CN112658221B - Continuous casting method of high-entropy alloy - Google Patents
Continuous casting method of high-entropy alloy Download PDFInfo
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Abstract
A continuous casting method of high-entropy alloy comprises the steps of firstly, carrying out high-energy ball milling on five or more metal element powders with equal molar ratio to enable the element powders to be uniformly mixed and mechanically alloyed, then loading the powders subjected to the high-energy ball milling into a hot-pressing die, electrifying the die and applying pressure to enable plasma discharge to occur among powder particles and further enable the powder to be melted, continuously extruding a molten liquid phase out of the die under the action of the pressure, and cooling to obtain a high-entropy alloy solid; the multi-component powder particles discharge in the grain boundary to form a liquid phase, the liquid phase is formed by extrusion and then is continuously cast to form a high-entropy alloy solid, and the problems that impurities are easily formed by a liquid phase method and the densification is difficult to realize by a powder method in a high-entropy alloy preparation method are solved.
Description
Technical Field
The invention relates to the technical field of alloy preparation, in particular to a continuous casting method of a high-entropy alloy, and particularly relates to a method for promoting powder to be melted by grain boundary discharge of powder, extruding powder melt under certain pressure and casting the powder while extruding.
Background
In 2004, the high-entropy alloy concept breaks through a metal material design framework taking a single element as a principal element, provides a brand-new idea for the development of materials, greatly expands the variety of the materials, and creates a new alloy system. Although the high-entropy alloy has a plurality of principal elements, the high-entropy alloy has high-performance phase compositions such as a simple solid solution phase, a nanoparticle dispersed phase and an amorphous phase. The structural characteristic of the structure enables the high-entropy alloy to have excellent performances such as high hardness, high strength, high corrosion resistance, high-temperature oxidation resistance and the like which are incomparable with the traditional alloy material.
The continuous development of science and technology puts higher requirements on the material performance. The appearance of the high-entropy alloy can break through the performance limit of the material and meet the higher requirements of people on the performance of the material. The high-entropy alloy has simple preparation process, low price, excellent performance and wide potential application value and application prospect, such as high-hardness, wear-resistant and corrosion-resistant grinding tools and tools, a hitting surface steel pipe of a golf club head and a hard surface of a rolling barrel, a magnetic core of a high-frequency transformer and a motor, a magnetic head, a magnetic disk, a magnetic shielding component, a turbine blade, a welding material, a heat exchanger, a heat-resistant component of a high-temperature resistant furnace and the like. The perfection of the preparation process of the high-entropy alloy can furthest increase the application potential of the high-entropy alloy and expand the application range of the high-entropy alloy. Therefore, research on the preparation process of the high-entropy alloy can undoubtedly play an important role in promoting and improving processing and manufacturing, aerospace and daily life.
At present, the preparation method of the high-entropy alloy mainly comprises electric arc melting, high-energy ball milling, powder metallurgy, laser cladding, magnetron sputtering and the like. The methods are not different from the traditional method for preparing the metal material, but when the method is used for preparing the high-entropy alloy, impurities are mixed in a liquid phase method due to the difference of atomic radius, melting point, electronegativity and the like among main elements of metal elements, and the phenomenon that the solid phase method cannot be completely densified exists.
The arc melting method is that all the components of the alloy are completely mixed in liquid state and then solidified in a water-cooled copper crucible. Melting is generally repeated several times to ensure chemical uniformity of the alloy, and the alloy ingot obtained by melting is in a button shape. The high-entropy alloy prepared by arc melting has the problem of uneven component segregation caused by the high and low difference of the melting point of each element, and can not be completely eliminated by melting for multiple times. The alloy block obtained by smelting has small volume, needs to be smelted for many times, has low efficiency and cannot efficiently prepare high-entropy alloy products.
Mechanical alloying is a powder preparation technique in which powder is subjected to repeated deformation, cold welding and crushing by a high-energy ball milling process to obtain alloyed powder. Almost all materials can be produced by this method and mechanical alloying is usually carried out at room temperature or below, avoiding possible element volatilization from melting and casting processes. However, the mechanical alloying method is only the first step of preparing the powder, and then the material needs to be densified by hot-press sintering or the like. However, the sintering temperature is generally lower than the melting point during the sintering process, and sintering in a solid phase causes a problem that densification cannot be performed.
High-entropy alloy materials are ideal materials under extreme conditions, and most of the reported manufacturing methods at present have the defects of easy formation of inclusions and difficult densification by a powder method. The existence of the defects causes the application of the high-entropy alloy material to be limited, and only the high-entropy alloy material can be in a test stage.
