CN104894354B - A kind of Low Temperature Hot Rolling plate prepares the production method of Thin Specs high magnetic induction grain-oriented silicon steel - Google Patents
A kind of Low Temperature Hot Rolling plate prepares the production method of Thin Specs high magnetic induction grain-oriented silicon steel Download PDFInfo
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Abstract
The present invention relates to material processing field, discloses the production method that a kind of Low Temperature Hot Rolling plate prepares Thin Specs high magnetic induction grain-oriented silicon steel, wherein, this method includes：S1, hot rolling；S2, normalizing heat treatment；S3, cold rolling；S4, decarburizing annealing processing；S5, cold rolling plate surface coat MgO coatings；S6, the high temperature anneal is carried out, wherein, S6 steps include：The cold-reduced sheet is inserted in Equipment for Heating Processing and heated up with the first heating rate, starts to be passed through NH into the Equipment for Heating Processing when temperature reaches 850 870 DEG C3, stop being passed through NH when temperature reaches the first temperature3, second temperature is then warming up to the second heating rate and is incubated.During nitridation steps are attached into the high temperature anneal, the nitridation steps after decarburizing annealing are not only saved, save the energy, also nitriding and high temperature secondary recrystallization is disposably completed in the high annealing stage, simplifies production technology, save production cost.
Description
Technical field
The present invention relates to material processing field, in particular it relates to which to prepare Thin Specs high magentic induction oriented for a kind of Low Temperature Hot Rolling plate
The production method of silicon steel.
Background technology
Orientation silicon steel has excellent magnetic property, is typically used as the iron core of transformer, is composition portion important in transformer
Point.The excellent magnetic property of orientation silicon steel comes from the single sharp Goss texture formed after secondary recrystallization, and good in order to obtain
Secondary recrystallization tissue, it is necessary to coordinate enough inhibitor to control growing up for primary recrystallization.
In order to solve to produce problem caused by high-temperature heating technology, production cost is reduced, usually using low-temperature heat skill
Art prepares orientation silicon steel.Low-temperature heat technology, generally only need to be by slab using low-temperature heat strand+follow-up nitridation technique
1100~1200 DEG C are heated to, the deficiency of inhibitor is being made up by follow-up nitridation process.
At present, the orientation silicon steel used in transformer is generally silicon steel sheet form, can be cast silicon steel by rolling mill practice
Base is processed as the silicon steel sheet of suitable thickness.The rolling mill practice generally includes hot rolling, normalizing, cold rolling, nitriding, decarburization, high annealing
Etc. step.However, such operation of rolling step is more, the production cycle is longer, and production cost is higher.
A kind of accordingly, it is desirable to provide production method of shorter high magnetic induction grain-oriented silicon steel sheet material of production cycle.
The content of the invention
It is an object of the invention to provide a kind of preparation method for the high magnetic induction grain-oriented silicon steel sheet material that can shorten the production cycle.
To achieve these goals, the present invention provides the life that a kind of Low Temperature Hot Rolling plate prepares Thin Specs high magnetic induction grain-oriented silicon steel
Production method, wherein, this method includes：S1, by the hot rolling of silicon steel strand it is hot rolled plate；S2, the hot rolled plate is carried out at normalizing heat
Reason；S3, normalizing is heat-treated after the hot rolled plate cold rolling be cold-reduced sheet；S4, decarburizing annealing processing is carried out to the cold-reduced sheet；
S5, the cold rolling plate surface coat MgO coatings；S6, the high temperature anneal is carried out to the cold-reduced sheet for coating MgO coatings,
Wherein, S6 steps include：The cold-reduced sheet is inserted in Equipment for Heating Processing and heated up with the first heating rate, when temperature reaches 850-
Start to be passed through NH into the Equipment for Heating Processing at 870 DEG C3, stop being passed through NH when temperature reaches the first temperature3, then with
Two heating rates are warming up to second temperature and are incubated.
Preferably, in step s 6, first temperature is 880-900 DEG C, and the second temperature is 1180-1200 DEG C,
Soaking time of the cold-reduced sheet under the second temperature is 15-20h.
