CN100455702C - Method for producing oriented silicon steel with good bottom by low-temperature heating - Google Patents
Method for producing oriented silicon steel with good bottom by low-temperature heating Download PDFInfo
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- CN100455702C CN100455702C CNB2005101108993A CN200510110899A CN100455702C CN 100455702 C CN100455702 C CN 100455702C CN B2005101108993 A CNB2005101108993 A CN B2005101108993A CN 200510110899 A CN200510110899 A CN 200510110899A CN 100455702 C CN100455702 C CN 100455702C
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Abstract
The invention supplies a method used to produce orientation silicon steel by low temperature heating. It includes the following steps: heating the plate blank under 1280 degree centigrade; hot rolling; once or double cold rolling to gain finished product sheet thickness; nitriding treatment; decarburizing annealing; coating insulator; high temperature annealing. In the nitriding technology, heating area dew point is controlled at -15-40 degree centigrade. The invention has the advantages of high nitriding efficiency, no influence from the surface oxide film, excellent MgO coat formula which makes the magnesium silicate substrate have good magnetic property, ensure the implementation for the next hot leveling annealing and insulating coating.
Description
Technical field
The present invention relates to a kind of low-temperature heat and produce the method for oriented silicon steel, the method that oriented silicon steel is produced in particularly a kind of low-temperature heat with good bottom.
Background technology
(1) production method of tradition directed silicon steel is as follows:
Basic chemical ingredients is Si (2.5～4.5%), [C] (0.01～0.10%), Mn (0.03～0.1%), S (0.012～0.050%), Als (0.01～0.05%), N (30～120ppm), the composition system that has also contains one or more in the elements such as Cu, Mo, Sb, Cr, B, Bi, and all the other are iron and unavoidable impurities element; The temperature of slab about special-purpose high temperature process furnace internal heating to 1400 ℃, and carry out insulation more than 30 minutes, make the abundant solid solution of inclusion, after the hot-rolled sheet normalizing, carry out pickling; With once cold rolling or comprise that twice above cold rolling process of process annealing rolls finished product thickness, to carry out decarburizing annealing [C] in the steel plate taken off the degree that do not influence finished product magnetic (generally should below 30ppm), coating is the annealing separating agent of main component with MgO; In the high-temperature annealing process, steel plate generation secondary recrystallization, separant and the surface oxide layer that forms when decarburizing annealing react and form Mg
2SiO
4Bottom purifies steel (remove in the steel S, N etc. to the deleterious element of magnetic) simultaneously; Through the coating insulating coating and the annealing that stretches, obtain the oriented silicon steel of commercial applications form at last.
There are following 2 remarkable deficiencies in the production method of above-mentioned tradition directed silicon steel:
(1) inhibitor is from steel-making, and in each operation thereafter, inhibitor all will allow it play a role, so must strict it be controlled and adjust;
(2) slab has reached the Limiting Level of process furnace 1400 ℃ of heat; Heat, scaling loss is big, the frequent repairing of process furnace causes utilization ratio low, the energy consumption height; The limit of hot rolled coil is split greatly, causes cold rolling process to produce difficulty, and lumber recovery is low, the cost height.
(2) owing to there is the defective of above-mentioned heat itself, the researchist of factory gropes and developed other technology again: promptly slab is in heating below 1250 ℃, and hot-rolled sheet is boundless to be split, and productivity is good.The nitriding of inhibitor after by decarburizing annealing obtains, and is a kind of posteriori acquisition type inhibitor.Such production method typical case is disclosed in the following document:
The patentee is the Japanese patent laid-open 5-112827 of Nippon Steel Manufacturing Corp, and the time of disclosure is 1993, and patent name is " the oriented silicon steel manufacture method of magnetic property and epithelium characteristic good ", and it discloses following method:
Chemical ingredients: [C] 0.025%～0.075%, Si 2.5%～4.5%, S≤0.012%, Als0.010～0.060%, N≤0.010%, Mn 0.08～0.45%, and P 0.015～0.045%, and all the other are Fe and inevitable inclusion.Slab carries out hot rolling after heating below 1200 ℃.Cold rolling or have the above cold rolling process of twice of process annealing to be rolled down to final product thickness with 1 time, steel plate carries out continuous nitriding after the decarburizing annealing in traveling process, carry out high temperature annealing behind the separant coating, remove impurities such as S, N and form glassy membrane, carry out the smooth processing of sintering again behind the coating coating insulating film, all good oriented silicon steels of production magnetic and bottom layer quality.
