CN113957276A - Liquid deep supercooling and solid phase change duplex coordination control method and device for metal material - Google Patents
Liquid deep supercooling and solid phase change duplex coordination control method and device for metal material Download PDFInfo
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- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
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- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/20—Measures not previously mentioned for influencing the grain structure or texture; Selection of compositions therefor
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- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/18—Hardening; Quenching with or without subsequent tempering
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
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Abstract
The invention belongs to the technical field of metal material preparation, and provides a liquid deep undercooling and solid phase change duplex coordination method and device for a metal material. The invention provides a metal material liquid deep undercooling and solid phase change dual cooperative control device which comprises a heating system (1), a cooling system (2) and a drawing system (3) connected with the heating system; the heating system (1) comprises a sample container (11) and a heat source (12); the sample container (11) is arranged in a heat source (12); the sample container (11) of the heating system (1) is brought into or out of the cooling system (2) by means of a drawing system (3). After the heating system is subjected to deep supercooling, the duplex cooperative control device provided by the invention directly pulls the sample container of the heating system into the cooling system through the drawing system to be cooled to obtain a cooled sample; and then, the cooled sample reciprocates in a heating system and a cooling system according to actual needs, so that the regulation and control of solid-state phase change are realized. The device can realize the integrated operation of deep supercooling and solid phase change regulation, and has simple operation and small operation difficulty.
Description
Technical Field
The invention relates to the technical field of metal material preparation, in particular to a liquid deep undercooling and solid phase change duplex coordination method and device for a metal material.
Background
The deep supercooling treatment can regulate and control the solidification structure of the metal material and optimize the microstructure of the metal material by controlling the liquid-solid phase change, thereby improving the physical and chemical properties of the metal material. The deep supercooling treatment is mainly to realize large thermodynamic supercooling by avoiding or eliminating heterogeneous crystal nuclei, so that the growth of the melt is not controlled by external heat dissipation conditions. At present, various container-free processing technologies, such as melt immersion, electromagnetic suspension, electrostatic suspension, tube drop and the like, can realize deep supercooling and rapid solidification of liquid metal. The melt immersion-floating method is characterized in that liquid metal is immersed into a molten glass purifying agent, and buoyancy is generated by the glass melt to realize similar container-free solidification. The glass cleaning agent has two functions: firstly, impurities in the metal are removed through the physical adsorption effect between the liquid metal and the molten glass, and secondly, the molten glass can isolate the liquid metal from the wall of the heating container so as to eliminate the nucleation catalysis effect. Generally, the glass scavenger has a softening temperature below the liquidus temperature of the alloy, does not react with the metal, and readily reacts with high melting point compounds and other impurities in the sample to form low melting point compounds. Compared with other methods, the melt immersion method is not limited by the size of a sample, and is one of important methods for realizing deep undercooling of three-dimensional large-volume liquid metal.
The solid phase transition treatment can also optimize the microstructure of the metal material and improve the physical and chemical properties of the material. For example, the hardness of the steel member after quenching is improved, but the steel member becomes brittle at the same time, and the brittleness can be eliminated after tempering treatment. The solid phase change regulation and control process of the metal material has multiple steps and long time consumption, and all operations need to be carried out in a vacuum environment, so that the requirement on the automation degree of the device is high. Patent CN213866327U discloses a casting solution and aging heat treatment device, wherein the processes of solution treatment, quenching and aging need to transfer materials into different furnace bodies, the device has large volume and complex operation, and the achievable heat treatment modes are few. Patent CN213866322U discloses a heat treatment apparatus for improving the hardness of alloy steel castings, which cools the castings only by air cooling and water cooling, and the cooling rate is limited.
The deep supercooling treatment and the solid phase transition treatment belong to different fields. In the prior art, deep supercooling treatment needs to be performed in a solidification apparatus, and the apparatus is required to have a metal material containerless processing capability and a high degree of vacuum. The solid phase transition treatment needs to be carried out in a heat treatment furnace, and the temperature control program of the device needs to be accurate and has more adjustable parameters. Therefore, if the deep supercooling treatment and the solid phase transition treatment are to be completed, a deep supercooling sample needs to be obtained in the solidification device and then moved to the heat treatment furnace, and the process is complicated and the operation difficulty is high.
