CN109402513B - Production method of high-magnetic-induction oriented silicon steel - Google Patents
Production method of high-magnetic-induction oriented silicon steel Download PDFInfo
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- CN109402513B CN109402513B CN201811519969.4A CN201811519969A CN109402513B CN 109402513 B CN109402513 B CN 109402513B CN 201811519969 A CN201811519969 A CN 201811519969A CN 109402513 B CN109402513 B CN 109402513B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1255—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest with diffusion of elements, e.g. decarburising, nitriding
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- C—CHEMISTRY; METALLURGY
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/12—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties
- C21D8/1244—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of articles with special electromagnetic properties the heat treatment(s) being of interest
- C21D8/1272—Final recrystallisation annealing
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- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
Abstract
The invention discloses a production method of high magnetic induction oriented silicon steel, which comprises the following steps: obtaining a plate blank; carrying out hot rolling, cold rolling and decarburization treatment on the plate blank to obtain a decarburization plate; curling the decarburized plate to obtain a steel coil; the high-temperature annealing of the steel coil comprises the following steps: the temperature is increased to 600-750 ℃ for the first time, and the temperature is kept for 10-20 h; the second temperature rise is firstly carried out to the lower limit temperature Tmin of the secondary recrystallization starting temperature; raising the temperature for the third time to the upper limit temperature Tmax of the secondary recrystallization starting temperature; the fourth temperature rise is 1170-1220 ℃, and the temperature is kept for 20-30 h; stretching and flattening the annealed steel coil to obtain the high-magnetic-induction oriented silicon steel; the lower limit temperature Tmin is determined by the maximum value P13max of the residual aluminum Alr and the strip iron loss value P13/50 of the decarburization plate, and the upper limit temperature Tmax is determined by the minimum value P13min of the residual aluminum Alr and the strip iron loss value P13/50 of the decarburization plate. According to the iron loss value P13/50 of the steel strip and the residual aluminum Alr, the furnace temperature range of the secondary recrystallization can be obtained, thereby improving the performance of the steel coil.
Description
Technical Field
The invention relates to the technical field of steel production, in particular to a production method of high-magnetic-induction oriented silicon steel.
Background
By researching the secondary recrystallization process of the low-temperature high-magnetic induction oriented silicon steelThe results show that: the driving force for the secondary recrystallization grain growth is a function of suppressing the growth of the primary recrystallization matrix by the stored driving force (P), the pinning force (Z) of the second phase particles, the type of the grains themselves, and the like. Wherein the secondary recrystallization growth driving force can be described as the average grain boundary energy γ and the average grain size
The function concerned is:
in the above formula, K is a proportionality coefficient. The formula shows that the driving force for abnormal growth of secondary recrystallization is inversely proportional to the primary crystal grain size, and the primary crystal grain size must be controlled within a proper range if enough driving force for abnormal growth of secondary recrystallization is available.
According to the well-known ZENER formula, the pinning force for precipitating relative grain growth can be calculated according to the following formula:
wherein f is the second phase particle precipitation volume. r is the average radius of the second phase particles. The above formula also shows that the larger the number of precipitates and the smaller the size, the stronger the ability to inhibit grain growth.
Therefore, in the preparation process of the low-temperature high-magnetic-induction oriented silicon steel, different primary recrystallization and inhibitor state products have different capacities of abnormal secondary recrystallization growth, so that the temperature points (secondary recrystallization temperature) of the abnormal secondary recrystallization growth under different component process state conditions are inconsistent.
The temperature range for starting secondary recrystallization is the temperature range in which the inhibition capability of the inhibitor is obviously weakened or disappeared, the slow temperature rise is usually adopted to ensure that the inhibition capability is slowly released, and Gaussian grains can preferentially grow and swallow other grains to form a single {110} <001> texture. For example:
japanese patent application laid-open No. Hei 8-311560 proposes that if the temperature is maintained at about 1000 ℃ for about 17 hours and then raised to 1100 ℃ at a rate of 10 ℃/h, the temperature rise rate at the highest point is 10 ℃/h and the temperature rise rate at the lowest point is 11 ℃/h, and the decrease in Δ P17 is significant. Japanese laid-open patent publication Hei 6-2043 proposes that the temperature is raised to 950-.
In the document with the chinese patent publication No. CN101775548A, in the high-temperature annealing process of the low-temperature high-magnetic-induction oriented silicon steel, a temperature rise rate of 15 ℃/H is adopted before the temperature of the high-temperature annealing high-heat-preservation purification platform is 1180 ℃ to 1200 ℃, and H is adopted before 1100 ℃2+N2The mixed atmosphere of (2) controls the content of steel grade nitrides to obtain good magnetic performance.
In the document with Chinese patent publication No. CN101348854A, in the high-temperature annealing process for preparing the low-temperature high-magnetic-induction oriented silicon steel by the nitriding method, a heating process with the temperature of 5-20 ℃/h in a lower range is adopted at 850-1100 ℃. The methods all adopt lower heating rate to ensure that the steel strip has enough time to grow up at the secondary recrystallization temperature in the high-temperature annealing process.
The above documents have a disadvantage that a fixed process range is adopted without considering the influence of Alr and primary recrystallization on the secondary recrystallization starting temperature.
The patent with publication number CN107858494A introduces a production method of low-temperature high-magnetic-induction oriented silicon steel, which estimates Ts through the size of primary recrystallized grains and the Alr content, sets an isothermal platform in the high-temperature annealing process, and realizes the slow temperature rise at the Ts position so as to improve the uniformity of the head and tail magnetism of the steel coil.
