A device and method for preparing bulk amorphous alloys

Abstract

The application discloses a bulk amorphous alloy preparation device, which comprises a reaction container, a vacuum pumping assembly, a heating assembly, a cooling assembly and a driving assembly. The reaction container is used for containing a sample for preparing a bulk amorphous alloy. The vacuum pumping assembly is communicated with the reaction container. The cooling assembly comprises a cooling liquid, which is cement mortar or a mixed liquid of water and cement. The heating assembly is arranged at the periphery of the reaction container to heat the reaction container. The driving assembly is drivingly connected with the reaction container to switch the reaction container between the heating assembly and the cooling assembly. The bulk amorphous alloy preparation device provided by the application has the advantages of simple structure and convenient operation. The cooling liquid is cement mortar or a mixed liquid of water and cement, so that the cooling rate can be improved, and the quality of the bulk amorphous alloy is ensured. The driving assembly can improve the safety of operation. The application further discloses a bulk amorphous alloy preparation method.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of amorphous alloy heat treatment, and particularly relates to a bulk amorphous alloy preparation device and a preparation method. BACKGROUND

[0002] Solid materials can be roughly divided into ordered structures and disordered structures according to the arrangement of atoms. Bulk amorphous alloy refers to a structure with long-range disorder and short-range order in the arrangement of atoms. Due to the unique arrangement of atoms in bulk amorphous alloy, bulk amorphous alloy does not have defects such as grain boundaries, dislocations and slip. Therefore, compared with traditional crystalline materials, bulk amorphous alloy has excellent mechanical properties and corrosion resistance, and the preparation of bulk amorphous alloy is particularly important.

[0003] The existing bulk amorphous alloy preparation device has the problem of slow cooling rate, which affects the quality of the bulk amorphous alloy

[0004] Therefore, how to improve the cooling rate of bulk amorphous alloy and ensure the quality of bulk amorphous alloy is a technical problem to be solved by those skilled in the art at present. SUMMARY

[0005] Therefore, the purpose of the present application is to provide a bulk amorphous alloy preparation device to improve the cooling rate of bulk amorphous alloy and ensure the quality of bulk amorphous alloy.

[0006] Another purpose of the present application is to provide a preparation method for preparing bulk amorphous alloy by using the above bulk amorphous alloy preparation device.

[0007] In order to achieve the above purpose, the present application provides the following technical scheme:

[0008] A bulk amorphous alloy preparation device comprises:

[0009] A reaction container for containing a sample for preparing bulk amorphous alloy;

[0010] A vacuum pumping assembly in communication with the reaction container;

[0011] A heating assembly arranged on the outer periphery of the reaction container to heat the reaction container;

[0012] A cooling assembly comprising a cooling liquid, the cooling liquid being a mixture of cement mortar or water and cement;

[0013] A driving assembly in driving connection with the reaction container to switch the reaction container between the heating assembly and the cooling assembly.

[0014] Optionally, in the above bulk amorphous alloy preparation device, the cooling assembly comprises a cooling liquid tank and a circulating pump in communication with the cooling liquid tank, and the cooling liquid tank is used for containing the cooling liquid.

[0015] Optionally, in the above bulk amorphous alloy preparation device, the heating assembly comprises an electromagnetic induction coil wound around the outer periphery of the reaction container.

[0016] Optionally, in the above bulk amorphous alloy preparation device, further comprising a first temperature measuring assembly electrically connected to the heating assembly.

[0017] The first temperature measuring assembly comprises a thermocouple arranged inside or outside the reaction container.

[0018] Optionally, in the above bulk amorphous alloy preparation device, further comprising a support assembly, and the reaction container, the heating assembly and the driving assembly are arranged on the support assembly.

[0019] Optionally, in the above bulk amorphous alloy preparation device, the driving assembly comprises a motor and a screw nut transmission mechanism, the fixed end of the motor is arranged on the support assembly, the transmission end of the motor is in transmission connection with the screw nut transmission mechanism, and the screw nut transmission mechanism is in transmission connection with the reaction container.

