Centrifugal high gravity coagulation device and coagulation test method

Abstract

The present invention discloses a supergravity solidification device and a solidification test method. A cooling system is installed at the bottom of the hanging cup, and a heating system, a crucible and a heat preservation system are installed above the cooling system. The crucible is located in the heating system, and a heat preservation system is provided in the hanging cup outside the heating system. The centrifugal supergravity solidification device is installed, and the alloy sample is placed. After vacuuming, the heating is started, and the supergravity centrifuge is started again until the alloy sample is completely melted. The cooling is controlled to separate layers or gradient distribution is performed. When the sample is completely solidified, the heating is turned off and the treatment is controlled. The present invention solves the key problem that traditional centrifugal casting cannot achieve controllable preparation, and realizes high-throughput material preparation or supergravity directional solidification under supergravity conditions. It has the advantages of simple structure, convenient operation and high safety factor.

Description

Technical Field

[0001] The present invention relates to a solidification device and a test method in the technical field of material preparation and directional solidification, and in particular to a directional solidification device and a solidification test method in a centrifugal high gravity environment. Background Art

[0002] High-throughput material preparation is fundamental to the successful implementation of the Materials Genome Project. Leveraging the characteristics of a hypergravity field—a constant hypergravity field at the same radius and a radial centrifugal force gradient—and leveraging the buoyancy convection effect generated by hypergravity-enhanced density differences, the nucleation and growth behavior and solidification microstructure formation sequence are manipulated by temperature, cooling rate, and hypergravity parameters to produce materials with compositional and microstructural gradients, thus enabling high-throughput material preparation. Hypergravity significantly alters heat and mass transfer processes, leading to significant changes in interface morphology and a significant reduction in the width of the mushy zone. The rapid flow of the liquid phase significantly increases the temperature gradient in the liquid phase at the interface front, greatly facilitating uniform mixing of liquid solutes and flat interfacial growth. This significantly alters the dendrite growth morphology, transforming from dendrites with distinct main axes to spikes with a fine microstructure. While traditional centrifugal casting can also achieve hypergravity solidification, the lack of in-situ heating and controlled cooling prevents precise control of the solidification process, severely limiting the improvement of material microstructural quality. Summary of the Invention

[0003] In order to solve the problems existing in the background technology, the present invention provides a centrifugal supergravity solidification device and method to address the key problem that traditional centrifugal casting cannot achieve controllable preparation, which solves the key problem of the difficulty in achieving temperature gradient during supergravity solidification, thereby realizing high-throughput material preparation or supergravity directional solidification under supergravity conditions.

[0004] The technical solution adopted in the present invention is:

[0005] 1. A centrifugal high gravity solidification device, characterized by:

[0006] The device includes a hanging cup, a heating system, a crucible, a cooling system and a thermal insulation system; the cooling system is installed at the bottom of the hanging cup, and the heating system, crucible and thermal insulation system are installed above the cooling system. The crucible is located in the heating system, and the thermal insulation system is provided in the hanging cup outside the heating system.

[0007] The hanging cup is fixedly mounted on the end of the rotating arm of the ultragravity centrifuge.

[0008] The hanging cup includes a hanging cup cavity and a hanging ear hole. The heating system, crucible system, cooling system and insulation system are placed in the hanging cup cavity. The side of the hanging cup cavity is provided with a hanging ear hole for connecting to the end of the rotating arm of the ultragravity centrifuge.

[0009] The heating system includes a heating chamber, a heating furnace tube, a heating wire and an insulation cover. The heating chamber is divided into an upper heating chamber located at the top and a lower heating chamber located at the top. The lower heating chamber is installed on the cooling system, and an insulation cover is provided at the upper port of the upper heating chamber; a lower heating furnace tube is provided on the inner wall of the lower heating chamber, and a lower heating wire is installed on the lower heating furnace tube; an upper heating furnace tube is provided on the inner wall of the upper heating chamber, and an upper heating wire is installed on the upper heating furnace tube.

[0010] The crucible is placed in a heating chamber of a heating system, and an upper thermocouple hole and a lower thermocouple hole for installing thermocouples are respectively provided on the upper part and the lower part.

[0011] The cooling system includes an insulating floor, a ventilation base, an insulating ring, a crucible support platform and a support base; the insulating floor is installed at the bottom of the hanging cup, and a ventilation base is fixedly installed in the center of the insulating floor. An insulating ring is arranged on the insulating floor around the ventilation base, and a cavity is provided on the top of the ventilation base. A crucible support platform is provided at the upper end of the cavity for sealing. An air inlet channel and an air outlet channel are respectively provided on both sides of the middle of the ventilation base, and the upper ends of the air inlet channel and the air outlet channel are connected to the cavity. One end of the air inlet pipe and the air outlet pipe passes through the insulating ring horizontally and extends into the ventilation base and is respectively connected to the lower ends of the air inlet channel and the air outlet channel; the other ends of the air inlet pipe and the air outlet pipe extend upward after passing through the insulating ring and are respectively connected to the external cooling air source and the outside of the experimental cabin; a support base for supporting the installation of the insulation system is provided above the insulating ring.

