CN110283981B - Production method capable of increasing oxygen content of low-temperature high-magnetic-induction oriented silicon steel - Google Patents
Production method capable of increasing oxygen content of low-temperature high-magnetic-induction oriented silicon steel Download PDFInfo
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Abstract
A production method capable of improving the oxygen content of low-temperature high-magnetic induction oriented silicon steel comprises the following steps: smelting in a conventional converter, carrying out vacuum treatment and continuously casting to form a blank; conventionally heating a casting blank; carrying out one-time cold rolling after acid pickling; annealing; annealing at high temperature; stretching and flattening, coating an insulating coating and finishing and packaging a finished product for later use. The invention can at least improve the oxygen content of the HiB at low temperature to be not less than 680PPm under the premise that the nitriding amount is not less than 200PPm without changing the prior production process, steel type components and nitriding time conditions in the decarburization annealing process, thereby improving the magnetic property to be not less than 1.91T from the prior 1.905T, and the invention has simple operation and is easy to implement.
Description
Technical Field
The invention relates to a production method of oriented silicon steel, in particular to a production method of high magnetic induction nitriding oriented silicon steel, and particularly relates to a production method for improving the oxygen content of low-temperature high magnetic induction oriented silicon steel.
Background
With the development trend of national power grid business, ultrahigh-pressure type and energy-saving and consumption-reducing type transformers above S13 type level become mainstream, so that the application range of low-temperature high-magnetic-induction oriented silicon steel (low-temperature HiB) and the magnetic requirements of the market on the low-temperature high-magnetic-induction oriented silicon steel are higher. Since the low temperature HiB is inhibited by means of the after-nitriding, the key process to improve the magnetic properties is its nitriding and oxidation during the primary annealing after cold rolling. How to increase the oxygen content of HiB at low temperature within the range of specific nitriding amount is the key to solve the problem of improving the magnetic performance. And are also problems faced by those skilled in the art.
At present, the following methods are mainly used for improving the low-temperature HiB oxygen content and obtaining the nitriding quantity more than or equal to 200 ppm:
1. the nitriding efficiency is improved and the nitriding amount is increased in unit time by changing the nitriding temperature;
2. different nitriding modes, such as a spraying mode, are changed, the nitriding efficiency is improved in unit time, and the nitriding amount is increased;
3. the oxygen content in the steel is increased by changing the content of the oxygen-philic components such as Cr and Sn elements in the steel so that the oxygen-philic components are more easily oxidized in the decarburization annealing.
Of the above three ways, from the result of production practice, the first and third ways need great changes to the low-temperature HiB component design and the primary annealing process, which is relatively high in failure risk for mature production enterprises.
The second mode needs hard fixed asset investment, equipment transformation and the like, can only solve the problem that the nitriding quantity of the HiB is more than or equal to 200ppm at low temperature, and cannot solve the problem of increasing the oxygen content.
The prior art generally introduces a lot of methods for obtaining more than or equal to 200ppm of low-temperature HiB, but in practice, under the condition that the nitriding amount is more than or equal to 200ppm, the oxygen content must be concerned to obtain the low-temperature HiB steel with excellent magnetism. The magnetic induction of the low-temperature HiB steel is increased along with the increase of the oxygen content, the main principle is that the oxygen content is increased, the bottom layer of the low-temperature HiB steel is completely formed, the nitriding amount is more than or equal to 200ppm, nitride inclusions are favorably formed, and the texture development of Gaussian components is more perfect, so that the magnetic induction is improved. The invention aims to obtain the nitriding quantity of more than or equal to 200ppm and improve the oxygen content so as to improve the magnetism of the low-temperature HiB steel.
In the prior art, attention is paid to the oxygen content of the high-magnetic-induction silicon steel, but the nitriding amount and the oxygen content are low, and if the contents are searched:
chinese patent application No. CN201110415831.1 discloses "a method for nitriding high magnetic induction grain-oriented silicon steel strip". The document introduces a nitriding method of high magnetic induction grain-oriented silicon steel, but according to the document, the nitriding amount can only be maintained between 120ppm and 180 ppm; the oxygen content is maintained at 400 ppm-450 ppm, and the capability of improving the HiB magnetism at low temperature is limited. Because the nitrogen content of the patent does not reach the range of more than or equal to 200ppm, the nitride inclusion components are less, the effective inhibition force is insufficient, the Gaussian component texture is incompletely developed, and the magnetic induction is difficult to improve.