Disclosure of Invention
In view of the above, the present invention provides a method and an apparatus for dual coordination of liquid deep undercooling and solid phase transition of a metal material. The duplex cooperative control device can complete the processes of deep supercooling solidification and solid phase change duplex cooperative control in the same device through a single experiment, and has the advantages of simple operation and small operation difficulty.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a liquid deep supercooling and solid phase change dual cooperative control device for a metal material, which comprises a heating system 1, a cooling system 2 and a drawing system 3 connected with the heating system;
the heating system 1 comprises a sample container 11 and a heat source 12; the sample container 11 is placed in a heat source 12;
the sample container 11 of the heating system 1 is brought into or out of the cooling system 2 by means of the pull system 3.
Preferably, the heating system 1 further comprises a graphite inductor 13 and a lifting component connected with the graphite inductor 13; the lifting part drives the graphite inductor 13 to enter or separate from the space between the sample container 11 and the heat source 12.
Preferably, the sample container 11 is an i-shaped sample container.
Preferably, the drawing system 3 comprises a drawing rod 31, a transmission 32 and a cylinder 33; one end of the drawing rod 31 is connected with the sample container 11 of the heating system 1; the other end of the pull rod 31 is connected with the cylinder 33 through a transmission device 32.
Preferably, the cylinder 33 is a double acting cylinder.
Preferably, the cooling system 2 comprises a cooling chamber 21 and a water-cooling ring layer 22 located on the outer wall of the cooling chamber 21.
Preferably, the device also comprises a vacuum system 4 and a temperature measuring system 5 which are connected with the heating system 1; and the control system 6 is connected with the vacuum system 4 and the temperature measuring system 5.
The invention also provides a method for carrying out the liquid deep supercooling and solid phase change duplex cooperative control on the metal material by utilizing the metal material liquid deep supercooling and solid phase change duplex cooperative control device in the technical scheme, which comprises the following steps of:
placing a metal material and a glass purifying agent in a sample container of a heating system, and performing deep supercooling to obtain a supercooled melt;
starting a drawing system, drawing the sample container filled with the supercooled melt into a cooling system, and cooling to obtain a cooled sample;
and reciprocating the cooled sample between a heating system and a cooling system to realize solid phase change regulation and control.
Preferably, the speed of the drawing-in or reciprocating is independently 30 to 500 mm/s.
Preferably, the supercooling degree of the supercooled melt is 100-300K.
The invention provides a liquid deep supercooling and solid phase change dual cooperative control device for a metal material, which comprises a heating system 1, a cooling system 2 and a drawing system 3 connected with the heating system; the heating system 1 comprises a sample container 11 and a heat source 12; the sample container 11 is placed in a heat source 12; the sample container 11 of the heating system 1 is brought into or out of the cooling system 2 by means of the pull system 3. After the sample of the duplex cooperative control device provided by the invention is subjected to deep supercooling in the heating system, the sample container of the heating system is directly pulled into the cooling system through the drawing system to be cooled, so that a cooled sample is obtained; and then, the cooled sample reciprocates in a heating system and a cooling system according to actual needs, so that the regulation and control of solid-state phase change are realized. The device can realize the integrated operation of deep supercooling and solid phase change regulation, and has simple operation and small operation difficulty.
The invention also provides a method for carrying out the liquid deep supercooling and solid phase change duplex cooperative control on the metal material by using the metal material liquid deep supercooling and solid phase change duplex cooperative control device in the technical scheme, which comprises the following steps of: placing a metal material and a glass purifying agent in a sample container of a heating system, and performing deep supercooling to obtain a supercooled melt; starting a drawing system, drawing the sample container filled with the supercooled melt into a cooling system, and cooling to obtain a cooled sample; and reciprocating the cooled sample between a heating system and a cooling system to realize solid phase change regulation and control. The method of the invention has simple operation and small operation difficulty.