[0012] The thermal insulation system includes an outer bottom thermal insulation ring, a middle bottom thermal insulation ring, an inner bottom thermal insulation ring, a fourth thermal insulation cavity plate, a third thermal insulation cavity plate, a second thermal insulation cavity plate, a first thermal insulation cavity plate, an upper first thermal insulation cover, an upper second thermal insulation cover and an upper third thermal insulation cover connected into one body;

[0013] The fourth layer of thermal insulation cavity plate, the third layer of thermal insulation cavity plate, the second layer of thermal insulation cavity plate and the first layer of thermal insulation cavity plate are all annular plates and are arranged concentrically from the outside to the inside. The upper end surfaces of the third layer of thermal insulation cavity plate, the second layer of thermal insulation cavity plate and the first layer of thermal insulation cavity plate are respectively fixed with an upper third layer of thermal insulation cover, an upper second layer of thermal insulation cover and an upper first layer of thermal insulation cover. The lower end surfaces of the third layer of thermal insulation cavity plate, the second layer of thermal insulation cavity plate and the first layer of thermal insulation cavity plate are respectively provided with an outer bottom thermal insulation ring, a middle bottom thermal insulation ring and an inner bottom thermal insulation ring with a central opening. The outer bottom thermal insulation ring is supported on the supporting base of the cooling system. A top cover for sealing the upper port of the hanging cup is also provided on the upper third layer of thermal insulation cover. The upper third layer of thermal insulation cover and the top cover are fixedly connected by an outer layer of fixing screws. The central openings of the outer bottom thermal insulation ring, the middle bottom thermal insulation ring and the inner bottom thermal insulation ring are concentrically and coaxially arranged.

[0014] The inner bottom insulation ring, the first layer insulation cavity plate and the upper first layer insulation cover form an inner insulation cavity, the inner insulation cavity contains a heating system and a crucible, and the top of the inner insulation cavity is fixed with the insulation cover of the heating system;

[0015] The fourth layer of thermal insulation cavity plate is welded together with the outer bottom thermal insulation ring and the upper third layer of thermal insulation cover. At the same time, it is fixed to the top cover through four outer fixing screws, and the top cover is fixed to the hanging cup through screws, which can increase the rigidity of the first, second and third layers of thermal insulation cavity.

[0016] The first and second insulation cavities are connected to the upper second insulation cover through inner fixing screws to form an integral structure, which provides overall structural strength and rigidity for the insulation system and can ensure the stability of the insulation system.

[0017] The inner bottom insulation ring, the first insulation cavity plate, and the upper first insulation cover are welded together to form an inner insulation cavity. The middle bottom insulation ring, the second insulation cavity plate, and the upper second insulation cover are welded together to form a second insulation cavity. The outer bottom insulation ring, the third insulation cavity plate, and the upper third insulation cover are welded together to form a third insulation cavity.

[0018] 2. A solidification test method using a centrifugal high-gravity solidification device, the method comprising the following steps:

[0019] The first step is to install the centrifugal ultragravity solidification device on the disc rotor of the rotating arm of the ultragravity centrifuge, and place the alloy sample to be solidified in the crucible of the centrifugal ultragravity solidification device;

[0020] Step 2: Start the vacuum system to make the vacuum degree in the experimental chamber of the ultragravity centrifuge reach 0.01Pa;

[0021] Step 3: After the vacuum degree in the experimental chamber reaches 0.01 Pa, the heating system in the centrifugal high gravity solidification device is started;

[0022] Step 4: When the crucible temperature detected by the thermocouple reaches 0.8 times the melting point of the alloy sample, start the ultragravity centrifuge;

[0023] Step 5: After the speed of the ultragravity centrifuge reaches the experimental setting speed, the crucible is continuously heated by the heating system until the alloy sample is completely melted into a melt, and the speed is maintained at the experimental setting speed for 10 minutes;

[0024] Step 6: Control the heating power of the heating system and the cooling rate in the upper and lower heating chambers of the heating system so that elements with different densities in the melt have enough time to separate and separate under the action of centrifugal force, so that the solidified alloy samples have different alloy compositions at different heights, achieving the purpose of preparing multiple alloy compositions in a single step;

[0025] Step 7: When the sample is completely solidified, turn off the heating system and make judgments and treatments:

[0026] When the crucible temperature detected by the thermocouple drops below the solidus temperature of the alloy, the ultragravity centrifuge is turned off;

[0027] When the crucible temperature detected by the thermocouple dropped below 200°C, the vacuum system was turned off.

[0028] 3. A solidification test method using a centrifugal high-gravity solidification device, the method comprising the following steps:

[0029] The first step is to install the centrifugal ultragravity solidification device on the disc rotor of the rotating arm of the ultragravity centrifuge, and place the alloy sample to be solidified in the crucible of the centrifugal ultragravity solidification device;

[0030] Step 2: Start the vacuum system to make the vacuum degree in the experimental cabin of the ultragravity centrifuge reach 10-2Pa;

[0031] Step 3: After the vacuum degree in the experimental chamber reaches 10-2Pa, the heating system in the centrifugal high gravity solidification device is started;

[0032] Step 4: When the crucible temperature detected by the thermocouple reaches 0.8 times the melting point of the alloy sample, start the ultragravity centrifuge;

[0033] Step 5: After the speed of the ultragravity centrifuge reaches the experimental setting speed, the crucible is continuously heated by the heating system until the alloy sample is completely melted, and the crucible is maintained at the experimental setting speed for 10 minutes;

[0034] Step 6:

[0035] Controlling the heating power of the heating system, controlling the temperature in the upper heating chamber of the heating system to remain constant and lowering the temperature in the lower heating chamber, and at the same time controlling the cooling system to start working to cool the bottom of the crucible, thereby forming a temperature gradient in the crucible with the temperature gradually increasing from the bottom to the top;

[0036] Step 7: When the sample is completely solidified, turn off the heating system and make judgments and treatments:

[0037] When the crucible temperature detected by the thermocouple drops below the solidus temperature of the alloy, the ultragravity centrifuge is turned off;

[0038] When the crucible temperature detected by the thermocouple drops below 200° C., the cooling system and the vacuum system are turned off.

