CN112575209A - Amorphous preparation method based on crystalline phase-amorphous phase conversion - Google Patents

Amorphous preparation method based on crystalline phase-amorphous phase conversion Download PDF

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CN112575209A
CN112575209A CN202011255805.2A CN202011255805A CN112575209A CN 112575209 A CN112575209 A CN 112575209A CN 202011255805 A CN202011255805 A CN 202011255805A CN 112575209 A CN112575209 A CN 112575209A
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amorphous
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phase
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王楠
韩三轩
杨瑞宁
白杨
姚文静
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Northwestern Polytechnical University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/11Making amorphous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/001Amorphous alloys with Cu as the major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C45/00Amorphous alloys
    • C22C45/10Amorphous alloys with molybdenum, tungsten, niobium, tantalum, titanium, or zirconium or Hf as the major constituent
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F3/00Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C2200/00Crystalline structure
    • C22C2200/02Amorphous

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Abstract

The invention relates to an amorphous preparation method based on crystalline phase-amorphous phase conversion, which adopts a laser melting and fusing technology to obtain an amorphous phase structure from the angle of eutectic growth control. Through cooperative operation, the laser comprises a laser, a three-dimensional platform system and an inert gas protection system, wherein the massive alloy is fixed on an operation platform after being polished and cleaned, the inert gas protection system and the laser are started, and the three-dimensional platform controller controls the motion track of the laser head. The transformation of 'crystal phase-amorphous phase' of the Ni-Nb and Cu-Zr alloy system is successfully and efficiently realized by controlling the corresponding laser power and scanning speed, and an amorphous phase structure is obtained.

Description

Amorphous preparation method based on crystalline phase-amorphous phase conversion
Technical Field
The invention belongs to an amorphous preparation method, and relates to an amorphous preparation method based on crystalline phase-amorphous phase conversion. The method comprises the steps of obtaining an eutectic-amorphous transition interface of an Ni-Nb and Cu-Zr alloy system from the eutectic growth control angle by adopting a laser melting technology through the cooperative operation of a laser, a three-dimensional platform system and an inert gas protection system, and representing the formation of an amorphous phase of the alloy through SEM and TEM.
Background
The amorphous alloy is a metastable metal material with short-range ordered and long-range disordered arrangement of internal structure atoms, has more excellent mechanical properties compared with the traditional crystalline alloy material, has the characteristics of high breaking strength, high hardness, high elastic limit, high corrosion resistance, excellent ferromagnetic property and the like, and shows extremely high application value and potential in various fields of national defense equipment, aerospace, precision machinery, biomedical and sports goods and the like. It is believed that the formation of the amorphous phase is mainly achieved by cooling the liquid metal, i.e. the alloy melt is cooled at a certain cooling rate, and nucleation is inhibited to obtain the amorphous phase. However, since the amorphous forming ability of different alloy systems is different, the difference of critical cooling rates even reaches three to four orders of magnitude, the control of the cooling rate becomes the key for preparing the amorphous, and the preparation conditions are strictly required, which brings great difficulty to the amorphous preparation. Therefore, there is a need for a novel method for preparing amorphous materials, which can more simply and efficiently obtain an amorphous structure.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides an amorphous preparation method based on 'crystalline phase-amorphous phase' conversion, which can successfully and efficiently realize the 'crystalline phase-amorphous phase' conversion of different alloy systems, and the formation of the amorphous phase of the alloy is also represented by SEM and TEM.
Technical scheme
An amorphous preparation method based on 'crystalline phase-amorphous phase' conversion is characterized by comprising the following steps:
step 1: polishing the surface of the cut alloy substrate by using sand paper, cleaning the surface by using acetone and alcohol to ensure that the surface is free from pollution, and fixing the substrate in the center of a three-dimensional platform after the substrate is dried; the thickness of the alloy substrate is more than 2 mm;
step 2: covering an inert gas protective cover on the substrate, enabling the protective cover to be tightly attached to the three-dimensional platform, and starting a switch of an inert gas conveying device to enable the inert gas to fully contact with the substrate and fill the protective cover to form an inert gas environment so as to prevent the substrate from being oxidized at high temperature during processing; keeping for 5min in inert gas atmosphere;
and step 3: starting a water cooling system to enable the laser to normally operate in a heat dissipation water temperature environment; adjusting the output position of the laser beam of the laser to enable the initial beam to be positioned on the boundary of the substrate area, adjusting the focus of the laser, setting the power P value range to be 300W to 500W, enabling the laser focus to be positioned on the surface of the substrate, starting to adjust the numerical control machine tool, and controlling the laser beam to run according to the set scanning track;
and 4, step 4: starting the three-dimensional platform and the laser, enabling the laser head to emit light from a scanning starting point, synchronously moving the laser head at a scanning speed V value range of 30mm/s to 60mm/s according to a given track, automatically closing the laser at a scanning end point, and forming a molten pool on the surface of the substrate along the scanning track;
and 5: after the laser fusing work is finished, closing the laser processing system and the three-dimensional platform system, then closing the inert gas protection system, and finally stopping the water cooling system; the "crystalline phase-amorphous phase" transition is completed.
Argon is selected as the inert gas.
The laser is a high-power solid laser, the maximum output power is 1000W, and the wavelength is 1.06 mu m.
In the step 5, the inert gas is closed and the sample is taken out after the substrate is cooled to the room temperature, so that the sample is prevented from being taken out and oxidized at the high temperature.
The laser working starting point and the laser working end point are more than 1mm away from the edge of the substrate.
Advantageous effects
The invention provides an amorphous preparation method based on crystalline phase-amorphous phase conversion, which adopts a laser melting and fusing technology to obtain an amorphous phase structure from the angle of eutectic growth control. Through cooperative operation, the laser comprises a laser, a three-dimensional platform system and an inert gas protection system, wherein the massive alloy is fixed on an operation platform after being polished and cleaned, the inert gas protection system and the laser are started, and the three-dimensional platform controller controls the motion track of the laser head. The transformation of 'crystal phase-amorphous phase' of the Ni-Nb and Cu-Zr alloy system is successfully and efficiently realized by controlling the corresponding laser power and scanning speed, and an amorphous phase structure is obtained.
The invention provides an amorphous preparation method based on crystal phase-amorphous phase conversion from the aspect of growth control. The principle is as follows: in the process of growing the metal crystal to the liquid phase, the supercooling degree of the liquid-solid interface is increased by continuously increasing the growth speed of the crystal phase interface when the metal crystal reaches the supercooling degree required by forming the amorphous (or is lower than the amorphous forming temperature T)gWhen) is changed from the crystalline phase directly to the amorphous phase. The present invention is accomplished using a laser fusion technique, as shown in fig. 1, which involves applying a high energy laser beam to and sweeping the surface of the sample, causing a thin layer of the surface to rapidly melt and form a molten pool and solidify at a very rapid cooling rate. The local solidification speed inside the molten pool is shown in FIG. 2, wherein Vb is the laser scanning speed, Vs is the local growth speed, and the included angle between the growth direction and the laser scanning speed direction is theta, so that the local growth speed is determined by the relationship between Vs and Vbcos theta. It can be seen that the local growth velocity Vs gradually increases from zero to a maximum value as the angle between the laser scanning velocity Vb and the local growth velocity Vs gradually decreases from the bottom of the molten pool to the surface. On the same scanning track, continuous change of corresponding organization structure when the solidification speed changes in a large range can be observed, and when the solidification speed reaches a certain numerical value, transformation of 'crystalline phase-amorphous phase' can occur, so that an 'eutectic-amorphous' transformation interface and a formed amorphous structure can be observed.
The laser comprises a laser, a water cooling system, a three-dimensional platform system, an inert gas protection system and the like through cooperative operation aiming at the situation, wherein a blocky alloy is fixed on an operation platform after being polished and cleaned, the inert gas protection system and the laser are started, and a three-dimensional platform controller controls the motion track of a laser head. The conversion of 'crystalline phase-amorphous phase' of different alloy systems is successfully and efficiently realized by controlling the corresponding laser power and scanning speed, and the amorphous phase is obtained.
Based on the existing laser melting method, the reasonable remelting region numerical value is selected in the process of melting different alloy systems by single laser, and the shape and the temperature gradient of the molten pool are accurately controlled in real time through linkage and cooperative operation, so that the transformation of a crystal phase-amorphous phase in the molten pool is ensured, and an amorphous phase structure is obtained.
The invention provides an amorphous preparation method for crystal phase-amorphous phase conversion, aiming at alloys with different amorphous forming capacities, and ensuring that each type of alloy has higher cooling rate by adjusting process parameters such as laser power, scanning speed and the like in the laser melting process, so that the crystal phase-amorphous phase conversion and the amorphous phase structure are obtained in a melting pool. And the resulting amorphous structure was verified by SEM and TEM characterization. Compared with the traditional amorphous preparation method (water quenching method, suction casting method, die casting method, single-roller method and the like), the method has the advantages of simplicity, high efficiency, cost saving and the like.
The beneficial effects and characteristics are as follows:
1. from the perspective of eutectic growth control, the laser melting technology can realize the transformation of 'crystalline phase-amorphous phase' and the preparation of amorphous for alloy systems with different amorphous forming abilities. The experimental parameters (laser power and scanning speed) can be accurately and easily controlled, and the experimental conditions are easy to achieve. For preparing the amorphous, the time and the material cost are saved, and certain economic benefit is brought.
2. Selecting proper eutectic alloy, reasonably selecting eutectic composition points of an alloy system through a phase diagram, ensuring the uniformity and accuracy of experimental sample components, knowing the transformation critical growth speed of eutectic-amorphous, and further reasonably selecting laser processing parameters to obtain a larger areaThe amorphous phase structure of (3). Selecting Ni60Nb40And Cu64Zr36The two alloy systems can observe clear 'crystalline phase-amorphous phase' transformation interfaces under different laser processing conditions, and the generation of the amorphous phase is determined by the electron diffraction pattern of a transmission electron microscope, so that the method is proved to successfully realize the transformation of the alloy 'crystalline phase-amorphous phase' and the preparation of the amorphous alloy.
Drawings
FIG. 1: schematic diagram of single-pass laser fusion process
FIG. 2: laser scanning speed V of central longitudinal section of molten poolbAnd local growth velocity VsSchematic diagram of relationship
FIG. 3: (a) a Ni-Nb phase diagram; (b) phase diagram of Cu-Zr
FIG. 4: ni60Nb40Single-laser melting (P300W; V35 mm/s) longitudinal section structure
(a) SEM picture; (b) a TEM image; (c) amorphous electron diffraction ring
FIG. 5: cu64Zr36Single-laser melting (P300W; V60 mm/s) longitudinal section structure
(a) SEM picture; (b) a TEM image; (c) amorphous electron diffraction ring
FIG. 6Cu64Zr36Single-laser melting (P500W; V60 mm/s) longitudinal section structure
(a) SEM picture; (b) a TEM image; (c) an amorphous electron diffraction ring.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
in order to achieve the purpose of the invention, the invention provides a laser melting system for realizing the conversion of crystal phase-amorphous phase of different alloy systems, which comprises a laser, a water cooling system, a three-dimensional platform controller and an inert gas protection system, wherein a blocky alloy is fixed on an operation table after being polished and cleaned, the inert gas protection system is opened to prevent a sample from being oxidized, the laser is started, and the three-dimensional platform controller controls the motion track of a laser head. The technological parameter range of the system is that the laser power is 300W-500W, the spot diameter is 700 mu m-900 mu m, and the scanning speed is 30mm/s-60 mm/s.
An amorphous preparation method for realizing the conversion of a crystalline phase to an amorphous phase on the basis of the existing laser melting method is characterized in that: on the basis of the existing laser melting method, through linkage cooperative operation, a high-power laser beam is used as a heat source, the running track of the laser beam is subjected to three-dimensional control through a high-precision numerical control machine tool, and through adjusting the parameters of a laser and the numerical control machine tool, in the process of melting different alloy systems by a single laser, a reasonable remelting region numerical value is selected, the shape and the temperature gradient of a melting pool are accurately controlled in real time, and the transformation of a crystal phase-an amorphous phase and an amorphous phase structure are obtained inside the melting pool. The laser melting amorphous preparation method with the transformation of 'crystalline phase-amorphous phase' comprises the following specific steps:
step 1: and mechanically cutting the irregular bulk alloy, selecting a position of a region with a proper size, and cutting a substrate with a certain thickness, so that the upper surface and the lower surface are parallel, and carrying out laser fusing on the substrate on the upper surface.
Step 2: and (3) polishing the cut substrate surface by using sand paper, cleaning the substrate surface by using acetone and alcohol to ensure that the surface is free from pollution, and fixing the substrate at the center of the three-dimensional platform after the substrate is dried.
And step 3: covering an inert gas protective cover on the substrate, enabling the protective cover to be tightly attached to the three-dimensional platform, and starting a switch of an inert gas conveying device to enable the inert gas to fully contact with the substrate and fill the protective cover to form an inert gas environment so as to prevent the substrate from being oxidized at high temperature during processing.
And 4, step 4: and starting the water cooling system to enable the laser to normally operate in a specified heat dissipation water temperature environment. Adjusting the output position of the laser beam of the laser to enable the initial beam to be located at the edge position of the substrate, adjusting the focus and the power of the laser at the moment to enable the laser focus to be located on the surface of the substrate, starting to adjust the numerical control machine tool, and controlling the scanning speed and the scanning track of the laser beam.
And 5: after the three-dimensional platform and the laser are ready, the laser head emits light from the scanning starting point, the laser head synchronously moves at a certain scanning speed according to a given track, the laser is automatically closed at the scanning end point, and a molten pool is formed on the surface of the substrate along the scanning track.
Step 6: and after the laser fusing work is finished, closing the laser processing system and the three-dimensional platform system, then closing the inert gas protection system, and finally stopping the water cooling system.
And 7: cutting a laser melting sample from the center of a melting pool along a scanning direction to obtain a longitudinal section of the melting pool, grinding and polishing the longitudinal section by abrasive paper until the surface of the longitudinal section is free of scratches, corroding by using corresponding corrosive liquid, and observing the internal organization structure of the melting pool by using a light mirror and a scanning electron microscope to find an obtained 'crystalline phase-amorphous phase' conversion interface and an obtained amorphous phase region.
In the step 1, the amorphous forming capability and the eutectic-amorphous transition point of the alloy with different components are different, the thickness of the substrate should be larger than 2mm for the same alloy by selecting the components near the eutectic point according to a phase diagram, so as to prevent the substrate from being melted through due to overlarge laser power during processing.
In the step 3, the alloy is easy to be oxidized in the air atmosphere, so that the sample needs to be kept in the inert gas atmosphere for more than 5min before the next step is carried out. And the inert gas is required to be kept introduced in the experiment preparation stage and during the experiment, and argon is selected as the inert gas.
In the step 4, the adopted laser is a high-power solid laser, the maximum output power is 1000W, and the wavelength is 1.06 μm. In order to obtain the crystal phase-amorphous phase transformation and the amorphous phase structure, the laser scanning speed and the laser power need to be adjusted to a reasonable value, and the required values are slightly different for different component alloys according to the higher cooling rate of amorphous formation. Multiple experiments are combined for verification, the laser power P in a specific numerical range is 300W to 500W, and the scanning speed V is 30mm/s to 60 mm/s.
In step 5, the given trajectory is a straight line having a starting point and an ending point on the upper surface of the substrate. When the laser works, the distance between the starting point and the end point of the scanning path and the edge of the substrate is ensured to be more than 1.5mm, so that the platform is prevented from being damaged by the laser.
In the step 6, the inert gas is closed and the sample is taken out after the substrate is cooled to the room temperature, so that the sample is prevented from being taken out and oxidized at the high temperature.
The method comprises the following steps: (1) the irregular bulk alloy was mechanically cut and a substrate having a thickness of 2.5mm was cut out at a position where an area of appropriate size was selected so that the upper and lower surfaces were parallel, and the substrate was laser fused on this upper surface. (2) And (3) polishing the cut substrate surface by using sand paper, cleaning the substrate surface by using acetone and alcohol to ensure that the surface is free from pollution, and fixing the substrate at the center of the three-dimensional platform after the substrate is dried. (3) Covering an inert gas protective cover on the substrate, enabling the protective cover to be tightly attached to the three-dimensional platform, and starting a switch of an inert gas conveying device to enable the inert gas to fully contact with the substrate and fill the protective cover to form an inert gas environment so as to prevent the substrate from being oxidized at high temperature during processing. (4) And starting the water cooling system to enable the laser to normally operate in a specified heat dissipation water temperature environment. Adjusting the output position of the laser beam of the laser to enable the initial beam to be positioned on the boundary of the substrate area, adjusting the focus and the power of the laser at the moment to enable the laser focus to be positioned on the surface of the substrate, starting to adjust the numerical control machine tool, and controlling the scanning speed and the scanning track of the laser beam. (5) After the three-dimensional platform and the laser are ready, the laser head emits light from the scanning starting point, the laser head synchronously moves at a certain scanning speed according to a given track, the laser is automatically closed at the scanning end point, and a molten pool is formed on the surface of the substrate along the scanning track. (6) And after the laser fusing work is finished, closing the laser processing system and the three-dimensional platform system, then closing the inert gas protection system, and finally stopping the water cooling system. (7) Cutting a laser melting sample from the center of a melting pool along a scanning direction to obtain a longitudinal section of the melting pool, grinding and polishing the longitudinal section by abrasive paper until the surface of the longitudinal section is free of scratches, corroding by using corresponding corrosive liquid, and observing the internal organization structure of the melting pool by using an optical lens, a scanning electron microscope and a transmission electron microscope to find an obtained 'crystalline phase-amorphous phase' conversion interface and an obtained amorphous phase region.
According to the phase diagram of Ni-Nb and Cu-Zr (FIG. 3), the substrate composition is selected near the eutectic point composition, and is Ni60Nb40Graph a in FIG. 3; cu64Zr36And b in fig. 3.
Example 1:
step 1: for irregular block Ni59.5Nb40.5The alloy is mechanically cut to a thickness of 2.5mm by selecting the location of the area greater than 10mm in diameter so that the upper and lower surfaces are parallel, and laser fusing the substrate on this upper surface.
Step 2: and (3) polishing the cut substrate surface by using sand paper, cleaning the substrate surface by using acetone and alcohol to ensure that the surface is free from pollution, and fixing the substrate at the center of the three-dimensional platform after the substrate is dried.
And step 3: covering an inert gas protective cover on the substrate, enabling the protective cover to be tightly attached to the three-dimensional platform, and starting a switch of an inert gas conveying device to enable the inert gas to fully contact with the substrate and fill the protective cover to form an inert gas environment so as to prevent the substrate from being oxidized at high temperature during processing.
And 4, step 4: and starting the water cooling system to enable the laser to normally operate in a specified heat dissipation water temperature environment. Adjusting the output position of the laser beam of the laser such that the initial beam is located at the boundary of the substrate area, while adjusting the focal point of the laser such that the focal point of the laser is located on the surface of the substrate, for Ni60Nb40Setting the power of the alloy to be 300W, starting to adjust the numerical control machine tool, and controlling the scanning speed of the laser beam to be 35mm/s and the linear scanning length to be 10 mm; for Cu64Zr36Alloy, set power 300W, and start adjusting the numerically controlled machine tool, controlling the scanning speed of the laser beam to 60mm/s and the linear scanning length to 10 mm. For Cu of the same composition64Zr36Setting the power of an alloy substrate to be 300W, adjusting a numerical control machine tool, and controlling the scanning speed of a laser beam to be 60mm/s and the linear scanning length to be 10 mm.
