Full-automatic cold and hot circulating equipment for regulating and controlling energy state of amorphous alloy

Abstract

The invention relates to the technical field of equipment for adjusting the energy state of amorphous alloy, in particular to full-automatic cold and hot circulating equipment for adjusting the energy state of the amorphous alloy. The device is composed of an oil bath heating device, a liquid nitrogen cooling device and a mechanical arm device. The rejuvenation degree of the amorphous alloy is controlled by adjusting the oil bath temperature, the cycle time and the total cycle index, and then the energy state of the amorphous alloy is adjusted and controlled, so that the plasticity of the amorphous alloy is improved. According to the invention, the cold and hot circulation experiment can be fully automatically carried out, and partial defects of the current cold and hot circulation experiment, such as time and labor consumption and easy frostbite, are solved. On the premise that the amorphous state characteristics of the amorphous alloy are not changed, the energy state of the amorphous alloy is effectively adjusted, namely, the internal atomic configuration of the amorphous alloy structure is adjusted, the disorder degree of the microscopic atomic structure is increased, the high-strength characteristic of the amorphous alloy can be combined with the excellent plastic deformation capacity, and the amorphous alloy is expected to be widely used in the engineering field.

Description

Technical Field

[0001] The present invention relates to the technical field of equipment for regulating the energy state of amorphous alloys, and in particular to a fully automatic hot and cold cycle device for regulating the energy state of amorphous alloys. Background Art

[0002] Amorphous alloys can generally be prepared by rapidly cooling molten metal. Generally speaking, any material can be amorphous if the cooling rate is fast enough. Since the first report in the 1960s, amorphous alloys have attracted widespread attention and great research interest due to their unique physical and chemical properties.

[0003] Unlike traditional crystalline materials, amorphous alloys do not have defects such as dislocations and twins. From a microscopic perspective, the atomic arrangement of amorphous alloys embodies the characteristics of long-range disorder and short-range order. It is precisely because of its unique atomic configuration that this new type of structural material has excellent mechanical properties, such as high strength, large elastic limit, good wear resistance, etc., and has broad application prospects in the engineering field. Compared with crystalline alloys, the plastic deformation of amorphous alloys is accompanied by a softening effect, and the plastic flow is usually confined to the shear band. Under uniaxial tension, local shear bands dominate the plastic deformation of bulk amorphous alloys, resulting in catastrophic damage and seriously hindering their practical application. In order to overcome the above problems, researchers have been working hard to explore new components or processing technologies to seek bulk amorphous alloys with good plasticity.

[0004] During annealing, amorphous alloys relax to a low energy state, at which point they are usually brittle. The opposite process is called rejuvenation, which refers to the process of absorbing external energy to make amorphous alloys transition from a lower energy state to a higher energy state, that is, rejuvenation allows amorphous alloys to enter a high energy, ductile state. Amorphous alloys in a rejuvenated state usually have improved plasticity, catalysis and tribological properties, and the mechanical properties of amorphous alloys can be optimized by rejuvenation methods. At present, there are many methods to achieve the rejuvenation of amorphous alloys. The basic principle is that by applying a certain amount of energy less than its crystallization activation energy to the amorphous alloy in an appropriate manner, it is possible to rejuvenate the amorphous alloy. For example, the surface shot peening method, a simple room temperature winding method, modulates the rejuvenation of amorphous alloys and improves their plasticity by applying a long-term fixed stress; the notch method, by changing the geometric shape of the amorphous alloy to achieve an increase in its energy state; the chemical treatment method, using alkaline conditions to treat amorphous alloys can also achieve a significant increase in energy. In addition, there are ion irradiation methods, strong deformation methods, and hot and cold cycle methods. Among them, the hot and cold cycle method is a simple hot and cold cycle treatment process, which is to immerse the amorphous alloy in liquid nitrogen or liquid helium, and then quickly heat it to room temperature and keep it for a few minutes, and repeat this process many times. After dozens of cycles, the energy of the amorphous alloy increases. After the hot and cold cycle, the hardness of the amorphous alloy is significantly reduced, and the macroscopic plasticity is increased. Compared with other methods, the hot and cold cycle method has the advantages of being non-destructive, not changing the shape, not limiting the sample size, and not generating shear bands. More importantly, it is easy to implement in industry and has low processing costs.

[0005] In summary, the prior art does not have a more accurate cyclic treatment and a more detailed research technical solution for the rejuvenation of amorphous alloys, and therefore a more accurate cyclic treatment and a more detailed research on this phenomenon are needed. Summary of the invention

[0006] The purpose of the present invention is to avoid the shortcomings of the prior art and provide a fully automatic hot and cold cycle equipment for regulating the energy state of amorphous alloys, which can achieve rejuvenation of amorphous alloys and improve their room temperature plastic properties without changing the amorphous state of the amorphous alloys.

