CN107245564A - A kind of control method of non-orientation silicon steel internal oxidation layer - Google Patents
A kind of control method of non-orientation silicon steel internal oxidation layer Download PDFInfo
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- CN107245564A CN107245564A CN201710464391.6A CN201710464391A CN107245564A CN 107245564 A CN107245564 A CN 107245564A CN 201710464391 A CN201710464391 A CN 201710464391A CN 107245564 A CN107245564 A CN 107245564A
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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
- 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
-
- 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
-
- 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
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
- C21D1/76—Adjusting the composition of the atmosphere
-
- 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
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- 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
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
Abstract
A kind of control method of non-orientation silicon steel internal oxidation layer：Conventional converter smelting, RH application of vacuum is casting continuously to form base；Conventional heating strand hot rolling, normalizing treatment, pickling and once cold rolling are to finished product thickness；Finished products：Control heating ramp rate is not less than 50 DEG C/s, and controls：The intrinsic standoff ratio of the intrinsic standoff ratio of vapor and hydrogen in annealing heating section atmosphere, annealing soak section vapor and hydrogen.The present invention by control continuous annealing furnace bringing-up section the rate of heat addition, annealing heating section atmosphere in vapor and hydrogen intrinsic standoff ratio in P (H2O)/P(H2), and annealing soak section vapor and hydrogen intrinsic standoff ratio, so as to realize internal oxidation layer thickness below 1 μm, reduce its adverse effect to magnetic history.
Description
Technical field
The present invention relates to a kind of method for producing non-oriented silicon steel, particularly belong in a kind of non-orientation silicon steel production on steel plate
Internal oxidation layer thickness control method.
Background technology
Non-orientation silicon steel is after cold rolling at least through a heat-treatment of annealing, the purpose of full-technique non-oriented annealing process of silicon steel
It is to make steel plate recrystallization, promotes crystal grain to grow up and be roughened, eliminates oxygen outside in rolling stress, annealing process and be diffused into steel plate base
With such as Si of the alloying element in silicon steel in body, Al, Mn, Cr etc. is combined in annealing process occurs oxidation reaction, in matrix
Produce layer oxide film, referred to as internal oxidation layer.Internal oxidation layer makes steel plate produce stress field, hinders the movement of neticdomain wall, makes iron
Increase is damaged, magnetic deteriorates.
Atmosphere in continuous annealing furnace, mainly N2、H2And H2The gaseous mixture atmosphere of O three.The oxidation of silicon steel, which is mainly, presses
Carried out according to below equation：
3Fe(s)+2O2(g)=Fe3O4(s) (1)
3Fe(s)+4H2O(g)=Fe3O4(s)+4H2(g) (2)
It is well known that intrinsic standoff ratio P (H2O)/P (H2) of vapor and hydrogen directly determines reaction in continuous annealing furnace atmosphere
Travel direction and degree.For the control of the intrinsic standoff ratio of vapor and hydrogen in continuous annealing furnace atmosphere, to reduce internal oxidition
Thickness degree, reduction makes steel plate produce stress field by internal oxidation layer, increases the movement of neticdomain wall, reduces iron loss, and magnetic property is improved.
In the art, people are in order to solve the increase of internal oxidation layer Thickness ness, the magnetic to orientation free silicon steel plate
Energy adverse effect, has carried out substantial amounts of experimental study and has taken measures, e.g., through retrieval：Japanese patent application publication No.
For JP2011-241416 A document, non-oriented magnetic steel sheet and its manufacture method that a kind of high frequency has excellent core loss are disclosed.
