CN112391583A - FeCo-based soft magnetic alloy and preparation method and application thereof - Google Patents
FeCo-based soft magnetic alloy and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of soft magnetic materials, and particularly relates to a FeCo-based soft magnetic alloy which comprises the chemical composition of (Fe)0.8Co0.2)aBbSicCudWherein a is more than or equal to 82 and less than or equal to 85, b is more than or equal to 13 and less than or equal to 16, c is 1,d is 1, and a + b + c + d is 100. The FeCo-based soft magnetic alloy is directly formed in the rapid cooling process, has the characteristics of high saturation magnetic induction intensity and low coercive force without a high-temperature annealing process, and solves the annealing brittleness problem caused by annealing.
Description
Technical Field
The invention belongs to the technical field of soft magnetic materials, and particularly relates to a FeCo-based soft magnetic alloy and a preparation method and application thereof.
Background
Currently, a new round of scientific and technological revolution and industrial transformation are in the future, and the competition pattern of new material industry in the world is slowly and greatly adjusted. The development in the fields of new generation information technology, aerospace, new energy and the like provides a wider development space for magnetic materials, particularly soft magnetic materials. Along with the high-speed development of economy in China, the energy problem is increasingly prominent, and power transformers in industrial enterprises are very commonly applied and have relatively large excavation potential in the aspect of energy conservation. The problems of large loss, complex production process and the like exist when the silicon steel sheet applied at present is used as the transformer iron core, and the requirement of energy conservation cannot be met. The amorphous soft magnetic alloy has excellent soft magnetic properties such as high saturation magnetic induction, low coercive force, low iron core loss (about 1/5-1/3 of silicon steel) and the like, is used as a transformer iron core, has the advantages of low loss and obvious energy-saving and environment-friendly advantages, meets the requirements of energy conservation and consumption reduction, and is widely applied to various power electronic devices. However, the amorphous state is a thermodynamically unstable state, and a coarse crystal phase may be precipitated when used at a high temperature, so that the coercive force thereof is rapidly increased. In addition, as the frequency of use increases, the soft magnetic properties of the amorphous alloy also deteriorate seriously, thus limiting its application range. Since amorphous alloys have problems such as low saturation induction and deterioration of magnetic properties at high frequencies, nanocrystals have been developed.
In 1988, researchers develop Fe-Si-B-Cu-Nb nanocrystalline alloy by using amorphous alloy through a proper annealing process for the first time, and further research finds that the saturation magnetic induction intensity of the alloy can be properly improved and the coercive force of the alloy can be reduced by adding certain alloy elements such as Nb, Mo, Y and the like and combining with the proper crystallization annealing process; in addition, the preparation of the nanocrystalline soft magnetic alloy in the prior art requires subsequent annealing treatment. However, the extreme brittleness of iron-based nanocrystalline magnetically soft alloys after annealing is a recognized disadvantage compared to amorphous and bulk glassy magnetically soft alloys. Since nanocrystalline soft magnetic alloys were first produced in the free Fe-Si-B-Nb-Cu system, it was generally accepted that overcoming brittleness was not possible in the past decades! So far, there is no report of synthesizing an iron-based nanocrystalline magnetically soft alloy having good bending toughness. In addition, a large amount of metallic amorphous forming elements in the alloy, such as: the addition of Al, Gd, Nb, Mo, Y and the like not only increases the production cost of the amorphous alloy, but also makes the alloy easy to generate oxidation reaction, and is not beneficial to production and transportation.
Disclosure of Invention
Based on the defects in the prior art, the invention provides a FeCo-based soft magnetic alloy and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a FeCo-based magnetically soft alloy with a chemical composition of (Fe)0.8Co0.2)aBbSicCudWherein, a is more than or equal to 82 and less than or equal to 85, b is more than or equal to 13 and less than or equal to 16, c is 1, d is 1, and a + b + c + d is 100.
Preferably, a is 84.
Preferably, the FeCo-based soft magnetic alloy has an amorphous nanocrystalline structure.
The invention also provides a preparation method of the FeCo-based soft magnetic alloy, which comprises the following steps:
s1, adding Fe, Co, Cu, Si and alloy Fe-B serving as raw materials into a non-consumable vacuum arc melting furnace, and melting under the protection of argon to prepare a master alloy ingot;
s2, cutting the master alloy ingot, polishing surface oxide skin, transferring the master alloy ingot into a quartz tube, and melting the master alloy ingot by using a medium-frequency induction melting furnace to obtain molten steel;
and S3, spraying the molten steel onto a copper roller by adopting a rapid quenching method for rapid cooling to prepare the FeCo-based magnetically soft alloy strip.
Preferably, in step S1, the melting is repeated 3 to 5 times.
Preferably, the degree of vacuum of the non-consumable vacuum arc melting furnace is 5X 10-3Pa or less.
