CN1220704A - Method for making electric sheet steel with oriented grains for manufacture of transfermer magnetic circuits in particular - Google Patents
Method for making electric sheet steel with oriented grains for manufacture of transfermer magnetic circuits in particular Download PDFInfo
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- CN1220704A CN1220704A CN98800332A CN98800332A CN1220704A CN 1220704 A CN1220704 A CN 1220704A CN 98800332 A CN98800332 A CN 98800332A CN 98800332 A CN98800332 A CN 98800332A CN 1220704 A CN1220704 A CN 1220704A
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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
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- 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
- C21D8/1216—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the working step(s) being of interest
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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
- C21D8/1261—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 following hot rolling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- 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
- C21D8/1205—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular fabrication or treatment of ingot or slab
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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
- C21D8/1277—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties involving a particular surface treatment
- C21D8/1288—Application of a tension-inducing coating
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Abstract
The invention concerns a method for making an electric sheet steel with oriented grains characterised in that the slab or strip has the following composition: less than 0.1 % carbon, more than 2.5 % silicon, less than 0.006 % sulphur, more than 0.002 % manganese, more than 0.008 % aluminium, more than 0.004 nitrogen, more than 0.02 % copper, less than 0.02 % tin. The method consists in subjecting the above slab to temperature less than 1350 DEG C and hot rolling such that: the percentage by mass of non-precipitated sulphur in the form of coarse particles of average diameter not less than 300 nanometers (nm) is higher than 0.004 %; the percentage by mass of precipitated nitrogen only on the form of fine particles of average diameter less than 100 nm is less than 40 % of the total percentage by mass of nitrogen.
Description
The present invention relates to make grain-oriented electrical steel sheet, in particular for the method for the electrical sheet of making transformer magnetic circuit, it may further comprise the steps successively:
-the steel continuous casting is become the operation of slab or band, in the Chemical Composition of described steel, contain (% weight) C, Si greater than 2.5% less than 0.1%, especially contain the element that is tending towards forming the precipitate that suppresses first crystal grain normal growth, Al, N, Mn, Cu and S, and look the Sn that particular case exists;
-with this base or the band reheating operation;
-for obtain thickness be 1-5mm sheet material carried out with this base, be determined on a case-by-case basis, should be with the hot rolled operation;
-operation that this hot-rolled sheet hot rolling is got;
-with this hot-rolled sheet or the operation of band annealed;
-be cold-rolled to the operation that thickness is equal to or less than 0.65mm with one step, or with the cold rolling operation of two steps being inserted with process annealing therebetween, the annealing of this hot-rolled sheet or band is chosen wantonly in this case;
-in advancing in containing N
2And H
2Wet atmosphere in primary recrystallization and the decarburizing annealing operation carried out;
The steel plate both sides of taking off carbon are coated with the operation that agent is recessed in the annealing that mainly contains magnesia MgO;
-batch the secondary recrystallization that carries out under the state and purifying the annealing operation;
-be coated with the operation of the insulating coating that brings out tensile stress and the annealing operation of firing this coating, in this process, this steel plate passes through the heat calendering process usually.
For making grain-oriented electrical sheet, will be before hot rolling through continuous casting and the steel billet reheat belong to contents known to the temperature that is higher than 1350 ℃.Must look and be enough to make the thick AlN that separates out separately or separate out jointly being higher than soaking time under 1350 ℃ the temperature, MnS and CuS particle dissolve again.These mean diameters are excessive when as cast condition, and large numbers of big particle makes secondary recrystallization can not take place.This makes the magnetic degradation of electrical sheet of gained.Since primary recrystallization cause 100}＜001〉on the direction, the misgrowth of crystal grain only at Individual existence or the mean diameter of mixing the MnS, the AlN that exist and CuS precipitate just take place when being significantly less than 100nm.100}＜001〉texture makes grain-oriented electrical sheet have good magnetic performance along rolling direction, knit at this and be easy to magnetized＜001 in structure axle and rolling direction almost parallel, and { the surperficial almost parallel of 110} face and this steel plate.
Mean diameter less than independent or the thin MnS of bonded, the AlN of 100nm and CuS precipitate be do not have 110}＜001〉inhibition of primary crystallization normal growth of direction.
Press known way control hot-rolled condition, steel billet is included in its heart portion to be enough to make, independent or bonded MnS, AlN and all dissolved time of CuS particle, reheat is to greater than 1350 ℃ temperature, thereby causes in this hot rolling band:
-whole S separates out with thin inhibition particulate form, and its straight footpath reaches significantly less than 100nm
-AlN does not take place during this hot rolling band annealing, mean diameter is separated out less than the inhibition AlN fine particle of 100nm.
With the sufficiently long time with the reheating of grain orientation steel billet to important disadvantages being arranged greater than 1350 ℃ temperature, it impels the formation of liquid oxidatively thing, this oxide compound accumulates in the reheating stove with the state of slag, thereby needs regular blowing out so that make it not blocked.This causes the loss of productivity and the maintenance cost of great number.
Known existence much prevents to stop up the method for steel billet reheating stove, especially referring to EP 0,219,611 and EP 0,339,474, wherein, with the steel billet reheat to temperature less than 1350 ℃.
According to someway, in steel billet reheating process, the AlN precipitate all again the dissolving, thereby, for the second time, recrystallize began before formation fine particulate main inhibition (Al, Si) N then carry out the nitriding operation to the steel plate that took off carbon.According to said method, S content is limited, and less than 0.012%.
According to from EP0,619,376 other method of learning, the MnS particle can not dissolve again in steel billet reheating process, and because they when retaining in this hot-rolled steel sheet with coarse grained form, thereby do not have a restraining effect yet.
Because the AlN particle is in the coarse particles state in hot-rolled steel sheet, its amount at least with always contain the N amount 60% suitable, so these particles only dissolve again with low ratio, nor inhibited.
Restraining effect mainly is to take place because of the CuS fine particle that forms when hot-rolled sheet is annealed.
According to EP 0,732, the other method described in 413, because steel billet has suitable Chemical Composition: S≤0.020%, Al≤0.030%, (%S * %Mn)＜160 * 10
-5, and (%Al * %N)＜240 * 10
-6So the precipitate that contains S and/or N when steel billet reheating dissolves again.
With this steel hot rolling, so that whole S is separated out with fine grain form.With this steel hot rolling, so that N is separated out with thin AlN particulate form.This is annealed through the hot rolled steel, so that N is separated out with the thin AlN particulate form that constitutes main inhibition.
The compound of at least a S and/or N can be added in the magnesia as annealing separating agent, this compound can produce further restraining effect.
The objective of the invention is to make the method for grain-oriented electrical steel sheet, it can be before hot rolling when being lower than 1350 ℃ temperature reheating steel billet or band, improve the magnetic quality of steel plate.
