of plate blank the preparation methods (referred to as " low temperature high magnetic induction grain-oriented silicon steel ").By
It can bring that lumber recovery is low, equipment loss is big, fuel consumption is more, one more than surface defects of products etc. in hot rolling slab heating temperature is excessively high
Serial metallurgical problems, therefore carrying out the production of high magnetic induction grain-oriented silicon steel using low temperature slab method is Main Trends of The Development.Not Tongfang
The different reason of the hot rolling slab heating temperature that method uses is caused by its used inhibitor type is different.Medium and high temperature slab
Method is used as congenital inhibitor due to using solid solubility temperature higher MnS, CuS etc., is added in the alloying process of steel-making
And it is formed in course of hot rolling, therefore heating temperature is higher；And low temperature slab method is due to obtaining inhibitor using process after silicon steel
Method reduces and relies on congenital inhibitor, re-started the requirement that ingredient designs and reduces solid solubility temperature, so that
Heating temperature successfully reduces 100 DEG C or more, is more in line with the environment protection requirement of future city manufacturing industry factory.
The acquisition of inhibitor will be sport technique segment extremely crucial in low temperature high magnetic induction grain-oriented silicon steel manufacturing technology the day after tomorrow, heavy
The property wanted and difficult point are embodied in two aspects: one, the inhibitor day after tomorrow controls the influence that secondary recrystallization is grown up；Two, after stable
It inhibits forming method.In a first aspect, influence of the congenital inhibitor of tradition to secondary recrystallization tying again for the first time in orientation silicon steel
Brilliant process has just started, so that high temperature slab method product primary recrystallization is smaller.And low temperature high magnetic induction grain-oriented silicon steel is due to congenital
Inhibitor is less, and the day after tomorrow, inhibitor was to be formed after decarburizing annealing, therefore first crystal grain is larger is difficult to control, it is not easy to obtain compared with
Good properties of product.Second aspect, it is enough that the inhibitor day after tomorrow relies on the Nitrizing Treatment after decarburizing annealing to obtain on silicon steel surface layer
Nitriding amount, be subsequently converted to nitride and be precipitated to be formed.The formation of nitride and steel grades design, nitriding temperature and high temperature
Annealing process control is related.
As low temperature high magnetic induction grain-oriented silicon steel manufacturing technology develops, it is found that there are still drawbacks for existing manufacturing method: 1. such as
The preceding nitriding just carries out after primary recrystallization is formed, and nitride precipitated phase is limited to the inhibiting effect of first crystal grain, still needs to
Alloy solute element is added in steelmaking alloy process and a certain amount of congenital inhibitor is provided, be easy to be mingled with influence in increase steel
Performance.2. nitriding carries out after primary recrystallization is formed, once first crystallite dimension is excessive during decarburizing annealing, it is difficult to control
Primary recrystallization size.Decarburization is completed to need longer annealing time, be easy to cause first coarse grains to influence final produce
Moral character energy, i.e. low-temperature steel technique " control window " are relatively narrow.3. silicon steel surface layer is formd by silica and iron oxide group after decarburization
At mixture oxide layer, hinder nitrogen to iron matrix spread；And first crystal grain crystal boundary of growing up tails off after decarburization, same shadow
Ring the diffusion rate of nitrogen.The two causes nitriding efficiency and medium utilization rate to reduce simultaneously.
In this regard, the technological improvement and innovation for inhibitor day after tomorrow acquisition methods are constantly proposed.
Research shows that nitriding efficiency is inversely proportional with nitriding temperature, because ammonia decomposition also rises as nitriding temperature increases
Height, activated nitrogen atom content are reduced, and cause the reduction of nitriding amount, and existing nitridation process is mostly implemented in 700 DEG C or more of range,
And the nitride precipitated phase that nitriding temperature equally will cause acquisition is different.The open patent of last century the nineties Japanese Laid-Open
Flat 2-247331, flat 7-118746 etc. disclose slab heating temperature lower than 1200 DEG C, and 700 DEG C~1000 DEG C are used after decarburization
Wider range nitriding forms the method that (Al, Si) N compensates congenital inhibitor manufacture orientation silicon steel, such method needs strict control
Primary recrystallization diameter simultaneously cooperates high-temperature annealing process, and there are still the problems that the first grain coarsening of the foregoing description is difficult to control.Europe
Continent patent EP0950120B1 discloses a kind of 850 DEG C~1050 DEG C of high temperature nitriding method, more due to the nitride that is formed at relatively high temperatures
Add stabilization, the nitrogen in later period is not easy to escape, it is thus possible to the decarburizing annealing stage just obtain stable AlN inhibitor to
Stable prod magnetic property, but nitriding temperature is higher so that nitriding efficiency is very low.
