CN113976910A - Method for preparing high-entropy amorphous micro-laminated composite material - Google Patents
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Abstract
The invention belongs to the technical field of composite material preparation, and relates to a method for preparing a high-entropy amorphous micro-laminated composite material, which comprises the steps of respectively filling amorphous alloy powder and high-entropy alloy powder with high toughness into a double-channel supersonic airflow powder conveying device, wherein the amorphous alloy powder is Fe-Cr-Y-Ta-B alloy powder, and the high-entropy alloy powder is Fe-Cr-Co-Ni-Mn-Si alloy powder; the vertical distance between the laser focus and the substrate is 16-30mm, and the laser power is as follows: 250W-550W; adjusting process parameters, and alternately sending out the two kinds of powder through supersonic airflow to finally form the high-entropy amorphous micro-laminated composite material. The invention adopts the special construction method of the micro-laminated composite material, so that the composite material can be used for integrating the advantageous properties of high strength and high toughness of the high-entropy alloy, and simultaneously, the composite material has a large number of interfaces, so that the composite material can be toughened by utilizing various favorable properties of the interfaces, and the comprehensive properties of the composite material are further improved.
Description
Technical Field
The invention belongs to the technical field of composite material preparation, relates to a method for preparing a high-entropy amorphous micro-laminated composite material, and particularly relates to a novel method for preparing a composite material by laser suspension melting and supersonic powder airflow deposition.
Background
The amorphous alloy is used as a novel alloy, is different from the traditional crystal material, has a microstructure with long-range disorder and short-range order, and has the advantages of high strength, high hardness, high wear resistance, good corrosion resistance and the like. However, amorphous alloys are brittle and thus have limited applications. Meanwhile, the preparation of the bulk amorphous alloy is difficult, and the critical dimension of the bulk amorphous alloy is difficult to improve. Particularly, the iron-based amorphous alloy has very high strength and hardness, but due to the limitation of brittleness and forming capability, the iron-based amorphous alloy is mainly used as a soft magnetic functional material in the industrialization of the iron-based amorphous alloy, and the application of excellent mechanical properties of the iron-based amorphous alloy is ignored. In fact, the strength of the iron-based bulk amorphous alloy can exceed 4000MPa, and the strength of the iron-based amorphous soft magnetic alloy can reach more than 3000MPa in industry. Therefore, the higher brittleness and the limitation of the preparation size of the amorphous alloy limit the further application of the amorphous alloy.
The high-entropy alloy is a disordered alloy discovered on the basis of exploring a bulk amorphous alloy in recent years, the most typical structure of the high-entropy alloy is a multi-component super solid solution, the solid solution strengthening effect is extremely strong, and the crystal lattice distortion exists. The unique crystal structure enables the high-entropy alloy to have some excellent performances which cannot be compared with the traditional alloy, such as high strength, high hardness, high room temperature toughness, high wear resistance, high corrosion resistance, high resistance to heat, excellent high temperature resistance and the like. The current research result shows that the fracture toughness of the high-entropy alloy is obviously superior to that of other alloys and is at the highest level of the current known materials.
There is no relevant literature report on the problem of using high-entropy alloy to provide high plasticity as a toughness layer to solve the brittleness of amorphous alloy.
Disclosure of Invention
The purpose of the invention is: the method for preparing the high-entropy amorphous micro-laminated composite material is characterized in that an amorphous layer and a high-entropy layer are alternately deposited on a substrate by controlling powder feeding, melting and deposition positions in a mode of combining laser suspension melting alloy powder and supersonic airflow high-speed deposition, and finally the bulk high-entropy amorphous micro-laminated composite material without size limitation is obtained.
