CN109576608B - In-situ generated cladding structure iron-based block amorphous alloy composition and preparation method thereof - Google Patents

In-situ generated cladding structure iron-based block amorphous alloy composition and preparation method thereof Download PDF

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CN109576608B
CN109576608B CN201811353350.0A CN201811353350A CN109576608B CN 109576608 B CN109576608 B CN 109576608B CN 201811353350 A CN201811353350 A CN 201811353350A CN 109576608 B CN109576608 B CN 109576608B
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alloy
cladding
amorphous alloy
melting
iron
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CN109576608A (en
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张志杰
耿遥祥
许俊华
喻利花
鞠洪博
李洁
樊世敏
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Jiangsu University of Science and Technology
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/02Amorphous alloys with iron as the major constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D18/00Pressure casting; Vacuum casting
    • B22D18/04Low pressure casting, i.e. making use of pressures up to a few bars to fill the mould
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D18/00Pressure casting; Vacuum casting
    • B22D18/06Vacuum casting, i.e. making use of vacuum to fill the mould
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D19/00Casting in, on, or around objects which form part of the product
    • B22D19/08Casting in, on, or around objects which form part of the product for building-up linings or coverings, e.g. of anti-frictional metal
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D19/00Casting in, on, or around objects which form part of the product
    • B22D19/16Casting in, on, or around objects which form part of the product for making compound objects cast of two or more different metals, e.g. for making rolls for rolling mills
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/003Making ferrous alloys making amorphous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C33/00Making ferrous alloys
    • C22C33/04Making ferrous alloys by melting
    • C22C33/06Making ferrous alloys by melting using master alloys

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention discloses an in-situ generated cladding structure iron-based block amorphous alloy composition. The composition comprises the following components in percentage by mass: 0-50% of Co, 3-6% of B, 2-5% of Si, 9-16% of Nb, 2-5% of Cu and the balance of iron. The rod-shaped block amorphous alloy with the cladding structure can be prepared by simple master alloy smelting and a copper mold suction casting method. According to the invention, through reasonable component optimization, a large amount of dissolved copper elements in the alloy melt are separated out in the process of solidifying the copper mold suction casting melt and coated on the outer surface of a rod-shaped sample to form a cladding structure of an amorphous core and a copper shell in situ, and the structure overcomes the defect of poor plasticity of the traditional iron-based amorphous alloy. The maximum diameter of the iron-based rod-shaped block amorphous sample with the cladding structure obtained by the invention is 2.5mm, the thickness of the copper cladding shell is 1-30 mu m, the maximum compression strength is 4000MPa, the maximum yield strength is 3800MPa, and the maximum compression plastic deformation rate can reach 5%. Can be applied to high-strength structural members.

Description

In-situ generated cladding structure iron-based block amorphous alloy composition and preparation method thereof
Technical Field
The invention belongs to the technical field of materials, relates to an alloy material, and more particularly relates to an in-situ generated iron-based rod-shaped block amorphous alloy composition with a copper-clad shell structure and a preparation method thereof.
Background
The iron-based amorphous alloy has excellent soft magnetism and mechanical property due to the unique atom disordered structure. In the aspect of soft magnetic performance, the iron-based amorphous alloy has the advantages of low coercive force, high magnetic permeability, low energy loss and the like, and is widely applied to the fields of transformer core materials, transformer cores, sensors and the like. In terms of mechanical properties, the iron-based amorphous alloy has ultrahigh strength (more than 3500MPa) and hardness (Vickers hardness more than 900), but the plastic deformation rate of the iron-based bulk amorphous alloy is extremely low, usually less than 2%, so that the iron-based bulk amorphous alloy cannot be industrially applied.