[0039] The testing process of the present invention's device must meet requirements such as high-temperature resistance, special atmosphere, high G-force, and cooling gas temperature reduction to ensure safe and stable operation. Considering the operating environment and the impact of high gravity, the present invention adopts a modular structure, which shortens the experimental preparation cycle, ensures a safe and reliable solidification process, and achieves high strength and low weight.

[0040] The beneficial effects of the present invention are:

[0041] The present invention can solve the key problem that traditional centrifugal casting cannot achieve controllable preparation, thereby realizing high-throughput material preparation or ultra-gravity directional solidification under ultra-gravity conditions.

[0042] The invention has the advantages of simple structure, convenient operation and high safety factor, is suitable for 1g-5000g hypergravity environment, the temperature ranges from room temperature to 1700°C, and the temperature gradient during directional solidification is not less than 10°C / cm. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 It is the overall structural diagram of the device of the present invention;

[0044] Figure 2 1 is a schematic diagram of the structure of the hanging cup 1, including a hanging cup cavity 1-1 and a hanging ear hole 1-2;

[0045] Figure 3 2 is a schematic diagram of the structure of the heating system 2, including an upper heating chamber 2-1, an upper heating furnace tube 2-2, an upper heating wire 2-3, a lower heating chamber 2-4, a lower heating furnace tube 2-5, a lower heating wire 2-6 and a heat preservation cover 2-7;

[0046] Figure 4 3 is a schematic structural diagram of a crucible 3, including an upper thermocouple hole 3-1 and a lower thermocouple hole 3-2;

[0047] Figure 5 Schematic diagram of the cooling system 4, including a heat-insulating floor 4-1, a ventilation base 4-2, a heat-insulating ring 4-3, a left swivel joint 4-4, an air inlet pipe 4-5, an air inlet channel 4-6, a right swivel joint 4-7, an air outlet pipe 4-8, an air outlet channel 4-9, a crucible support 4-10, a support base 4-11, a right fixing hole 4-12, a left fixing hole 4-13, an annular boss 4-14, and a cavity 4-15;

[0048] Figure 6 1 is a schematic diagram of the structure of the thermal insulation system 5, including an outer bottom insulation ring 5-1, a middle bottom insulation ring 5-2, an inner bottom insulation ring 5-3, a fourth layer of thermal insulation cavity plate 5-4, a third layer of thermal insulation cavity plate 5-5, a second layer of thermal insulation cavity plate 5-6, a first layer of thermal insulation cavity plate 5-7, an upper first layer of thermal insulation cover 5-8, an upper second layer of thermal insulation cover 5-9, an upper third layer of thermal insulation cover 5-10, a top cover 5-11, an outer layer fixing screw 5-12, and an inner layer fixing screw 5-13;

[0049] Figure 7 Schematic diagram of the arrangement of hanging cup 1 on the centrifuge;

[0050] Figure 8 It is a schematic diagram of the connection between the centrifugal high gravity coagulation device and the centrifuge;

[0051] Figure 9 It is a process roadmap for high-throughput preparation of materials under hypergravity conditions;

[0052] Figure 10 It is the process roadmap of directional solidification under high gravity conditions. DETAILED DESCRIPTION

[0053] The present invention will be further described below with reference to the accompanying drawings and specific implementations.

[0054] like Figure 1 As shown, the device includes a hanging cup 1, a heating system 2, a crucible 3, a cooling system 4 and a heat preservation system 5; the cooling system 4 is installed at the bottom of the hanging cup 1, and the heating system 2, the crucible 3 and the heat preservation system 5 are installed above the cooling system 4. The crucible 3 is located in the heating system 2, and the heat preservation system 5 is provided in the hanging cup 1 outside the heating system 2.

[0055] The device of the invention is used for being installed on an ultra-gravity centrifuge and is driven by the ultra-gravity centrifuge to rotate centrifugally.

[0056] Specifically, if Figure 7 As shown, the hanging cup 1 is fixedly installed at the end of the rotating arm of the ultragravity centrifuge, and a hanging cup 1 is connected and installed at each end of the rotating arm of the ultragravity centrifuge.

[0057] like Figure 2 As shown, the hanging cup 1 is mainly used to install the heating system 2, crucible 3, cooling system 4 and insulation system 5. It includes a hanging cup cavity 1-1 and a lifting ear hole 1-2. The heating system 2, crucible system 3, cooling system 4 and insulation system 5 are placed in the hanging cup cavity 1-1. The side of the hanging cup cavity 1-1 is provided with a lifting ear hole 1-2 for connecting to the end of the rotating arm of the ultragravity centrifuge. The hanging cup 1 is connected to the disc rotor of the centrifuge rotating arm through the lifting ear hole 1-2.

[0058] In a specific implementation, the hanging cup cavity 1 - 1 and the hanging ear hole 1 - 2 are processed as one piece, which can ensure the strength of the hanging cup 1 .

[0059] like Figure 3As shown, the main function of the heating system 2 is to heat the crucible 3, including a heating chamber, a heating furnace tube, a heating wire and a thermal insulation cover 2-7. The upper port of the heating chamber is provided with a thermal insulation cover 2-7. The heating chamber is divided into an upper heating chamber 2-1 located at the upper part and a lower heating chamber 2-4 located at the upper part. The lower heating chamber 2-4 is installed on the supporting base 4-11 of the cooling system 4, and the upper port of the upper heating chamber 2-1 is provided with a thermal insulation cover 2-7; the inner wall of the lower heating chamber 2-4 is provided with a lower heating furnace tube 2-5, and the lower heating furnace tube 2-5 is provided with a lower heating wire 2-6; the inner wall of the upper heating chamber 2-1 is provided with an upper heating furnace tube 2-2, and the upper heating furnace tube 2-2 is provided with an upper heating wire 2-3.

