CN114807512B - Method for refining grain structure of oriented silicon steel through LF refining process - Google Patents

Method for refining grain structure of oriented silicon steel through LF refining process Download PDF

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CN114807512B
CN114807512B CN202210611384.5A CN202210611384A CN114807512B CN 114807512 B CN114807512 B CN 114807512B CN 202210611384 A CN202210611384 A CN 202210611384A CN 114807512 B CN114807512 B CN 114807512B
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refining
silicon steel
oriented silicon
steel
yttrium oxide
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CN114807512A (en
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郭志红
朱立光
郑亚旭
刘鹏鋆
王旗
韩宝臣
鲁素玲
孙会兰
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Hebei University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21CPROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/04Removing impurities by adding a treating agent
    • C21C7/06Deoxidising, e.g. killing
    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21CPROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
    • C21C7/00Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
    • C21C7/0037Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00 by injecting powdered material

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Treatment Of Steel In Its Molten State (AREA)

Abstract

The invention relates to the technical field of electrical steel production, in particular to a method for refining grain structures of oriented silicon steel through an LF refining process, which is characterized in that the temperature and oxygen content of the molten steel are controlled in the LF refining process of the oriented silicon steel, the molten steel state is adjusted to the optimal adding state of nano yttrium oxide crystals, and specific nano yttrium oxide crystals are added into the molten steel, wherein the nano yttrium oxide crystals can be used as heterogeneous nuclei in the molten steel, so that crystal nuclei formed during solidification and crystallization of the molten steel are preferentially adsorbed on the nano yttrium oxide crystals, the nucleation rate is improved, the solidification structures are refined, the grain structure size of the finally prepared oriented silicon steel is reduced by more than 30 percent compared with that of the oriented silicon steel prepared through a common process, and great progress is achieved in magnetic performance and mechanical performance.

