CN110283981A - A kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content - Google Patents
A kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content Download PDFInfo
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- CN110283981A CN110283981A CN201910670784.1A CN201910670784A CN110283981A CN 110283981 A CN110283981 A CN 110283981A CN 201910670784 A CN201910670784 A CN 201910670784A CN 110283981 A CN110283981 A CN 110283981A
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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
- 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
Abstract
A kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content: it through conventional converter smelting, is vacuum-treated and is casting continuously to form base;To slab conventional heating;Disposable cold rolling is carried out after pickling;Annealing;High annealing;Stretching and leveling, coating insulating coating and finished product finishing packaging, for use.The present invention can not change existing production technology, steel grades, and the nitriding time condition during decarburizing annealing, and under the premise of nitriding amount is not less than 200PPm, it is increased to the oxygen content of low temperature HiB at least not less than 680PPm, and then improve magnetic property to not less than 1.91T by existing 1.905T, and it is easy to operate, easily implement.
Description
Technical field
The present invention relates to a kind of production methods of orientation silicon steel, definitely belong to a kind of life of high magnetic strength nitriding orientation silicon steel
In particular a kind of production method for improving low temperature high magnetic induction grain-oriented silicon steel oxygen content of production method.
Background technique
With the development trend of national grid cause, energy-saving type transformer more than extra-high die mould, S13 type grade becomes
Mainstream can make the application range of low temperature high magnetic induction grain-oriented silicon steel (low temperature HiB) and market can be higher to its magnetic demand.Due to
Low temperature HiB is inhibitor to be obtained by way of the nitriding day after tomorrow, therefore improving magnetic critical process is that it is first after cold rolling
Nitriding and oxidation in annealing process.How in the range of specific nitriding amount, the oxygen content for improving low temperature HiB is to solve to mention
The key of high magnetic characteristics.It is also those skilled in the art of the present technique's problem encountered.
Method is mainly the following currently, improving low temperature HiB oxygen content and obtaining nitriding amount >=200ppm:
1, by changing nitriding temperature, nitriding efficiency is promoted within the unit time and increases nitriding amount;
2, change different nitriding modes, such as spray regime promotes nitriding efficiency within the unit time and increases nitriding amount;
3, by the content of oxyphie ingredient such as Cr, Sn element in change steel, its is made to be easier to aoxidize in decarburizing annealing,
To increase oxygen content in steel.
In three of the above mode, from the point of view of the result of production practices, first and the third mode, it is required to low temperature HiB
Ingredient design and first annealing technique carry out big change, and for mature manufacturing enterprise, risk of failure is relatively high for this.
The second way then needs investment in fixed assets, the scrap build etc. of hardness, and can only solve low temperature HiB nitriding
Amount >=200ppm problem, raising problem for oxygen content cannot simultaneously solve.
The prior art introduces ground very much, but in practice generally directed to low temperature HiB acquisition >=200ppm method, to obtain excellent
The low temperature HiB steel of good magnetism, under conditions of nitriding amount >=200ppm, it is necessary to also pay close attention to oxygen content.Low temperature HiB steel magnetic strength with
Oxygen content increase and increases, cardinal principle be oxygen content raising, the bottom of low temperature HiB steel formed completely, nitriding amount >=
200ppm is conducive to nitride inclusion and is formed, and the development of Gauss component texture is more perfect, to improve magnetic strength.The present invention be exactly in order to
Both >=nitriding the amount of 200ppm was obtained, improves oxygen content again, so that it is magnetic to improve low temperature HiB steel.
The prior art also has oxygen content to high magnetic strength silicon steel to have to be paid close attention to, but nitriding amount, oxygen content are lower,
As through retrieving:
Chinese Patent Application No. is the document of CN201110415831.1, discloses a kind of " high magnetic induction grain-oriented silicon steel strip infiltration
Nitrogen processing method ".The document describes the nitriding method of high magnetic induction grain-oriented silicon steel, can only but obtain nitriding amount according to the document
Maintain 120ppm~180ppm;Oxygen content maintains 400ppm~450ppm, and the ability for improving low temperature HiB magnetism is limited.Cause
Do not reach the >=range of 200ppm for the nitrogen content of the patent, nitride inclusion component is on the low side, and effective restraint is insufficient, Gauss
Component texture ateliosis, magnetic strength are difficult to improve.