It is similarly and solves nitriding efficiency, Chinese invention patent application (application publication number: CN101294268A, application
Date of publication: 2008-10-29) it proposes to use plasma low-temperature nitriding, it can be effectively reduced nitriding temperature and improve nitriding efficiency,
Properties of product and stability are also improved.But this technical equipment demand and higher cost.
On the other hand, nitriding efficiency can also be improved to the inhibition of nitriding by solving internal oxidation layer.Chinese invention patent Shen
Please (application publication number: CN101748259A, data of publication of application: 2010-06-23) proposes that decarburization plate passes through 1.5% before nitriding
~3% small reduction ratio deformation failure internal oxidation layer, to reach preferable nitriding efficiency, but this method is in continuous decarburization nitriding
Cold rolling process is increased in annealing, and the dry operation of rolling is more demanding to roll, will increase product cost.
Getting rid of influence of the gas nitriding to surface and performance also has innovative approach, Japanese Unexamined Patent Application to improve nitriding efficiency
62-40315 more early discloses orientation silicon steel and coats the MgO for containing MnN or nitrided ferromanganese after decarburization as interleaving agent in high temperature
The method that annealing operation carries out nitriding, although excellent magnetic property can be obtained, this method receives the influence of MgO coating processes,
It can be difficult to uniformly in the process environments magnetic of high annealing volume.
Further, in order to avoid the influence of nitriding after decarburization, the technology that nitriding is carried out before decarbonization process is completed starts
Occur:
Chinese invention patent application (application publication number: CN102041440A, data of publication of application: 2011-05-04) proposes
Normalizing process before decarburizing annealing carries out Nitrizing Treatment and obtains nitride precipitation as inhibitor reinforcement, obtains good magnetic
Performance.But in actual production due to after low temperature nitriding nitride precipitated phase it is unstable, the escape and nitriding in advance of rear process nitrogen
Have an impact to first crystal grain, performance is easy unstable.
Japanese Patent Laid-Open 2-294428 carries out high magentic induction oriented silicon using the method for synchronous decarburization and nitriding annealing
The production of steel, this method can be improved nitriding efficiency and production efficiency, but not account for first caused by nitridation process variation
Crystal grain variation, properties of product are easy to happen unstable.
Therefore, though above-mentioned improved process can effectively improve nitriding efficiency, the first crystal grain after decarburization
There are technological deficiencies on stability contorting, so that production energy consumption can not be being reduced, improve product on the basis of raising production efficiency
Energy.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of processes for preparing low temperature high magnetic induction grain-oriented silicon steel.
The process not only starts nitriding within the scope of primary recrystallization start temperature, and by different strip thickness control nitrogen contents and takes off
Internal oxidation layer is formed to reduce the escape of nitrogen and contribute to form stable nitride precipitated phase during carbon.Moreover, control nitriding
Primary recrystallization Grain Surface after decarburization it is smaller and with central core crystallite dimension ratio within OK range, increase Gauss
Nucleus quantity, reducing finished product crystallite dimension to reach reduces iron loss purpose.To realize improvement product iron loss and ensure performance
Stable dual purpose.
