CN115747664A - 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
- CN115747664A CN115747664A CN202211574788.8A CN202211574788A CN115747664A CN 115747664 A CN115747664 A CN 115747664A CN 202211574788 A CN202211574788 A CN 202211574788A CN 115747664 A CN115747664 A CN 115747664A
- Authority
- CN
- China
- Prior art keywords
- silicon steel
- steel wire
- nanocrystalline
- preparing
- ball milling
- 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.)
- Granted
Links
- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 143
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 34
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000006698 induction Effects 0.000 claims abstract description 24
- 238000005098 hot rolling Methods 0.000 claims abstract description 21
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 39
- 239000000956 alloy Substances 0.000 claims description 39
- 239000002245 particle Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 18
- 238000000713 high-energy ball milling Methods 0.000 claims description 16
- 239000010949 copper Substances 0.000 claims description 13
- 238000009768 microwave sintering Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 238000005491 wire drawing Methods 0.000 claims description 12
- 229910052796 boron Inorganic materials 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 10
- 229910052684 Cerium Inorganic materials 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- 238000005245 sintering Methods 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910052698 phosphorus Inorganic materials 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 5
- 238000005280 amorphization Methods 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
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical class [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000005275 alloying 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
- 229910052710 silicon Inorganic materials 0.000 abstract description 13
- 229910052742 iron Inorganic materials 0.000 abstract description 12
- 239000010703 silicon Substances 0.000 abstract description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000009987 spinning Methods 0.000 abstract description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 6
- 238000007731 hot pressing Methods 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000002505 iron Chemical class 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 238000002074 melt spinning Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000007712 rapid solidification Methods 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 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
- 238000010586 diagram Methods 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 230000035699 permeability Effects 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
- 239000010959 steel Substances 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Images
Landscapes
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to high silicon steelIn particular to a strong magnetic induction nanocrystalline high silicon steel wire and a preparation method thereof. The preparation method of the high-strength magnetic induction nanocrystalline high-silicon steel wire comprises smelting, high-vacuum strip spinning preparation of a high-silicon steel thin strip, non-crystallization treatment, microwave hot-press molding, three-pass hot rolling and hot drawing. The high-intensity magnetic induction nanocrystalline high-silicon steel wire prepared by the preparation method provided by the invention has the advantages that the grain size is 500-800nm, the tissue is uniform, the room-temperature tensile elongation can reach 10.50% at most, the saturation magnetic induction intensity Ms reaches 2.01T, the coercive force Hc can reach 15.8A/m at most, and the iron loss P is P 1.0/400 The lowest value is 7.9W/kg, and the composite material 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 silicon content close to 6.5wt% is an advanced crystalline soft magnetic material, and is suitable for motors, transformers and inductors in medium and high frequency ranges. The resistivity of Si was increased by 54% to 83. Mu. Ω. Cm by Fe-6.5wt% as compared with that of the currently widely used Fe-3.2wt% Si electric steel. 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 operational noise while reducing hysteresis losses. However, increasing the silicon content also results in B2 and DO 3 Due to the formation of ordered phases, the conventional high silicon steel manufacturing process often causes 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 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 the strong magnetic induction nanocrystalline high silicon steel wire and the preparation method thereof, and the strong magnetic induction nanocrystalline high silicon steel wire prepared by the method has the advantages of uniform tissue, fine grains, good ductility, low iron loss and good magnetic induction performance.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a preparation method of high-intensity magnetically-induced nanocrystalline high-silicon steel comprises the following steps:
a. smelting of high-silicon steel alloy: the high silicon steel comprises the following chemical components in percentage by mass: c:0.0040 to 0.0055%, si:6.1% -6.9%, 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: 0.012-0.015 percent and the balance of Fe; adding alloy elements Ce and B after smelting the master alloy for 1-4 times, wherein the B element is added in the form of boron-iron-based coordination compound, and then adding AlN ceramic particles according to the ratio of Al to N;
b. preparing the high-silicon steel alloy into a high-silicon steel thin strip by adopting a high-vacuum single-roller strip throwing machine;
c. amorphization treatment: ball-milling the high-silicon steel thin strip to perform non-crystallization treatment, and adding nano Cu particles accounting for 3-5 wt% of the high-silicon steel thin strip in the ball-milling process to prepare high-silicon steel powder with the average particle size of 200-300 nm;
d. and (2) 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 wire drawing on the high-silicon steel bar to obtain a strong-magnetism-sensing nanocrystalline high-silicon steel wire with the diameter of 0.8-1.4 mm.