[0060] In a specific implementation, the upper heating wire 2-3 is mounted on the boss of the upper heating furnace tube 2-2 and then placed in the upper heating chamber 2-1, forming the upper heating zone of the heating system 2. The lower heating wire 2-6 is mounted on the boss of the lower heating furnace tube 2-5 and then placed in the lower heating chamber 2-4, forming the lower heating zone of the heating system 2. The assembled upper heating wire 2-3, upper heating furnace tube 2-2, and upper heating chamber 2-1 are then placed above the assembled lower heating wire 2-6, lower heating furnace tube 2-5, and lower heating chamber 2-4. The insulation cover 2-7 is installed above the upper heating chamber 2-1 to maintain heat and prevent heat loss.

[0061] like Figure 8 As shown, the heating system 2 is connected to the ground power supply system through the cable on the centrifuge disc rotating arm through the electrical slip ring.

[0062] like Figure 4 As shown, the crucible 3 is placed in the heating chamber of the heating system 2. The crucible 3 is mainly used to place the smelted alloy. Different crucible materials are selected according to the smelting temperature and the alloy type. The upper and lower parts are respectively provided with an upper thermocouple hole 3-1 and a lower thermocouple hole 3-2 for installing thermocouples.

[0063] The upper thermocouple hole 3-1 is used to install a thermocouple to control the temperature of the upper heating zone. The lower thermocouple hole 3-2 is used to install a thermocouple to control the temperature of the lower heating zone. During smelting, different types of thermocouples can be rotated and installed according to the melting temperature.

[0064] like Figure 8 As shown, the thermocouple is connected to the ground temperature control system through an electrical slip ring via a fixed bracket on the centrifuge disc rotating arm.

[0065] like Figure 5As shown, the cooling system 4 is mainly used to control the cooling rate of the solidification process, and an air cooling structure is designed. It includes an insulating floor 4-1, a ventilation base 4-2, an insulation ring 4-3, a crucible support platform 4-10 and a support base 4-11; the insulating floor 4-1 is installed at the bottom of the hanging cup cavity 1-1 of the hanging cup 1, and the insulating floor 4- can prevent the heat generated by the heating system 2 when working from being transferred to the hanging cup 1; a ventilation base 4-2 is fixedly installed in the center of the insulating floor 4-1, and an insulation ring 4-3 is arranged on the insulating floor 4-1 around the ventilation base 4-2, and a cavity 4-15 is provided on the top of the ventilation base 4-2, and a crucible support platform 4-10 is provided on the upper end of the cavity 4-15 for sealing, and the crucible support platform 4-10 is fixed to the top of the ventilation base 4-2, and an air inlet channel 4-6 and an air outlet channel 4-9 are respectively provided on both sides of the middle part of the ventilation base 4-2, and the upper ends of the air inlet channel 4-6 and the air outlet channel 4-9 are respectively provided. The ends of the air inlet pipe 4-5 and the air outlet pipe 4-8 are connected with the cavity 4-15, one end of the air inlet pipe 4-5 and the air outlet pipe 4-8 pass through the insulation ring 4-3 horizontally and extend into the ventilation base 4-2 and are respectively connected to the lower ends of the air inlet channel 4-6 and the air outlet channel 4-9, one end of the air inlet pipe 4-5 and the air outlet pipe 4-8 are respectively connected with the lower ends of the air inlet channel 4-6 and the air outlet channel 4-9 through the left turning joint 4-4 and the right turning joint 4-7; the other ends of the air inlet pipe 4-5 and the air outlet pipe 4-8 pass through the insulation ring 4-3 and extend upward and are respectively connected to the external cooling air source and the outside of the experimental cabin; a support base 4-11 for supporting the installation of the insulation system 5 is provided on the insulation ring 4-3, and the other ends of the air inlet pipe 4-5 and the air outlet pipe 4-8 pass through the left fixing hole 4-13 and the right fixing hole 4-12 opened on the support base 4-11.

[0066] An annular boss 4-14 for positioning and installing the heating system 2 is provided on the edge of the top surface of the ventilation base 4-2.

[0067] The ventilation base 4-2 is placed flat on the upper part of the insulation floor 4-1. During operation, the insulation floor 4-1 is in close contact with the ventilation base 4-2 under the action of centrifugal force, and supports the centrifugal weight of the entire heating system 2 and the crucible 3.

[0068] During installation, the air inlet pipe 4-5 passes through the left fixing hole 4-13 of the support base 4-11, and then connects to the air inlet pipe 4-5 through the left rotating joint 4-4, forming the air inlet channel of the cooling system 4. The air outlet pipe 4-8 passes through the right fixing hole 4-12 of the support base 4-11, and then connects to the air outlet pipe 4-8 through the right rotating joint 4-7, forming the air outlet channel of the cooling system 4.

[0069] The crucible support platform 4-10 is installed in the groove on the upper part of the ventilation base 4-2 and covers the cavity 4-15. The crucible 3 is placed directly on the crucible support platform 4-10, and the heating system 2 is installed inside the annular boss 4-14 to prevent the heating system 2 and the crucible 3 from moving left and right when the system is running.

[0070] The function of the crucible support platform 4-10 is to support the pressure generated by the crucible 3 and the heating system 2 under supergravity, so the material of the crucible support platform 4-10 is high-strength graphite material.

[0071] like Figure 8 As shown, the air inlet pipe 4-5 is connected to the cooling air source outside the experimental chamber through the ventilation bracket on the centrifuge disc rotating arm and the centrifuge slip ring, providing cooling air for the cooling system. The air outlet pipe 4-8 is connected to the ventilation bracket on the centrifuge disc rotating arm and the centrifuge slip ring, and directly leads to the outside of the experimental chamber.