Continuous nitriding method: protective atmosphere is H
2And N
2Mixed gas, NH wherein
3Content is more than the 1000ppm, and the oxygen gesture is PH
2O/PH
2≤ 0.04, nitriding dew point 0～-15 ℃, nitriding temperature is 500～900 ℃.
During high temperature annealing, in 600～850 ℃ temperature range, keep weak oxide atmosphere.
● the patentee for the TOHKEMY 2000-273550 patent disclosure of Nippon Steel Manufacturing Corp a kind of denomination of invention be " glassy membrane and the oriented steel board fabrication method that has excellent magnetic characteristics ", this method discloses: C:0.021～0.075%, Si:2.5～4.0%, Mn:0.05～0.45%, below the S:0.014%, Als:0.010～0.040%, N:0.0030～0.0130%, less than 1280 ℃ of following heating slabs, hot rolling then, cold rolling, decarburizing annealing, nitriding are handled, the coating separant, carry out final high temperature annealing then.As the active CAA40%=120 of annealing separating agent citric acid～250 seconds, and CAA70% value/CAA40% value=2～10, and in the slurries of separant, add water capacity S compound 0.02～0.5%, be coated on the steel plate after nitriding is handled, after drying below 300 ℃, carry out high temperature annealing, the oriented steel board fabrication method that forms glassy membrane and have excellent magnetic characteristics.
● the patentee is " the oriented steel board fabrication method that magnetic property and glassy membrane are good " for the Japanese kokai publication sho 60-145382 of Nippon Steel Manufacturing Corp discloses a kind of denomination of invention, this method is introduced: C:0.030～0.10%, Si:2.5～4.0%, use sulfide, at least a in the nitride as inhibitor, carry out hot rolling, one time the process annealing secondary is above cold rolling, obtain the finished product thickness of slab, carry out decarburizing annealing again, the coating annealing separating agent, add 0.05～2.0% antimony trisulfate in the separant, also contain a kind of in addition in the antimony trisulfate or more than one 5～20% Sb, Sr, Ti, the muriate of Zr, 0.5～10% contain the Ti compound.The oriented steel board fabrication method that forms glassy membrane and have excellent magnetic characteristics.
● the Chinese patent application of Nippon Steel Manufacturing Corp application number is that 95106060.0 denomination of invention discloses a kind of annealing spacer that is used to produce grain-oriented siliconized plate for " annealing spacer and the using method thereof with sound response that are used for siliconized plate ", and it contains one or more compounds that is selected from following general formula:
(Mg
1-xM
3+ x) O, (Mg
1-xM
2+ x) O or (Mg
1-xM
2+ X1M
3+ X2) O,
M in the formula
2+Be one or more divalent metals that are selected from Be, Ca, Ba, Sr, Sn, Mn, Fe, Co, Ni, Cu or Zn;
M
3+Be one or more trivalent metals that are selected from Al, Fe, Cr, Co, B, Ti, Sb;
0.01≤X≤0.40; And
X＝X1+X2。
This annealing spacer that has than low melting point and higher level of reactivity is applied to through on the steel band of decarburizing annealing, and it has improved the performance of glassy membrane, has film outward appearance and good sealing function and carbon performance especially uniformly.
● Nippon Steel Manufacturing Corp has applied for that denomination of invention is the Chinese patent application of " production technique with grain-oriented electrical steel sheet of fine glass film and magnetic property " numbers 95197201.4, this invention is the technology that a kind of production has the grain-oriented electrical steel sheet of fine glass film and magnetic property, promptly use the annealing separation agent coated steel plates, the steel plate finished products, the agent of baking insulating coating, comprise with the steel plate of annealing separation agent coating through decarburizing annealing, this annealing separation agent is being prepared in the process in slurry stage in the step of MgO coated steel plates by the step of producing MgO, in the MgO of 100 parts of weight, introduce with F, Cl, Br and I weight are calculated the F that is selected from of 0.015 to 0.020 part of weight, Cl, the halogen compounds of Br and I, and steel plate is done finished product anneal.
