CN115747664B - Strong magnetic induction nanocrystalline high silicon steel wire and preparation method thereof - Google Patents
Strong magnetic induction nanocrystalline high silicon steel wire and preparation method thereof Download PDFInfo
- Publication number
- CN115747664B CN115747664B CN202211574788.8A CN202211574788A CN115747664B CN 115747664 B CN115747664 B CN 115747664B CN 202211574788 A CN202211574788 A CN 202211574788A CN 115747664 B CN115747664 B CN 115747664B
- Authority
- CN
- China
- Prior art keywords
- silicon steel
- high silicon
- magnetic induction
- steel wire
- nanocrystalline
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 150
- 230000006698 induction Effects 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000003723 Smelting Methods 0.000 claims abstract description 35
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005098 hot rolling Methods 0.000 claims abstract description 21
- 238000002074 melt spinning Methods 0.000 claims abstract description 17
- 229910052742 iron Inorganic materials 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims description 42
- 239000000956 alloy Substances 0.000 claims description 42
- 239000002245 particle Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 238000000498 ball milling Methods 0.000 claims description 16
- 239000010949 copper Substances 0.000 claims description 13
- 238000000713 high-energy ball milling Methods 0.000 claims description 12
- 238000009768 microwave sintering Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 229910052796 boron Inorganic materials 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 238000005280 amorphization Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000000465 moulding Methods 0.000 claims description 7
- 229910052698 phosphorus Inorganic materials 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims 1
- 229920006395 saturated elastomer Polymers 0.000 abstract description 2
- 238000007731 hot pressing Methods 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 7
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005491 wire drawing Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to the technical field of preparation of high silicon steel, and particularly discloses a strong magnetic induction nanocrystalline high silicon steel wire and a preparation method thereof. The preparation method of the strong magnetic induction nanocrystalline high silicon steel wire comprises smelting, preparing a high silicon steel thin strip by high vacuum melt-spinning, amorphizing, microwave hot-press forming, three hot-rolling and hot-drawing. The grain size of the strong magnetic induction nanocrystalline high silicon steel wire prepared by the preparation method of the strong magnetic induction nanocrystalline high silicon steel wire is between 500 and 800nm, the structure is uniform, the room temperature stretching elongation can reach 10.50 percent, the saturated magnetic induction intensity Ms reaches 2.01T, the coercive force Hc reaches 15.8A/m, and the iron loss P is 15.8A/m 1.0/400 The minimum value is 7.9W/kg, and the product has good comprehensive performance.
Description
Technical Field
The invention relates to the technical field of high silicon steel preparation, in particular to a strong magnetic induction nanocrystalline high silicon steel wire and a preparation method thereof.
Background
High silicon steel with a silicon content of approximately 6.5wt% is an advanced crystalline soft magnetic material suitable for motors, transformers and inductors in the medium and high frequency range. Compared with the current widely used Fe-3.2wt% Si electrical steel, the resistivity of Fe-6.5wt% Si is improved by 54%, reaching 83 mu omega cm. This increase in resistivity reduces eddy current losses, making Fe-6.5wt% Si particularly suitable for higher frequency applications. In addition to lower eddy current losses, fe-6.5wt% Si also has high permeability and near zero magnetostriction, thereby minimizing operating noise while reducing hysteresis losses. However, increasing the silicon content also leads to B2 and DO 3 The formation of ordered phases, and therefore conventional high silicon steel manufacturing processes tend to result in brittle fracture.
The rapid solidification technology can effectively inhibit the generation of ordered phases in the high silicon steel, improve the plasticity and greatly improve the mechanical properties of the high silicon steel. However, the problems of difficult control of solidification structure, low yield, difficult control of grain size and high iron loss still exist in the industrial production process of the high-silicon steel thin strip, and the use requirement of the high-silicon steel is difficult to meet.
Disclosure of Invention
Aiming at the problems of the existing Fe-6.5wt% Si high silicon steel, the invention provides a strong magnetic induction nanocrystalline high silicon steel wire and a preparation method thereof.