In order to solve the technical problem, the technical scheme of the invention is as follows:
a method for preparing a high-entropy amorphous micro-laminated composite material comprises the steps of respectively filling amorphous alloy powder and high-entropy alloy powder with high toughness into a two-channel supersonic airflow powder conveying device, wherein the amorphous alloy powder is Fe-Cr-Y-Ta-B alloy prefabricated powder, and the high-entropy alloy powder is Fe-Cr-Co-Ni-Mn-Si alloy prefabricated powder;
the vertical distance between the laser focus and the substrate is 16-30mm, and the laser power is as follows: 250W-550W;
adjusting the technological parameters, alternately sending out two powders through a gas flow with supersonic speed:
heating the amorphous alloy powder to a molten state through laser suspension, simultaneously blowing and cooling the amorphous alloy powder to a supercooled liquid state through supersonic airflow in the process of flying to a deposition substrate, and depositing on the substrate to form an amorphous alloy layer;
heating the high-entropy alloy powder to a molten state through laser suspension, and depositing on a substrate to form a high-entropy alloy layer;
and performing alternate deposition in such a way, and finally forming the high-entropy amorphous micro-laminated composite material. The supersonic gas flow is adopted to help the alloy powder (melt) to carry out compact deposition and also help the quenching of the alloy, not only to realize rapid solidification by the heat conduction of a substrate, but also to realize rapid solidificationThe heat load on the substrate is reduced. The room temperature fracture strength of the Fe-Cr-Y-Ta-B amorphous alloy layer is more than or equal to 3500MPa, and the room temperature fracture toughness of the Fe-Cr-Co-Ni-Mn-Si high-entropy alloy layer is more than or equal to 65 MPa-m1/2The design of the material combination can superpose structures with different mechanical properties to obtain an excellent composite effect.
When alternately depositing, the amorphous alloy layer and the high entropy alloy layer have no precedence relationship.
When preparing the amorphous alloy layer, the vertical distance between the laser focus and the substrate is 16-20mm, and the laser power is as follows: 250W to 350W. Adopting the laser power of 250-350W to melt the Fe-Cr-Y-Ta-B amorphous alloy powder, subjecting the powder to a deep supercooling interval in the quenching solidification process, and depositing the powder on a substrate in the supercooling interval to form amorphous alloy; the laser power is too low to melt the alloy powder fully, and too high to cause the melt temperature to be too high, which affects the formation of the amorphous structure.
When the high-entropy alloy layer is prepared, the vertical distance between a laser focus and the substrate is 25-30mm, and the laser power is as follows: 450W to 550W. When the Fe-Cr-Co-Ni-Mn-Si high-entropy alloy powder is melted by laser, the high power of 450W-550W is needed, on one hand, the melting point of the alloy is high, and on the other hand, six elements of Fe, Cr, Co, Ni, Mn and Si are needed to be fully melted and uniformly mixed, so that a high-entropy stable solid solution structure is formed.
The thickness of the high-entropy alloy layer and the amorphous alloy layer is 10-200 mu m. Preferably, the thickness is 30 to 100 μm. The thickness of the layer is 30-100 mu m, so that various toughening modes such as passivation, deflection, bending and the like of cracks can be better promoted, and the micro-laminated composite material has excellent strength and plastic toughness.
The nozzle of the supersonic airflow powder feeding device forms an included angle which is larger than zero degree and smaller than 45 degrees with the laser beam; the size of a light spot at the laser focus is not smaller than the size of the cross section of the powder airflow.
The gas flow is He or N2Or a mixture of one or more of Ar.
The pressure of the gas is relatively adjusted according to the powder feeding amount and the technological requirements of the deposition process, and the range is 0.5-5 MPa. The gas temperature range is 0-600 ℃.
The method is used for depositing for multiple times to form the bulk high-entropy amorphous micro-laminated composite material with a certain thickness.
The invention has the beneficial effects that:
the invention utilizes the idea of the micro-laminated composite material, enables the amorphous alloy to be used as a component of the micro-laminated composite material through the design of the microstructure, and prepares the micro-laminated composite material by utilizing the excellent mechanical property of the amorphous alloy to be matched with other materials. The toughness layer is made of high-entropy alloy with high toughness. The amorphous alloy is used for providing high strength as a strong layer, the high-entropy alloy is used for providing high plasticity as a toughness layer, and the micro-laminated composite material with excellent comprehensive mechanical properties can be prepared. By adopting the design concept, the problem of brittleness of the amorphous alloy can be solved, the limitation of forming capacity of the amorphous alloy can be overcome, and the micro-laminated composite material without size and shape constraints can be prepared.