The ductility of the high-silicon steel alloy is improved by adding cerium, the fluidity of the remelting alloy can be improved by adding boron, and the plasticity and yield of the soft magnetic high-silicon steel ultra-thin strip can be further improved by adding cerium and boron. The AlN nano ceramic particles are added, so that the high-silicon steel alloy can be attached to the AlN nano ceramic particles to be nucleated again in the microwave sintering process, the crystallinity of the nano crystals is improved to obtain more uniform and fine crystal grains, and a good tissue basis is provided for improving the magnetism and the plasticity of the high-silicon steel wire.
The rapid solidification technology can effectively inhibit ordered phases B2 and DO 3 By suppressing disordered opposite ordered phases B2 and DO 3 The transformation of (A) can effectively solve the brittleness problem of high-silicon steel, and the mechanical properties of the high-silicon steel are improved on the basis of phase transformation.
The high silicon steel powder can be heated uniformly in the pressing and forming process through microwave heating and pressing and forming. The nano Cu particles fully fill gaps of the high-silicon steel powder in the microwave hot pressing process, so that the compactness and the wire drawing performance of a hot-press forming sample are greatly improved;
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 chemical components of the high-silicon steel except for alloying 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 Pa below, then injecting high-purity Ar to keep the vacuum degree of the vacuum smelting furnace at-0.07 to-0.04 MPa, repeatedly smelting the molten master alloy at 1450 to 1550 ℃ for 1 to 4 times, and then preserving heat for 4 to 6 minutes;
a2, cooling to 1400-1450 ℃, adding rare earth cerium and boron-iron-based coordination compound, repeatedly smelting for 2-4 times, and then preserving heat for 3-5 minutes;
a3, cooling to 1350-1400 ℃, adding the 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 the rare earth cerium element and the AlN nano ceramic particles on one hand, and can ensure the uniform smelting of all elements in the master alloy on the other hand.
Preferably, in the step b, the surface linear speed of the copper roller of the high-vacuum single-roller melt-spun machine is controlled to be between 30m/s and 40m/s, and the melt-spun chamber is kept at 1 x 10 -4 ～6×10 -4 Pa, the thickness of the prepared high silicon steel thin strip is between 20 and 45 um.
Preferably, in the step c, a high-energy ball mill is adopted for ball milling, and the rotating speed of the high-energy ball mill is controlled at 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 carried out in two stages, wherein the rotating speed of the first-stage high-energy ball milling is controlled to be 800-1000 rpm/min, the ball milling is carried out for 20-40min, the nano Cu particles are added in the process of the first-stage high-energy ball milling, and the rotating speed of the second-stage high-energy ball milling is controlled to be 600-800 rpm/min, and the ball milling is carried out for 40-80min.
The high-silicon steel thin strip can be more fully amorphized 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 through high-temperature microwave sintering treatment to re-nucleate, so that a uniform nanocrystalline structure is obtained, and the plasticity of the high-silicon steel bar is greatly improved.
Preferably, the hot rolling with large plastic deformation comprises the following specific steps: carrying out three times of hot rolling at 850-1050 ℃, wherein the reduction of each time is 35-40%, and carrying out vacuum annealing at 950-1200 ℃ for 3-5 min after each time of hot rolling.
Preferably, the hot drawing and wire drawing treatment comprises the following specific steps: and (2) at the temperature of 850-950 ℃, performing 20-25 times of drawing on the high-silicon steel wire by using a horizontal drawing machine, wherein the deformation of each time is 5-8%.