[0072] During operation, the ventilation base 4-2 is used to connect the crucible 3, the heating system 2, and the cooling system 4. Cooling gas is introduced into the cavity 4-15 below the crucible support 4-10 through the air inlet pipe 4-5 and the air inlet channel 4-6. Heat exchange between the bottom of the crucible 3 and the cooling gas reduces the temperature of the melt in the crucible 3. The cooled gas is then discharged to the outside of the hanging cup 1 through the air outlet channel 4-9, the air outlet pipe 4-8, the ventilation bracket of the centrifuge disc rotor, and the centrifuge slip ring. By controlling the ventilation flow rate, pressure, and the degree of hypergravity, the temperature distribution of the crucible along the hypergravity direction is changed, thereby controlling the cooling rate of the melt and achieving controllable and adjustable hypergravity solidification process.

[0073] like Figure 6 As shown, the main function of the thermal insulation system 5 is to prevent the heat of the heating system 3 from being transferred to the surroundings, and includes an outer bottom thermal insulation ring 5-1, a middle bottom thermal insulation ring 5-2, an inner bottom thermal insulation ring 5-3, a fourth thermal insulation cavity plate 5-4, a third thermal insulation cavity plate 5-5, a second thermal insulation cavity plate 5-6, a first thermal insulation cavity plate 5-7, an upper first thermal insulation cover 5-8, an upper second thermal insulation cover 5-9 and an upper third thermal insulation cover 5-10 that are connected into one body;

[0074] The fourth layer of heat-insulating cavity plate 5-4, the third layer of heat-insulating cavity plate 5-5, the second layer of heat-insulating cavity plate 5-6, and the first layer of heat-insulating cavity plate 5-7 are all annular plates and are arranged concentrically from the outside to the inside. There is an annular gap between adjacent heat-insulating cavity plates. The upper end surfaces of the third layer of heat-insulating cavity plate 5-5, the second layer of heat-insulating cavity plate 5-6, and the first layer of heat-insulating cavity plate 5-7 are respectively sealed and fixed with an upper third layer of heat-insulating cover 5-10, an upper second layer of heat-insulating cover 5-9, and an upper first layer of heat-insulating cover 5-8. Adjacent heat-insulating covers are arranged in parallel and have gaps. The upper third layer of heat-insulating cover 5-10, the upper second layer of heat-insulating cover 5-9, and the upper first layer of heat-insulating cover 5-8 respectively seal the upper end surfaces of the third layer of heat-insulating cavity plate 5-5, the second layer of heat-insulating cavity plate 5-6, and the first layer of heat-insulating cavity plate 5-7. The cover, the lower end surfaces of the third layer of insulation cavity plate 5-5, the second layer of insulation cavity plate 5-6 and the first layer of insulation cavity plate 5-7 are respectively provided with an outer bottom insulation ring 5-1, a middle bottom insulation ring 5-2 and an inner bottom insulation ring 5-3 with central openings. Adjacent insulation rings are arranged in parallel and have gaps. The outer bottom insulation ring 5-1 is supported on the support base 4-11 of the cooling system 4. A top cover 5-11 for sealing the upper port of the hanging cup cavity 1-1 of the hanging cup 1 is also provided on the upper third layer of insulation cover 5-10. The upper third layer of insulation cover 5-10 and the top cover 5-11 are fixedly connected by an outer layer fixing screw 5-12. The central openings of the outer bottom insulation ring 5-1, the middle bottom insulation ring 5-2 and the inner bottom insulation ring 5-3 are arranged concentrically and coaxially from bottom to top.

[0075] The inner bottom insulation ring 5-3, the first insulation cavity plate 5-7, and the upper first insulation cover 5-8 form an inner insulation cavity. The inner insulation cavity houses the heating system 2 and the crucible 3. The insulation cover 2-7 of the heating system 2 is fixedly arranged at the top of the inner insulation cavity. The second insulation cavity is formed by the middle bottom insulation ring 5-2, the second insulation cavity plate 5-6, and the upper second insulation cover 5-9. The third insulation cavity is formed by the outer bottom insulation ring 5-1, the third insulation cavity plate 5-5, and the upper third insulation cover 5-10. The fourth insulation cavity is formed by the outer bottom insulation ring 5-1, the fourth insulation cavity plate 5-4, and the upper third insulation cover 5-10.

[0076] In a specific embodiment, the outer bottom insulation ring 5-1, the middle bottom insulation ring 5-2, and the inner bottom insulation ring 5-3 are all circular plates, and their thickness can be selected based on the maximum temperature of the heating system 2. The fourth layer insulation cavity plate 5-4, the third layer insulation cavity plate 5-5, the second layer insulation cavity plate 5-6, and the first layer insulation cavity plate 5-7 are all cylindrical plates, which are metal insulation screens or ceramic insulation screens. Their thickness can be selected based on the maximum temperature of the heating system 2. The upper first layer insulation cover 5-8, the upper second layer insulation cover 5-9, and the upper third layer insulation cover 5-10 are all flat circular plates, and their thickness can be selected based on the maximum temperature of the heating system 2. The top cover 5-11 is made of WMo alloy. The outer layer fixing screw 5-12 and the inner layer fixing screw 5-13 are both WMo metal screws.

[0077] The inner bottom insulation ring 5-3, the first insulation cavity plate 5-7, and the upper first insulation cover 5-8 are welded together to form an inner insulation cavity. The middle bottom insulation ring 5-2, the second insulation cavity plate 5-6, and the upper second insulation cover 5-9 are welded together to form a second insulation cavity. The outer bottom insulation ring 5-1, the third insulation cavity plate 5-5, and the upper third insulation cover 5-10 are welded together to form a third insulation cavity.