Theme of the present invention is a kind of manufacturing grain-oriented electrical steel sheet, and in particular for the method for the electrical sheet of producing transformer magnetic circuit, this method comprises in order:
-the steel continuous casting is become the operation of the shape of steel billet or band, contain (% weight) C in the Chemical Composition of this steel less than 0.1%, greater than 2.5% silicon, especially contain to trend towards forming element al, N, Mn, Cu and the S of the precipitate that suppresses first crystal grain normal growth and contain and look the Sn that particular case exists;
-with this steel billet or the band reheat operation;
-for obtaining thick 1-5mm steel plate, the operation of this steel billet of hot rolling and this band of hot rolling that is determined on a case-by-case basis;
-operation that the hot-rolled sheet hot rolling is got;
-with this hot-rolled sheet or the operation of band annealed;
-be cold-rolled to the operation of the final thickness that is equal to or less than 0.65mm with one step, or be inserted with the cold rolling operation of two steps of process annealing with the centre, this annealing of hot-rolled sheet or band is chosen wantonly in the case;
-in advancing in the wet N that contains
2And H
2Atmosphere in primary recrystallization and the decarburizing annealing operation carried out;
-in the operation that is coated with through annealed steel plate both sides with the annealing separating agent that mainly contains magnesia MgO;
-batch the secondary recrystallization that carries out under the state and purifying the annealing operation;
The annealing operation that-coating is brought out the insulating coating of tensile stress and fired this coating, in the process of this operation, steel plate is usually through the heat calendering process, and the feature of this method is:
-will have the steel billet or the steel plate of following composition (% weight),
-less than 0.1% C,
-greater than 2.5% Si,
-greater than 0.006% S,
-greater than 0.02% Mn,
-be 0.008% Al,
-greater than 0.004% N,
-greater than 0.02% Cu,
-Sn less than 0.02%, the Fe of surplus and impurity, reheating is carried out hot rolling then to the temperature that is lower than 1350 ℃, so that:
-make in this hot-rolled steel sheet, the quality percentage composition that is equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter is not greater than 0.004%,
-make in this hot-rolled steel sheet, only the quality percentage composition of the N that separates out less than the thin AlN particle form of 100nm with mean diameter is less than 40% of total quality percentage composition of N, and
To obtain hot-rolled steel sheet like this and stand at least once to anneal operation, only separate out less than the fine grain form of 100nm with mean diameter so that account for the N of total mass per-cent more than 60%.
Further feature of the present invention is:
-in the composition of this steel billet or band, contain especially (% weight):
0.02％＜C＜0.07％
3％＜Si＜4％
0.006％＜S＜0.035％
Mn＞0.02％
0.008％＜Al＜0.035％
0.004％＜N＜0.009％
0.02％＜Cu＜0.30％
0.02％＜Sn＜0.20％,
-this steel billet or band also contain the Sn of 0.08%-0.20%, and the quality percentage composition that is not equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter in this hot-rolled steel sheet is greater than 0.004%,
-this steel billet or band also contain and are less than 0.08% Sn, and the mass percent that is not equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter in this hot-rolled steel sheet is greater than 0.006%,
After-the annealing, the mass percent that is equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter is not greater than 0.006%, and preferably greater than 0.008%,
After-the annealing, the mass percent of the S that separates out less than the fine particulate form of 100nm with mean diameter is greater than 0.006%, and is more preferably greater than 0.008%,
-described annealing comprises this steel plate is incubated at least 50 seconds under 900 ℃-1150 ℃ temperature, and is cold soon then,
-finish after the annealing, be cold-rolled to final thickness with one step,
-this is annealed into the process annealing operation, it is to carry out after the operation of first cold rolling this hot-rolled sheet between the cold rolling operational period of two steps, carry out after this annealing cold soon,
-this annealing was carried out before cold rolling, or the operation of first cold rolling this hot-rolled sheet in the cold rolling operation process of two steps or band after carry out, carry out after this annealing cold soon,
-before primary recrystallization and decarburizing annealing, carry out cold rollingly, its draft is greater than 70%,
-before primary recrystallization and decarburizing annealing, carry out at least one passage of cold rolling step under greater than 150 ℃ temperature,
-this magnesia removes the TiO that is determined on a case-by-case basis and adds
2, also contain compound, antimony chloride or the tin sulphate of compound, one or more S and N of one or more compounds, one or more N of compound, S or S independent or bonded B or B outward,
-in ammoniated atmosphere, make steel plate stand the gas nitriding operation through decarburization.
The invention still further relates to by the resulting grain-oriented electrical steel sheet of present method.
Below statement and accompanying drawing all be that mode with indefiniteness embodiment provides, they will make the present invention be able to clearly be understood.
Fig. 1 shows not the quality percentage composition of the S that separates out more than or equal to the coarse particles form of 300nm with diameter in hot-rolled sheet, situation before the curve A explanation steel plate annealing, situation behind the curve B explanation steel plate annealing, this figure has also showed the relation between the total mass percentage composition of the quality percentage composition of the undecomposed S in the steel billet of reheating to 1300 ℃ and S.
Fig. 2 a, 2b and 2c have showed the magnetic property of this steel plate, the final thickness of this steel plate after cold rolling is 0.285mm, scribble the insulation compound that brings out tensile stress, and steel billet is reheated 1300 ℃, and described magnetic property is the function of the mass percent of the S that do not separate out more than or equal to the coarse particles form of 300nm with diameter in the hot-rolled sheet before the annealing.
Fig. 3 has showed as the function of hot-rolled sheet annealing temperature, the magnetic strength B800 of the finished product of cold rolling back thickness of slab 0.285mm, and this steel billet is reheated 1300 ℃.
Fig. 4 has showed as the function that is reheated the quality percentage composition of S in 1300 ℃ the steel billet, the average grain diameter after primary recrystallization and the decarburizing annealing (μ m), and the thickness of this hot rolling band is respectively 2.3mm and 2mm.
Fig. 5 has showed the magnetic property of the finished product of the thick 0.285mm of being, and after this performance was primary recrystallization and decarburizing annealing, diameter was greater than the function of the crystal grain per-cent of 15 μ m, and this steel billet is reheated 1300 ℃.
Fig. 6 a, 6b and 6c have showed that thickness is the magnetic property of the final product of 0.285mm, and after this performance was primary recrystallization and decarburizing annealing, diameter was less than the function of the crystal grain per-cent of 5 μ m, and this steel billet is reheated 1300 ℃.
Fig. 7 has showed that thickness is the iron loss of the finished product when 1.7T and 50Hz of 0.285mm, and this iron loss is the function that is reheated the quality percentage composition of soluble aluminum to 1300 ℃ the steel billet.
Fig. 8 a, 8b and 8c have showed that thickness is the magnetic property of the final product of 0.285mm, and this performance is the function that is not equal to or greater than the quality percentage composition I of the S that the coarse particles shape of 300nm separates out before the quality percentage composition of Sn in the steel billet of reheat to 1300 ℃ and the annealing in the hot-rolled sheet with diameter.
In general, " fine particle " is interpreted as the particle of its mean diameter less than 300nm, and the most mean diameter in these particles is less than 100nm; " coarse particles " is interpreted as the particle that its mean diameter is equal to or greater than 300nm, particularly should " the not S that separates out with the coarse particles shape " be interpreted as mainly the S that separates out with fine particulate form and the S of solid solution attitude, the major part among the S that separates out has the mean diameter less than 100nm.
This shows: the particulate electron microscope feature that can play the inhibitor effect has constituted to be differentiated at low temperature, promptly is lower than the optimal path of the whole bag of tricks of reheating steel billet under 1350 ℃ the temperature.This be because be difficult to provide the heat that causes this precipitation state in the hot-rolled sheet and hot machine process in detail and accurate pattern.