Most of performances to improve high magnetic strength silicon steel are still to be improved its magnetic property by improving the nitriding amount of steel
, and the oxygen content of steel is not paid close attention to, as through retrieving:
Chinese Patent Application No. is the document of CN201310348135.2, is disclosed " a kind of to utilize Nano-composite Electrodeposition
Method of the technology to orientation silicon steel nitriding ", the document can significantly improve low temperature HiB nitriding amount to 220ppm~260ppm.It should
Increase of the document due to being concerned only with nitriding amount, although i.e. nitriding amount has reached 220ppm~260ppm, due to not with pass
Infuse oxygen content increase, the oxygen content which obtains be 250ppm~450ppm, oxygen content deficiency cause nitriding amount >=
Under conditions of 200ppm, the formation of low temperature HiB steel bottom is not fine and close, even if nitriding amount is very high, but nitride inclusion forming process
In, nitrogen, which can be overflowed by unsound bottom gap to steel strip surface, escapes, and Gauss component texture inside steel band is caused to be developed not
Completely, so being still unable to satisfy the requirement of high magnetic strength silicon-steel magnetic energy further increased.
Chinese Patent Application No. is the document of CN201420326832.8, discloses a kind of " orientation silicon steel nitriding spray
Beam ", although document nitriding amount has reached 200ppm~240ppm, it needs to install special equipment, causes to invest and produce
Increased costs, and the also not increase with concern oxygen content, so being still unable to satisfy further mentioning for high magnetic strength silicon-steel magnetic energy
High requirement.
Summary of the invention
The invention reside in the shortcomings of the prior art is overcome, provide it is a kind of do not change existing production technology, steel grade at
Point and first annealing during nitriding time condition, and nitriding amount be not less than 200PPm under the premise of, make low temperature HiB
Oxygen content be at least increased to not less than 680PPm, and then improve magnetic property to not less than 1.91T by existing 1.905T
The production method of low temperature high magnetic induction grain-oriented silicon steel oxygen content.
The measure of existing above-mentioned purpose:
A kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content, step:
1) through conventional converter smelting, be vacuum-treated and be casting continuously to form low temperature HiB steel steel billet;The percentage composition content of slab
Are as follows: Si content is 2.8%~3.3%, and C content is 400ppm~700ppm, and N content is in 65ppm~85ppm, Als content
240ppm~305ppm, remaining is Fe and other impurities element.
2) warp is to slab conventional heating, and carries out conventional breaking down finish rolling and batch, and steel plate thickness is 2.3 ± 0.1mm;
3) disposable cold rolling is carried out after pickling;
4) annealing process is carried out:
A, it is incremented by first, in accordance with intrinsic standoff ratio in furnace and carries out decarburizing annealing with the mode combined of successively decreasing, annealing temperature control exists
820 DEG C~860 DEG C, furnace atmosphere is the nitrogen and hydrogen mixture of wet type, and wherein hydrogen volume accounting is 38%~45%;Annealing time
For 140s;
Therebetween: in the time of the preceding 100s of decarburizing annealing, controlling the P in annealing furnaceH2O/PH2Intrinsic standoff ratio are as follows: basis point
Plus incremental intrinsic standoff ratio on the basis of pressure ratio;The basis intrinsic standoff ratio is to appoint the value taken in 0.4~0.6;It is described to pass
The intrinsic standoff ratio of increasing refers to: every annealing 25s increases intrinsic standoff ratio 0.05;
It is greater than this period of 100s to 140s in annealing time, intrinsic standoff ratio uses decreasing fashion in annealing furnace, i.e., often moves back
Fiery 10s reduces intrinsic standoff ratio 0.01;
B, after decarburizing annealing, into the Nitrizing Treatment stage, the atmosphere in annealing furnace is still wet type nitrogen and hydrogen mixture;It seeps
For nitrogen temperature at 850 DEG C~900 DEG C, nitriding time is conventional 20s~45s;The ammonia flow being passed through is in 30~40m3/h;Nitriding
Intrinsic standoff ratio P in stage furnaceH2O/PH2The height of the nitrogen content of intrinsic standoff ratio and steel grade setting 0.2~0.4, and in furnace is at positive
Pass relationship;
5) conventional to carry out high annealing;
6) stretching and leveling, coating insulating coating and finished product finishing packaging are carried out, for use.
