CN117626151A - Amorphous micrometer wire with high saturation magnetic induction intensity and high magnetic conductivity and heat treatment method - Google Patents
Amorphous micrometer wire with high saturation magnetic induction intensity and high magnetic conductivity and heat treatment method Download PDFInfo
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- CN117626151A CN117626151A CN202311724159.3A CN202311724159A CN117626151A CN 117626151 A CN117626151 A CN 117626151A CN 202311724159 A CN202311724159 A CN 202311724159A CN 117626151 A CN117626151 A CN 117626151A
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000006698 induction Effects 0.000 title claims abstract description 19
- 229910000808 amorphous metal alloy Inorganic materials 0.000 claims abstract description 62
- 238000000137 annealing Methods 0.000 claims abstract description 28
- 230000035699 permeability Effects 0.000 claims abstract description 14
- 210000003632 microfilament Anatomy 0.000 claims description 22
- 239000000126 substance Substances 0.000 claims description 4
- 102000002151 Microfilament Proteins Human genes 0.000 claims description 3
- 108010040897 Microfilament Proteins Proteins 0.000 claims description 3
- 238000005253 cladding Methods 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000000956 alloy Substances 0.000 abstract description 41
- 229910045601 alloy Inorganic materials 0.000 description 39
- 238000004804 winding Methods 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 20
- 239000010453 quartz Substances 0.000 description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 16
- 238000003723 Smelting Methods 0.000 description 15
- 238000001816 cooling Methods 0.000 description 12
- 239000000498 cooling water Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910017061 Fe Co Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910000697 metglas Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The invention provides an amorphous micrometer wire with high saturation magnetic induction and high magnetic conductivity and a heat treatment method, and relates to the technical field of amorphous alloy materials. The amorphous alloy micrometer wire is subjected to low-temperature annealing under the condition of magnetic field application, and current is applied in the low-temperature annealing process; the temperature of the low-temperature annealing is 200-400 ℃; the magnetic field is applied along the radial direction of the amorphous alloy micrometer wire. After the amorphous alloy micrometer wire is treated by the heat treatment method provided by the invention, the amorphous alloy micrometer wire can be endowed with high saturation magnetic induction intensity and high magnetic permeability.
Description
Technical Field
The invention relates to the technical field of amorphous alloy materials, in particular to an amorphous micrometer wire with high saturation magnetic induction and high magnetic permeability and a heat treatment method.
Background
Since the 60 s of the 20 th century, the professor Duwez has invented au—si amorphous alloys, which have been developed to a great extent. With the invention and application of Metglas 2605 (FeSiB, domestic trademark 1K 101) and Finemet (FeSiBNbCu, domestic trademark 1K 107), the soft magnetic amorphous alloy strip has been widely used in the fields of electronic power components, such as common mode inductance, mutual inductor, reactor, distribution transformer, and the like.
However, there is currently little research on amorphous alloy wires, particularly amorphous alloy micro wires with high magnetic permeability. The Fe-Co-based amorphous alloy micrometer wire has been applied to the fields of medical guide wires, weak magnetic sensors and the like in a small scale due to excellent mechanical properties and magnetic properties.
At present, amorphous wires with high saturation induction (Bs) and high magnetic permeability are not available, and reports on the aspects are not available.
Disclosure of Invention
The invention aims to provide an amorphous micrometer wire with high saturation magnetic induction and high magnetic permeability and a heat treatment method.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a heat treatment method of amorphous alloy micrometer wires, which comprises the following steps: carrying out low-temperature annealing on the amorphous alloy micrometer wire under the condition of applying a magnetic field, and applying current in the low-temperature annealing process; the temperature of the low-temperature annealing is 200-400 ℃; the magnetic field is applied along the radial direction of the amorphous alloy micrometer wire.
Preferably, the strength of the magnetic field is 800-1200 Gs.
Preferably, the magnetic field is provided by a C-type permanent magnet.
Preferably, the low-temperature annealing time is 5-20 min.
Preferably, the time for applying the current is 5 to 20 seconds.
Preferably, the magnitude of the current is > 0 and less than or equal to 30A.
Preferably, the current is a direct current.