The quality percentage composition I of the S that does not separate out with the coarse particles form in the hot-rolled sheet equals poor by between the quality percentage composition of the determined S of usefulness scanning electron microscope that separates out with the coarse particles form in the quality percentage composition of S total in the determined steel billet of chemical analysis and the hot-rolled sheet.In order to eliminate the error of mensuration, only consider that mean diameter is equal to or greater than the precipitate that contains S of 300nm.Above steel plate, microscopic cross-section is carried out adjacent field scan to lower surface, magnification 1000, electron accelerating voltage is 15KV.The ratio of the total area that the surperficial ratio that contains the S precipitate equals to contain the S precipitate and the detected total area.On whole cross section, the surperficial ratio of precipitate equals the volume share of precipitate.The volume share of knowing the S that separates out with the coarse particles form just can calculate the quality percentage composition of the S that rice separates out with this form, then calculates not the quality percentage composition that is equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter.
According to an embodiment who implements the inventive method, the steel continuous casting that composition is shown in table 1 becomes the steel billet of thick 210mm.This steel billet is stood:
-with the reheating under 1300 ℃ of temperature of its core, the core of this steel billet is included in more than 1280 ℃ and is incubated 30 minutes insulation more than 1250 ℃ 50 minutes,
-being rolled to the hot roughing of 45mm thickness with several passages (being 5 passages) in this Application Example, the temperature when last passage finishes is 1080 ℃-1090 ℃, and
-with, such as, 7 hot finishings that passage is finished, the beginning temperature of hot finishing is 1060 ℃-1075 ℃, and the end temp of hot finishing is 925 ℃-935 ℃.
This hot roughing and finish rolling operation be by passing through milling train in turn, and such as, 12 base frameworks and carry out continuously, the draft in turn of roughing is 21,39,20,25 and 25%, and the draft in turn of finish rolling is 53,38,43,38,26,18 and 4%.
Under 510 ℃-540 ℃ temperature, batch the hot-rolled sheet that thickness is 2.3mm.
With 100 seconds temperature is risen to 1100 ℃, insulation was annealed to the hot-rolled sheet in advancing in 160 seconds in the time of 1100 ℃, was chilled to 800 ℃ with 30 seconds, was chilled to 65 ℃ with 10 seconds again.
To pass through hot rolling and annealed cold-rolling of steel plate thickness with a step then to 0.285mm, this step comprises that each draft is equivalent to 6 passages of about 30% order, and to be equivalent to total draft be 6 passages of 87.6%, and the rolling temperature during at least one passage is greater than 150 ℃.
This cold-reduced sheet through primary recrystallization and decarburization operation, is wherein especially comprised with about 15 seconds time temperature is risen to 700 ℃, with about 100 seconds temperature is risen to 820 ℃ from 700 ℃, at wet N
2/ H
2In the atmosphere, in 820 ℃ of insulations 40 seconds.
Apply this decarburization steel plate with the magnesia emulsion, this emulsion contains 150gMgO/ premium on currency, 6gTiO
2/ 100gMgO and antimony chloride/100gMgO of 0.04% are then with this steel plate drying.
The decarburization steel plate that then this has been coated with magnesia stands secondary recrystallization annealing operation, its heat-up rate be 15 ℃/time, atmosphere is 25%N
2/ 75%H
2, insulation when reaching at 1200 ℃ for 650 ℃ and 1200 ℃ in hydrogen is till the purification of S that finishes this metal and nitrogen.
Stand through the steel plate that purifies:
-coating the operation carried out with the solution that contains silicon-dioxide, aluminum phosphate and chromic acid;
-be 800 ℃ of operations of firing this steel plate of heat calendering after the coatings on the steel plate.
Except as otherwise noted, for whole embodiment, the treatment condition in each period all are identical during manufacturing
Table 1: the Chemical Composition of steel billet (% quality)
| Numbering | ????C | ???Si | ???Mn | ????S | ??Al sol | ?????N | ???Cu | ???Sn | ???? |
| Steel | |||||||||
| 1 | ??0.056 ??0.054 ??0.057 ??0.059 ??0.058 | ??3.12 ??3.26 ??3.22 ??3.24 ??3.21 | ??0.078 ??0.079 ??0.079 ??0.080 ??0.081 | ??0.011 ??0.015 ??0.022 ??0.025 ??0.027 | ??0.019 ??0.020 ??0.019 ??0.022 ??0.019 | ??0.0062 ??0.0066 ??0.0065 ??0.0066 ??0.0068 | ??0.144 ??0.085 ??0.083 ??0.082 ??0.085 | ??0.008 ??0.069 ??0.068 ??0.070 ??0.072 | ＜0.025 ＜0.025 ＜0.025 ＜0.025 ＜0.025 |
Table 2: resulting magnetic property when being 0.0285mm as the cold rolling back final thickness of the function of steel billet core reheat temperature
| Numbering | The reheat temperature | ??W(1.5/50) ?????W/kg | ???W(1.7/50) ?????W/kg | The B800 tesla | ????I ????％ |
| Steel 1 steel 1 steel 2 steel 2 steel 3 steel 3 steel 4 steel 5 | ???1250℃ ???1300℃ ???1250℃ ???1300℃ ???1250℃ ???1300℃ ???1300℃ ???1300℃ | ????0.95 ????0.94 ????0.81 ????0.79 ????1.28 ????0.76 ????0.77 ????0.76 | ?????1.41 ?????1.36 ?????1.14 ?????1.09 ?????2.08 ?????1.03 ?????1.04 ?????1.02 | ???1.83 ???1.84 ???1.87 ???1.89 ???1.63 ???1.92 ???1.90 ???1.92 | ??0.0037 ??0.0055 ??0.0063 ??0.0065 ??0.0014 ??0.0080 ??0.0104 ??0.0086 |
Curve A among Fig. 1 demonstrates beyond expectationly, of the present invention with continuously cast bloom reheating to 1300 ℃, then under the hot rolled condition, the quality percentage composition of the S that does not separate out with the coarse particles form in the unannealed hot-rolled steel sheet also increases when total S content increases in this base.What know is thereupon, Fig. 2 a, 2b and 2c show: in hot-rolled sheet, the quality percentage composition of the S that separates out with the coarse particles form was not greater than 0.006% o'clock, 1.5 the iron loss during tesla is less than 0.8W/kg, 1.7 the iron loss during tesla is less than 1.1W/kg, and magnetic strength B800 is equal to or greater than 1.88 teslas, and described steel billet is by reheating to 1300 ℃, and the thickness of cold rolling back the finished product is 0.285mm.
Total S per-cent lower (only 0.011%), and the No.1 steel billet that does not contain the Sn that have a mind to add has caused such product: it is characterized by medium magnetic quality, the quality percentage composition that is not equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter in the hot-rolled sheet is 0.0055%.
Compare with 5 steel with No.3,4, it is 0.015% that its steel billet total contains the S amount, the quality percentage composition of the S that does not separate out with the coarse particles form in its hot-rolled sheet is poor slightly greater than the magnetic quality of 0.006% No.2 steel, and the feature of the hot-rolled sheet of No.3,4 and 5 steel is: the percentage ratio of the S that separates out with the coarse particles form is not more.Fig. 3 shows, by the steel billet of reheating to 1300 ℃, the firm optimum annealing temperature that obviously departs near 1000 ℃ of its annealing temperature, then for for the hot-rolled sheet of No.2 steel, the magnetic quality of representing with the B800 magnetic strength just greatly descends, particularly like this when annealing temperature equals 1050-1150 ℃, the thickness of cold rolling back final product is 0.285mm.On the other hand, if the same significantly words of decline in the annealing temperature of the hot-rolled sheet of steel 3,4 and the 5 magnetic quality during near 1150 ℃, so when the annealing temperature of this hot-rolled sheet equals 1050 ℃, because it is higher not to be equal to or greater than the quality percentage composition of the S that the coarse particles state of 300nm separates out with mean diameter, thereby the magnetic quality does not almost descend.