Patent publication No. CN107988472A introduces an energy-saving method for producing high-magnetic-induction oriented silicon steel, which estimates the secondary recrystallization starting temperature through parameters such as Als, nitrogen increase, primary recrystallization size and the like, and realizes the shortening of high-temperature annealing time by improving the temperature rise speed before and after an isothermal platform, thereby realizing the improvement of high-temperature annealing efficiency and the reduction of cost.
All of the above patents are addressed bySThe mode of section staying and heat preservation fully completes the secondary recrystallization, wherein T is also treatedSThe calculation method of (2) is described. However, from a large number of experiments, the secondary recrystallization starting temperature cannot be accurately estimated, and the secondary recrystallization starting temperatures in the length direction of the steel coil are different due to differences of structures of various parts of the steel coil. Therefore, the process setting is performed according to the single secondary recrystallization starting temperature, and deviation is inevitably caused to influence the performance of the steel coil.
Disclosure of Invention
The application provides a high magnetic induction grain-oriented silicon steel production method, has solved among the prior art not considering Alr and the influence to secondary recrystallization start temperature of primary recrystallization to and carry out the process setting according to single secondary recrystallization start temperature, cause and have the deviation with actual crystallization temperature, thereby influence the technical problem of coil of strip performance. The application provides a production method of high magnetic induction oriented silicon steel, which comprises the following chemical components in percentage by weight: c: 0.03 to 0.07%, Si: 2.0-3.8%, Mn: 0.05-0.2%, S: 0.005-0.01%, Al: 0.020-0.035%, N: 0.005-0.01%, Cu: 0.05 to 0.25 percent, and the balance being Fe and inevitable impurities;
the production method comprises the following steps:
obtaining a plate blank;
carrying out hot rolling, cold rolling and decarburization treatment on the plate blank to obtain a decarburization plate;
curling the decarburized plate to obtain a steel coil;
the high-temperature annealing of the steel coil comprises the following steps: the temperature is increased to 600-750 ℃ for the first time, and the temperature is kept for 10-20 h; the second temperature rise is firstly carried out to the lower limit temperature Tmin of the secondary recrystallization starting temperature; raising the temperature for the third time to the upper limit temperature Tmax of the secondary recrystallization starting temperature; the fourth temperature rise is 1170-1220 ℃, and the temperature is kept for 20-30 h;
stretching and flattening the annealed steel coil to obtain the high-magnetic-induction oriented silicon steel;
wherein the third temperature increase rate is lower than the second temperature increase rate, the lower limit temperature Tmin is determined by a maximum value P13max of the remaining aluminum Alr and a strip iron loss value P13/50 of the decarburization plate, and the upper limit temperature Tmax is determined by a minimum value P13min of the remaining aluminum Alr and a strip iron loss value P13/50 of the decarburization plate.
Preferably, the third heating rate V ═ 0.053(Tmax-Tmin)/R, R — represents the thickness of the steel coil.
Preferably, the rate of the second temperature rise and the rate of the fourth temperature rise are 40-75 ℃/h.
Preferably, 100% N is introduced when the temperature is raised for the first time to the second time2。
Preferably, H is introduced at the beginning of the third temperature rise2And N2And (3) mixing the gas, wherein N2% is 25+ 2.5V, and the temperature rise speed V is not more than 17 ℃/h.
Preferably, 100% H is introduced at the end of the fourth temperature rise2。
Preferably, the lower limit temperature Tmin is determined by the residual aluminum Alr and the maximum value P13max of the strip iron loss value P13/50 of the decarburization plate, specifically:
the lower limit temperature Tmin is obtained according to lnTmin ═ a-b ═ P13max + c ═ Alr, wherein a ═ 7.0 to 7.1, b ═ 0.05 to 0.06, and c ═ 8.4 to 8.5.
Preferably, the upper limit temperature Tmax is determined by the minimum value P13min of the residual aluminum Alr and the steel strip iron loss P13/50 of the decarburization plate, and specifically is as follows:
obtaining the upper limit temperature Tmax according to lnTmax ═ a-b ═ P13min + c ═ Alr; wherein a is 7.0-7.1, b is 0.05-0.06, and c is 8.4-8.5.
Preferably, the temperature of the decarburization treatment is controlled to 800-860 ℃.
Preferably, the cold rolling of the slab comprises:
and (3) carrying out aging rolling for at least one time by adopting a one-time rolling method, wherein the thickness of a finished product is less than or equal to 0.3 mm.
The beneficial effect of this application is as follows:
the technical scheme of this application is based on the research to low temperature high magnetic induction oriented silicon steel secondary recrystallization, and online measurement's steel band iron loss value P13/50 has synthesized the influence that has reflected size, phase, the nitriding amount of primary recrystallization crystalline grain, and steel band iron loss value P13/50 curve is not completely straight, and the difference exists certain fluctuation in the position promptly, consequently, the secondary recrystallization temperature that corresponds the position also is diverse, and the upper and lower limit of secondary recrystallization start temperature just makes according to this principle in this scheme. The quantity of the residual aluminum Alr reflects the strength of the capability of converting into AlN at the front section of nitriding in the subsequent procedure and high-temperature annealing, the more the quantity of the Alr is, the more the finally formed ALN is, the stronger the capability of inhibiting the growth of non-Gaussian grains in the high-temperature annealing process is, and the higher the secondary recrystallization starting temperature is. Therefore, according to the iron loss value P13/50 of the steel strip and the residual aluminum Alr, the furnace temperature range for starting secondary recrystallization can be obtained, high-temperature annealing can be carried out according to the actual crystallization temperature, the performance of the steel strip is improved, and the technical problem that the influence of Alr and primary recrystallization on the secondary recrystallization starting temperature is not considered in the prior art, and the deviation of the process setting according to the single secondary recrystallization starting temperature and the actual crystallization temperature is caused, so that the performance of the steel strip is influenced is solved.