In order to achieve the above purpose, the embodiment of the invention adopts the following technical scheme:
the preparation method of the strong magnetic induction nanocrystalline high silicon steel comprises the following steps:
a. smelting high silicon steel alloy: the high silicon steel comprises the following chemical components in percentage by mass: c:0.0040% -0.0055%, si:6.1 to 6.9 percent of Mn:0.16% -0.24%, S:0.02% -0.04%, ce:0.02% -0.05%, B:0.04% -0.08%, P: < 0.004%, al:0.029% -0.037%, N:0.012 to 0.015 percent and the balance of Fe; the alloy elements Ce and B are added after mother alloy is smelted for 1-4 times, wherein the B element is added in the form of ferroboron-iron-base coordination compound, and AlN ceramic grains are added according to the proportion of Al and N;
b. preparing the high silicon steel alloy into a high silicon steel thin strip by adopting a high vacuum single-roller strip casting machine;
c. amorphization treatment: performing amorphization treatment on the high silicon steel ribbon by ball milling, and adding nano Cu particles accounting for 3-5wt% of the high silicon steel ribbon in the ball milling process to prepare high silicon steel powder with the average particle size of 200-300 nm;
d. and carrying out microwave hot-press molding and microwave sintering on the high-silicon steel powder to obtain a high-silicon steel bar, and carrying out large plastic deformation hot rolling and hot drawing treatment on the high-silicon steel bar to obtain the strong magnetic induction nanocrystalline high-silicon steel wire with the diameter of 0.8-1.4 mm.
Cerium is added to improve the ductility of the high silicon steel alloy, boron element can improve the fluidity of the remelted alloy, and the addition of cerium element and boron element can further improve the plasticity and the yield of the soft magnetic high silicon steel ultrathin strip. The AlN nano ceramic particles are added, so that the high silicon steel alloy is adhered to the AlN nano ceramic particles in the microwave sintering process to form nuclei again, the crystallinity of the nano crystal is improved, more uniform and fine crystal grains are obtained, and a good tissue foundation is provided for improving the magnetism and plasticity of the high silicon steel wire.
The rapid solidification technology can effectively inhibit ordered phases B2 and DO 3 By suppressing the generation of disordered to ordered phases B2 and DO 3 The transformation of the (C) can effectively solve the brittleness problem of the high silicon steel, and the mechanical property of the high silicon steel is improved on the basis of phase transformation.
The high silicon steel powder can be ensured to be heated uniformly in the compression molding process through microwave heating compression molding. The nano Cu particles fully fill the gaps of the high silicon steel powder in the microwave hot pressing process, so that the compactness and wire drawing performance of a hot pressed sample are greatly improved;
in the step a, the specific smelting steps of the high silicon steel alloy are as follows:
a1, according toThe high silicon steel chemical components except the alloy elements Ce, B, al and N are fed into a vacuum smelting furnace, wherein the vacuum degree of the vacuum smelting furnace is controlled to be 6.0x10 -4 Under Pa, then injecting high-purity Ar to keep the vacuum degree of a vacuum smelting furnace at-0.07 to-0.04 MPa, repeatedly smelting the melted master alloy at 1450-1550 ℃ for 1-4 times, and then preserving the heat for 4-6 minutes;
a2, cooling to 1400-1450 ℃, adding the rare earth cerium and the ferroboron-iron-based coordination compound, repeatedly smelting for 2-4 times, and preserving heat for 3-5 minutes;
a3, cooling to 1350-1400 ℃, adding AlN nano ceramic particles, and repeatedly smelting for 2-3 times to obtain the high silicon steel alloy.
The staged smelting can improve the yield of rare earth cerium element and AlN nano ceramic particles on one hand and ensure the uniform smelting of each element in the master alloy on the other hand.
Preferably, in the step b, the linear speed of the copper roller surface of the high-vacuum single-roller melt-spinning machine is controlled between 30m/s and 40m/s, and the melt-spinning chamber is kept at 1 multiplied by 10 -4 ～6×10 -4 The thickness of the prepared high silicon steel thin strip is 20-45 um.
Preferably, in the step c, a high-energy ball mill is adopted for ball milling, the rotating speed of the high-energy ball mill is controlled to be 600-1000 rpm/min, and the ball milling is carried out for 70-100min.
More preferably, in the step c, the high-energy ball milling is performed in two stages, wherein the rotating speed of the high-energy ball milling in the first stage is controlled to be 800-1000 rpm/min, the ball milling is performed for 20-40min, nano Cu particles are added in the process of the high-energy ball milling in the first stage, the rotating speed of the high-energy ball milling in the second stage is controlled to be 600-800 rpm/min, and the ball milling is performed for 40-80min.
