CN103695620B - The production method of the oriented silicon steel that a kind of bottom layer quality is excellent - Google Patents
The production method of the oriented silicon steel that a kind of bottom layer quality is excellent Download PDFInfo
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Abstract
The production method of the oriented silicon steel that a kind of bottom layer quality is excellent: continuously cast bloom is heated; Hot rolling; Adopt once cold rolling method or twice cold-rolling practice rolling containing middle gross decarburization annealing; Coating annealing separating agent also makes its water-content 2 ~ 4%; High temperature annealing also, before first time, warming temperature reached 800 DEG C, adopts purity nitrogen or carries out oxidizing annealing process with the nitrogen argon atmospher of arbitrary proportion mixing; Stretching and leveling is annealed and is coated with insulating coating.The present invention is by controlling the water-content in the oxygen level of steel plate after decarburizing annealing and separant, and carry out oxidizing annealing process or/and the cooling stages after decarburization Nitrizing Treatment or in decarburization Nitrizing Treatment is or/and cooling stages that is rear in middle gross decarburization annealing or that anneal at middle gross decarburization in the high temperature annealing stage, and or/and carry out oxidizing annealing process in recovery annealing, form to utilize the development that outer oxide layer limits internal oxidition, and reach the object reducing or eliminating oriented silicon steel point-like and reveal golden defect, raising finished product bottom layer quality.
Description
Technical field
The present invention relates to a kind of production method of oriented silicon steel, belong to the production method of the excellent oriented silicon steel of a kind of bottom layer quality particularly, the point-like definitely for solving oriented silicon steel bottom reveals the production method of the oriented silicon steel of golden defect.
Background technology
Before the eighties, oriented silicon steel is produced primarily of two kinds of methods, is the general oriented silicon steel (CGO) that hot-rolled process adopts strand high temperature (more than 1360 DEG C) heating, rear operation adopts twice cold-rolling practice containing process annealing to produce respectively; And slab heating temperature is more than 1380 DEG C, high magnetic induction grain-oriented silicon steel (Hi-B) production method that rear operation adopts large pressure once cold rolling method to produce.Because slab heating temperature is too high, this two classes steel grade is made to there is the series of problems such as energy consumption is high, lumber recovery is low, productivity is poor at hot-rolled process.The existence of this problem, seriously constrains with the raising of the seed output and quality of the strand heat oriented silicon steel that is feature.Since the eighties, people are in order to reduce production difficulty and the production cost of this kind of oriented silicon steel, successively develop slab heating temperature lower than 1300 DEG C, rear operation adopts and to anneal the general oriented silicon steel that twice cold rolling process produce containing middle gross decarburization, and slab heating temperature is lower than 1200 DEG C, the general oriented silicon steel that rear operation adopts the once cold rolling method containing Nitrizing Treatment to produce and high magnetic induction grain-oriented silicon steel.This kind of steel grade is due to the singularity of composition and technique, finished surface often easily produces the bottom defect that one is referred to as point-like dew gold (being also called surface metal bright spot), this point-like reveals the existence of golden bottom defect owing to reducing layer insulation performance during siliconized plate lamination, finally can affect effect when oriented silicon steel uses as transformer core.
With slab heating temperature lower than 1300 DEG C, during rear operation adopts oriented silicon steel that twice cold-rolling practice containing the annealing of middle gross decarburization is manufacturing feature to produce, to anneal carbon content in steel is reduced to below 30ppm through middle the gross decarburization of long period during process annealing; Afterwards, second time is cold rolled to finished product thickness, is more directly coated with magnesium oxide annealing separating agent or is coated with magnesium oxide annealing separating agent again carries out high temperature annealing and subsequent disposal through low temperature recovery annealing.Be different from over conventional annealing process just because of the annealing of middle gross decarburization, low temperature recovery annealing, cause and adopt the oriented silicon steel surface produced in this way and very easily produce bottom defect, and point-like to reveal gold be a kind of major defect wherein.
