A full-automatic cold and hot cycle device for regulating energy state of amorphous alloy

By using a fully automated hot and cold circulation system combined with an oil bath heating and liquid nitrogen cooling device, the energy state of amorphous alloys can be precisely controlled, solving the problems of limited plasticity improvement and time-consuming and labor-intensive operation in existing technologies, and improving the plasticity properties of amorphous alloys.

CN119776631BActive Publication Date: 2026-02-17NORTHWESTERN POLYTECHNICAL UNIV
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Patent Information

Application Number
CN202411834915.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-13
Publication Date
2026-02-17
Estimated Expiration
2044-12-13

AI Technical Summary

Technical Problem

Existing technologies lack accurate methods for regulating the energy state of amorphous alloys through cyclic processing, which limits the improvement of their plasticity during the rejuvenation process. Furthermore, the hot and cold cycling process is time-consuming and labor-intensive, and can easily damage the samples.

Method used

A fully automatic thermal cycling device was designed, including an oil bath heating device, a liquid nitrogen cooling device, and a robotic arm device, to realize automatic thermal cycling of amorphous alloys under amorphous conditions. The energy state of the amorphous alloy is adjusted by controlling the oil bath temperature, cycling time, and number of cycles.

Benefits of technology

This method enables the effective adjustment of the energy state of amorphous alloys without altering their amorphous characteristics, thereby improving their plasticity, simplifying the thermal cycling process, avoiding the risk of frost damage, and making it suitable for amorphous alloy samples of various compositions and sizes.

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Abstract

The present application relates to the technical field of equipment for adjusting energy state of amorphous alloy, and particularly relates to a full-automatic cold and hot cycle equipment for adjusting energy state of amorphous alloy. The equipment is composed of an oil bath heating device, a liquid nitrogen cooling device and a mechanical arm device. By adjusting the oil bath temperature, the cycle time and the total cycle number, the rejuvenation degree of the amorphous alloy is controlled, and then the energy state of the amorphous alloy is adjusted, so as to improve the plasticity of the amorphous alloy. The cold and hot cycle experiment can be automatically carried out, and the defects of the current cold and hot cycle experiment, such as time-consuming, labor-consuming and easy to freeze, are solved. Without changing the amorphous state characteristics of the amorphous alloy, the energy state of the amorphous alloy is effectively adjusted, that is, the atomic configuration in the structure of the amorphous alloy is adjusted, and the disorder degree of the micro-atomic structure is increased, so that the high strength characteristics of the amorphous alloy can be combined with the excellent plastic deformation ability, and the amorphous alloy can be widely used in the engineering field.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of equipment for adjusting energy state of amorphous alloy, and particularly relates to a full-automatic cold-heat cycle equipment for adjusting energy state of amorphous alloy. BACKGROUND

[0002] Amorphous alloy can be generally prepared by rapidly cooling a molten metal liquid. Generally, if the cooling rate is fast enough, any substance can form an amorphous state. Since first reported in the 1960s, amorphous alloy has attracted extensive attention and great research interest due to its unique physical and chemical properties.

[0003] Different from traditional crystalline materials, amorphous alloy does not have defects such as dislocations and twins. From a microscopic point of view, the atomic arrangement of amorphous alloy exhibits the characteristics of long-range disorder and short-range order. Due to its unique atomic configuration, 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, plastic deformation of amorphous alloy is accompanied by softening effect, and plastic flow is usually limited within shear bands. In the uniaxial tension state, local shear bands dominate the plastic deformation of bulk amorphous alloy, leading to catastrophic failure and seriously hindering its practical application. In order to overcome the above problems, researchers have been trying to explore new components or processing technology to seek bulk amorphous alloys with good plasticity.