The amorphization treatment of the high silicon steel thin strip can be more sufficient by staged high energy ball milling.
Preferably, in the step d, the temperature of the microwave hot press molding is 800-900 ℃ and the pressure is 40-50 Mpa.
Preferably, the sintering temperature of the microwave sintering is 950-1150 ℃ and the sintering time is 20-25 min.
The high-silicon steel bar is uniformly heated inside and outside to be re-nucleated through high-temperature microwave sintering treatment, so that uniform nanocrystalline tissues are obtained, and the plasticity of the high-silicon steel bar is greatly improved.
Preferably, the hot rolling of large plastic deformation comprises the following specific steps: three times of hot rolling are carried out at 850-1050 ℃, the reduction of each time is 35-40%, and vacuum annealing is carried out for 3-5 min at 950-1200 ℃ after each time of hot rolling.
Preferably, the hot drawing wire treatment comprises the following specific steps: and (3) drawing the high-silicon steel wire rod for 20-25 times by adopting a horizontal drawing machine at the temperature of 850-950 ℃, wherein the deformation of each pass is 5-8%.
The strong magnetic induction nanocrystalline high silicon steel wire prepared by the preparation method provided by the invention has high yield, uniform grain size, good plasticity and low iron loss, and the average grain size of the strong magnetic induction nanocrystalline high silicon steel wire is 500-800nm, the maximum room temperature stretching elongation of the strong magnetic induction nanocrystalline high silicon steel wire can reach 10.50%, the saturated magnetic induction intensity Ms reaches 2.01T, the maximum coercivity Hc reaches 15.8A/m, and the iron loss P is seen from figure 2 1.0/400 The minimum value is 7.9W/kg, and the product has good comprehensive performance.
Drawings
FIG. 1 is a microstructure of a high silicon steel strip produced in example 1 of the present invention
FIG. 2 is a microstructure of a strong magnetic induction nanocrystalline high silicon steel wire produced in example 1 of the present invention
FIG. 3 is a drawing showing a tensile test of a strong magnetic induction nanocrystalline high silicon steel wire produced in example 1 of the present invention
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.
Example 1
A preparation method of a strong magnetic induction nanocrystalline high silicon steel wire comprises the following steps:
the high silicon steel alloy comprises the following components in percentage by mass:
c:0.0040% -0.0055%, si:6.1 to 6.9 percent of Mn:0.16% -0.24%, S:0.02% -0.04%, ce:0.02% -0.05%, B:0.04% -0.08%, P: < 0.004%, al:0.029% -0.037%, N:0.012 to 0.015 percent and the balance of Fe;
a. smelting a high silicon steel alloy: c, si, mn, S, fe is added into a high-vacuum arc melting furnace according to the proportion of the high-silicon steel alloy, and the vacuum degree of a melting chamber is controlled to be 6.0x10 -4 And (3) injecting high-purity Ar below Pa to keep the vacuum degree of a smelting chamber at-0.07 to-0.04 MPa, repeatedly smelting at 1500 ℃ for 2 times, then preserving heat for 6 minutes, and adding AlN ceramic particles and a ferroboron-stacked coordination compound according to the proportion of Al, N and B in the high-silicon steel alloy, and smelting for 3 times to obtain the high-silicon steel alloy.
b. Preparing a high silicon steel thin strip by high vacuum single-roller melt spinning: the high vacuum single-roller melt-spinning machine is adopted, the surface linear speed of copper rollers of the high vacuum high-speed single-roller melt-spinning machine is controlled at 45m/s, and the melt-spinning chamber is kept at 6 multiplied by 10 -4 And (3) preparing the high-silicon steel alloy into a high-silicon steel thin strip with the thickness of 35m, uniform structure and good plasticity by high vacuum degree of Pa.
c. Amorphization treatment: amorphizing the high-silicon steel thin strip by a high-energy ball mill at the speed of 600rpm/min for 100min, and adding nano Cu particles accounting for 4wt% of the high-silicon steel thin strip in the high-energy ball milling process to prepare the high-silicon steel powder with the average particle diameter of 250 nm.