Meanwhile, the whole time of the high-temperature annealing process is shortened, the production efficiency is improved, and the cost is saved. Compared with the normal process, the average value of P17/50 is reduced by 0.03-0.08W/KG, B8 is improved by 0.01-0.03T, and the time for high-temperature annealing is saved by 3-18 hours.
In the high-temperature annealing temperature rise process, because the volume of the steel coil is large, the obvious temperature unevenness phenomenon exists on the upper end surface and the lower end surface of the inner ring and the outer ring in the common process, the larger the volume of the steel coil is, the larger the difference value between the maximum temperature and the minimum temperature is, in order to ensure that the temperature of the inner ring and the outer ring reaches the set temperature range, different temperature rise speeds are set according to the size of the steel coil, and all parts of the steel coil can be ensured to successfully reach the secondary recrystallization starting temperature in.
The second stage of heating adopts 100% N2In the atmosphere N2The increase slows the outward diffusion of N atoms in the steel and reduces Si3N4The tendency of (Al, Si) N, (Mn, Si) N and fine AlN decomposition, so that the temperature rise speed can be greatly increased without rapid decomposition of the inhibitor, which leads to abnormal growth of primary crystal grainsCompared with the prior art, the time for high-temperature annealing is saved by 3-18 hours, and the production efficiency is obviously improved. Meanwhile, the increase of the number of AlN coarsening of the steel in a pure N atmosphere can be avoided by increasing the temperature rise speed, the inhibition capability is weakened, and secondary recrystallization occurs in advance at a lower temperature, so that the conditions of inaccurate crystal grain phase and high iron loss are caused.
The third temperature rise process adopts variable N2The proportion is that the inhibitor is gradually decomposed in the process of starting secondary recrystallization, the decomposition speed is influenced by the N potential in the furnace atmosphere besides the temperature, and the temperature rise speed of the third section is different according to the difference of the upper limit and the lower limit of the secondary recrystallization temperature of the steel coil, so that the N is adjusted2The proportion of (a) is actually just adjusting the decomposition speed of the inhibitor to match the third-stage heating speed, so that secondary recrystallization is ensured to occur within a proper temperature range, and the magnetic level of the steel coil is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention.
FIG. 1 is a flow chart of a method for producing high magnetic induction grain-oriented silicon steel according to the present application;
FIG. 2 is a graph comparing a temperature rise profile of the production process of FIG. 1 with a temperature rise profile of the prior art.
Detailed Description
In order to better understand the technical solution, the technical solution will be described in detail with reference to the drawings and the specific embodiments.
In order to solve the technical problems that Alr and primary recrystallization influence the secondary recrystallization starting temperature and the actual crystallization temperature is deviated due to the fact that the process setting is carried out according to the single secondary recrystallization starting temperature, so that the performance of a steel coil is influenced, the application provides a high-magnetic-induction oriented silicon steel production method.
Firstly, introducing the high magnetic induction oriented silicon steel, wherein the high magnetic induction oriented silicon steel comprises the following chemical components in percentage by weight: c: 0.03 to 0.07%, Si: 2.0-3.8%, Mn: 0.05-0.2%, S: 0.005-0.01%, Al: 0.020-0.035%, N: 0.005-0.01%, Cu: 0.05 to 0.25%, and the balance of Fe and inevitable impurities.
The production method of the present application, as shown in fig. 1 and 2, is described in detail below, and includes the following steps:
and step 110, obtaining a slab. Specifically, a slab is generally obtained by smelting and continuous casting of molten steel.
And 120, carrying out hot rolling, cold rolling and decarburization treatment on the plate blank to obtain a decarburized plate.
Specifically, the hot rolling may be heated using conventional low temperature slab heating temperatures. In the present embodiment, after the slab is hot-rolled, the slab may be further acid-washed and normalized, specifically, a conventional two-stage normalization process may be adopted.
The cold rolling can adopt a one-time rolling method, at least one time of aging rolling is carried out, and the thickness of a finished product is less than or equal to 0.3 mm. After cold rolling, decarburization treatment can be carried out, and the decarburization temperature is controlled at 800-860 ℃. In the embodiment, after the decarburization treatment, nitriding treatment can be performed, the nitriding temperature is controlled at 800-950 ℃, and then the high-temperature annealing separant mainly coated with MgO is performed.
And step 130, curling the decarburized plate to obtain a steel coil.
Step 140, annealing the steel coil at a high temperature, comprising: the temperature is increased to 600-750 ℃ for the first time, and the temperature is kept for 10-20 h; the second temperature rise is firstly carried out to the lower limit temperature Tmin of the secondary recrystallization starting temperature; raising the temperature for the third time to the upper limit temperature Tmax of the secondary recrystallization starting temperature; the fourth temperature rise is carried out to 1170-1220 ℃, and the temperature is kept for 20-30 h.
Wherein the third temperature rise rate is smaller than the second temperature rise rate. Specifically, the third heating rate V is 0.053(Tmax-Tmin)/R, R — represents the thickness of the steel coil, and the second heating rate and the fourth heating rate are 40 to 75 ℃/h.
The lower limit temperature Tmin is determined by the maximum value P13max of the residual aluminum Alr and the strip iron loss value P13/50 of the decarburization plate, and the upper limit temperature Tmax is determined by the minimum value P13min of the residual aluminum Alr and the strip iron loss value P13/50 of the decarburization plate. The strip iron loss value P13/50 of the decarburization plate can be measured by a continuous iron loss meter. The remaining aluminum Alr means: after completion of hot rolling, the portion of Al that is not bonded to N is soluble in acid.