[0007] To achieve the above-mentioned purpose, the technical solution adopted by the present invention is as follows: the fully automatic hot and cold cycle equipment for regulating the energy state of amorphous alloys comprises an oil bath heating device, a liquid nitrogen cooling device and a mechanical arm device;

[0008] The mechanical arm device comprises a base, on which a plurality of connecting rods are connected via a plurality of joints, a sample clamp is arranged on the uppermost connecting rod, and the joints are composed of a motor, a reducer, a transmission mechanism and an encoder.

[0009] The oil bath heating device comprises a first box body, a first box cover is hingedly provided on the upper part of the first box body, a support is provided in the first box body, an oil bath barrel is provided on the support, the oil bath barrel is composed of an inner and outer layer of the oil bath barrel and a middle insulation layer, a magnetic stirrer is provided at the bottom of the oil bath barrel, and a sample tank is provided on the upper part of the oil bath barrel;

[0010] The liquid nitrogen cooling device comprises a second box body, in which a sample placement platform for placing samples to be cooled and a nitrogen storage tank for storing liquid nitrogen are arranged, and the nitrogen storage tank is connected to a liquid nitrogen tank for providing liquid nitrogen arranged outside the second box body through an input pipeline.

[0011] The base is the supporting and fixing part of the mechanical arm device. The base and the connecting rod are made of aluminum alloy. The sample clamp of the mechanical arm device realizes the clamping and movement of the sample through the controller. The joint drives the connecting rod to realize the movement and transmit the force. The sample clamp is provided with a clamping claw for clamping the sample.

[0012] The oil bath barrel is of circular structure, and a heater for heating the oil bath barrel is arranged under the oil bath barrel. The heater is mounted on a support, and the support is used to fix and support the heater. The support is fixedly connected to the first box body. A temperature sensor is also installed in the middle of the oil bath barrel, and the insulation layer is used to keep the heat warm to ensure that the working efficiency of the instrument is improved; the magnetic stirrer sets a safe temperature and ensures uniform heating; the temperature sensor detects the temperature in real time to ensure that the set temperature is accurately reached; the sample slot is directly placed on the oil bath barrel for placing samples, and a fixed switch is installed at the switch between the first box cover and the first box body.

[0013] The sample placement platform and the nitrogen storage tank are fixed in the box body through an insulating fixing bracket. The nitrogen storage tank is also provided with an output pipe. Liquid nitrogen transports the liquid nitrogen in the liquid nitrogen tank into the nitrogen storage tank through the input pipe and leaves the nitrogen storage tank through the output pipe. The input pipe, the output pipe and the second box body are all provided with heat insulation materials. The sample placement platform is provided with a temperature sensor for measuring the surface temperature of the sample placement platform. The temperature tested by the temperature sensor is the ambient temperature of the sample. The test result is fed back to the control system to change the liquid nitrogen transmission speed to achieve the control temperature. A second box cover is provided on the upper part of the second box body. The second box body and the second box cover are used for heat preservation of the entire system. The second box cover is used for placing and taking out the test sample.

[0014] The upper part of the sample placement platform is also provided with a cooling temperature control device and a cable.

[0015] The nitrogen storage tank is provided with a baffle, a heat transfer rod, a liquid level sensor, and a heat transfer shock absorbing device. The baffle is used to intercept liquid nitrogen and make it drip into the nitrogen storage tank to prevent it from directly contacting the gas outlet and the heat transfer rod. The heat transfer rod and the heat transfer shock absorbing device are used to contact liquid nitrogen and nitrogen gas and cool them. The heat transfer shock absorbing device is used to buffer vibrations. The liquid level sensor is used to measure the liquid level height.

[0016] The beneficial effects of the present invention are as follows: the fully automatic hot and cold cycle equipment for regulating the energy state of amorphous alloys can be used for fully automatic hot and cold cycle treatment of amorphous alloys of various components through the cooperation of an oil bath heating device, a liquid nitrogen cooling device and a mechanical arm device, and is not limited to the size of amorphous alloy samples, and can achieve wide temperature range regulation. By adjusting the oil bath temperature, cycle time, and total number of cycles, the degree of rejuvenation of the amorphous alloy can be controlled, and the energy state of the amorphous alloy can be adjusted and regulated, so as to improve the plastic properties of the amorphous alloy. The present invention can fully automatically perform hot and cold cycle experiments, solving some defects of current hot and cold cycle experiments, such as time-consuming, labor-intensive, and easy to frostbite. The present invention effectively adjusts the energy state of the amorphous alloy without changing the amorphous characteristics of the amorphous alloy, that is, adjusts the internal atomic configuration of the amorphous alloy structure, increases the disorder of the microscopic atomic structure, and then can combine the high strength characteristics of the amorphous alloy with the excellent plastic deformation ability, so as to be widely adopted in the engineering field. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the structure of the cold and hot cycle device of the present invention;