By in the above-mentioned domestic and international patent documentation based on the producing oriented silicon steel by heating low temperature casting blank analysis of technology of nitridation process, as can be seen:
(1) Ri Ben technology concentrates on after the decarburizing annealing in the secondary recrystallization process the steel plate nitriding, nitriding temperature is low, inhibitor is the effect that reaches inhibitor in the steel plate by the later stage nitriding, the primary recrystallization grain-size is by the temperature and time in each technology control, requires the control of little narrow, decarburizing annealing of process window control fluctuation (tolerance) and nitridation process to require high; On the other hand, because nitriding is carried out after decarburizing annealing, it is the zone of oxidation of main component with SiO2 that surface of steel plate after the decarburizing annealing has formed one deck, and the homogeneity of nitriding and nitriding behavior are subject to the influence of surface oxide layer, and nitriding is inhomogeneous, then in high-temperature annealing process, based on the separant of MgO, the effusion of the N that is subject to infiltrate in the steel in the process that forms glassy membrane influence causes producing multiple bottom defective, cause the brilliant defective of the many dew in surface, finally magnetic is exerted an influence.
(2) contain among the employed separant MgO in the above-mentioned technology and added Sb, Sr, the muriate of Ti, Zr, sulfide; In MgO, introduce the halogen compounds of F, Cl, Br and I in addition.But, can not form good bottom at indivedual positions owing to be subjected to the influence of halogen compounds.
Summary of the invention
Therefore, the objective of the invention is to obtain to have the oriented silicon steel of good stripping film bottom and excellent magnetism energy, energy consumption is reduced, enhance productivity.
For achieving the above object, the present invention considers the directional silicon steel slab at existing technology temperature production, before suitable decarburizing annealing section He after the heating zone, the nitriding section is set, and under suitable dew point, atmosphere, steel plate is carried out nitriding and handle, this moment, surface of steel plate did not have zone of oxidation, made the nitriding amount be easy to control and grasp, then in the decarburizing annealing process, steel plate is in the atmosphere of high dew point, forms (Al, Si) N is favourable and be mingled with, can control the primary recrystallization tissue of steel plate effectively.Utilizing the special aquation rate that contains is 1.5～6% the special-purpose magnesium oxide of silicon steel, the oxide compound or the salt that add water miscible a kind of or the Na more than two kinds, K, Zn, Ca, Cr, Zr, Sr, Ti, Sb again, add-on is 0.1～10% of a MgO weight, other composition in the slurries is conventional additive, the slurries of making are coated in the oriented silicon steel surface after the nitriding decarburizing annealing, so that discharge an amount of moisture content in the first half of final high temperature annealing, can improve the oxygen position in the coil of strip lamellar spacing, guarantee in the decarburizing annealing process, to be formed on the Fe of surface of steel plate
2SiO
4Be not reduced, strengthened MgO to matrix surface SiO
2The diffusion area of layer has reduced the formation temperature of Magnesium Silicate q-agent bottom, thereby guarantees to form excellent oriented silicon steel Magnesium Silicate q-agent bottom and magnetic properties.