P13max and P13min in W/kg. The residual aluminum Alr can be calculated from Alr ═ Als- (27/14) × N, where Als is the acid-soluble aluminum content in the steelmaking component and N is the N content in the steelmaking component in ppm units.
Specifically, the lower limit temperature Tmin is determined by the remaining aluminum Alr and the maximum value P13max of the strip iron loss value P13/50 of the decarburized sheet steel, specifically:
the lower limit temperature Tmin is obtained according to lnTmin ═ a-b ═ P13max + c ═ Alr, wherein a ═ 7.0 to 7.1, b ═ 0.05 to 0.06, and c ═ 8.4 to 8.5. Preferably, a is 7.039, b is 0.0571, and c is 8.47; a is 7.0, b is 0.05, and c is 8.4; a is 7.1, b is 0.06 and c is 8.5.
Specifically, the upper limit temperature Tmax is determined by the minimum value P13min of the residual aluminum Alr and the steel strip iron loss value P13/50 of the decarburization plate, and specifically comprises the following steps:
obtaining the upper limit temperature Tmax according to lnTmax ═ a-b ═ P13min + c ═ Alr; wherein a is 7.0-7.1, b is 0.05-0.06, and c is 8.4-8.5. Preferably, a is 7.039, b is 0.0571, and c is 8.47.
In addition, 100% N is introduced when the temperature is raised for the first time to the second time2H is introduced when the third temperature rise is started2And N2Mixed gas, wherein N2% is 25+ 2.5V, the temperature rising speed V is not more than 17 ℃/H, and 100% H is introduced at the end of the fourth temperature rising2. By passing in N2The decomposition of AlN is inhibited, the inhibitor is kept at a higher temperature, the secondary crystal grain phase is better, and the obtained magnetism is better.
150, stretching and flattening the annealed steel coil to obtain the high-magnetic-induction oriented silicon steel;
the technical scheme of this application is based on the research to low temperature high magnetic induction oriented silicon steel secondary recrystallization, and online measurement's steel band iron loss value P13/50 has synthesized the influence that has reflected size, phase, the nitriding amount of primary recrystallization crystalline grain, and steel band iron loss value P13/50 curve is not completely straight, and the difference exists certain fluctuation in the position promptly, consequently, the secondary recrystallization temperature that corresponds the position also is diverse, and the upper and lower limit of secondary recrystallization start temperature just makes according to this principle in this scheme. The quantity of the residual aluminum Alr reflects the strength of the capability of converting into AlN at the front section of nitriding in the subsequent procedure and high-temperature annealing, the more the quantity of the Alr is, the more the finally formed ALN is, the stronger the capability of inhibiting the growth of non-Gaussian grains in the high-temperature annealing process is, and the higher the secondary recrystallization starting temperature is. Therefore, according to the iron loss value P13/50 of the steel strip and the residual aluminum Alr, the furnace temperature range for starting secondary recrystallization can be obtained, high-temperature annealing can be carried out according to the actual crystallization temperature, the performance of the steel strip is improved, and the technical problems that the influence of Alr and primary recrystallization on the secondary recrystallization starting temperature is not considered in the prior art, the deviation of the process setting according to the single secondary recrystallization starting temperature and the actual crystallization temperature is caused, and the performance of the steel strip is influenced are solved. Meanwhile, the whole time of the high-temperature annealing process is shortened, the production efficiency is improved, and the cost is saved. Compared with the normal process, the average value of P17/50 is reduced by 0.03-0.08W/KG, B8 is improved by 0.01-0.03T, and the time for high-temperature annealing is saved by 3-18 hours.
In the high-temperature annealing temperature rise process, because the volume of the steel coil is large, the obvious temperature unevenness phenomenon exists on the upper end surface and the lower end surface of the inner ring and the outer ring in the common process, the larger the volume of the steel coil is, the larger the difference value between the maximum temperature and the minimum temperature is, in order to ensure that the temperature of the inner ring and the outer ring reaches the set temperature range, different temperature rise speeds are set according to the size of the steel coil, and all parts of the steel coil can be ensured to successfully reach the secondary recrystallization starting temperature in.
The second stage of heating adopts 100% N2In the atmosphere N2The increase slows the outward diffusion of N atoms in the steel and reduces Si3N4The (Al, Si) N, (Mn, Si) N and fine AlN are decomposed, so the temperature rise speed can be greatly improved, the condition that the inhibitor is rapidly decomposed to cause abnormal growth of primary crystal grains can not occur, compared with the prior art, the time for high-temperature annealing is saved by 3 to 18 hours, and the production efficiency is obviously improved. Meanwhile, the increase of the number of AlN coarsening of the steel in a pure N atmosphere can be avoided by increasing the temperature rise speed, the inhibition capability is weakened, and secondary recrystallization occurs in advance at a lower temperature, so that the conditions of inaccurate crystal grain phase and high iron loss are caused.
The third temperature rise process adopts variable N2The proportion is that the inhibitor is gradually decomposed in the process of starting secondary recrystallization, the decomposition speed is influenced by the N potential in the furnace atmosphere besides the temperature, and the temperature rise speed of the third section is different according to the difference of the upper limit and the lower limit of the secondary recrystallization temperature of the steel coil, so that the N is adjusted2The proportion of (a) is actually just adjusting the decomposition speed of the inhibitor to match the third-stage heating speed, so that secondary recrystallization is ensured to occur within a proper temperature range, and the magnetic level of the steel coil is improved.