The document is proposed according to P (H2O)/P(H2)≤0.015 × (Cr+Si+Al) controls the intrinsic standoff ratio of vapor and hydrogen, alloying element
Si, Al, Cr content are higher, P (H2O)/P(H2) upper control limit it is higher, also imply that steam vapour amount is bigger or amounts of hydrogen
Lower, oxidisability in atmosphere is improved, and reproducibility weakens, and actually alloy content higher particularly Al content is higher is easy to
Aoxidize, the intrinsic standoff ratio control of the patent is significant adverse to the control of internal oxidation layer.In addition, the patent is taken into consideration only according to conjunction
Gold content adjustment P (H2O)/P(H2), and for the P (H of whole annealing furnace2O)/P(H2) all identical, do not account for each bringing-up section
With the specific P (H of soaking zone2O)/P(H2) control, in addition annealing heating speed in actual annealing process, the heating-up time of bringing-up section
Can all influence be produced on the thickness of oxide layer, with speed, the soaking temperature of soaking zone for different stove area P (H2O)/P(H2)
Control is also not quite similar.
There is provided one kind for the document that China Patent Publication No. is the A of CN 101812571《At electrical hot-rolled strip steel normalizing
The method that internal oxidation layer is prevented in reason》.The document is by the control to normalizing process, to reduce and eliminate hot-strip normalizing
When the internal oxidation layer that produces, i.e., furnace hearth roller salamander during final annealing is eliminated from source.The document is mainly for hot-strip
Surface cord problem, propose in non-oxidation furnace using straight fire heating, air-fuel ratio, dew point and oxygen content in control stove, gas in stove
Atmosphere is pure N2.Although the internal oxidation layer generation during control normalizing plays one to the finished product internal oxidation layer control after cold rolled annealed
Determine advantageous effect, but the internal oxidation layer control after finished products can not be played a decisive role.
The content of the invention
It is an object of the invention to overcome deficiency present in above-mentioned document to pass through there is provided one kind while controlling continuous annealing
Stove heat section the rate of heat addition, annealing heating section atmosphere in vapor and hydrogen intrinsic standoff ratio in P (H2O)/P(H2)≤0.10,
And the intrinsic standoff ratio of annealing soak section vapor and hydrogen, to realize internal oxidation layer thickness in the non-orientation silicon steel below 1 μm
The control method of oxide layer.
Realize the measure of above-mentioned purpose：
A kind of control method of non-orientation silicon steel internal oxidation layer, its step：
1）Conventional converter smelting, RH application of vacuum is casting continuously to form base；
2) conventional heating strand hot rolling, normalizing treatment, pickling and once cold rolling are to finished product thickness；
3) finished products：Wherein：
Control heating ramp rate is not less than 50 DEG C/s, and annealing process uses N2、H2And vapor mixed gas is carried out, and control
System：The intrinsic standoff ratio of vapor and hydrogen is in P (H in annealing heating section atmosphere2O)/P(H2) ≤0.10；
Intrinsic standoff ratio P (the H of annealing soak section vapor and hydrogen2O)/P(H2) meet below equation：
In formula：T-be soaking zone soaking temperature, unit for DEG C.
Further：Heating ramp rate is not less than 80 DEG C/s.
Further：The intrinsic standoff ratio of vapor and hydrogen is in P (H in annealing heating section atmosphere2O)/P(H2) 0.04 ~
0.08。
Further：Intrinsic standoff ratio P (the H of vapor and hydrogen in annealing soak section atmosphere2O)/P(H2) ≤0.25。
It is：Its composition and weight percent content for being applied to non-orientation silicon steel exist：C:≤ 0.003%, N:≤
0.003%, S:≤ 0.002%, P:≤ 0.05%, Si:0.5 ~ 3.5%, Al are no more than 1.5%, Mn:0.2~2.0%.
The mechanism of main technique and effect in the present invention
It is due to iron by the internal oxidation layer thickness control of orientation free silicon steel plate below 1.0 μm why in the art
Oxide with aluminium is all namagnetic substance, and according to skin effect principle, the magnetic flux density close to material surface is concentrated, therefore is leaned on
The internal oxidation layer of nearly material surface directly results in surface magnetic domain movement difficulty, iron loss increase.After oxidated layer thickness is more than 1.0 μm
High-frequency loss deteriorates particularly evident.
