CN103572157A - Production method for improving insulating property by adding trace elements in oriented silicon steel barrier-coat - Google Patents
Production method for improving insulating property by adding trace elements in oriented silicon steel barrier-coat Download PDFInfo
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Abstract
The invention discloses a production method for improving the insulating property by adding trace elements in an oriented silicon steel barrier-coat. The production method comprises the following steps of smelting, processing in vacuum, refining and continuously casting into a blank; carrying out hot rolling; normalizing and acid pickling; carrying out once cold rolling, wherein the reduction rate is greater than or equal to 82%; decarbonizing and annealing, wherein the temperature is 750-890 DEG C, the atmosphere dew-point temperature is 25-75 DEG C, the decarbonization time is 90-350 seconds, and the total oxygen [O] of the surface of a steel belt is greater than or equal to 170/t and less than or equal to 315/t; coating a magnesium oxide coating added with trace elements on the surface of the steel belt; carrying out high temperature annealing, wherein the atmosphere dew-point temperature is less than or equal to 30 DEG C, two low thermal insulation steps and one high thermal insulation step are arranged, and the nitridation amount of nitrogen is greater than or equal to 16ppm; stretching and smoothing and annealing, namely, coating, annealing and smoothing. In high temperature annealing stage, silicon dioxide and magnesium oxide on the surface of the steel belt carry out chemical reaction so as to generate a magnesium silicate bottom layer, and additives are added into the magnesium oxide coating so as to help to obtain excellent finished product magnetism and good magnesium silicate bottom layer.
Description
Technical field
the invention belongs to oriented silicon steel production field, relate in particular to the production method of adding trace element, raising insulating property in oriented silicon steel barrier coat.
Background technology
1, the production method of general cold-rolled orientation silicon steel is as follows traditionally:
(1), with converter (or electric furnace) steel-making, carry out vacuum-treat, composition refining and alloying, continuous casting becomes slab, its basic chemical composition is: Si(2.5～5.0), C(0.01～0.10), Mn(0.02～0.10), S(0.01～0.05), Als(0.01～0.05), N(0.003～0.015), some composition systems also contain one or more in the elements such as Mo, Sb, Cr, B, Bi, all the other are iron and inevitable impurity element, and product also may contain Cu sometimes;
(2), before slab hot rolling, in special heating furnace, be heated to the temperature of 1400 ℃ of left and right, and carry out above insulation in 30 minutes, make the abundant solid solution of favourable inclusion, to separate out Second Phase Particles tiny, disperse in silicon steel matrix in course of hot rolling subsequently---be inhibitor;
(3), after Hot Rolled Plate Normalizing (or not normalizing), carry out pickling, remove the iron scale of steel strip surface;
(4) (in traditional method, mostly general oriented silicon steel is cold rollingly just can roll finished product thickness with twice, by twice cold-rolling practice comprising process annealing, to roll finished product thickness, so need there is process annealing between cold rolling twice, have now a kind of high magnetic induction grain-oriented silicon steel can be with a rolling);
(5), carry out decarburizing annealing and coating and take the annealing separating agent that magnesium oxide is main component, in magnesium oxide coating, add the additives such as kind is suitable, quantity is appropriate Ti, B, Sb, and the carbon in steel plate is taken off to the level of finished product magnetic that do not affect (generally should below 30ppm);
(6), in high-temperature annealing process, occur successively: MgSiO
4the formation reaction of bottom (generating after the magnesium oxide of coating and the silicon dioxde reaction of surface of steel plate), the generation of secondary recrystallization, grow and grow up, (this stage is the final stage in high-temperature annealing process part to purify steel, element except iron and silicon in silicon steel is removed totally as much as possible, be included in oriented silicon steel production process above as favourable be mingled with protected and before secondary recrystallization occurs as the N of inhibitor integral part, the compositions such as S) physical-chemical reaction, acquisition orientation degree is high, iron loss low and surface coverage have evenly, the cold-rolled orientation silicon steel of fine and close silver gray Magnesium Silicate q-agent bottom,
, at steel strip surface coating insulating coating and carry out stretching and leveling annealing, obtain the oriented silicon steel of commercial applications form.