Importance for this index of quality percentage composition I of showing the S that does not separate out with the coarse particles form in the sign hot-rolled sheet, base reheat to its core with steel No.3 reaches 1250 ℃ in another embodiment, the core of the steel billet that this 210mm is thick is in insulation more than 1200 ℃ 45 minutes, comprising being incubated 32 minutes more than 1230 ℃.Temperature when hot roughing finishes is 1075 ℃, and the temperature when hot finishing begins is 1030 ℃, and the temperature when hot finishing finishes is 950 ℃, and coiling temperature is 525 ℃.This hot-rolled sheet was annealed 160 seconds down at 1100 ℃, and intensification reaches cooling conditions again and narrates.The very poor reason of resulting magnetic mass (B800=1.63 tesla) is: the quality percentage composition I deficiency (0.0014%) that is not equal to or greater than the S that the coarse particles state of 300nm separates out with diameter.This means: with steel No.3 reheating, hot rolling and make hot-rolled sheet annealed condition inappropriate; Especially, the soaking time 1250 ℃ the time falls short of.If this quality percentage composition of the S of this steel billet is lower, such as just as the steel No.2 in the table 2,1250 ℃ of reheating under similarity condition cause the decline slightly of magnetic quality, and according to the present invention, described steel No.2 " I " value after reheating to 1250 ℃ and hot rolling is 0.0063%.
With the long time with steel billet or band this hot-rolled sheet of reheating just can the raising or in being with, be not equal to or greater than the quality percentage composition of the S that the coarse particles form of 300nm separates out with diameter.Therefore, under following condition, with the core reheating to 1300 of steel billet No.3 ℃: the soaking time more than 1250 is 65 minutes, comprising insulation more than 1280 ℃ 45 minutes.Under these conditions, the quality percentage composition of the S that does not separate out with the coarse particles form in this hot-rolled sheet is 0.013%, rather than 0.008% (table 2).By the present invention, this hot-rolled sheet must be annealed under such condition: the percentage ratio that is equal to or greater than the S that the coarse particles form of 300nm separates out with mean diameter does not have increase.Annealing conditions of the present invention must help being partly dissolved the precipitate that mean diameter is equal to or greater than 300nm, and the S that helps the solid solution attitude separates out less than the fine particulate form of 100nm with mean diameter in process of cooling.Curve B among Fig. 1 has been showed more such examples: after hot-rolled sheet annealing, be not equal to or less than the S that the coarse particles form of 300nm is separated out by the present invention with mean diameter, it is the example of the quality percentage composition of the example of quality percentage composition of S of solid solution attitude and the S that separates out less than the fine particulate form of 100nm with mean diameter basically.After hot-rolled steel sheet annealing, under the situation of steel 3,4 and 5, the mass percent of solid solution attitude S and the S that separates out with the fine particle attitude is greater than 0.010%.
In general, method of the present invention makes the S of solid solution attitude before for the first time cold rolling and/or in the annealing process of carrying out afterwards, in the decarburizing annealing process, during secondary recrystallization annealing, especially before beginning, secondary recrystallization separates out less than the fine particulate form of 100nm with mean diameter.
By the present invention, hot-rolled steel sheet or band are annealed under such condition: this condition makes N with 60% amount greater than the total mass percentage composition of N, and the fine particulate form that is less than or equal to 100nm with mean diameter is separated out.
Table 3: the mass percent of the N that in the hot rolling band, separates out with the AlN state
| Numbering | The reheating temperature | N (10 among the AlN -4％) |
| | ?????1250℃ ?????1300℃ ?????1250℃ ?????1300℃ ?????1250℃ ?????1300℃ ?????1300℃ ?????1300℃ | ????????6 ????????2 ????????8 ????????4 ???????14 ????????4 ????????9 ????????8 |
The principle of the method for the quality percentage composition of the N that measurement is separated out is as follows: with the bromo-carbinol mixture matrix is dissolved, select the Al that separates out by filtering on film, the NaOH dissolving AlN with dilution penetrates spectroscopic analysis Al with the ICP width of cloth, calculates corresponding N content then.
Table 4: the quality percentage composition of the N that separates out with the AlN form after the hot-rolled sheet annealing
| Numbering | The reheating temperature | N (10 among the AlN -4％) |
| | ?????1250℃ ?????1300℃ ?????1250℃ ?????1300℃ ?????1250℃ ?????1300℃ ?????1300℃ ?????1300℃ | ????????50 ????????55 ????????58 ????????50 ????????53 ????????57 ????????56 |
Table 3 and 4 has been listed the representative value of the quality percentage composition of the N that separates out before or after the hot-rolled sheet annealing.Confirm through transmission electron microscope(TEM): before or after hot-rolled sheet annealing, this N particulate mean diameter that contains is all less than 100nm.
By the present invention, there are some to make hot-rolled sheet or band annealed condition, these conditions impel the mass percent of the S that separates out more than or equal to the coarse particles form of 300nm with mean diameter to descend simultaneously and make independent or with the S bonded, mean diameter is separated out less than the AlN fine particle of 100nm.Above-mentioned example and of the present invention, comprise intensification, under given temperature the insulation and cold soon, especially be included in the annealing operation process that is incubated 50 seconds at least between 900 ℃-1150 ℃ and conform to.
Also can adopt more complicated operations process, such as, be warming up to 800 ℃ with 50 seconds, rose to 1100 ℃ with 40 seconds from 800 ℃, 1100 ℃-1125 ℃ insulations 50 seconds, be chilled to 900 ℃ with 30 seconds from 1125 ℃, be incubated 160 seconds and be chilled to 100 ℃ from 900 ℃ with the time that is less than 40 seconds at 900 ℃.
By the present invention, iron loss when the steel billet of No.3 steel obtains 1.7 teslas and 50Hz is 1.01W/kg, 1.5 the iron loss when tesla and 50Hz is 0.75W/kg, and magnetic strength B800 is 1.94 teslas, above-mentioned steel billet reheating to 1300 ℃, product final thickness with single stage after cold rolling is 0.285mm, and this final product is coated with the insulating compound that brings out tensile stress.
Especially in %Al * %N＞120 * 10 of product
-6And %Mn * %S＞140 * 10 of product
-5, S and solubility Al amount each greater than 0.018% and steel billet in Sn content greater than 0.05% o'clock, obtain these performances.
Fig. 2 a, 2b and 2c have showed the example of the magnetic behavior of final product, the thickness of this product after single stage is cold rolling is 0.285mm, and scribble the insulating coating that brings out tensile stress, this steel billet is by reheating to 1300 ℃, these magnetic properties are: frequency is 50Hz and power loss W (1.5/50) and W (the 1.7/50) (unit: W/kg) of work magnetic strength when being respectively 1.5 and 1.7 teslas, B800 magnetic strength when being 800A/m with magnetic field, these performances are functions of the mass percent of the S that do not separate out with the coarse particles form in the hot-rolled sheet (annealing before).