Why the present invention controls heating ramp rate to be not less than 50 DEG C/s, and control annealing heating section atmosphere reclaimed water is steamed
The intrinsic standoff ratio of vapour and hydrogen is in P (H2O)/P(H2The problem of)≤0.10：
The applicant shows that the formation of the internal oxidation layer of orientation free silicon steel plate and oxygen gesture are close in the result through substantial amounts of experimental study
Cut is closed, and oxygen gesture is mainly by P (H2O)/P(H2) influence.And it is required for hypoxemia in heat temperature raising stage and soaking holding stage
Gesture, especially in the heat temperature raising stage with greater need for hypoxemia gesture, because hypoxemia potential energy prevents the quick formation of internal oxidation layer；In addition,
Alloying element is diffused to the surface in heating process, but in the oxygen haptoreaction spread in interface and atmosphere to matrix
It is the important stage of the formation of internal oxidation layer, has literature research to show that the temperature of above-mentioned oxidation reaction often improves 10 DEG C, reaction speed
Degree brings up to original 2-4 times, therefore in order to reduce the abundant catalytic machine of iron and other alloys and oxygen in the heating period
Rate, therefore heating ramp rate is set in and is not less than 50 DEG C/s by the present invention, to reduce the reaction time, while the heat temperature raising stage is
The initial and important stage of internal oxidation layer formation, but it is also in unstable state, it is now strict to control P (H2O)/P(H2), make
Internal oxidation layer is difficult to stable formation or is reduced rapidly, is that good basis is laid in the internal oxidation layer control of follow-up soaking zone.
The present invention why set up annealing soak section atmosphere in vapor and hydrogen intrinsic standoff ratio in P (H2O)/P(H2)
Mathematical modeling, i.e. P (H2O)/P(H2)≤1-T/1200 be because：
According to reaction equation（1）With（2）, understand that the molar Gibbs free energy of chemical reaction is positive and negative by Material Thermodynamics relative theory
Direction and the speed of reaction, speed and direction, the P (O of reaction are directly determined with size2), P (H2O)/P(H2) closely related, and P
(O2), P (H2O)/P(H2) depending on environment temperature during reaction, temperature adjustment P (H during especially in accordance with soaking2O)/P(H2),
Reaction can just be controlled（2）Direction, because the annealing soak stage is finished product recrystallization and stage for growing up of crystal grain, it must be protected
The enough temperature levels of card just can guarantee that the properties of finished product, therefore the H in can only reducing air in the soaking stage2O and combustion
The H of generation after burning2The reaction of O and steel plate reduces its reaction speed, so as to finally control the thickness of internal oxidation layer in finished product.
Shown by lot of experimental data and the observation of internal oxidation layer result：Annealing soak temperature is higher, iron and other alloys,
With H2O reaction is more violent, now in order to reduce reaction speed or even control reaction reversely, it is necessary to reduce water vapor partial pressure, increases H2
Partial pressure, that is, reduce P (H2O)/P(H2) value, it can effectively reduce internal oxidation layer thickness.
And annealing soak temperature is lower, iron and other alloys and H2O reaction is slower, now can suitably reduce H2Point
Pressure, reduces production cost, that is, properly increases P (H2O)/P(H2) value, now internal oxidation layer thickness also will not substantially rise.By testing
Data can obtain drawing a conclusion
When meeting formula
When, it can effectively control soaking zone internal oxidation layer thickness.
The present invention compared with prior art, by control continuous annealing furnace bringing-up section the rate of heat addition, annealing heating section gas
The intrinsic standoff ratio of vapor and hydrogen is in P (H in atmosphere2O)/P(H2)≤0.10, and annealing soak section vapor and hydrogen partial pressure
Than so that internal oxidation layer thickness is realized below 1 μm, so as to reduce its adverse effect to magnetic history.
Brief description of the drawings
The internal oxidation layer distribution map for the non-orientation silicon steel steel plate that Fig. 1 is produced for the present invention.