d. Microwave hot press molding: and carrying out microwave hot pressing on the high-silicon steel powder, wherein the microwave heating temperature is 800 ℃, and the microwave hot pressing pressure is 50Mpa, so that the high-silicon steel bar with the diameter of 45mm is prepared.
e. And (3) microwave sintering: and (3) carrying out microwave sintering on the high silicon steel bar at the sintering temperature of 930 ℃ for 25min to obtain the nanocrystalline high silicon steel bar.
f. Large plastic deformation hot rolling: and carrying out large plastic deformation hot rolling on the nanocrystalline high silicon steel bar, carrying out three times of hot rolling at 830 ℃, wherein the rolling reduction is 40% each time, and carrying out vacuum annealing at 930 ℃ for 5min after each time of hot rolling to obtain the nanocrystalline high silicon steel bar with the diameter of 10 mm.
g. And (3) hot drawing wire drawing treatment: and carrying out hot drawing treatment on the nanocrystalline high-silicon steel wire rod, wherein the hot drawing temperature is 900 ℃, the deformation amount is 6% each time, and 24 times of hot drawing are carried out to prepare the strong magnetic induction nanocrystalline high-silicon steel wire rod with the diameter of 1.2 mm.
Example 2
A preparation method of a strong magnetic induction nanocrystalline high silicon steel wire comprises the following steps:
the high silicon steel alloy comprises the following components in percentage by mass:
c:0.0040% -0.0055%, si:6.1 to 6.9 percent of Mn:0.16% -0.24%, S:0.02% -0.04%, ce:0.02% -0.05%, B:0.04% -0.08%, P: < 0.004%, al:0.029% -0.037%, N:0.012 to 0.015 percent and the balance of Fe;
a. smelting a high silicon steel alloy: controlling the vacuum degree of a C, si, mn, S, fe smelting chamber to be 6.0 multiplied by 10 according to the proportion of the high silicon steel alloy -4 And (3) Pa or below, injecting high-purity Ar to keep the vacuum degree of a smelting chamber at-0.07 to-0.04 MPa, repeatedly smelting at 1550 ℃ for three times, then preserving heat for 6 minutes, adding rare earth cerium and ferroboron-iron-based coordination compound into the alloy, repeatedly smelting at 1400 ℃ for three times, preserving heat for 5 minutes, and finally adding AlN nano ceramic particles into the alloy, and repeatedly smelting at 1400 ℃ for three times to obtain the high silicon steel alloy.
b. Preparing a high silicon steel thin strip by high vacuum single-roller melt spinning: the high vacuum single-roller melt-spinning machine is adopted, the surface linear speed of copper rollers of the high vacuum high-speed single-roller melt-spinning machine is controlled at 40m/s, and the melt-spinning chamber is kept at 5 multiplied by 10 -4 And (3) preparing the high-silicon steel alloy into a high-silicon steel thin strip with the thickness of 30m, uniform structure and good plasticity by high vacuum degree of Pa.
c. Amorphization treatment: amorphizing the high-silicon steel thin strip by a high-energy ball mill, wherein the rotating speed of the high-energy ball mill at one stage is controlled at 900rpm/min, the ball milling is performed for 30min, nano Cu particles accounting for 5wt% of the high-silicon steel thin strip are added in the high-energy ball milling process at one stage, the rotating speed of the high-energy ball mill at two stages is controlled at 700rpm/min, and the ball milling is performed for 60min, so that the high-silicon steel powder with the average particle size of 240nm is prepared.
d. Microwave hot press molding: and carrying out microwave hot pressing on the high-silicon steel powder, wherein the microwave hot pressing temperature is 850 ℃, and the microwave hot pressing pressure is 50Mpa, so that the high-silicon steel bar with the diameter of 45mm is prepared.
e. And (3) microwave sintering: and (3) carrying out microwave sintering on the high silicon steel bar at the sintering temperature of 1000 ℃ for 23min to obtain the nanocrystalline high silicon steel bar.
f. Large plastic deformation hot rolling: and carrying out large plastic deformation hot rolling on the nanocrystalline high silicon steel bar, carrying out three times of hot rolling at 830 ℃, wherein the rolling reduction is 40% each time, and carrying out vacuum annealing at 1000 ℃ for 5min after each time of hot rolling to obtain the nanocrystalline high silicon steel bar with the diameter of 10 mm.
g. And (3) hot drawing wire drawing treatment: and carrying out hot drawing treatment on the nanocrystalline high-silicon steel wire rod, wherein the hot drawing temperature is 900 ℃, the deformation amount is 8% each time, and carrying out 21-pass hot drawing to obtain the strong magnetic induction nanocrystalline high-silicon steel wire rod with the diameter of 1.1 mm.