By the present invention and another embodiment, because the solubilized Al content in the steel billet of reheating to 1300 ℃ equals 0.020%, S content equal 0.018% and Sn content less than 0.02%, the mass percent of the S that this hot-rolled steel sheet is not separated out with the coarse particles form before and after annealing is greater than 0.06%, the quality percentage composition of the N that only separates out less than the 100nm fine particulate form with mean diameter before the annealing of this hot-rolled sheet is less than 40%, and this mass percent also contains B and TiO with the form of amidosulphuric acid to 100g greater than 60% after annealing
2Magnesia in add 1gS, the cold rolling back of single stage thickness is 0.285mm and the iron loss W (1.5/50) that scribbles the final product of insulating compound less than 0.86W/kg and W (1.7/50) less than 1.25W/kg, and B800 is greater than 1.86T.When the thickness after single stage is cold rolling is 0.335mm, iron loss W (1.5/50)＜0.92W/kg, iron loss W (1.7/50) is less than 1.25W/kg, and B800＞1.86T.Resulting loss equated when the iron loss W when unexpectedly, thickness is 0.335mm (1.7/50) was 0.285mm with thickness.Owing to deliberately do not add Sn, so promoted decarburization.
For making not quality percentage composition I＞0.006% of the S that separates out with the coarse particles form, with regard to 0.335mm thickness of slab same after single stage is cold rolling, with steel billet reheating to 1300 ℃, carry out hot rolling and annealing by the present invention, the result obtains following magnetic property: W (1.5/50)=0.88W/kg; W (1.7/50)=1.15W/kg; B800=1.91T; The chemical ingredients of used steel billet is (a % quality): C=0.058%, Si=3.24%, Mn=0.083%, S=0.029%, Al
S01=0.022%, N=0.0062%, Sn=0.07%; Cu=0.08%.
By the present invention, with with steel billet or steel band reheating to method of temperature less than 1350 ℃, before primary recrystallization and the decarburizing annealing, cold rolling draft greater than 70% just may reach＞the B800 magnetic strength of 1.84T, and if before primary recrystallization and decarburizing annealing, be not equal to or greater than quality percentage composition＞0.006% of the S that the coarse particles form of 300nm separates out, then B800 magnetic strength possibility＞1.90T also with mean diameter.
For obtaining the steel plate of final thickness less than 0.285mm, preferably carry out with two steps cold rolling, process annealing operation at one point.The second time after the process annealing is cold rolling＞and 70% draft can reach＞the B800 magnetic strength of 1.84T, and if quality percentage composition＞0.006% of the S that in hot-rolled sheet, does not separate out with the coarse particles form, this steel billet contains＜0.08% Sn, or mass percent I＞0.004%, this base contains＞during 0.08% Sn, and B800 magnetic strength possibility＞1.90T also then.
In a word:
If I＞0.004%, or＞0.006%, then
Sn＞0.08%, or＜0.08%.
Such as, be (% quality) with Chemical Composition: C=0.056%, Si=3.19%, Mn=0.081%, S=0.022%, Al
S01=0.022%, the steel billet reheating to 1300 of N=0.0070%, Sn=0.112%, Cu=0.081% ℃, then by the present invention, with such method hot rolling: make in the hot-rolled sheet of thick 2.3mm, the quality percentage composition I of the S that separates out more than or equal to the coarse particles form of 300nm with mean diameter does not equal 0.0054%, this hot-rolled sheet is cold-rolled to the thickness of 1.55mm, with its annealing,, have rolling temperature＞150 during the passage ℃ at least with being cold-rolled to the thickness of 0.215mm.
After primary recrystallization, decarburization, secondary recrystallization and the purifying treatment of metal, and after being coated with insulating compound, the magnetic property of gained is as follows: W (1.5/50)=0.69W/kg; W (1.7/50)=0.98W/kg, B800=1.89T.
When Sn content is higher in the steel billet, the quality percentage composition of the S that does not separate out more than or equal to the coarse particles form of 300nm with mean diameter in the hot-rolled sheet before the annealing may＜0.006%, but for obtaining good magnetic quality, necessary＞0.004% of this value.
At least be incubated 50 second when cold rolling preceding process annealing is included in 900 ℃-1150 ℃ the second time in hot-rolled sheet or band annealed operation and the cold rolling operation of two steps that makes before single stage is cold rolling, cold soon then.
Under the situation of the cold rolling operation of two steps, can before cold rolling operation for the first time, make this hot-rolled sheet or band annealing.This annealing helps obtaining good magnetic quality.This annealing comprises: in the time of 900 ℃-1150 ℃, be incubated 50 seconds at least, and cold soon then.This helps to contain S coarse particles local dissolution, and contains the S fine particle and/or contain the N particle and separate out.Must cause forming thick containing S and/or contain the annealing of N particulate in no instance.
By the present invention, with the method for temperature that steel billet reheating is lower than 1350 ℃ to its core temperature, before primary recrystallization and decarburizing annealing, this steel plate is incubated under greater than 150 ℃ temperature, soaking time be at least cold rolling step-individual passage, simultaneously cold rollingly carry out with one or two step.During several passages, the temperature of steel plate rises to more than 150 ℃, has caused good magnetic quality, if cold draft＞70% is then particularly like this.
Unexpectedly, the S that separates out with the coarse particles form has not produced influence to the crystal grain diameter that forms because of primary recrystallization, and the mean diameter of this crystal grain after primary recrystallization and decarburization be according to the present invention, for less than 15 μ m.When not adopting condition according to the invention, especially the mass percent of the S that ought be not separate out with coarse particles, before primary recrystallization and decarburizing annealing, less than 0.006% o'clock, since the S quantity not sufficient solid solution attitude and that separate out less than the fine particulate form of 100 μ m with mean diameter, the mean diameter of some primary crystallization crystal grain＞15 μ m.This has caused bad secondary recrystallization and has made the magnetic downgrade.Fig. 4 has showed that after primary recrystallization and decarburizing annealing the quality percentage composition of S is to the influence of the mean diameter (μ m) of this crystal grain in the steel billet.
When the thickness of hot rolling and cold rolling strap was respectively 2.3mm with 0.285mm (this is consistent with the cold draft of single stage 87.60%), when total S quality percentage composition rose in steel billet, the mean diameter of primary crystallization crystal grain reduced.
On the other hand, when the hot rolling tape thickness is 2mm, and draft is 85.75% o'clock, the mean diameter of first crystal grain is the not variation of total S quality percentage composition and changing in the invar base almost, this with hot-rolled sheet in not separate out the quality percentage composition of S with the coarse particles form of mean diameter 〉=300nm relevant, this relation is shown among Fig. 1.
In this embodiment, demonstrate that to adopt the hot-rolled sheet thickness of 2mm be preferred concerning improving the magnetic quality.Be 2.3mm with thickness, Chemical Composition (% quality) is: C=0.058%; Si=3.20%; Mn=0.079%; S=0.023%; Al
S01=0.020%; N=0.0076%; Sn=0.065%, the iron loss of the hot rolling band gained of Cu=0.085% is compared with B800, and iron loss when 1.5T and 1.7T and the improvement of B800 are respectively 3%, 4% and 1%.
If the final thickness of cold-reduced sheet is 0.261mm, the improvement of then this iron loss and B800 aspect is respectively 6%, 5% and 1%, when the thickness of hot-rolled sheet is 2m rather than 2.3mm, is cold rollingly undertaken by single stage.