According to one embodiment of present invention, the invention provides a kind of low-temperature heat and produce the method for oriented silicon steel, mainly comprise: will heat down less than 1280 ℃ with the directional silicon steel slab of existing technology temperature production, hot rolling then, carry out once or secondary cold-rolling obtains the finished product thickness of slab, carry out first nitriding again and handle, back decarburizing annealing, apply separant, carry out final high temperature annealing at last, wherein, in nitridation process, the heating zone dew point is controlled at-15 ℃～-40 ℃; Nitriding temperature is controlled at 750 ℃～900 ℃; Nitriding time is 5～50 seconds; Nitriding medium is NH
3, dew point is controlled at below-40 ℃; Protective atmosphere is H
2And N
2Mixed gas, the atmosphere dew point is at-15 ℃～-40 ℃; In follow-up decarburizing annealing technology, under conventional decarburizing annealing temperature, the atmosphere dew point is controlled at 50 ℃～75 ℃; In coating separant technology, utilize the aquation rate to make the annealing separating agent slurries at the special-purpose MgO of 1.5～6% silicon steel, and in the slurries of separant, add weight percent and be oxide compound or the salt of 0.1～10% a kind of or the Na more than two kinds, K, Zn, Ca, Cr, Zr, Sr, Ti, Sb, the slurries of making are coated on the surface of steel plate after the nitriding decarburization.
According to another embodiment of the invention, in described nitridation process, H
2Account for 20～75% (volume percent) of gas gross, NH
3Account for 0.1～25% (volume percent) of gas gross;-20 ℃～-35 ℃ of heating zone dew point controls; In decarburizing annealing technology, the atmosphere dew point is controlled at 70～75 ℃.
According to still another embodiment of the invention, described method also comprises the afterwards cold rolling normalizing process before of hot rolling, in this processing step; hot-rolled sheet kept 1～20 second down at 1050～1180 ℃; kept 30～200 seconds down at 850～950 ℃, and cool off fast, speed of cooling is greater than 25 ℃/s.
According to still a further embodiment, the composition of described directional silicon steel slab is (weight percent): C :≤0.065%, and Si :≤3.5%, Als≤0.035%, Mn :≤0.20%, Cu≤0.12%, Sn≤0.15%, other is that Fe and inevitable impurity are formed.
Below be the key point of master operation:
1) smelts
C: Si≤0.065% :≤3.5%, Als≤0.035%, Mn :≤0.20%, Cu≤0.12%, Sn≤0.15%, and control few N, S technology composition.
2) hot rolling
Strand rolls into the hot-rolled sheet of 1.5～3.5mm thickness in process furnace internal heating to 1100～1200 ℃.
3) normalizing
Hot-rolled sheet carries out the normalizing annealing of 1050～1180 ℃ (1～20 seconds)+(850～950 ℃ * 30～200 seconds), and cools off fast, and speed of cooling is greater than 25 ℃/s.
4) cold rolling
With once or the band process annealing the above cold rolling process of secondary roll production board thickness.
5) nitriding, decarburization, coating MgO, high temperature annealing
Centre in heating zone and decarburizing annealing section is provided with the nitriding section, and in suitable dew point, under the atmosphere steel plate that rolls finished product thickness being carried out nitriding handles, the dew point of nitriding section is controlled at-15 ℃～-40 ℃, preferably be controlled at-20 ℃～-35 ℃, surface of steel plate does not have zone of oxidation at this moment, make the nitriding amount be easy to control and grasp, then in follow-up decarburizing annealing process, control high dew point atmosphere, make the nitrogen of steel further diffuse to form (Al, Si) N is favourable is mingled with, control the primary recrystallization tissue of steel plate effectively, simultaneously with the steel plate decarburization to less than below the 30ppm.Utilize a kind of special-purpose MgO of silicon steel that contains certain aquation rate to make the annealing separating agent slurries then, and in the slurries of separant, add water miscible a kind of or two kinds Na, K, Zn, Ca, Cr, Zr, Sr, Ti, the oxide compound of Sb or salt, add-on is 0.1～10% of a MgO amount, the slurries of making are coated on the surface of steel plate after the nitriding decarburization, after drying below 300 ℃, enter high-temperature annealing furnace and carry out common process high temperature annealing system, discharge an amount of moisture content in first half of final high temperature annealing through the separant of 300 ℃ of oven dry, improve the oxygen position in the coil of strip lamellar spacing, guaranteed in the decarburizing annealing process, to be formed on the Fe of surface of steel plate
2SiO
4Be not reduced, can obtain the stripping film bottom and the excellent magnetism energy of good adhesion.