Specifically, the special construction method of the Fe-Cr-Y-Ta-B amorphous alloy and the Fe-Cr-Co-Ni-Mn-Si high-entropy alloy micro-laminated composite material is adopted, so that the composite material can be used for integrating the advantageous properties of high strength and high toughness of the amorphous alloy, and simultaneously can be toughened by utilizing various favorable properties of the interface due to the large number of interfaces in the composite material, thereby further improving the integrated performance of the composite material. The Fe-Cr-Y-Ta-B amorphous alloy and the Fe-Cr-Co-Ni-Mn-Si high-entropy alloy have better physical and chemical compatibility and can form an interface with good bonding quality.
When the Fe-Cr-Y-Ta-B/Fe-Cr-Co-Ni-Mn-Si micro-laminated composite material is subjected to bending or impact, after cracks are generated, frequent deflection occurs in the process of expansion, not only is the crack expansion path prolonged, but also the deflection direction of the cracks is changed, and the favorable direction is changed into the unfavorable direction. Meanwhile, when the composite material is deformed integrally, the toughness phase of the composite material is subjected to plastic deformation, so that the stress intensity factor of the crack tip is reduced, and the crack propagation resistance is increased. The toughening modes mainly comprise three types: during the crack propagation process of the Fe-Cr-Y-Ta-B amorphous layer, the crack tip meets the Fe-Cr-Co-Ni-Mn-Si toughness layer at the interface, the direction deflects, and a non-planar crack is formed. When the composite material deforms, the volume of the Fe-Cr-Co-Ni-Mn-Si toughness layer increases to form a strain region, and after the crack tip in the Fe-Cr-Y-Ta-B amorphous layer enters the strain region, stress acts on the front edge of the crack tip, so that the stress concentration degree is reduced, and passivation reaction occurs. And thirdly, cracks in the Fe-Cr-Y-Ta-B amorphous layer are prevented by the Fe-Cr-Co-Ni-Mn-Si phase with larger fracture energy in the process of expanding, the phase is bypassed, and the cracks are curled. Therefore, when the thickness of the alloy layer is more than 100 μm, the crack in the amorphous layer can not extend to the high-entropy alloy layer, so that the whole material can be broken, and the toughening effect is not generated in the whole process; and when the thickness of the alloy layer is less than 30 mu m, the preparation difficulty is higher, and the performance of the composite material is not improved along with the reduction of the thickness of the layer.
The high-entropy amorphous micro-laminated composite material is prepared by adopting laser suspension melting supersonic powder airflow deposition, so that on one hand, the amorphous alloy can go through a deep supercooling interval in the quenching solidification process and is deposited on a substrate in the supercooling interval to form the amorphous alloy; on the other hand, the gas velocity is supersonic, and the powder and the melt are driven to move at high speed to impact the substrate to form compressive stress, so that the tensile stress generated by the solidification of the melt is neutralized, and the near-stress-free deposition is realized; moreover, due to the layer-by-layer prepared structure, three-dimensional complex shape forming without size limitation can be finally realized.
Specifically, the present invention has the following advantages:
1. the designed Fe-Cr-Y-Ta-B/Fe-Cr-Co-Ni-Mn-Si micro-laminated composite material can fully utilize the high strength of the Fe-Cr-Y-Ta-B amorphous alloy and the high toughness of the Fe-Cr-Co-Ni-Mn-Si high-entropy alloy, and obtains an excellent composite effect through the structural superposition of different mechanical properties; by reasonably designing the thickness of the alloy layer, cracks can be promoted to generate various toughening modes such as passivation, deflection, bending and the like, and the plasticity and toughness of the material are obviously improved.
2. The adopted preparation method can realize the formation of a complete amorphous structure of Fe-Cr-Y-Ta-B and the formation of a high-entropy stable solid solution structure of Fe-Cr-Co-Ni-Mn-Si, and can form a good bonding interface.
3. By adopting the technical scheme of the invention, the problem of brittleness of the amorphous alloy can be solved, the limit of forming capacity of the amorphous alloy can be broken through, and the micro-laminated composite material without size and shape constraints can be prepared.
Detailed Description
Features of various aspects of embodiments of the invention will be described in detail below. In the following description, well-known structures and techniques are not shown to avoid unnecessarily obscuring the present invention.