Preferably, in step s 6, first heating rate is 8-10K/s, and second heating rate is 18-20K/
s。
Preferably, in step s 6, it is passed through NH3Speed be 1-2L/min.
Preferably, in step s 6, the atmosphere of the insulation is pure hydrogen atmosphere.
Preferably, in step sl, by the silicon steel heating strand to carrying out hot rolling after 1000-1200 DEG C.
Preferably, in step sl, the silicon steel strand by 7-9 hot rolling pass by thickness for 300mm-330mm
Finish to gauge is the hot rolled plate that thickness is 2.2-2.4mm, wherein, the reduction ratio of each hot rolling pass is 30%-60%.
Preferably, in step s3, it is that thickness is 0.16- by the hot rolled plate finish to gauge by 6-8 cold rolling pass
0.18mm cold-reduced sheet, wherein, the reduction ratio of each cold rolling pass is 20%-40%.
Preferably, in step s3, aging strengthening model is carried out between adjacent cold rolling pass：The hot rolled plate is inserted into heat
In processing equipment, 5-10min is incubated at 240-250 DEG C.
Preferably, two-part normalizing heat treatment is carried out in step s 2, wherein, step S2 includes：S2-1, by the hot rolling
Plate is incubated 150-160s at 1050 DEG C~1100 DEG C；S2-2, by the hot rolled plate air cooling to 900-950 DEG C and it is incubated 90-
100s；S2-3, by the hot rolled plate air cooling to 800-820 DEG C, be subsequently placed in 90-100 DEG C of water and cool down.
Preferably, in step s3, pickling processes are carried out to the hot rolled plate before cold rolling.
Preferably, in step s 4, the cold-reduced sheet is inserted in Equipment for Heating Processing, 3- is incubated at 850-900 DEG C
4min, while be 4-5 by the volume ratio of nitrogen and hydrogen：3 mixed gas is passed through the heat after being soaked in 80-85 DEG C of water
Carbonization treatment is carried out in processing equipment.
Preferably, the mass percent of the chemical composition of the silicon steel strand is：Si：2.6~3.45%, C：0.050~
0.080%, Mn：0.08~0.12%, S：0.005~0.007%, Cr：0.08~0.12%, Cu：0.006~0.012%,
Al：0.02~0.03%, N：0.0050~0.008%, Sn：0.04~0.06%, surplus Fe.
Pass through above-mentioned technical proposal, during nitridation steps are attached into the high temperature anneal, not only save de-
Nitridation steps after carbon annealing, save the energy, also disposably complete nitriding and high temperature secondary recrystallization in the high annealing stage,
Production technology is simplified, saves production cost.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The embodiment of the present invention is described in detail below.It is it should be appreciated that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to limit the invention.
The invention provides the production method that a kind of Low Temperature Hot Rolling plate prepares Thin Specs high magnetic induction grain-oriented silicon steel, wherein, should
Method includes：S1, by the hot rolling of silicon steel strand it is hot rolled plate；S2, normalizing heat treatment is carried out to the hot rolled plate；S3, by normalizing heat
The hot rolled plate cold rolling after processing is cold-reduced sheet；S4, decarburizing annealing processing is carried out to the cold-reduced sheet；S5, in the cold rolling
Plate surface coats MgO coatings；S6, the high temperature anneal is carried out to the cold-reduced sheet for coating MgO coatings, wherein, S6 step bags
Include：By the cold-reduced sheet insert in Equipment for Heating Processing with the first heating rate heat up, start when temperature reaches 850-870 DEG C to
NH is passed through in the Equipment for Heating Processing3, stop being passed through NH when temperature reaches the first temperature3, then heated up with the second heating rate
To second temperature and it is incubated.
In preparation method on described above, during nitridation steps are attached into the high temperature anneal, not only save
Nitridation steps after decarburizing annealing, save the energy, nitriding are disposably also completed in the high annealing stage and high temperature is secondary again
Crystallization, simplifies production technology, saves production cost.