Concrete technical specification is as follows:
Nitriding equipment
The characteristics of nitridation technique of the present invention are to carry out nitriding before the decarburizing annealing to handle on horizontal annealing furnace, this horizontal annealing furnace comprises: heating zone, nitriding section, decarbonization section, reduction section and cooling section, three atmosphere disrupters are set between heating zone, nitriding section, decarbonization section, reduction section, independent with the atmosphere that guarantees each section, the convenient atmosphere of controlling each stove section respectively.Final purpose is fast steel band to be heated to best nitriding temperature scope steel plate is carried out nitriding, and form with (Al, Si) N is main inhibitor, N further spreads in decarbonization section, simultaneously with the steel plate decarburization to less than below the 30ppm, at cooling section steel plate is cooled to below 120 ℃.
Nitridation process
Nitriding method of the present invention hangs down the dew point nitriding before decarburization, be mingled with to form effectively.
● the heating zone dew point of nitridation process :-15 ℃～-40 ℃; Preferably control is-20 ℃～-35 ℃
● nitriding temperature: 750～900 ℃;
● nitriding time: 5～50 seconds;
● nitriding medium: NH
3, require to use dried NH
3, dew point is below-40 ℃;
● protective atmosphere: H
2With N
2Mixed gas, H
2Content: 20～75% ,-15 ℃～-40 ℃ of atmosphere dew points (being the nitriding dew point), NH
3Concentration accounts for the gas volume total amount: 0.1～25%;
● nitriding amount: 50～250ppm.The nitriding amount does not have secondary recrystallization during less than 50ppm, and magnetic induction density B 8 is low, and the nitriding amount is during greater than 250ppm because nitrogen content is too high, during high temperature annealing AlN, SiN decompose emit between substrate and Magnesium Silicate q-agent, form bubble, expose matrix.
Decarburizing annealing
In the carbon rejection process after nitriding is finished, decarburizing annealing temperature according to routine, control 50 ℃～75 ℃ of high dew points, be preferably in 70～75 ℃ dew point, finish carbon rejection process carbon and reduce to, formed the separant that helps with based on MgO at surface of steel plate simultaneously and carried out zone of oxidation FeO, the SiO that solid state reaction generates the magnesium silicate glass film less than 30ppm
2, and the nitrogen that infiltrates surface of steel plate also continuing diffusion, and forms and be mingled with based on (Al, Si) the favourable of N, to the restraining effect of having grown up of a crystal grain, is convenient to carry out the adjustment of grain structure.
The preparation and the The high temperature anneal of MgO separant slurries
Utilize aquation rate (Hydrability) to make high temperature annealing separant slurries at the special-purpose magnesium oxide of 1.5～6% silicon steel, in 100 parts of MgO, add a kind of or more than two kinds weight percent be 0.1～10% Na, K, Zn, Ca, Cr, Zr, Sr, Ti, Sb muriate, sulfide, oxide compound, all the other additives are the additive of the conventional usefulness of oriented silicon steel.And be coated in oriented silicon steel surface after nitriding processing and the decarburizing annealing, carry out 200～400 ℃ oven dry, enter again in the high-temperature annealing furnace according to the high-temperature annealing process of the routine purifying treatment of annealing, first half of high temperature annealing through the Mg (OH) in the separant of oven dry
2And TiO
2Discharge oxygen and an amount of moisture content of moisture release Deng compound, improved the oxygen position in the coil of strip lamellar spacing, FeO increases, MgO increased to the Liquid Phase Diffusion area of matrix when glassy membrane was formed, the temperature that glassy membrane begins to form reduces, can prevent to absorb nitrogen too much in the atmosphere, help forming fine glass has guaranteed to be formed on surface of steel plate in the decarburizing annealing process Fe
2SiO
4Be not reduced, thereby guarantee to obtain excellent Magnesium Silicate q-agent bottom and excellent magnetism energy.
Compare with the method that has traditional low-temperature heat production oriented silicon steel now, beneficial effect of the present invention shows as:
1) nitriding efficient height, the steel plate nitriding does not have the influence of surface film oxide;
2) You Yi MgO coating formula, it is good, even that the Magnesium Silicate q-agent bottom is formed, and obtains good magnetic performance.