Embodiment
The present invention is described in detail below：
Table 1 is technique value and the internal oxidation layer thickness list of the embodiment of the present invention 1 and comparative example；
Table 2 is technique value and the internal oxidation layer thickness list of the embodiment of the present invention 2 and comparative example；
Table 3 is technique value and the internal oxidation layer thickness list of the embodiment of the present invention 3 and comparative example；
Table 4 is technique value and the internal oxidation layer thickness list of the embodiment of the present invention 4 and comparative example；
Table 5 is technique value and the internal oxidation layer thickness list of the embodiment of the present invention 5 and comparative example；
Various embodiments of the present invention are produced according to following steps：
1）Conventional converter smelting, RH application of vacuum is casting continuously to form base；
2) conventional heating strand hot rolling, normalizing treatment, pickling and once cold rolling are to finished product thickness；
3) finished products：Wherein：
Control heating ramp rate is not less than 50 DEG C/s, and annealing process uses N2、H2And vapor mixed gas is carried out, and control
System：The intrinsic standoff ratio of vapor and hydrogen is in P (H in annealing heating section atmosphere2O)/P(H2) ≤0.10；
Intrinsic standoff ratio P (the H of annealing soak section vapor and hydrogen2O)/P(H2) meet below equation：
In formula：T-be soaking zone soaking temperature, unit for DEG C.
Embodiment 1
The present embodiment is through using converter smelting, and RH application of vacuum is casting continuously to form after base, and strand composition is C:0.0015%, Si:2.5%,
Al:1.4%, Mn:1.5%, P:0.02%, S:0.0008%, N:0.0014%；Carried out after strand hot rolling after normalizing treatment and pickling, warp
Once cold rolling is rolling to thickness to 0.50mm；Through carrying out finished products, annealing relevant parameter and correspondence internal oxidation layer to cold-reduced sheet
Thickness is shown in Table 1：
Table 1
From table 1, when using present invention process, internal oxidation layer thickness can be controlled below 1 μm.
Embodiment 2
The present embodiment is through using converter smelting, and RH application of vacuum is casting continuously to form after base, and strand composition is C:0.0018%, Si:1.5%,
Al:0.4%, Mn:0.5%, P:0.015%, S:0.0013%, N:0.0019%；Carried out after strand hot rolling after normalizing treatment and pickling,
Thickness is rolling to 0.35mm through once cold rolling；Through carrying out finished products, annealing relevant parameter and correspondence internal oxidition to cold-reduced sheet
Thickness degree is shown in Table 2：
Table 2
From table 2, when using present invention process, internal oxidation layer thickness can be controlled below 1 μm.
Embodiment 3
The present embodiment is through using converter smelting, and RH application of vacuum is casting continuously to form after base, and strand composition is C:0.0021%, Si:0.8%,
Al:0.6%, Mn:0.2%, P:0.018%, S:0.0017%, N:0.0021%；Carried out after strand hot rolling after normalizing treatment and pickling,
Thickness is rolling to 0.30mm through once cold rolling；Through carrying out finished products, annealing relevant parameter and correspondence internal oxidition to cold-reduced sheet
Thickness degree is shown in Table 3：
Table 3
From table 3, when using technique 5- 8, internal oxidation layer thickness can be controlled below 1 μm, especially with preferred work
During skill 7,8, internal oxidation layer thickness is smaller.
Embodiment 4
The present embodiment is through using converter smelting, and RH application of vacuum is casting continuously to form after base, and strand composition is C:0.0024%, Si:2.6%,
Al:0.9%, Mn:0.35%, P:0.028%, S:0.0013%, N:0.0011%；Carried out after strand hot rolling after normalizing treatment and pickling,
Thickness is rolling to 0.27mm through once cold rolling；Through carrying out finished products, annealing relevant parameter and correspondence internal oxidition to cold-reduced sheet
Thickness degree is shown in Table 4：
Table 4
From table 4, when using present invention process, internal oxidation layer thickness can be controlled below 1 μm.