[0004] During annealing, amorphous alloys relax to a low-energy state, at which point they are typically brittle. The opposite process is called rejuvenation, which refers to the process by which an amorphous alloy absorbs external energy, causing it to transition from a lower energy state to a higher energy state; in other words, rejuvenation brings the amorphous alloy into a high-energy, ductile state. Rejuvenated amorphous alloys usually exhibit improved plasticity, catalytic properties, and tribological properties, and their mechanical properties can be optimized through rejuvenation methods. Currently, there are many methods to achieve rejuvenation of amorphous alloys. The basic principle is to apply an energy lower than its crystallization activation energy to the amorphous alloy in an appropriate manner, which may induce rejuvenation. For example, surface shot peening, a simple room-temperature winding method, modulates the rejuvenation and improves the plasticity of the amorphous alloy by applying a fixed stress for a long time; notching increases the energy state by changing the geometry of the amorphous alloy; chemical treatment, using alkaline conditions to treat the amorphous alloy, can also achieve a significant energy increase. Other methods include ion irradiation, strong deformation, and thermal cycling. One method is the thermal cycling method, a simple process involving immersing an amorphous alloy in liquid nitrogen or liquid helium, then rapidly heating it to room temperature and holding it for several minutes. This cycle is repeated multiple times, and after dozens of cycles, the amorphous alloy's energy level increases. After thermal cycling, the hardness of the amorphous alloy significantly decreases, while its macroscopic plasticity increases. Compared to other methods, the thermal cycling method has advantages such as being non-destructive, not altering the shape, not limiting sample size, and not generating shear bands. More importantly, it is easy to implement industrially and has low processing costs.

[0005] In summary, existing technologies lack more accurate cyclic processing and more detailed research solutions for the rejuvenation of amorphous alloys. Therefore, more accurate cyclic processing and more detailed research are needed for this phenomenon. Summary of the Invention

[0006] The purpose of this invention is to overcome the shortcomings of the prior art and provide a fully automatic hot and cold cycle device for regulating the energy state of amorphous alloys, which can rejuvenate amorphous alloys and improve their room temperature plasticity without changing the amorphous state of the amorphous alloys.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows: a fully automatic hot and cold cycle device for regulating the energy state of amorphous alloys, comprising an oil bath heating device, a liquid nitrogen cooling device, and a robotic arm device.

[0008] The robotic arm device includes a base, on which multiple links are connected by multiple joints. A sample clamp is mounted on the uppermost link. Each joint consists of a motor, a reducer, a transmission mechanism, and an encoder.

[0009] The oil bath heating device includes a first box, a first box cover is hinged to the upper part of the first box, a support is provided inside the first box, an oil bath is provided on the support, the oil bath is composed of an inner and outer layer and a middle insulation layer, a magnetic stirrer is provided at the bottom of the oil bath, and a sample tank is provided at the top of the oil bath.

[0010] The liquid nitrogen cooling device includes a second chamber, which contains a sample placement platform for placing the sample to be cooled and a nitrogen storage tank for storing liquid nitrogen. The nitrogen storage tank is connected to a liquid nitrogen tank outside the second chamber for supplying liquid nitrogen via an input pipe.

[0011] The base is the supporting and fixing part of the robotic arm device. The base and the connecting rod are made of aluminum alloy. The sample gripper of the robotic arm device realizes the gripping and movement of the sample through the controller. The joint drives the connecting rod to realize the movement and transmit the force. The sample gripper is equipped with a gripper for gripping the sample.

[0012] The oil bath is circular, with a heater installed at the bottom for heating it. The heater is mounted on a support, which is used to fix and support the heater. The support is fixedly connected to the first chamber. A temperature sensor is installed in the middle of the oil bath. An insulation layer is used to keep the heat in place, ensuring increased instrument efficiency. The magnetic stirrer is set to a safe temperature and ensures uniform heating. The temperature sensor monitors the temperature in real time to ensure accurate attainment of the set temperature. The sample holder is placed directly on the oil bath for placing samples. A fixed switch is installed at the switch between the first chamber lid and the first chamber.

[0013] The sample placement platform and nitrogen storage tank are fixed inside the enclosure by an insulated bracket. The nitrogen storage tank is also equipped with an output pipe. Liquid nitrogen is transported from the liquid nitrogen tank into the nitrogen storage tank through the input pipe and exits the nitrogen storage tank through the output pipe. The input pipe, output pipe, and the second enclosure are all equipped with heat insulation material. The sample placement platform is equipped with a temperature sensor for measuring the surface temperature of the sample placement platform. The temperature measured 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 control the temperature. The second enclosure is equipped with a second enclosure lid. The second enclosure and the second enclosure lid are used for heat preservation of the entire system. The second enclosure lid is used for placing and removing test samples.