3) owing to formed the enforcement that uniform bottom has guaranteed smooth annealing of subsequent thermal and insulating coating.
Embodiment
With the steel-making of 500kg vacuum oven, the chemical ingredients of smelting:
C: Si≤0.065% :≤3.5%, Als≤0.035%, Mn :≤0.20%, Cu≤0.12%, Sn≤0.15%, and control few N, S technology composition, form blank plates of silicon steels.
● blank plates of silicon steels is in heating below 1280 ℃;
● the cooling of 1150 ℃ of normalizing conditions * 5s+930 ℃ * 70s+50 ℃/s, cold rolling of strip steel be to 0.30mm, 850 ℃ of nitridings, heating zone dew point :-15 ℃～-40 ℃;
● nitriding time: 5～50 seconds;
● nitriding medium: NH
3, require to use dried NH
3, dew point is below-40 ℃;
● protective atmosphere: H
2With N
2Mixed gas, H
2Content: 20～75% ,-15 ℃～-40 ℃ of atmosphere dew points (being the nitriding dew point), NH
3Concentration accounts for gas gross: 0.1～25%;
The about 170ppm of nitriding target, 50 ℃～75 ℃ of the dew points of decarburizing annealing, utilize the special-purpose MgO of special silicon steel, its aquation rate (Hydrability) is 1.5～6%, make high temperature annealing separant slurries, the prescription of slurries is in 100 parts of MgO, add 1～10% a kind of or two kinds of Na, K, Zn, Ca, Zr, Sr, Ti, Sb muriate, sulfide, oxide compound, all the other additives are the additive of the conventional usefulness of oriented silicon steel, carry out after the coating carrying out high temperature annealing again after the drying, measure magnetic and coating tack, and observe surface quality.
Dew point is as shown in table 1 to the influence of nitriding amount:
The relation of table 1 dew point and nitriding amount
| Numbering | The heating zone dew point (℃) | The nitriding dew point (℃) | Nitriding amount (ppm) |
| 1 | -15 | -15 | 102 |
| 2 | -20 | -30 | 162 |
| 3 | -25 | -25 | 158 |
| 4 | -35 | -30 | 170 |
| 5 | -40 | -40 | 194 |
The relation of nitriding time and nitriding amount is as shown in table 2:
The relation of table 2 nitriding time and nitriding amount
| Numbering | NH 3Dew point | NH 3Concentration % | Nitriding time (s) | Nitriding amount (ppm) |
| 1 | ＜-40℃ | 0.1 | 20 | 46 |
| 2 | ＜-40℃ | 5 | 30 | 64 |
| 3 | ＜-40℃ | 10 | 5 | 54 |
| 4 | ＜-40℃ | 20 | 15 | 89 |
| 5 | ＜-40℃ | 15 | 25 | 178 |
| 6 | ＜-40℃ | 20 | 35 | 203 |
| 7 | ＜-40℃ | 25 | 50 | 287 |
Annotate: NH
3Concentration % be meant NH
3Volume accounts for the percentage ratio % of total shielding gas volume
The relation of nitriding amount and magnetic is as shown in table 3:
The relation of table 3 nitriding amount and magnetic
| Numbering | Nitriding amount (ppm) | B8(T) | P1.7/50(w/kg) |
| 1 | 50 | 1.429 | 2.16 |
| 2 | 145 | 1.931 | 0.95 |
| 3 | 150 | 1.915 | 0.98 |
| 4 | 250 | 1.894 | 1.09 |
| 5 | 108 | 1.902 | 1.01 |
The relation of decarburization dew point and magnetic is shown in Table 4:
The relation of table 4 decarburization dew point and magnetic
| Numbering | Decarburization dew point ℃ | B8(T) | P1.7/50(w/kg) |
| 1 | 50 | 1.581 | 2.56 |
| 2 | 68 | 1.930 | 0.95 |
| 3 | 65 | 1.921 | 0.98 |
| 4 | 70 | 1.912 | 1.03 |
| 5 | 75 | 1.907 | 1.08 |
The relation of MgO aquation rate and bottom surface state and tack is shown in Table 5:
The relation of table 5MgO aquation rate and bottom surface state and tack