Preferably: basic intrinsic standoff ratio appoints the value taken in 0.07~0.15.
The present invention controls the P in annealing furnace why before decarburizing annealing in the time of 100sH2O/PH2Intrinsic standoff ratio are as follows:
Plus incremental intrinsic standoff ratio on the basis of basic intrinsic standoff ratio;The basis intrinsic standoff ratio is to appoint one taken in 0.4~0.6
Value;The incremental intrinsic standoff ratio refers to: every annealing 25s increases intrinsic standoff ratio 0.05.Be due in decarburizing annealing leading portion, especially before
Intrinsic standoff ratio P in 25s, if to obtain more multi-component oxygen, in annealing furnaceH2O/PH2It must control 0.4 or more;Later according to
Every annealing 25s increases intrinsic standoff ratio 0.05, is due to the progress with decarburizing annealing, if being continuously maintained at P after 25SH2O/PH2?
Within 0.4, SiO is caused2Component abnormal increase and it is roughened, forms fine and close oxide layer on steel band time surface layer, decarburization can be hindered.
It is exactly to obtain enough SiO that gradient, which increases intrinsic standoff ratio,2Balance is obtained between decarburization.
When annealing time is greater than 100s to 140s, intrinsic standoff ratio uses decreasing fashion, i.e., every annealing 10s reduces intrinsic standoff ratio
0.01;, be due to be greater than 100s after, the decarbonizing process in low temperature HiB in steel band is basically completed major part, in decarbonizing process,
Carbon reacts production CO and H with vapor in steel band2, it is reducing atmosphere.When decarburization latter end, 100s to 140s, decarburization is produced
Raw reducing atmosphere has weakened, and reduces the P in furnace with having gradientH2O/PH2It can prevent peroxidating atmosphere from causing belt steel surface
Oxidation, subsequent obstruction nitriding.
Why the intrinsic standoff ratio in nitriding stage furnace is controlled in P the present inventionH2O/PH2In any value of 0.2~0.4 range,
It is in nitriding process, suitably to use partial pressure P due to finding by practiceH2O/PH2Moisture mixed with ammonia after in strip table
Face forms the complex compound of FeO and amino, can effectively facilitate nitriding, improves nitriding efficiency.
The present invention does not change furnace equipment structure on the basis of existing low temperature HiB decarburizing annealing furnace apparatus and process conditions,
And make nitriding amount not less than 200PPm, it realizes that oxygen content increases by process optimization, realizes that low temperature HiB is magnetic more preferable.It is main former
Reason are as follows: by adjusting the atmosphere P in first annealing different time stageH2O/PH2Intrinsic standoff ratio, so that oxygen content is high and is that bottom is formed
Reactant SiO2Component increases, and then improves low temperature HiB oxygen content.It is original by the nitriding phasic change in decarburizing annealing
Dry gas atmosphere nitriding environments realize PH2O/PH2Low intrinsic standoff ratio wet gas environments nitriding improves nitriding efficiency.In nitriding mode, nitriding
Between, nitriding temperature it is constant under conditions of guarantee that nitriding amount is not less than 200PPm.