To achieve the above object, the invention discloses a kind of processes for preparing low temperature high magnetic induction grain-oriented silicon steel, it is wrapped
It includes and is casting continuously to form base, slab heating, hot rolling, normalizing annealing, cold rolling, continuous nitriding and decarburizing annealing, surface are coated, batched, high temperature
Annealing stretches, is smooth, applying insulating layer coating and dry solidification annealing；
Wherein, the continuous nitriding and decarburization annealing process specifically include following process:
1) cold-reduced sheet is warming up to soaking between 500~670 DEG C and carries out Nitrizing Treatment, nitriding atmosphere NH3+N2+H2It is mixed
Close gas；
2) steel band nitriding increment △ N after the completion of nitriding-decarburizing annealing, the steel are controlled according to the soaking Nitrizing Treatment time
Band nitriding increment △ N meets such as following formula I relationship:
Wherein, △ N, steel band nitriding increment, unit, ppm；
T, Nitrizing Treatment time, unit, s；
D, thickness of strips, unit, mm；
3) it being warming up to soaking between 820~860 DEG C and carries out decarburizing annealing processing, the decarburizing annealing time is 120~360s,
Steel band carbon content and nitriding increment △ N are detected after the completion of decarburization, carbon content is lower than 5ppm in steel band after control decarburization, controls steel band
Nitriding increment △ N meets such as Formula Il relationship:
(185-155 × D)≤△ N≤(198-91 × D) Formula II；
4) after nitriding to be done and decarburization annealing process, steel band rolls the grain Distribution on section and is, following table on steel band
Face away from the average grain size in its 1/4 thickness section with away from steel band to respectively rolling to above and below kernel of section line in 1/4 thickness section
The ratio between average grain size n*≤0.76；And ratio n* meets following formula III relationship:
Wherein, n2To roll to the crystal grain quantity above and below kernel of section line in 1/4 thickness section；
n1It is steel band upper and lower surface to respectively away from the crystal grain quantity in its 1/4 thickness section.
Further, in step 1), the NH3Volumn concentration A meet following formula IV relationship:
A=0.165 × 10-6×T2-0.962×10-4× T+0.055 formula IV；
Wherein, T be Nitrizing Treatment temperature, unit, DEG C.
Further, in step 1), the N2With H2Volume ratio be 1:3.
Further, in step 3), decarburizing annealing atmosphere is the N of humidification2+H2Gaseous mixture, wherein steam partial pressure ratio p=
pVapor/pHydrogenIt is 0.27~0.35.
Further, the high magnetic induction grain-oriented silicon steel by mass percent be in terms of including following component；
C:0.035%~0.060%, Si:2.55~3.55%, Als:0.0100~0.0350%, Mn:0.03~
0.2%, S:0.0020~0.0100%, N:0.0040~0.0100%, Cu < 0.07%, Cr:0.03~0.2%, remaining is
Fe and inevitable field trash.
Further, the high magnetic induction grain-oriented silicon steel by mass percent be in terms of including following component；
C:0.035%~0.060%, Si:3.0~3.3%, Als:0.0100~0.0350%, Mn:0.085~
0.095%, S:0.0020~0.0100%, N:0.0062~0.0086%, Cu < 0.04%, Cr:0.03~0.16%, remaining
For Fe and inevitable field trash.
Further, the slab heating process includes 1100~1250 DEG C of heating temperature of control.
Further, the hot rolling technology includes conventional is rolled into a thickness of the hot rolled coil of 1.5~3.8mm specification.
Further, the cold-rolling process include be cold-rolled to according to 87~92% reduction ratio it is thick no more than 0.30mm at
Product.
Further, the high annealing includes control purification temperature between 1150 DEG C~1250 DEG C, after annealing
Nitrogen content and sulfur content are not higher than 10ppm in steel band.
Preferably, the surface is applied to coating MgO interleaving agent.
The principle of present invention process method is: traditional Nitrizing Treatment is advanceed to decarburizing annealing after decarburizing annealing
The low-temperature zone of temperature rise period carries out, and avoids such as normalizing nitriding layer in other technologies and is difficult to retain through pickling, and traditional nitriding
At relatively high temperatures carry out inefficiency, primary recrystallization be difficult to control and internal oxidation layer formed after influenced by Nitrizing Treatment
The advantages such as drawback has nitriding high-efficient, and energy medium loss is small, and finished surface is high-quality, and magnetic property is excellent.Wherein, specifically
The principle of technological parameter is as follows:
(1) why the present invention proposes lower nitriding temperature range between 500~670 DEG C, is because of the humidity province
Domain is the temperature that the primary recrystallization of Fe+3%Si alloy orientation silicon steel takes place, and the first crystal grain of fine uniform is in this temperature
Under the conditions of quickly formed, at this time have most primary recrystallization crystal grain and number of grain boundaries, facilitate the promotion of nitriding efficiency, together
When Nitrizing Treatment prior involvement inhibit surface layer primary recrystallization to grow up well.