| Numbering | MgO aquation rate % | The bottom tack | Condition of surface |
| 1 | 2.8 | ○ | ○ |
| 2 | 6 | ◎ | ○ |
| 3 | 5.1 | ◎ | ◎ |
| 4 | 4 | ◎ | ◎ |
| 5 | 1.5 | △ | △ |
The relation of additive and bottom surface state and tack is shown in Table 6 among the MgO:
The relation of additive and bottom surface state and tack among the table 6MgO
| Numbering | MgO aquation rate % | (ZrO/MgO)*100 | The bottom tack | Condition of surface |
| 1 | 4 | 0.1 | ○ | ○ |
| 2 | 3.5 | 2.5 | ◎ | ◎ |
| 3 | 3.2 | 3 | ◎ | ◎ |
| 4 | 3.0 | 2 | ◎ | ◎ |
| 5 | 3.3 | 7 | ◎ | ○ |
| Numbering | MgO aquation rate % | (Cr 2O3/MgO)*100 | The bottom tack | Condition of surface |
| 1 | 5.2 | 0.5 | ○ | ○ |
| 2 | 4.2 | 1.5 | ◎ | ◎ |
| 3 | 3.6 | 2.2 | ◎ | ◎ |
| 4 | 3.1 | 4.0 | ◎ | ○ |
| 5 | 3.3 | 8 | ◎ | △ |
The additive add-on among the MgO and the relation of bottom surface state and tack are shown in Table 7:
The additive add-on among the table 7MgO and the relation of bottom surface state and tack
| Numbering | Additive add-on % | The bottom tack | Condition of surface |
| 1 | 0.1 | ○ | ○ |
| 2 | 2 | ◎ | ◎ |
| 3 | 4 | ◎ | ◎ |
| 4 | 7 | ◎ | ○ |
| 5 | 10 | ○ | ○ |
Annotate: the test method of tack: tighten the subsides scotch tape in test with the orientation steel plate, use
Crooked 180 ° of 10mm rod sample flattening, again with tape stripping, is judged the area that peels off that sticks to the adhesive tape upper nonconductive Film.◎: do not have and peel off; Zero: minute quantity is peeled off; △: peel off on a small quantity; *: peel off in a large number.
Claims (4)
1. the method for oriented silicon steel is produced in a low-temperature heat, mainly comprise: will heat below 1280 ℃ with the directional silicon steel slab of common explained hereafter, hot rolling then, carry out once or secondary cold-rolling obtains the finished product thickness of slab, carrying out first nitriding again handles, back decarburizing annealing, coating separant, carry out final high temperature annealing at last, it is characterized in that
In nitridation process, the heating zone dew point is controlled at-15 ℃～-40 ℃; At 750 ℃～900 ℃ following nitriding times of conventional nitriding temperature is 5～50 seconds; Nitriding medium is NH
3, dew point is controlled at below-40 ℃; Protective atmosphere is H
2And N
2Mixed gas, the atmosphere dew point is at-15 ℃～-40 ℃;
In follow-up decarburizing annealing technology, under conventional decarburizing annealing temperature, the atmosphere dew point is controlled at 50～75 ℃;
In coating separant technology, utilize the aquation rate to make the annealing separating agent slurries at the special-purpose MgO of 1.5～6% silicon steel, and in the slurries of separant, adding is oxide compound or the salt of 0.1～10% a kind of or Na, K more than two kinds, Zn, Ca, Cr, Zr, Sr, Ti, Sb with respect to the weight percent of MgO weight, and the slurries of making are coated on the surface of steel plate after the nitriding decarburization.
2. method according to claim 1 is characterized in that, percentage calculation by volume, the NH in the protective atmosphere
3Account for 0.1～25% of gas gross.
3. method according to claim 1 is characterized in that, in described nitridation process, and-20 ℃～-35 ℃ of heating zone dew point controls.