Compared with prior art, the present invention can not change existing production technology, steel grades and decarburizing annealing process
In nitriding time condition, and nitriding amount be not less than 200PPm under the premise of, be increased to the oxygen content of low temperature HiB at least not
It lower than 680PPm, and then improves magnetic property to not less than 1.91T by existing 1.905T, and easy to operate, easily implements.
Specific embodiment
The present invention is described in detail below:
Embodiment 1
A kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content, step:
1) through conventional converter smelting, be vacuum-treated and be casting continuously to form low temperature HiB steel steel billet;The percentage composition content of slab
Are as follows: Si content is 2.85%, C content 421ppm, and for N content in 68ppm, Als content is 260ppm, remaining for Fe and other
Impurity element;
2) warp is to slab conventional heating, and carries out conventional breaking down finish rolling and batch, and steel plate thickness is 2.3 ± 0.1mm;
3) disposable cold rolling is carried out after pickling, is rolled to a thickness of 0.27mm;
4) annealing process is carried out:
A, it is incremented by first, in accordance with intrinsic standoff ratio in furnace and carries out decarburizing annealing with the mode combined of successively decreasing, annealing temperature control exists
835 DEG C, furnace atmosphere is the nitrogen and hydrogen mixture of wet type, and wherein hydrogen volume accounting is 39%;Annealing time is 140s;Therebetween:
In the annealing time of 100s, basic intrinsic standoff ratio P is selectedH2O/PH2It is 0.4, and uses incremental manner, i.e., every annealing 25s, which increases, is divided
Pressure ratio 0.05;Intrinsic standoff ratio is 0.6 when to 100s;
It is greater than 100s to 140s time period in annealing time, intrinsic standoff ratio uses decreasing fashion, i.e., every annealing 10s, which is reduced, to be divided
Pressure ratio 0.01;At the end of decarburizing annealing, intrinsic standoff ratio 0.56.
B, after decarburizing annealing, into the Nitrizing Treatment stage, the atmosphere in annealing furnace is still wet type nitrogen and hydrogen mixture;It seeps
For nitrogen temperature at 885 DEG C, nitriding time is conventional 28s;The ammonia flow being passed through is in 33m3/h;Since the N content of setting exists
68ppm, so the intrinsic standoff ratio P in nitriding stage furnaceH2O/PH2It is 0.21;
5) conventional to carry out high annealing;
6) stretching and leveling, coating insulating coating and finished product finishing packaging are carried out, for use.
Through detecting, the oxygen content of the present embodiment is 680PPm, improves 36.2% than existing conventional techniques;Nitriding amount is
200PPm,;Magnetic strength is 1.91T.
Embodiment 2
1) through conventional converter smelting, be vacuum-treated and be casting continuously to form low temperature HiB steel steel billet;The percentage composition content of slab
Are as follows: Si content is 3.02%, C content 550ppm, and for N content in 72ppm, Als content is 275ppm, remaining for Fe and other
Impurity element;
2) warp is to slab conventional heating, and carries out conventional breaking down finish rolling and batch, and steel plate thickness is 2.3 ± 0.1mm;
3) disposable cold rolling is carried out after pickling, is rolled to a thickness of 0.27mm;
4) annealing process is carried out:
A, it is incremented by first, in accordance with intrinsic standoff ratio in furnace and carries out decarburizing annealing with the mode combined of successively decreasing, annealing temperature control exists
828 DEG C, furnace atmosphere is the nitrogen and hydrogen mixture of wet type, and wherein hydrogen volume accounting is 40%;Annealing time is 140s;
Therebetween: in the annealing time of 100s, selecting basic intrinsic standoff ratio PH2O/PH2It is 0.48, and uses incremental manner, i.e.,
Every annealing 25s increases intrinsic standoff ratio 0.05;Intrinsic standoff ratio is 0.68 when to 100s;
It is greater than 100s to 140s time period in annealing time, intrinsic standoff ratio uses decreasing fashion, i.e., every annealing 10s, which is reduced, to be divided
Pressure ratio 0.01;At the end of decarburizing annealing, intrinsic standoff ratio 0.64.
