CN116921652A - Metal reinforced amorphous matrix composite material and preparation method thereof - Google Patents
Metal reinforced amorphous matrix composite material and preparation method thereof Download PDFInfo
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- CN116921652A CN116921652A CN202310880695.6A CN202310880695A CN116921652A CN 116921652 A CN116921652 A CN 116921652A CN 202310880695 A CN202310880695 A CN 202310880695A CN 116921652 A CN116921652 A CN 116921652A
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- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 63
- 239000002184 metal Substances 0.000 title claims abstract description 62
- 239000011159 matrix material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 44
- 239000000956 alloy Substances 0.000 claims abstract description 42
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 38
- 239000000463 material Substances 0.000 claims abstract description 34
- 238000005266 casting Methods 0.000 claims abstract description 25
- 238000000137 annealing Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000003723 Smelting Methods 0.000 claims abstract description 19
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 38
- 229910052721 tungsten Inorganic materials 0.000 claims description 24
- 239000010937 tungsten Substances 0.000 claims description 24
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 12
- 230000003014 reinforcing effect Effects 0.000 claims description 12
- 229910052726 zirconium Inorganic materials 0.000 claims description 12
- 230000009477 glass transition Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 23
- 239000010949 copper Substances 0.000 description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 13
- 229910052802 copper Inorganic materials 0.000 description 13
- 239000007789 gas Substances 0.000 description 12
- 238000005086 pumping Methods 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 7
- 238000011010 flushing procedure Methods 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000009210 therapy by ultrasound Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000004615 ingredient Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000009715 pressure infiltration Methods 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D18/00—Pressure casting; Vacuum casting
- B22D18/06—Vacuum casting, i.e. making use of vacuum to fill the mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D19/00—Casting in, on, or around objects which form part of the product
- B22D19/14—Casting in, on, or around objects which form part of the product the objects being filamentary or particulate in form
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0075—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for rods of limited length
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/10—Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/08—Making alloys containing metallic or non-metallic fibres or filaments by contacting the fibres or filaments with molten metal, e.g. by infiltrating the fibres or filaments placed in a mould
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/10—Refractory metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/14—Alloys containing metallic or non-metallic fibres or filaments characterised by the fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
- C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
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Abstract
The application discloses a metal reinforced amorphous matrix composite material and a preparation method thereof. The metal reinforced amorphous-based composite material comprises a metal reinforced phase material and an amorphous-based alloy substrate. The preparation method comprises the following steps: (1) A cross beam is arranged in the die, and a metal reinforced phase material is hung on the cross beam; (2) Putting a mother alloy ingot serving as an amorphous base alloy substrate into an arc melting and suction casting system, starting an arc in a protective gas atmosphere, melting, and opening a suction casting valve when shaking and rotation of a mother alloy melt are observed; (3) Cooling after smelting suction casting is finished, taking out the amorphous matrix composite material, and adopting high-frequency ultrasonic and/or high-pressure annealing treatment to remove gaps and hollows of the amorphous matrix composite material to obtain the metal reinforced amorphous matrix composite material; the ultrasonic frequency of the high-frequency ultrasonic wave is more than 10000 Hz; the isostatic pressure applied to the amorphous-based composite material in the high-pressure annealing process is more than 3 GPa.
Description
Technical Field
The application relates to the technical field of composite materials, in particular to a metal reinforced amorphous matrix composite material and a preparation method thereof.
Background
The amorphous alloy is a novel metal material obtained from a high-temperature melt through an ultra-fast cooling process, and the microstructure of the amorphous alloy is characterized by long-range disorder and short-range ordered arrangement due to the fact that the amorphous alloy is not cooled. Based on this unique amorphous atomic structure, amorphous alloys exhibit many excellent mechanical properties, such as high toughness, high strength, high elastic strain limit, and good wear resistance. Nowadays, due to the excellent mechanical properties, various amorphous alloy materials are widely applied to various fields, and have wide application prospects in aerospace, electronic information and precision instruments. However, the desire to use amorphous alloys as structural materials also requires overcoming a number of obstacles. For example, the problems of room temperature brittleness, strain softening and the like of amorphous alloys in the deformation process greatly restrict the practical application of the amorphous alloys as structural materials.