(2) why the present invention proposes that the consumption of required nitriding medium ammonia under the conditions of different nitriding temperatures accounts for infiltration
The percent by volume of nitrogen mixed gas is because ammonia is with nitriding temperature in the nitriding process within the scope of 500 DEG C~1100 DEG C
Raising resolution ratio it is also higher, the activated nitrogen atom of steel band absorption is also fewer, and nitriding efficiency can be declined, and the present invention is according to big
Measuring test result proposes nitriding process ammonia consumption with non-linear relation A=0.165 × 10 of nitriding temperature-6×T2-0.962
×10-4×T+0.055；
(3) present invention ensures final products magnetic according to nitrogen increased amount △ N required for different-thickness product after nitriding-decarburization
Performance, is found by experiment that optimum controling range and the wired sexual intercourse of cold rolling coil thickness of △ N, ensures different thickness to propose
Spend the method for the stable suitable nitriding amount of properties of product；
(4) why the present invention proposes steam partial pressure ratio p=pVapor/pHydrogenIt is because this is de- for 0.27~0.35 range
Suitable internal oxidation layer can be generated under carbon atmosphere, mitigate escape of low temperature early period nitriding during de- fire, to ensure nitriding-
Nitriding increment △ N is in target control range after the completion of decarburizing annealing.
(5) present invention why propose the ratio between the average grain size of nitriding-decarburizing annealing surface layer and central core n*≤
0.76, be because the inventive technique can effective guarantee nitrided case depth, before primary recrystallization is grown up and be roughened just successfully
The first crystal grain in surface layer is inhibited to grow up, surface layer grain size is less than central core and in proper ratio value n* range after the completion of decarburizing annealing
Within.It is in the first crystal grain for being mainly formed in surface layer due to Gauss nucleus from analysis in electrical sheet material principle, surface layer is brilliant
Particle size reduction help to obtain tiny, greater number of Gauss nucleus as secondary recrystallization nucleus, to reduce finished product crystalline substance
Particle size reduces conducive to the iron loss of low temperature high magnetic induction grain-oriented silicon steel.And average crystal grain in different zones is calculated according to formula III
Dimension ratio n*, this is because steel band upper and lower surface is to the area respectively away from its 1/4 thickness range and rolls above and below kernel of section line
1/4 thickness range area equation is (as shown in Figure 1, S1=S2), observe the number of dies n in two regions1And n2Later, due to
Mean radius
Formula formula III can be extrapolated.
Therefore, compared with prior art, the present invention solving the drawbacks of traditional handicraft Nitrizing Treatment, due to being mentioned in low-temperature zone
Preceding nitriding effectively inhibits primary recrystallization, reduces the congenital inhibition this kind of to MnS, AlN of low temperature high magnetic induction grain-oriented silicon steel
Orientation silicon steel alloy smelting control window has been widened in the dependence of agent, if this kind of congenital inhibitor formation element content of Mn is wider, after
The content requirement range of its inhibitor formation element Als is also very fast, thus the stability of actual production is preferable.And it improves
Nitriding efficiency reduces nitriding medium consumption.Oxide layer is destroyed by Nitrizing Treatment after avoiding decarburization simultaneously, is conducive to improve production
Product surface quality.Final products magnetic strength is not less than 1.914T, and adhesion is horizontal not less than B grades, and the iron loss of equivalent specifications product
It is worth opposite traditional handicraft and at least declines 4.8% or more.