This method core concept is, carries out nitriding before magnesium oxide coating forms magnesium silicate layer, magnesium silicate bottom is general
900 DEG C~1000 DEG C are formed at, nitriding is carried out at 850~900 DEG C can avoid the formation of magnesium silicate bottom from hindering nitrogenizing effect, because
High-temperature annealing process and nitriding process can be combined together by this, reduce operating procedure.It can be formed directly with after nitriding
The AlN inhibitor of effect, rather than form Si3N4(Si, Mn) N particles.Using this method, nitridation can be saved in high annealing
The transition process of thing particle, shorten the high annealing time.
Further, in step s 6, first temperature is 880-900 DEG C, and the second temperature is 1180-1200
DEG C, soaking time of the cold-reduced sheet at 1180-1200 DEG C is 15-20h.As described above, magnesium silicate reaches 900 DEG C in temperature
Initially form later, therefore, can stop being passed through NH when temperature reaches 880-900 DEG C3, what is remained afterwards still can support
Nitrizing Treatment process is carried out.Continue to be warming up at 1180-1200 DEG C and be incubated carry out high annealing.
In addition, in step s 6, first heating rate is 8-10K/s, second heating rate is 18-20K/s.
In addition, in step s 6, it is passed through NH3Speed be 1-2L/min.
In addition, in step s 6, the atmosphere of the insulation is pure hydrogen atmosphere, the surface of the cold-reduced sheet is protected not by high temperature
Corrode.
In addition, in step sl, by the heating strand to carrying out hot rolling after 1000-1200 DEG C.
Wherein, in step sl, the silicon steel strand finish to gauge by 7-9 hot rolling pass by thickness for 300-330mm
The hot rolled plate for being 2.2-2.4mm for thickness, wherein, the reduction ratio of each hot rolling pass is 30%-60%.Wherein hot rolling pass
Reduction ratio can be gradually lowered, and little by little improve rolling accuracy.
Further, in step s3, it is that thickness is 0.16- by the hot rolled plate finish to gauge by 6-8 cold rolling pass
0.18mm cold-reduced sheet, wherein, the reduction ratio of each cold rolling pass is 20%-40%.
In addition, in step s3, aging strengthening model is carried out between cold rolling pass：The hot rolled plate is inserted into Equipment for Heating Processing
In, it is incubated 5-10min at 240-250 DEG C.Avoid after secondary recrystallization crystallite dimension excessive and cause iron loss to raise, increase is just
Goss texture components after secondary recrystallization, reduce secondary recrystallization crystal particle dimension.Wherein it is possible to aging strengthening model is selected as needed
Number and carried out between corresponding cold rolling pass.For example, in step s3, cold rollings can be carried out by 6 passages, and can be with
Between the first passage and second time, between the 3rd passage and four-pass and between four-pass and the 5th passage respectively
Carry out an aging strengthening model.
In addition, two-part normalizing heat treatment is carried out in step s 2, wherein, step S2 includes：S2-1, by the hot rolled plate
150-160s is incubated at 1050 DEG C~1100 DEG C；S2-2, by the hot rolled plate air cooling to 900-950 DEG C and it is incubated 90-100s；
S2-3, by the hot rolled plate air cooling to 800-820 DEG C, be subsequently placed in 90-100 DEG C of water and cool down.At two-period form normalizing heat
Reason can be such that particle fully separates out, and ensure the uniformity of primary recrystallization tissue.
In addition, in step s3, pickling processes are carried out to the hot rolled plate before cold rolling, to remove the hot rolled plate table
The impurity in face.Hydrochloric acid, sulfuric acid or other common acids or mixing pickle can be used to carry out pickling, and washed using clear water.
In addition, in step s 4, the cold-reduced sheet is inserted in Equipment for Heating Processing, 3-4min is incubated at 850-900 DEG C,
It is simultaneously 4-5 by the volume ratio of nitrogen and hydrogen：3 mixed gas is passed through the heat treatment after being soaked in 80-85 DEG C of water
Carbonization treatment is carried out in equipment.High magentic induction oriented steel requires that carbon content is low as much as possible, it is therefore desirable to decarburization is carried out after rolling
Processing.The mixed gas of nitrogen and hydrogen can improve temperature after being soaked in the water of higher temperature, can accelerate the speed of decarburization
Degree, while good oxide-film can also be formed.
In addition, the mass percent of the chemical composition of the silicon steel strand is：Si：2.6~3.45%, C：0.050~
0.080%, Mn：0.08~0.12%, S：0.005~0.007%, Cr：0.08~0.12%, Cu：0.006~0.012%,
Al：0.02~0.03%, N：0.0050~0.008%, Sn：0.04~0.06%, surplus Fe.Wherein, the silicon steel strand
In be inevitably present a small amount of other impurity, be not described further herein.
Advantages of the present invention will be illustrated by embodiment below.
The mass percent of the chemical composition of used silicon steel strand is in the examples below：Si：2.6~
3.45%, C：0.050~0.080%, Mn：0.08~0.12%, S：0.005~0.007%, Cr：0.08~0.12%, Cu：
0.006~0.012%, Al：0.02~0.03%, N：0.0050~0.008%, Sn：0.04~0.06%, surplus be Fe and
Inevitable impurity.
Embodiment 1
S1, by the silicon steel strand of 300mm thickness, (mass percent of the chemical composition of silicon steel strand is：Si：2.6%, C：
0.050%, Mn：0.08%, S：0.005%, Cr：0.08%, Cu：0.006%, Al：0.02%, N：0.0050%, Sn：
0.04%, surplus is Fe and inevitable impurity) it is heated to carry out hot rolling after 1000 DEG C to obtain 2.4mm hot rolled plate, its heat
Rolling degree such as table 1 below
Table 1
| Hot rolling pass | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Reduction ratio | 60% | 54% | 51% | 49% | 50% | 45% | 37% |
S2, by the hot rolled plate carry out two-period form normalizing heat treatment, wherein,
S2-1, the hot rolled plate is incubated 155s at 1080 DEG C；
S2-2, the hot rolled plate air cooling to 900 DEG C and is incubated 100s；
S2-3, by the hot rolled plate air cooling to 820 DEG C, be subsequently placed in 90 DEG C of water and cool down.
S3, the hot rolled plate carried out to be cold rolled to 0.16mm, wherein, the cold rolling system such as table 2 below,
Table 2
S4, the cold-reduced sheet inserted in Equipment for Heating Processing, be incubated 3min at 880 DEG C, while by nitrogen and hydrogen
Volume ratio is 4：3 mixed gas is passed through in the Equipment for Heating Processing after being soaked in 80 DEG C of water and carries out carbonization treatment.
S5, take out the cold-reduced sheet coating MgO coatings after carbonization treatment.
S6, the cold-reduced sheet is inserted in Equipment for Heating Processing and heated up with 10K/s heating rate, when temperature reaches 850 DEG C
When, start to be passed through NH into the Equipment for Heating Processing with 1L/min flow velocity3, stop being passed through NH when temperature reaches 880 DEG C3, so
1180 DEG C are warming up to 20K/s heating rate and be incubated 18h under pure hydrogen atmosphere afterwards.
Embodiment 2
S1, by the silicon steel strand of 330mm thickness, (mass percent of the chemical composition of silicon steel strand is：：Si：3.45%,
C：0.080%, Mn：0.12%, S：0.007%, Cr：0.12%, Cu：0.012%, Al：0.03%, N：0.008%, Sn：
0.06%, surplus is Fe and inevitable impurity) it is heated to carry out hot rolling after 1200 DEG C to obtain 2.2mm hot rolled plate, its heat
Rolling degree such as table 3 below
Table 3
| Hot rolling pass | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| Reduction ratio | 58% | 52% | 49% | 42% | 40% | 39% | 36% | 32% | 30% |
S2, by the hot rolled plate carry out two-period form normalizing heat treatment, wherein,
S2-1, the hot rolled plate is incubated 150s at 1050 DEG C；
S2-2, the hot rolled plate air cooling to 950 DEG C and is incubated 90s；
S2-3, by the hot rolled plate air cooling to 800 DEG C, be subsequently placed in 95 DEG C of water and cool down.