The arc melting method commonly used in the preparation of high-entropy alloys is to heat the powder above its melting point by electric arc so that it can be mixed in the liquid phase. However, the high-entropy alloy prepared by the method is uneven in components, and the phenomenon of uneven components is caused due to large melting point difference and different cooling rates among elements. The other preparation method of the high-entropy alloy is cold pressing after mechanical alloying, although the method can avoid component segregation caused by different melting points in the liquid phase solidification process, the subsequent steps of the method are sintered and compacted under a solid phase, and the phenomenon that the densification cannot be realized or more impurities exist.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a continuous casting method of a high-entropy alloy, which is characterized in that a high-purity high-compactness high-entropy alloy sheet is obtained by utilizing grain boundary discharge of mixed powder under plasma, assisting in melting metal powder grain boundaries at high pressure, extruding the melted metal powder grain boundaries under the action of high-pressure extrusion to form a liquid flow, and then continuously casting; the invention relates to a method for carrying out extrusion and casting while discharging grain boundaries under plasma, which solves the problems that liquid-phase preparation components are not uniformly distributed and powder preparation cannot be densified in the preparation process of high-entropy alloy.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a continuous casting method of high-entropy alloy comprises the following steps:
firstly, five or more pure metal powders with the particle size of 10-300 mu m are mixed in an equal molar ratio or a nearly equal molar ratio, wherein the nearly equal molar ratio means that the molar ratio of each component accounts for 5-35mol% of the total amount, and the pure metal powders comprise copper powder, iron powder, nickel powder, chromium powder, aluminum powder, vanadium powder, molybdenum powder, manganese powder, cobalt powder, zinc powder, zirconium powder and tin powder; then carrying out high-energy ball milling on the mixed metal powder to mechanically alloy the powder; and finally, melting the mechanically alloyed powder by a plasma discharge method, applying pressure to extrude the powder while casting the powder, and obtaining the sheet high-entropy alloy.
The high-energy ball milling mode is as follows: five or more mixed metal powders are put into a high-energy ball milling tank body, the mass ratio of ball materials is 2:1-80:1, the filling coefficient is 0.2-0.8, the ball milling tank body is vacuumized or filled with argon and nitrogen protective gas, and the high-energy ball milling is carried out for 0.5-40 hours.
The process of extruding and casting the edges comprises the following steps: and (3) putting the mechanically alloyed powder into a die, heating the die by adopting discharge plasma, heating the die to a temperature 20-2000 ℃ lower than the melting point of the high-entropy alloy powder, preserving the heat, then extruding and casting the melted metal powder under the pressure of 0.5-30MPa to obtain the high-entropy alloy material, and designing a cutter at a finished product outlet to manufacture the material into a required size and shape.
The powder of mechanical alloying is put into the mould, and the mould structure is: the powder raw material is placed in the die cavity, the upper pressing head and the lower pressing head are arranged at two ends of the die and are respectively communicated with a positive electrode and a negative electrode, the upper pressing head and the lower pressing head are heated by adopting discharge plasma, the lower pressing head is provided with a finished product outlet, and when the upper pressing head applies pressure, the material can be extruded from the finished product outlet of the lower pressing head.
The invention has the advantages that:
the invention adopts a plasma heating mode to ensure that the powder is discharged in the grain boundary to achieve the purpose of melting, then utilizes the pressure to extrude the molten liquid phase, and the rest part continuously generates liquid flow to achieve the effect of extruding and casting simultaneously so as to prepare the high-entropy alloy.
The invention overcomes the problems of easy formation of inclusions, non-uniform components and difficult densification of a powder method in the existing liquid phase method in the preparation process of the high-entropy alloy, and is a new process technology: discharging the powder grain boundary to form a liquid phase, and performing high-pressure extrusion to form a liquid flow and further performing continuous casting.
Drawings
Fig. 1 is a schematic view of a mold structure involved in the present invention.
FIG. 2 is a gold phase diagram of the morphology of a product of the example.
FIG. 3 is a composition diagram of different time phases of the high-entropy alloy powder ball milling.
FIG. 4 is a gold phase diagram of the morphology of the six products of the example.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Referring to fig. 1, the mechanically alloyed powder according to the present invention is charged into a mold and heated by a discharge plasma, and the mold has a structure of: the powder raw material is placed in the die cavity, the upper pressing head and the lower pressing head are arranged at two ends of the die and are respectively communicated with a positive electrode and a negative electrode, the upper pressing head and the lower pressing head are heated by adopting discharge plasma, the lower pressing head is provided with a finished product outlet, and when the upper pressing head applies pressure, the material can be extruded from the finished product outlet of the lower pressing head. The same mold was used for each of the following examples.
Example one
The steps of this embodiment are:
20g of 20-micrometer powder with equal molar ratio, namely, aluminum powder, iron powder, nickel powder, chromium powder and vanadium powder, with particle size of 45-300 micrometers are placed into a vibration type ball milling tank for high-energy ball milling, the ball milling tank is vacuumized to be less than 100Pa, the filling coefficient of the ball milling tank is set to be 0.75, the ball-material ratio is 10:1, and the ball milling time is 3 hours; the ball-milled powder is obtained.