At present, the means for improving the plasticity of the iron-based amorphous alloy is mainly carried out from the following aspects: element substitution: the Ni element with relatively large Poisson ratio is used for replacing the Fe element in the iron-based amorphous alloy, but the method has limited plastic deformation rate for improving the iron-based amorphous alloy, and the plastic deformation rate is generally within 2%; purifying oxide: by means of B2O3When oxides are purified in vacuum above the melting point of the alloy, the method can effectively improve the plastic deformation capacity of the bulk amorphous alloy, but the method has extremely complex process, needs to be purified at high temperature for a long time (tens of hours), can only obtain the amorphous alloy by a water quenching method, cannot obtain large-size bulk amorphous alloy due to limited cooling speed and amorphous forming capacity of iron-based alloy, generally the diameter of a rod-shaped sample is less than 2mm, and cannot realize large-scale preparation; ③ second phase precipitation method: through reasonable component design, crystal grains are dispersed and precipitated in situ in a rod-shaped amorphous sample while a copper mold is used for suction casting, the method can also greatly improve the forming capacity of the iron-based bulk amorphous alloy, but because the cooling speed of a metal melt in a cavity is uneven in the suction casting process of the copper mold, the uniform distribution of precipitated phases cannot be realized, the method is only limited to the preparation of the bulk amorphous sample with the diameter of about 1mm, after the size is enlarged, a large amount of coarse crystallized phases are precipitated in the center of the sample, and the strength and the plasticity of the alloy are rapidly deteriorated; and fourthly, compounding with additional materials: the method comprises two types, wherein one type is that materials such as a spring or a metal rod and the like are added into a copper die cavity before a copper die is applied for suction casting, so that an alloy melt covers the spring or the metal rod in the suction casting process, and a composite material of the spring or the metal rod and amorphous alloy is finally formed, the plastic deformation capacity of the iron-based amorphous alloy can be improved to a certain extent, but in the suction casting process, the alloy melt and the materials such as the metal rod or the spring cannot be completely wetted, and defects such as holes and the like are easily generated at the interface of the two types of materials, so that the mechanical property of the materials is reduced.The other type is that a layer of metal material is sprayed or electroplated on the surface of the iron-based amorphous alloy bar to form a cladding structure, but the amorphous and shell surface of the material core prepared by the methods has poor bonding force and is easy to fall off.
In conclusion, a simple and effective method for improving the plastic deformation capacity of the iron-based bulk amorphous alloy does not exist in the current stage, and a new idea needs to be developed to improve the plastic deformation capacity of the iron-based bulk amorphous alloy.
Disclosure of Invention
The purpose of the invention is: aiming at the defects of limited plastic deformation capability, complex process and the like of the iron-based amorphous alloy improved by the traditional method, the Fe-Co-B-Si-Nb-Cu bulk amorphous alloy with the in-situ generated cladding structure is prepared by reasonably optimizing components and combining with a simple copper mold suction casting process, and the plastic deformation capability of the iron-based amorphous alloy is effectively improved.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
an iron-based bulk amorphous alloy composition with an in-situ generated cladding structure comprises the following components in percentage by mass: 0-50% of Co, 3-6% of B, 2-5% of Si, 9-16% of Nb, 2-5% of Cu and the balance of Fe, wherein the total mass percentage is 100%.
More preferably, the purity of the Co is more than or equal to 99.9 percent of pure cobalt.
Further preferably, the purity of B is not less than 99.5% of pure boron.
More preferably, the purity of the Si is not less than 99.99% of pure silicon.
Further preferably, the purity of the Nb is more than or equal to 99.95 percent of pure niobium.
More preferably, the purity of the Cu is more than or equal to 99.99 percent of pure copper.
Further preferably, the purity of the Fe is more than or equal to 99.99 percent of pure iron.