[0018] Figure 2 It is a schematic diagram of the structure of the mechanical arm of the present invention;

[0019] Figure 3 It is a schematic diagram of the structure of the oil bath heating device of the present invention;

[0020] Figure 4 For the present invention Figure 3 A schematic diagram of a top view structure;

[0021] Figure 5 This is a schematic diagram of the structure of the liquid nitrogen cooling device of the present invention;

[0022] Figure 6 For the present invention Figure 5 Schematic diagram of the enlarged structure;

[0023] Figure 7 It is a schematic diagram of the hot and cold cycle control program when implementing the present invention.

[0024] In the figure, 100, mechanical arm device; 101, base; 102, joint; 103, connecting rod; 104, sample clamp; 200, oil bath heating device; 201, support; 202, heater; 203, magnetic stirrer; 204, temperature sensor; 205, insulation layer; 206, inner and outer layers of oil bath barrel; 207, sample slot; 208, first box cover; 209, first box body; 210, fixed switch; 30 0. Liquid nitrogen cooling device; 301. Cable; 302. Output pipeline; 303. Input pipeline; 304 Liquid nitrogen tank; 305. Cooling and temperature control device; 306 Insulation fixing bracket; 307. Second box body; 308. Second box cover; 309. Sample placement platform; 310. Temperature sensor; 311. Baffle; 312. Nitrogen storage tank; 313. Heat transfer rod; 314. Liquid level sensor; 315. Heat transfer and shock absorption device. DETAILED DESCRIPTION

[0025] The principles and features of the present invention are described below in conjunction with the accompanying drawings. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.

[0026] In order to achieve the above object, the present invention provides the following specific implementation methods:

[0027] Example 1: Figure 1 , 2 , 3, and 4, a fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy, comprising an oil bath heating device 200, a liquid nitrogen cooling device 300, and a robotic arm device 100;

[0028] The robot arm device 100 includes a base 101, on which a plurality of connecting rods 103 are connected via a plurality of joints 102, a sample clamp 104 is arranged on the uppermost connecting rod, and the joint 102 is composed of a motor, a reducer, a transmission mechanism and an encoder.

[0029] The oil bath heating device 200 comprises a first box body 209, a first box cover 208 is hingedly provided on the upper part of the first box body 209, a support 201 is provided in the first box body 209, an oil bath barrel is provided on the support 201, the oil bath barrel is composed of an inner and outer layer 206 of the oil bath barrel and a heat-insulating layer 205 in the middle, a magnetic stirrer 203 is provided at the bottom of the oil bath barrel, and a sample tank 207 is provided on the upper part of the oil bath barrel;

[0030] The liquid nitrogen cooling device 300 includes a second box body 307, in which a sample placement platform 309 for placing samples to be cooled and a nitrogen storage tank 312 for storing liquid nitrogen are arranged. The nitrogen storage tank 312 is connected to a liquid nitrogen tank 304 for providing liquid nitrogen arranged outside the second box body 307 through an input pipe 303.

[0031] The base 101 is the supporting and fixing part of the robotic arm device. The base 101 and the connecting rod 103 are made of aluminum alloy. The sample clamp 104 of the robotic arm device realizes the clamping and movement of the sample through the controller. The joint 102 drives the connecting rod 103 to realize movement and transmit force. The sample clamp 104 is provided with a clamping claw for clamping the sample.

[0032] The oil bath is a circular structure, and a heater 202 for heating the oil bath is provided below the oil bath. The heater 202 is installed on a support 201, and the support 201 is used to fix and support the heater 202. The support 201 is fixedly connected to the first box body 209. A temperature sensor 204 is also installed in the middle of the oil bath, and the insulation layer 205 is used to keep the heat warm to ensure that the working efficiency of the instrument is improved; the magnetic stirrer 203 sets a safe temperature and ensures uniform heating; the temperature sensor 204 detects the temperature in real time to ensure that the set temperature is accurately reached; the sample slot 207 is directly placed on the oil bath for placing samples, and a fixed switch 210 is installed at the switch between the first box cover 208 and the first box body 209.