[0014] The sample placement platform is also equipped with a cooling and temperature control device and cables.

[0015] The nitrogen storage tank is equipped with a baffle, a heat transfer rod, a liquid level sensor, and a heat transfer damping device. The baffle is used to intercept liquid nitrogen and cause it to drip into the nitrogen storage tank, preventing it from directly contacting the gas outlet and the heat transfer rod. The heat transfer rod and the heat transfer damping device are used to contact the liquid nitrogen and nitrogen gas and cool them. The heat transfer damping device is used to buffer vibration. The liquid level sensor is used to measure the liquid level height.

[0016] The beneficial effects of this invention are as follows: The fully automated thermal cycling equipment for regulating the energy state of amorphous alloys, through the coordination of an oil bath heating device, a liquid nitrogen cooling device, and a robotic arm, can be used for fully automated thermal cycling treatment of amorphous alloys of various compositions. It is not limited by the size of the amorphous alloy sample, achieving wide temperature range control. By adjusting the oil bath temperature, cycling time, and total number of cycles, the degree of rejuvenation of the amorphous alloy can be controlled, thereby adjusting and regulating its energy state to improve its plasticity. This invention can perform thermal cycling experiments fully automatically, solving some of the shortcomings of current thermal cycling experiments, such as being time-consuming, labor-intensive, and prone to freezing damage. Without altering the amorphous characteristics of the amorphous alloy, this invention effectively adjusts the energy state of the amorphous alloy, that is, it adjusts the internal atomic configuration of the amorphous alloy structure, increasing the degree of disorder in the microscopic atomic structure. This allows for the combination of the high strength and excellent plastic deformation capacity of amorphous alloys, aiming for widespread application in engineering fields. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the thermal cycling device of the present invention;

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

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

[0020] Figure 4 For the present invention Figure 3 A top-view structural diagram;

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

[0022] Figure 6 For the present invention Figure 5 An enlarged structural diagram;

[0023] Figure 7 This is a schematic diagram of the hot and cold cycle control program during the implementation of the present invention.

[0024] In the diagram, 100 is the robotic arm device; 101 is the base; 102 is the joint; 103 is the connecting rod; 104 is the sample holder; 200 is the oil bath heating device; 201 is the support; 202 is the heater; 203 is the magnetic stirrer; 204 is the temperature sensor; 205 is the insulation layer; 206 is the inner and outer layers of the oil bath tank; 207 is the sample tank; 208 is the first box cover; 209 is the first box body; 210 is the fixed switch; 30 is the sample holder. 0. Liquid nitrogen cooling device; 301. Cable; 302. Output pipe; 303. Input pipe; 304. Liquid nitrogen tank; 305. Cooling and temperature control device; 306. Insulation fixing bracket; 307. Second chamber; 308. Second chamber 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 Implementation

[0025] The principles and features of the present invention are described below with reference to the accompanying drawings. The examples given are only for explaining the present invention and are not intended to limit the scope of the present invention.

[0026] To achieve the above objectives, the present invention provides the following specific embodiments:

[0027] Example 1: As Figure 1 , 2 As shown in Figures 3 and 4, a fully automatic hot and cold circulation device for regulating the energy state of amorphous alloys includes an oil bath heating device 200, a liquid nitrogen cooling device 300, and a robotic arm device 100.

[0028] The robotic arm device 100 includes a base 101, on which multiple links 103 are connected by multiple joints 102. A sample clamp 104 is provided on the uppermost link. The joints 102 are composed of a motor, a reducer, a transmission mechanism and an encoder.

[0029] The oil bath heating device 200 includes a first box 209, a first box cover 208 is hinged to the upper part of the first box 209, a support 201 is provided inside the first box 209, an oil bath is provided on the support 201, the oil bath is composed of an inner and outer layer 206 and a middle insulation layer 205, a magnetic stirrer 203 is provided at the bottom of the oil bath, and a sample tank 207 is provided at the top of the oil bath.

[0030] The liquid nitrogen cooling device 300 includes a second housing 307, which contains a sample placement platform 309 for placing samples to be cooled and a nitrogen storage tank 312 for storing liquid nitrogen. The nitrogen storage tank 312 is connected to a liquid nitrogen tank 304 outside the second housing 307 for supplying liquid nitrogen via an input pipe 303.