A preparation method of an iron-based bulk amorphous alloy composition with an in-situ generated cladding structure comprises the following steps:
step S1: preparing materials: weighing the elementary substances according to the weight percentage of Fe-Co-B-Si-Nb-Cu alloy components, wherein the weight is accurate to 0.001 g in the weighing process;
step S2: smelting a master alloy ingot: mixing the simple substance alloy weighed in the step S1, putting the mixed simple substance alloy into a vacuum melting furnace, wherein the vacuum degree is less than 10Pa, putting the niobium simple substance on the uppermost side of the mixture in the mixing process, then carrying out non-consumable arc melting in a water-cooled copper crucible under the protection of argon or nitrogen, turning an alloy ingot up and down after the first melting is finished, carrying out second melting, and so on, and finally melting the alloy four times to ensure that the mother alloy ingot is uniformly melted; the weight loss of the master alloy ingot after smelting is controlled within 1 percent;
step S3: preparing a rod-shaped block amorphous alloy with a cladding structure: and (2) placing the master alloy ingot in a water-cooled copper crucible with a round hole at the lower part, directly melting the master alloy ingot by electric arc under the protection of argon, then sucking the master alloy ingot into a cylindrical water-cooled copper mold cavity under negative pressure, and rapidly cooling to obtain the iron-based block amorphous with the cylindrical copper cladding structure with the cladding thickness of 1-30 mu m.
The experimental detection means of the invention is as follows:
and carrying out structure detection on the prepared block sample by using an X-ray diffractometer. If the X-ray diffraction pattern shows a diffuse steamed bun peak with typical amorphous characteristics, the alloy is a single amorphous structure and can be confirmed by a transmission electron microscope. Determining thermal parameters of the amorphous sample using a thermal analyzer, comprising: the glass transition temperature, the crystallization temperature, the melting starting temperature and the melting ending temperature are characteristic parameters for representing the thermal stability of the amorphous alloy, and the higher the crystallization temperature is, the stronger the crystallization resistance of the amorphous sample is, and the higher the thermal stability is. The thickness of the copper clad was observed and measured using a metallographic microscope and a scanning electron microscope. The compression mechanical property of the cladding block amorphous sample is tested by using a universal mechanical testing machine, and the method comprises the following steps: compressive strength and plastic deformation rate, the diameter of the rod-shaped sample is 1-2.5mm, and the radial length is 2 times of the diameter.
The invention has the advantages and beneficial effects that:
(1) by reasonable component optimization, the in-situ precipitation of a copper film is realized on the surface of a rodlike block amorphous sample, the Fe-Co-B-Si-Nb-Cu block amorphous alloy with a copper cladding of 1-30 mu m is formed, the plastic deformation rate of the iron-based block amorphous alloy can be effectively improved, the diameter of the obtained cladding structure block amorphous alloy is 1-2.5mm, the maximum compression strength is 4000MPa, the maximum yield strength is 3800MPa, and the maximum compression plastic deformation rate can reach 5%. Compared with the traditional copper mold suction casting method, the plastic deformation rate of the bulk amorphous alloy with the cladding structure obtained by the method can be improved by more than 1 time;
(2) the copper-clad shell iron-based block amorphous alloy can be prepared by simple alloy smelting and copper mold suction casting, and the complexity of preparing the block amorphous alloy by an oxide purification method is overcome;
(3) the copper-clad iron-based bulk amorphous alloy can obtain rod-shaped samples with any diameter as long as the forming capability of the amorphous alloy is allowed in principle, and overcomes the limitation of the size of the bulk amorphous alloy prepared by an oxide purification method and a second-phase precipitation method;
(4) the copper clad shell iron-based bulk amorphous alloy has the advantages that the copper clad shell is precipitated in situ in the process of melt solidification, so that the interface bonding force is strong and the defects are avoided, and the defects that the bulk amorphous alloy prepared by an additional material compounding method has weak bonding force and holes are overcome.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to examples. 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:
firstly, the iron-based amorphous alloy composition comprises the following components in percentage by weight:
Fe82B5Si2Nb9Cu2wherein the purity of Fe is more than or equal to 99.99 percent, the purity of B is more than or equal to 99.5 percent, the purity of Si is more than or equal to 99.99 percent, the purity of Nb is more than or equal to 99.95 percent, and the purity of Cu is more than or equal to 99.99 percent.