And for slab heating temperature 1080 ~ 1200 DEG C, rear operation adopts heavy reduction rate one cold-rolling practice to be rolled to finished product thickness, carrying out decarburizing annealing and Nitrizing Treatment is again during the oriented silicon steel of manufacturing feature is produced, due to the difference of steel grades composition, and steel plate also must carry out the special process such as Nitrizing Treatment after completing decarburizing annealing.In order to take into account the composite request relevant to the electromagnetic performance, bottom layer quality (as finished product bottom tack, bottom defect) etc. of final finished of surface of steel plate zone of oxidation structure, primary recrystallization grain size, Nitrizing Treatment effect etc. after decarburizing annealing, often process window is too narrow.Be easy to produce point-like in products production and reveal golden class bottom defect.Nitrizing Treatment is the link that must adopt in such products production, but is also the one of the main reasons that generation point-like reveals golden defect.
The general oriented silicon steel of high temperature (the i.e. CGO steel that past is comparatively ripe; main using MnS as inhibitor) or high magnetic induction grain-oriented silicon steel (i.e. Hi-B steel; main using MnS+AlN as inhibitor) reason one that obtains good bottom is that reason on its steel grades not easily produces point-like and reveals golden defect; two is after cold-rolling of steel plate to finished product thickness; decarburizing annealing under only need completing protective atmosphere at 820 ~ 870 DEG C or surface treatment annealing, and suitable zone of oxidation (mainly Fe can be obtained at surface of steel plate by adjustment decarburizing annealing technique
2siO
4and SiO
2), after high temperature annealing, finally form good, fine and close Magnesium Silicate q-agent bottom at surface of steel plate.Excellent finished surface insulation layer effect can be obtained after being coated with insulating coating on this basis.
In order to the problem that the bottom layer quality occurred when solving oriented silicon steel production is bad, for many years, researchist has carried out the large quantifier elimination product that electromagnetic performance is excellent to obtain, the few insulating coating of bottom defect is effective.And existing a large amount of patent documentation is delivered, as N
o4.127.429 United States Patent (USP) (N
o51-79720 Japanese Patent), N
o1468934 USSR (Union of Soviet Socialist Republics) ACCCCP patents and RU2095433CI Russ P etc.; propose the method forming high-quality Magnesium Silicate q-agent bottom; its method, mainly in the high temperature annealing stage, in different temperature ranges, improves bottom by adjusting the forming of protective atmosphere, the dew point that are made up of nitrogen hydrogen.In addition, Russian document (с т а л ь, 2001.5P57 ~ 59) is also mentioned and is such as adopted high aquation rate magnesium oxide, the middle decarburizing annealing technique of adjustment and add the methods such as magnesium oxide additive to improve bottom layer quality.Proposing the oriented silicon steel bearing copper of the interpolation Cr+Ni to twice cold-rolling practice production of annealing containing middle gross decarburization in EP0709470A1 patent, is 600 ~ 750 DEG C, intrinsic standoff ratio (P in temperature
h2O/ P
h2, lower same) and be carry out recovery annealing process in the atmosphere of 0.62 ~ 0.88, to improve bottom layer quality.In fact, oriented silicon steel bottom defect has multiple, and as bad in stealth dew crystalline substance, surface oxidation, tack and point-like dew gold etc., its Crack cause difference, solution are different.These methods are take measures to improve bottom layer quality from single operation mostly above, implement and are also difficult to obtain more stable effect.Particularly point-like reveals golden defect, completely de-ly anneal with centre, the process relation of the operation such as recovery annealing and high temperature annealing closely, need consider and take measures.Chinese patent (ZL200510020003.2) is the oriented silicon steel of manufacturing feature for employing containing middle gross decarburization twice cold-rolling practice of annealing, the method of the bottom layer quality that atmosphere, temperature and steel plate oxygen level when proposing decarburizing annealing and recovery annealing in the middle of controlling obtain simultaneously, but do not consider high temperature annealing mesosilicic acid magnesium bottom formed before stage on the impact of bottom layer quality, therefore and insufficient.