B, after decarburizing annealing, into the Nitrizing Treatment stage, the atmosphere in annealing furnace is still wet type nitrogen and hydrogen mixture;It seeps
For nitrogen temperature at 875 DEG C, nitriding time is conventional 29s;The ammonia flow being passed through is in 35m3/h;Since the N content of setting exists
72ppm, so the intrinsic standoff ratio P in nitriding stage furnaceH2O/PH2It is 0.25;
5) conventional to carry out high annealing;
6) stretching and leveling, coating insulating coating and finished product finishing packaging are carried out, for use.
Through detecting, the oxygen content of the present embodiment is 760PPm, improves 51.2% than existing conventional techniques;Nitriding amount is
225PPm,;Magnetic strength is 1.911T.
Embodiment 3
1) through conventional converter smelting, be vacuum-treated and be casting continuously to form low temperature HiB steel steel billet;The percentage composition content of slab
Are as follows: Si content is 3.2%, C content 624ppm, and for N content in 83ppm, Als content is 298ppm, remaining for Fe and other
Impurity element;
2) warp is to slab conventional heating, and carries out conventional breaking down finish rolling and batch, and steel plate thickness is 2.3 ± 0.1mm;
3) disposable cold rolling is carried out after pickling, is rolled to a thickness of 0.27mm;
4) annealing process is carried out:
A, it is incremented by first, in accordance with intrinsic standoff ratio in furnace and carries out decarburizing annealing with the mode combined of successively decreasing, annealing temperature control exists
845 DEG C, furnace atmosphere is the nitrogen and hydrogen mixture of wet type, and wherein hydrogen volume accounting is 41%;Annealing time is 140s;
Therebetween: in the annealing time of 100s, selecting basic intrinsic standoff ratio PH2O/PH2It is 0.58, and uses incremental manner, i.e.,
Every annealing 25s increases intrinsic standoff ratio 0.05;Intrinsic standoff ratio is 0.78 when to 100s;
It is greater than 100s to 140s time period in annealing time, intrinsic standoff ratio uses decreasing fashion, i.e., every annealing 10s, which is reduced, to be divided
Pressure ratio 0.01;At the end of decarburizing annealing, intrinsic standoff ratio 0.74.
B, after decarburizing annealing, into the Nitrizing Treatment stage, the atmosphere in annealing furnace is still wet type nitrogen and hydrogen mixture;It seeps
For nitrogen temperature at 890 DEG C, nitriding time is conventional 28s;The ammonia flow being passed through is in 38m3/h;Since the N content of setting exists
83ppm, so the intrinsic standoff ratio P in nitriding stage furnaceH2O/PH2It is 0.38;
5) conventional to carry out high annealing;
6) stretching and leveling, coating insulating coating and finished product finishing packaging are carried out, for use.
Through detecting, the oxygen content of the present embodiment is 1050PPm, improves 110% than existing conventional techniques;Nitriding amount is
245PPm,;Magnetic strength is 1.9113T.
Embodiment 4
1) through conventional converter smelting, be vacuum-treated and be casting continuously to form low temperature HiB steel steel billet;The percentage composition content of slab
Are as follows: Si content is 3.11%, C content 606ppm, and for N content in 78ppm, Als content is 289ppm, remaining for Fe and other
Impurity element;
2) warp is to slab conventional heating, and carries out conventional breaking down finish rolling and batch, and steel plate thickness is 2.3 ± 0.1mm;
3) disposable cold rolling is carried out after pickling, is rolled to a thickness of 0.27mm;
4) annealing process is carried out:
A, it is incremented by first, in accordance with intrinsic standoff ratio in furnace and carries out decarburizing annealing with the mode combined of successively decreasing, annealing temperature control exists
857 DEG C, furnace atmosphere is the nitrogen and hydrogen mixture of wet type, and wherein hydrogen volume accounting is 43%;Annealing time is 140s;
Therebetween: in the annealing time of 100s, selecting basic intrinsic standoff ratio PH2O/PH2It is 0.52, and uses incremental manner, i.e.,
Every annealing 25s increases intrinsic standoff ratio 0.05;Intrinsic standoff ratio is 0.72 when to 100s;
It is greater than 100s to 140s time period in annealing time, intrinsic standoff ratio uses decreasing fashion, i.e., every annealing 10s, which is reduced, to be divided
Pressure ratio 0.01;At the end of decarburizing annealing, intrinsic standoff ratio 0.68.