Secondly, preparing the iron-based bulk amorphous alloy with the cladding structure:
s1: preparing materials: according to the mass percentage, each element is expressed as Fe82B5Si2Nb9Cu2Weighing the alloy components, wherein the mass is accurate to 0.001 g in the weighing process;
s2: smelting a master alloy ingot: mixing the simple substance alloy weighed in the step S1, putting the mixed simple substance alloy into a vacuum melting furnace, wherein the vacuum degree is less than 10Pa, putting the niobium simple substance on the uppermost side of the mixture in the mixing process, then carrying out non-consumable arc melting in a water-cooled copper crucible under the protection of argon or nitrogen, turning an alloy ingot up and down after the first melting is finished, carrying out second melting, and so on, and finally melting the alloy four times to ensure that the mother alloy ingot is uniformly melted; the weight loss of the master alloy ingot after smelting is controlled within 1 percent;
s3: preparing a rod-shaped block amorphous alloy with a cladding structure: and (2) placing the master alloy ingot in a water-cooled copper crucible with a circular hole at the lower part, directly melting the master alloy ingot by electric arc under the protection of argon, then sucking the master alloy ingot into a cylindrical water-cooled copper mold cavity under negative pressure, and rapidly cooling to obtain the iron-based block amorphous with the cylindrical copper cladding structure with the cladding thickness of 1 mu m.
Third, the mechanical property test and beneficial effects of the embodiment
1. And (3) testing mechanical properties:
carrying out structure detection on the prepared amorphous alloy sample by using an X-ray diffractometer and a transmission electron microscope; observing the thickness of the copper cladding by using a metallographic microscope scanning electron microscope; and (3) detecting the thermal parameters of the amorphous sample by using a thermal analyzer, and testing the compression strength and the plastic deformation rate of the sample by using a universal mechanical testing machine.
2. Has the advantages that:
1) the diameter of the rod-shaped amorphous sample of copper clad obtained by this example was 2.5mm, and the thickness of the copper clad was about 1 μm;
2) the yield strength of the rod-shaped amorphous sample with a copper-clad shell obtained by the example was 3860MPa, and the plastic deformation rate was 1%.
Example 2:
firstly, the iron-based amorphous alloy composition comprises the following components in percentage by weight:
Fe50Co25B5Si3Nb13Cu4wherein the purity of Fe is more than or equal to 99.99 percent, the purity of Co is more than or equal to 99.9 percent, the purity of B is more than or equal to 99.5 percent, the purity of Si is more than or equal to 99.99 percent, the purity of Nb is more than or equal to 99.95 percent, and the purity of Cu is more than or equal to 99.99 percent.
Secondly, preparing the iron-based bulk amorphous alloy with the cladding structure:
same as example 1
Third, the mechanical property test and beneficial effects of the embodiment
1. And (3) testing mechanical properties:
the same as in example 1.
2. Has the advantages that:
1) the diameter of the rod-shaped amorphous sample of copper clad obtained by this example was 1.5mm, and the thickness of the copper clad was about 5 μm;
2) the yield strength of the copper-clad rod-shaped amorphous sample obtained in the example is 3900MPa, and the plastic deformation rate is 3%.
Example 3:
firstly, the iron-based amorphous alloy composition comprises the following components in percentage by weight:
Fe70B6Si4Nb15Cu5wherein the purity of Fe is more than or equal to 99.99 percent, the purity of B is more than or equal to 99.5 percent, the purity of Si is more than or equal to 99.99 percent, the purity of Nb is more than or equal to 99.95 percent, and the purity of Cu is more than or equal to 99.99 percent.
Secondly, preparing the iron-based bulk amorphous alloy with the cladding structure:
same as example 1
Third, the mechanical property test and beneficial effects of the embodiment
1. And (3) testing mechanical properties:
the same as in example 1.
2. Has the advantages that:
1) the diameter of the rod-shaped amorphous sample of the copper clad obtained by this example was 1mm, and the thickness of the copper clad was about 20 μm;
2) the yield strength of the copper-clad rod-shaped amorphous sample obtained by the embodiment is 4000MPa, and the plastic deformation rate is 5%.