The beneficial effects are mainly reflected as follows following aspects:
1, the present invention solves the problems, such as nitriding inefficiency described in the prior art, higher cost, and is different from passing
Nitridation technique before decarburization after the cold rolling of system starts nitriding within the scope of primary recrystallization start temperature, and passes through different plate thickness controls
Internal oxidation layer is formed to reduce the escape of nitrogen and contribute to form stable nitride precipitated phase in nitrogen content and decarbonizing process processed.And
And this method control nitriding decarburization after primary recrystallization Grain Surface it is smaller and with central core crystallite dimension ratio in suitable model
Within enclosing, Gauss nucleus quantity is increased, reducing finished product crystallite dimension to reach reduces iron loss purpose；Reaching improves product iron loss
The dual purpose stable with performance is ensured.
2, in the method for the present invention by embodiment low temperature high magnetic induction oriented silicon steel produced at a lower temperature into
Row Nitrizing Treatment, nitriding medium consumption at least reduce 5.7%；In the final products of same size, using embodiment technique magnetic
Performance B800 average value reduces by 4.8% or more compared with comparative example in 1.914T or more, iron loss P17/50；And product adheres in the present invention
Property grading reach B grades or more.
Detailed description of the invention
Fig. 1 is that steel band section of the present invention crystal grain counts schematic diagram；
Wherein, S in Fig. 11Steel band upper and lower surface is represented to the division respectively away from its 1/4 thickness section, S2Representative is rolled into section
1/4 thickness section above and below heart line.
Specific embodiment
In order to better explain the present invention, below in conjunction with the specific embodiment main contents that the present invention is furture elucidated, but
The contents of the present invention are not limited solely to following embodiment.
The invention discloses a kind of processes for preparing low temperature high magnetic induction grain-oriented silicon steel, it includes following process flow:
(1) according to component and weight percent content are as follows: C:0.035%~0.060%, Si:2.55~3.55%, Als:
0.0100~0.0350%, Mn:0.03~0.2%, S:0.0020~0.0100%, N:0.0040~0.0100%, Cu <
0.07%, Cr:0.03~0.2%, remaining is that Fe and inevitable field trash are smelted；
(2) slab is heated after being casting continuously to form base, heating and temperature control is at 1100~1250 DEG C；
(3) conventional to be rolled into a thickness of the hot rolled coil of 1.5~3.8mm specification, and frequent annealing；
(4) finished product thickness no more than 0.30mm thickness is cold-rolled to according to 87~92% reduction ratio；
(5) cold-reduced sheet carries out continuous nitriding-decarburizing annealing after conventional alkali cleaning:
5.1) it is warming up to soaking between 500~670 DEG C and carries out Nitrizing Treatment, nitriding atmosphere NH3+N2+H2Gaseous mixture
(wherein N2:H2=1:3), while according to Nitrizing Treatment temperature, used ammonia percent by volume A meets following formula I V relationship:
A=0.165 × 10-6×T2-0.962×10-4× T+0.055 formula IV；
Wherein, T be Nitrizing Treatment temperature, unit, DEG C.
5.2) steel band nitriding increment after the completion of nitriding-decarburizing annealing is controlled according to the soaking Nitrizing Treatment time, soaking is seeped
The method that nitrogen handles the time to control steel band nitriding increment △ N after the completion of nitriding-decarburizing annealing is Formulas I relationship according to the following formula:
Wherein, △ N, steel band nitriding increment, unit, ppm；
T, Nitrizing Treatment time, unit, s；
D, thickness of strips, unit, mm.
5.3) it is warming up to soaking between 820~860 DEG C and carries out decarburizing annealing processing, decarburizing annealing atmosphere is the N of humidification2+H2
Gaseous mixture, wherein steam partial pressure ratio p=pVapor/pHydrogenIt is 0.27~0.35, the decarburizing annealing time is 120~360s.Decarburization is complete
At the rear detection for carrying out steel band carbon content and nitriding increment △ N, carbon content is lower than 5ppm in steel band after control decarburization, controls steel band
Nitriding increment meeting formula II；(185-155 × D)≤△ N≤(198-91 × D) Formula II；
5.4) after completing nitriding-decarburizing annealing by above-mentioned steps, the feature of crystal grain distribution on section is rolled in steel band and is existed
In, steel band upper and lower surface to respectively away from (being rolled away from steel band to section in the average grain size and remaining range in its 1/4 thickness range
Center line is up and down in 1/4 thickness range) the ratio between average grain size n*≤0.76；And III is calculated n* according to the following formula:
Wherein, n2To roll to the crystal grain quantity above and below kernel of section line in 1/4 thickness section；
n1It is steel band upper and lower surface to respectively away from the crystal grain quantity in its 1/4 thickness section.