B, after decarburizing annealing, into the Nitrizing Treatment stage, the atmosphere in annealing furnace is still wet type nitrogen and hydrogen mixture;It seeps
For nitrogen temperature at 887 DEG C, nitriding time is conventional 31s;The ammonia flow being passed through is in 13m3/h;Since the N content of setting exists
78ppm, so the intrinsic standoff ratio P in nitriding stage furnaceH2O/PH2It is 0.03;
5) conventional to carry out high annealing;
6) stretching and leveling, coating insulating coating and finished product finishing packaging are carried out, for use.
Through detecting, the oxygen content of the present embodiment is 830PPm, improves 66% than existing conventional techniques;Nitriding amount is
236PPm,;Magnetic strength is 1.912T.
Present embodiment is only the best example, not to the restricted implementation of technical solution of the present invention.
Claims (2)
1. a kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content, step:
1) through conventional converter smelting, be vacuum-treated and be casting continuously to form low temperature HiB steel steel billet;The percentage composition content of slab are as follows: Si
Content is 2.8% ~ 3.3%, and C content is 400ppm ~ 700ppm, N content in 65ppm ~ 85ppm, Als content be 240ppm ~
305ppm, remaining is Fe and other impurities element;
2) warp is to slab conventional heating, and carries out conventional breaking down finish rolling and batch, and steel plate thickness is 2.3 ± 0.1mm;
3) disposable cold rolling is carried out after pickling;
4) annealing process is carried out:
A, it is incremented by first, in accordance with intrinsic standoff ratio in furnace and carries out decarburizing annealing with the mode combined of successively decreasing, annealing temperature is controlled 820
DEG C ~ 860 DEG C, furnace atmosphere is the nitrogen and hydrogen mixture of wet type, and wherein hydrogen volume accounting is 38% ~ 45%;Annealing time is 140s;
Therebetween: in the time of the preceding 100s of decarburizing annealing, controlling the P in annealing furnaceH2O/PH2Intrinsic standoff ratio are as follows: in basic intrinsic standoff ratio
On the basis of plus incremental intrinsic standoff ratio;The basis intrinsic standoff ratio is to appoint the value taken in 0.4 ~ 0.6;Incremental point
Pressure ratio refers to: every annealing 25s increases intrinsic standoff ratio 0.05;
It is greater than this period of 100s to 140s in annealing time, intrinsic standoff ratio uses decreasing fashion, i.e., every annealing 10s in annealing furnace
Reduce intrinsic standoff ratio 0.01;
B, after decarburizing annealing, into the Nitrizing Treatment stage, the atmosphere in annealing furnace is still wet type nitrogen and hydrogen mixture;Nitriding temperature
For degree at 850 DEG C ~ 900 DEG C, nitriding time is conventional 20s ~ 45s;The ammonia flow being passed through is in 30 ~ 40m3/h;Nitriding stage furnace
Interior intrinsic standoff ratio PH2O/PH2The height positive correlation of the nitrogen content of intrinsic standoff ratio and steel grade setting 0.2 ~ 0.4, and in furnace;
5) conventional to carry out high annealing;
6) stretching and leveling, coating insulating coating and finished product finishing packaging are carried out, for use.
2. a kind of production method that can improve low temperature high magnetic induction grain-oriented silicon steel oxygen content as described in claim 1, it is characterised in that:
Basic intrinsic standoff ratio appoints the value taken in 0.4 ~ 0.58.
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