In the prior art, researchers propose adding a material capable of enhancing toughness to an amorphous alloy, so that the amorphous alloy has the advantages of high strength, high hardness and high wear resistance of the amorphous alloy and the advantage of high toughness of a tough material, and the novel material is called an amorphous matrix composite material. Various preparation methods have been proposed for amorphous-based composite materials, such as a pressure infiltration method and a stainless steel pipe water quenching method. The pressure infiltration method is to infiltrate the molten amorphous alloy melt into the wrapped material under a certain pressure condition, so that the interface combination condition of the amorphous alloy and the reinforcement can be effectively improved, the internal structure of the obtained composite material is compact, the problem of wrapping gas and inclusion can be avoided by controlling the melting process, and the method is a better method for preparing the amorphous composite material, however, the too slow cooling rate is one of the reasons for crystallizing the amorphous matrix. Meanwhile, the water quenching method of the stainless steel tube also has the problem of limited cooling speed, can directly influence the crystallization behavior of an amorphous base, and cannot ensure the forming size of the obtained composite material. At present, a plurality of problems are solved for preparing the amorphous-based composite material so as to be further applied, and the improvement of the preparation method is particularly important.
Many metal elements have excellent mechanical properties, so metals such as tungsten are commonly selected as reinforcing materials in the preparation of composite materials. The addition of a ductile phase, such as particles, fibers or filaments, to the amorphous matrix to enhance the toughness of the amorphous material is a reinforcing phase that is currently in common use. In particular, the metal reinforced amorphous matrix composite material has high strength, high hardness, wear resistance and other excellent properties, also has very excellent impact resistance and armor piercing performance, and has potential armor application prospect. The amorphous base alloy component selected by the application is Zr 61 Ti 2 Cu 25 Al 12 Amorphous alloys (of course, the application is also applicable to other amorphous alloys), and a great deal of research in the early stage proves that Zr 61 Ti 2 Cu 25 Al 12 The amorphous alloy component has excellent mechanical property and high fracture toughness. However, since there are a large number of voids in the resulting composite between the metal reinforcing phase material and the metal reinforcing phase material, between the metal reinforcing phase material and the amorphous matrix, this also affects the metal reinforcing non-crystalline matrixOne of the important factors of the mechanical properties of the crystal-based composite material.
Impact toughness refers to the ability of a material to absorb plastic deformation work and fracture work under impact load, reflects fine defects and impact resistance inside the material, and reflects the resistance of a metal material to external impact load. Materials with high impact toughness are often used in engineering construction, aerospace, military industry and other fields. Because the amorphous alloy has excellent mechanical properties, a novel amorphous-based composite material is prepared by taking a high-strength metal reinforced phase material as a reinforced material, and the application prospect of the amorphous-based composite material in the aspect of impact toughness can be searched.
In summary, the existing preparation methods of metal reinforced amorphous-based composite materials still face the problems of easy crystallization of amorphous-based alloy materials, introduction of gaps and holes, etc., and the key to solve these problems is to find a new preparation method or to improve the existing process.
Disclosure of Invention
The application provides a preparation method of a metal reinforced amorphous-based composite material, which comprises the steps of hanging a metal reinforced phase material on a cross beam fixed in a die, preparing the metal reinforced amorphous-based composite material by adopting an arc melting and suction casting method, and carrying out specific high-frequency ultrasonic and/or high-pressure annealing treatment on the prepared composite material to finally obtain the amorphous-based composite material with high impact toughness, wherein an amorphous base of the amorphous-based composite material is not easy to crystallize and has no obvious gaps and holes.
A method for preparing a metal reinforced amorphous matrix composite material, wherein the metal reinforced amorphous matrix composite material comprises a metal reinforced phase material and an amorphous matrix alloy substrate;
the preparation method comprises the following steps:
(1) A cross beam is arranged in the die, and a metal reinforced phase material is hung on the cross beam;
(2) Putting a mother alloy ingot serving as an amorphous base alloy substrate into an arc melting and suction casting system, starting an arc in a protective gas atmosphere, melting, and opening a suction casting valve when shaking and rotation of a mother alloy melt are observed;
(3) Cooling after smelting suction casting is finished, taking out the amorphous matrix composite material, and adopting high-frequency ultrasonic and/or high-pressure annealing treatment to remove gaps and hollows of the amorphous matrix composite material to obtain the metal reinforced amorphous matrix composite material; the ultrasonic frequency of the high-frequency ultrasonic wave is more than 10000 Hz; and the isostatic pressure applied to the amorphous-based composite material in the high-pressure annealing process is more than 3 GPa.
In the step (1), the metal reinforcing phase material may be one or a combination of a plurality of metal wires, metal sheets, metal rods, metal plates, etc. Wherein, the thickness of the metal sheet is not more than 0.2mm, the thickness of the metal plate is more than 0.2mm, the diameter of the metal wire is not more than 1mm, and the diameter of the metal rod is more than 1mm.
In one embodiment, in step (1), the metal reinforcement phase material is a metal wire.
The diameter of the metal wire can be 0.1-1 mm, and the length of the metal wire can be 1-10 cm.
The number of wires to be hung may be 1 to 50.
In one embodiment, in step (1), the metal reinforcing phase material is a tungsten reinforcing phase material.
In step (2), the master alloy may be a zirconium-based master alloy, such as Zr 61 Ti 2 Cu 25 Al 12 Etc.
In step (2), the shielding gas may be a rare gas.
In one embodiment, in the step (3), the ultrasonic frequency of the high-frequency ultrasonic wave is 10000-50000 Hz.
In one embodiment, in the step (3), the treatment time of the high-frequency ultrasonic wave is 0.5-2 hours.
In one embodiment, in the step (3), the isostatic pressure applied to the amorphous-based composite material during the high-pressure annealing is 3-10 GPa.
In one embodiment, in step (3), the high pressure anneal is at a temperature of 0.5T g ~0.9T g Wherein T is g Is the glass transition temperature of the amorphous base alloy substrate, and is in units of ℃.
In one embodiment, in the step (3), the high-pressure annealing treatment time is 0.5 to 2 hours.
The application also provides the metal reinforced amorphous matrix composite prepared by the preparation method.
The application aims to solve the problems that amorphous base alloy is easy to crystallize and gaps and holes exist in a metal reinforced amorphous base composite material. The application hangs the metal reinforced phase material on the beam fixed in the mould, adopts the electric arc melting and suction casting method, and solves the problems that the amorphous base alloy in the metal reinforced amorphous base composite material is easy to crystallize, has gaps and holes and the like in the high-frequency ultrasonic and/or high-pressure annealing treatment mode.
Compared with the prior art, the application has the beneficial effects that:
1. compared with the traditional method, the method has the advantages that the arc melting and suction casting method is firstly applied to the preparation of the metal reinforced amorphous matrix composite material, the amorphous matrix of the prepared composite material is amorphous due to the ultra-fast cooling rate, the state of the amorphous matrix alloy in the composite material is only related to the amorphous forming capacity of the amorphous matrix, the method is not influenced by the preparation method, the amorphous composite material with larger size can be prepared, and the crystallization problem of the amorphous matrix is reduced.
2. The high-frequency ultrasonic and high-pressure annealing treatment method adopted by the application can effectively reduce the problems of gaps and holes in the amorphous base caused by rapid cooling casting, and enhance the compactness and mechanical properties of the composite material.
3. The method has the advantages of simple process, easy operation of equipment, low cost and high efficiency, and is convenient for subsequent large-scale industrial production and application.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of tungsten filament and matrix amorphous alloy material in amorphous-based composite material provided in example 1 of the present application;
fig. 2 is an X-ray diffraction (XRD) pattern of a matrix amorphous alloy material in an amorphous-based composite material provided in example 1 of the present application.
Detailed Description
The application will be further elucidated with reference to the drawings and to specific embodiments. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application.