(6) steel strip surface coats high annealing interleaving agent after decarburizing annealing, then batches；
(7) conventional high temperature annealing is carried out, high annealing purification temperature is between 1150 DEG C~1250 DEG C, steel after annealing
Nitrogen content and sulfur content are not higher than 10ppm in band；
(8) conventional stretching, smooth, painting insulating layer coating and dry solidification annealing are carried out；For use.
Low temperature high magnetic induction grain-oriented silicon steel is prepared according to above-mentioned alloying element composition and technical process and parameter, obtains table 1, table
2 and table 3, wherein the nitriding mode of embodiment 1~11 is at the equal thermal nitridation of low-temperature zone of decarburizing annealing temperature-rise period of the present invention
Reason；The nitriding mode of comparative example 1~11 is Nitrizing Treatment after traditional decarburizing annealing；
The element of each embodiment of table 1 and comparative example composition
The technological parameter list of each embodiment of table 2 and comparative example
The material parameter and product of each embodiment of table 3 and comparative example are magnetic
By above-mentioned table 1, table 2 and table 3 it is found that using bringing-up section low temperature nitridation process phase and traditional decarburization nitriding of the invention
Technique is compared, and reaches identical nitrogen increased amount △ N using identical nitriding time, and the tolerance of nitriding medium saves 5.7%~64.5%,
Product surface adhesion reaches B grades or more.Product magnetic strength is not less than 1.914T, compared to comparative example product iron loss P17/50At least
Reduce 4.8% or more.
Low temperature high magnetic induction grain-oriented silicon steel is prepared according to above-mentioned alloying element composition and technical process and parameter, obtains table 4, table
5 and table 6, wherein embodiment 12~17 is according to above-mentioned gold element composition and technical process and parameter, and comparative example 12~17 is not
Within the above range.
The element of each embodiment of table 4 and comparative example composition
The technological parameter list of each embodiment of table 5 and comparative example
The material parameter and product of 6 embodiment of table and comparative example are magnetic
Wherein, the adhesion classification standard in above table is determined according to GB/T2522-2007.
By above-mentioned table 4, table 5 and table 6 it is found that only working as nitridation process and decarbonization process this application claims in range, produce
Product magnetic property is just preferable, other than the application protection scope, even if using nitriding-decarbonization process, product magnetic property or table
Face adhesion quality will receive influence.
Above embodiments are only best citing, rather than a limitation of the embodiments of the present invention.Except above-described embodiment
Outside, there are also other embodiments by the present invention.All technical solutions formed using equivalent substitution or equivalent transformation, all fall within the present invention
It is required that protection scope.
Claims (10)
1. a kind of process for preparing low temperature high magnetic induction grain-oriented silicon steel, it includes being casting continuously to form base, slab heating, hot rolling, normalizing
Annealing, cold rolling, continuous nitriding and decarburizing annealing, surface coats, batches, high annealing, stretching, it is smooth, apply insulating layer coating and dry
Dry solidification annealing；
Wherein, the continuous nitriding and decarburization annealing process specifically include following process:
1) cold-reduced sheet is warming up to soaking between 500~670 DEG C and carries out Nitrizing Treatment, nitriding atmosphere NH3+N2+H2Mixing
Gas；
2) steel band nitriding increment △ N after the completion of nitriding-decarburizing annealing is controlled according to the soaking Nitrizing Treatment time, the steel band seeps
Nitrogen increment △ N meets such as following formula I relationship:
Wherein, △ N, steel band nitriding increment, unit, ppm；
T, Nitrizing Treatment time, unit, s；
D, thickness of strips, unit, mm；
3) it is warming up to soaking between 820~860 DEG C and carries out decarburizing annealing processing, the decarburizing annealing time is 120~360s, decarburization
Steel band carbon content and nitriding increment △ N are detected after the completion, and carbon content is lower than 5ppm in steel band after control decarburization, controls steel band nitriding
Increment △ N meets such as Formula Il relationship:
(185-155 × D)≤△ N≤(198-91 × D) Formula II；
4) after nitriding to be done and decarburization annealing process, steel band rolls the grain Distribution on section and is, steel band upper and lower surface arrives
Respectively roll away from the average grain size in its 1/4 thickness section and away from steel band to the crystalline substance above and below kernel of section line in 1/4 thickness section
The ratio between grain average-size n*≤0.76；And ratio n* meets following formula III relationship:
Wherein, n2To roll to the crystal grain quantity above and below kernel of section line in 1/4 thickness section；
n1It is steel band upper and lower surface to respectively away from the crystal grain quantity in its 1/4 thickness section.