[0031] The base 101 is the support 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 the movement and transmit the force. The sample clamp 104 is equipped with a gripper for clamping the sample.

[0032] The oil bath has a circular structure, and a heater 202 is installed at the bottom of the oil bath for heating it. The heater 202 is mounted on a support 201, which is used to fix and support the heater 202. The support 201 is fixedly connected to the first housing 209. A temperature sensor 204 is also installed in the middle of the oil bath. An insulation layer 205 is used to keep the heat warm and ensure that the instrument's working efficiency is increased. The magnetic stirrer 203 is set to 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 tank 207 is placed directly on the oil bath for placing the sample. A fixed switch 210 is installed at the switch between the first housing cover 208 and the first housing 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 by the heat-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 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 307 are all provided with heat insulation materials. The sample placement platform 309 is provided with a temperature sensor 310 for measuring the surface temperature of the sample placement platform. The temperature measured by the temperature sensor 310 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 control the temperature. The second box 307 is provided with a second box cover 308. The second box 307 and the second box cover 308 are used for heat insulation of the entire system. The second box cover 308 is used for putting in and taking out the test sample.

[0034] The upper part of the sample placement platform 309 is also equipped with a cooling and temperature control device 305 and a cable 301.

[0035] The nitrogen storage tank 312 is equipped with a baffle 311, a heat transfer rod 313, a liquid level sensor 314, and a heat transfer damping device 315. The baffle 311 is used to intercept liquid nitrogen and cause it to drip into the nitrogen storage tank 312, preventing it from directly contacting the gas outlet and the heat transfer rod 313. The heat transfer rod 313 and the heat transfer damping device 315 are used to contact the liquid nitrogen and nitrogen gas and cool it. The heat transfer damping device 315 is used to buffer vibration. The liquid level sensor 314 is used to measure the liquid level height.

[0036] The working principle of the fully automatic thermal cycling equipment for regulating the energy state of amorphous alloys is as follows: After the thermal cycling scheme is determined, the experimental program is input into the control system, the test sample is placed on the sample holder 104 of the robotic arm 100, the operating system starts the experiment, and the sample is circulated between the sample tank 207 of the oil bath heating device 200 and the sample placement platform 309 of the liquid nitrogen cooling device 300 by the robotic arm 100. The robotic arm 100 works in coordination with the first box cover 208 and the second box cover 308 through the control system. After each stage of the experiment, automatic sample loading and unloading is realized until the end of the experiment.

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

[0038] The fully automated hot and cold cycling equipment for regulating the energy state of amorphous alloys provided by this invention, in the method for preparing bulk amorphous alloys, uses a Zr-based high-strength amorphous alloy system, and specifically includes the following steps:

[0039] Step 1: Determine the thermal cycling scheme and subject the bulk amorphous alloy sample to thermal cycling 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. For Zr-based amorphous alloys, the T1 temperature range is 270K-475K, and the T2 temperature is 77K. The total number of thermal cycles n needs to be tested according to the Zr-based amorphous alloy system used. For Zr-based amorphous alloy systems, 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] For bulk amorphous alloy samples, cylindrical or cubic specimens should be selected.

[0042] The second step is to conduct a hot and cold cycle process. By setting different total number of hot and cold cycles n, heat treatment time t1, cryogenic treatment time t2, oil bath temperature T1, and cryogenic treatment temperature T2, multiple experiments are conducted to determine 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, room temperature compression is performed to verify the rejuvenation effect. The central control system automatically adjusts the flow rate and temperature of the cooling medium according to the real-time monitored parameters such as temperature and pressure to ensure that the sample reaches the optimal cooling rate and temperature gradient during the cycle.

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

[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 principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A fully automated cooling and heating cycle device for regulating the energy state of amorphous alloys, characterized by, 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), a plurality of connecting rods (103) connected by a plurality of joints (102) on the base (101), and a sample clamp (104) arranged on the uppermost connecting rod. The oil bath heating device (200) comprises a first box body (209), a first box cover (208) arranged on the upper part of the first box body (209) through hinging, a support (201) arranged in the first box body (209), an oil bath barrel arranged on the support (201), the oil bath barrel being composed of an inner and outer layer (206) and an intermediate heat preservation layer (205), a magnetic stirrer (203) arranged at the bottom of the oil bath barrel, and a sample groove (207) arranged at the upper part of the oil bath barrel. The liquid nitrogen cooling device (300) comprises a second box body (307), a sample placing platform (309) for placing samples to be cooled and a nitrogen storage tank (312) for storing liquid nitrogen arranged in the second box body (307), and the nitrogen storage tank (312) is connected with a liquid nitrogen tank (304) arranged outside the second box body (307) for providing liquid nitrogen through an input pipeline (303).