Embodiment 5
The present embodiment is through using converter smelting, and RH application of vacuum is casting continuously to form after base, and strand composition is C:0.0022%, Si:3.1%,
Al:1.2%, Mn:0.52%, P:0.024%, S:0.0012%, N:0.0016%；Carried out after strand hot rolling after normalizing treatment and pickling,
Thickness is rolling to 0.20mm through once cold rolling；Through carrying out finished products, annealing relevant parameter and correspondence internal oxidition to cold-reduced sheet
Thickness degree is shown in Table 5：
Table 5
From table 5, when using present invention process, internal oxidation layer thickness can be controlled below 1 μm.
From table 1- tables 5, whenever heating ramp rate is less than 50 DEG C/s or bringing-up section P (H2O)/P(H2) be more than 0.1 when
Or soaking zone P (H2O)/P(H2) be more than 1-T/1200 when, can cause steel plate internal oxidation layer thickness be more than 1 μm, it is impossible to realize
The purpose of the present invention；Only meeting heating ramp rate is not less than 50 DEG C/s, bringing-up section P (H simultaneously2O)/P(H2) it is less than 0.1, move back
Intrinsic standoff ratio P (the H of fiery soaking zone vapor and hydrogen2O)/P(H2) formula, i.e.,, steel could be controlled
The thickness of plate internal oxidation layer is less than 1 μm, could improve the magnetic property of orientation free silicon steel plate.
Above-described embodiment is only most preferably to enumerate, and is not the restriction to embodiments of the present invention.
Claims (5)
1. a kind of control method of non-orientation silicon steel internal oxidation layer, its step：
1）Conventional converter smelting, RH application of vacuum is casting continuously to form base；
2) conventional heating strand hot rolling, normalizing treatment, pickling and once cold rolling are to finished product thickness；
3) finished products：Wherein：
Control heating ramp rate is not less than 50 DEG C/s, and annealing process uses N2、H2And vapor mixed gas is carried out, and control：
The intrinsic standoff ratio of vapor and hydrogen is in P (H in annealing heating section atmosphere2O)/P(H2) ≤0.10；
Intrinsic standoff ratio P (the H of annealing soak section vapor and hydrogen2O)/P(H2) meet below equation：
In formula：T-be soaking zone soaking temperature, unit for DEG C.
2. a kind of control method of non-orientation silicon steel internal oxidation layer as claimed in claim 1, it is characterised in that：Heat temperature raising speed
Rate is not less than 80 DEG C/s.
3. a kind of control method of non-orientation silicon steel internal oxidation layer as claimed in claim 1, it is characterised in that：Annealing heating section
The intrinsic standoff ratio of vapor and hydrogen is in P (H in atmosphere2O)/P(H2) 0.04 ~ 0.08.
4. a kind of control method of non-orientation silicon steel internal oxidation layer as claimed in claim 1, it is characterised in that：Annealing soak section
Intrinsic standoff ratio P (the H of vapor and hydrogen in atmosphere2O)/P(H2) ≤0.25。
5. a kind of control method of non-orientation silicon steel internal oxidation layer as claimed in claim 1, it is characterised in that：It is applied to nothing
The composition and weight percent content of orientation silicon steel exist：C:≤ 0.003%, N:≤ 0.003%, S:≤ 0.002%, P:≤
0.05%, Si:0.5 ~ 3.5%, Al are no more than 1.5%, Mn:0.2~2.0%.
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| WO2020111006A1 (en) * | 2018-11-26 | 2020-06-04 | Ｊｆｅスチール株式会社 | Manufacturing method for non-oriented magnetic steel sheet |
| JP2022509865A (en) * | 2018-11-30 | 2022-01-24 | ポスコ | Electrical steel sheet and its manufacturing method |
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| CN107245564B (en) | 2019-01-25 |
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