In the case of the above embodiments, Fig. 5 and 6 has showed: be respectively under the situation of 2.00mm and 0.285mm at hot-rolled sheet and Cold Rolled Plate Thickness, per-cent＜25% when the first crystal grain of diameter＞15 μ m, and be more preferably＜20% o'clock, and per-cent＞10% of the first crystal grain of diameter＜5 μ m o'clock, minimum iron loss when having reached best magnetic quality-1.5T and 1.7T and the highest B800, the average grain diameter after primary recrystallization and decarburizing annealing is about 10 μ m.
Except being determined on a case-by-case basis, add TiO
2In magnesia, add the compound of the compound, S of B or boron or a kind or several sulphur individually or jointly outward.The compound of one or more S and N, the compound of antimony chloride or tin can improve the magnetic quality.These additives that add in the magnesia have improved during secondary recrystallization annealing, suppress the effect of normal first grain growing.In these additives, sal epsom, manganous sulfate, Sulfothiorine, ammonium sulfate, ammonium thiosulfate, amidosulphuric acid (or thionamic acid), urea, thiocarbamide and tin sulphate can improve magnetic property.
After decarburization, under＞500 ℃ temperature, be used in N
2/ H
2It is the another kind of measure that improves restraining effect and improve magnetic property that the ammonia that dilutes in the mixture carries out nitriding.
In the method for the invention:
The quality percentage composition of S in-continuously cast bloom or the band is necessary＞and 0.006%, so that in this hot-rolled sheet or band, obtain＞0.006%, the quality percentage composition of the S that separates out with the coarse particles form of mean diameter 〉=300nm not.For in purifying annealing process, reaching complete desulfurization, the quality percentage composition of S is best＜and 0.05%.For avoiding forming Edge crack when hot rolling steel billet or the steel band, this percentage ratio is best＜and 0.035%.
The quality percentage composition of N in-continuously cast bloom or the band is necessary＞and 0.004%, so that it is enough big to obtain its amount, form the AlN fine particle of main inhibition.For avoiding on the steel surface, forming bubble (foaming phenomenon), this quality percentage composition＜0.012%, best＜0.009%.
The quality percentage composition of the solubility Al of-continuously cast bloom or band is necessary＞and 0.008%, so that it is enough big to obtain number, form the thin AlN particle of main inhibition, so that in decarburization after gas nitriding or finish under the situation of adding nitrogen by add one or more nitrogen compounds to magnesia, have enough free, unconjugated Al.Dissolve for making in the reheating process of AlN precipitate before hot rolling, this quality percentage composition answers＜0.04%, and be more preferably＜0.03%.
Fig. 7 has showed the beneficial effect that increases the quality percentage composition of solubility Al in the steel billet, the Chemical Composition of this base (% quality) is: C=0.058%, Si=3.20%, Mn=0.080%, S=0.023%, N=0.007%, Sn=0.07%, Cu=0.08%, this steel billet is by reheating to 1300 ℃, the I value that hot rolling before cold rolling and annealing have caused according to the invention＞0.006%, and to have obtained thickness with 87.6% cold draft of single stage be the final product of 0.285mm.S content is risen to 0.029% from 0.023% just can reduce iron loss.When solubility Al too high levels, just caused not taking place secondary recrystallization, and unacceptable magnetic mass.Under identical annealing, cold rolling and primary recrystallization, decarburization and secondary recrystallization annealed condition before cold rolling, handle the hot rolling band that contains 0.022% solubility Al and processing and contain highlyer significantly, be impossible such as the hot rolling band of 0.03% solubility Al.
The quality percentage composition of Mn in-continuously cast bloom or the band is necessary＞and 0.02%, so that the acquisition amount is enough big, can improve the inhibition ability, thin MnS particle, so that adding under the situation of S, have the q.s free, unconjugated Mn by the compound that in magnesia, adds S or one or more S.
The quality percentage composition of Cu in-continuously cast bloom or the band is necessary＞and 0.02%, so that restriction S separates out in hot-rolled sheet with coarse grained form.For avoiding pecking the seal problem, this mass percent＜0.50% and being more preferably＜0.030%.
The quality percentage composition of Cu in the steel billet is elevated to 0.15% from 0.08%, just may be before annealing by the present invention the quality percentage composition I of the S that does not separate out with the coarse particles form in the hot-rolled sheet be brought up to 0.015% from 0.010%, the Chemical Composition of this steel billet is: C=0.058%, Si=3.23%, Mn=0.079%, S=0.025%, Al
S01=0.022%, N=0.0067%, Sn=0.069%, Cu=0.08% or 0.15%, this steel billet by the present invention by reheating to 1300 ℃.Thickness is that the magnetic quality of final product of 0.285mm is as follows: when Cu=0.08%, and W (1.5/50)=0.77W/kg, W (1.7/50)=1.04W/kg, B800=1.90T; And during Cu=0.15%, W (1.5/50)=0.76W/kg, W (1.7/50)=1.03W/kg, B800=1.91T.
-in order to have the magnetic property measurer is had tangible beneficial effect, in continuously cast bloom or the band quality percentage composition of Sn necessary＞0.02%.This per-cent is limited to 0.20%, so that avoid pecking seal problem and decarburization problem.
Fig. 8 has illustrated the useful influence to the magnetic quality of the Sn content that improves in the steel billet, and this steel billet is heated to 1300 ℃, hot rolling and annealing, and the thickness of hot rolling and cold rolling strap is respectively 2.3mm and 0.285mm.Without in the annealed hot-rolled sheet not with the coarse particles form separate out the quality percentage composition I of S be shown among Fig. 8.Only count I 〉=0.006% o'clock at the quality percentage composition, this useful influence of Sn is just given full play to.During the Sn that lack to have a mind to adds, percentage ratio I is necessary 〉=and the 0.008%th, desirable.When Sn content is high, because the magnetic quality is not best, percentage ratio I is necessary＜0.006%.With the quality percentage composition of 0.112% Sn and with 0.0054% the corresponding experimental point of quality percentage composition I not on the line of expression iron loss or B800 value, described value is the function (Fig. 8 a, 8b and 8c) of the quality percentage composition of Sn.
-in order to have low magnetic loss, quality percentage composition＞2.5% of the Si of continuously cast bloom or band.The quality percentage composition of Si is high more, and then this loss is low more, but, the per-cent of Si is mentioned on 4%, then make the cold rolling difficulty that becomes.
-the quality percentage composition of C in continuously cast bloom or the band is confined to 0.10%, to be limited to 0.07% be to make the decarburization difficulty because be higher than this value and be more preferably.Make percentage composition＞0.02% of C, with the magnetic quality that obtains.
By the present invention, only however the quality percentage composition of the S that separates out more than or equal to the coarse particles form of 300nm with mean diameter before primary recrystallization and decarburizing annealing still＞0.006%, can improve more than the Mn content to 0.20%, improve content as the Mn that promotes the γ phase forming element that austenite forms, can reduce simultaneously S content and C-γ mutually forming element-content and/or improve the content that Si-promotes to form ferritic α phase forming element (alphagenic) element.In order in steel billet or band reheating process, to dissolve AlN, importantly keep certain austenite share.