[0078] The fourth layer of insulation cavity plate 5-4 and the outer bottom insulation ring 5-1 and the upper third layer of insulation cover 5-10 are welded together, and fixed to the top cover 5-11 by four outer layer fixing screws 5-12, and the top cover 5-11 is fixed to the hanging cup 1 by screws, which can increase the rigidity of the first, second and third layers of insulation cavity.

[0079] The first and second insulation cavities are connected to the upper second insulation cover 5-9 through the inner fixing screw 5-13 to form an integral structure, providing the overall structural strength and rigidity of the insulation system 5 and ensuring the stability of the insulation system 5.

[0080] like Figure 8 As shown, after the device is assembled, the cable for heating system 2 extends to the outside of hanging cup 1, then passes through the cable on the centrifuge disc arm and connects to the ground power supply system via an electrical slip ring. The temperature-control thermocouple extends to the outside of hanging cup 1, then passes through a fixed bracket on the centrifuge disc arm and connects to the ground temperature control system via an electrical slip ring.

[0081] The cooling gas can be liquid nitrogen, compressed air, etc. The cooling gas temperature is not higher than 5°C and the pressure is not higher than 5MPa, but the pressure is controllable and adjustable. The cooling gas type can be changed according to the temperature gradient requirements.

[0082] The invention is suitable for a 1g-5000g hypergravity environment and a temperature ranging from room temperature to 1700°C.

[0083] The interface between centrifugal high gravity coagulation device and centrifuge is shown in Figure 8 .

[0084] The heating system 2 of the centrifugal high gravity coagulation device of the present invention includes but is not limited to two independent heating zones. Therefore, during use, one system can realize two coagulation schemes, which are specifically described as follows:

[0085] 1. The first set of solidification schemes: high-throughput preparation of materials by centrifugal ultra-gravity, see Figure 9 .

[0086] Before the experiment, the alloy melting temperature and centrifugal main engine speed are determined according to the type of alloy to be cast. The following details the use and operation process of the invention:

[0087] Step 1: Install the centrifugal high-gravity solidification device on the disc rotor of the rotating arm of the ultra-gravity centrifuge. The heating system 2, thermocouple, and cooling system 4 on the device are connected to the ground power supply system, temperature control system, and cooling air source respectively through the cable bracket, ventilation bracket, and electrical slip ring on the centrifuge disc rotating arm. Place the alloy sample to be solidified in the crucible 3 of the centrifugal high-gravity solidification device.

[0088] Step 2: Start the vacuum system to make the vacuum degree in the experimental chamber of the ultragravity centrifuge reach 10 -2 Pa;

[0089] Step 3: Wait until the vacuum degree in the experimental chamber reaches 10 -2 After Pa, the heating system 2 in the centrifugal high gravity coagulation device is started;

[0090] Step 4: When the temperature of the crucible 3 detected by the thermocouple reaches 0.8 times the melting point of the alloy sample, start the ultragravity centrifuge; specifically, the ultragravity centrifuge can be started while heating.

[0091] Step 5: After the speed of the ultragravity centrifuge reaches the experimentally set speed, the crucible 3 is continuously heated by the heating system 2 until the alloy sample is completely melted into a melt, and the speed is maintained at the experimentally set speed for 10 minutes;

[0092] Step 6: The heating power of heating system 2 is controlled by the ground temperature control system to keep the ultragravity centrifuge running. The cooling rates in the upper and lower heating chambers of heating system 2, i.e., the cooling rates in the upper and lower heating zones, are controlled to allow sufficient time for elements of different densities in the melt to separate out in layers under the action of centrifugal force. This allows the solidified alloy samples to have different alloy compositions at different heights, thus achieving the goal of preparing multiple alloy compositions in a single pass, thereby realizing high-throughput preparation of materials solidified by ultragravity.

[0093] Step 7: When the sample is completely solidified, turn off the heating system 2 and make judgments and take action:

[0094] When the temperature of the crucible 3 detected by the thermocouple drops below the solidus temperature of the alloy, the ultragravity centrifuge is turned off;

[0095] When the temperature of the crucible 3 detected by the thermocouple drops below 200° C., the vacuum system is turned off.

[0096] 2. The second solidification scheme: directional solidification of materials under centrifugal high gravity, see Figure 10

[0097] Before the experiment, the alloy melting temperature, temperature gradient and centrifuge main engine speed are determined according to the type of molten alloy. The following details the use and operation process of the invention:

[0098] Step 1: Install the centrifugal high-gravity solidification device on the disc rotor of the rotating arm of the ultra-gravity centrifuge. The heating system 2, thermocouple, and cooling system 4 on the device are connected to the ground power supply system, temperature control system, and cooling air source respectively through the cable bracket, ventilation bracket, and electrical slip ring on the centrifuge disc rotating arm. Place the alloy sample to be solidified in the crucible 3 of the centrifugal high-gravity solidification device.

[0099] Step 2: Start the vacuum system to make the vacuum degree in the experimental cabin of the ultragravity centrifuge reach 10-2Pa;

[0100] Step 3: After the vacuum degree in the experimental chamber reaches 10-2Pa, start the heating system 2 in the centrifugal high gravity solidification device;

[0101] Step 4: When the temperature of the crucible 3 detected by the thermocouple reaches 0.8 times the melting point of the alloy sample, start the ultragravity centrifuge; specifically, the ultragravity centrifuge can be started while heating.