2. The full-automatic cooling and heating cycle device for regulating energy state of amorphous alloy according to claim 1, characterized in that, The base (101) is a support and fixing part of the mechanical arm device, the base (101) and the connecting rods (103) are made of aluminum alloy material, the sample clamp (104) of the mechanical arm device realizes clamping and moving of samples through a controller, the joint (102) drives the connecting rod (103) to realize movement and transmit force, and the sample clamp (104) is provided with a clamping jaw for clamping samples.

3. The full-automatic cooling and heating cycle device for regulating energy state of amorphous alloy according to claim 1, characterized in that, The joint (102) is composed of a motor, a speed reducer, a transmission mechanism and an encoder.

4. The full-automatic cooling and heating cycle device for regulating energy state of amorphous alloy according to claim 1, characterized in that, The oil bath barrel has a circular structure, and a heater (202) for heating the oil bath barrel is further arranged below the oil bath barrel, the heater (202) is installed on the support (201), the support (201) is used for fixing and supporting the heater (202), the support (201) is fixedly connected with the first box body (209), a temperature sensor (204) is further installed at the middle part of the oil bath barrel, the heat preservation layer (205) is used for heat preservation to ensure high working efficiency of the instrument, the magnetic stirrer (203) sets a safe temperature and ensures uniform heating, the temperature sensor (204) detects temperature in real time to ensure that the set temperature is accurately reached, the sample groove (207) is directly placed on the oil bath barrel for placing samples, and a fixed switch (210) is arranged at the switch between the first box cover (208) and the first box body (209).

5. The full-automatic cooling and heating cycle device for regulating energy state of amorphous alloy according to claim 1, characterized in that, The sample placement platform (309) and the nitrogen storage tank (312) are fixed in the box through the heat insulation fixed support (306), the nitrogen storage tank (312) is further provided with an output pipeline (302), liquid nitrogen in the liquid nitrogen tank (304) is transported into the nitrogen storage tank (312) through the input pipeline (303), and the liquid nitrogen leaves the nitrogen storage tank (312) through the output pipeline (302); the input pipeline (303), the output pipeline (302) and the second box (307) are all provided with heat insulation materials, 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 environment temperature of the sample, and the test result is fed back to a control system, so that the liquid nitrogen transmission speed is changed to control the temperature, the second box (307) is provided with a second box cover (308) at the upper portion, the second box (307) and the second box cover (308) are used for heat preservation of the whole system, and the second box cover (308) is used for placing and taking out the test sample.

6. The fully automated thermal cycler for regulating energy states of amorphous alloys of claim 5, wherein, The upper portion of the sample placement platform (309) is further provided with a cooling temperature control device (305) and a cable (301).

7. A full-automatic cooling and heating cycle device for regulating energy state of amorphous alloy according to any one of claims 1-6, characterized in that, The nitrogen storage tank (312) is internally provided with a baffle (311), a heat transfer rod (313), a liquid level sensor (314) and a heat transfer damping device (315), the baffle (311) is used for intercepting liquid nitrogen and making the liquid nitrogen drop into the nitrogen storage tank (312), so that the liquid nitrogen is prevented from directly contacting the gas outlet and the heat transfer rod (313), the heat transfer rod (313) and the heat transfer damping device (315) are used for contacting liquid nitrogen and nitrogen gas and refrigerating, and the heat transfer damping device (315) is used for buffering vibration; and the liquid level sensor (314) is used for measuring the liquid level.

Citation Information

Patent Citations

  • Device and process for improving cryogenic cycle induced rejuvenation capability of Zr-based amorphous alloy

    CN114480994A

  • Method for driving amorphous alloy to rapidly rejuvenate or relax in low-temperature circulation mode

    CN115449727A