Example 3
A preparation method of a strong magnetic induction nanocrystalline high silicon steel wire comprises the following steps:
the high silicon steel alloy comprises the following components in percentage by mass:
c:0.0040% -0.0055%, si:6.1 to 6.9 percent of Mn:0.16% -0.24%, S:0.02% -0.04%, ce:0.02% -0.05%, B:0.04% -0.08%, P: < 0.004%, al:0.029% -0.037%, N:0.012 to 0.015 percent and the balance of Fe;
a. smelting a high silicon steel alloy: controlling the vacuum degree of a C, si, mn, S, fe smelting chamber to be 6.0 multiplied by 10 according to the proportion of the high silicon steel alloy -4 And (3) Pa or below, injecting high-purity Ar to keep the vacuum degree of a smelting chamber at-0.07 to-0.04 MPa, repeatedly smelting at 1450 ℃ for three times, then preserving heat for 4 minutes, adding rare earth cerium and ferroboron-iron-based coordination compound into the alloy, repeatedly smelting at 1430 ℃ for three times, preserving heat for 5 minutes, and finally adding AlN nano ceramic particles into the alloy, and repeatedly smelting at 1350 ℃ for three times to obtain the high silicon steel alloy.
b. Preparing a high silicon steel thin strip by high vacuum single-roller melt spinning: by usingHigh vacuum single-roller melt-spinning machine, copper roller surface linear speed of high vacuum high speed single-roller melt-spinning machine is controlled at 25m/s, and melt-spinning chamber is maintained at 5×10 -4 And (3) preparing the high-silicon steel alloy into a high-silicon steel thin strip with the thickness of 25m, uniform structure and good plasticity by high vacuum degree of Pa.
c. Amorphization treatment: amorphizing the high-silicon steel thin strip by a high-energy ball mill, wherein the rotating speed of the high-energy ball mill at one stage is controlled at 1000rpm/min, the ball milling is carried out for 250min, nano Cu particles accounting for 5wt% of the high-silicon steel thin strip are added in the high-energy ball milling process at one stage, the rotating speed of the high-energy ball mill at two stages is controlled at 600rpm/min, and the ball milling is carried out for 70min, so that the high-silicon steel powder with the average particle size of 270nm is prepared.
d. Microwave hot press molding: and carrying out microwave hot pressing on the high-silicon steel powder, wherein the microwave hot pressing temperature is 950 ℃, and the microwave hot pressing pressure is 55Mpa, so that the high-silicon steel bar with the diameter of 45mm is prepared.
e. And (3) microwave sintering: and (3) carrying out microwave sintering on the high silicon steel bar at 1100 ℃ for 20min to obtain the nanocrystalline high silicon steel bar.
f. Large plastic deformation hot rolling: and carrying out large plastic deformation hot rolling on the nanocrystalline high silicon steel bar, carrying out three times of hot rolling at 1000 ℃, wherein the rolling reduction is 36% each time, and carrying out vacuum annealing at 1200 ℃ for 5min after each time of hot rolling to obtain the nanocrystalline high silicon steel bar with the diameter of 9 mm.
g. And (3) hot drawing wire drawing treatment: and carrying out hot drawing treatment on the nanocrystalline high-silicon steel wire rod, wherein the hot drawing temperature is 950 ℃, the deformation amount is 7% each time, and carrying out 23-pass hot drawing to obtain the strong magnetic induction nanocrystalline high-silicon steel wire rod with the diameter of 1.0 mm.
Comparative example 1
The high silicon steel alloy comprises the following components in percentage by mass: si:6.50%, C:0.015%, S:0.0054%, ti:0.015, mn:0.02%, P:0.056%, cr:0.013%, B:0.0008%, the balance being iron.
Alloy smelting: the raw materials are put into a vacuum induction furnace for smelting according to the proportion, refined for 5min at 1550 ℃, and then vacuum cast into cast ingots.