Most of the methods for improving the performance of the high-magnetic-induction silicon steel still improve the magnetic performance of the high-magnetic-induction silicon steel by improving the nitriding amount of the steel, and the oxygen content of the steel is not concerned, such as searched:
the Chinese patent application No. CN201310348135.2 discloses a method for nitriding oriented silicon steel by using a nano composite electrodeposition technology, and the document can obviously improve the low-temperature HiB nitriding amount to 220 ppm-260 ppm. In the document, only attention is paid to increase of nitriding amount, namely, although nitriding amount reaches 220ppm to 260ppm, the increase of oxygen content is not paid attention to, the oxygen content obtained in the patent is 250ppm to 450ppm, and the low-temperature HiB steel bottom layer is not compact under the condition that the nitriding amount is not less than 200ppm due to insufficient oxygen content, even if the nitriding amount is very high, nitrogen overflows to the surface of a steel strip through a gap of the compact bottom layer in the formation process of nitride inclusions, so that the development of Gaussian component texture in the steel strip is incomplete, and the requirement of further improving the magnetic performance of the high-magnetic-strength silicon steel cannot be met.
Chinese patent application No. CN201420326832.8 discloses "a spray beam for nitriding oriented silicon steel", which requires installation of special equipment to increase investment and production costs, and does not concern about increase of oxygen content even though the nitriding amount reaches 200ppm to 240ppm, and thus cannot satisfy the requirement of further improvement of magnetic performance of high magnetic induction silicon steel.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a production method for improving the oxygen content of the low-temperature HiB to be not less than 680PPm at least and further improving the magnetic performance from the prior 1.905T to be not less than 1.91T on the premise of not changing the prior production process, steel type components and nitriding time condition in the primary annealing process and not lowering the nitriding amount to be not less than 200 PPm.
The measures for the above purposes are as follows:
a production method capable of improving the oxygen content of low-temperature high-magnetic induction oriented silicon steel comprises the following steps:
1) smelting in a conventional converter, carrying out vacuum treatment and carrying out continuous casting to obtain a low-temperature HiB steel billet; the casting blank comprises the following components in percentage by weight: the content of Si is 2.8-3.3%, the content of C is 400-700 ppm, the content of N is 65-85 ppm, the content of Als is 240-305 ppm, and the balance is Fe and other impurity elements.
2) Conventionally heating a casting blank, and performing conventional blooming, finish rolling and coiling to obtain a steel plate with the thickness of 2.3 +/-0.1 mm;
3) carrying out one-time cold rolling after acid pickling;
4) and (3) annealing process:
A. firstly, decarburization annealing is carried out in a mode of combining ascending and descending of the partial pressure ratio in the furnace, the annealing temperature is controlled to be 820-860 ℃, the atmosphere in the furnace is wet nitrogen-hydrogen mixed gas, wherein the volume ratio of hydrogen is 38-45%; the annealing time is 140 s;
during the process: controlling P in the annealing furnace during the first 100s of decarburization annealingH2O/PH2The partial pressure ratio is as follows: adding an increasing voltage division ratio on the basis of the basic voltage division ratio; the basic partial pressure ratio is a value arbitrarily selected from 0.4-0.6; the increasing partial pressure ratio refers to: the partial pressure ratio is increased by 0.05 every 25s of annealing;
in the time period of annealing time being more than 100s to 140s, the partial pressure ratio in the annealing furnace adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing;
B. after the decarburization annealing is finished, entering a nitriding treatment stage, wherein the atmosphere in the annealing furnace is still wet nitrogen-hydrogen mixed gas; nitriding temperature is 850-900 ℃, and nitriding time is conventional 20-45 s; the flow of the introduced ammonia gas is 30-40 m3H; partial pressure ratio P in the furnace during nitriding stageH2O/PH2The pressure-dividing ratio in the furnace is 0.2-0.4, and the pressure-dividing ratio in the furnace is in positive correlation with the nitrogen content set by the steel grade;
5) conventionally carrying out high-temperature annealing;
6) and stretching and flattening, coating an insulating coating and finishing and packaging the finished product for later use.
Preferably: the base partial pressure ratio is any value within 0.07-0.15.
The invention controls P in the annealing furnace within 100s before decarburization annealingH2O/PH2The partial pressure ratio is as follows: adding an increasing voltage division ratio on the basis of the basic voltage division ratio; the basic partial pressure ratio is a value arbitrarily selected from 0.4-0.6; the increasing partial pressure ratio refers to: the partial pressure ratio was increased by 0.05 per 25s of annealing. Is due to the fact that in the fore-stage decarburization annealing, especially in the first 25s, if oxygen of a larger composition is to be obtained, the partial pressure ratio P in the annealing furnace is made higherH2O/PH2Must be controlled above 0.4; the reason why the partial pressure ratio is increased by 0.05 per 25S of annealing is that the P value is maintained after 25S if P is continuously maintained after 25S as decarburization annealing proceedsH2O/PH2Within 0.4, resulting in SiO2The components are abnormally increased and coarsened, and a dense oxide layer is formed on the subsurface layer of the steel strip, which hinders decarburization. The purpose of increasing the partial pressure ratio in a gradient manner is to obtain sufficient SiO2And the decarburization.