The following are exemplified:
example one:
1. the steel-making components are as follows:
| element(s) | C | Si | Mn | S | Cu | Als | N |
| Example 1 and comparative example 1 | 0.04 | 2.6 | 0.1 | 0.005 | 0.06 | 0.0267 | 0.0079 |
The balance being Fe and inevitable impurities.
2. The heating temperature of hot rolling is 1160 ℃;
3. two-stage annealing normalization is adopted, and the temperature of the first stage is 1060 ℃; the temperature of the second section is 900 ℃;
4. adopting a one-step rolling method, wherein the aging temperature is 220 ℃, and the thickness of a finished product is 0.27 mm;
5. controlling the decarburization annealing temperature at 830 ℃, controlling the nitriding temperature at 850 ℃, coating a MgO-based high-temperature annealing separant after decarburization annealing and nitriding treatment, wherein the online P13min is 2.494, and the online P13max is 3.317;
6) high-temperature annealing: the temperature is increased to 700 ℃ for the first time, and the temperature is kept for 15 h; the temperature is firstly raised to the lower limit temperature Tmin of the secondary recrystallization starting temperature in the second heating, and is then raised to the upper limit temperature Tmax of the secondary recrystallization starting temperature in the third heating, wherein the upper limit temperature Tmax is 1090 ℃; the fourth time, the temperature is raised to 1170 ℃, and the temperature is preserved for 20 hours. The third heating rate V is 4.8 ℃/h, the second heating rate and the fourth heating rate are 45 ℃/h. And after the heat preservation at 1170 ℃ is finished, cooling at 20 ℃/h.
100 percent N is introduced into the first heating section to the second heating section2(ii) a H is introduced when the third temperature rise is started2+N2Mixed gas of N2The content of the active ingredients is 37 percent; at the end of the fourth temperature riseIntroduction of 100% H2。
Tmax, Tmin, V and N2The% can be determined according to empirical formulas (1) to (4).
lnTmax＝7.039-0.0571P13min+8.47Alr (1)
lnTmin＝7.039-0.0571P13max+8.47Alr (2)
V＝0.053(Tmax-Tmin)/R (3)
N2％＝25+2.5*V (4)
In the formula: p13max- -represents the maximum value of the decarburized sheet P13/50 measured by a continuous iron loss meter in W/kg; p13min- - -represents the minimum value of the decarburized sheet P13/50 measured by a continuous iron loss gauge in W/kg; alr- - -represents the remaining aluminum, calculated by Alr- -Als- (27/14). times.N, where Als is the acid soluble aluminum content in the steel and N is the N content in the steelmaking components in ppm; r represents the thickness of the steel coil in m
7) Stretching, flattening and annealing, and coating an insulating coating.
Comparative example one:
other processes are the same as the examples, and the high-temperature annealing process is carried out according to the conventional process: the temperature is increased to 750 ℃ for the first time, the temperature rising speed is the same as that of the embodiment, and the temperature is kept at 750 ℃ for 15 h; the temperature is raised for the second time to 1170 ℃ according to the temperature of 17 ℃/h, and the temperature is preserved for 20h under 1170 ℃; the temperature reduction process is the same as the embodiment.
Example two:
1. the steel-making components are as follows:
| element(s) | C | Si | Mn | S | Cu | Als | N |
| Example 2 and comparative example 2 | 0.06 | 2.9 | 0.05 | 0.006 | 0.06 | 0.0283 | 0.0082 |
The balance being Fe and inevitable impurities.
2. The hot rolling heating temperature is 1170 ℃;
3. two-stage annealing normalization is adopted, and the temperature of the first stage is 1070 ℃; the temperature of the second section is 920 ℃;
4. adopting a primary rolling method, and carrying out at least one time of aging rolling, wherein the aging temperature is as follows: the temperature is 205 ℃, and the thickness of the finished product is 0.27 mm;
5. controlling the decarburization annealing temperature at 820 ℃, controlling the nitriding temperature at 880 ℃, coating a high-temperature annealing separant mainly containing MgO after decarburization annealing and nitriding treatment, wherein the online P13min is 2.485, and the online P13max is 3.133;
6) high-temperature annealing: the temperature is increased to 700 ℃ for the first time, and the temperature is kept for 15 h; the temperature is firstly raised to the lower limit temperature Tmin of the secondary recrystallization starting temperature at the second temperature rise of 1060 ℃, and the temperature is slowly raised to the upper limit temperature Tmax of the secondary recrystallization starting temperature at the third temperature rise of 1100 ℃; the temperature is raised to 1190 ℃ for the fourth time, and the temperature is kept for 20 hours. The third heating rate V is 5.3 ℃/h, the second heating rate and the fourth heating rate are 50 ℃/h. And after the heat preservation at 1170 ℃ is finished, cooling at 20 ℃/h.
Introducing 100% N2 in the first heating section to the second heating section; introducing H2+ N2 mixed gas when the third temperature rise starts, wherein the N2 accounts for 38%; at the end of the fourth temperature rise, 100% H2 was introduced.
Tmax, Tmin, V and N2% can be determined according to empirical formulas (1) to (4).
lnTmax＝7.039-0.0571P13min+8.47Alr (1)
lnTmin＝7.039-0.0571P13max+8.47Alr (2)
V＝0.053(Tmax-Tmin)/R (3)
N2％＝25+2.5*V (4)
In the formula: p13max- -represents the maximum value of the decarburized sheet P13/50 measured by a continuous iron loss meter in W/kg; p13min- - -represents the minimum value of the decarburized sheet P13/50 measured by a continuous iron loss gauge in W/kg; alr- - -represents the remaining aluminum, calculated by Alr- -Als- (27/14). times.N, where Als is the acid soluble aluminum content in the steel and N is the N content in the steelmaking components in ppm; r represents the thickness of the steel coil in m
7) Stretching, flattening and annealing, and coating an insulating coating.