[0102] Step 5: After the speed of the ultragravity centrifuge reaches the experimentally set speed, the crucible 3 is continuously heated by the heating system 2 until the alloy sample is completely melted, and the crucible is maintained at the experimentally set speed for 10 minutes;

[0103] Step 6:

[0104] The heating power of the heating system 2 is controlled by the temperature control system on the ground to keep the ultragravity centrifuge working. The temperature in the upper heating chamber of the heating system 2 is controlled to remain unchanged while the temperature in the lower heating chamber is reduced. That is, the temperature of the upper heating zone is kept unchanged while the temperature of the lower heating zone is reduced. At the same time, the cooling system 4 is controlled to start working to cool the bottom of the crucible 3, thereby forming a temperature gradient in the crucible 3 that gradually increases from the bottom to the top, thereby achieving directional solidification under ultragravity conditions.

[0105] During the specific implementation process, the temperature gradient required for solidification is used to determine the amount of cooling gas required to lower the temperature of the alloy melt per unit time through calculation, and then the temperature, pressure and flow rate of the cooling gas are determined to control the position of the solidification interface, thereby forming the required temperature gradient at the liquid-solid interface at the solidification front.

[0106] During the experiment, the temperature gradient during the solidification process is controllable and adjustable by changing the size of the hypergravity, the temperature, flow, pressure and time of the cooling gas. The cooling system 4 is then coordinated with the heating system 2 to achieve different temperature gradient requirements.

[0107] Step 7: When the sample is completely solidified, turn off the heating system 2 and make judgments and take action:

[0108] When the temperature of the crucible 3 detected by the thermocouple drops below the solidus temperature of the alloy, the ultragravity centrifuge is turned off;

[0109] When the temperature of the crucible 3 detected by the thermocouple drops below 200° C., the heating system 2 , the cooling system 4 and the vacuum system are shut down.

Claims

1. A centrifugal high gravity coagulation device, characterized in that: The invention comprises a hanging cup (1), a heating system (2), a crucible (3), a cooling system (4) and a heat preservation system (5); the bottom of the hanging cup (1) is provided with a cooling system (4); the heating system (2), the crucible (3) and the heat preservation system (5) are installed above the cooling system (4); the crucible (3) is located in the heating system (2); and the heat preservation system (5) is provided in the hanging cup (1) outside the heating system (2); The cooling system (4) comprises a heat-insulating floor (4-1), a ventilation base (4-2), an insulation ring (4-3), a crucible support platform (4-10) and a support base (4-11); the heat-insulating floor (4-1) is installed at the bottom of the hanging cup (1); the ventilation base (4-2) is fixedly installed in the center of the heat-insulating floor (4-1); the heat-insulating ring (4-3) is arranged on the heat-insulating floor (4-1) around the ventilation base (4-2); a cavity (4-15) is provided on the top of the ventilation base (4-2); the crucible support platform (4-10) is provided at the upper end of the cavity (4-15) for sealing; and air inlet channels (4-15) are respectively provided on both sides of the middle of the ventilation base (4-2). 6) and an air outlet channel (4-9), the upper ends of the air inlet channel (4-6) and the air outlet channel (4-9) are both connected to the cavity (4-15), one end of the air inlet pipe (4-5) and the air outlet pipe (4-8) passes horizontally through the heat insulation ring (4-3) and then extends into the ventilation base (4-2) and is respectively connected to the lower ends of the air inlet channel (4-6) and the air outlet channel (4-9); the other ends of the air inlet pipe (4-5) and the air outlet pipe (4-8) pass through the heat insulation ring (4-3) and then extend upward and are respectively connected to an external cooling air source and the outside of the experimental cabin; a support base (4-11) for supporting and installing the insulation system (5) is provided on the heat insulation ring (4-3); The thermal insulation system (5) comprises an outer bottom thermal insulation ring (5-1), a middle bottom thermal insulation ring (5-2), an inner bottom thermal insulation ring (5-3), a fourth thermal insulation cavity plate (5-4), a third thermal insulation cavity plate (5-5), a second thermal insulation cavity plate (5-6), a first thermal insulation cavity plate (5-7), an upper first thermal insulation cover (5-8), an upper second thermal insulation cover (5-9) and an upper third thermal insulation cover (5-10) which are connected into one body; the fourth thermal insulation cavity plate (5-4), the third thermal insulation cavity plate (5-5), the second thermal insulation cavity plate (5-6) and the first thermal insulation cavity plate (5-7) are all annular plates and are arranged at intervals from the outside to the inside concentrically; the upper end surfaces of the third thermal insulation cavity plate (5-5), the second thermal insulation cavity plate (5-6) and the first thermal insulation cavity plate (5-7) are respectively sealed and fixed with the upper third thermal insulation cover (5-10) The lower end surfaces of the second-layer insulation cover (5-9), the first-layer insulation cover (5-8), the third-layer insulation cavity plate (5-5), the second-layer insulation cavity plate (5-6), and the first-layer insulation cavity plate (5-7) are respectively provided with an outer bottom insulation ring (5-1) with a central opening, a middle bottom insulation ring (5-2), and an inner bottom insulation ring (5-3), the outer bottom insulation ring (5-1) is supported on a support base (4-11) of the cooling system (4), and a top cover (5-11) for sealing the upper port of the hanging cup (1) is further provided on the third-layer insulation cover (5-10), the third-layer insulation cover (5-10) and the top cover (5-11) are fixedly connected by an outer-layer fixing screw (5-12), and the central openings of the outer bottom insulation ring (5-1), the middle bottom insulation ring (5-2), and the inner bottom insulation ring (5-3) are arranged concentrically and coaxially.

2. The centrifugal high gravity coagulation device according to claim 1, characterized in that: The hanging cup (1) is fixedly mounted on the end of the rotating arm of the ultragravity centrifuge.

3. The centrifugal high gravity coagulation device according to claim 1, characterized in that: The hanging cup (1) comprises a hanging cup cavity (1-1) and a hanging ear hole (1-2); a heating system (2), a crucible (3), a cooling system (4) and a heat preservation system (5) are placed in the hanging cup cavity (1-1); and a hanging ear hole (1-2) for connecting to the end of a rotating arm of an ultragravity centrifuge is provided on the side of the hanging cup cavity (1-1).