2, the distinguishing feature of the production method of the general cold-rolled orientation silicon steel of tradition has:
(1), inhibitor starts just to form from steel-making, in each operation, to adjust it, control subsequently, owing to carrying out successively middle inhibitor in each operation, lose, must made up by rights, to play a role to crucial moment, after having acted on, to from steel, remove;
(2) the slab heat, before hot rolling, Heating temperature, up to 1400 ℃ of left and right, is the Limiting Level of general process furnace, it is also the limit of existing hot rolling technology that the cooling of hot-rolling line is controlled;
(3), the key of production technology is to control tissue, the texture of each stage steel plate of each operation, and the form of inhibitor, quantity and behavior;
, because slab heating temperature is high, process furnace needs frequent repairing, utilising efficiency is low, steel billet scaling loss is large simultaneously, energy consumption is high, hot rolling crimping splits greatly, causes cold rolling process to be produced difficult, lumber recovery is low, comprehensive cost is high;
, the complex manufacturing of the general cold-rolled orientation silicon steel of high temperature heating of plate blank, with high content of technology, investment of production equipment is large.This technology is through the development of over half a century, very ripe, for very large contribution has been made in the development of electric power, electronic industry, but just because of its complex manufacturing, with high content of technology, the blockade on new techniques between investment of production equipment great He manufacturing enterprise, has limited the very fast development of its output, especially the country of rapid economic development as China, can not meet the market requirement of quick increase toward contact.
3, relevant improvement and patented technology
In order to address these problems, in long-term production practice and in research work, people grope and have developed some successful ways, are now summarized as follows:
(1), the method of introducing in Japanese patent laid-open 5-112827, its chemical composition is: [C] 0.025～0.075%, Si2.90～4.50%, S≤0.012%, Als0.010～0.060%, N≤0.010%, Mn0.08～0.45%, P0.015～0.045%, all the other are Fe and inevitable inclusion, after 1200 ℃ of following heating of slab, carry out hot rolling, just time cold rolling or be rolled down to final finished thickness with more than twice method of process annealing with one, after decarburizing annealing, steel band carries out continuous nitriding in traveling process, after general painting magnesium oxide separant, carry out high temperature annealing, the all good oriented silicon steels of production magnetic and bottom layer quality.Continuous nitriding method: protective atmosphere is the mixed gas of hydrogen and nitrogen, wherein NH
3content is more than 1000ppm, and oxygen gesture is that PH2O/PH2≤0.04 nitriding temperature is 500～900 ℃.
⑵, Korea S POSCO Co., Ltd., its low-temperature oriented silicon steel chemical composition is: [C] 0.020～0.045%, Si2.90～3.30%, S≤0.006%, Als0.005～0.019%, N0.003～0.008%, Mn0.05～0.30%, Cu0.30～0.70%, Ni0.30～0.70%, Cr0.30～0.70%, all the other are Fe and inevitable impurity, in addition, in steel, contain B0.001～0.012%.Decarburization and nitriding are carried out simultaneously, nitriding in wet atmosphere.The basis of the method is to take BN as main inhibitor.
(3), the patent of Chinese Baosteel application method as described in ZL200410099080.7 and CN101768697 A is before decarburization that nitriding or decarburization and high temperature annealing two-step all need nitriding simultaneously.
By inquiry and analysis to the patent of the domestic and international producing oriented silicon steel by heating low temperature casting blank based on nitridation process, document etc., can find: because the mode of low temperature heating of plate blank causes in silicon strip when original inhibitor has arrived 1000 ℃ of left and right of high-temperature annealing, seem inadequate, must by nitriding, be supplemented rear operation (must be before 1020 ℃ of high temperature annealings), namely increased (Al, Si) N novel inhibitors.But the process of nitriding again can not be influential to the formation reaction of Magnesium Silicate q-agent bottom, it is simple can guarantee the stable and even of nitriding that the process of nitriding is wanted, and everything is all to guarantee that cold-rolled orientation silicon steel has the primary condition of good magnetic and surperficial Magnesium Silicate q-agent bottom, the present invention solves these problems preferably.
Summary of the invention
Owing to producing general cold-rolled orientation silicon steel technology with high temperature heating of plate blank, have that energy consumption is high, spillage of material is high, Edge of Steel Strip splits greatly, productivity is bad and high in cost of production inherent defect, low temperature slab heating technique is produced general cold-rolled orientation silicon steel and can be addressed these problems preferably, thereby has powerful exploitation power.From current disclosed patent documentation and relevant technical information by low temperature slab heating technique, produce general cold-rolled orientation silicon steel, be nearly all based upon on nitridation process basis.