The methods of operation, under which specific conditions are not noted in the examples below, are generally in accordance with conventional conditions, or in accordance with the conditions recommended by the manufacturer.
Example 1
The tungsten filament reinforced amorphous matrix composite material with 15 doped tungsten filaments is prepared.
Step one: zr of the required zirconium-based amorphous alloy 61 Ti 2 Cu 25 Al 12 The ingredients are mixed according to chemical compositions.
Step two: placing the ingredients prepared in the first step into an arc melting and suction casting system; regulating the vacuum degree of the cavity to be below 10Pa by a rough pumping valve, and filling argon gas to ensure that the air pressure of the cavity is 4 multiplied by 10 2 Pa, the rough pumping valve is regulated again to vacuumize, and the above process is repeated for 5 times;
when the vacuum degree of the cavity is reduced to below 5Pa, the rough pumping valve is closed, the electromagnetic valve and the high valve are opened, and the vacuum degree of the cavity is pumped to 5 multiplied by 10 -3 Pa, and then flushing argon shielding gas with the pressure of 0.05 MPa;
adjusting the power of the arc gun to 40W for arcing, gradually increasing the power to 100-120W in the smelting process, avoiding alloy loss caused by overhigh temperature in the smelting process, overturning an alloy ingot for secondary smelting after the primary smelting is completed, and repeating the smelting process for 4 times;
and cooling the alloy in a furnace after smelting is finished, and taking out the master alloy.
Step three: tungsten wire placed on copper mould
The diameter of the tungsten wire is 0.4mm, the length is 6cm, 15 tungsten wires are bundled into a bundle and hung on a beam fixed in a copper die, the tungsten wire and the beam are in a T shape, the tungsten wire is suspended in the copper die, and the copper die is a cylindrical die with the diameter of 5cm and the length of 10cm.
Step four: copper mould suction casting bar
Putting the master alloy ingot prepared in the second step into an arc melting and suction casting system;
adjusting the vacuum degree of the cavity to 1 through the rough pumping valveFilling argon gas under 0Pa to make the pressure of cavity be 4×10 2 Pa, the rough pumping valve is regulated again to vacuumize, and the above process is repeated for 5 times;
when the vacuum degree of the cavity is reduced to below 5Pa, the rough pumping valve is closed, the electromagnetic valve and the high valve are opened, and the vacuum degree of the cavity is pumped to 5 multiplied by 10 -3 Pa, and then flushing argon shielding gas with the pressure of 0.05 MPa;
adjusting the power of the arc gun to 40W for arcing, gradually increasing the power to 100W in the smelting process, keeping for a period of time, and pressing down a suction casting valve when the shake of the melt is observed and the melt rotates rapidly;
and after smelting suction casting is finished, cooling the copper mold and the bar material in the furnace.
Step five: high frequency ultrasonic treatment
Putting the zirconium-based amorphous alloy bar prepared in the step four into a high-frequency ultrasonic container, tightly contacting a bar-shaped sample with the high-frequency ultrasonic container, wherein the ultrasonic frequency is 20000Hz, and the ultrasonic treatment time is 0.5h, so as to obtain the tungsten wire reinforced amorphous composite material with 15 doped tungsten wires.
Characterization of tungsten filament reinforced amorphous matrix composites with 15 doped tungsten filaments.
The zirconium-based amorphous alloy bar subjected to high-frequency ultrasonic treatment in the step five is cut into sections by a diamond cutter, and is tested by a scanning electron microscope, and as shown in the figure 1, tungsten wires are well combined with amorphous bases, and no obvious holes or gaps exist.
X-ray diffraction analysis is carried out on the zirconium-based amorphous alloy bar subjected to high-frequency ultrasonic treatment in the step five, and as a result, as shown in a figure 2, the amorphous base is of an amorphous structure and has no obvious crystallization phenomenon.