4. The centrifugal high gravity coagulation device according to claim 1, characterized in that: The heating system (2) comprises a heating chamber, a heating furnace tube, a heating wire and a heat-insulating cover (2-7). The heating chamber is divided into an upper heating chamber (2-1) located at the upper part and a lower heating chamber (2-4) located at the lower part. The lower heating chamber (2-4) is installed on the cooling system (4). The upper end of the upper heating chamber (2-1) is provided with a heat-insulating cover (2-7). The inner wall of the lower heating chamber (2-4) is provided with a lower heating furnace tube (2-5), and the lower heating furnace tube (2-5) is provided with a lower heating wire (2-6). The inner wall of the upper heating chamber (2-1) is provided with an upper heating furnace tube (2-2), and the upper heating furnace tube (2-2) is provided with an upper heating wire (2-3).

5. The centrifugal high gravity coagulation device according to claim 1, characterized in that: The crucible (3) is placed in the heating chamber of the heating system (2), and an upper thermocouple hole (3-1) and a lower thermocouple hole (3-2) for installing a thermocouple are provided on the upper and lower parts respectively.

6. The centrifugal high gravity coagulation device according to claim 1, characterized in that: The inner bottom insulation ring (5-3), the first layer insulation cavity plate (5-7) and the upper first layer insulation cover (5-8) form an inner insulation cavity, the inner insulation cavity contains the heating system (2) and the crucible (3), and the top of the inner insulation cavity is fixed with the insulation cover (2-7) of the heating system (2); the fourth layer insulation cavity plate (5-4) and the outer bottom insulation ring (5-1) and the upper third layer insulation cover (5-10) are welded together, and at the same time, four The outer fixing screw (5-12) is fixed to the top cover (5-11), and the top cover (5-11) is fixed to the hanging cup (1) by screws, which can increase the rigidity of the first, second and third insulation cavities; the first and second insulation cavities are connected to the upper second insulation cover (5-9) by the inner fixing screw (5-13) to form an integral structure, providing the overall structural strength and rigidity of the insulation system (5), and ensuring the stability of the insulation system (5).

7. A coagulation test method applied to the centrifugal high gravity coagulation device according to any one of claims 1 to 6, characterized in that: The method includes the following processes: The first step is to install the centrifugal ultra-gravity solidification device on the disc rotor of the rotating arm of the ultra-gravity centrifuge, and place the alloy sample to be solidified in the crucible (3) of the centrifugal ultra-gravity solidification device; Step 2: Start the vacuum system to make the vacuum degree in the experimental chamber of the ultragravity centrifuge reach 0.01Pa; Step 3: After the vacuum degree in the experimental chamber reaches 0.01 Pa, start the heating system (2) in the centrifugal high gravity solidification device; Step 4: When the temperature of the crucible (3) detected by the thermocouple reaches 0.8 times the melting point of the alloy sample, start the ultra-gravity centrifuge; Step 5: After the speed of the ultragravity centrifuge reaches the speed set in the experiment, the crucible (3) is continuously heated by the heating system (2) until the alloy sample is completely melted into a melt, and the crucible (3) is kept at the speed set in the experiment for 10 minutes; Step 6: Control the heating power of the heating system (2) and the cooling rate in the upper and lower heating chambers of the heating system (2) so that elements with different densities in the melt have enough time to separate in layers under the action of centrifugal force, so that the solidified alloy samples have different alloy compositions at different heights, thereby achieving the purpose of preparing multiple alloy compositions in a single step; Step 7: When the sample is completely solidified, turn off the heating system (2) and make a judgment: When the temperature of the crucible (3) detected by the thermocouple drops below the solidus temperature of the alloy, the ultragravity centrifuge is turned off; When the temperature of the crucible (3) detected by the thermocouple drops below 200°C, the vacuum system is turned off.

8. A coagulation test method applied to the centrifugal high gravity coagulation device according to any one of claims 1 to 6, characterized in that: The method includes the following processes: The first step is to install the centrifugal ultra-gravity solidification device on the disc rotor of the rotating arm of the ultra-gravity centrifuge, and place the alloy sample to be solidified in the crucible (3) of the centrifugal ultra-gravity solidification device; Step 2: Start the vacuum system to make the vacuum degree in the experimental cabin of the ultragravity centrifuge reach 10-2Pa; Step 3: After the vacuum degree in the experimental chamber reaches 10-2Pa, start the heating system (2) in the centrifugal high gravity solidification device; Step 4: When the temperature of the crucible (3) detected by the thermocouple reaches 0.8 times the melting point of the alloy sample, start the ultra-gravity centrifuge; Step 5: After the speed of the ultragravity centrifuge reaches the speed set in the experiment, the crucible (3) is continuously heated by the heating system (2) until the alloy sample is completely melted, and the crucible is kept at the speed set in the experiment for 10 minutes; Step 6: Control the heating power of the heating system (2), control the temperature in the upper heating chamber of the heating system (2) to remain unchanged, reduce the temperature in the lower heating chamber, and at the same time control the cooling system (4) to start working to cool the bottom of the crucible (3), thereby forming a temperature gradient in the crucible (3) with the temperature gradually increasing from the bottom to the top; Step 7: When the sample is completely solidified, turn off the heating system (2) and make a judgment: When the temperature of the crucible (3) detected by the thermocouple drops below the solidus temperature of the alloy, the ultragravity centrifuge is turned off; When the temperature of the crucible (3) detected by the thermocouple drops below 200°C, the cooling system (4) and the vacuum system are turned off.

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