For slab heating temperature 1080 ~ 1200 DEG C, to adopt containing heavy reduction rate one cold-rolling practice of Nitrizing Treatment be the oriented silicon steel of manufacturing feature to rear operation, Japanese Patent proposes multiple method to improve bottom layer quality, as flat 3-20412 patent proposes 500 ~ 700 DEG C of scopes in the high temperature annealing temperature rise period, N2 is adopted to carry out exhaust repeatedly, air feed to reduce oxidisability in atmosphere to improve finished product bottom; When JP 2000-161106 proposes high temperature annealing, when steel roll end temperature is 600 ~ 650 DEG C, atmosphere intrinsic standoff ratio is controlled more than 0.1, method when temperature is more than 900 DEG C below 0.5; The atmosphere that JP 2006-193798 proposes to control high temperature annealing cooling stages improves bottom; Unexamined Patent 11-279642 proposes high temperature annealing from intensification to 750 ~ 850 DEG C, adopts 0.05 ~ 0.3 intrinsic standoff ratio atmosphere, is controlled below 0.05 by intrinsic standoff ratio afterwards, and controls 900 DEG C of later heat-up rates and improve bottom.In addition, dry type nitrogen nitrogen atmosphere is adopted to carry out reduction treatment to improve bottom to steel plate at 500 ~ 900 DEG C before nitriding annealing after flat 4-183817 proposes decarburizing annealing; Also have flat 4-183817 to think, point-like reveals the Producing reason of golden defect: one is because nitrogen in steel amount after nitriding is too much, or causes because nitrogen pick-up additional in annealing process afterwards makes the nitrogen quantity in steel increase; Two FeO of surface of steel plate when being decarburizing annealing too high levels.Thus propose, in control nitriding amount, decarburizing atmosphere intrinsic standoff ratio and steel, FeO content and high temperature annealing adopted the method containing Ar, He atmosphere of intrinsic standoff ratio more than 0.003 to obtain the product with good bottom before 900 DEG C.
Though most Japanese Patent is from this key link of high temperature annealing, the bad problem of bottom comprising point-like and reveal golden defect is solved by means such as the intrinsic standoff ratios of controlled atmosphere, but all have employed nitrogen nitrogen atmosphere, and control certain intrinsic standoff ratio, indivedual patent documentation also obtains good bottom in conjunction with the FeO content of steel plate during decarburizing annealing and high temperature annealing intrinsic standoff ratio, but the oxide compound of surface of steel plate has multiple during decarburizing annealing, as SiO2, MnO, FeO, Cr2O3 etc., independent control FeO is insufficient, and the FeO content formed in decarburizing annealing is little, accurate control is more difficult.In addition, during high temperature annealing, row annealing is involved in because steel plate is rolled into, steel plate scribble MgO annealing separating agent between layers, MgO separant before coating existing partial hydrolysis becomes Mg (OH) 2, therefore, the high temperature annealing temperature rise period, moisture will be had among annealing separating agent to disengage, this produces larger impact to the intrinsic standoff ratio of atmosphere on the one hand, on the other hand, because temperature-rise period light plate steam between layers disengages, the atmosphere pressures of interlayer is made to be greater than the pressure of furnace atmosphere, thus hinder the interlayer that furnace atmosphere enters steel plate, therefore, adjustment by means of only temperature-rise period furnace atmosphere improves bottom, its effect is also unstable, also should consider the factor of MgO, namely be the water ratio of the annealing separating agent of main component with MgO.According to above reason, these methods are adopted often to be difficult to obtain good effect.
The applicant is after a large amount of experimental studies, and reason oriented silicon steel generation point-like being revealed to golden defect is described below:
General containing about 3%Si, the silicon steel sheet containing the elements such as a certain amount of Mn, Cr simultaneously, when carrying out decarburizing annealing under certain atmospheric condition, near surface of steel plate, form zone of oxidation.Zone of oxidation from outside to inside, is generally made up of double-layer structure, is containing Fe, Mn, Cr (Fe, Mn) 2SiO4 or Fe(Fe, Cr respectively) internal oxidation layer of 2O4 oxide compound and the internal oxidation layer containing SiO2 oxide compound, the former is positioned at skin.Along with the reduction internal oxidation layer of carbon amounts in steel plate thickens, when carbon is low to (below 10ppm is even lower) during a certain value, continues to anneal in wet type nitrogen nitrogen atmosphere, along with constantly thickening of SiO2 layer, pure iron layer will be occurred in steel plate most surface.Pure iron layer increases along with containing SiO2 internal oxidation layer thickness increases.Research finds, it is relevant with this one deck pure iron layer that final finished generation point-like reveals golden defect, and pure iron layer is thicker, and point-like is revealed golden defect and occurred more serious, is even difficult to form Magnesium Silicate q-agent bottom.