Description

Method for refining grain structure of oriented silicon steel through LF refining process
Technical Field
The invention belongs to the technical field of electrical steel production, and particularly relates to a method for refining grain structure of oriented silicon steel through an LF refining process.
Background
The oriented silicon steel is especially small in size and light in weight, is an indispensable material for manufacturing large-scale transformer, generator and motor iron cores, and the demand and performance requirements of the market on the oriented silicon steel are continuously improved along with the great increase of Chinese generated energy and the rising of manufacturing industry in recent years.
The properties of oriented silicon steel are mainly divided into two modes, namely magnetic properties and mechanical properties. The magnetic property and the mechanical property of the oriented silicon steel are important factors for reflecting the quality and the processing property of the oriented silicon steel, and the grain structure size in the oriented silicon steel determines the movement of grain boundaries and the movement of magnetic domains of the grains, so that the magnetic property and the mechanical property of the oriented silicon steel are determined: the larger the grain structure is, the higher the iron loss and eddy current loss of the oriented silicon steel are; the solidification structure in the oriented silicon steel is coarse, deformation is dispersed in fewer crystal grains under the same plastic deformation amount, so that the deformation is uneven, meanwhile, the dislocation density dispersed in each crystal grain is increased, the problem of stress concentration is also caused by the smaller deformation amount during plastic deformation, and the cracking probability is increased, so that the grain refinement of the oriented silicon steel is always the focus of research of metallurgical workers.
Disclosure of Invention
Aiming at the technical problems of high iron loss, weak magnetic induction and poor mechanical and processing properties of the oriented silicon steel caused by large grain size in the prior art, the invention provides a method for refining the grain structure of the oriented silicon steel by an LF refining process, which can effectively reduce the grain structure in the oriented silicon steel, improve the hardness and the yield strength, reduce the abnormal loss and the eddy current loss and improve the magnetic property and the mechanical property of the oriented silicon steel.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
on one hand, the embodiment of the invention provides a method for refining grain structure of oriented silicon steel by an LF refining process, which comprises the following steps of:
s1: transferring the silicon steel liquid smelted by the converter into an LF refining furnace, adding slag charge required by refining, and heating to enable the temperature of the molten steel to be 1620-1630 ℃;
s2: adding deoxidizer into molten steel, heating to 1640-1650 ℃, and adjusting the content of dissolved oxygen in the molten steel to be less than or equal to 10 multiplied by 10 -6 Continuing smelting until the molten steel components meet the requirements of target silicon steel;
s3: adding nanometer yttrium oxide (Y) into the molten steel obtained in S2 2 O 3 ) And (3) uniformly dispersing the crystals, continuing smelting until the LF refining end temperature is 1620-1630 ℃, and finishing LF refining.
Compared with the prior art, according to the method for refining the grain structure of the oriented silicon steel through the LF refining process, nanometer yttrium oxide crystals are added into the molten steel in the LF refining process of the molten steel, the nanometer yttrium oxide crystals belong to heterogeneous nucleation in the molten silicon steel, and the molten silicon steel belongs to homogeneous nucleation, when the molten silicon steel is solidified and crystallized, the nucleation work of the heterogeneous nucleation is smaller than that of the homogeneous nucleation, so that the crystal nuclei can be preferentially adsorbed on the heterogeneous nucleation, and the effects of improving the nucleation rate and refining the solidification structure are achieved. The control of temperature and the adjustment of the content of dissolved oxygen in silicon steel liquid in the LF refining process can lead the state of the silicon steel liquid to reach the optimal state of adding nano yttrium oxide crystals, thereby avoiding the nano yttrium oxide crystals from entering slag after being added, and leading the nano yttrium oxide crystals to be uniformly dispersed in the silicon steel liquid and furthest playing the effect of refining grains. Compared with the traditional smelting process, the method for refining grain structure of the oriented silicon steel can reduce the grain size in the oriented silicon steel by more than 30 percent, and can effectively improve the magnetic property and mechanical property of the oriented silicon steel.
Preferably, the particle size of the nano yttrium oxide crystals is 50-200 nm.
Preferably, the addition amount of the nanometer yttrium oxide crystal is 0.2-1 kg/ton of molten silicon steel.
Preferably, the nano yttrium oxide crystals are added in a manner of iron foil wrapping or immersion blowing.
The preferable adding mode can avoid the direct contact of the nano yttrium oxide crystals with the molten steel in the adding process, avoid the loss in the adding process, ensure the distribution state of the nano yttrium oxide crystals in the molten steel, and further improve the technical effect of refining the grain structure of the oriented silicon steel by the nano yttrium oxide crystals.
And preferably, after the slag charge is added in the S1, controlling the flow rate of bottom blowing gas in the LF refining furnace to be 5-15 NL/(min per ton of molten silicon steel).
The preferential bottom blowing gas flow after the slag charge is added can avoid the bottom blowing gas to take away excessive heat in the molten steel, thereby ensuring the temperature uniformity of each part in the molten steel while rapidly heating the molten steel and achieving the effect of rapid slag melting.
And preferably, after the deoxidizer in the S2 is added, controlling the flow rate of bottom blowing gas in the LF refining furnace to be 20-40 NL/(min.ton of molten silicon steel).
Preferably, after the nano yttrium oxide crystal is added in the S3, controlling the flow rate of bottom blowing gas in the LF refining furnace to be 5-10 NL/(min.ton of molten silicon steel).
The flow of the bottom blowing gas is optimized after the nano yttrium oxide crystals are added, so that the nano yttrium oxide crystals can be rapidly and uniformly distributed in molten steel, meanwhile, the loss of the nano yttrium oxide crystals in the dispersing process is avoided, and the effect of refining crystal grains of the nano yttrium oxide crystals is exerted to the greatest extent.