2. preparing the process of low temperature high magnetic induction grain-oriented silicon steel according to claim 1, it is characterised in that: in step 1),
The NH3Volumn concentration A meet following formula IV relationship:
A=0.165 × 10-6×T2-0.962×10-4× T+0.055 formula IV；
Wherein, T be Nitrizing Treatment temperature, unit, DEG C.
3. preparing the process of low temperature high magnetic induction grain-oriented silicon steel according to claim 1, it is characterised in that: in step 1),
The N2With H2Volume ratio be 1:3.
4. preparing the process of low temperature high magnetic induction grain-oriented silicon steel according to claim 1, it is characterised in that: in step 3),
Decarburizing annealing atmosphere is the N of humidification2+H2Gaseous mixture, wherein steam partial pressure ratio p=pVapor/pHydrogenIt is 0.27~0.35.
5. preparing the process of low temperature high magnetic induction grain-oriented silicon steel described according to claim 1~any one of 4, feature exists
Including following component in terms of: the high magnetic induction grain-oriented silicon steel is by mass percent；
C:0.035%~0.060%, Si:2.55~3.55%, Als:0.0100~0.0350%, Mn:0.03~0.2%, S:
0.0020~0.0100%, N:0.0040~0.0100%, Cu < 0.07%, Cr:0.03~0.2%, remaining is Fe and can not
Avoid field trash.
6. preparing the process of low temperature high magnetic induction grain-oriented silicon steel according to claim 5, it is characterised in that: the high magnetic strength
Orientation silicon steel by mass percent be in terms of including following component；
C:0.035%~0.060%, Si:3.0~3.3%, Als:0.0100~0.0350%, Mn:0.085~0.095%,
S:0.0020~0.0100%, N:0.0062~0.0086%, Cu < 0.04%, Cr:0.03~0.16%, remaining is for Fe and not
It can avoid field trash.
7. preparing the process of low temperature high magnetic induction grain-oriented silicon steel described according to claim 1~any one of 4, feature exists
In: the slab heating process includes 1100~1250 DEG C of heating temperature of control.
8. preparing the process of low temperature high magnetic induction grain-oriented silicon steel described according to claim 1~any one of 4, feature exists
In: the hot rolling technology includes conventional is rolled into a thickness of the hot rolled coil of 1.5~3.8mm specification.
9. preparing the process of low temperature high magnetic induction grain-oriented silicon steel described according to claim 1~any one of 4, feature exists
In: the cold-rolling process includes that the finished product no more than 0.30mm thickness is cold-rolled to according to 87~92% reduction ratio.
10. preparing the process of low temperature high magnetic induction grain-oriented silicon steel, feature described according to claim 1~any one of 4
Be: the high annealing includes control purification temperature between 1150 DEG C~1250 DEG C, nitrogen content in steel band after annealing
10ppm is not higher than with sulfur content.
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| CN114045385A (en) * | 2021-09-30 | 2022-02-15 | 武汉钢铁有限公司 | Method for improving adhesiveness of low-temperature high-magnetic-induction oriented silicon steel |
| CN116162771A (en) * | 2023-04-25 | 2023-05-26 | 首钢智新迁安电磁材料有限公司 | Method, device and equipment for improving capture precision of secondary recrystallization of oriented silicon steel |
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