The high-intensity magnetic induction nanocrystalline high-silicon steel wire prepared by the preparation method provided by the invention has the advantages of high yield, uniform grain size, good plasticity and low iron loss, the attached figure 2 shows that the average grain size of the high-intensity magnetic induction nanocrystalline high-silicon steel wire is 500-800nm, the room-temperature tensile elongation of the high-intensity magnetic induction nanocrystalline high-silicon steel wire can reach 10.50% at most, the saturation magnetic induction intensity Ms reaches 2.01T, the highest coercive force Hc reaches 15.8A/m, and the iron loss P is P 1.0/400 The lowest value is 7.9W/kg, and the composite material has good comprehensive performance.
Drawings
FIG. 1 is a micro-topography of a thin high silicon steel strip produced in example 1 of the present invention
FIG. 2 is a microscopic morphology diagram of a strongly magnetic induction nanocrystalline high silicon steel wire produced in example 1 of the present invention
FIG. 3 is a drawing of a tensile test of a strongly magnetically sensitive nanocrystalline high silicon steel wire produced in example 1 of the present invention
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit 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% -6.9%, 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: 0.012-0.015 percent and the balance of Fe;
a. smelting a high-silicon steel alloy: adding C, si, mn, S and Fe into a high-vacuum arc melting furnace according to the proportion of the high-silicon steel alloy, and controlling the vacuum degree of a melting chamber to be 6.0 multiplied by 10 -4 And Pa below, then injecting high-purity Ar to keep the vacuum degree of the smelting chamber between-0.07 MPa and-0.04 MPa, repeatedly smelting for 2 times at 1500 ℃, then preserving the heat for 6 minutes, then adding AlN ceramic particles and the boron-laminated iron-based 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-spun machine is adopted, the surface linear velocity of a copper roller of the high-vacuum high-speed single-roller melt-spun machine is controlled at 45m/s, and a melt-spun chamber is kept at 6 multiplied by 10 -4 And Pa, preparing the high-silicon steel alloy into a high-silicon steel thin strip with the thickness of 35m, uniform structure and good plasticity.
c. Amorphization treatment: and carrying out non-crystallization treatment on the high-silicon thin strip by using a high-energy ball mill, wherein the ball milling speed is 600rpm/min, the ball milling time is 100min, and adding nano Cu particles accounting for 4wt% of the high-silicon thin strip in the high-energy ball milling process to prepare high-silicon steel powder with the average particle size of 250 nm.
d. Microwave hot-press molding: and (3) 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 as to prepare the high-silicon steel bar with the diameter of 45 mm.
e. Microwave sintering: and (3) performing 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. Hot rolling with large plastic deformation: and (2) 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 reduction per time is 40%, and carrying out vacuum annealing at 930 ℃ for 5min after each time of hot rolling to obtain the nanocrystalline high-silicon steel wire rod with the diameter of 10 mm.
g. Hot drawing and wire drawing treatment: and carrying out hot drawing and wire drawing treatment on the nanocrystalline high-silicon steel wire at the temperature of 900 ℃ with the deformation of 6% each time for 24 times to prepare the strongly magnetic induction nanocrystalline high-silicon steel wire 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% -6.9%, 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: 0.012-0.015 percent and the balance of Fe;
a. smelting a high-silicon steel alloy: controlling the vacuum degree of a C, si, mn, S and Fe smelting chamber to be 6.0 multiplied by 10 according to the proportion of the high-silicon steel alloy -4 Pa below, injecting high-purity Ar to maintain the vacuum degree of the smelting chamber at-0.07-0.04 MPa, repeatedly smelting at 1550 deg.C for three times, holding the temperature for 6 min, adding rare earth cerium and boron-laminated iron-based coordination compound, repeatedly smelting at 1400 deg.C for three times, holding the temperature for 5min, and adding high-purity Ar to the alloyAdding AlN nano ceramic particles into the alloy, and repeatedly smelting for three times at 1400 ℃ to obtain the high-silicon steel alloy.