Preferably, the saturation magnetization B of the FeCo-based soft magnetic alloy stripsSatisfies the following conditions: 1.3T is less than or equal to Bs≤1.7T。
Preferably, the linear speed of the copper roller is 20-55 m/s.
Preferably, the width of the FeCo-based soft magnetic alloy strip is 1-3mm, and the thickness is less than 26 μm.
The invention also provides an application of the FeCo-based soft magnetic alloy in any one of the schemes or the FeCo-based soft magnetic alloy strip prepared by the preparation method in any one of the schemes, and the FeCo-based soft magnetic alloy strip is used as a transformer iron core.
Compared with the prior art, the invention has the beneficial effects that:
(1) the two-phase structure of the FeCo-based amorphous nanocrystalline alloy is directly formed in the rapid cooling process, has the characteristics of high saturation magnetic induction intensity and low coercive force without a high-temperature annealing process, and solves the annealing brittleness problem caused by annealing.
(2) The preparation method is simpler, the flow is more convenient, and the production period is greatly shortened; the raw materials used for smelting in the invention are common and cheap Fe, Co, Si, Cu and the intermediate alloy Fe-B, and do not contain expensive rare metals, such as: gd. Nb and the like; and the purity of the raw materials reaches the industrial grade purity, so that the cost of the raw materials is greatly reduced.
(3) The FeCo-based soft magnetic alloy strip prepared by the invention not only has good soft magnetic performance, high magnetic flux density and low coercive force, but also has good bending toughness, is convenient for subsequent processing and production, and is easy to realize industrialized production.
Drawings
FIG. 1 is a photograph of the soft magnetic alloy strip of examples 1 to 4 of the present invention, which is (Fe) in the order from the left to the right0.8Co0.2)85B13Si1Cu1、(Fe0.8Co0.2)84B14Si1Cu1、(Fe0.8Co0.2)83B15Si1Cu1、(Fe0.8Co0.2)82B16Si1Cu1；
FIG. 2 is photographs (a, b) of the process of folding and photograph (c) of the unfolded soft magnetic alloy strip of example 1 of the present invention;
FIG. 3 is an XRD spectrum of the soft magnetic alloy strips of examples 1-4 of the present invention;
FIG. 4 is a DSC curve of the soft magnetic alloy ribbon of examples 1-4 of the present invention;
FIG. 5 is a graph of the magnetic induction intensity of the soft magnetic alloy strips of examples 1-4 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following specific examples.
In each embodiment of the invention, Fe, Co, B, Si and Cu are selected as alloy components, and raw materials are Fe, Co, Si and Cu with the industrial purity of more than 99.9 percent and intermediate alloy Fe-B.
Example 1:
this example prepares (Fe)0.8Co0.2)85B13Si1Cu1A crystalline magnetically soft alloy ribbon comprising the steps of:
firstly, preparing needed raw materials of Fe, Co, Si, Cu and intermediate alloy Fe-B, grinding off an oxide film on the metal surface, and enabling the purity of the adopted raw materials to reach an industrial grade purity standard, and then according to the formula (Fe)0.8Co0.2)85B13Si1Cu1The atomic percentage of (A) is prepared;
secondly, uniformly putting the proportioned raw materials into a copper crucible, and carrying out the process under high vacuum degree, wherein the vacuum degree is generally 5 multiplied by 10-3And Pa, introducing high-purity argon, and melting the raw materials into molten steel by using a non-consumable vacuum arc melting furnace under the protection of the argon. At the same time, isThe obtained master alloy reaches the standard of uniform components, and the master alloy is repeatedly smelted for 3-5 times to obtain a master alloy ingot;
thirdly, cutting the obtained master alloy ingot through wire cutting, polishing surface oxide skin, putting the master alloy ingot into a quartz tube, keeping the distance between the quartz tube and a copper roller at 0.3-2cm, remelting the alloy into molten steel through a medium-frequency induction melting furnace in an electromagnetic induction heating mode, and spraying the molten steel onto the copper roller with the linear velocity of 20-55m/s to obtain the FeCo-based soft magnetic alloy strip, wherein the width is about 1mm (not limited to 1mm, but also 2mm, 3mm and the like) and the thickness is about 22 mu m as shown in figure 1.
Fourthly, carrying out a series of performance testing on the obtained alloy strip, as shown in figure 2, comparing the alloy strip before and after folding, which shows that the alloy strip has better bending toughness; as shown in fig. 3, the XRD pattern showed a distinct crystalline phase α -Fe, and then the thermodynamic characteristic temperature of the finished strip was determined by using a Differential Scanning Calorimeter (DSC), as shown in fig. 4; using Squid, the saturation magnetization B was measuredsAt 1.58T, as shown in fig. 5, the resulting FeCo-based soft magnetic alloy ribbon is known as a typical soft magnetic material.