The object of the present invention is to provide a kind of method of producing general cold-rolled orientation silicon steel by once cold rolling method, by carrying out Hot Rolled Plate Normalizing annealing process, especially
in oriented silicon steel barrier coat, add the production method of trace element, raising insulating property, the present inventionutilize the special time period nitriding before slab final magnetic behavior when high temperature annealing forms, to form enough (Al, Si) N is favourable, be mingled with, utilize its restraining effect to primary recrystallization crystal grain, impel the growing up of secondary recrystallization crystal grain, growth and perfect, in magnesium oxide coating, add kind additive suitable, that quantity is appropriate, be conducive to obtain good finished product magnetic and good Magnesium Silicate q-agent bottom.Overcome in other patent and used the detrimentally affect of ammonia nitriding to Magnesium Silicate q-agent bottom, overcome in decarburizing annealing and this two-step of high temperature annealing simultaneously and all needed nitriding to bring being difficult in operation and in nitriding amount to control.
In order to achieve the above object, technical scheme of the present invention is:
Of the present invention
in oriented silicon steel barrier coat, add the production method of trace element, raising insulating property, comprise the steps:
(1), smelt
With converter (or electric furnace), make steel, molten steel is carried out to vacuum-treat, composition refining and Alloying Treatment, then continuous casting becomes slab, its basic chemical composition is (unit is weight percentage): Si(2.5～5.0), C(0.01～0.10), Mn(0.02～0.10), S(0.01～0.05), Als(0.01～0.05), N(0.003～0.015), in some composition systems, also contain Mo, Sb, Cr, etc. one or more in element, all the other are iron and inevitable impurity element, and this product is generally containing Cu;
(2), hot rolling
Before slab hot rolling, in silicon steel special heating furnace, be heated to the temperature of 1180-1300 ℃, and carry out the insulation of 30 minutes above (at least 30 minutes), make the abundant solid solution of favourable inclusion, to separate out tiny in course of hot rolling subsequently in silicon steel matrix, the Second Phase Particles of disperse---is inhibitor---, and this is the prerequisite of guaranteeing that oriented silicon steel had not only had good surface insulation performance but also had good inherent magnetic, be with magnesium oxide coating of the present invention in Additive complementary, otherwise surface insulated preferably and magnetic has reduced this and has not just been oriented silicon steel.
Adopt low temperature heating of plate blank, the Heating temperature of directional silicon steel slab is at 1180-1300 ℃, and to be that hot rolled coil is boundless split its advantage, and productivity is good, process furnace long service life, and silicon steel lumber recovery is high; Its shortcoming is that favourable to be mingled with solid solution abundant not, and the amount of inhibitor is effectively supplemented by oozing N in rear operation;
(3), normalizing adds pickling
Hot Rolled Plate Normalizing is annealed and is carried out pickling, removes the iron scale of steel strip surface; Normalizing annealing temperature: 1050～1185 ℃ of (1～20s)+850～980 ℃ (30～180s), speed of cooling: 60 ℃/s～10 ℃/s; Acid washing conditions: pickling in the hydrochloric acid soln of 5% left and right;
(4), cold rolling
By once cold rolling (or twice), from hot-rolled sheet thickness, roll finished product thickness, cold rolling draft >=82%.Heavy reduction rate significantly increases the dislocation desity in steel band interior tissue, the a large amount of dislocations and the goss texture that produce, the forming core that is conducive to Gauss's nucleus, as long as there are enough favourable existence that is mingled with when high temperature annealing operation secondary recrystallization occurs, these Gauss's nucleus just can develop into perfect secondary recrystallization;
(5), decarburizing annealing
After the cold rolling silicon strip that obtains finished product thickness is carried out to decarburizing annealing and be coated with magnesium oxide coating, described magnesium oxide coating take for adopting the annealing separating agent coating that magnesium oxide is main component, and described annealing separating agent comprises MgO, B and TiO
2, be wherein added with the B of the 0.01-0.10%wt that accounts for annealing separating agent quality, account for the TiO of 0.01-0.30%wt of annealing separating agent quality
2and 0 Bi that is less than or equal to 0.2%wt that is more than or equal to that accounts for annealing separating agent quality, in magnesium oxide coating, added kind element suitable, that quantity is appropriate, and decarburization temperature controlling range: 750～890 ℃, protective atmosphere is hydrogen, nitrogen mixture gas, H2 content accounts for 15～80%, 25～75 ℃ of protective atmosphere dew points; Decarburization time: 90～350 seconds, and the carbon in steel plate is taken off to the level of finished product magnetic that do not affect (generally should below 30ppm); The de-total oxygen of steel strip surface [O]: 170/t≤[O]≤315/t(t is steel band actual (real) thickness mm); The interpolation trace element of above-mentioned steps of the present invention, makes its effect of playing the enough silicon-dioxide in protection silicon strip surface before Magnesium Silicate q-agent bottom generates, is conducive to form the Magnesium Silicate q-agent bottom of silicon strip surface uniform, densification.
Add trace element, when the formation reaction of Magnesium Silicate q-agent bottom is carried out, can promote silicon-dioxide and magnesium oxide coating fully to react, add micro-ly, after Magnesium Silicate q-agent bottom forms, make bottom take root deeply in matrix steel band and there is good tack.
By testing, determine that suitable trace element the best adds mode and the method for masking liquid; Test and the suitable trace element of optimizing optimum matching.
Above-mentioned annealing separating agent adopts qualified silicon steel special magnesium oxide formulated, wherein added the 0.01-0.10%wt that accounts for annealing separating agent quality B, be greater than 0 and be less than or equal to the Bi of 0.2%wt and the TiO of 0.01-0.30%wt
2.
(6), high temperature annealing
(first is 600 ℃ of < in high temperature annealing operation, to adopt two steps, second 700 ℃ of <) low temperature insulation and only have the soak (purification steel) of a step, at the low temperature holding stage of second step with in being warmed up to the process before 1020 ℃, in stove, adopt pure N
2gas is made shielding gas, and steel band is carried out to nitriding, the dew point requirement of logical people's purity nitrogen≤-60 ℃, and the dew point of furnace atmosphere requires≤30 ℃;
In high-temperature annealing process, occur successively: MgSiO
4the formation reaction of bottom (magnesium oxide of coating and the silicon dioxde reaction of surface of steel plate generate), the generation of secondary recrystallization, growth and growth, (this stage is the final stage in high-temperature annealing process part to purify steel, element except iron and silicon in silicon steel is removed totally as much as possible, be included in oriented silicon steel production process above as favourable be mingled with protected and before secondary recrystallization occurs as the compositions such as N, S of inhibitor integral part) physical-chemical reaction, obtain the cold-rolled orientation silicon steel that orientation degree is high, iron loss is low;
(7), stretching and leveling annealing
Stretching and leveling annealing process routinely carries out.
The remarkable advantage of the inventive method:
(1) in hot-rolled step of the present invention, adopt low temperature heating of plate blank, the Heating temperature of directional silicon steel slab is 1200 ℃ of left and right, and to be that hot rolled coil is boundless split its advantage, and productivity is good, process furnace long service life, and silicon steel lumber recovery is high; Its shortcoming is that favourable to be mingled with solid solution abundant not, and the amount of inhibitor need to be supplemented by oozing N in rear operation;
Use in cold rolling step of the present invention once (or twice) cold-rolling practice directly from hot-rolled sheet thickness, roll finished product thickness, heavy reduction rate significantly increases the dislocation desity in steel band interior tissue, the a large amount of dislocations that produce and the formation that is conducive to goss texture, the forming core that is conducive to Gauss's nucleus, when high temperature annealing operation secondary recrystallization occurs, had enough favourable existence that is mingled with, this just can develop into perfect (110) [001] secondary recrystallization tissue;
(3) in decarburizing annealing step of the present invention, in magnesium oxide coating, add suitable trace element; make it before Magnesium Silicate q-agent bottom generates, play the effect of the enough silicon-dioxide in protection silicon strip surface; when carrying out, the formation reaction of Magnesium Silicate q-agent bottom can promote silicon-dioxide and magnesium oxide coating fully to react; after Magnesium Silicate q-agent bottom forms, make bottom take root deeply in matrix steel band and there is good tack, thus the whole Magnesium Silicate q-agent bottom layer quality that improves silicon strip surface.