Drawings
FIG. 1 is a schematic diagram of a liquid deep supercooling and solid phase transition dual cooperative control device for a metal material provided by the present invention;
FIG. 2 is a schematic view of a heating system without a graphite inductor;
FIG. 3 is a schematic view of a heating system incorporating a graphite inductor;
FIG. 4 is a schematic view of a heating system including a graphite sensor, an I-shaped sample container;
FIG. 5 is a schematic diagram of a metal material liquid deep supercooling and solid phase transition dual cooperative control device comprising a vacuum system, a temperature measuring system and a control system;
FIG. 6 is a schematic flow chart of a liquid deep undercooling and solid phase transition duplex coordination method for metal materials according to the present invention;
wherein, 1 is a heating system, 11 is a sample container, 12 is a heat source, and 13 is a graphite inductor; 2, a cooling system, 21, a cooling chamber and 22, a water-cooling ring layer; 3, a drawing system, 31, a drawing rod, 32, a transmission device and 33, a cylinder; 4, a vacuum system; 5 is a temperature measuring system; 6 is a control system; 9 is a glass cleaning agent; 10 is a metal material.
Detailed Description
The invention provides a liquid deep supercooling and solid phase change dual cooperative control device for a metal material, which comprises a heating system 1, a cooling system 2 and a drawing system 3 connected with the heating system;
the heating system 1 comprises a sample container 11 and a heat source 12; the sample container 11 is placed in a heat source 12;
the sample container 11 of the heating system 1 is brought into or out of the cooling system 2 by means of the pull system 3.
Fig. 1 is a schematic diagram of a liquid deep undercooling and solid phase transition dual cooperative control device for a metal material provided by the invention. The liquid deep undercooling and solid phase transition dual cooperative control device for the metal material provided by the invention is described in detail with reference to fig. 1.
The metal material liquid deep undercooling and solid phase change dual cooperative control device provided by the invention comprises a heating system 1; the heating system 1 preferably comprises a sample container 11 and a heat source 12; the sample container 11 is placed within a heat source 12. In the present invention, fig. 2 is a schematic view of a heating system provided by the present invention.
In the present invention, the heating system 1 preferably further includes a graphite inductor 13 and a lifting member connected to the graphite inductor 13; the lifting part drives the graphite inductor 13 to enter or separate from the space between the sample container 11 and the heat source 12. The present invention does not specifically limit the elevating member as long as the above object can be achieved. Fig. 3 is a schematic view of a heating system including a graphite inductor according to the present invention.
In the present invention, the sample container 11 is preferably an I-shaped sample container. Fig. 4 is a schematic diagram of a heating system including a graphite inductor, an i-shaped sample container. In the invention, the sample container is processed into the sample groove with a specific part shape, so that the in-situ part preparation processing is realized.
In the present invention, the sample container 11 is preferably a crucible; the crucible is preferably made of aluminum oxide (Al)2O3) Graphite or Boron Nitride (BN).
In the present invention, the heat source 12 is preferably an induction coil; the induction coil is preferably formed by winding a red copper tube.
In the present invention, when the graphite inductor 13 is interposed between the heat source 12 and the sample container 11, the heating system is heated by induction heat transfer; when the graphite inductor 13 is not interposed between the heat source 12 and the sample container 11, the heating system is heated by direct induction heating. The heating system can control the heating system to contain or not contain the graphite inductor by controlling the lifting part connected with the graphite inductor, so that the free conversion of induction heat transfer heating and direct induction heating is realized, and the operation is simple.
The metal material liquid deep supercooling and solid phase change dual cooperative control device provided by the invention comprises a cooling system 2; the cooling system 2 preferably comprises a cooling chamber 21 and a water cooling ring 22 located on the outer wall of the cooling chamber 21. In the present invention, the cooling chamber 21 may be filled with liquid metal. In the invention, when the sample container filled with the melt is pulled into the cooling system through the drawing system and the water cooling ring layer of the cooling system is closed, the cooling mode is air cooling; when the sample container filled with the melt is pulled into the cooling system through the drawing system, and the water cooling ring layer of the cooling system is started, the cooling mode is preferably air cooling and water cooling; when the melt in the sample container is directly filled into a cooling chamber of a cooling system and a water cooling ring layer of the cooling system is closed, the cooling mode is liquid metal cooling; when the melt in the sample container is filled into a cooling chamber of the cooling system, a water cooling ring layer of the cooling system is started, and the cooling mode is preferably liquid metal cooling and water cooling. In the present invention, in terms of the cooling rate, air cooling < air cooling + water cooling < liquid metal cooling + water cooling. The cooling system provided by the invention can provide various cooling modes by matching with different drawing speeds of the drawing system.