b. Preparing a high-silicon steel thin strip by high-vacuum single-roller strip spinning: the high-vacuum single-roller melt-spun machine is adopted, the surface linear velocity of a copper roller of the high-vacuum high-speed single-roller melt-spun machine is controlled to be 40m/s, and a melt-spun chamber is kept at 5 multiplied by 10 -4 And Pa, preparing the high-silicon steel alloy into a high-silicon steel thin strip with the thickness of 30m, uniform structure and good plasticity.
c. Amorphization treatment: and carrying out non-crystallization treatment on the high-silicon thin strip by using a high-energy ball mill, wherein the rotating speed of the first-stage high-energy ball milling is controlled at 900rpm/min, the ball milling is carried out for 30min, nano Cu particles accounting for 5wt% of the high-silicon thin strip are added in the first-stage high-energy ball milling process, the rotating speed of the second-stage high-energy ball milling is controlled at 700rpm/min, the ball milling is carried out for 60min, and 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 at the temperature of 850 ℃ and under the pressure of 50Mpa to obtain the high-silicon steel bar with the diameter of 45 mm.
e. 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. Hot rolling with large plastic deformation: and (3) 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 reduction per time is 40%, and carrying out vacuum annealing at 1000 ℃ for 5min after each time of hot rolling to obtain the nanocrystalline high-silicon steel wire rod with the diameter of 10 mm.
g. Hot drawing and wire drawing treatment: and carrying out hot drawing and wire drawing treatment on the nanocrystalline high-silicon steel wire at the temperature of 900 ℃ with the deformation of 8% each time for 21 times to prepare the strongly magnetic induction nanocrystalline high-silicon steel wire 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 to 0.0055%, si:6.1% -6.9%, 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: 0.012-0.015 percent and the balance of Fe;
a. smelting a high-silicon steel alloy: controlling the vacuum degree of a C, si, mn, S and Fe smelting chamber to be 6.0 multiplied by 10 according to the proportion of the high-silicon steel alloy -4 Pa below, then injecting high-purity Ar to keep the vacuum degree of a smelting chamber between-0.07 MPa and-0.04 MPa, repeatedly smelting for three times at 1450 ℃, then preserving heat for 4 minutes, then adding rare earth cerium and boron-laminated iron-based coordination compound into the alloy, repeatedly smelting for three times at 1430 ℃, preserving heat for 5 minutes, finally adding AlN nano ceramic particles into the alloy, and repeatedly smelting for three times at 1350 ℃ to prepare 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-spun machine is adopted, the surface linear velocity of a copper roller of the high-vacuum high-speed single-roller melt-spun machine is controlled to be 25m/s, and a melt-spun chamber is kept at 5 multiplied by 10 -4 And Pa, preparing the high-silicon steel alloy into a high-silicon steel thin strip with the thickness of 25m, uniform structure and good plasticity.
c. Amorphization treatment: and carrying out non-crystallization treatment on the high-silicon thin strip by using a high-energy ball mill, wherein the rotating speed of the first-stage high-energy ball milling is controlled at 1000rpm/min, the ball milling is carried out for 250min, nano Cu particles accounting for 5wt% of the high-silicon thin strip are added in the first-stage high-energy ball milling process, the rotating speed of the second-stage high-energy ball milling is controlled at 600rpm/min, the ball milling is carried out for 70min, and 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 at the temperature of 950 ℃ and the pressure of 55Mpa to obtain the high-silicon steel bar with the diameter of 45 mm.
e. Microwave sintering: and (3) carrying out microwave sintering on the high-silicon steel bar at the sintering temperature of 1100 ℃ for 20min to obtain the nanocrystalline high-silicon steel bar.
f. Hot rolling with large plastic deformation: and (3) 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 reduction per time is 36%, and carrying out vacuum annealing at 1200 ℃ for 5min after each time of hot rolling to obtain the nanocrystalline high-silicon steel wire rod with the diameter of 9 mm.
g. Hot drawing and wire drawing treatment: and carrying out hot drawing and wire drawing treatment on the nanocrystalline high-silicon steel wire at the hot drawing and wire drawing temperature of 950 ℃ and the deformation of 7% each time, and carrying out hot drawing for 23 times to prepare the strongly magnetic induction nanocrystalline high-silicon steel wire 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 percent and the balance of iron.