Oriented silicon steel as improper process control when carrying out (centre) decarburizing annealing, all may produce point-like and reveal golden defect when causing internal oxidation layer thicker.Therefore, when reasonably must control (centre) decarburizing annealing, steel plate internal layer degree of oxidation, prevents the generation of pure iron layer, so just can reduce the generation that finished product point-like reveals golden defect to a certain extent.But, after steel plate completes decarburizing annealing, also need to carry out high temperature annealing to complete secondary recrystallization, to obtain excellent finished product magnetic.When high temperature annealing, the temperature rise period of steel plate before bottom is formed, steel plate is applicable to as being still in the wet type nitrogen nitrogen atmosphere forming internal oxidition, then internal oxidation layer also being made to thicken further, causing surperficial pure iron layer produce and thicken, and finished product can be caused equally to produce point-like dew gold.Steel plate is referred to as additional internal oxidition at the internal oxidition that the temperature rise period of high temperature annealing occurs by us.Therefore, the additional internal oxidition produced in high temperature annealing is also the one of the main reasons that finished product point-like reveals the generation of golden defect.
The formation of oriented silicon steel Magnesium Silicate q-agent bottom is in the high temperature annealing stage, temperature is about 850 ~ 1000 DEG C of scopes, the quality of Magnesium Silicate q-agent bottom formation front spring quality of oxide layer determines the formation quality of final bottom, the water ratio of the decarburizing annealing in the middle gross decarburization annealing in twice cold-rolling practice, recovery annealing and employing Nitrizing Treatment once cold rolling method, Nitrizing Treatment technique, annealing separating agent, and the high-temperature annealing process before the formation of Magnesium Silicate q-agent bottom all can have an impact to the quality of bottom layer quality.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, under a kind of prerequisite ensureing directional silicon steel performance being provided, reducing or eliminating bottom point-like and revealing golden defect, thus obtain the excellent oriented silicon steel production method of bottom layer quality.
Realize the measure of above-mentioned purpose
A production method for the oriented silicon steel that bottom layer quality is excellent, its step:
1) heat oriented silicon steel continuously cast bloom, heating and temperature control is at 1080 ~ 1320 DEG C;
2) by heating after oriented silicon steel continuously cast bloom routinely technique make hot-rolled sheet after carrying out hot rolling, then pickling or normalizing pickling;
3) the once cold rolling method containing decarburization nitriding annealing or twice cold-rolling practice containing middle gross decarburization annealing is adopted by cold-rolling of steel plate to finished product thickness; When adopt containing decarburization nitriding annealing once cold rolling method time, carry out decarburization and Nitrizing Treatment after being cold-rolled to finished product thickness, and by the carbon content control in steel in below 30ppm, oxygen level in 400 ~ 750ppm scope; When adopting twice cold-rolling practice containing middle gross decarburization annealing, first time is cold-rolled to the laggard interline gross decarburization annealing of interior thickness, by the carbon content control in steel in below 30ppm, oxygen level in 400 ~ 750ppm scope, second time be cold-rolled to finished product thickness after under 500 ~ 600 DEG C of conditions, carry out recovery annealing;
4) being coated with in the usual way with magnesium oxide is the annealing separating agent of main component, and control the moisture weight degree in separant 2 ~ 4% scope;
5) carry out high temperature annealing after steel strip coiling, in temperature rise period first time of high temperature annealing, reach before 800 DEG C in temperature, adopt purity nitrogen atmosphere or carry out oxidizing annealing process with the nitrogen argon atmospher of arbitrary proportion mixing, all the other stages of high temperature annealing carry out routinely;
6), after coil of strip completes high temperature annealing, carry out stretching and leveling annealing routinely and be coated with insulating coating.
It is characterized in that: the cooling stages after adopting the once cold rolling method containing decarburization nitriding annealing to carry out decarburization Nitrizing Treatment or in decarburization Nitrizing Treatment carries out oxidizing annealing process: treatment temp is 500 ~ 880 DEG C, atmosphere adopt dew point be 0 ~ 10 DEG C wet type nitrogen or with arbitrary proportion mixing nitrogen argon mixture gas, adopt intrinsic standoff ratio higher than 0.9 wet type nitrogen hydrogen or nitrogen argon hydrogen mixture, the treatment time is no more than 60 seconds.
It is characterized in that: when adopting the once cold rolling method containing decarburization nitriding annealing, when the cooling stages after decarburization Nitrizing Treatment or in decarburization Nitrizing Treatment carries out oxidizing annealing process, high temperature annealing adopts conventional annealing process.