The metal material liquid deep supercooling and solid phase change dual cooperative control device provided by the invention comprises a drawing system 3; the drawing system 3 preferably comprises a drawing rod 31, a transmission 32 and a cylinder 33; one end of the drawing rod 31 is preferably connected with the sample container 11 of the heating system 1; the other end of the pull rod 31 is preferably connected to the cylinder 33 via a transmission 32. In the present invention, the cylinder 33 is preferably a double acting cylinder. In the present invention, the withdrawal system enables the sample container of the heating system to be reciprocated between the heating system and the cooling system.
The metal material liquid deep undercooling and solid phase change dual cooperative control device provided by the invention preferably further comprises a vacuum system 4 and a temperature measuring system 5 which are connected with the heating system 1; and the control system 6 is connected with the vacuum system 4 and the temperature measuring system 5.
In the present invention, the vacuum system 4 preferably comprises a vacuum chamber, a vacuum pump and an inert gas source; the vacuum chamber is preferably connected to a vacuum pump and a source of inert gas via a conduit.
In the invention, the temperature measuring system 5 preferably consists of an infrared thermometer and a display; the infrared thermometer is preferably fixed above the vacuum chamber of the vacuum system 4, and can observe the temperature change of the sample in the sample container in the heating system in real time. In the invention, the temperature measurement range of the infrared thermometer is preferably 300-2500 ℃.
In the present invention, the control system 6 preferably consists of a control cabinet and control software; the control cabinet can control the vacuum system, the heating system, the drawing system and the temperature measuring system. The automatic operation of the processes of heating, heat preservation, cooling and the like can be realized through control software. For the treatment process with complex flow, the whole device can be automatically finished only by inputting basic parameters in control software.
FIG. 5 is a schematic diagram of a metal material liquid deep supercooling and solid phase transition dual cooperative control device comprising a vacuum system, a temperature measuring system and a control system.
The invention also provides a method for carrying out the liquid deep supercooling and solid phase change duplex cooperative control on the metal material by utilizing the metal material liquid deep supercooling and solid phase change duplex cooperative control device in the technical scheme, which comprises the following steps of:
placing a metal material and a glass purifying agent in a sample container of a heating system, and performing deep supercooling to obtain a supercooled melt;
starting a drawing system, drawing the sample container filled with the supercooled melt into a cooling system, and cooling to obtain a cooled sample;
and reciprocating the cooled sample between a heating system and a cooling system to realize solid phase change regulation and control.
The invention puts metal material and glass cleaning agent into the sample container of heating system, and carries on deep super cooling, and gets super cooling melt.
In the present invention, the metallic material preferably includes carbon steel, Cu-14.5Al-5Ni shape memory alloy or Inconel 718 alloy. The type of the glass purifying agent is not particularly limited, and the glass purifying agent can be selected according to the selected metal material. In the present invention, the glass scavenger is selected from the following criteria: the glass cleaning agent cannot react with the melt of the metal material; the softening temperature of the glass purifying agent is lower than the liquidus temperature of the metal material; the glass purifying agent preferably has high adhesiveness, and can effectively adsorb heterogeneous cores in the metal material melt and separate the heterogeneous cores from the metal material melt; the glass purifying agent reacts with high-melting-point oxides and other heterogeneous cores in the metal material to generate low-melting-point compounds. In the present invention, the glass scavenger preferably comprises B2O3、Al2O3、SiO2、Na2O、Na2B4O7One or more of (a). In a specific embodiment of the present invention, when the metal material is preferably carbon steel, the glass scavenger is preferably B2O3(ii) a When the metal material is preferably Cu-14.5Al-5Ni shape memory alloy, the glass scavenger is preferably B2O3、Na2B4O7、Al2O3And Na2The mass ratio of O is 3:2:1:1, a mixed glass cleaning agent; when the metal material is preferably Inconel 718 alloy, the glass cleaning agent is preferably B2O3And SiO2The mass ratio is 2:1 of the mixed glass cleaning agent.
After the metal material and the glass purifying agent are placed in a sample container of a heating system and before deep supercooling, the invention preferably further comprises vacuumizing the heating system, and the operation and parameter setting of vacuumizing are not particularly limited, and the metal material and the glass purifying agent can be selected according to actual metal materials and glass purifying agents.