Example 2:
this example prepares (Fe)0.8Co0.2)84B14Si1Cu1Amorphous nanocrystalline soft magnetic alloy strip, including the following steps:
firstly, preparing needed raw materials of Fe, Co, Si, Cu and intermediate alloy Fe-B, grinding off an oxide film on the metal surface, and enabling the purity of the adopted raw materials to reach an industrial grade purity standard, and then according to the formula (Fe)0.8Co0.2)84B14Si1Cu1The atomic percentage of (A) is prepared;
secondly, uniformly putting the proportioned raw materials into a copper crucible, and carrying out the process under high vacuum degree, wherein the vacuum degree is generally 5 multiplied by 10-3And Pa, introducing high-purity argon, and melting the raw materials into molten steel by a non-consumable vacuum arc melting furnace under the protection of the argon. Meanwhile, in order to ensure that the obtained master alloy reaches the standard of uniform compositionRepeatedly smelting the master alloy for 3-5 times to obtain a master alloy ingot;
thirdly, cutting and cutting the obtained master alloy ingot through wire cutting, polishing surface oxide skin, then putting the master alloy ingot into a quartz tube, keeping the distance between the quartz tube and a copper roller at 1-2cm, then remelting the alloy into molten steel through a medium-frequency induction smelting furnace in an electromagnetic induction heating mode, and then spraying the molten steel onto the copper roller with the linear velocity of 20-55m/s to obtain the FeCo-based magnetically soft alloy strip, wherein the width is about 1mm, and the thickness is about 23 μm, as shown in figure 1.
Fourthly, a series of performance tests are carried out on the obtained alloy strip, as shown in fig. 3, an XRD (X-ray diffraction) spectrum shows an obvious amorphous nanocrystalline dual-phase structure, and then the thermodynamic characteristic temperature of the finished strip is determined by using a Differential Scanning Calorimeter (DSC), as shown in fig. 4; using Squid, the saturation magnetization B was measuredsAt 1.66T, the resulting FeCo-based soft magnetic alloy strip is known to be a typical soft magnetic material as shown in fig. 5.
Example 3:
this example prepares (Fe)0.8Co0.2)83B15Si1Cu1An amorphous soft magnetic alloy ribbon comprising the steps of:
firstly, preparing needed raw materials of Fe, Co, Si, Cu and intermediate alloy Fe-B, grinding off an oxide film on the metal surface, and enabling the purity of the adopted raw materials to reach an industrial grade purity standard, and then according to the formula (Fe)0.8Co0.2)83B15Si1Cu1The atomic percentage of (A) is prepared;
secondly, uniformly putting the proportioned raw materials into a copper crucible, and carrying out the process under high vacuum degree, wherein the vacuum degree is generally 5 multiplied by 10-3And Pa, introducing high-purity argon, and melting the raw materials into molten steel by using a non-consumable vacuum arc melting furnace under the protection of the argon. Meanwhile, in order to enable the obtained master alloy to reach the standard of uniform components, repeatedly smelting the master alloy for 3-5 times to obtain a master alloy ingot;
thirdly, cutting and cutting the obtained master alloy ingot through wire cutting, polishing surface oxide skin, then putting the master alloy ingot into a quartz tube, keeping the distance between the quartz tube and a copper roller at about 1-2cm, then remelting the alloy into molten steel through a medium-frequency induction smelting furnace in an electromagnetic induction heating mode, and then spraying the molten steel onto the copper roller with the linear velocity of 20-55m/s to obtain the FeCo-based magnetically soft alloy strip, wherein the width is about 1mm, and the thickness is about 22 μm, as shown in figure 1.
Fourthly, a series of performance tests are carried out on the obtained alloy strip, as shown in fig. 3, an XRD (X-ray diffraction) spectrum shows obvious amorphous state, and then the thermodynamic characteristic temperature of the finished strip is determined by using a Differential Scanning Calorimeter (DSC), as shown in fig. 4; using Squid, the saturation magnetization B was measuredsAt 1.41T, as shown in fig. 5, the resulting FeCo-based soft magnetic alloy ribbon is known as a typical soft magnetic material.
Example 4:
the amorphous soft magnetic alloy strip of the present embodiment is different from embodiment 3 in that: chemical composition of (Fe)0.8Co0.2)82B16Si1Cu1The procedure was as in example 3.
The resulting alloy strip was subjected to a series of performance tests, as shown in figure 3, showing a distinct amorphous state on the XRD pattern, and the thermodynamic characteristic temperature of the finished strip was determined by using a Differential Scanning Calorimeter (DSC), as shown in figure 4; using Squid, the saturation magnetization B was measuredsAt 1.37T, as shown in fig. 5, the resulting FeCo-based soft magnetic alloy ribbon is known as a typical soft magnetic material.
The performance parameters of the soft magnetic alloy strips produced in the above examples are summarized in table 1.
TABLE 1 Performance parameters of Soft magnetic alloy strips obtained in examples 1-4
The FeCo-based soft magnetic alloy of the embodiment of the invention has the characteristics of high saturation magnetic induction and low coercive force without annealing treatment, thereby solving the annealing brittleness problem caused by annealing to a certain extent.
The FeCo-based soft magnetic alloy of the embodiment of the invention is used as a transformer iron core and is applied to a power transformer.
The saturation magnetization intensity B of the FeCo-based soft magnetic alloy strip can be realized by adjusting the percentage of each componentsSatisfies the following conditions: 1.3T is less than or equal to Bs≤1.7T。
The foregoing has outlined rather broadly the preferred embodiments and principles of the present invention and it will be appreciated that those skilled in the art may devise variations of the present invention that are within the spirit and scope of the appended claims.
Claims (10)
1. A FeCo-based soft magnetic alloy characterized by having a chemical composition of (Fe)0.8Co0.2)aBbSicCudWherein, a is more than or equal to 82 and less than or equal to 85, b is more than or equal to 13 and less than or equal to 16, c is 1, d is 1, and a + b + c + d is 100.
2. A FeCo-based soft magnetic alloy according to claim 1, wherein a has a value of 84.
3. A FeCo-based soft magnetic alloy according to claim 2, wherein said FeCo-based soft magnetic alloy is of amorphous nanocrystalline structure.
4. A method for preparing a FeCo-based soft magnetic alloy according to any of claims 1 to 3, comprising the steps of:
s1, adding Fe, Co, Cu, Si and alloy Fe-B serving as raw materials into a non-consumable vacuum arc melting furnace, and melting under the protection of argon to prepare a master alloy ingot;
s2, cutting the master alloy ingot, polishing surface oxide skin, transferring the master alloy ingot into a quartz tube, and melting the master alloy ingot by using a medium-frequency induction melting furnace to obtain molten steel;
and S3, spraying the molten steel onto a copper roller by adopting a rapid quenching method for rapid cooling to prepare the FeCo-based magnetically soft alloy strip.
5. The production method according to claim 4, wherein the melting is repeated 3 to 5 times in step S1.
6. The method according to claim 4, wherein a degree of vacuum of the non-consumable vacuum arc melting furnace is 5 x 10-3Pa or less.
7. The production method according to claim 4, wherein the saturation magnetization B of the FeCo-based soft magnetic alloy stripsSatisfies the following conditions: 1.3T is less than or equal to Bs≤1.7T。
8. The production method according to claim 4, wherein the linear velocity of the copper roller is 20 to 55 m/s.
9. The production method according to claim 4, wherein the FeCo-based soft magnetic alloy strip has a width of 1 to 3mm and a thickness of less than 26 μm.
10. Use of a FeCo-based soft magnetic alloy according to any of claims 1 to 3 or of a FeCo-based soft magnetic alloy strip produced by the method of production according to any of claims 4 to 9 as a transformer core.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5225006A (en) * | 1988-05-17 | 1993-07-06 | Kabushiki Kaisha Toshiba | Fe-based soft magnetic alloy |
| DE19639428A1 (en) * | 1995-09-25 | 1997-03-27 | Alps Electric Co Ltd | High frequency composite material with soft magnetic properties |
| CN106119739A (en) * | 2016-06-24 | 2016-11-16 | 郑州大学 | Iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof |
| CN107103976A (en) * | 2016-02-22 | 2017-08-29 | 天津大学 | A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy and preparation method thereof |
| CN110993239A (en) * | 2019-04-19 | 2020-04-10 | 东南大学 | Iron-cobalt-based amorphous soft magnetic alloy and preparation method thereof |
-
2020
- 2020-11-26 CN CN202011343348.2A patent/CN112391583A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5225006A (en) * | 1988-05-17 | 1993-07-06 | Kabushiki Kaisha Toshiba | Fe-based soft magnetic alloy |
| DE19639428A1 (en) * | 1995-09-25 | 1997-03-27 | Alps Electric Co Ltd | High frequency composite material with soft magnetic properties |
| CN107103976A (en) * | 2016-02-22 | 2017-08-29 | 天津大学 | A kind of iron cobalt-based toughness nano-crystal soft magnetic alloy and preparation method thereof |
| CN106119739A (en) * | 2016-06-24 | 2016-11-16 | 郑州大学 | Iron-based amorphous and nanocrystalline soft magnetic alloy and preparation method thereof |
| CN110993239A (en) * | 2019-04-19 | 2020-04-10 | 东南大学 | Iron-cobalt-based amorphous soft magnetic alloy and preparation method thereof |
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