For given reheating temperature T and N quality percentage composition, the quality percentage composition of Al in consoluet continuously cast bloom of the present invention during the reheating of AlN precipitate before hot rolling or the band can be calculated by following formula:
log(％Al×％N)=-10.062/T+2.72。
Method of the present invention be at thickness be 150-300mm continuously cast bloom and by being stated.Steel billet is thick more, and it is also long more then to reach the required time of the core temperature of the base that meets the requirements.Such as, in advancing under the situation of reheating, when base is thick when being 210mm-240mm, it is desirable that the speed of steel billet by stove must slow down.When steel billet is thin, when being about 15-100mm, can improve the speed of steel billet by the reheating stove such as thickness.Hot rolling is got quality percentage composition 〉=0.004% that temperature must make not the S that separates out with the coarse particles form, and be more preferably 〉=0.006%, and the quality percentage composition that only must make the N that separates out with fine particulate form is less than 40% of the total mass percentage composition of the N in the hot-rolled sheet.This temperature is general＜and 700 ℃.
Method of the present invention also may be implemented in by casting molten steel between two cold rollers and get, and thickness is the thin steel band of 1-10mm, because its thickness is little, so can be before hot rolling the rapid reheating of this steel band be arrived＜1350 ℃ core temperature.
Hot rolled passage number depends on the initial thickness of steel billet or band and the thickness of hot-rolled sheet.If the thickness of continuously cast bloom or band is enough little, then can save thick hot rolling.
If quality percentage composition＞0.006% of the S that separates out with the coarse particles form of mean diameter 〉=300nm not, and if only the quality percentage composition of the N that separates out with fine particulate then can save reheating and hot rolling to continuous casting of thin strip less than 40% of the total mass percentage composition of the nitrogen in the workblank sheet material of casting between two rollers.Make this strip stand at least one the present invention's annealing operation then.
By the steel plate of the inventive method gained magnetic strength B 〉=1.86T when the 800A/m magnetic field, the iron loss when 1.7T and 50Hz is for the thickness of slab of＞0.30mm, for less than 1.30W/kg.During final thickness of slab≤0.30mm, with the steel plate of this method gained magnetic strength B 〉=1.86T when the 800A/m magnetic field, and the iron loss＜1.25W/kg when 1.7T and 50Hz.
Claims (16)
1. manufacturing grain-oriented electrical steel sheet, especially for the method for the electrical sheet of producing transformer magnetic circuit, it comprises in order:
-steel is pressed the operation of the form continuous casting of steel billet or band, contain in the Chemical Composition of this steel (% weight):＜0.1%C, 〉=2.5% Si, particularly element al, N, Mn, Cu and S, these elements tend to form the precipitate that suppresses first crystal grain normal growth, and look the Sn that particular case exists;
-with this steel billet or the band reheating operation;
-for acquisition thickness is the steel plate of 1-5mm, the operation of this steel billet of hot rolling and this band of hot rolling that is determined on a case-by-case basis;
-operation that this hot-rolled steel sheet hot rolling is got;
-with this hot-rolled steel sheet or the operation of band annealed;
-be cold-rolled to the operation of thickness≤0.65mm with one step, or to be inserted with the cold rolling operation of two steps of process annealing, the annealing of hot-rolled sheet or band is chosen wantonly in this case;
-at the wet H that contains
2And N
2Atmosphere in, primary recrystallization that in advancing, carries out and decarburizing annealing operation;
-be coated with the operation of the annealing separating agent that mainly contains magnesia MgO in decarburization steel plate both sides;
-to batch secondary recrystallization and the purification annealing operation that state carries out;
-annealing the operation that is coated with the operation of the insulation compound that brings out tensile stress and fires this coating, steel plate stands heat calendering usually during this period;
It is characterized in that having following % weight composition:
C≤0.1％
Si＞2.5％
S＞0.006％
Mn＞0.02％
Al＞0.008％
N＞0.004％
Cu＞0.02％
Sn＜020% surplus is the steel billet of Fe and impurity or the steel plate reheating temperature to its core＜1350 ℃, makes it through hot rolling then, thereby makes:
Quality percentage composition＞0.006% of the S that does not separate out with the coarse particles form of mean diameter 〉=300nm in-this hot-rolled steel sheet;
In-this hot-rolled steel sheet only with the quality percentage composition of the N that mean diameter＜the 100nm fine particulate form is separated out less than 40% of the total mass percentage composition of N;
With the hot-rolled steel sheet that obtains like this through the operation of at least once annealing, thereby the N of total mass percentage composition more than 60% only separated out with the fine grain form of mean diameter＜100nm.
2. the method for claim 1 is characterized in that especially containing in the % weight composition of this steel billet or band:
0.020％＜C＜0.07％
3％＜Si＜4％
0.006％＜S＜0.035％
Mn＞0.02％
0.008％＜Al＜0.030％
0.004％＜N＜0.009％
0.02％＜Cu＜0.30％
0＜Sn＜0.20％。
3. claim 1 and 2 method is characterized in that this steel billet or band also contain the Sn of 0.08%-0.20%, quality percentage composition＞0.004% of the S that does not separate out with the coarse particles form of mean diameter 〉=300nm in this hot-rolled steel sheet.
4. claim 1 and 3 method is characterized in that this steel billet or band also contain＜0.08% Sn, quality percentage composition＞0.006% of the S that does not separate out with the coarse particles form of mean diameter 〉=300nm in this hot-rolled steel sheet.
5. the method for claim 1-4, it is characterized in that annealing after, quality percentage composition＞0.006% of the S that separates out with the coarse particles form of mean diameter 〉=300nm not and is more preferably＞0.008%.
6. the method for claim 5, it is characterized in that annealing after, quality percentage composition＞0.006% of the S that separates out less than the fine particulate form of 100nm with mean diameter and is more preferably＞0.008%.
7. the method for claim 1-6 is characterized in that this annealing is included under 900 ℃-1150 ℃ the temperature this steel plate insulation 50 seconds at least, and is cold soon then.
8. the method for claim 1-7 is characterized in that, this annealing was carried out before being cold-rolled to final thickness with one step.
9. the method for claim 1-7 is characterized in that this is annealed into the process annealing operation, and it carries out after hot-rolled steel sheet or band are finished the first cold rolling operation in the cold rolling operation process of two steps, and this annealing back is for cold soon.
10. the method for claim 1-7 is characterized in that carrying out this annealing is finished the first cold rolling operation to hot-rolled steel sheet or band before cold rolling and in the cold rolling operation process of two steps after, and this annealing back is for cold soon.
11. the method for claim 1-10 is characterized in that the cold rolling draft with＞70% before primary recrystallization and the decarburizing annealing carries out.
12. the method for claim 1-11 is characterized in that at least one passage in cold rolling before primary recrystallization and the decarburizing annealing is carried out under＞150 ℃ temperature.
13. the method for claim 1-12 is characterized in that this magnesia removes the TiO that is determined on a case-by-case basis and adds
2Also contain separately or the compound of compound, S or one or more S of bonded B or B compound, antimony chloride or the tin sulphate of the compound of one or more N, one or more S and N outward.
14. the method for claim 1-13 is characterized in that making this decarburization steel plate to stand the gas nitriding operation in ammoniated atmosphere.
15. the grain-oriented electrical steel sheet of thickness＞0.30mm that the method for claim 1-14 obtains, the magnetic strength B 〉=1.86T when it is characterized in that the magnetic field of its 800A/m, and the iron loss＜1.30W/kg when 1.7T and 50Hz.