Preferably, the amorphous alloy micrometer wire has a chemical formula of Co a Fe b Si c B d Wherein a+b>70, a+b+c+d=100, a, b, c and d being atomic percentages of the corresponding elements.
Preferably, the amorphous alloy microfilaments are prepared by a glass cladding method.
The invention provides an amorphous micrometer wire with high saturation magnetic induction and high magnetic conductivity, which is obtained by heat treatment of an amorphous alloy micrometer wire by the heat treatment method.
The invention provides a heat treatment method of amorphous alloy micrometer wires, which comprises the following steps: carrying out low-temperature annealing on the amorphous alloy micrometer wire under the condition of applying a magnetic field, and applying current in the low-temperature annealing process; the temperature of the low-temperature annealing is 200-400 ℃; the magnetic field is applied along the radial direction of the amorphous alloy micrometer wire. After the amorphous alloy micrometer wire is treated by the heat treatment method provided by the invention, the amorphous alloy micrometer wire can be endowed with high saturation magnetic induction intensity and high magnetic permeability.
Drawings
FIG. 1 is a schematic diagram of a preparation structure of amorphous alloy microfilaments;
FIG. 2 shows the permeability curves of example 1, comparative example 1 and comparative example 1';
fig. 3 shows hysteresis loops of example 1, comparative example 1 and comparative example 1'.
Detailed Description
The invention provides a heat treatment method of amorphous alloy micrometer wires, which comprises the following steps: carrying out low-temperature annealing on the amorphous alloy micrometer wire under the condition of applying a magnetic field, and applying current in the low-temperature annealing process; the temperature of the low-temperature annealing is 200-400 ℃; the magnetic field is applied along the radial direction of the amorphous alloy micrometer wire.
In the invention, the chemical formula of the amorphous alloy micrometer wire is preferably Co a Fe b Si c B d Wherein a+b>70, a+b+c+d=100, a, b, c and d being atomic percentages of the corresponding elements. In the embodiment of the invention, the amorphous alloy micrometer wire has the specific composition of Co 51 Fe 22 Si 12 B 15 、Co 55 Fe 18 Si 12 B 15 、Co 59 Fe 14 Si 12 B 15 、Co 63 Fe 10 Si 12 B 15 Or Co 67 Fe 6 Si 12 B 15 。
The preparation process of the amorphous alloy micrometer wire has no special requirement, and the amorphous alloy micrometer wire is prepared by a glass cladding method well known in the art.
In the invention, the preparation method of the amorphous alloy microfilament preferably comprises the following steps:
weighing and mixing the preparation raw materials according to the composition of each element in the chemical formula to obtain a mixed raw material;
smelting the mixed raw materials to obtain a master alloy;
placing the master alloy into a quartz tube of a wire making device, vacuumizing the quartz tube, introducing argon, carrying out induction heating on the quartz tube filled with the master alloy, and drawing the quartz tube and the master alloy into amorphous alloy micrometer wires by using a drawing rod after the bottom of the quartz tube and the master alloy are in a molten state; and cooling by using cooling water in the traction process.
In the invention, the smelting times are preferably 3-4 times, and the invention preferably carries out smelting in an arc furnace; the smelting is preferably performed in a vacuum environment. The invention has no special requirement on the induction heating condition, and adopts an induction heating mode which is well known in the field. FIG. 1 is a flow chart of the preparation of amorphous alloy microfilaments according to the invention.
The invention carries out low-temperature annealing on the amorphous alloy micrometer wire under the condition of applying a magnetic field.
In the present invention, the strength of the magnetic field is preferably 1000Gs; the magnetic field is applied along the radial direction of the amorphous alloy micrometer wire; the magnetic field is preferably provided by a C-type permanent magnet. The time of applying the magnetic field is the same as the time of low-temperature annealing.
In the present invention, the low temperature annealing temperature is 200 to 400 ℃, preferably 250 to 350 ℃, more preferably 280 to 320 ℃; the time for the low-temperature annealing is preferably 5 to 20 minutes, more preferably 8 to 17 minutes, and even more preferably 10 to 15 minutes. In the present invention, the low temperature annealing is preferably performed under a vacuum atmosphere, and the vacuum degree is preferably < 10Pa.