Comparative example two:
other processes are the same as the embodiment, and the high-temperature annealing process is carried out according to the conventional process: the temperature is raised to 700 ℃ for the first time, the temperature raising speed is the same as that of the embodiment, and the temperature is kept for 15h at 700 ℃; heating to 1190 ℃ according to the temperature of 17 ℃/h for the second time, and preserving the heat for 20h at the temperature of 1190 ℃; the temperature reduction process is the same as the embodiment.
Example three:
1. the steel-making components are as follows:
| element(s) | C | Si | Mn | S | Cu | Als | N |
| Example 3 and comparative example 3 | 0.042 | 2.7 | 0.09 | 0.004 | 0.08 | 0.249 | 0.0071 |
The balance being Fe and inevitable impurities.
2. The hot rolling heating temperature is 1155 ℃;
3. two-stage annealing normalization is adopted, and the temperature of the first stage is 1090 ℃; the temperature of the second section is 900 ℃;
4. adopting a primary rolling method, and carrying out at least one time of aging rolling, wherein the aging temperature is as follows: the thickness of the finished product is 0.20mm at 195 ℃;
5. controlling the decarburization annealing temperature at 840 ℃, controlling the nitriding temperature at 860 ℃, coating a high-temperature annealing separant mainly containing MgO after decarburization annealing and nitriding treatment, wherein the online P13min is 2.452, and the online P13max is 3.613;
6) high-temperature annealing: the temperature is increased to 700 ℃ for the first time, and the temperature is kept for 15 h; the temperature is firstly raised to the lower limit temperature Tmin of the secondary recrystallization starting temperature for the second time, and is slowly raised to the upper limit temperature Tmax of the secondary recrystallization starting temperature for the third time, wherein the upper limit temperature Tmax is 1090 ℃; the fourth temperature rise is carried out to 1200 ℃ and the temperature is kept for 20 h. The third heating rate V is 7.27 ℃/h, the second heating rate is 70 ℃ and the fourth heating rate is 60 ℃/h. Cooling at the temperature of 20 ℃/h after the heat preservation at the temperature of 1200 ℃.
Introducing 100% N2 in the first heating section to the second heating section; introducing H2+ N2 mixed gas when the third temperature rise starts, wherein N2 accounts for 43%; at the end of the fourth temperature rise, 100% H2 was introduced.
Tmax, Tmin, V and N2% can be determined according to empirical formulas (1) to (4).
lnTmax＝7.039-0.0571P13min+8.47Alr (1)
lnTmin＝7.039-0.0571P13max+8.47Alr (2)
V＝0.053(Tmax-Tmin)/R (3)
N2％＝25+2.5*V (4)
In the formula: p13max- -represents the maximum value of the decarburized sheet P13/50 measured by a continuous iron loss meter in W/kg; p13min- - -represents the minimum value of the decarburized sheet P13/50 measured by a continuous iron loss gauge in W/kg; alr- - -represents the remaining aluminum, calculated by Alr- -Als- (27/14). times.N, where Als is the acid soluble aluminum content in the steel and N is the N content in the steelmaking components in ppm; r represents the thickness of the steel coil in m
7) Stretching, flattening and annealing, and coating an insulating coating.
Comparative example three:
other processes are the same as the embodiment, and the high-temperature annealing process is carried out according to the conventional process: the temperature is raised to 700 ℃ for the first time, the temperature raising speed is the same as that of the embodiment, and the temperature is kept for 15h at 700 ℃; the temperature is raised to 1200 ℃ for the second time according to the speed of 17 ℃/h, and the temperature is kept for 20h at 1200 ℃; the temperature reduction process is the same as the embodiment.
Example four:
1. the steel-making components are as follows:
| element(s) | C | Si | Mn | S | Cu | Als | N |
| Example 4 and comparative example 4 | 0.065 | 3.6 | 0.11 | 0.005 | 0.15 | 0.0274 | 0.0080 |
The balance being Fe and inevitable impurities.
2. The hot rolling heating temperature is 1165 ℃;
3. two-stage annealing normalization is adopted, and the temperature of the first stage is 1060 ℃; the temperature of the second section is 910 ℃;
4. adopting a primary rolling method, and carrying out at least one time of aging rolling, wherein the aging temperature is as follows: the thickness of the finished product is 0.18mm at 200 ℃;
5. controlling the decarburization annealing temperature at 850 ℃, controlling the nitriding temperature at 910 ℃, coating a high-temperature annealing separant mainly containing MgO after decarburization annealing and nitriding treatment, wherein the online P13min is 2.726, and the online P13max is 3.566;
6) high-temperature annealing: the temperature is increased to 700 ℃ for the first time, and the temperature is kept for 15 h; the temperature is firstly raised to the lower limit temperature Tmin of the secondary recrystallization starting temperature for the second time, and is 1030 ℃, and the temperature is slowly raised to the upper limit temperature Tmax of the secondary recrystallization starting temperature for the third time, and is 1095 ℃; the fourth time, the temperature is raised to 1210 ℃ and the temperature is kept for 20 hours. The third heating rate V is 6.89 ℃/h, the second heating rate is 75 ℃ and the fourth heating rate is 70 ℃/h. And cooling at the temperature of 20 ℃/h after the heat preservation at the temperature of 1210 ℃ is finished.
100 percent N is introduced into the first heating section to the second heating section2(ii) a H is introduced when the third temperature rise is started2+N2Mixed gas of N2The content of the active ingredients is 42 percent; at the end of the fourth temperature rise, 100% H2 was introduced.