And 5: after the three-dimensional platform and the laser are ready, the laser head emits light from the scanning starting point, the laser head synchronously moves at a certain scanning speed according to a given track, the laser is automatically closed at the scanning end point, and a molten pool is formed on the surface of the substrate along the scanning track.
Step 6: and after the laser fusing work is finished, closing the laser processing system and the three-dimensional platform system, then closing the inert gas protection system, and finally stopping the water cooling system.
Cutting a laser melting sample from the center of a melting pool along a scanning direction to obtain a longitudinal section of the melting pool, grinding and polishing the longitudinal section of the melting pool by sand paper until the surface of the melting pool is free of scratches, corroding the longitudinal section for 20s by using hydrofluoric acid corrosive liquid, and observing the organization structure inside the melting pool by scanning and a transmission electron microscope (figure 4) to find an obtained 'crystalline phase-amorphous phase' conversion interface and an obtained amorphous phase region.
Example 2:
step 1: for irregular bulk Cu64Zr36The alloy is mechanically cut to a thickness of 2.5mm by selecting the location of the area greater than 10mm in diameter so that the upper and lower surfaces are parallel, and laser fusing the substrate on this upper surface.
Step 2: and (3) polishing the cut substrate surface by using sand paper, cleaning the substrate surface by using acetone and alcohol to ensure that the surface is free from pollution, and fixing the substrate at the center of the three-dimensional platform after the substrate is dried.
And step 3: covering an inert gas protective cover on the substrate, enabling the protective cover to be tightly attached to the three-dimensional platform, and starting a switch of an inert gas conveying device to enable the inert gas to fully contact with the substrate and fill the protective cover to form an inert gas environment so as to prevent the substrate from being oxidized at high temperature during processing.
And 4, step 4: and starting the water cooling system to enable the laser to normally operate in a specified heat dissipation water temperature environment. Adjusting the output position of the laser beam of the laser such that the initial beam is located at the boundary of the substrate area, while adjusting the focal point of the laser such that the focal point of the laser is located on the surface of the substrate, for Ni60Nb40Setting the power of the alloy to be 300W, starting to adjust the numerical control machine tool, and controlling the scanning speed of the laser beam to be 35mm/s and the linear scanning length to be 10 mm; for Cu64Zr36Alloy, arrangementThe power is 300W, and the numerically controlled machine tool is started to adjust, the scanning speed of the laser beam is controlled to be 60mm/s, and the linear scanning length is controlled to be 10 mm. For Cu of the same composition64Zr36Setting the power of an alloy substrate to be 300W, adjusting a numerical control machine tool, and controlling the scanning speed of a laser beam to be 60mm/s and the linear scanning length to be 10 mm.
And 5: after the three-dimensional platform and the laser are ready, the laser head emits light from the scanning starting point, the laser head synchronously moves at a certain scanning speed according to a given track, the laser is automatically closed at the scanning end point, and a molten pool is formed on the surface of the substrate along the scanning track.
Step 6: and after the laser fusing work is finished, closing the laser processing system and the three-dimensional platform system, then closing the inert gas protection system, and finally stopping the water cooling system.
Cutting a laser melting sample from the center of a melting pool along a scanning direction to obtain a longitudinal section of the melting pool, grinding and polishing the longitudinal section of the melting pool by sand paper until the surface of the melting pool is free of scratches, corroding the longitudinal section for 20s by using hydrofluoric acid corrosive liquid, and observing the organization structure inside the melting pool by scanning and a transmission electron microscope (figure 5) to find an obtained 'crystalline phase-amorphous phase' conversion interface and an obtained amorphous phase region.