[0033] like Figure 5 and Figure 6 As shown, the sample placement platform 309 and the nitrogen storage tank 312 are fixed in the box body through the insulation fixing bracket 306, and the nitrogen storage tank 312 is also provided with an output pipe 302. The liquid nitrogen transports the liquid nitrogen in the liquid nitrogen tank 304 into the nitrogen storage tank 312 through the input pipe 303, and leaves the nitrogen storage tank 312 through the output pipe 302; the input pipe 303, the output pipe 302 and the second box body 307 are all provided with heat insulation materials, and the sample placement platform 309 is provided with a temperature sensor 310 for measuring the surface temperature of the sample placement platform. The temperature tested by the temperature sensor 310 is the ambient temperature of the sample, and the test result is fed back to the control system to change the liquid nitrogen transmission speed to achieve the control temperature. The second box body 307 is provided with a second box cover 308 on the upper part, and the second box body 307 and the second box cover 308 are used for heat preservation of the entire system, and the second box cover 308 is used for placing and taking out the test sample.

[0034] A cooling temperature control device 305 and a cable 301 are also provided on the upper part of the sample placement platform 309 .

[0035] A baffle 311, a heat transfer rod 313, a liquid level sensor 314, and a heat transfer shock absorbing device 315 are provided inside the nitrogen storage tank 312. The baffle 311 is used to intercept liquid nitrogen and make it drip into the nitrogen storage tank 312 to prevent it from directly contacting the gas outlet and the heat transfer rod 313. The heat transfer rod 313 and the heat transfer shock absorbing device 315 are used to contact liquid nitrogen and nitrogen gas and cool them. The heat transfer shock absorbing device 315 is used to buffer vibrations. The liquid level sensor 314 is used to measure the liquid level.

[0036] The working principle of the fully automatic hot and cold cycle equipment for regulating the energy state of amorphous alloys is as follows: after the hot and cold cycle plan is determined, the experimental program is input into the control system, the test sample is placed on the sample clamp 104 of the robot arm 100, the operating system starts the experiment, and the sample is circulated and transported between the sample slot 207 of the oil bath heating device 200 and the sample placement platform 309 of the liquid nitrogen cooling device 300 by the robot arm 100. The robot arm 100 and the first box cover 208 and the second box cover 308 work together through the control system. After each stage of the experiment, automatic sampling is realized until the end of the experiment.

[0037] The equipment provided by the invention can be widely used in the research and production of amorphous alloy materials, including but not limited to new structural materials, functional materials, biomedical materials, etc.

[0038] The method for preparing a bulk amorphous alloy using the fully automatic hot and cold cycle equipment for regulating the energy state of the amorphous alloy provided by the present invention, wherein the amorphous alloy adopts a Zr-based high-strength amorphous alloy system, specifically comprises the following steps:

[0039] Step 1: Determine the hot-cold cycle scheme, subject the bulk amorphous alloy sample to hot-cold cycle treatment, including heat treatment and cryogenic treatment, the heat treatment temperature, i.e., the oil bath temperature T1, is set below the glass transition temperature Tg of the amorphous alloy sample used, and the cryogenic treatment temperature is T2, i.e., the liquid nitrogen temperature;

[0040] The oil bath temperature T1 and the cryogenic treatment temperature T2 are determined by the specific amorphous alloy system. The T1 temperature range of the Zr-based amorphous alloy is 270K-475K, and the T2 temperature is 77K. The total number of hot and cold cycles n needs to be tested according to the Zr-based amorphous alloy system used. For the Zr-based amorphous alloy system, the heat treatment time t1 and the cryogenic treatment time t2 are set to 800s, and the oil bath temperature T1 is set to 0.4Tg-0.7Tg.

[0041] Bulk amorphous alloy samples are cylindrical or cubic specimens;

[0042] Step 2: Carry out hot and cold cycle process, by setting different total number of hot and cold cycle n, heat treatment time t1, deep cold treatment time t2, oil bath temperature T1, deep cold treatment temperature T2 parameters, conduct multiple experimental measurements, and select the optimal parameters.

[0043] The characteristic parameters of the hot and cold cycles are precisely controlled by the central control system. After the hot and cold cycle treatment, compression is carried out at room temperature to verify the rejuvenation effect. The central control system automatically adjusts the flow rate and temperature of the cooling medium according to real-time monitored parameters such as temperature and pressure to ensure that the sample achieves the optimal cooling rate and temperature gradient during the cycle.

[0044] Figure 7As shown, T1, T2, t1, t2, and n are respectively the oil bath temperature, the liquid nitrogen control temperature, the liquid nitrogen bath duration, the oil bath duration, and the total number of cycles.