When the annealing time is more than 100s to 140s, the partial pressure ratio adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing; the reason is that after the temperature is more than 100s, the decarburization process in the steel strip in the HiB at the low temperature is basically completed for most parts, and in the decarburization process, carbon in the steel strip reacts with steam to produce CO and H2All are reducing atmospheres. When the decarburization period is 100s to 140s, the reducing atmosphere generated by the decarburization is weakened, and the P in the furnace is reduced in a gradient mannerH2O/PH2Can prevent the oxidation of the surface of the strip steel caused by the peroxide atmosphere and the subsequent inhibition of nitriding.
The invention controls the partial pressure ratio in the furnace at the nitriding stage to be PH2O/PH2Any value within the range of 0.2-0.4 is due to the fact that the partial pressure P is properly adopted in the nitriding processH2O/PH2After being mixed with ammonia gas, the moisture and the ammonia gas form a complex of FeO and amino on the surface of the strip steel, thereby effectively promoting nitriding and improving nitriding efficiency.
The invention does not change the prior low-temperature HiB decarburization annealing furnace equipment and process conditionsThe structure of furnace body equipment is changed, the nitriding amount is not less than 200PPm, the oxygen content is increased through process optimization, and the low-temperature HiB magnetism is better. The main principle is as follows: by adjusting the atmosphere P of the primary annealing in different time stagesH2O/PH2Partial pressure ratio such that the oxygen content is high and is a reactant SiO formed in the bottom layer2The components are increased, and further the low-temperature HiB oxygen content is improved. The original dry nitriding environment is changed in the nitriding stage of decarburization annealing to realize PH2O/PH2And nitriding in a low partial pressure ratio and a wet gas environment, so that nitriding efficiency is improved. And ensuring that the nitriding amount is not less than 200PPm under the condition of unchanging the nitriding mode, the nitriding time and the nitriding temperature.
Compared with the prior art, the method can at least improve the oxygen content of the low-temperature HiB to be not less than 680PPm on the premise of not changing the prior production process, steel type components and nitriding time conditions in the decarburization annealing process and not less than 200PPm, further improve the magnetic property from the prior 1.905T to be not less than 1.91T, and is simple to operate and easy to implement.
Detailed Description
The present invention is described in detail below:
example 1
A production method capable of improving the oxygen content of low-temperature high-magnetic induction oriented silicon steel comprises the following steps:
1) smelting in a conventional converter, carrying out vacuum treatment and carrying out continuous casting to obtain a low-temperature HiB steel billet; the casting blank comprises the following components in percentage by weight: the Si content is 2.85 percent, the C content is 421ppm, the N content is 68ppm, the Als content is 260ppm, and the balance is Fe and other impurity elements;
2) conventionally heating a casting blank, and performing conventional blooming, finish rolling and coiling to obtain a steel plate with the thickness of 2.3 +/-0.1 mm;
3) carrying out one-time cold rolling after acid pickling until the thickness is 0.27 mm;
4) and (3) annealing process:
A. firstly, decarburization annealing is carried out in a mode of combining ascending and descending of the partial pressure ratio in the furnace, the annealing temperature is controlled at 835 ℃, the atmosphere in the furnace is wet nitrogen-hydrogen mixed gas, wherein the volume of hydrogen accounts for 39 percent(ii) a The annealing time is 140 s; during the process: the base partial pressure ratio P is selected within an annealing time of 100sH2O/PH20.4 and adopts an incremental mode, namely, the partial pressure ratio is increased by 0.05 every 25s of annealing; the pressure-dividing ratio was 0.6 at 100 s;
during the time period when the annealing time is more than 100s to 140s, the partial pressure ratio adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing; by the end of the decarburization annealing, the partial pressure ratio was 0.56.
B. After the decarburization annealing is finished, entering a nitriding treatment stage, wherein the atmosphere in the annealing furnace is still wet nitrogen-hydrogen mixed gas; the nitriding temperature is 885 ℃, and the nitriding time is conventional 28 s; the flow rate of the introduced ammonia gas is 33m3H; since the N content is set at 68ppm, the partial pressure ratio P in the furnace during the nitriding stageH2O/PH2Is 0.21;
5) conventionally carrying out high-temperature annealing;
6) and stretching and flattening, coating an insulating coating and finishing and packaging the finished product for later use.