Tmax, Tmin, V and N2% can be determined according to empirical formulas (1) to (4).
lnTmax＝7.039-0.0571P13min+8.47Alr (1)
lnTmin＝7.039-0.0571P13max+8.47Alr (2)
V＝0.053(Tmax-Tmin)/R (3)
N2％＝25+2.5*V (4)
In the formula: p13max- -represents the maximum value of the decarburized sheet P13/50 measured by a continuous iron loss meter in W/kg; p13min- - -represents the minimum value of the decarburized sheet P13/50 measured by a continuous iron loss gauge in W/kg; alr- - -represents the remaining aluminum, calculated by Alr- -Als- (27/14). times.N, where Als is the acid soluble aluminum content in the steel and N is the N content in the steelmaking components in ppm; r represents the thickness of the steel coil in m
7) Stretching, flattening and annealing, and coating an insulating coating.
Comparative example four:
other processes are the same as the embodiment, and the high-temperature annealing process is carried out according to the conventional process: the temperature is raised to 700 ℃ for the first time, the temperature raising speed is the same as that of the embodiment, and the temperature is kept for 15h at 700 ℃; the temperature is raised to 1210 ℃ for the second time according to the speed of 17 ℃/h, and the temperature is preserved for 20h at 1210 ℃; the temperature reduction process is the same as the embodiment.
Example five:
1. the steel-making components are as follows:
| element(s) | C | Si | Mn | S | Cu | Als | N |
| Example 5 and comparative example 5 | 0.045 | 2.8 | 0.08 | 0.01 | 0.03 | 0.0294 | 0.0085 |
The balance being Fe and inevitable impurities.
2. The hot rolling heating temperature is 1175 ℃;
3. two-stage annealing normalization is adopted, and the temperature of the first stage is 1065 ℃; the temperature of the second section is 880 ℃;
4. adopting a primary rolling method, and carrying out at least one time of aging rolling, wherein the aging temperature is as follows: the thickness of the finished product is 0.3mm at 220 ℃;
5. controlling the decarburization annealing temperature at 855 ℃, controlling the nitriding temperature at 880 ℃, coating a high-temperature annealing separant mainly containing MgO after decarburization annealing and nitriding treatment, wherein the online P13min is 2.636, and the online P13max is 3.04;
6) high-temperature annealing: the temperature is increased to 700 ℃ for the first time, and the temperature is kept for 15 h; the temperature is firstly raised to the lower limit temperature Tmin of the secondary recrystallization starting temperature in the second temperature rise, and is 1070 ℃, and the temperature is slowly raised to the upper limit temperature Tmax of the secondary recrystallization starting temperature in the third temperature rise, and is 1095 ℃; the fourth time, the temperature is raised to 1170 ℃, and the temperature is preserved for 20 hours. The third heating rate V is 2.29 ℃/h, the second heating rate is 40 ℃ and the fourth heating rate is 40 ℃/h. And after the heat preservation at 1170 ℃ is finished, cooling at 20 ℃/h.
Introducing 100% N2 in the first heating section to the second heating section; introducing H2+ N2 mixed gas when the third temperature rise starts, wherein N2 accounts for 31%; at the end of the fourth temperature rise, 100% H2 was introduced.
Tmax, Tmin, V and N2% can be determined according to empirical formulas (1) to (4).
lnTmax＝7.039-0.0571P13min+8.47Alr (1)
lnTmin＝7.039-0.0571P13max+8.47Alr (2)
V＝0.053(Tmax-Tmin)/R (3)
N2％＝25+2.5*V (4)
In the formula: p13max- -represents the maximum value of the decarburized sheet P13/50 measured by a continuous iron loss meter in W/kg; p13min- - -represents the minimum value of the decarburized sheet P13/50 measured by a continuous iron loss gauge in W/kg; alr- - -represents the remaining aluminum, calculated by Alr- -Als- (27/14). times.N, where Als is the acid soluble aluminum content in the steel and N is the N content in the steelmaking components in ppm; r represents the thickness of the steel coil in m
7) Stretching, flattening and annealing, and coating an insulating coating.
Comparative example five:
other processes are the same as the embodiment, and the high-temperature annealing process is carried out according to the conventional process: the temperature is raised to 700 ℃ for the first time, the temperature raising speed is the same as that of the embodiment, and the temperature is kept for 15h at 700 ℃; the temperature is raised for the second time to 1170 ℃ according to the temperature of 17 ℃/h, and the temperature is preserved for 20h under 1170 ℃; the temperature reduction process is the same as the embodiment.
Example six:
1. the steel-making components are as follows:
the balance being Fe and inevitable impurities.
2. The hot rolling heating temperature is 1195 ℃;
3. two-stage annealing normalization is adopted, and the temperature of the first stage is 1050 ℃; the temperature of the second section is 880 ℃;
4. adopting a primary rolling method, and carrying out at least one time of aging rolling, wherein the aging temperature is as follows: the thickness of the finished product is 0.23mm at 220 ℃;
5. controlling the decarburization annealing temperature at 855 ℃, controlling the nitriding temperature at 880 ℃, coating a high-temperature annealing separant mainly containing MgO after decarburization annealing and nitriding treatment, wherein the online P13min is 2.75, and the online P13max is 3.485;
6) high-temperature annealing: the temperature is increased to 700 ℃ for the first time, and the temperature is kept for 15 h; the temperature is firstly raised to the lower limit temperature Tmin of the secondary recrystallization starting temperature at the second temperature rise, and is raised to the upper limit temperature Tmax of the secondary recrystallization starting temperature at the third temperature rise, wherein the Tmax is 1080 ℃; the fourth time, the temperature is increased to 1180 ℃, and the temperature is kept for 20 hours. The third heating rate V is 4.1 ℃/h, the second heating rate is 60 ℃ and the fourth heating rate is 55 ℃/h. And cooling at the temperature of 1180 ℃ according to the speed of 20 ℃/h after the heat preservation is finished.