In the present invention, the deep supercooling preferably includes the sequential steps of the super-heat melting, the heat preservation and the solidification. In the invention, the temperature of the overheating melting is preferably Mp + (100-200) DEG C, and the Mp is the liquidus temperature of the metal material; namely, the temperature of the overheated melting is 100 to 200 ℃ higher than the liquidus temperature of the metal material. In the present invention, the manner of the superheated melting preferably includes direct induction heating or induction heat transfer heating; the direct induction heating is preferably realized by the heating system shown in fig. 2, i.e., the sample container is directly placed inside the heat source, and the metal material in the sample container is directly heated by the vortex electromagnetic field generated by the heat source. In the present invention, the direct induction heating is characterized by high heating efficiency, and can heat and melt a sample in a short time, but the temperature difference in the sample is large, and the temperature near the middle area of the coil is usually higher than the upper and lower ends. In the present invention, the induction heat transfer heating is preferably implemented according to the heating system shown in fig. 3 and 4, that is, a graphite inductor is placed inside a heat source, a sample container is placed in the graphite inductor, the heat source heats the graphite inductor through a vortex electromagnetic field, and the graphite inductor transfers heat to the metal material in the sample container to heat the metal material. In the invention, the induction heat transfer heating has the characteristics of uniform heat, small temperature difference at each position of a sample, low heating efficiency and long required time.
In the invention, the heat preservation time is preferably 2-10 min.
In the present invention, the solidification is preferably performed under the condition that the heat source of the heating system is turned off.
In the invention, the processes of overheating melting, heat preservation and solidification are repeated for 3-6 times.
In the invention, the supercooling degree of the supercooled melt is preferably 100-300K.
After the supercooled melt is obtained, the drawing system is started, and the sample container filled with the supercooled melt is drawn into the cooling system to be cooled, so that a cooled sample is obtained.
In the present invention, the drawing speed is preferably 30 to 500 mm/s.
In the present invention, the cooling method preferably includes air cooling, air cooling + water cooling, liquid metal cooling, and liquid metal cooling + water cooling. In the present invention, the air cooling preferably draws the sample vessel containing the supercooled melt into the cooling system by means of a drawing system, the water-cooled ring of the cooling system being closed. In the present invention, the air cooling and water cooling preferably pull the sample container with the supercooled melt into the cooling system through a drawing system, and open the water cooling loop of the cooling system. In the present invention, the liquid metal cooling is preferably performed by filling the supercooled melt in the sample container into the cooling chamber of the cooling system, and closing the water-cooled ring layer. In the invention, the liquid metal cooling and water cooling are preferably implemented by filling the supercooled melt in the sample container into a cooling chamber of a cooling system and opening a water cooling ring layer.
After the cooling sample is obtained, the cooling sample is reciprocated between the heating system and the cooling system, so that solid phase change regulation and control are realized.
The solid phase change regulation and control process is not particularly limited, and the solid phase change regulation and control method can be selected according to actual conditions. In the invention, the heating process in the solid phase change regulation is carried out in a heating system, and the cooling process is carried out in a cooling system; different cooling modes can be regulated and controlled through a cooling system; the heating system can regulate and control different heating modes.
FIG. 6 is a schematic flow chart of a liquid deep undercooling and solid phase transition duplex coordination method for a metal material according to the present invention.
The following describes the liquid deep undercooling and solid phase transition two-stage cooperative control method and apparatus for metal materials in accordance with the present invention in detail with reference to the following examples, which should not be construed as limiting the scope of the present invention.
Example 1
1. Mixing a metallic material of carbon steel and B2O3The glass purifying agent is put into a BN crucible, and the crucible is put into an induction coil. Starting a vacuum system to pump the vacuum chamber to 1 × 10-6Pa, then filling high-purity inert gas to 1 × 104Pa, repeat this process 5 times.
2. Starting a heating system, heating the metal material and the glass purifying agent by adopting a direct induction heating mode, observing the temperature change of the sample through a temperature measuring system, preserving the temperature for 10min after the sample is molten, wherein the preserving temperature is 100 ℃ higher than the liquidus temperature of the metal material, closing the heating system after the heat preservation is finished, starting the heating system again after the sample is solidified, and repeating the step for 4 times to obtain the supercooled melt, wherein the supercooling degree of the supercooled melt is 300K.