And (3) die forging: and forging the cast ingot at 1050 ℃ to obtain the high-silicon steel bar with the diameter of 13 mm.
Rolling: and (3) carrying out abnormal rolling on the high silicon steel bar at 900 ℃, wherein the reduction of each pass is 1mm, 7 passes are carried out, and the intermediate tempering is carried out for 3 times, so that the high silicon steel bar with the diameter of 6mm is prepared.
And (3) heat treatment: and (3) preserving the temperature of the high-silicon steel wire at 850 ℃ for 1h, and then cooling with brine.
Acid washing: and (3) pickling the high silicon steel wire after heat treatment to remove the oxide scale.
And (3) hot drawing: and (3) carrying out hot drawing on the high silicon steel wire subjected to acid washing treatment by adopting a horizontal drawing machine, carrying out total drawing for 15 times, wherein the deformation of each time is 5%, the total deformation is 73%, and finally obtaining the high silicon steel wire with the diameter of 1.60 mm.
Test examples
The magnetic induction performance, iron loss and plastic deformation amount were measured for the high silicon steel wire rods prepared in examples 1 to 3 and comparative example 1, and the measurement results are shown in table 1.
TABLE 1 magnetic induction performance, iron loss value and plastic deformation to failure of high silicon steel wire
From the test data in table 1, it is clear that the strong magnetic induction nanocrystalline high silicon steel wire prepared in examples 1 to 3 has excellent magnetic properties, extremely low iron loss and good ductility.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, or alternatives falling within the spirit and principles of the invention.
Claims (10)
1. The preparation method of the strong magnetic induction nanocrystalline high silicon steel wire is characterized by comprising the following steps:
a. smelting high silicon steel alloy: the high silicon steel comprises the following chemical components in percentage by mass: c:0.0040% -0.0055%, si:6.1 to 6.9 percent of Mn:0.16% -0.24%, S:0.02% -0.04%, ce:0.02% -0.05%, B:0.04% -0.08%, P: < 0.004%, al:0.029% -0.037%, N:0.012 to 0.015 percent and the balance of Fe; the alloy elements Ce and B are added after mother alloy is smelted for 1-4 times, wherein the B element is added in the form of ferroboron-iron-base coordination compound, and AlN ceramic grains are added according to the proportion of Al and N;
b. preparing the high silicon steel alloy into a high silicon steel thin strip by adopting a high vacuum single-roller strip casting machine;
c. amorphization treatment: performing amorphization treatment on the high silicon steel ribbon by ball milling, and adding nano Cu particles accounting for 3-5wt% of the high silicon steel ribbon in the ball milling process to prepare high silicon steel powder with the average particle size of 200-300 nm;
d. and carrying out microwave hot-press molding and microwave sintering on the high-silicon steel powder to obtain a high-silicon steel bar, and carrying out large plastic deformation hot rolling and hot drawing treatment on the high-silicon steel bar to obtain the strong magnetic induction nanocrystalline high-silicon steel wire with the diameter of 0.8-1.4 mm.
2. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, which is characterized in that: in the step a, the specific smelting steps of the high silicon steel alloy are as follows:
a1, feeding the high silicon steel into a vacuum melting furnace according to the chemical components of the high silicon steel except for alloy elements Ce, B, al and N, wherein the vacuum degree of the vacuum melting furnace is controlled to be 6.0 multiplied by 10 -4 Under Pa, then injecting high-purity Ar to keep the vacuum degree of a vacuum smelting furnace at-0.07 to-0.04 MPa, repeatedly smelting the melted master alloy at 1450-1550 ℃ for 1-4 times, and then preserving the heat for 4-6 minutes;
a2, cooling to 1400-1450 ℃, adding the rare earth cerium and the ferroboron-iron-based coordination compound, repeatedly smelting for 2-4 times, and preserving heat for 3-5 minutes;
a3, cooling to 1350-1400 ℃, adding AlN nano ceramic particles, and repeatedly smelting for 2-3 times to obtain the high silicon steel alloy.
3. The strong of claim 1The preparation method of the magnetic induction nanocrystalline high-silicon steel wire is characterized by comprising the following steps: in the step b, the linear speed of the copper roller surface of the high-vacuum single-roller melt-spinning machine is controlled between 30m/s and 40m/s, and the melt-spinning chamber is kept to be 1 multiplied by 10 -4 ～6×10 -4 The thickness of the prepared high silicon steel thin strip is 20-45 um.
4. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, which is characterized in that: in the step c, a high-energy ball mill is adopted for ball milling, the rotating speed of the high-energy ball mill is controlled to be 600-1000 r/min, and the ball milling is carried out for 70-100min.
5. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 4, which is characterized in that: in the step c, the high-energy ball milling is carried out in two stages, wherein the rotating speed of the high-energy ball milling in the first stage is controlled to be 800-1000 r/min, the ball milling is carried out for 20-40min, nano Cu particles are added in the high-energy ball milling process in the first stage, and the rotating speed of the high-energy ball milling in the second stage is controlled to be 600-800 r/min, and the ball milling is carried out for 40-80min.
6. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, which is characterized in that: in the step d, the temperature of the microwave hot press molding is 800-900 ℃ and the pressure is 40-50 MPa.
7. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, which is characterized in that: the sintering temperature of the microwave sintering is 950-1150 ℃ and the sintering time is 20-25 min.
8. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, which is characterized in that: the specific steps of large plastic deformation hot rolling are as follows: three times of hot rolling are carried out at 850-1050 ℃, the reduction of each time is 35-40%, and vacuum annealing is carried out for 3-5 min at 950-1200 ℃ after each time of hot rolling.
9. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, which is characterized in that: the hot drawing wire treatment comprises the following specific steps: and (3) drawing the high-silicon steel wire rod for 20-25 times by adopting a horizontal drawing machine at the temperature of 850-950 ℃, wherein the deformation of each pass is 5-8%.
10. The strong magnetic induction nanocrystalline high silicon steel wire manufactured by the method for manufacturing the strong magnetic induction nanocrystalline high silicon steel wire according to any one of claims 1 to 9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211574788.8A CN115747664B (en) | 2022-12-08 | 2022-12-08 | Strong magnetic induction nanocrystalline high silicon steel wire and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211574788.8A CN115747664B (en) | 2022-12-08 | 2022-12-08 | Strong magnetic induction nanocrystalline high silicon steel wire and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115747664A CN115747664A (en) | 2023-03-07 |
| CN115747664B true CN115747664B (en) | 2023-11-10 |
Family
ID=85344622
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211574788.8A Active CN115747664B (en) | 2022-12-08 | 2022-12-08 | Strong magnetic induction nanocrystalline high silicon steel wire and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115747664B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1863934A (en) * | 2003-10-06 | 2006-11-15 | 新日本制铁株式会社 | High-strength magnetic steel sheet and worked part therefrom, and process for producing them |
| CN101466851A (en) * | 2006-06-16 | 2009-06-24 | 新日本制铁株式会社 | High intensity electromagnetic steel plate and method of manufacturing the same |
| CN101935800A (en) * | 2010-09-30 | 2011-01-05 | 东北大学 | High-silicon-steel thin belt and preparation method thereof |
| CN102543347A (en) * | 2011-12-31 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | Iron-based nanometer crystal magnetically soft alloy and preparation method thereof |
| KR20150073798A (en) * | 2013-12-23 | 2015-07-01 | 주식회사 포스코 | Non-oriented electrical steel sheets and method for manufacturing the same |
| CN105755404A (en) * | 2016-05-16 | 2016-07-13 | 河北工业大学 | Fe-based amorphous/nanocrystalline soft magnetic alloy thin belt and preparation method thereof |
| JP2017145490A (en) * | 2016-02-19 | 2017-08-24 | Ｊｆｅスチール株式会社 | Manufacturing method of oriented electromagnetic steel sheet |
| CN111451515A (en) * | 2020-03-16 | 2020-07-28 | 深圳顺络电子股份有限公司 | Low-power-consumption soft magnetic alloy material, preparation method thereof and electronic device |
| CN114293089A (en) * | 2021-12-31 | 2022-04-08 | 河北科技大学 | Soft magnetic high silicon steel ultra-thin strip and preparation method thereof |
-
2022