The zirconium-based amorphous alloy bar subjected to high-frequency ultrasonic treatment in the step five is subjected to impact toughness performance test, and the result is shown in table 1, and the obtained tungsten wire reinforced amorphous composite material has excellent impact toughness performance, and when the number of doped tungsten wires is 15, the impact toughness is 16J/cm 2 。
Example 2
The tungsten filament reinforced amorphous matrix composite material with the number of the doped tungsten filaments being 25 is prepared.
Step one: zr of the required zirconium-based amorphous alloy 61 Ti 2 Cu 25 Al 12 The ingredients are mixed according to chemical compositions.
Step two: placing the ingredients prepared in the first step into an arc melting and suction casting system; regulating the vacuum degree of the cavity to be below 10Pa by a rough pumping valve, and flushing argon gas to ensure that the air pressure of the cavity is 4 multiplied by 10 2 Pa, the rough pumping valve is regulated again to vacuumize, and the above process is repeated for 5 times;
when the vacuum degree of the cavity is reduced to below 5Pa, the rough pumping valve is closed, the electromagnetic valve and the high valve are opened, and the vacuum degree of the cavity is pumped to 5 multiplied by 10 -3 Pa, and then flushing argon shielding gas with the pressure of 0.05 MPa;
adjusting the power of the arc gun to 40W for arcing, gradually increasing the power to 100-120W in the smelting process, avoiding alloy loss caused by overhigh temperature in the smelting process, overturning an alloy ingot for secondary smelting after the primary smelting is completed, and repeating the smelting process for 4 times;
and cooling the alloy in a furnace after smelting is finished, and taking out the master alloy.
Step three: tungsten wire placed on copper mould
The diameter of the tungsten wire is 0.4mm, the length is 6cm, 25 tungsten wires are bundled into a bundle and hung on a beam fixed in a copper die, the tungsten wire and the beam are in a T shape, the tungsten wire is suspended in the copper die, and the copper die is a cylindrical die, has the diameter of 5cm and the length of 10cm.
Step four: copper mould suction casting bar
Placing the master alloy ingot prepared in the second step into an arc melting and suction casting system;
regulating the vacuum degree of the cavity to be below 10Pa by a rough pumping valve, and flushing argon gas to ensure that the air pressure of the cavity is 4 multiplied by 10 2 Pa, the rough pumping valve is regulated again to vacuumize, and the above process is repeated for 5 times;
when the vacuum degree of the cavity is reduced to below 5Pa, the rough pumping valve is closed, the electromagnetic valve and the high valve are opened, and the vacuum degree of the cavity is pumped to 5 multiplied by 10 -3 Pa, and then flushing argon shielding gas with the pressure of 0.05 MPa;
adjusting the power of the arc gun to 40W for arcing, gradually increasing the power to 100W in the smelting process, keeping for a period of time, and pressing down a suction casting valve when the shake of the melt is observed and the melt rotates rapidly;
and after smelting suction casting is finished, cooling the copper mold and the bar material in the furnace.
Step five: high pressure annealing treatment
Putting the zirconium-based amorphous alloy bar prepared in the fourth step into a high-pressure die, then putting the high-pressure die into a vacuum annealing furnace, and applying an isostatic pressure of 7GPa to a sample in the high-pressure annealing process to obtain Zr 61 Ti 2 Cu 25 Al 12 T of (2) g The high-pressure annealing temperature is 300 ℃ and the high-pressure annealing time is 1h at 350 ℃ to obtain the tungsten filament reinforced amorphous-based composite material with 25 doped tungsten filaments.
Characterization of tungsten filament reinforced amorphous matrix composites with 25 doped tungsten filaments.
The zirconium-based amorphous alloy bar subjected to the high-pressure annealing treatment in the step five is cut into sections by a diamond cutter, and is tested by a scanning electron microscope, so that tungsten wires are well combined with an amorphous base, and no obvious holes or gaps exist;
and (3) carrying out X-ray diffraction analysis on the zirconium-based amorphous alloy bar subjected to the high-pressure annealing treatment in the step five, wherein the amorphous base is an amorphous structure and has no obvious crystallization phenomenon.