Alloy smelting: the raw materials are put into a vacuum induction furnace to be smelted according to the proportion and refined for 5min at 1550 ℃, and then the materials are cast into ingots in vacuum.
Die forging: and die forging the cast ingot at 1050 ℃ to prepare the high-silicon steel bar with the diameter of 13 mm.
Rolling: and (3) carrying out special-shaped rolling on the high-silicon steel bar at 900 ℃, wherein the reduction of each pass is 1mm, the pass is 7, and the intermediate tempering is 3 times to obtain the high-silicon steel wire with the diameter of 6 mm.
And (3) heat treatment: and (3) preserving the heat of the high-silicon steel wire at 850 ℃ for 1h, and then cooling with brine.
Acid washing: and (4) carrying out acid washing on the high-silicon steel wire subjected to heat treatment to remove oxide scale.
Hot drawing: and (3) carrying out hot drawing on the acid-washed high-silicon steel wire by using a horizontal drawing machine, carrying out 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 properties, iron loss and plastic deformation under failure of the high silicon steel wires prepared in examples 1 to 3 and comparative example 1 were measured, and the results are shown in table 1.
TABLE 1 magnetic induction properties, iron loss values and plastic deformation upon failure of high silicon steel wires
As is apparent from the test data in Table 1, the strongly magnetic nanocrystalline high silicon steel wires prepared in examples 1 to 3 have excellent magnetic properties, extremely low iron loss and good ductility.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the invention is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (10)
1. A preparation method of a strong magnetic induction nanocrystalline high silicon steel wire is characterized by comprising the following steps:
a. smelting of 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% -6.9%, 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; adding alloy elements Ce and B after smelting the master alloy for 1-4 times, wherein the B element is added in the form of a boron-iron-based coordination compound, and then adding AlN ceramic particles according to the ratio of Al to N;
b. preparing the high-silicon steel alloy into a high-silicon steel thin strip by adopting a high-vacuum single-roller strip throwing machine;
c. amorphization treatment: ball-milling the high-silicon steel thin strip to perform non-crystallization treatment, and adding nano Cu particles accounting for 3-5 wt% of the high-silicon steel thin strip in the ball-milling process to prepare high-silicon steel powder with the average particle size of 200-300 nm;
d. and (2) 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 wire drawing on the high-silicon steel bar to obtain a strong magnetic induction nanocrystalline high-silicon steel wire with the diameter of 0.8-1.4 mm.
2. The method for preparing the strongly magnetic nanocrystalline high silicon steel wire according to claim 1, 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 chemical components of the high-silicon steel except for alloying 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 Pa below, then injecting high-purity Ar to keep the vacuum degree of the vacuum smelting furnace at-0.07 to-0.04 MPa, repeatedly smelting the molten master alloy at 1450 to 1550 ℃ for 1 to 4 times, and then preserving heat for 4 to 6 minutes;
a2, cooling to 1400-1450 ℃, adding rare earth cerium and boron-iron-based coordination compound, repeatedly smelting for 2-4 times, and then 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 method for preparing the strongly magnetic nanocrystalline high silicon steel wire according to claim 1, characterized in that: in the step b, the surface linear velocity of the copper roller of the high-vacuum single-roller melt-spun machine is controlled between 30m/s and 40m/s, and the melt-spun chamber is kept at 1 multiplied by 10 -4 ～6×10 -4 Pa, and the thickness of the prepared high silicon steel thin strip is between 20 and 45 um.