The method comprises the following specific steps:
respectively filling amorphous alloy powder and high-entropy alloy powder into a material taking port of a double-channel powder feeding device, and adjusting the powder supply amount and gas pressure in unit time.
And adjusting the relative positions of the powder feeding airflow, the laser beam and the substrate to ensure that the powder feeding airflow and the laser beam form a certain included angle, and the light spot at the laser focus is not smaller than the cross section size of the powder feeding airflow. The laser focus and the powder feeding airflow converge at one point.
And thirdly, opening the powder feeding airflow I, adjusting the gas feeding pressure, simultaneously opening the laser control power supply, melting the amorphous powder flowing at high speed at the laser focus position, and flying to the substrate. In the flying process, the amorphous alloy melt is blown to the supercooled liquid by high-speed airflow, and when the supercooled liquid is deposited on the substrate, the amorphous alloy is rapidly solidified through airflow cooling and substrate heat conduction to form the amorphous alloy.
And opening the powder feeding airflow II, adjusting the gas feeding pressure, and simultaneously opening the laser control power supply, so that the high-entropy powder flowing at high speed is melted at the laser focus position and then flies to the substrate to deposit and form a high-entropy alloy layer.
The amorphous alloy layer deposited on the substrate can be synchronously destressed by utilizing the airflow and the powder particles which move at high speed. The gas flow and the powder particles impact the substrate to generate compressive stress, so that the tensile stress generated by the glass transition of the supercooled liquid can be neutralized or removed. Therefore, the pressure and the speed of the gas can be controlled, the stress state of the amorphous layer can be adjusted, and the near-stress-free state or the stress control can be realized.
And forming the bulk high-entropy amorphous micro-laminated composite material with a certain thickness by multiple alternate deposition.
The gas is He or N2Or one or more of Ar, the pressure of the gas is relatively adjusted according to the powder feeding amount and the technological requirements of the deposition process, and the basic range is 0.5-5 MPa. The gas can be in a cold state, and the temperature can also be increased so as to improve the flight speed of the powder, wherein the temperature range is 0-600 ℃. The included angle between the airflow and the laser beam and the relative position between the airflow and the substrate are relatively adjusted according to the process requirements of the deposition process, the included angle between the airflow and the laser beam is larger than zero degree and smaller than 45 degrees, and the included angle between the airflow and the vertical direction of the laser beam and the substrate is not more than 45 degrees. The spot size at the laser focus is not smaller than the cross section size of the powder airflow, so that all the powder can be fully melted. The laser power is 250W-550W.
The distance between the laser focus position and the substrate deposition position is relatively adjusted according to the process requirement of the deposition process and the performance of the alloy, and the range is 16-30 mm.
The process of the present invention is described in detail below with reference to specific examples.
Example 1:
and respectively filling Fe-Cr-Y-Ta-B amorphous alloy prefabricated powder and Fe-Cr-Co-Ni-Mn-Si high-entropy alloy prefabricated powder into a material taking port of a double-channel powder feeding device, wherein the particle size of the powder is 70-100 mu m, and the thicknesses of a high-entropy alloy layer and an amorphous alloy layer are 50-80 mu m. The preparation method comprises the following specific steps:
1 adjusting the powder supply amount and gas pressure of the amorphous alloy. Firstly, opening gas, determining a gas flow path according to a track form formed by amorphous alloy gas flow, then opening laser, and determining the relative positions of the gas flow, the laser beam and the substrate. The distance between the laser focus and the substrate is 18 mm; laser power: 300W.
2 setting the powder supply temperature at 25 deg.C, gas pressure at 80psi, and the angle between the gas flow and the laser beam at 15 deg.C, which are symmetrically distributed with respect to the substrate vertical direction. Dust suction equipment is arranged beside the sample table for powder recovery.
And 3, opening a powder feeding airflow switch and a laser power switch to deposit. While adjusting the position of the substrate, a plate-like specimen having a width of 15mm and a length of 30mm was formed.