(4) (first is 600 ℃ of < in high temperature annealing operation of the present invention, to adopt two steps, second 700 ℃ of <) low temperature insulation and the soak (purifying the steel of silicon strip) of a step, the low temperature holding stage of second step be warmed up to the process before 1020 ℃ in adopt pure N in stove
2gas is made shielding gas, and steel band is carried out to nitriding, the dew point requirement of logical people's purity nitrogen≤-60 ℃, and the dew point of furnace atmosphere requires≤30 ℃; The object of now nitriding is the amount that increases inhibitor, make to have in silicon strip sufficient amount favourable be mingled with to protect be about to or ongoing secondary recrystallization completes smoothly and grows perfect, inhibitor just forms when steel-making, in hot rolling and change form and lose in each operation subsequently, need suitably to supplement, this role of nitriding is constantly exactly first complete inhibitor (Al, Si) N etc., so that improve secondary recrystallization; The major ingredient of evidence inhibitor---AlN, MnS, SiN etc.
5) feature of nitriding is here directly with purity nitrogen, to ooze, not to carry out nitriding (having avoided the many disadvantageous effects with ammonia nitriding) with ammonia, in the high temperature annealing stage, under the prerequisite that does not increase total annealing cycle, increase a low temperature insulation step, second low holding stage and 1020 ℃ of temperature rise periods before form logical purity nitrogen nitriding, this role of respective stage while still having played high temperature annealing in nitriding; The nitriding here neither carry out nitriding with hydrogen, nitrogen mixture gas as the patent Introduction having, but with purity nitrogen, neither, in decarburizing annealing and high temperature annealing nitriding simultaneously, only at high temperature annealing, in earlier stage carry out.The opportunity of nitriding, nitriding amount etc. are all only for an object---and strengthening inhibitor is in secondary recrystallization stage performance effect fully, so in advance little in operation nitriding role above.After secondary recrystallization body completes, the historic mission of inhibitor also just completes, and now its effect in oriented silicon steel is from changing into harmful being mingled with original favourable being mingled with.Because in oriented silicon steel finished product, except iron and silicon, other elements all have inhibition to magnetic history more or less in existence, so unfavorable to the magnetic of material.And in oriented silicon steel, to have the elements such as a certain amount of carbon, manganese, sulphur, aluminium in steel-making, this is the needs for middle Working Procedure Controlling---its object only has one: develop and improve secondary recrystallization---, and this is that cold-rolled orientation silicon steel is peculiar, is also the why good reason of magnetic of oriented silicon steel.
Embodiment
described in specification sheets of the present invention or claimsthe meaning that wt% or %wt are all weight percentage.
in oriented silicon steel barrier coat of the present invention, add the production method of trace element, raising insulating property,comprise the steps: (1) to smelt, vacuum-treat, refining continuous casting become base; (2) hot rolling; (3) normalizing adds pickling; (4) once cold rolling draft>=82%; (5) 830 ℃ of decarburizing annealing temperature, atmosphere dew point: 50 ℃, decarburization time: 200 seconds, steel strip surface total oxygen demand: [O] is 200/t, then added micro-magnesium oxide coating in steel strip surface coating; (6) high temperature annealing, 5 ℃ of atmosphere dew points, high temperature annealing arranges the high insulation of the gentle step of minimum living of two steps, N air infiltration nitrogen amount 20ppm; (7) stretching and leveling annealing.
Concrete steps are:
(1) smelt
Molten steel is carried out to vacuum-treat, composition refining and Alloying Treatment, then continuous casting becomes directional silicon steel slab, basic chemical composition in its directional silicon steel slab drops on by weight percentage in following scope Si and is 2.5-5.0%, C is 0.01-0.10%, Mn is 0.02-0.10%, S is 0.01-0.05%, sour molten aluminium Als is 0.01-0.05%, N is 0.003-0.015%, and all the other are iron and impurity; The table 1 of embodiment one during concrete enforcement;
(2) hot rolling
Directional silicon steel slab is heated to the temperature (while specifically implementing, its concrete Heating temperature is in Table 2) of 1180-1300 ℃ before hot rolling, in silicon steel special heating furnace, and carry out the insulation of 40 minutes, be conducive to the abundant solid solution of inclusion wherein, to separate out Second Phase Particles (being inhibitor) tiny, disperse in silicon steel matrix in course of hot rolling subsequently; Directional silicon steel slab adopts low-temperature heat, and its Heating temperature forms hot-rolled sheet (while specifically implementing, its concrete finishing temperature is in Table 2) at 1180-1300 ℃, and the amount of inhibitor is effectively supplemented by oozing N in rear operation;
(3) normalizing adds pickling
Hot Rolled Plate Normalizing is annealed and is carried out pickling, removes the iron scale of steel strip surface; Normalizing annealing step is: in temperature, be first that 1050-1185 ℃ of normalizing annealings, normalizing annealing time are 1-20s, in temperature, be that 850-980 ℃ of normalizing annealings, normalizing annealing time are 30-180s again, after normalizing annealing, carry out cooling, speed of cooling: 60 ℃/s-10 ℃/s (while specifically implementing, its specific experiment data are shown in described in 3 steps of following embodiment); The acid washing conditions carrying out after normalizing annealing: pickling in the hydrochloric acid soln of 5wt%;
(4) cold rolling
By cold-rolling practice once or twice, the thickness of hot-rolled sheet is rolled to the silicon strip of finished product thickness, cold rolling draft >=82%; Heavy reduction rate significantly increases the dislocation desity in steel band interior tissue, and a large amount of dislocations and the goss texture of generation are conducive to the forming core of Gauss's nucleus, and Gauss's nucleus just can develop into perfect secondary recrystallization;
(5) decarburizing annealing
To the cold rolling silicon strip that obtains finished product thickness, carry out after decarburizing annealing and the annealing separating agent that magnesium oxide is main component is take in coating, described annealing separating agent comprises Mgo composition, and the additive of the new interpolation in the additive in following embodiment and content interval fall into following scope: be wherein added with B 0.01-0.10%wt and/or Bi≤0.2%wt and TiO
20.01-0.30%wt, while specifically implementing, concrete additive and content are shown in the table 4 of following embodiment; Its temperature controlling range of described decarburizing annealing: 750-890 ℃, protective atmosphere is hydrogen, nitrogen mixture gas, wherein H
2content accounts for 15-80 wt%, and the dew-point temperature of protective atmosphere is 25-75 ℃; Decarburization time: 90-350 second, and the carbon in silicon strip is taken off below 30ppm; The de-total oxygen of steel strip surface [O] reaches in following scope: 170/t≤[O]≤315/t, and wherein t is silicon strip actual (real) thickness mm;
(6) high temperature annealing
In high temperature annealing operation, adopt the low temperature insulation of two steps and only have the soak of a step to purify the steel of silicon strip, the low temperature holding temperature 400-600 ℃ of first step, the low temperature holding temperature of second step is 650-800 ℃; The low temperature holding stage of second step and be warmed up to the intensification before 1020 ℃ process in, in its stove, adopt pure N
2gas is made shielding gas, and silicon strip is carried out to nitriding, the dew point requirement of logical people's purity nitrogen≤-60 ℃, and the dew point of furnace atmosphere requires≤30 ℃;
(7) stretching and leveling annealing.
Following embodiment all tests by above-described step (1)-(7).
embodiment mono-:
1, with 500 kilograms of vacuum ovens, according to the method for step (1), smelt steel-making and obtain A and two kinds of ultimate constituents of B of table 1, and by the method hot rolling of step (2), the concrete optimum condition of hot rolling is as table 2:
Table 1, experimental steel steel-making composition (wt%)
Table 2, experimental steel hot-rolled condition (℃)
2, by step (3) normalizing, add acid pickling step and carry out, in temperature, be first that 1120 ℃ of normalizing annealings, normalizing annealing time are 5s, then be that 900 ℃ of normalizing annealings, normalizing annealing time are 60s in temperature, after normalizing annealing, carry out cooling, 50 ℃/s of speed of cooling; The acid washing conditions carrying out after normalizing annealing: pickling in the hydrochloric acid soln of 5wt%, its normalizing condition is specifically preferably: 1120 ℃ * 5s+900 ℃ * 60s+50 ℃/s's is cooling;
3, cold rolling by step (4) cold rolling process: to use cold-rolling practice once or twice the thickness of hot-rolled sheet to be rolled to the silicon strip of finished product thickness, cold rolling draft >=82%; Heavy reduction rate significantly increases the dislocation desity in steel band interior tissue, the a large amount of dislocations and the goss texture that produce, the forming core that is conducive to Gauss's nucleus, Gauss's nucleus just can develop into perfect secondary recrystallization, make cold rolling band steel to 0.30mm, by above-mentioned steps (5) mode decarburizing annealing and coating, be added with take after the annealing separating agent that magnesium oxide is main component of suitable interpolation element and carry out the described high temperature annealing of above-mentioned steps (6) and the described conventional stretching and leveling annealing (containing being coated with insulation layer) of above-mentioned steps (7), measure magnetic, experimental result is as table 3:
Table 3, experimental result
aC in table 3 refers to that A in table 1 and the C in table 2 test; AD refers to that A in table 1 and the D in table 2 test;bC
b in finger table 1 and the C in table 2 test;bD
b in finger table 1 and the D in table 2 test.
embodiment bis-:
The steel band obtaining with the A composition in the middle of above-mentioned table 1 and the C hot-rolled condition in table 2 carries out the nitriding experiment in early stage in high temperature annealing stage by above-mentioned method, normalizing annealing through step (3), step (4) cold rolling, the decarburizing annealing of step (5), in magnesium oxide coating, add after different kinds and element of magnitude as shown in table 4 on the impact of the interlamination resistance value of silicon strip surface Magnesium Silicate q-agent bottom, magnesium oxide coating adopts take annealing separating agent that magnesium oxide is main component and makes and form, annealing separating agent weight in table 4 is double centner, described annealing separating agent comprises MgO, B and TiO
2, be wherein added with the B of the 0.01-0.10wt% that accounts for annealing separating agent quality, account for the TiO of 0.01-0.30wt% of annealing separating agent quality
2, and account for annealing separating agent quality be more than or equal to 0 Bi that is less than or equal to 0.2wt%, above-mentioned MgO, B and TiO
2and the weight percent content sum of Bi is 100%.
Table 4 is for adding the relation of different elements and silicon strip surface Magnesium Silicate q-agent bottom interlamination resistance value in double centner MgO annealing separating agent
Aforesaid method of the present invention has solved oriented silicon steel Magnesium Silicate q-agent bottom layer quality inhomogeneous problem in surface when producing with low-temperature heat effectively, and with Japan, the method of the states such as Korea S and comparing with the method for domestic Baosteel etc., the present invention improves the dislocation desity in steel strip substrate by the once cold rolling of heavy reduction, be conducive to the formation of goss texture, coating add during magnesium oxide kind suitable the appropriate element of quantity, and by purity nitrogen, carry out nitriding in the high temperature annealing stage, make to form in steel band (the Al of increase, Si) N, add MnS in steel band etc., what make sufficient amount is favourablely mingled with effective inhibition primary recrystallization tissue, stable to obtaining, perfect secondary recrystallization is organized highly beneficial.Present method is only in abundant nitriding in the early stage of high temperature annealing simultaneously, do not adopt nitriding multiple operation, special to process, do not need nitriding device, to the formation of good Magnesium Silicate q-agent bottom, very favourable to the raising of oriented silicon steel finished product magnetic, from table 4, the interlamination resistance of the known product of the present invention of testing data is obviously greater than comparative example, the B of product of the present invention
8(T) be significantly less than comparative example; The P of product of the present invention
17/50be significantly less than comparative example.
In low temperature slab heating technique and magnesium oxide coating, add certain element and produce the developing direction that oriented silicon steel has represented oriented silicon steel, the facilities and equipments of the inventive method are the conventional equipment of producing oriented silicon steel, and enforcement technology is simple.Thereby there is good popularizing application prospect.
Claims (3)
1. one kind
in oriented silicon steel barrier coat, add the production method of trace element, raising insulating property, comprise the steps: (1) to smelt, vacuum-treat, refining continuous casting become base; (2) hot rolling; (3) normalizing adds pickling; (4) once cold rolling draft>=82%; (5) decarburizing annealing temperature: 750-890 ℃, atmosphere dew point: 25-75 ℃, decarburization time: 90-350 seconds, steel strip surface total oxygen demand: 170/t≤[O]≤315/t, then added micro-magnesium oxide coating in steel strip surface coating; (6) high temperature annealing, atmosphere dew point≤30 ℃, high temperature annealing arranges the high insulation of the gentle step of minimum living of two steps, N air infiltration nitrogen amount>=16ppm; (7) stretching and leveling annealing.