4. The method for preparing the strongly magnetic nanocrystalline high silicon steel wire according to claim 1, characterized in that: and c, ball milling by using a high-energy ball mill, wherein the rotating speed of the high-energy ball mill is controlled at 600-1000 rpm/min, and the ball milling is carried out for 70-100min.
5. The method for preparing the strongly magnetic nanocrystalline high silicon steel wire according to claim 4, wherein the method comprises the following steps: and c, performing high-energy ball milling 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 high-energy ball milling in the first stage, and 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.
6. The method for preparing the strongly magnetic nanocrystalline high silicon steel wire according to claim 1, 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 strongly magnetic nanocrystalline high silicon steel wire according to claim 1, 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 strongly magnetic nanocrystalline high silicon steel wire according to claim 1, characterized in that: the hot rolling with large plastic deformation comprises the following specific steps: carrying out three times of hot rolling at 850-1050 ℃, wherein the reduction of each time is 35-40%, and carrying out vacuum annealing at 950-1200 ℃ for 3-5 min after each time of hot rolling.
9. The method for preparing the strong magnetic induction nanocrystalline high silicon steel wire according to claim 1, characterized in that: the hot drawing and wire drawing treatment comprises the following specific steps: and (2) at the temperature of 850-950 ℃, performing 20-25 times of drawing on the high-silicon steel wire by using a horizontal drawing machine, wherein the deformation of each time is 5-8%.
10. The strongly magnetic nanocrystalline high silicon steel wire produced by the method of producing a strongly magnetic 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 true CN115747664A (en) | 2023-03-07 |
| CN115747664B 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 |
|---|---|
| CN115747664B (en) | 2023-11-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109338200B (en) | High-temperature high-damping high-entropy alloy and preparation method thereof | |
| CN100535164C (en) | Fe-36Ni based alloy wire and manufacturing method thereof | |
| CN112522645B (en) | Preparation method of high-strength high-toughness homogeneous fine-grain CrCoNi intermediate-entropy alloy thin plate | |
| JP7387008B2 (en) | Iron-based amorphous alloy containing sub-nanoscale ordered clusters, method for preparing the same, and nanocrystalline alloy derivatives using the same | |
| 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 | |
| CN113136531B (en) | Powder metallurgy stainless steel | |
| CN103556020A (en) | Manganese copper-based high-damping alloy with high mechanical properties and high manganese content | |
| JP2015507695A (en) | High silicon steel plate excellent in productivity and magnetic properties and method for producing the same | |
| CN102212712A (en) | Beryllium copper alloy, copper bush for amorphous and/or nano crystal strip production equipment and preparation method | |
| CN115198162B (en) | Entropy alloy in high-toughness heterogeneous multi-phase core-shell organization structure and preparation method thereof | |
| CN107858579A (en) | The method for improving high-entropy alloy magnetic property is heat-treated using Constant charge soil | |
| JP2021529262A (en) | High hardness and high conductivity Cu-Ag-Sc alloy and its manufacturing method | |
| CN111455222A (en) | FeCoVZr soft magnetic alloy with excellent high-temperature performance and preparation method thereof | |
| CN107541591A (en) | A kind of manufacture method of super electromagnetic pure iron DT4C bars | |
| CN102361371A (en) | Method for preparing neodymium iron boron magnet for high-speed motor | |
| 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 | |
| WO2022170862A1 (en) | High-strength r-t-b rare earth permanent magnet and preparation method therefor | |
| JP7194780B2 (en) | Method for preparing improved sintered neodymium-iron-boron cast slab | |
| CN112522636A (en) | Nb-doped Fe-Cr-Co permanent magnetic alloy and preparation method thereof | |
| CN112877615B (en) | High-magnetic-induction iron-based amorphous soft magnetic alloy and preparation method thereof | |
| CN114420432B (en) | Preparation method for improving magnetic performance of samarium cobalt permanent magnet material | |
| CN117737578A (en) | Surface treatment method of high silicon steel for motor rotor-stator | |
| CN106710769B (en) | A kind of Nd-Fe-B permanent magnetism thin strip magnet and preparation method thereof |
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 |