CN103252496A - High-entropy alloy powder containing amorphous nanocrystalline and fabrication method thereof - Google Patents
High-entropy alloy powder containing amorphous nanocrystalline and fabrication method thereof Download PDFInfo
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Abstract
The invention relates to high-entropy alloy powder containing amorphous nanocrystalline and a fabrication method thereof. A high-entropy alloy coating is composed of, by atomic percent, 14.3% of Al, 14.3% of Fe, 14.3% of Co, 14.3% of Ni, 14.3% of Cr, 14.3% of Mo and 14.2% of Si, and the total percentage is 100%. The fabrication method includes the following steps: S1, high-entropy alloy master alloy is fabricated through a medium-frequency induction smelting technique, wherein weighed metallic raw materials are put in a carborundum crucible in sequence and according to melting points from low to high, then the carborundum crucible is vacuumized until the pressure is lower than 6.0*10MPa; argon gas is inflated in the carborundum crucible, the metallic raw materials are melted under the condition that the pressure of the argon air is 3*10-2 Pa, the smelting current is 75A, the melting time is 25min, the alloy composition is segregated with the assistance of electromagnetic stirring, the alloy composition is poured into a magnesia framework after the alloy composition is melted completely, and the high-entropy alloy master alloy which is even in ingredients is obtained; S2, high-entropy alloy powdered materials are fabricated through gas atomization equipment. The fabrication method of the high-entropy alloy powder is used for fabricating the high-entropy alloy coating containing the amorphous nanocrystalline or bulk alloy materials of more superior performance.
Description
Technical field
The present invention relates to a kind of amorphous nano-crystalline high-entropy alloy powder and preparation method thereof that contains, can be used for preparing combination property superior high-entropy alloy coating and block materials.
Background technology
High-entropy alloy is a kind of novel alloy system that grows up on the basis of block amorphous alloy, form by being not less than 5 kinds of essential elements, wherein every kind of element all occupies higher percentage, surpass 50% without any a kind of element atomic percent, can be considered the composite on the atomic scale, be easy to form simple solid solution, as cast condition can be separated out nanophase even amorphous phase, make alloy obtain characteristics such as high strength, high rigidity, high corrosion-resistant, high-fire resistance, special electricity, magnetic property, be with a wide range of applications.The aerosolization method is one of main method of preparation metal dust, characteristics such as have the cooldown rate height, powder size is controlled, oxygen content is low, good sphericity, pollution are few.Usually need cooldown rate greater than 10
3During K/s, could keep the metal liquid tissue and form amorphous phase.The present invention organically combines high-entropy alloy characteristic and aerosolization rapid solidification characteristics, makes alloy can separate out nanophase and amorphous phase under less cooldown rate condition.Adopted mechanical alloying method to prepare the high-entropy alloy dusty material at present, but because the powder sphericity of mechanical alloying method preparation is not high, be not suitable for sprayed on material, range of application is narrower, and the high-entropy alloy dusty material that adopts the preparation of aerosolization flash set technology to contain amorphous nano-crystalline does not appear in the newspapers as yet.
Summary of the invention
The object of the present invention is to provide a kind of high-entropy alloy powder that contains amorphous nano-crystalline and preparation method thereof, it is characterized in that alloying component is by waiting atomic percent to form, wherein Al:14.3%, Fe:14.3%, Co:14.3%, Ni:14.3%, Cr:14.3%, Mo:14.3%, Si:14.2%, percent of total is 100%.
Put into the diamond dust crucible successively by fusing point order from low to high, be evacuated to air pressure then and be lower than 6 * 10
-2MPa charges into argon gas, is 3 * 10 in Ar Pressure
-2Begin melting under the Pa condition, the melting electric current is 75A, and smelting time is 25min, introduces electromagnetic agitation to reduce the alloying component segregation.After melting is finished, alloy solution is cast in the magnesia formwork, obtains the uniform high-entropy alloy foundry alloy of composition.