2. one kind
in oriented silicon steel barrier coat, add the production method of trace element, raising insulating property, comprise the steps:
1) smelt
Molten steel is carried out to vacuum-treat, composition refining and Alloying Treatment, then continuous casting becomes directional silicon steel slab, basic chemical composition in its directional silicon steel slab is by weight percentage: Si is 2.5-5.0%, C is 0.01-0.10%, Mn is 0.02-0.10%, S is 0.01-0.05%, sour molten aluminium Als is 0.01-0.05%, N is 0.003-0.015%, and all the other are iron and impurity;
2) hot rolling
Directional silicon steel slab is heated to the temperature of 1180-1300 ℃ before hot rolling, in silicon steel special heating furnace, and carry out above insulation in 30 minutes, be conducive to the abundant solid solution of inclusion wherein, to separate out Second Phase Particles tiny, disperse in silicon steel matrix in course of hot rolling subsequently, Second Phase Particles is inhibitor;
Directional silicon steel slab adopts low-temperature heat, and its Heating temperature forms hot-rolled sheet at 1180-1300 ℃, and the amount of inhibitor is effectively supplemented by oozing N in rear operation;
3) normalizing adds pickling
Hot Rolled Plate Normalizing is annealed and is carried out pickling, removes the iron scale of steel strip surface; Normalizing annealing step is: in temperature, be first that 1050-1185 ℃ of normalizing annealings, normalizing annealing time are 1-20s, in temperature, be that 850-980 ℃ of normalizing annealings, normalizing annealing time are 30-180s again, after normalizing annealing, carry out cooling, speed of cooling: 60 ℃/s-10 ℃/s; The acid washing conditions carrying out after normalizing annealing: pickling in the hydrochloric acid soln of 3-6 %wt;
4) cold rolling
By cold-rolling practice once or twice, the thickness of hot-rolled sheet is rolled to the silicon strip of finished product thickness, cold rolling draft >=82%; Heavy reduction rate significantly increases the dislocation desity in steel band interior tissue, and a large amount of dislocations and the goss texture of generation are conducive to the forming core of Gauss's nucleus, and Gauss's nucleus just can develop into perfect secondary recrystallization;
5) decarburizing annealing
After the cold rolling silicon strip that obtains finished product thickness is carried out to decarburizing annealing and be coated with magnesium oxide coating, described magnesium oxide coating take for adopting the annealing separating agent coating that magnesium oxide is main component, and described annealing separating agent comprises MgO, B and TiO
2, be wherein added with the B of the 0.01-0.10%wt that accounts for annealing separating agent quality, account for the TiO of 0.01-0.30%wt of annealing separating agent quality
2, and 0 Bi that is less than or equal to 0.2%wt that is more than or equal to that accounts for annealing separating agent quality, its temperature controlling range of described decarburizing annealing: 750-890 ℃, protective atmosphere is hydrogen, nitrogen mixture gas, wherein the H in hydrogen, nitrogen mixture gas
2content accounts for 15-80 wt%, and the dew-point temperature of protective atmosphere is 25-75 ℃; Decarburization time: 90-350 second, and the carbon in silicon strip is taken off below 30ppm; The de-total oxygen of steel strip surface [O] reaches in following scope: 170/t≤[O]≤315/t, and wherein t is silicon strip actual (real) thickness mm;
6) high temperature annealing
In high temperature annealing operation, adopt the low temperature insulation of two steps and only have the soak of a step to purify the steel of silicon strip, the low temperature holding temperature 400-600 ℃ of first step, the low temperature holding temperature of second step is 650-800 ℃; At the low temperature holding stage of second step with in being warmed up to the process of the intensification before 1020 ℃, in its stove, adopt pure N
2gas is made shielding gas, and silicon strip is carried out to nitriding, and the dew point that passes into purity nitrogen requires≤and-60 ℃, the dew point of furnace atmosphere requires≤30 ℃;
7) stretching and leveling annealing.
3. as claimed in claim 1 or 2
in oriented silicon steel barrier coat, add the production method of trace element, raising insulating property, it is characterized in that: annealing separating agent adopts qualified silicon steel special magnesium oxide formulated, wherein added the 0.01-0.10%wt that accounts for annealing separating agent quality B, be greater than 0 and be less than or equal to the Bi of 0.2%wt and the TiO of 0.01-0.30%wt
2.
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