Preferably, the deoxidizer in S3 is aluminum particles.
Preferably, the method further comprises the process of preparing the oriented silicon steel sheet billet from the LF refined silicon steel liquid through continuous casting, hot rolling, normalizing, cold rolling and annealing.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The invention is further illustrated below in the form of a number of examples.
Example 1
The embodiment provides a method for refining grain structure of oriented silicon steel through an LF refining process, which specifically comprises the following steps:
s1: after 100 tons of silicon steel liquid smelted by a converter enters an LF refining furnace, detecting the temperature of the molten steel to 1578 ℃, adding slag charge required by refining when the content of dissolved oxygen in the molten steel is 318ppm, lowering an electrode into slag for submerged arc heating, and refining to the temperature of 1625+/-5 ℃ when the flow rate of bottom blowing argon is 12 NL/(min ton of silicon steel liquid);
s2: the flow rate of the bottom blowing gas is regulated to 30 NL/(min per ton of silicon steel liquid), aluminum particles are added for further deoxidization, so that the content of dissolved oxygen in the molten steel is less than or equal to 10ppm, and after the temperature of the molten steel is 1645+/-5 ℃, smelting is continued until the molten steel components reach the target oriented silicon steel standard;
s3: 30kg of nano Y with the particle size range of 50-200 nm and the average particle size of 168nm 2 O 3 Adding the crystal into molten steel under the wrapping of iron foil, adjusting the flow rate of bottom blowing gas to 8 NL/(min.ton of silicon steel liquid), and continuing smelting until the temperature of the molten steel is reduced to 1625+/-5 DEG CCompleting an LF refining task;
s4: and carrying out continuous casting, hot rolling, normalizing, cold rolling, annealing and other working procedures on the molten steel subjected to LF refining to obtain the oriented silicon steel plate blank.
Example 2
The embodiment provides a method for refining grain structure of oriented silicon steel through an LF refining process, which specifically comprises the following steps:
s1: after 210 tons of silicon steel liquid smelted by a converter enters an LF refining furnace, detecting the temperature of the molten steel to 1569 ℃, adding slag charge required by refining when the content of dissolved oxygen in the molten steel is 342ppm, lowering an electrode into slag for submerged arc heating, and refining to 1625+/-5 ℃ when the flow rate of bottom blowing argon is 12 NL/(min ton of silicon steel liquid);
s2: the flow rate of the bottom blowing gas is regulated to 30 NL/(min per ton of silicon steel liquid), aluminum particles are added for further deoxidization, so that the content of dissolved oxygen in the molten steel is less than or equal to 9ppm, and after the temperature of the molten steel is 1645+/-5 ℃, smelting is continued until the molten steel components reach the target oriented silicon steel standard;
s3: 63kg of nano Y with the particle size range of 50-200 nm and the average particle size of 168nm 2 O 3 The crystal is added into molten steel under the wrapping of iron foil, and nano Y 2 O 3 The adding amount of the crystal is 63kg, the flow rate of bottom blowing gas is adjusted to 8 NL/(min.t), smelting is continued until the temperature of molten steel is reduced to 1625+/-5 ℃, and LF refining is completed;
s4: and carrying out continuous casting, hot rolling, normalizing, cold rolling, annealing and other working procedures on the molten steel subjected to LF refining to obtain the oriented silicon steel plate blank.
Comparative example 1
This comparative example provides a method for LF refining of oriented molten silicon steel, which is compared with example 1 except that nano Y is not added during LF refining 2 O 3 The remaining materials, process parameters and treatment process outside the crystal were identical to those of example 1.
Comparative example 2
This comparative example provides a method for LF refining of an oriented molten silicon steel, which is compared with example 1 except that Y of equal mass and large particles are added during LF refining 2 O 3 Crystals (average particle size 7mm, particle size range)3-10 mm), the remaining materials, process parameters and treatment process were identical to those of example 1.
Comparative example 3
This comparative example provides a method of LF refining of oriented molten silicon steel, which is compared with example 2 except that nano Y is not added during LF refining 2 O 3 The remaining materials, process parameters and treatment process outside the crystal were identical to those of example 2.
Comparative example 4
This comparative example provides a method for LF refining of an oriented molten silicon steel, which is compared with example 2 except that Y of equal mass and large particles are added during LF refining 2 O 3 The remaining materials, process parameters and treatment process were identical to those of example 2, except for the crystals (average particle size 7mm, particle size 3-10 mm).
Test case
(1) The chemical components of the slabs prepared in example 1 and comparative examples 1 to 2 were detected, and the crystal grains in the slabs prepared in example 1 and comparative examples 1 to 2 were observed by a metallographic microscope, and metallographic microscopic pictures were processed by image pl software to obtain average sizes of the crystal grains, and the results are shown in table 1:
(2) Detecting chemical components of the oriented silicon steel slabs prepared in the example 2 and the comparative examples 3-4, observing crystal grains in the slabs prepared in the example 2 and the comparative examples 3-4 through a metallographic microscope, and processing metallographic microscopic pictures through image pl software to obtain average sizes of the crystal grains; the results are shown in Table 2.
TABLE 1
Respectively, into separate parts Si(%) Y(%) C (%) S (%) T. [O](%) N(%) P (%) Fe Average grain size (μm)
Example 1 3.0 0.015 0.0048 0.0038 0.0017 0.0044 0.0078 Allowance of 151
Comparative example 1 3.0 0 0.0046 0.0036 0.0016 0.0043 0.0076 Allowance of 236
Comparative example 2 2.9 0.015 0.0046 0.0035 0.0015 0.0042 0.0075 Allowance of 201
TABLE 2
Respectively, into separate parts Si(%) Y(%) C (%) S (%) T. [O](%) N(%) P (%) Fe Average grain size (μm)
Example 2 6.5 0.016 0.0042 0.0031 0.0016 0.0042 0.0071 Allowance of 169
Comparative example 3 6.3 0 0.0041 0.0033 0.0018 0.0041 0.0073 Allowance of 245
Comparative example 4 6.4 0.015 0.0044 0.0032 0.0017 0.0044 0.0074 Allowance of 216
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the particular embodiments disclosed, but on the contrary, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.