S3, the hot rolled plate carried out to be cold rolled to 0.18mm, wherein, the cold rolling system such as table 4 below,
Table 4
S4, the cold-reduced sheet inserted in Equipment for Heating Processing, be incubated 3.5min at 850 DEG C, while by nitrogen and hydrogen
Volume ratio be 1.5：1 mixed gas is passed through in the Equipment for Heating Processing after being soaked in 80 DEG C of water and carries out carbonization treatment.
S5, take out the cold-reduced sheet coating MgO coatings after carbonization treatment.
S6, the cold-reduced sheet is inserted in Equipment for Heating Processing and heated up with 9K/s heating rate, when temperature reaches 870 DEG C
When, start to be passed through NH into the Equipment for Heating Processing with 1.5L/min flow velocity3, stop being passed through NH when temperature reaches 900 DEG C3,
Then 1190 DEG C are warming up to 18K/s heating rate and are incubated 15h under pure hydrogen atmosphere.
Embodiment 3
S1, by the silicon steel strand of 320mm thickness, (mass percent of the chemical composition of silicon steel strand is：Si：3.05%,
C：0.070%, Mn：0.09%, S：0.006%, Cr：0.11%, Cu：0.010%, Al：0.025%, N：0.007%, Sn：
0.05%, surplus is Fe and inevitable impurity) it is heated to carry out hot rolling after 1100 DEG C to obtain 2.3mm hot rolled plate, its heat
Rolling degree such as table 5 below
Table 5
| Hot rolling pass | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 |
| Reduction ratio | 57% | 51% | 47% | 49% | 49% | 40% | 41% | 30% |
S2, by the hot rolled plate carry out two-period form normalizing heat treatment, wherein,
S2-1, the hot rolled plate is incubated 160s at 1100 DEG C；
S2-2, the hot rolled plate air cooling to 925 DEG C and is incubated 95s；
S2-3, by the hot rolled plate air cooling to 810 DEG C, be subsequently placed in 100 DEG C of water and cool down.
S3, the hot rolled plate carried out to be cold rolled to 0.17mm, wherein, the cold rolling system such as table 2 below,
Table 6
S4, the cold-reduced sheet inserted in Equipment for Heating Processing, be incubated 4min at 900 DEG C, while by nitrogen and hydrogen
Volume ratio is 5：3 mixed gas is passed through in the Equipment for Heating Processing after being soaked in 80 DEG C of water and carries out carbonization treatment.
S5, take out the cold-reduced sheet coating MgO coatings after carbonization treatment.
S6, the cold-reduced sheet is inserted in Equipment for Heating Processing and heated up with 8K/s heating rate, when temperature reaches 860 DEG C
When, start to be passed through NH into the Equipment for Heating Processing with 2L/min flow velocity3, stop being passed through NH when temperature reaches 890 DEG C3, so
1200 DEG C are warming up to 19K/s heating rate and be incubated 20h under pure hydrogen atmosphere afterwards.
Comparative example
Carried out successively at Nitrizing Treatment and high annealing by the cold-reduced sheet prepared in above example 3 through step S1-S4
Reason, wherein, the cold-reduced sheet is warming up to 860 DEG C, is passed through NH3, nitriding time 1min；By the cold-reduced sheet after nitriding at 1200 DEG C
And it is incubated 20h under pure hydrogen atmosphere.
The magnetic property such as table 7 below of the silicon plate prepared by three embodiments described above and comparative example,
Table 7
| Embodiment | Magnetic strength B8 | Iron loss P17/50 |
| 1 | 1.91 | 0.9 |
| 2 | 1.90 | 1.0 |
| 3 | 1.92 | 0.86 |
| Comparative example | 1.82 | 1.33 |
By visible with upper table 7, compared with product prepared by conventional method, the silicon plate of method of the invention preparation
Magnetic property is good, and the combination of nitridation steps and high-temperature annealing step does not cause product magnetic property to decline, while simplifies life
Production. art, save production cost.