50g of mechanically alloyed high-entropy alloy powder is filled into a graphite die with the inner diameter of 300mm, the powder is loosely filled and leveled, the graphite die is heated to the temperature of 980-1100 ℃ in a discharge plasma furnace, the melting point of the high-entropy alloy is higher than 1200 ℃, an implementation device is shown in figure 1, the temperature is kept for 0.5 hour at the temperature, pressure is applied to the melt in the heat preservation process, the pressure is about 30MPa, so that the liquefied powder is extruded out of the die in time, and a sample is collected.
The effect is as follows: referring to fig. 2, it can be seen that the product obtained in this example is dense, free of defects such as voids, free of composition segregation, and uniform in phase distribution. FIG. 3 is a composition diagram of different time phases of the high-entropy alloy powder ball milling. The hardness of the product can reach 1850 HV.
Example two
The steps of this embodiment are:
putting 35% of nickel powder, 15% of iron powder, 2% of aluminum powder, 20% of copper powder and 28% of manganese powder in a planetary ball milling tank for high-energy ball milling, wherein the particle size of each element is 150-350 mu m, filling argon gas into the ball milling tank as protective gas, setting the filling coefficient of the ball milling tank to be 0.5, the ball-material ratio to be 60:1, the rotating speed to be 200rpm and the ball milling time to be 40 hours, and obtaining the ball-milled high-entropy alloy powder.
The ball-milled high-entropy alloy powder is filled into a square-hole graphite die with an inner hole of 200 x 150mm, the die and the diamond powder are heated to about 850-960 ℃, the lowest melting temperature of the high-entropy alloy is 1000 ℃, the pressure of a pressure head is increased to 20MPa in the process of heat preservation for 0.5 hour at the temperature, then the liquid-phase powder extruded along with the pressure head is collected, and the extruded liquid phase is conveyed through a furnace body conveyor belt to be a next liquid-phase emptying position.
The effect is as follows: the product obtained in the embodiment is compact, has no defects such as holes and the like, and has uniform phase distribution.
EXAMPLE III
The steps of this embodiment are:
2kg of aluminum powder, copper powder, iron powder, chromium powder, cobalt powder and manganese powder with equal molar ratio and particle size of 45-300 mu m are put into a stirring type ball milling tank for high-energy ball milling, argon is filled into the ball milling tank as protective gas, the filling coefficient of the ball milling tank is set to be 0.3, the ball-material ratio is 5:1, the stirring speed is 500rpm, and the ball milling time is 2 hours, so that the ball-milled high-entropy alloy powder is obtained.
The ball-milled high-entropy alloy powder is filled into the lower part of a graphite die with the inner diameter of 200mm, the die and the graphite powder are heated in a vacuum furnace to the temperature of 980-1060 ℃, the temperature is kept for half an hour, the pressure of a pressure head is increased to 20MPa in the process of keeping the temperature for 0.5 hour, then the liquid-phase powder extruded along with the pressure head is collected, the extruded liquid phase is conveyed through a furnace body conveyor belt and is emptied to the next liquid-phase position, and therefore the high-entropy alloy material is continuously obtained.
The effect is as follows: the product obtained in the embodiment is compact, has no defects such as holes and the like, and has uniform phase distribution.
Example four
The steps of this embodiment are:
putting iron powder, chromium powder, copper powder, aluminum powder and nickel powder with the particle size of 74-150 mu m and the molar ratio of 15-35% into a planetary ball milling tank, carrying out high-energy ball milling, vacuumizing the ball milling tank to be less than 100Pa, setting the filling coefficient of the ball milling tank to be 0.6, setting the ball-material ratio to be 15:1, the rotating speed to be 200rpm and the ball milling time to be 20 hours; and obtaining the high-entropy alloy powder after ball milling.
The ball-milled high-entropy alloy powder is filled into the lower part of a graphite die with the inner diameter of 200mm, the die and the graphite powder are heated in a vacuum furnace to the temperature of 980-1060 ℃, the temperature is kept for half an hour at the temperature, the pressure of a pressure head is increased to 20MPa in the process of keeping the temperature for 0.5 hour at the temperature, then the liquid-phase powder extruded along with the pressure head is collected, the extruded liquid phase is conveyed through a furnace body conveyor belt and is emptied to the next liquid-phase position, and therefore the high-entropy alloy material is continuously obtained.
The effect is as follows: the product obtained by the embodiment has no composition segregation, is compact, has no defects such as holes and the like, and has uniform phase distribution.
EXAMPLE five
The steps of this embodiment are:
mixing aluminum powder, iron powder, copper powder, manganese powder and cobalt powder with the particle size of 100-; and obtaining the high-entropy alloy powder after ball milling.