It is characterized in that: when adopting twice cold-rolling practice containing middle gross decarburization annealing, anneal at middle gross decarburization or carry out oxidizing annealing process at the cooling stages that middle gross decarburization is annealed: treatment temp is 500 ~ 880 DEG C, atmosphere adopt dew point be 0 ~ 10 DEG C wet type nitrogen or with arbitrary proportion mixing nitrogen argon mixture gas, adopt intrinsic standoff ratio higher than 0.9 wet type nitrogen hydrogen or nitrogen argon hydrogen mixture, the treatment time is no more than 60 seconds.
It is characterized in that: in recovery annealing process, the atmosphere of recovery annealing divides two sections of settings, and wherein one section adopts dew point to be that the wet type nitrogen of 10 ~ 20 DEG C or nitrogen argon-mixed atmosphere carry out oxidizing annealing process, and treatment temp is annealing temperature.
It is characterized in that: when adopting twice cold-rolling practice containing the annealing of middle gross decarburization, can after process annealing, in the annealing of the cooling stages of process annealing, middle gross decarburization and one of them of high temperature annealing temperature rise period first time carry out oxidizing annealing process.
The effect of master operation in the present invention
The present invention is by revealing the analysis of golden Defects Forming Mechanism to point-like, in conjunction with the feature of iron-silicon alloy surface oxidation, use the formation condition of internal oxidition and external oxidation thing, propose appropriate utilization external oxidation to suppress this scheme of further intensification of internal oxidition, thus reach the object reducing or eliminating oriented silicon steel point-like and reveal golden defect.In the present invention, the effect of master operation is: the stages such as the middle gross decarburization annealing in oriented silicon steel production process or decarburization nitriding annealing, by the oxygen level of steel plate after control decarburizing annealing, and on this basis, to the high temperature annealing stage after completing the annealing of middle gross decarburization or decarburization nitriding annealing or/and steel plate implement to be intended to make steel plate to form oxidizing annealing processing links for the purpose of outer oxide layer, thus reach and form at surface of steel plate the effect that external oxidation further develops to suppress internal oxidation layer in steel.In the high temperature annealing stage, the steel plate external oxidation annealing of this programme implements like this: the high temperature annealing temperature rise period before Magnesium Silicate q-agent bottom is formed, purity nitrogen (argon) the atmosphere formation high oxidative atmosphere utilizing the moisture in annealing separating agent and pass into, make surface of steel plate form external oxidation to suppress further developing of internal oxidition, thus reach minimizing and even eliminate the object that oriented silicon steel point-like reveals golden defect.By abovementioned technology, can make to occur in oriented silicon steel that the ratio that point-like reveals golden defect is reduced to less than 1%.
Compared with prior art, the present invention is by controlling the moisture content in the oxygen level of steel plate after decarburizing annealing and separant, and carry out oxidizing annealing process or/and cooling stages after decarburization Nitrizing Treatment or in decarburization Nitrizing Treatment in the high temperature annealing stage, or/and cooling stages that is rear in middle gross decarburization annealing or that anneal at middle gross decarburization, and or/and carry out oxidizing annealing process in recovery annealing process, further developing of internal oxidition is limited to utilize formation outer oxide layer, thus reach and reduce or eliminate oriented silicon steel point-like and reveal golden defect, improve the object of finished product bottom layer quality.
Accompanying drawing explanation
Fig. 1 is the bottom layer quality situation map of directional silicon steel of the invention process;
Fig. 2 is the bottom layer quality situation map of the directional silicon steel before the present invention.
Embodiment
With the form of embodiment, the present invention is described below:
Following embodiment is all carried out according to following technique, its step:
1) heat oriented silicon steel continuously cast bloom, heating and temperature control is at 1080 ~ 1320 DEG C;
2) by heating after oriented silicon steel continuously cast bloom routinely technique make hot-rolled sheet after carrying out hot rolling, then pickling or normalizing pickling;
3) the once cold rolling method containing decarburization nitriding annealing or twice cold-rolling practice containing middle gross decarburization annealing is adopted by cold-rolling of steel plate to finished product thickness; When adopt containing decarburization nitriding annealing once cold rolling method time, carry out decarburization and Nitrizing Treatment after being cold-rolled to finished product thickness, and by the carbon content control in steel in below 30ppm, oxygen level in 400 ~ 750ppm scope; When adopting twice cold-rolling practice containing middle gross decarburization annealing, first time is cold-rolled to the laggard interline gross decarburization annealing of interior thickness, by the carbon content control in steel in below 30ppm, oxygen level in 400 ~ 750ppm scope, second time be cold-rolled to finished product thickness after under 500 ~ 600 DEG C of conditions, carry out recovery annealing;
4) being coated with in the usual way with magnesium oxide is the annealing separating agent of main component, and control the moisture weight degree in separant 2 ~ 4% scope;
5) carry out high temperature annealing after steel strip coiling, in temperature rise period first time of high temperature annealing, reach before 800 DEG C in temperature, adopt purity nitrogen atmosphere or carry out oxidizing annealing process with the nitrogen argon atmospher of arbitrary proportion mixing, all the other stages of high temperature annealing carry out routinely;
6), after coil of strip completes high temperature annealing, carry out stretching and leveling annealing routinely and be coated with insulating coating.