Example 3: the same operation was carried out with the material of example 2, except that the conditions were not changed, with the laser power being changed to 500W, in which a laser-fused sample was cut from the center of the molten pool in the scanning direction to obtain a longitudinal section of the molten pool, after sanding and polishing until the surface was free from scratches, the molten pool was etched with a hydrofluoric acid etching solution for 20s, and the microstructure inside the molten pool was observed by scanning and transmission electron microscopy (fig. 6), and the resulting "crystalline phase-amorphous phase" transition interface and amorphous phase region were found.
The invention successfully obtains Ni based on the transformation of 'crystalline phase-amorphous phase' of the alloy by a laser melting technology60Nb40And Cu64Zr36A "eutectic-amorphous" transition interface, and an amorphous phase. Selecting corresponding eutectic composition point, fusing on a substrate with thickness of 2.5mm, treating the molten pool, and adding Ni60Nb40In a sampleIt is clearly observed that as the growth rate increases, the structure undergoes a "matrix phase-lamellar eutectic phase-amorphous phase" transition and an amorphous phase is produced uppermost (fig. 4). Processing Cu with laser power of 300W and 500W and scanning speed of 60mm/s64Zr36The transition interface of "crystalline phase-amorphous phase" was also observed in the sample, respectively, and the amorphous phase was also generated in the region above the crystalline phase (fig. 5-6), confirming that the method successfully achieved the transition of alloy "crystalline phase-amorphous phase" and the preparation of amorphous.

Claims (5)

1. An amorphous preparation method based on 'crystalline phase-amorphous phase' conversion is characterized by comprising the following steps:
step 1: polishing the surface of the cut alloy substrate by using sand paper, cleaning the surface by using acetone and alcohol to ensure that the surface is free from pollution, and fixing the substrate in the center of a three-dimensional platform after the substrate is dried; the thickness of the alloy substrate is more than 2 mm;
step 2: covering an inert gas protective cover on the substrate, enabling the protective cover to be tightly attached to the three-dimensional platform, and starting a switch of an inert gas conveying device to enable the inert gas to fully contact with the substrate and fill the protective cover to form an inert gas environment so as to prevent the substrate from being oxidized at high temperature during processing; keeping for 5min in inert gas atmosphere;
and step 3: starting a water cooling system to enable the laser to normally operate in a heat dissipation water temperature environment; adjusting the output position of the laser beam of the laser to enable the initial beam to be positioned on the boundary of the substrate area, adjusting the focus of the laser, setting the power P value range to be 300W to 500W, enabling the laser focus to be positioned on the surface of the substrate, starting to adjust the numerical control machine tool, and controlling the laser beam to run according to the set scanning track;
and 4, step 4: starting the three-dimensional platform and the laser, enabling the laser head to emit light from a scanning starting point, synchronously moving the laser head at a scanning speed V value range of 30mm/s to 60mm/s according to a given track, automatically closing the laser at a scanning end point, and forming a molten pool on the surface of the substrate along the scanning track;
and 5: after the laser fusing work is finished, closing the laser processing system and the three-dimensional platform system, then closing the inert gas protection system, and finally stopping the water cooling system; the "crystalline phase-amorphous phase" transition is completed.
2. An amorphous preparation method based on "crystalline phase-amorphous phase" transition as claimed in claim 1, characterized in that: argon is selected as the inert gas.
3. An amorphous preparation method based on "crystalline phase-amorphous phase" transition as claimed in claim 1, characterized in that: the laser is a high-power solid laser, the maximum output power is 1000W, and the wavelength is 1.06 mu m.
4. An amorphous preparation method based on "crystalline phase-amorphous phase" transition as claimed in claim 1, characterized in that: in the step 5, the inert gas is closed and the sample is taken out after the substrate is cooled to the room temperature, so that the sample is prevented from being taken out and oxidized at the high temperature.
5. An amorphous preparation method based on "crystalline phase-amorphous phase" transition as claimed in claim 1, characterized in that: the laser working starting point and the laser working end point are more than 1mm away from the edge of the substrate.
CN202011255805.2A 2020-11-11 2020-11-11 Amorphous preparation method based on crystalline phase-amorphous phase conversion Pending CN112575209A (en)

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