The preferred embodiment of the present invention described in detail above, still, the present invention are not limited in above-mentioned embodiment
Detail, in the range of the technology design of the present invention, a variety of simple variants can be carried out to technical scheme, this
A little simple variants belong to protection scope of the present invention.
It is further to note that each particular technique feature described in above-mentioned embodiment, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should equally be considered as content disclosed in this invention.
Claims (8)
1. a kind of Low Temperature Hot Rolling plate prepares the production method of Thin Specs high magnetic induction grain-oriented silicon steel, it is characterised in that this method includes：
S1, by the hot rolling of silicon steel strand it is hot rolled plate；
S2, normalizing heat treatment is carried out to the hot rolled plate；
S3, normalizing is heat-treated after the hot rolled plate cold rolling be cold-reduced sheet；
S4, decarburizing annealing processing is carried out to the cold-reduced sheet；
S5, the cold rolling plate surface coat MgO coatings；
S6, the high temperature anneal is carried out to the cold-reduced sheet for coating MgO coatings,
Wherein, S6 steps include：
The cold-reduced sheet is inserted in Equipment for Heating Processing and heated up with the first heating rate, is started when temperature reaches 850-870 DEG C
NH is passed through into the Equipment for Heating Processing3, stop being passed through NH when temperature reaches the first temperature3, then with the second heating rate liter
Temperature is to second temperature and is incubated；
Wherein, in step sl, by the silicon steel heating strand to carrying out hot rolling after 1000-1200 DEG C；Also, pass through 7-9
Thickness is that the 300-330mm silicon steel strand finish to gauge is the hot rolled plate that thickness is 2.2-2.4mm by hot rolling pass, wherein, often
The reduction ratio of individual hot rolling pass is 30%-60%；
Wherein, in step s3, it is that thickness is the cold of 0.16-0.18mm by the hot rolled plate finish to gauge by 6-8 cold rolling pass
Plate is rolled, wherein, the reduction ratio of each cold rolling pass is 20%-40%, also, aging strengthening model is carried out between cold rolling pass：Will
The hot rolled plate is inserted in Equipment for Heating Processing, and 5-10min is incubated at 240-250 DEG C；
Wherein, the mass percent of the chemical composition of the silicon steel strand is：Si：2.6~3.45%, C：0.050~
0.080%, Mn：0.08~0.12%, S：0.005~0.007%, Cr：0.08~0.12%, Cu：0.006~0.012%,
Al：0.02~0.03%, N：0.0050~0.008%, Sn：0.04~0.06%, surplus Fe.
2. according to the method for claim 1, it is characterised in that in step s 6, first temperature is 880-900 DEG C,
The second temperature is 1180-1200 DEG C, and soaking time of the cold-reduced sheet under the second temperature is 15-20h.
3. according to the method for claim 1, it is characterised in that in step s 6, first heating rate is 8-10K/
S, second heating rate are 18-20K/s.
4. according to the method for claim 1, it is characterised in that in step s 6, be passed through NH3Speed be 1-2L/min.
5. according to the method for claim 1, it is characterised in that in step s 6, the atmosphere of the insulation is pure hydrogen atmosphere.
6. according to the method for claim 1, it is characterised in that two-part normalizing heat treatment is carried out in step s 2, wherein,
Step S2 includes：
S2-1, the hot rolled plate is incubated 150-160s at 1050 DEG C~1100 DEG C；
S2-2, by the hot rolled plate air cooling to 900-950 DEG C and it is incubated 90-100s；
S2-3, by the hot rolled plate air cooling to 800-820 DEG C, be subsequently placed in 90-100 DEG C of water and cool down.
7. according to the method for claim 1, it is characterised in that in step s3, the hot rolled plate is entered before cold rolling
Row pickling processes.
8. according to the method for claim 1, it is characterised in that in step s 4, the cold-reduced sheet is inserted into heat treatment and set
In standby, 3-4min is incubated at 850-900 DEG C, while be 4-5 by the volume ratio of nitrogen and hydrogen：3 mixed gas is in 80-85
DEG C water in soak after be passed through in the Equipment for Heating Processing and carry out carbonization treatment.
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