16. the grain-oriented electrical steel sheet of thickness＞0.30mm that the method for claim 1-14 obtains, the magnetic strength B 〉=1.86T when it is characterized in that the magnetic field of its 800A/m, and the iron loss＜1.25W/kg when 1.7T and 50Hz.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR97/03451 | 1997-03-21 | ||
| FR9703451A FR2761081B1 (en) | 1997-03-21 | 1997-03-21 | METHOD FOR MANUFACTURING AN ELECTRIC STEEL SHEET WITH ORIENTED GRAINS FOR THE MANUFACTURE, IN PARTICULAR OF MAGNETIC CIRCUITS OF TRANSFORMERS |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1220704A true CN1220704A (en) | 1999-06-23 |
Family
ID=9505038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98800332A Pending CN1220704A (en) | 1997-03-21 | 1998-03-18 | Method for making electric sheet steel with oriented grains for manufacture of transfermer magnetic circuits in particular |
Country Status (10)
| Country | Link |
|---|---|
| EP (1) | EP0912768B1 (en) |
| JP (1) | JP2001506704A (en) |
| KR (1) | KR20000011149A (en) |
| CN (1) | CN1220704A (en) |
| AT (1) | ATE266742T1 (en) |
| CZ (1) | CZ375398A3 (en) |
| DE (1) | DE69823771T2 (en) |
| FR (1) | FR2761081B1 (en) |
| PL (1) | PL330039A1 (en) |
| WO (1) | WO1998042882A1 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103878175A (en) * | 2012-12-21 | 2014-06-25 | 鞍钢股份有限公司 | Hot rolling method in low-grade cold-rolled silicon steel hot rolling procedure |
| CN106661655A (en) * | 2014-08-27 | 2017-05-10 | 蒂森克虏拉塞斯坦有限公司 | Method for producing nitrided packaging steel |
| CN107002158A (en) * | 2014-11-26 | 2017-08-01 | Posco公司 | Oriented electrical steel annealing separator composition and the manufacture method using its oriented electrical steel |
| CN108291268A (en) * | 2015-12-04 | 2018-07-17 | 杰富意钢铁株式会社 | The manufacturing method of grain-oriented magnetic steel sheet |
| CN111020140A (en) * | 2019-12-17 | 2020-04-17 | 无锡晶龙华特电工有限公司 | Magnesium oxide annealing separant for oriented silicon steel with excellent magnetism and coating process thereof |
| CN111996354A (en) * | 2020-08-27 | 2020-11-27 | 上海实业振泰化工有限公司 | Preparation method of liquid additive for oriented silicon steel |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1162280B1 (en) * | 2000-06-05 | 2013-08-07 | Nippon Steel & Sumitomo Metal Corporation | Method for producing a grain-oriented electrical steel sheet excellent in magnetic properties |
| JP4272557B2 (en) * | 2004-02-12 | 2009-06-03 | 新日本製鐵株式会社 | Method for producing unidirectional electrical steel sheet with excellent magnetic properties |
| KR100953755B1 (en) * | 2005-06-10 | 2010-04-19 | 신닛뽄세이테쯔 카부시키카이샤 | Process for producing the grain-oriented magnetic steel sheet with extremely high magnetic property |
| JP4823719B2 (en) * | 2006-03-07 | 2011-11-24 | 新日本製鐵株式会社 | Method for producing grain-oriented electrical steel sheet with extremely excellent magnetic properties |
| CN106319174B (en) * | 2016-09-23 | 2018-10-16 | 武汉钢铁有限公司 | Improve the annealing separating agent of low temperature casting blank heating high magnetic induction grain-oriented silicon steel bottom layer quality |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5948934B2 (en) * | 1981-05-30 | 1984-11-29 | 新日本製鐵株式会社 | Manufacturing method of high magnetic flux density unidirectional electrical steel sheet |
| DE4311151C1 (en) * | 1993-04-05 | 1994-07-28 | Thyssen Stahl Ag | Grain-orientated electro-steel sheets with good properties |
| FR2731713B1 (en) * | 1995-03-14 | 1997-04-11 | Ugine Sa | PROCESS FOR THE MANUFACTURE OF A SHEET OF ELECTRIC STEEL WITH ORIENTED GRAINS FOR THE PRODUCTION OF MAGNETIC TRANSFORMER CIRCUITS IN PARTICULAR |
-
1997
- 1997-03-21 FR FR9703451A patent/FR2761081B1/en not_active Expired - Fee Related
-
1998
- 1998-03-18 DE DE69823771T patent/DE69823771T2/en not_active Expired - Lifetime
- 1998-03-18 WO PCT/FR1998/000540 patent/WO1998042882A1/en not_active Application Discontinuation
- 1998-03-18 CZ CZ983753A patent/CZ375398A3/en unknown
- 1998-03-18 CN CN98800332A patent/CN1220704A/en active Pending
- 1998-03-18 PL PL98330039A patent/PL330039A1/en unknown
- 1998-03-18 EP EP98914939A patent/EP0912768B1/en not_active Expired - Lifetime
- 1998-03-18 AT AT98914939T patent/ATE266742T1/en active
- 1998-03-18 KR KR1019980709309A patent/KR20000011149A/en not_active Application Discontinuation
- 1998-03-18 JP JP54511998A patent/JP2001506704A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103878175A (en) * | 2012-12-21 | 2014-06-25 | 鞍钢股份有限公司 | Hot rolling method in low-grade cold-rolled silicon steel hot rolling procedure |
| CN106661655A (en) * | 2014-08-27 | 2017-05-10 | 蒂森克虏拉塞斯坦有限公司 | Method for producing nitrided packaging steel |
| CN106661655B (en) * | 2014-08-27 | 2018-09-28 | 蒂森克虏拉塞斯坦有限公司 | The method of the packaging steel of manufacture nitridation |
| CN107002158A (en) * | 2014-11-26 | 2017-08-01 | Posco公司 | Oriented electrical steel annealing separator composition and the manufacture method using its oriented electrical steel |
| CN107002158B (en) * | 2014-11-26 | 2019-06-18 | Posco公司 | The manufacturing method of oriented electrical steel annealing separator composition and the oriented electrical steel using it |
| CN108291268A (en) * | 2015-12-04 | 2018-07-17 | 杰富意钢铁株式会社 | The manufacturing method of grain-oriented magnetic steel sheet |
| CN111020140A (en) * | 2019-12-17 | 2020-04-17 | 无锡晶龙华特电工有限公司 | Magnesium oxide annealing separant for oriented silicon steel with excellent magnetism and coating process thereof |
| CN111996354A (en) * | 2020-08-27 | 2020-11-27 | 上海实业振泰化工有限公司 | Preparation method of liquid additive for oriented silicon steel |
| CN111996354B (en) * | 2020-08-27 | 2022-04-19 | 上海实业振泰化工有限公司 | Preparation method of liquid additive for oriented silicon steel |
Also Published As
| Publication number | Publication date |
|---|---|
| DE69823771T2 (en) | 2005-05-12 |
| ATE266742T1 (en) | 2004-05-15 |
| EP0912768B1 (en) | 2004-05-12 |
| JP2001506704A (en) | 2001-05-22 |
| EP0912768A1 (en) | 1999-05-06 |
| PL330039A1 (en) | 1999-04-26 |
| CZ375398A3 (en) | 1999-07-14 |
| FR2761081A1 (en) | 1998-09-25 |
| KR20000011149A (en) | 2000-02-25 |
| FR2761081B1 (en) | 1999-04-30 |
| WO1998042882A1 (en) | 1998-10-01 |
| DE69823771D1 (en) | 2004-06-17 |
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