3. And starting a drawing system, setting the drawing speed to be 500mm/s, drawing the supercooled melt and the crucible into a cooling system together, and rapidly cooling the supercooled melt by adopting a liquid metal cooling method to obtain a cooled sample.
4. The crucible and the cooled sample are lifted into a heating system through a drawing system, the cooled sample is heated to 850 ℃ by adopting an induction heat transfer heating mode, and the temperature is kept for 60 min; and starting the drawing system, setting the speed at 500mm/s, drawing the sample into the cooling system, and quenching the sample by adopting a liquid metal and water cooling method. After the temperature of the sample is reduced to room temperature, the sample is lifted into a heating system, the sample is heated to 180 ℃ by adopting an induction heat transfer heating mode, and the temperature is kept for 2 hours; drawing the sample into a cooling system at a speed of 30mm/s, tempering the sample in an air cooling mode, and taking a sample after the temperature of the heating system is reduced to room temperature.
Example 2
1. Mixing the metallic materials Cu-14.5Al-5Ni shape memory alloy and B2O3、Na2B4O7、Al2O3、Na2Placing the mixed glass purifying agent with the mass ratio of O being 3:2:1:1 into an I-shaped graphite crucible shown in figure 4, and placing the crucibleIs placed in an induction coil. Starting a vacuum system to pump the vacuum chamber to 1 × 10-6Pa, then filling high-purity inert gas to 0.5 multiplied by 105Pa, this process was repeated 3 times.
2. Starting a heating system, heating the metal material and the mixed glass purifying agent by adopting an induction heat transfer heating mode, observing the temperature change of the sample through a temperature measuring system, preserving the heat for 3 minutes after the sample is melted, wherein the heat preservation temperature is 200 ℃ higher than the liquidus temperature of the metal material, closing the heating system after the heat preservation is finished, starting the heating system again after the sample is solidified, and repeating the step for 4 times to obtain the supercooled melt, wherein the supercooling degree of the supercooled melt is 100K.
3. And starting a drawing system, setting the speed to be 300mm/s, drawing the supercooled melt and the crucible into a cooling system together, and rapidly cooling the sample by adopting an air cooling and water cooling method to obtain a cooled sample.
4. And (2) lifting the crucible and the cooled sample into a heating system through a drawing system, heating the sample to 800 ℃ by adopting an induction heat transfer heating mode, preserving heat for 10min, starting the drawing system, setting the speed to be 500mm/s, drawing the sample into the cooling system, quenching the sample by adopting a liquid metal cooling method, and taking a sample after the heating system is cooled to room temperature.
Example 3
1. Mixing metallic material Inconel 718 alloy with B2O3、SiO2Adding the mixed glass purifying agent with the mass ratio of 2:1 into Al2O3And a crucible, which is placed in the induction coil. Starting a vacuum system to pump the vacuum chamber to 1 × 10-6Pa, then filling high-purity inert gas to 1 × 105Pa, this process was repeated 3 times.
2. Starting a heating system to heat the metal material and the mixed glass purifying agent, observing the temperature change of the sample through a temperature measuring system, preserving the heat for 2min after the sample is melted, wherein the heat preservation temperature is 150 ℃ higher than the liquidus temperature of the metal material, closing the heating system after the heat preservation is finished, starting the heating system again after the sample is solidified, and repeating the step for 4 times to obtain the supercooled melt, wherein the supercooling degree of the supercooled melt is 150K.
3. And starting a drawing system, setting the speed to be 200mm/s, drawing the supercooled melt and the crucible into a cooling system together, and rapidly cooling the sample by adopting a liquid metal cooling and water cooling method to obtain a cooled sample.