- 2022-12-08 CN CN202211574788.8A patent/CN115747664B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1863934A (en) * | 2003-10-06 | 2006-11-15 | 新日本制铁株式会社 | High-strength magnetic steel sheet and worked part therefrom, and process for producing them |
| CN101466851A (en) * | 2006-06-16 | 2009-06-24 | 新日本制铁株式会社 | High intensity electromagnetic steel plate and method of manufacturing the same |
| CN101935800A (en) * | 2010-09-30 | 2011-01-05 | 东北大学 | High-silicon-steel thin belt and preparation method thereof |
| CN102543347A (en) * | 2011-12-31 | 2012-07-04 | 中国科学院宁波材料技术与工程研究所 | Iron-based nanometer crystal magnetically soft alloy and preparation method thereof |
| KR20150073798A (en) * | 2013-12-23 | 2015-07-01 | 주식회사 포스코 | Non-oriented electrical steel sheets and method for manufacturing the same |
| JP2017145490A (en) * | 2016-02-19 | 2017-08-24 | Ｊｆｅスチール株式会社 | Manufacturing method of oriented electromagnetic steel sheet |
| CN105755404A (en) * | 2016-05-16 | 2016-07-13 | 河北工业大学 | Fe-based amorphous/nanocrystalline soft magnetic alloy thin belt and preparation method thereof |
| CN111451515A (en) * | 2020-03-16 | 2020-07-28 | 深圳顺络电子股份有限公司 | Low-power-consumption soft magnetic alloy material, preparation method thereof and electronic device |
| CN114293089A (en) * | 2021-12-31 | 2022-04-08 | 河北科技大学 | Soft magnetic high silicon steel ultra-thin strip and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115747664A (en) | 2023-03-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112522645B (en) | Preparation method of high-strength high-toughness homogeneous fine-grain CrCoNi intermediate-entropy alloy thin plate | |
| CN102851577B (en) | High grade non-oriented silicon steel produced by continuous casting and rolling of sheet billet and production method thereof | |
| JP7387008B2 (en) | Iron-based amorphous alloy containing sub-nanoscale ordered clusters, method for preparing the same, and nanocrystalline alloy derivatives using the same | |
| JP6025864B2 (en) | High silicon steel plate excellent in productivity and magnetic properties and method for producing the same | |
| CN102071339A (en) | Samarium-cobalt permanent magnet material and preparation method thereof | |
| CN106868379A (en) | A kind of high-entropy alloy with big magnetostriction coefficient and preparation method thereof | |
| CN111826545B (en) | Copper-iron alloy material and preparation method and application thereof | |
| CN102212712A (en) | Beryllium copper alloy, copper bush for amorphous and/or nano crystal strip production equipment and preparation method | |
| CN107858579A (en) | The method for improving high-entropy alloy magnetic property is heat-treated using Constant charge soil | |
| CN115198162B (en) | Entropy alloy in high-toughness heterogeneous multi-phase core-shell organization structure and preparation method thereof | |
| CN104831036A (en) | Preparation method of Fe-6.5%Si through thin-strip casting, high-temperature rolling and quick quenching process | |
| CN107541591A (en) | A kind of manufacture method of super electromagnetic pure iron DT4C bars | |
| CN102982935B (en) | A kind of without heavy rare earth permanent magnetic material and hot pressing method for preparing thereof | |
| CN102650016B (en) | Manufacturing method for high-magnetic induction low-cost 250 MPa cold-rolled magnetic pole steel | |
| Liang et al. | Effect of heat treatment on mechanical properties of heavily cold-rolled Fe-6.5 wt% Si alloy sheet | |
| CN115747664B (en) | Strong magnetic induction nanocrystalline high silicon steel wire and preparation method thereof | |
| CN114107799B (en) | High-strength silicon steel thin strip plate with excellent high-frequency electromagnetic performance and production process | |
| CN103695756B (en) | The half-technique non oriented silicon steel adopting CSP to produce and method | |
| CN105957675A (en) | Preparation method of rare-earth permanent magnet material | |
| CN114657461B (en) | High-strength non-oriented silicon steel based on solid solution strengthening and preparation method thereof | |
| CN102176507A (en) | Preparation method of FeGaYB lamellate magnetostriction material | |
| CN113278826B (en) | Preparation method of high-permeability copper-infiltrated wire | |
| CN112080699B (en) | Method for preparing high-magnetic-performance powder silicon steel sheet | |
| CN113621894A (en) | Preparation method of FeCrAl alloy steel strip | |
| CN112877581B (en) | Preparation method of improved sintered neodymium iron boron cast sheet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |