CN117721397A - Fe-Sc-M bulk amorphous alloy with high glass forming capability and preparation method and application thereof - Google Patents

Fe-Sc-M bulk amorphous alloy with high glass forming capability and preparation method and application thereof Download PDF

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Publication number
CN117721397A
CN117721397A CN202311699466.0A CN202311699466A CN117721397A CN 117721397 A CN117721397 A CN 117721397A CN 202311699466 A CN202311699466 A CN 202311699466A CN 117721397 A CN117721397 A CN 117721397A
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China
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amorphous alloy
bulk amorphous
alloy
high glass
glass forming
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CN202311699466.0A
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Chinese (zh)
Inventor
汪林立
黄丰
聂铭
梁永纯
吕旺燕
黄正
罗啸宇
谢文平
岳楹超
董重里
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Priority to CN202311699466.0A priority Critical patent/CN117721397A/en
Publication of CN117721397A publication Critical patent/CN117721397A/en
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Abstract

The invention discloses Fe-Sc-M bulk amorphous alloy with high glass forming capability, a preparation method and application thereof, and relates to the field of metal materials. The atomic percentage expression of the bulk amorphous alloy is: fe (Fe) 91 Sc 7 M 2 Wherein M is T i or B, and can be applied to the field of magnetic materials. According to the invention, the glass forming capability in the Fe-Sc blocky amorphous alloy system is optimized by adding T i or B, so that the Fe-based amorphous alloy with high glass forming capability and excellent soft magnetization performance is obtained, the magnetization of the amorphous alloy rapidly rises with the increase of a magnetic field and then gradually reaches saturation under a low magnetic field, and the alloy system shows typical soft magnetic performance and can be prepared into a shapeThe complex magnetic device has simple and easy preparation method and wide application space in the field of magnetic materials.

Description

Fe-Sc-M bulk amorphous alloy with high glass forming capability and preparation method and application thereof
Technical Field
The invention relates to the field of metal materials, in particular to Fe-Sc-M bulk amorphous alloy with high glass forming capability, and a preparation method and application thereof.
Background
In recent years, iron-based amorphous alloys have attracted increasing attention from researchers due to their high strength, extremely strong corrosion resistance and good soft magnetic properties. Iron-based alloys have low amorphous forming ability and require a high cooling rate during cooling, so that the resulting samples are all in the form of filaments or ribbons. As soft magnetic materials, iron-based amorphous alloy strips have been applied in the field of magnetic materials, however, the preparation of iron-based bulk amorphous alloys is more difficult than La-, zr-, pd-, mg-based bulk amorphous alloys.
In practical application, the iron-based amorphous alloy thin strips reduce the saturation magnetization due to gaps among the thin strips, so that the efficiency of the transformer is reduced. In addition, due to the influence of the size, the iron-based amorphous alloy is difficult to prepare a magnetic device with a complex shape, and thus the application of the iron-based amorphous alloy is greatly limited, so that the iron-based bulk amorphous alloy with a large glass forming capability is urgently required to be searched.
Disclosure of Invention
The invention provides an Fe-Sc-M bulk amorphous alloy with high glass forming capability, a preparation method and application thereof, so as to provide an Fe-based bulk amorphous alloy with excellent glass forming capability and thermal stability and excellent soft magnetic performance.
In order to solve the technical problems, one of the purposes of the invention is to provide an Fe-Sc-M bulk amorphous alloy with high glass forming capability, wherein the atomic percentage expression of the bulk amorphous alloy is as follows: fe (Fe) 91 Sc 7 M 2 Wherein M is Ti or B.
As a preferable scheme, the atomic percentage expression of the bulk amorphous alloy is: fe (Fe) 91 Sc 7 Ti 2
As a preferable scheme, the atomic percentage expression of the bulk amorphous alloy is: fe (Fe) 91 Sc 7 B 2
Preferably, the bulk amorphous alloy has a thickness of 35 μm or less.
Preferably, the bulk amorphous alloy has an amorphous structure.
In order to solve the above technical problems, a second object of the present invention is to provide a method for preparing a bulk amorphous alloy of Fe-Sc-M with high glass forming ability, comprising the steps of:
(1) Weighing the elemental raw materials of each metal element according to the stoichiometric ratio of the massive amorphous alloy, placing the elemental raw materials in a crucible according to the sequence of low melting point and high melting point, vacuumizing, introducing argon to-0.08-0.03 Mpa, smelting to form an alloy ingot, cooling, turning over the alloy ingot, and repeatedly smelting for 5-10 to obtain the alloy ingot;
(2) Placing the alloy ingot into a crucible of a pouring system, vacuumizing, introducing argon to 350-400mbar, completely melting the alloy ingot, pouring the alloy ingot into a mold, and cooling and forming.
Preferably, in the steps (1) and (2), the vacuum is applied to 3.5X10 -3 -5×10 -3 Pa。
Preferably, in step (2), the alloy ingot is melted at a current of 200-300A, and then the alloy ingot is completely melted at a current of 400-500A.
In the step (1), the metal element simple substance raw materials are sequentially ultrasonically cleaned in petroleum ether and absolute ethyl alcohol before being used.
In order to solve the technical problems, the invention provides an application of Fe-Sc-M bulk amorphous alloy with high glass forming capability in the field of preparing magnetic materials.
Compared with the prior art, the embodiment of the invention has the following beneficial effects:
1. according to the invention, the glass forming capability in the Fe-Sc blocky amorphous alloy system is optimized by adding Ti or B, so that the Fe-based amorphous alloy with high glass forming capability and excellent soft magnetization performance is obtained, and the magnetization intensity of the amorphous alloy is rapidly increased along with the increase of a magnetic field under a low magnetic field and then gradually reaches saturation, so that the alloy system shows typical soft magnetic performance, a magnetic device with a complex shape can be prepared, the preparation method is simple and easy to implement, and the amorphous alloy has wide application space in the field of magnetic materials.
2. The method controls the proper content of Ti or B element in the amorphous alloy, and if the value of x is too large or too small, the glass forming capacity of the amorphous alloy is changed, so that an amorphous structure is not easy to form.
Drawings
Fig. 1: for Fe in examples 1-2 of the present invention 91 Sc 7 Ti 2 And Fe (Fe) 91 Sc 7 B 2 X-ray diffraction image of bulk amorphous alloy;
fig. 2: fe in comparative examples 1 to 3 according to the present invention 89 Sc 11 、Fe 90 Sc 10 And Fe (Fe) 91 Sc 9 X-ray diffraction image of bulk amorphous alloy;
fig. 3: for Fe in example 1 of the present invention 91 Sc 7 Ti 2 A saturation magnetization curve of the bulk amorphous alloy;
fig. 4: for Fe in example 2 of the present invention 91 Sc 7 B 2 Saturation magnetization curve of bulk amorphous alloy;
Fig. 5: for Fe in example 1 of the present invention 91 Sc 7 Ti 2 DSC curve of bulk amorphous alloy;
fig. 6: for Fe in example 2 of the present invention 91 Sc 7 B 2 DSC curve of bulk amorphous alloy;
fig. 7: fe in comparative examples 1 to 3 according to the present invention 89 Sc 11 、Fe 90 Sc 10 And Fe (Fe) 91 Sc 9 DSC curve of bulk amorphous alloy.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A Fe-Sc-M bulk amorphous alloy with high glass forming ability has an atomic percentage expression of Fe 91 Sc 7 Ti 2 The thickness is 35 mu m, and the preparation method comprises the following specific steps:
(1) Using Fe, sc and Ti metal simple substances with purity not less than 99.9% as raw materials, and converting the simple substances into mass percentages according to an alloy component atomic percentage expression for batching;
(2) Placing the raw materials into copper crucible in order of low melting point and high melting point, and vacuumizing to 3.5X10 -3 Pa, introducing high-purity argon with the purity of 99.99wt% as protective gas, stopping charging until the pressure in the furnace chamber reaches-0.08 Mpa, smelting raw materials, wherein the smelting current is 450A, cooling and turning over the alloy ingot after all the raw materials are melted to form the alloy ingot, smelting again, starting magnetic stirring, and repeating smelting for 6 times to obtain the alloy ingot;
(3) Placing the alloy cast ingot into a copper crucible of a casting system, placing a copper mold with the diameter of 2mm below, and vacuumizing a furnace chamber to 3.5X10 -3 Pa after filling high purity argonAnd (3) gas is up to 400mbar, firstly, the cast ingot is melted under 200A current, then the alloy cast ingot is completely melted under 500A current, the copper crucible is turned over to flow into a copper mold, and the Fe-Sc-M massive amorphous alloy is obtained after cooling and molding.
Example two
The Fe-Sc-M bulk amorphous alloy with high glass forming capability is prepared by the same preparation method, the same reagents and technological parameters as those in the first embodiment, except that the atomic percentage expression is Fe 91 Sc 7 B 2 The thickness was 35. Mu.m.
Comparative example one
The Fe-Sc bulk amorphous alloy with high glass forming ability is prepared by the same preparation method, the same reagents and technological parameters as those in the first embodiment, except that the atomic percentage expression is Fe 89 Sc 11 The thickness was 35. Mu.m.
Comparative example two
The Fe-Sc bulk amorphous alloy with high glass forming ability is prepared by the same preparation method, the same reagents and technological parameters as those in the first embodiment, except that the atomic percentage expression is Fe 90 Sc 10 The thickness was 35. Mu.m.
Comparative example three
The Fe-Sc bulk amorphous alloy with high glass forming ability is prepared by the same preparation method, the same reagents and technological parameters as those in the first embodiment, except that the atomic percentage expression is Fe 91 Sc 9 The thickness was 35. Mu.m.
Performance test
As-cast alloys of examples 1-2 and comparative examples 1-3 having a thickness of 35 μm were subjected to coercivity and saturation magnetization project test using a Vibrating Sample Magnetometer (VSM), an alternating signal was induced in the detection coil by vibration of the sample in the coil, the alternating voltage was proportional to the magnetic moment of the sample, and the hysteresis loop measured by VSM was analyzed to obtain coercivity and saturation magnetization results, the test results are shown in Table 1, the saturation magnetization test results of example 1 are shown in FIG. 3, and the saturation magnetization test results of example 2 are shown in FIG. 4. Meanwhile, the glass transition temperature Tg and the crystallization temperature Tx were obtained by DSC experiment analysis, the DSC curve of example 1 is shown in FIG. 5, the DSC curve of example 2 is shown in FIG. 6, and the DSC curves of comparative examples 1 to 3 are shown in FIG. 7.
TABLE 1 As-cast alloy Performance index in examples 1-2 and comparative examples 1-3
As shown in FIG. 1, examples 1-2 of the present application produced an Fe-Sc-M as-cast alloy having a thickness of 35 μm in an amorphous structure.
As shown in table 1, in examples 1-2 of the present application, the saturation magnetization of the sample was changed singly with the doping element, showing a reduced tendency to change. In the embodiment 1, T i element is added into the Fe-Sc alloy system, so that the soft magnetic property of a final alloy sample is obviously changed, the saturation magnetization is obviously increased, and the soft magnetic property of the alloy sample is improved; in example 2, the B element is added into the Fe-Sc alloy system, so that the soft magnetic property of a final alloy sample is obviously changed, and the saturation magnetization is increased, so that the soft magnetic property of the alloy sample is improved. The saturation magnetization and permeability in examples 1-2 are both higher than those in comparative examples 1-3, indicating that the examples have superior soft magnetic properties compared to the comparative examples.
Referring to FIGS. 5-6, DSC curves show that the as-cast alloys of examples 1-2 of the present invention have a broader supercooled liquid region and thus have higher thermal stability and glass forming ability.
Referring to fig. 3-4, the amorphous alloy of examples 1-2 showed a sharp rise in magnetization with increasing magnetic field and then gradually reached saturation at low magnetic fields, indicating that the alloy system exhibited typical soft magnetic properties.
The foregoing embodiments have been provided for the purpose of illustrating the general principles of the present invention, and are not to be construed as limiting the scope of the invention. It should be noted that any modifications, equivalent substitutions, improvements, etc. made by those skilled in the art without departing from the spirit and principles of the present invention are intended to be included in the scope of the present invention.

Claims (9)

1. An Fe-Sc-M bulk amorphous alloy with high glass forming ability, characterized in that the bulk amorphous alloy has an atomic percentage expression: fe (Fe) 91 Sc 7 M 2 Wherein M is Ti or B.
2. A high glass-forming Fe-Sc-M bulk amorphous alloy according to claim 1, wherein the atomic percent expression of said bulk amorphous alloy is: fe (Fe) 91 Sc 7 Ti 2
3. A high glass-forming Fe-Sc-M bulk amorphous alloy according to claim 1, wherein the atomic percent expression of said bulk amorphous alloy is: fe (Fe) 91 Sc 7 B 2
4. A high glass-forming Fe-Sc-M bulk amorphous alloy according to claim 1, wherein the bulk amorphous alloy has a thickness of less than or equal to 35 μm.
5. A high glass-forming Fe-Sc-M bulk amorphous alloy according to claim 1, wherein said bulk amorphous alloy is amorphous.
6. A method for producing a high glass forming ability Fe-Sc-M bulk amorphous alloy according to any one of claims 1 to 5, comprising the steps of:
(1) Weighing the elemental raw materials of each metal element according to the stoichiometric ratio of the massive amorphous alloy, placing the elemental raw materials in a crucible according to the sequence of low melting point and high melting point, vacuumizing, introducing argon to-0.08-0.03 Mpa, smelting to form an alloy ingot, cooling, turning over the alloy ingot, and repeatedly smelting for 5-10 to obtain the alloy ingot;
(2) Placing the alloy ingot into a crucible of a pouring system, vacuumizing, introducing argon to 350-400mbar, completely melting the alloy ingot, pouring the alloy ingot into a mold, and cooling and forming.
7. The method of producing a bulk amorphous Fe-Sc-M alloy having high glass-forming ability as defined in claim 6, wherein in the steps (1) and (2), the vacuum is applied to 3.5X10 -3 -5×10 -3 Pa。
8. A method of producing a high glass-forming Fe-Sc-M bulk amorphous alloy according to claim 6, wherein in step (2), the alloy ingot is melted at a current of 200 to 300A, and then the alloy ingot is completely melted at a current of 400 to 500A.
9. Use of a bulk amorphous alloy of Fe-Sc-M with high glass forming ability according to any one of claims 1-5 in the field of preparing magnetic materials.
CN202311699466.0A 2023-12-12 2023-12-12 Fe-Sc-M bulk amorphous alloy with high glass forming capability and preparation method and application thereof Pending CN117721397A (en)

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CN202311699466.0A CN117721397A (en) 2023-12-12 2023-12-12 Fe-Sc-M bulk amorphous alloy with high glass forming capability and preparation method and application thereof

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CN117721397A true CN117721397A (en) 2024-03-19

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