Introducing 100% N2 in the first heating section to the second heating section; introducing H2+ N2 mixed gas when the third temperature rise starts, wherein the N2 accounts for 35%; at the end of the fourth temperature rise, 100% H2 was introduced.
Tmax, Tmin, V and N2% can be determined according to empirical formulas (1) to (4).
lnTmax＝7.039-0.0571P13min+8.47Alr (1)
lnTmin＝7.039-0.0571P13max+8.47Alr (2)
V＝0.053(Tmax-Tmin)/R (3)
N2％＝25+2.5*V (4)
In the formula: p13max- -represents the maximum value of the decarburized sheet P13/50 measured by a continuous iron loss meter in W/kg; p13min- - -represents the minimum value of the decarburized sheet P13/50 measured by a continuous iron loss gauge in W/kg; alr- - -represents the remaining aluminum, calculated by Alr- -Als- (27/14). times.N, where Als is the acid soluble aluminum content in the steel and N is the N content in the steelmaking components in ppm; r represents the thickness of the steel coil in m
7) Stretching, flattening and annealing, and coating an insulating coating.
Comparative example six:
other processes are the same as the embodiment, and the high-temperature annealing process is carried out according to the conventional process: the temperature is raised to 700 ℃ for the first time, the temperature raising speed is the same as that of the embodiment, and the temperature is kept for 15h at 700 ℃; heating to 1180 ℃ according to the temperature of 17 ℃/h for the second time, and keeping the temperature at 1180 ℃ for 20 h; the temperature reduction process is the same as the embodiment.
The test results of the examples and comparative examples are shown in table 1:
table 1 shows the measured head and tail magnetic properties of each example and comparative example
As can be seen from Table 1, the process P according to the invention is used17/50Can reduce the weight by 0.08W/kg at most, B8The maximum 0.025T can be improved, and the high-temperature annealing time is saved by 14.44h at most.
The present embodiments are merely preferred examples, and are not intended to limit the scope of the present invention.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. The production method of the high magnetic induction oriented silicon steel is characterized in that the high magnetic induction oriented silicon steel comprises the following chemical components in percentage by weight: c: 0.03 to 0.07%, Si: 2.0-3.8%, Mn: 0.05-0.2%, S: 0.005-0.01%, Al: 0.020-0.035%, N: 0.005-0.01%, Cu: 0.05 to 0.25 percent, and the balance being Fe and inevitable impurities;
the production method comprises the following steps:
obtaining a plate blank;
carrying out hot rolling, cold rolling and decarburization treatment on the plate blank to obtain a decarburization plate;
curling the decarburized plate to obtain a steel coil;
the high-temperature annealing of the steel coil comprises the following steps: the temperature is increased to 600-750 ℃ for the first time, and the temperature is kept for 10-20 h; the second temperature rise is firstly carried out to the lower limit temperature Tmin of the secondary recrystallization starting temperature; raising the temperature for the third time to the upper limit temperature Tmax of the secondary recrystallization starting temperature; the fourth temperature rise is 1170-1220 ℃, and the temperature is kept for 20-30 h;
stretching and flattening the annealed steel coil to obtain the high-magnetic-induction oriented silicon steel;
wherein the third temperature increase rate is lower than the second temperature increase rate, the lower limit temperature Tmin is determined by a maximum value P13max of the remaining aluminum Alr and a strip iron loss value P13/50 of a decarburization plate of the decarburization plate, and the upper limit temperature Tmax is determined by a minimum value P13min of the remaining aluminum Alr and a strip iron loss value P13/50 of the decarburization plate;
the lower limit temperature Tmin is determined by the residual aluminum Alr and the maximum value P13max of the steel strip iron loss value P13/50 of the decarburization plate, and specifically comprises the following steps: obtaining said lower limit temperature Tmin from lnTmin ═ a-b ═ P13max + c ═ Alr;
the upper limit temperature Tmax is determined by the residual aluminum Alr and the minimum value P13min of the iron loss P13/50 of the steel strip of the decarburization plate, and specifically comprises the following steps: obtaining the upper limit temperature Tmax according to lnTmax ═ a-b ═ P13min + c ═ Alr; wherein a is 7.0-7.1, b is 0.05-0.06, and c is 8.4-8.5.
2. The production method as claimed in claim 1, wherein the third heating rate V ═ 0.053(Tmax-Tmin)/R, R —, represents the thickness of the steel coil.
3. The method of claim 1, wherein the rate of the second temperature increase and the rate of the fourth temperature increase are 40 to 75 ℃/h.
4. The method of claim 1, wherein 100% N is introduced during the first heating to the second heating2。
5. The process according to claim 4, wherein H is introduced at the start of the third temperature increase2And N2And (3) mixing the gas, wherein N2% is 25+ 2.5V, and the temperature rise speed V is not more than 17 ℃/h.
6. The method of claim 5, wherein 100% H is introduced at the end of the fourth ramp2。
7. The production method as claimed in claim 1, wherein the temperature of the decarburization treatment is controlled to 800-860 ℃.
8. The production method according to claim 1, wherein said cold rolling of said slab comprises:
and (3) carrying out aging rolling for at least one time by adopting a one-time rolling method, wherein the thickness of a finished product is less than or equal to 0.3 mm.
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