Claims (8)

1. A method for refining grain structure of oriented silicon steel by LF refining technology is characterized in that nanometer yttrium oxide crystals are added in the LF refining process of molten steel, and the method specifically comprises the following steps:
s1: transferring the silicon steel liquid smelted by the converter into an LF refining furnace, adding slag charge required by refining, and heating to enable the temperature of the molten steel to be 1620-1630 ℃;
s2: adding a deoxidizer into the molten steel, heating to 1640-1650 ℃, and adjusting the content of dissolved oxygen in the molten steel to be less than or equal to 10ppm, and continuing smelting until the components of the molten steel meet the requirements of target silicon steel;
s3: and adding nano yttrium oxide crystals into the molten steel and uniformly dispersing the nano yttrium oxide crystals, wherein the addition amount of the nano yttrium oxide crystals is 0.2-1 kg/ton of molten silicon steel, and continuing smelting until the LF refining endpoint temperature is 1620-1630 ℃, thereby finishing LF refining.
2. The method for refining grain structure of oriented silicon steel by an LF refining process as claimed in claim 1, wherein the grain size of the nano yttrium oxide crystals ranges from 50 nm to 200nm.
3. The method for refining grain structure of oriented silicon steel by LF refining process according to claim 1, wherein the nano yttrium oxide crystals are added in the form of iron foil wrapping or immersed blowing.
4. The method for refining grain structure of oriented silicon steel through an LF refining process according to claim 1, wherein after slag is added in S1, the flow rate of bottom blowing gas in an LF refining furnace is controlled to be 5-15 NL/(min ton of molten silicon steel).
5. The method for refining grain structure of oriented silicon steel by an LF refining process according to claim 1, wherein after the deoxidizer is added in S2, the flow rate of bottom blowing gas in the LF refining furnace is controlled to be 20-40 NL/(min.ton of molten silicon steel).
6. The method for refining grain structure of oriented silicon steel by an LF refining process according to claim 1, wherein after adding nano yttrium oxide crystals in S3, the flow rate of bottom blowing gas in the LF refining furnace is controlled to be 5-10 NL/(min.ton of molten silicon steel).
7. The method for refining grain structure of oriented silicon steel by LF refining process as claimed in claim 1, wherein the deoxidizer in S3 is aluminum grain.
8. The method for refining grain structure of oriented silicon steel by LF refining process according to claim 1, further comprising subjecting the LF refined molten steel to continuous casting, hot rolling, normalizing, cold rolling, annealing to obtain an oriented silicon steel sheet billet.
CN202210611384.5A 2022-06-01 2022-06-01 Method for refining grain structure of oriented silicon steel through LF refining process Active CN114807512B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001234227A (en) * 2000-02-21 2001-08-28 Kawasaki Steel Corp Secondary refining method for high-chromium molten steel
CN103397266A (en) * 2013-08-15 2013-11-20 上海卓然工程技术有限公司 Heat-resisting steel and preparation method thereof
CN110791613A (en) * 2019-09-30 2020-02-14 鞍钢股份有限公司 Method for adding nano particles into steel, refining structure of nano particles and strengthening and toughening steel

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001234227A (en) * 2000-02-21 2001-08-28 Kawasaki Steel Corp Secondary refining method for high-chromium molten steel
CN103397266A (en) * 2013-08-15 2013-11-20 上海卓然工程技术有限公司 Heat-resisting steel and preparation method thereof
CN110791613A (en) * 2019-09-30 2020-02-14 鞍钢股份有限公司 Method for adding nano particles into steel, refining structure of nano particles and strengthening and toughening steel

Non-Patent Citations (1)

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Title
普碳钢中添加ZrO2纳米粒子对其组织和力学性能的影响;安静;中国优秀硕士学位论文全文数据库(工程科技I辑)(第6期);第B020-199页 *

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