Through detection, the oxygen content of the embodiment is 680PPm, which is improved by 36.2 percent compared with the prior conventional technology; the nitriding amount is 200 PPm; the magnetic induction was 1.91T.
Example 2
1) Smelting in a conventional converter, carrying out vacuum treatment and carrying out continuous casting to obtain a low-temperature HiB steel billet; the casting blank comprises the following components in percentage by weight: the Si content is 3.02%, the C content is 550ppm, the N content is 72ppm, the Als content is 275ppm, and the balance is Fe and other impurity elements;
2) conventionally heating a casting blank, and performing conventional blooming, finish rolling and coiling to obtain a steel plate with the thickness of 2.3 +/-0.1 mm;
3) carrying out one-time cold rolling after acid pickling until the thickness is 0.27 mm;
4) and (3) annealing process:
A. firstly, decarburization annealing is carried out according to a mode of combining ascending and descending of the partial pressure ratio in the furnace, the annealing temperature is controlled at 828 ℃, the atmosphere in the furnace is wet nitrogen-hydrogen mixed gas, and the volume ratio of hydrogen is 40%; the annealing time is 140 s;
during the process: the base partial pressure ratio P is selected within an annealing time of 100sH2O/PH20.48 and in an incremental manner, i.e. increasing the partial pressure ratio by 0.05 per 25s of annealing; the pressure-dividing ratio was 0.68 by 100 s;
during the time period when the annealing time is more than 100s to 140s, the partial pressure ratio adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing; by the end of the decarburization annealing, the partial pressure ratio was 0.64.
B. After the decarburization annealing is finished, entering a nitriding treatment stage, wherein the atmosphere in the annealing furnace is still wet nitrogen-hydrogen mixed gas; the nitriding temperature is 875 ℃, and the nitriding time is 29s which is conventional; the flow rate of the introduced ammonia gas is 35m3H; the partial pressure ratio P in the furnace at the nitriding stage is due to the N content set at 72ppmH2O/PH2Is 0.25;
5) conventionally carrying out high-temperature annealing;
6) and stretching and flattening, coating an insulating coating and finishing and packaging the finished product for later use.
Through detection, the oxygen content of the embodiment is 760PPm, which is 51.2% higher than that of the conventional technology; the nitriding amount is 225 PPm; the magnetic induction was 1.911T.
Example 3
1) Smelting in a conventional converter, carrying out vacuum treatment and carrying out continuous casting to obtain a low-temperature HiB steel billet; the casting blank comprises the following components in percentage by weight: the Si content is 3.2 percent, the C content is 624ppm, the N content is 83ppm, the Als content is 298ppm, and the balance is Fe and other impurity elements;
2) conventionally heating a casting blank, and performing conventional blooming, finish rolling and coiling to obtain a steel plate with the thickness of 2.3 +/-0.1 mm;
3) carrying out one-time cold rolling after acid pickling until the thickness is 0.27 mm;
4) and (3) annealing process:
A. firstly, decarburization annealing is carried out according to a mode of combining ascending and descending of the partial pressure ratio in the furnace, the annealing temperature is controlled at 845 ℃, the atmosphere in the furnace is wet nitrogen-hydrogen mixed gas, wherein the volume ratio of hydrogen is 41 percent; the annealing time is 140 s;
during the process: the base partial pressure ratio P is selected within an annealing time of 100sH2O/PH20.58 and in an incremental manner, i.e. increasing the partial pressure ratio by 0.05 per 25s of annealing; to 1The voltage division ratio is 0.78 when the time is 00 s;
during the time period when the annealing time is more than 100s to 140s, the partial pressure ratio adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing; by the end of the decarburization annealing, the partial pressure ratio was 0.74.
B. After the decarburization annealing is finished, entering a nitriding treatment stage, wherein the atmosphere in the annealing furnace is still wet nitrogen-hydrogen mixed gas; the nitriding temperature is 890 ℃, and the nitriding time is conventional 28 s; the flow rate of the introduced ammonia gas is 38m3H; since the N content is 83ppm, the partial pressure ratio P in the furnace during the nitriding stageH2O/PH2Is 0.38;
5) conventionally carrying out high-temperature annealing;
6) and stretching and flattening, coating an insulating coating and finishing and packaging the finished product for later use.
Through detection, the oxygen content of the embodiment is 1050PPm, which is 110% higher than that of the prior conventional technology; the nitriding amount is 245 PPm; the magnetic induction was 1.9113T.