The high-entropy alloy foundry alloy is heated to fusing with the induction coil in the atomization plant, it is overheated to keep, and the formation diameter is the metal liquid stream of 4-6mm, feed nitrogen by nozzle ring simultaneously, stream pressure is 0.4-0.6MPa, and air velocity is 280-300m/s, high velocity air impacts metal liquid stream, destroy the adhesion between metallic atom, airflow kinetic energy is converted into drop surface energy, namely obtain the high-entropy alloy dusty material.
Adopt the preparation of aerosolization flash set technology, less than 10
3Under the cooldown rate condition of K/s, separate out nanophase and amorphous phase, obtaining with simple solid solution is matrix, and nano-crystalline and amorphous is the dusty material of hardening constituent.Powder organization's composition evenly, good fluidity, oxygen content be low, can be used for preparing combination property superior high-entropy alloy coating and block materials.
The complex effect that above-mentioned 7 kinds of essential elements mix the high entropic effect of back generation, distortion of lattice, sluggish diffusion and element performance promotes that alloy has simple solid solution structure, owing to have solution strengthening, precipitation strength, dispersion-strengtherning mechanism, make alloy have higher intensity and hardness.The aerosolization fast solidification technology has higher cooldown rate, can suppress atom diffusion and reallocation, reduces component segregation, improves the alloy solid solution degree, makes that alloy structure and composition are more even.Adopt high pure nitrogen as atomizing medium, avoided the oxidation of molten metal in the atomization process, the high-entropy alloy powder that makes is purer, has avoided environmental pollution simultaneously, and can control powder size by adjusting nitrogen pressure and flow velocity, improves the powder recovery rate.
The present invention has further optimized alloy structure and performance, can obtain the dusty material that different grain size distributes, can prepare the superior high-entropy alloy coating of combination property or powder metallurgical technique prepares the high-entropy alloy block materials by plasma spray technology, give full play to the potential of high-entropy alloy material, widen the range of application of high-entropy alloy.
Description of drawings
Accompanying drawing 1 is the high-entropy alloy dusty material SEM figure of embodiment one
Accompanying drawing 2 is the high-entropy alloy dusty material X ray diffracting spectrum of embodiment one
Accompanying drawing 3 is the high-entropy alloy power applications design sketch of embodiment one
Accompanying drawing 4 is the high-entropy alloy coating XRD collection of illustrative plates of embodiment one
Accompanying drawing 5 is high-entropy alloy coating amorphous phase TEM bright field image, full-resolution picture and the selected diffraction style of embodiment one
Accompanying drawing 6 is high-entropy alloy coating nanophase TEM bright field image, dark field image and the selected diffraction style of embodiment one
The specific embodiment
The present invention realizes by following measure:
Embodiment one:
1) raw material metal that will remove impurity and oxide-film is pressed atomic percent weighings such as near, percent of total is 100%, wherein Al:14.3%, Fe:14.3%, Co:14.3%, Ni:14.3%, Cr:14.3%, Mo:14.3%, Si:14.2%, percent of total is 100%, put into the diamond dust crucible successively by fusing point order from low to high, be evacuated to air pressure then and be lower than 6 * 10
-2MPa charges into argon gas, is 3 * 10 in Ar Pressure
-2Begin melting under the Pa condition, the melting electric current is 75A, and smelting time is 25min, introduces electromagnetic agitation to reduce the alloying component segregation.After melting is finished, alloy solution is cast in the magnesia formwork, obtains the uniform high-entropy alloy foundry alloy of composition.
2) the high-entropy alloy foundry alloy is heated to fusing with the induction coil in the atomization plant, it is overheated to keep, and to form diameter be the metal liquid stream of 4mm, feeds nitrogen by nozzle ring simultaneously, stream pressure is 0.4MPa, air velocity is 280m/s, and high velocity air impacts metal liquid stream, destroys the adhesion between metallic atom, airflow kinetic energy is converted into the drop surface can, namely obtaining the high-entropy alloy dusty material, is high-entropy alloy dusty material SEM figure as Fig. 1, and powder particle is all spherical in shape.Utilizing its phase composition of XRD analysis, is XRD x ray diffraction collection of illustrative plates as Fig. 2, can find the diffraction maximum broadening.Utilize Scherrer formula (wherein constant is got 0.89, λ and got 0.154056nm) to calculate the powder average grain size less than 40nm.
Dusty material obtains particle size range between-200～+ 800 orders through screening, reaches 90% sprayed on material less than the powder particle volume of 70 μ m.Adopt cold spray technique, at the ZM5 magnesium alloy substrate preparation cold spraying coating through the sandblast alligatoring, spray distance 15cm, powder feeding rate 150g/min, 450 ℃ of gas temperatures, gas pressure 3.2MPa, spray time 2min, preparation high-entropy alloy coating layer thickness is 0.3mm, hardness HV
0.2Be 700.The coating structure densification, good with matrix bond, bond strength is 50MPa, coating SEM pattern is as shown in Figure 3.Adopt X-ray diffraction to coating phase composition analyze, the result shows the main simple body-centered cubic structure solid solution of coating, and the diffraction maximum broadening, as shown in Figure 4.Utilizing the tem observation coating, can find that coating contains amorphous phase, is amorphous phase TEM bright field image as Fig. 5 (a), (b) is the amorphous phase high-definition picture, (c) is amorphous phase selected diffraction style, is made up of the donut of disperse, is typical amorphous diffraction pattern.Fig. 6 (a) is nanophase bright field image in the coating, (b) is the nanophase dark field image, (c) is nanophase selected diffraction style, is made up of bright and sharp donut, is the nanocrystalline diffraction pattern of typical case.Utilize the microhardness of HVS-1000 type digital display microhardness testers testing coating to be HV
0.2700.
Embodiment two:
1) raw material metal that will remove impurity and oxide-film is pressed atomic percent weighings such as near, percent of total is 100%, wherein Al:14.3%, Fe:14.3%, Co:14.3%, Ni:14.3%, Cr:14.3%, Mo:14.3%, Si:14.2%, percent of total is 100%, put into the diamond dust crucible successively by fusing point order from low to high, be evacuated to vacuum then and be lower than 6 * 10
-2MPa charges into argon gas, is 3 * 10 in Ar Pressure
-2Begin melting under the Pa condition, the melting electric current is 75A, and smelting time is 25min, introduces electromagnetic agitation to reduce the alloying component segregation.After melting is finished, alloy solution is cast in the magnesia formwork, obtains the uniform high-entropy alloy foundry alloy of composition.
2) the high-entropy alloy foundry alloy is heated to fusing with the induction coil in the atomization plant, it is overheated to keep, and to form diameter be the metal liquid stream of 5mm, feeds nitrogen by nozzle ring simultaneously, and stream pressure is 0.5MPa, air velocity is 290m/s, high velocity air impacts metal liquid stream, destroys the adhesion between metallic atom, and airflow kinetic energy is converted into the drop surface can, namely obtain the high-entropy alloy dusty material, utilize field emission scanning electron microscope similar to embodiment one with XRD diffractometer analysis result.
Dusty material obtains particle size range between-200～+ 800 orders through screening, reaches 90% sprayed on material less than the powder particle volume of 70 μ m.Adopt cold spray technique, at the ZM5 magnesium alloy substrate preparation cold spraying coating through the sandblast alligatoring, spray distance 20cm, powder feeding rate 165g/min, 500 ℃ of gas temperatures, gas pressure 4MPa, spray time 3min, preparation high-entropy alloy coating layer thickness is 0.4mm, hardness HV
0.2Be 718.The coating structure densification, good with matrix bond, bond strength is 62MPa.Utilize the microhardness of HVS-1000 type digital display microhardness testers testing coating to be HV
0.2718.Coating SEM microstructure, XRD diffracting spectrum and transmission electron microscope analysis result are similar to embodiment 1.
Embodiment three:
1) raw material metal that will remove impurity and oxide-film is pressed atomic percent weighings such as near, percent of total is 100%, wherein Al:14.3%, Fe:14.3%, Co:14.3%, Ni:14.3%, Cr:14.3%, Mo:14.3%, Si:14.2%, percent of total is 100%, put into the diamond dust crucible successively by fusing point order from low to high, be evacuated to vacuum then and be lower than 6 * 10
-2MPa charges into argon gas, is 3 * 10 in Ar Pressure
-2Begin melting under the Pa condition, the melting electric current is 75A, and smelting time is 25min, introduces electromagnetic agitation to reduce the alloying component segregation.After melting is finished, alloy solution is cast in the magnesia formwork, obtains the uniform high-entropy alloy foundry alloy of composition.