The foregoing is only a preferred embodiment of the present invention. The present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore intended that all such equivalent changes and modifications as would be obvious to one skilled in the art be included herein are deemed to be within the scope and spirit of the present invention as defined by the appended claims.

Claims (8)

1. An iron-based bulk amorphous alloy composition with a cladding structure generated in situ is characterized by comprising the following elements in percentage by mass: 0-50% of Co, 3-6% of B, 2-5% of Si, 9-16% of Nb, 2-5% of Cu and the balance of Fe, wherein the total mass percentage is 100%; is prepared by the following steps:
step 1, preparing materials: weighing the elementary substances according to the weight percentage of Fe-Co-B-Si-Nb-Cu alloy components, wherein the weight is accurate to 0.001 g in the weighing process;
step 2, smelting a master alloy ingot: mixing the simple substance alloy weighed in the step one, putting the mixed simple substance alloy into a vacuum melting furnace, putting the Nb simple substance on the uppermost side of the mixture in the mixing process, then carrying out non-consumable arc melting in a water-cooled copper crucible under the protection of argon or nitrogen, turning an alloy ingot up and down after the first melting is finished to carry out second melting, and so on, and finally melting the alloy four times to ensure that the mother alloy ingot is uniformly melted; the weight loss of the master alloy ingot after smelting is controlled within 1 percent;
step 3, preparing the rod-shaped block amorphous alloy with the cladding structure: and (2) placing the master alloy ingot in a water-cooled copper crucible with a round hole at the lower part, directly melting the master alloy ingot by electric arc under the protection of argon, then sucking the master alloy ingot into a cylindrical water-cooled copper mold cavity under negative pressure, and rapidly cooling to obtain the iron-based block amorphous with the cylindrical copper cladding structure, wherein the cladding thickness is 1-30 mu m.
2. The in-situ grown cladding structured fe-based bulk amorphous alloy composition according to claim 1, wherein the Co purity is greater than or equal to 99.9% pure cobalt.
3. The in-situ grown cladding structured fe-based bulk amorphous alloy composition according to claim 1, wherein B has a purity of 99.5% or more pure boron.
4. The in-situ grown cladding structured fe-based bulk amorphous alloy composition according to claim 1, wherein the Si has a purity of 99.99% or more pure Si.
5. The in-situ grown cladding structured fe-based bulk amorphous alloy composition according to claim 1, wherein said Nb has a purity of 99.95% or more pure niobium.
6. The in-situ grown cladding structured fe-based bulk amorphous alloy composition according to claim 1, wherein the Cu has a purity of 99.99% or more pure Cu.
7. The in-situ grown cladding structured Fe-based bulk amorphous alloy composition according to claim 1, wherein the Fe purity is greater than or equal to 99.99% pure Fe.
8. A method of making the in situ cladding structured fe-based bulk amorphous alloy composition according to claim 1, comprising the steps of:
step one, preparing materials: weighing the elementary substances according to the weight percentage of Fe-Co-B-Si-Nb-Cu alloy components, wherein the weight is accurate to 0.001 g in the weighing process;
step two, smelting a master alloy ingot: mixing the simple substance alloy weighed in the step one, putting the mixed simple substance alloy into a vacuum melting furnace, putting the Nb simple substance on the uppermost side of the mixture in the mixing process, then carrying out non-consumable arc melting in a water-cooled copper crucible under the protection of argon or nitrogen, turning an alloy ingot up and down after the first melting is finished to carry out second melting, and so on, and finally melting the alloy four times to ensure that the mother alloy ingot is uniformly melted; the weight loss of the master alloy ingot after smelting is controlled within 1 percent;
step three, preparing the rod-shaped block amorphous alloy with the cladding structure: and (2) placing the master alloy ingot in a water-cooled copper crucible with a round hole at the lower part, directly melting the master alloy ingot by electric arc under the protection of argon, then sucking the master alloy ingot into a cylindrical water-cooled copper mold cavity under negative pressure, and rapidly cooling to obtain the iron-based block amorphous with the cylindrical copper cladding structure, wherein the cladding thickness is 1-30 mu m.
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