4. method according to claim 1 is characterized in that, in decarburizing annealing technology, the atmosphere dew point is controlled at 70～75 ℃.
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|---|---|---|---|
| CNB2005101108993A CN100455702C (en) | 2005-11-29 | 2005-11-29 | Method for producing oriented silicon steel with good bottom by low-temperature heating |
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|---|---|---|---|
| CNB2005101108993A CN100455702C (en) | 2005-11-29 | 2005-11-29 | Method for producing oriented silicon steel with good bottom by low-temperature heating |
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| Publication Number | Publication Date |
|---|---|
| CN1978707A CN1978707A (en) | 2007-06-13 |
| CN100455702C true CN100455702C (en) | 2009-01-28 |
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| CN101333619B (en) * | 2007-06-25 | 2010-10-13 | 宝山钢铁股份有限公司 | Technological process for controlling secondary recrystallization crystal particle dimension of oriented silicon steel |
| CN101545072B (en) | 2008-03-25 | 2012-07-04 | 宝山钢铁股份有限公司 | Method for producing oriented silicon steel having high electromagnetic performance |
| CN101638766B (en) * | 2008-07-28 | 2011-03-30 | 宝山钢铁股份有限公司 | Method and device for spraying silicic acid produced from oriented silicon steel having good bottom layer |
| CN101845582B (en) * | 2009-03-26 | 2011-09-21 | 宝山钢铁股份有限公司 | Production method of high magnetic induction oriented silicon steel |
| CN102443736B (en) * | 2010-09-30 | 2013-09-04 | 宝山钢铁股份有限公司 | Method for producing high magnetic flux-density oriented silicon steel product |
| CN102286659B (en) * | 2011-03-24 | 2013-10-16 | 北京中钢贸科技发展有限公司 | Method for improving magnetic properties of cold rolling non-oriented silicon steel |
| CN103114181A (en) * | 2013-01-24 | 2013-05-22 | 广东盈泉钢制品有限公司 | Coating formula of oriented silicon steel barrier coat |
| 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 |
| CN110643796B (en) * | 2019-11-13 | 2021-06-15 | 武汉钢铁有限公司 | Preparation method of high-magnetic-induction oriented silicon steel with good bottom layer adhesion |
| 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 |
| CN112030168B (en) * | 2020-08-18 | 2022-10-04 | 武汉钢铁有限公司 | Process method for improving surface bright spot defect of nitriding oriented silicon steel |
| CN112522613B (en) * | 2020-11-19 | 2021-12-14 | 武汉钢铁有限公司 | High-magnetic-induction oriented silicon steel with excellent bottom layer quality and production method thereof |
| CN112941286B (en) * | 2021-01-29 | 2022-07-08 | 武汉钢铁有限公司 | High-magnetic-induction oriented silicon steel manufacturing method for improving effective nitrogen and bottom layer quality |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05112827A (en) * | 1988-04-25 | 1993-05-07 | Nippon Steel Corp | Manufacture of grain-oriented silicon steel sheet excellent in magnetic property and coating film pr0perty |
| CN1125773A (en) * | 1994-05-13 | 1996-07-03 | 新日本制铁株式会社 | Anneal isolating objects with good reactivity and used for silica steel sheet |
| JP2000273550A (en) * | 1999-03-26 | 2000-10-03 | Nippon Steel Corp | Glass coating film and production of grain oriented silicon steel sheet excellent in magnetic property |
-
2005
- 2005-11-29 CN CNB2005101108993A patent/CN100455702C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05112827A (en) * | 1988-04-25 | 1993-05-07 | Nippon Steel Corp | Manufacture of grain-oriented silicon steel sheet excellent in magnetic property and coating film pr0perty |
| CN1125773A (en) * | 1994-05-13 | 1996-07-03 | 新日本制铁株式会社 | Anneal isolating objects with good reactivity and used for silica steel sheet |
| JP2000273550A (en) * | 1999-03-26 | 2000-10-03 | Nippon Steel Corp | Glass coating film and production of grain oriented silicon steel sheet excellent in magnetic property |
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