Table 1 is for adopting the embodiment 1 and comparative example result that contain decarburization nitriding annealing manufacturing oriented silicon steel with one-step cold rolling;
Table 2 is for adopting the embodiment 2 and comparative example result that contain decarburization nitriding annealing manufacturing oriented silicon steel with one-step cold rolling;
Table 3 for the present embodiment after the annealing of middle gross decarburization or its cooling stages carry out the technique of oxidizing annealing process;
The scheme of oxidizing annealing process implemented by table 4 in recovery annealing process during twice cold-rolling practice containing middle gross decarburization annealing for adopting;
Embodiment 3 and the comparative example result of table 5 for adopting twice cold-rolling practice containing middle gross decarburization annealing to produce oriented silicon steel.
Embodiment 1
Chemical composition and weight percent are: 3.15%Si; 0.040%C; 0.22%Mn; 0.021%S; 0.021%Als; 0.0090%N; 0.052%Cu; 0.046%Sn; 0.04%Cr; 0.010%P; 0.002%Ti; All the other be the continuously cast bloom of Fe and inevitable impurity after 1180 DEG C of heating temperatures, be rolled into the hot rolled coil that thickness is 2.3mm.
After hot rolled coil normalizing annealing, once cold rolling is to 0.30mm, 0.27mm gauge; through continuous decarburizing annealing and nitriding annealing, to be coated with magnesium oxide be the annealing separating agent of main component; then carry out the high temperature annealing with oxidizing annealing treatment process, all the other techniques are carried out routinely.Its result of implementation is as shown in table 1.
Decarburization nitriding annealing once cold rolling method the results list that table 1 the present embodiment and comparative example all adopt
Embodiment 2
Continuously cast bloom composition and weight percent are: 3.20%Si; 0.056%C; 0.08%Mn; 0.011%S; 0.030%AIs; 0.0085%N; 0.025%Cu; 0.050%Sn; 0.01%Cr; 0.018%P; 0.002%Ti; All the other are Fe and inevitable impurity.Strand, after 1200 DEG C of heating, is rolled into 2.3mm thickness hot rolling.
0.23mm, 0.27mm thickness is cold-rolled to after hot rolled coil normalizing annealing; then the cooling stages after continuous decarburizing annealing or/and in decarburization Nitrizing Treatment carries out oxidizing annealing process; be the annealing separating agent of main component with magnesium oxide through coating; or/and adopt purity nitrogen atmosphere to carry out oxidizing annealing process in temperature rise period first time of high temperature annealing, other stage process of high temperature annealing carries out routinely.The smooth annealing of drawn the result obtained after being coated with insulating coating is as shown in table 2.
Decarburization nitriding annealing once cold rolling method the results list that table 2 the present embodiment and comparative example all adopt
Embodiment 3
Continuously cast bloom composition (weight percent) is: 0.033-36%C, 3.16-3.20%Si, 0.18-0.19%Mn, 0.0040-0.0060%S, 0.014-0.16%Als, 0.0086-0.0093%N, 0.48-0.50%Cu, all the other are after the continuously cast bloom 1250 DEG C heating of Fe and inevitable impurity, are rolled into the hot rolled coil that thickness is 2.3mm.After pickling, be cold-rolled to 0.65mm, after middle gross decarburization annealing, a part of coil of strip carries out oxidizing annealing process.Oxidizing annealing processing scheme parameter is in table 3.All coil of strips are cold-rolled to the finished product thickness of 0.30mm, at 580 DEG C of recovery annealings, carry out oxidizing annealing process when part twists in recovery annealing, scheme is in table 4 again.Being coated with afterwards with magnesium oxide is the annealing separating agent of main component, and by its moisture control at 2.0-3.0%, in the high temperature annealing temperature rise period, adopt purity nitrogen atmosphere to carry out oxide treatment before part twists in 700 DEG C, part is rolled up technique routinely and carried out.After high temperature annealing completes, carry out stretching and leveling annealing and be coated with insulating coating, the finished product bottom point-like obtained reveals golden defect situation in table 5.