4. And (3) lifting the crucible and the cooled sample into a heating system through a drawing system, heating the sample to 1040 ℃ by adopting an induction heat transfer heating mode, preserving the temperature for 10 hours, and carrying out solid solution treatment on the sample. And then reducing the temperature to 870 ℃, preserving the temperature for 10 hours, and carrying out aging treatment on the sample. And starting the drawing system, setting the speed at 300mm/s, drawing the sample into the cooling system, cooling the sample by adopting an air cooling method, and taking a sample after the temperature of the heating system is reduced to the room temperature.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A metal material liquid deep undercooling and solid phase change dual cooperative control device comprises a heating system (1), a cooling system (2) and a drawing system (3) connected with the heating system;
the heating system (1) comprises a sample container (11) and a heat source (12); the sample container (11) is arranged in a heat source (12);
the sample container (11) of the heating system (1) is brought into or out of the cooling system (2) by means of a drawing system (3).
2. The twin protocol control device according to claim 1, wherein the heating system (1) further comprises a graphite inductor (13) and a lifting member connected to the graphite inductor (13); the lifting component drives the graphite inductor (13) to enter or separate from the space between the sample container (11) and the heat source (12).
3. The twin protocol device of claim 1 wherein the sample container (11) is an i-shaped sample container.
4. The coordinated twin control device according to claim 1, wherein said drawing system (3) comprises a drawing rod (31), a transmission device (32) and a cylinder (33); one end of the pull rod (31) is connected with the sample container (11) of the heating system (1); the other end of the drawing rod (31) is connected with the cylinder (33) through a transmission device (32).
5. A twin slave device according to claim 4, characterised in that the cylinder (33) is a double acting cylinder.
6. The twin protocol control device according to claim 1, characterized in that the cooling system (2) comprises a cooling chamber (21) and a water cooling ring layer (22) on the outer wall of the cooling chamber (21).
7. The twin coordinated control device according to claim 1, further comprising a vacuum system (4) and a temperature measuring system (5) connected to said heating system (1); and the control system (6) is connected with the vacuum system (4) and the temperature measuring system (5).
8. A method for carrying out liquid deep supercooling and solid phase change duplex cooperative control on a metal material by using the metal material liquid deep supercooling and solid phase change duplex cooperative control device as claimed in any one of claims 1 to 7, comprising the following steps of:
placing a metal material and a glass purifying agent in a sample container of a heating system, and performing deep supercooling to obtain a supercooled melt;
starting a drawing system, drawing the sample container filled with the supercooled melt into a cooling system, and cooling to obtain a cooled sample;
and reciprocating the cooled sample between a heating system and a cooling system to realize solid phase change regulation and control.
9. A method according to claim 8, wherein the speed of said drawing-in or reciprocation is independently 30-500 mm/s.
10. The method of claim 8, wherein the supercooling degree of the supercooled melt is 100 to 300K.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008174423A (en) * | 2007-01-19 | 2008-07-31 | Inductotherm Corp | Directional solidification of metal |
| CN102703986A (en) * | 2012-06-21 | 2012-10-03 | 上海大学 | Method for transforming columnar crystal-orienting isometric crystal of directional solidified alloy with strong static magnetic field induction |
| CN105543952A (en) * | 2015-12-28 | 2016-05-04 | 北京航空航天大学 | Rapid directional solidification equipment and rapid directional solidification method |
| CN111230077A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学 | Wide speed-regulating directional solidification device for high-temperature alloy |
| CN111230078A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学 | Directional solidification method for metal material |
| CN111299553A (en) * | 2020-04-10 | 2020-06-19 | 西北工业大学 | Multi-mode excited deep supercooling directional solidification device and method |
-
2021
- 2021-10-26 CN CN202111246251.4A patent/CN113957276B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008174423A (en) * | 2007-01-19 | 2008-07-31 | Inductotherm Corp | Directional solidification of metal |
| CN102703986A (en) * | 2012-06-21 | 2012-10-03 | 上海大学 | Method for transforming columnar crystal-orienting isometric crystal of directional solidified alloy with strong static magnetic field induction |
| CN105543952A (en) * | 2015-12-28 | 2016-05-04 | 北京航空航天大学 | Rapid directional solidification equipment and rapid directional solidification method |
| CN111230077A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学 | Wide speed-regulating directional solidification device for high-temperature alloy |
| CN111230078A (en) * | 2020-03-09 | 2020-06-05 | 西北工业大学 | Directional solidification method for metal material |
| CN111299553A (en) * | 2020-04-10 | 2020-06-19 | 西北工业大学 | Multi-mode excited deep supercooling directional solidification device and method |
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