Example 4
1) Smelting in a conventional converter, carrying out vacuum treatment and carrying out continuous casting to obtain a low-temperature HiB steel billet; the casting blank comprises the following components in percentage by weight: the Si content is 3.11 percent, the C content is 606ppm, the N content is 78ppm, the Als content is 289ppm, and the balance is Fe and other impurity elements;
2) conventionally heating a casting blank, and performing conventional blooming, finish rolling and coiling to obtain a steel plate with the thickness of 2.3 +/-0.1 mm;
3) carrying out one-time cold rolling after acid pickling until the thickness is 0.27 mm;
4) and (3) annealing process:
A. firstly, decarburization annealing is carried out in a mode of combining ascending and descending of the partial pressure ratio in the furnace, the annealing temperature is controlled to be 857 ℃, the atmosphere in the furnace is wet nitrogen-hydrogen mixed gas, and the volume ratio of hydrogen is 43 percent; the annealing time is 140 s;
during the process: the base partial pressure ratio P is selected within an annealing time of 100sH2O/PH20.52 and in an incremental manner, i.e. increasing the partial pressure ratio by 0.05 per 25s of annealing; the pressure-dividing ratio was 0.72 by 100 s;
during the time period when the annealing time is more than 100s to 140s, the partial pressure ratio adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing; by the end of the decarburization annealing, the partial pressure ratio was 0.68.
B. After the decarburization annealing is finished, entering a nitriding treatment stage, wherein the atmosphere in the annealing furnace is still wet nitrogen-hydrogen mixed gas; the nitriding temperature is 887 ℃, and the nitriding time is conventional 31 s; the flow rate of the introduced ammonia gas is 13m3H; since the N content is set at 78ppm, the partial pressure ratio P in the furnace during the nitriding stageH2O/PH2Is 0.03;
5) conventionally carrying out high-temperature annealing;
6) and stretching and flattening, coating an insulating coating and finishing and packaging the finished product for later use.
Through detection, the oxygen content of the embodiment is 830PPm, which is 66% higher than that of the prior art; the nitriding amount is 236 PPm; the magnetic induction is 1.912T.
The present embodiments are merely preferred examples, and are not intended to limit the scope of the present invention.
Claims (2)
1. A production method capable of improving the oxygen content of low-temperature high-magnetic induction oriented silicon steel comprises the following steps:
1) smelting in a conventional converter, carrying out vacuum treatment and carrying out continuous casting to obtain a low-temperature HiB steel billet; the casting blank comprises the following components in percentage by weight: the content of Si is 2.8-3.3%, the content of C is 400-700 ppm, the content of N is 65-85 ppm, the content of Als is 240-305 ppm, and the balance is Fe and other impurity elements;
2) conventionally heating a casting blank, and performing conventional blooming, finish rolling and coiling to obtain a steel plate with the thickness of 2.3 +/-0.1 mm;
3) carrying out one-time cold rolling after acid pickling;
4) and (3) annealing process:
A. firstly, decarburization annealing is carried out in a mode of combining ascending and descending of the partial pressure ratio in the furnace, the annealing temperature is controlled to be 820-860 ℃, the atmosphere in the furnace is wet nitrogen-hydrogen mixed gas, and the volume ratio of hydrogen is 38-45%; the annealing time is 140 s;
during the process: controlling P in the annealing furnace during the first 100s of decarburization annealingH2O/PH2The partial pressure ratio is as follows: adding an increasing voltage division ratio on the basis of the basic voltage division ratio; the basic partial pressure ratio is a value arbitrarily selected from 0.4-0.6; the increasing partial pressure ratio refers to: the partial pressure ratio is increased by 0.05 every 25s of annealing;
in the time period of annealing time being more than 100s to 140s, the partial pressure ratio in the annealing furnace adopts a decreasing mode, namely the partial pressure ratio is reduced by 0.01 every 10s of annealing;
B. after the decarburization annealing is finished, entering a nitriding treatment stage, wherein the atmosphere in the annealing furnace is based on wet nitrogen-hydrogen mixed gas and the flow rate is 30-40 m3H ammonia gas; nitriding at 850-900 ℃ for 20-45 s conventionally; partial pressure ratio P in the furnace during nitriding stageH2O/PH2The pressure-dividing ratio in the furnace is 0.2-0.4, and the pressure-dividing ratio in the furnace is in positive correlation with the nitrogen content set by the steel grade;
5) conventionally carrying out high-temperature annealing;
6) and stretching and flattening, coating an insulating coating and finishing and packaging the finished product for later use.
2. The production method capable of increasing the oxygen content of the low-temperature high-magnetic-induction oriented silicon steel as claimed in claim 1, wherein the production method comprises the following steps: the base partial pressure ratio is any value within 0.4-0.58.
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