The invention applies current in the low-temperature annealing process; the time for applying the current is preferably 5 to 20 seconds, more preferably 8 to 17 seconds, and still more preferably 10 to 15 seconds. The current can be applied at any stage of the low-temperature annealing, and preferably, the current is applied at the beginning of the low-temperature annealing.
In the present invention, the magnitude of the current is preferably > 0 and 30A or less, more preferably 5 to 20A, and still more preferably 10 to 15A. In the present invention, the current is preferably a direct current.
After the amorphous alloy micrometer wire is treated by the method, the saturation magnetic induction intensity and the magnetic permeability of the amorphous alloy micrometer wire can be remarkably improved.
The invention provides an amorphous micrometer wire with high saturation magnetic induction and high magnetic conductivity, which is obtained by heat treatment of an amorphous alloy micrometer wire by the heat treatment method.
The amorphous microfilaments and the heat treatment method having both high saturation induction and high magnetic permeability according to the present invention will be described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Co 51 Fe 22 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 51 Fe 22 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
Under vacuum, a magnetic field is applied along the radial direction of the amorphous alloy micrometer wire, the magnetic field is heat treated by 1000Gs at 300 ℃ for 10min, and the direct current is applied by 20A and 10s (when the magnetic field is applied at the beginning).
Example 2
Co 55 Fe 18 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 55 Fe 18 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
Under vacuum, a magnetic field is applied along the radial direction of the amorphous alloy micrometer wire, and the magnetic field is heat treated at 1000Gs,350 ℃ for 5min, and the direct current is applied at 20A,5s (when the magnetic field is applied at the beginning).
Example 3
Co 59 Fe 14 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 59 Fe 14 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
Under vacuum, a magnetic field is applied along the radial direction of the amorphous alloy micrometer wire, the magnetic field is used for heat treatment of 1000Gs,250 ℃ and 15min, and the direct current is used for heat treatment of 15A,10s (applied when the magnetic field starts to be applied).
Example 4
Co 63 Fe 10 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 63 Fe 10 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
Under vacuum, a magnetic field is applied along the radial direction of the amorphous alloy micrometer wire, and the magnetic field is heat treated for 1000Gs,350 ℃, and the direct current is applied for 25A,10s (when the magnetic field is applied at the beginning).
Example 5
Co 67 Fe 6 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 67 Fe 6 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
Under vacuum, a magnetic field is applied along the radial direction of the amorphous alloy micrometer wire, and the magnetic field is heat treated at 1000Gs,300 ℃ for 15min, and the DC current is applied at 20A,15s (when the magnetic field is applied at the beginning).
Comparative example 1
Co 51 Fe 22 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 51 Fe 22 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
The electric current joule heat treatment was performed for 20A-10s (no magnetic field was applied and no heating was performed).
Comparative example 1'
Co 51 Fe 22 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 51 Fe 22 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
Heat-treating 1000Gs at 300 ℃ for 10min.
Comparative example 2
Co 55 Fe 18 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and feeding by a winding deviceRolling to obtain Co 55 Fe 18 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
The electric current joule heat treatment was performed for 20A-5s (no magnetic field was applied and no heating was performed).
Comparative example 3
Co 59 Fe 14 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 59 Fe 14 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
And carrying out electric current Joule heat treatment for 15A-10s.
Comparative example 4
Co 63 Fe 10 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing, putting into a quartz tube, drawing in a molten state, cooling with cooling water, and winding by a winding device to obtain Co 63 Fe 10 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
The electric current joule heat treatment 25A-10s (no magnetic field applied and no heating).
Comparative example 5
Co 67 Fe 6 Si 12 B 15 Alloy
S1, burdening;
s2, smelting in high vacuum for 4 times to ensure that the master alloy components are uniform, and 20-30 g of alloy ingots;
s3, crushing and then putting the crushed materials into a quartz tube, and carrying out melting stateDrawing wire, cooling with cooling water, and winding by a winding device to obtain Co 67 Fe 6 Si 12 B 15 Amorphous alloy microfilaments;
s4, performing heat treatment on the amorphous wire
The electric current joule heat treatment was performed for 20A-15s (no magnetic field was applied and no heating was performed).