Table 3 the present embodiment after the annealing of middle gross decarburization or its cooling stages carry out the technique of oxidizing annealing process
Table 4 the present embodiment is with the recovery annealing process program of oxidizing annealing process
| Process program | Temperature | Time | Atmosphere |
| 1 | 580℃ | 120 seconds | Full stove is arranged by two sections of atmosphere: first paragraph: 25%H2, intrinsic standoff ratio: 0.32; Second segment: 100%N2, dew point: 12 DEG C |
| 2 | 580℃ | 120 seconds | Full stove is arranged by two sections of atmosphere: first paragraph: 25%H2, intrinsic standoff ratio: 0.32; Second segment: 100%N2, dew point: 20 DEG C |
| 3 | 580℃ | 120 seconds | Full stove is arranged by two sections of atmosphere: first paragraph: 25%H2, intrinsic standoff ratio: 0.32; Second segment: 100%N2, dew point: 15 DEG C |
The test-results list of table 5 the present embodiment and comparative example
Above-described embodiment is only the best and exemplifies, and is not the restriction to embodiments of the present invention.
Claims (6)
1. a production method for the oriented silicon steel that bottom layer quality is excellent, its step:
1) heat oriented silicon steel continuously cast bloom, heating and temperature control is at 1080 ~ 1320 DEG C;
2) by heating after oriented silicon steel continuously cast bloom routinely technique make hot-rolled sheet after carrying out hot rolling, then pickling;
3) the once cold rolling method containing decarburization nitriding annealing or twice cold-rolling practice containing middle gross decarburization annealing is adopted by cold-rolling of steel plate to finished product thickness; When adopt containing decarburization nitriding annealing once cold rolling method time, carry out decarburization and Nitrizing Treatment after being cold-rolled to finished product thickness, and by the carbon content control in steel in below 30ppm, oxygen level in 400 ~ 750ppm scope; When adopting twice cold-rolling practice containing middle gross decarburization annealing, first time is cold-rolled to the laggard interline gross decarburization annealing of interior thickness, by the carbon content control in steel in below 30ppm, oxygen level in 400 ~ 750ppm scope, second time be cold-rolled to finished product thickness after under 500 ~ 600 DEG C of conditions, carry out recovery annealing;
4) being coated with in the usual way with magnesium oxide is the annealing separating agent of main component, and control the moisture weight degree in separant 2 ~ 4% scope;
5) carry out high temperature annealing after steel strip coiling, in temperature rise period first time of high temperature annealing, reach before 800 DEG C in temperature, adopt purity nitrogen atmosphere or carry out oxidizing annealing process with the nitrogen argon atmospher of arbitrary proportion mixing, all the other stages of high temperature annealing carry out routinely;
6), after coil of strip completes high temperature annealing, carry out stretching and leveling annealing routinely and be coated with insulating coating.
2. the production method of the oriented silicon steel that a kind of bottom layer quality as claimed in claim 1 is excellent, it is characterized in that: the cooling stages after adopting the once cold rolling method containing decarburization nitriding annealing to carry out decarburization Nitrizing Treatment or in decarburization Nitrizing Treatment carries out oxidizing annealing process: treatment temp is 500 ~ 880 DEG C, atmosphere adopt dew point be 0 ~ 10 DEG C wet type nitrogen or with arbitrary proportion mixing nitrogen argon mixture gas, adopt intrinsic standoff ratio higher than 0.9 wet type nitrogen hydrogen or nitrogen argon hydrogen mixture, the treatment time is no more than 60 seconds.
3. the production method of the oriented silicon steel that a kind of bottom layer quality as claimed in claim 1 is excellent, it is characterized in that: when adopting the once cold rolling method containing decarburization nitriding annealing, when the cooling stages after decarburization Nitrizing Treatment or in decarburization Nitrizing Treatment carries out oxidizing annealing process, high temperature annealing adopts conventional annealing process; Its oxidizing annealing treatment temp is 500 ~ 880 DEG C, atmosphere adopt dew point be 0 ~ 10 DEG C wet type nitrogen or with arbitrary proportion mixing nitrogen argon mixture gas, adopt intrinsic standoff ratio higher than 0.9 wet type nitrogen hydrogen or nitrogen argon hydrogen mixture, the treatment time is no more than 60 seconds.