[0045] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A fully automatic hot and cold cycle device for regulating the energy state of amorphous alloys, characterized in that: It comprises an oil bath heating device (200), a liquid nitrogen cooling device (300) and a mechanical arm device (100); The mechanical arm device (100) comprises a base (101), on which a plurality of connecting rods (103) are connected via a plurality of joints (102), and a sample clamp (104) is arranged on the uppermost connecting rod. The oil bath heating device (200) comprises a first box body (209), the upper part of the first box body (209) is provided with a first box cover (208) by hinged connection, a support (201) is provided inside the first box body (209), an oil bath barrel is provided on the support (201), the oil bath barrel is composed of an inner and outer layer (206) of the oil bath barrel and a heat-insulating layer (205) in the middle, a magnetic stirrer (203) is provided at the bottom of the oil bath barrel, and a sample tank (207) is provided at the upper part of the oil bath barrel; The liquid nitrogen cooling device (300) comprises a second box (307), wherein a sample placement platform (309) for placing a sample to be cooled and a nitrogen storage tank (312) for storing liquid nitrogen are arranged in the second box (307), and the nitrogen storage tank (312) is connected to a liquid nitrogen tank (304) for providing liquid nitrogen arranged outside the second box (307) via an input pipe (303).

2. A fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy as claimed in claim 1, characterized in that: The base (101) is a supporting and fixing part of the mechanical arm device. The base (101) and the connecting rod (103) are made of aluminum alloy. The sample clamp (104) of the mechanical arm device realizes the clamping and movement of the sample through a controller. The joint (102) drives the connecting rod (103) to realize movement and transmit force. The sample clamp (104) is provided with a clamping claw for clamping the sample.

3. A fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy as claimed in claim 1 or 2, characterized in that: The joint (102) is composed of a motor, a reducer, a transmission mechanism and an encoder.

4. A fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy as claimed in claim 1, characterized in that: The oil bath barrel is a circular structure, and a heater (202) for heating the oil bath barrel is also arranged below the oil bath barrel, and the heater (202) is installed on a support (201), and the support (201) is used to fix and support the heater (202), and the support (201) is fixedly connected to the first box body (209). A temperature sensor (204) is also installed in the middle of the oil bath barrel, and the insulation layer (205) is used to keep the heat warm to ensure that the working efficiency of the instrument is improved; the magnetic stirrer (203) sets a safe temperature and ensures uniform heating; the temperature sensor (204) detects the temperature in real time to ensure that the set temperature is accurately reached; the sample slot (207) is directly placed on the oil bath barrel for placing samples, and a fixed switch (210) is installed at the switch between the first box cover (208) and the first box body (209).

5. A fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy as claimed in claim 1, characterized in that: The sample placement platform (309) and the nitrogen storage tank (312) are fixed in the box body through an insulating fixing bracket (306); the nitrogen storage tank (312) is also provided with an output pipe (302); liquid nitrogen is transported from the liquid nitrogen tank (304) into the nitrogen storage tank (312) through an input pipe (303) and leaves the nitrogen storage tank (312) through the output pipe 302; thermal insulation materials are provided in the input pipe (303), the output pipe (302) and the second box body (307); The sample placement platform (309) is provided with a temperature sensor (310) for measuring the surface temperature of the sample placement platform. The temperature tested by the temperature sensor (310) is the ambient temperature of the sample. The test result is fed back to the control system so as to change the liquid nitrogen transmission speed to achieve the controlled temperature. A second box cover (308) is provided on the upper part of the second box body (307). The second box body (307) and the second box cover (308) are used for heat preservation of the entire system. The second box cover (308) is used for placing and taking out the test sample.

6. A fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy as claimed in claim 5, characterized in that: A cooling temperature control device (305) and a cable (301) are also provided on the upper part of the sample placement platform (309).

7. A fully automatic hot and cold cycle device for regulating the energy state of an amorphous alloy as described in any one of claims 1 to 6, characterized in that: The nitrogen storage tank (312) is provided with a baffle (311), a heat transfer rod (313), a liquid level sensor (314), and a heat transfer shock absorbing device (315). The baffle (311) is used to intercept liquid nitrogen and make it drip into the nitrogen storage tank (312) to prevent it from directly contacting the gas outlet and the heat transfer rod (313). The heat transfer rod (313) and the heat transfer shock absorbing device (315) are used to contact liquid nitrogen and nitrogen gas and cool them. The heat transfer shock absorbing device (315) is used to buffer vibration. The liquid level sensor (314) is used to measure the liquid level.

Images