2) the high-entropy alloy foundry alloy is heated to fusing with the induction coil in the atomization plant, it is overheated to keep, and to form diameter be the metal liquid stream of 6mm, feeds nitrogen by nozzle ring simultaneously, and stream pressure is 0.6MPa, air velocity is 300m/s, high velocity air impacts metal liquid stream, destroys the adhesion between metallic atom, and airflow kinetic energy is converted into the drop surface can, namely obtain the high-entropy alloy dusty material, utilize field emission scanning electron microscope similar to embodiment one with XRD diffractometer analysis result.
Dusty material obtains particle size range between-200～+ 800 orders through screening, reaches 90% sprayed on material less than the powder particle volume of 70 μ m.Adopt cold spray technique, at the ZM5 magnesium alloy substrate preparation cold spraying coating through the sandblast alligatoring, spray distance 25cm, powder feeding rate 180g/min, 600 ℃ of gas temperatures, gas pressure 5MPa, spray time 4min, preparation high-entropy alloy coating layer thickness is 0.5mm, hardness HV
0.2Be 721.8.The coating structure densification, good with matrix bond, bond strength is 70MPa.Utilize the microhardness of HVS-1000 type digital display microhardness testers testing coating to be HV
0.2721.Coating SEM microstructure, XRD diffracting spectrum and transmission electron microscope analysis result are similar to embodiment 1.
Claims (4)
1. one kind contains amorphous nano-crystalline high-entropy alloy powder, it is characterized in that high-entropy alloy powder composition is composed as follows by the nearly atomic percent that waits: Al:14.3%, Fe:14.3%, Co:14.3%, Ni:14.3%, Cr:14.3%, Mo:14.3%, Si:14.2%, percent of total are 100%.
2. the amorphous nano-crystalline high-entropy alloy powder that contains according to claim 1 is characterized in that preparing each pantogen material purity of high-entropy alloy powder all greater than 99.9%.
3. the preparation method who contains amorphous nano-crystalline high-entropy alloy powder according to claim 1 is characterized in that carrying out according to the following steps:
One, adopt the Medium frequency induction smelting technology to prepare the high-entropy alloy foundry alloy, concrete steps are as follows:
1) earlier each raw material metal impurity and oxide-film are removed, press the atomic percent weighing again, percent of total is 100%, wherein Al:14.3%, Fe:14.3%, Co:14.3%, Ni:14.3%, Cr:14.3%, Mo:14.3%, Si:14.2%, and percent of total is 100%;
2) load weighted each raw material metal is put into the diamond dust crucible successively by fusing point order from low to high, be evacuated to air pressure then and be lower than 6.0 * 10
-2MPa;
3) charging into argon gas, is 3 * 10 in Ar Pressure
-2Begin melting under the Pa condition, the melting electric current is 75A, and smelting time is 25min, is aided with electromagnetic agitation and reduces the alloying component segregation, is cast in the magnesia formwork after the fusion fully, obtains the uniform high-entropy alloy foundry alloy of composition;
Two, adopt aerosolization equipment to prepare the high-entropy alloy dusty material, concrete steps are as follows:
The high-entropy alloy foundry alloy of step 1 preparation is heated to fusing with the induction coil in the atomization plant, and it is overheated to keep, and the formation diameter is the metal liquid stream of 4～6mm; Feed nitrogen by nozzle ring, stream pressure is 0.4～0.6MPa, and air velocity is 280～300m/s, namely obtains containing amorphous nano-crystalline high-entropy alloy powder.
4. the application that contains amorphous nano-crystalline high-entropy alloy powder that obtains according to the described method of claim 3 is characterized in that: for the preparation of the high-entropy alloy coating that contains amorphous nano-crystalline or the more excellent block high-entropy alloy material of performance.
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