4, adjusting the powder supply amount and the gas pressure of the high-entropy alloy. Firstly, opening gas, determining a gas flow path according to a track form formed by high-entropy alloy gas flow, and then opening laser to determine the relative positions of the gas flow, the laser beam and the substrate. The distance between the laser focus and the substrate is 26 mm; laser power: 500W.
5 setting the powder supply temperature at 25 deg.C, gas pressure at 100psi, and the angle between the gas flow and the laser beam at 20 deg.C, which are symmetrically distributed with respect to the substrate vertical direction. Dust suction equipment is arranged beside the sample table for powder recovery.
And 6, opening a powder feeding airflow switch and a laser power switch, and depositing the high-entropy alloy layer on the deposited amorphous alloy layer. And meanwhile, the position, shape and size of the substrate are adjusted to be consistent with those of the amorphous alloy layer.
And 7, continuously and alternately depositing the amorphous alloy layer and the high-entropy alloy layer, and reducing the height of the substrate every time 6 layers are deposited so as to ensure the effective flying distance between the laser focus and the substrate.
And 8, when the thickness of the deposition layer is 5mm, stopping deposition, taking down the substrate, and separating the deposition layer from the substrate to obtain the high-entropy amorphous micro-laminated composite material part with the width of 15mm, the length of 30mm and the thickness of 5 mm.
The room temperature strength of the prepared Fe-Cr-Y-Ta-B/Fe-Cr-Co-Ni-Mn-Si micro-laminated composite material reaches 3289MPa, the plasticity reaches 15.6 percent, and the comprehensive performance is obviously superior to that of Fe-Cr-Y-Ta-B amorphous alloy (the room temperature strength is 3677MPa, and the plasticity is 2.3 percent).
Claims (10)
1. A method for preparing a high-entropy amorphous micro-laminated composite material is characterized by comprising the following steps: respectively filling amorphous alloy powder and high-entropy alloy powder with high toughness into a double-channel supersonic airflow powder conveying device, wherein the amorphous alloy powder is Fe-Cr-Y-Ta-B alloy prefabricated powder, and the high-entropy alloy powder is Fe-Cr-Co-Ni-Mn-Si alloy prefabricated powder;
the vertical distance between the laser focus and the substrate is 16-30mm, and the laser power is as follows: 250W-550W;
adjusting the technological parameters, alternately sending out two powders through a gas flow with supersonic speed:
heating the amorphous alloy powder to a molten state through laser suspension, simultaneously blowing and cooling the amorphous alloy powder to a supercooled liquid state through supersonic airflow in the process of flying to a deposition substrate, and depositing on the substrate to form an amorphous alloy layer;
heating the high-entropy alloy powder to a molten state through laser suspension, and depositing on a substrate to form a high-entropy alloy layer;
and performing alternate deposition in such a way, and finally forming the high-entropy amorphous micro-laminated composite material.
2. The method of claim 1, wherein: when alternately depositing, the amorphous alloy layer and the high entropy alloy layer have no precedence relationship.
3. The method of claim 1, wherein: when preparing the amorphous alloy layer, the vertical distance between the laser focus and the substrate is 16-20mm, and the laser power is as follows: 250W to 350W.
4. The method of claim 1, wherein: when the high-entropy alloy layer is prepared, the vertical distance between a laser focus and the substrate is 25-30mm, and the laser power is as follows: 450W to 550W.
5. The method of claim 1, wherein: the thickness of the high-entropy alloy layer and the amorphous alloy layer is 10-200 mu m.
6. The method of claim 1, wherein: the nozzle of the supersonic airflow powder feeding device forms an included angle which is larger than zero degree and smaller than 45 degrees with the laser beam; the size of a light spot at the laser focus is not smaller than the size of the cross section of the powder airflow.
7. The method of claim 1, wherein: the gas flow is He or N2Or a mixture of one or more of Ar.
8. The method of claim 1, wherein: the pressure of the gas is relatively adjusted according to the powder feeding amount and the technological requirements of the deposition process, and the range is 0.5-5 MPa.
9. The method of claim 1, wherein: the gas temperature range is 0-600 ℃.
10. The method of claim 1, wherein: the method is used for depositing for multiple times to form the bulk high-entropy amorphous micro-laminated composite material with a certain thickness.
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