4. the production method of the oriented silicon steel that a kind of bottom layer quality as claimed in claim 1 is excellent, it is characterized in that: when adopting twice cold-rolling practice containing middle gross decarburization annealing, anneal rear at middle gross decarburization or carry out oxidizing annealing process at the cooling stages that middle gross decarburization is annealed: treatment temp is 500 ~ 880 DEG C, atmosphere adopt dew point be 0 ~ 10 DEG C wet type nitrogen or with arbitrary proportion mixing nitrogen argon mixture gas, adopt intrinsic standoff ratio higher than 0.9 wet type nitrogen hydrogen or nitrogen argon hydrogen mixture, the treatment time is no more than 60 seconds.
5. the production method of the oriented silicon steel that a kind of bottom layer quality as claimed in claim 1 is excellent, it is characterized in that: in recovery annealing process, the atmosphere of recovery annealing divides two sections of settings, wherein one section adopts dew point to be that the wet type nitrogen of 10 ~ 20 DEG C or nitrogen argon-mixed atmosphere carry out oxidizing annealing process, and treatment temp is annealing temperature.
6. the production method of the oriented silicon steel that a kind of bottom layer quality as claimed in claim 1 is excellent, it is characterized in that: when adopting twice cold-rolling practice containing middle gross decarburization annealing, in the cooling stages, recovery annealing of rear, the middle gross decarburization annealing of middle gross decarburization annealing, one of them carries out oxidizing annealing process, and high temperature annealing adopts conventional annealing process; Wherein when the cooling stages of rear, the middle gross decarburization annealing of middle gross decarburization annealing carries out oxidizing annealing process, oxidizing annealing treatment temp is 500 ~ 880 DEG C, atmosphere adopt dew point be 0 ~ 10 DEG C wet type nitrogen or with arbitrary proportion mixing nitrogen argon mixture gas, adopt intrinsic standoff ratio higher than 0.9 wet type nitrogen hydrogen or nitrogen argon hydrogen mixture, the treatment time is no more than 60 seconds; When carrying out oxidizing annealing process in recovery annealing, the atmosphere of recovery annealing divides two sections of settings, and wherein one section adopts dew point to be that the wet type nitrogen of 10 ~ 20 DEG C or nitrogen argon-mixed atmosphere carry out oxidizing annealing process, and treatment temp is annealing temperature.
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| CN105525087B (en) * | 2015-10-10 | 2017-05-10 | 广东盈泉高新材料有限公司 | Method for improving quality of bottom layer of oriented silicon steel |
| CN106399856B (en) * | 2016-09-28 | 2018-07-27 | 武汉科技大学 | A method of improving silicon containing steel surface quality |
| CN107164624B (en) * | 2017-04-10 | 2020-02-21 | 首钢集团有限公司 | Method for controlling pockmark defects on surface of phosphorus-containing cold-rolled high-strength steel |
| CN110283981B (en) * | 2019-07-24 | 2020-12-11 | 武汉钢铁有限公司 | Production method capable of increasing oxygen content of low-temperature high-magnetic-induction oriented silicon steel |
| 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 |
| CN113832322B (en) * | 2021-09-26 | 2023-04-28 | 武汉钢铁有限公司 | High-efficiency decarburization annealing process for high-magnetic induction oriented silicon steel |
| CN114717401A (en) * | 2022-04-14 | 2022-07-08 | 无锡普天铁心股份有限公司 | Method for improving point-like gold exposure on surface of oriented silicon steel |
| CN114921711B (en) * | 2022-05-25 | 2023-10-24 | 湖南华菱湘潭钢铁有限公司 | Production method of Q620-grade high-corrosion-resistance high-strength offshore structural steel |
| CN115505694A (en) * | 2022-09-23 | 2022-12-23 | 无锡普天铁心股份有限公司 | Low-temperature ultrahigh-magnetic-induction oriented silicon steel and manufacturing method thereof |
| CN116121622A (en) * | 2022-11-18 | 2023-05-16 | 无锡普天铁心股份有限公司 | Production process of excellent bottom layer oriented silicon steel |
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