The ball-milled high-entropy alloy powder is filled into the lower part of a graphite die with the inner diameter of 200mm, the die and the graphite powder are heated in a vacuum furnace to the temperature of 980-1060 ℃, the temperature is kept for half an hour at the temperature, the pressure of a pressure head is increased to 20MPa in the process of keeping the temperature for 0.5 hour at the temperature, then the liquid-phase powder extruded along with the pressure head is collected, the extruded liquid phase is conveyed through a furnace body conveyor belt and is emptied to the next liquid-phase position, and therefore the high-entropy alloy material is continuously obtained.
The effect is as follows: the product obtained in the embodiment is compact, has no defects such as holes and the like, and has uniform phase distribution.
EXAMPLE six
The steps of this embodiment are:
mixing 17% of aluminum powder, 20% of iron powder, 24% of chromium powder, 49% of nickel powder and 5% of vanadium powder in molar ratio, putting the mixed powder into a planetary ball milling tank, carrying out high-energy ball milling, vacuumizing the ball milling tank to be less than 100Pa, setting the filling coefficient of the ball milling tank to be 0.6, setting the ball-material ratio to be 15:1, rotating speed to be 200rpm, and ball milling time to be 40 hours; and obtaining the high-entropy alloy powder after ball milling.
The ball-milled high-entropy alloy powder is filled into the lower part of a graphite die with the inner diameter of 200mm, the die and the graphite powder are heated in a vacuum furnace to the temperature of 1000-1200 ℃, the temperature is kept for 15 minutes, the pressure of a pressure head is increased to 25MPa in the process of keeping the temperature for 0.5 hour, then the liquid-phase powder extruded along with the pressure head is collected, the extruded liquid phase is conveyed through a furnace body conveyor belt to empty the position for the next liquid phase, and therefore the high-entropy alloy material is continuously obtained.
The effect is as follows: referring to fig. 4, it can be seen that the product obtained in this example is dense, free from defects such as voids, and uniform in phase distribution. The hardness of the product can reach 881.1 HV.
Claims (1)
1. A continuous casting method of a high-entropy alloy is characterized by comprising the following steps:
firstly, five or more pure metal powders with the particle size of 10-300 mu m are mixed in an equal molar ratio or a nearly equal molar ratio, wherein the nearly equal molar ratio means that the molar ratio of each component accounts for 5-35mol% of the total amount, and the pure metal powders comprise copper powder, iron powder, nickel powder, chromium powder, aluminum powder, vanadium powder, molybdenum powder, manganese powder, cobalt powder, zinc powder, zirconium powder and tin powder; then carrying out high-energy ball milling on the mixed metal powder to mechanically alloy the powder; finally, melting the mechanically alloyed powder by a plasma discharge method, applying pressure to extrude and cast the powder simultaneously to obtain a sheet high-entropy alloy;
the high-energy ball milling mode is as follows: putting five or more mixed metal powders into a high-energy ball milling tank body, wherein the mass ratio of ball materials is 2:1-80:1, the filling coefficient is 0.2-0.8, vacuumizing the ball milling tank or filling argon and nitrogen protective gas into the ball milling tank body, and performing high-energy ball milling for 0.5-40 hours;
the process of extruding and casting the edges comprises the following steps: loading the mechanically alloyed powder into a die, heating the die by adopting discharge plasma, heating the die to a temperature 20-2000 ℃ lower than the melting point of the high-entropy alloy powder, preserving the heat, then extruding and casting the melted metal powder under the pressure of 0.5-30MPa to obtain a high-entropy alloy material, and designing a cutter at a finished product outlet to make the material into a required size and shape;
the powder of mechanical alloying is put into the mould, and the mould structure is: the powder raw material is placed in the die cavity, the upper pressing head and the lower pressing head are arranged at two ends of the die and are respectively communicated with a positive electrode and a negative electrode, the upper pressing head and the lower pressing head are heated by adopting discharge plasma, the lower pressing head is provided with a finished product outlet, and when the upper pressing head applies pressure, the material can be extruded from the finished product outlet of the lower pressing head.
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| CN113927032B (en) * | 2021-09-02 | 2022-09-16 | 山东晶盾新材料科技有限公司 | Mold structure for rapid hot-pressing sintering |
| CN114990407B (en) * | 2022-04-25 | 2023-05-30 | 哈尔滨工程大学 | High-entropy alloy with shielding function and preparation method thereof |
| CN114959404A (en) * | 2022-05-16 | 2022-08-30 | 哈尔滨工业大学 | Multi-element high-entropy alloy powder and preparation method and application thereof |
| CN115652173B (en) * | 2022-10-25 | 2024-04-05 | 锑玛（苏州）精密工具股份有限公司 | Cobalt-free and carbon-free FeCrNiCuAl high-entropy alloy cutter special for nuclear power site sampling and preparation method |
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