Saturation induction intensity measurement was performed using a quantium Design VSM, permeability measurement was performed using a Keysight impedance analyzer, and saturation induction intensity and permeability of amorphous microwires after heat treatment of examples and comparative examples are shown in table 1, wherein permeability curves of example 1 and comparative example 1 are shown in fig. 2, and hysteresis loops of example 1 and comparative example 1 are shown in fig. 3.
Table 1 composition, heat treatment pattern and heat treatment result of amorphous alloy microfilaments of examples and comparative examples
| Composition of the components | Heat treatment mode | Bs/T | μ@1kHz | |
| Example 1 | Co 51 Fe 22 Si 12 B 15 | Magnetic field + current | 0.9 | 21423 |
| Example 2 | Co 55 Fe 18 Si 12 B 15 | Magnetic field + current | 0.86 | 17826 |
| Example 3 | Co 59 Fe 14 Si 12 B 15 | Magnetic field + current | 0.81 | 16987 |
| Example 4 | Co 63 Fe 10 Si 12 B 15 | Magnetic field + current | 0.76 | 12598 |
| Example 5 | Co 67 Fe 6 Si 12 B 15 | Magnetic field + current | 0.69 | 9886 |
| Comparative example 1 | Co 51 Fe 22 Si 12 B 15 | Electric current | 0.81 | 6668 |
| Comparative example 1' | Co 51 Fe 22 Si 12 B 15 | Magnetic field | 0.79 | 4628 |
| Comparative example 2 | Co 55 Fe 18 Si 12 B 15 | Electric current | 0.82 | 6345 |
| Comparative example 3 | Co 59 Fe 14 Si 12 B 15 | Electric current | 0.78 | 6215 |
| Comparative example 4 | Co 63 Fe 10 Si 12 B 15 | Electric current | 0.73 | 5387 |
| Comparative example 5 | Co 67 Fe 6 Si 12 B 15 | Electric current | 0.63 | 4654 |
As is apparent from the results of table 1, according to the present invention, by annealing the amorphous alloy microfilaments by applying a magnetic field and a current at the same time, the saturation induction and the magnetic permeability of the amorphous alloy microfilaments can be significantly improved compared to the case of applying a single current annealing or a single magnetic field annealing.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (10)
1. The heat treatment method of the amorphous alloy micrometer wire is characterized by comprising the following steps of: carrying out low-temperature annealing on the amorphous alloy micrometer wire under the condition of applying a magnetic field, and applying current in the low-temperature annealing process; the temperature of the low-temperature annealing is 200-400 ℃; the magnetic field is applied along the radial direction of the amorphous alloy micrometer wire.
2. The heat treatment method according to claim 1, wherein the strength of the magnetic field is 800 to 1200Gs.
3. A heat treatment method according to claim 1 or 2, wherein the magnetic field is provided by a C-type permanent magnet.
4. The heat treatment method according to claim 1, wherein the time of the low-temperature annealing is 5 to 20 minutes.
5. The heat treatment method according to claim 1, wherein the time for applying the electric current is 5 to 20 seconds.
6. The heat treatment method according to claim 1, wherein the magnitude of the current is > 0 and 30A or less.
7. The heat treatment method according to claim 1, 5 or 6, wherein the electric current is a direct current.
8. The heat of claim 1The treatment method is characterized in that the chemical formula of the amorphous alloy micrometer wire is Co a Fe b Si c B d Wherein a+b>70, a+b+c+d=100, a, b, c and d being atomic percentages of the corresponding elements.
9. The heat treatment method according to claim 1 or 8, wherein the amorphous alloy microfilaments are prepared by a glass cladding method.
10. An amorphous microfilament having both high saturation induction and high magnetic permeability, which is obtained by heat-treating an amorphous alloy microfilament by the heat treatment method according to any one of claims 1 to 9.
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- 2023-12-14 CN CN202311724159.3A patent/CN117626151A/en active Pending
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| US6217672B1 (en) * | 1997-09-24 | 2001-04-17 | Yide Zhang | Magnetic annealing of magnetic alloys in a dynamic magnetic field |
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