Impact toughness performance test was conducted on the zirconium-based amorphous alloy bar subjected to the high-pressure annealing treatment in the step five, and when the number of doped tungsten wires was 25, the impact toughness was 48J/cm as shown in Table 1 2 The impact toughness is far greater than that of 15 doped tungsten wires, which indicates that the impact toughness of the tungsten wire reinforced amorphous-based composite material has a great relationship with the number of doped tungsten wires.
TABLE 1
Examples | Number of tungsten filament dopes (root) | Experimental temperature (. Degree. C.) | Sample size (mm) | Impact toughness (J/cm) 2 ) |
Example 1 | 15 | Room temperature | 5 | 16 |
Example 2 | 25 | Room temperature | 5 | 48 |
As can be seen from the examples 1 and 2, the tungsten wire reinforced amorphous-based composite bar is prepared by adopting an arc melting and water-cooling copper mold suction casting method, then the tungsten wire reinforced amorphous-based composite material is treated by adopting high-frequency ultrasonic and high-pressure annealing, and gaps and holes introduced by the amorphous-based composite material in the suction casting process are removed, so that the tungsten wire reinforced amorphous-based composite material with high impact toughness is prepared.
Further, it is to be understood that various changes and modifications of the present application may be made by those skilled in the art after reading the above description of the application, and that such equivalents are intended to fall within the scope of the application as defined in the appended claims.
Claims (10)
1. The preparation method of the metal reinforced amorphous matrix composite material is characterized in that the metal reinforced amorphous matrix composite material comprises a metal reinforced phase material and an amorphous matrix alloy base material;
the preparation method comprises the following steps:
(1) A cross beam is arranged in the die, and a metal reinforced phase material is hung on the cross beam;
(2) Putting a mother alloy ingot serving as an amorphous base alloy substrate into an arc melting and suction casting system, starting an arc in a protective gas atmosphere, melting, and opening a suction casting valve when shaking and rotation of a mother alloy melt are observed;
(3) Cooling after smelting suction casting is finished, taking out the amorphous matrix composite material, and adopting high-frequency ultrasonic and/or high-pressure annealing treatment to remove gaps and hollows of the amorphous matrix composite material to obtain the metal reinforced amorphous matrix composite material; the ultrasonic frequency of the high-frequency ultrasonic wave is more than 10000 Hz; and the isostatic pressure applied to the amorphous-based composite material in the high-pressure annealing process is more than 3 GPa.
2. The method according to claim 1, wherein in the step (1), the metal reinforcing phase material is one or a combination of a plurality of metal wires, metal sheets, metal rods and metal plates.
3. The method according to claim 2, wherein in the step (1), the thickness of the metal sheet is not more than 0.2mm, the thickness of the metal sheet is more than 0.2mm, the diameter of the metal wire is not more than 1mm, and the diameter of the metal rod is more than 1mm.
4. The method of claim 2, wherein in step (1), the metal reinforcing phase material is a metal wire; the diameter of the metal wire is 0.1-1 mm, and the length is 1-10 cm; the number of the suspended metal wires is 1-50.
5. The method according to any one of claims 1 to 4, wherein in the step (1), the metal reinforcing phase material is a tungsten reinforcing phase material.
6. The method of claim 1, wherein in step (2), the master alloy is a zirconium-based master alloy.
7. The production method according to claim 1, wherein in the step (2), the shielding gas is a rare gas.
8. The method according to claim 1, wherein in the step (3), the ultrasonic frequency of the high-frequency ultrasonic wave is 10000 to 50000Hz, and the treatment time of the high-frequency ultrasonic wave is 0.5 to 2 hours.
9. The method according to claim 1, wherein in the step (3), the isostatic pressure applied to the amorphous-based composite material during the high-pressure annealing is 3 to 10GPa, and the high-pressure annealing is performed at a temperature of 0.5T g ~0.9T g Wherein T is g The glass transition temperature of the amorphous base alloy substrate is unit ℃, and the high-pressure annealing treatment time is 0.5-2 h.
10. The metal-reinforced amorphous-based composite material prepared by the preparation method according to any one of claims 1 to 9.
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