[0020] A bulk amorphous alloy preparation method is prepared by using the above bulk amorphous alloy preparation device, comprising the following steps:

[0021] Placing a sample for preparing a bulk amorphous alloy, and placing the sample for preparing the bulk amorphous alloy in the reaction container.

[0022] Repeating the gas washing and vacuumizing of the reaction container by the vacuumizing assembly.

[0023] Heating the reaction container, starting the heating assembly, and heating the reaction container after completing the gas washing.

[0024] Cooling the reaction container, driving the reaction container to separate from the heating assembly by the driving assembly, and entering the cooling assembly for cooling.

[0025] Filling the inert gas into the reaction container, introducing the inert gas into the reaction container after completing the cooling by the vacuumizing assembly until the pressure in the reaction container returns to the atmospheric pressure.

[0026] Optionally, in the above bulk amorphous alloy preparation method, in the step of repeating the gas washing and vacuumizing of the reaction container by the vacuumizing assembly, the inert gas of 0.9 MPa is filled into the reaction container for the last time of gas washing.

[0027] Optionally, in the bulk amorphous alloy preparation method, in the heating reaction container step, the heating assembly can adjust the heating power according to the temperature measured by the first temperature measuring assembly.

[0028] Optionally, in the bulk amorphous alloy preparation method, in the heating reaction container step, the driving assembly drives the reaction container to be placed in the center of the heating assembly.

[0029] The bulk amorphous alloy preparation device provided by the application is used to place a sample for preparing a bulk amorphous alloy in a reaction container, repeatedly washes and evacuates the reaction container through the vacuum pumping assembly. After the sample is washed, the reaction container is heated, and after the heating is completed, the driving assembly drives the reaction container to separate from the heating assembly, and the reaction container is cooled. After cooling, the reaction container is again filled with inert gas through the vacuum pumping assembly, so that the pressure in the reaction container is restored to atmospheric pressure, and a bulk amorphous alloy is obtained.

[0030] As can be seen from the above technical solution, the bulk amorphous alloy preparation device provided by the application has the advantages of simple structure, convenient operation, and the use of cement mortar or a mixture of water and cement as a cooling liquid to improve the cooling rate and ensure the quality of the bulk amorphous alloy. The heating assembly is arranged on the outer periphery of the reaction container, which can make the heating more uniform, and the driving assembly drives the reaction container to switch between the heating assembly and the cooling assembly, which can ensure the switching rate between the heating state and the cooling state of the prepared sample and ensure the quality of the prepared bulk amorphous alloy. At the same time, the arrangement of the driving assembly can avoid the safety problems caused by manual operation and ensure the personal safety of the operator.

[0031] The bulk amorphous alloy preparation method provided by the application simplifies the preparation process of the bulk amorphous alloy and improves the safety of the operation. BRIEF DESCRIPTION OF DRAWINGS

[0032] In order to more clearly illustrate the technical solutions in the embodiments of the application or the prior art, the following will briefly introduce the drawings needed to be used in the embodiments or the prior art description. Obviously, the drawings in the following description are only some embodiments of the application, and those skilled in the art can also obtain other drawings according to these drawings without creative labor.

[0033] Figure 1 The structure diagram of the reaction container disclosed in the embodiments of the application is shown in the following figure:

[0034] Figure 2 The structure diagram of the driving assembly connected to the reaction container disclosed in the embodiments of the application is shown in the following figure: Figure 1 ;

[0035] Figure 3This is a schematic diagram of the structure of the drive component connected to the reaction vessel according to an embodiment of the present invention. Figure 2 ;

[0036] Figure 4 This is a schematic diagram of the heating process of the bulk amorphous alloy preparation apparatus disclosed in an embodiment of the present invention;

[0037] Figure 5 This is a schematic diagram of the cooling process of the bulk amorphous alloy preparation apparatus disclosed in an embodiment of the present invention;

[0038] Figure 6 This is a flowchart of the bulk amorphous alloy preparation method disclosed in the embodiments of the present invention;

[0039] Figure 7 The thermal conductivity data of cement mortar as disclosed in the finite element simulation of this invention embodiment;

[0040] Figure 8 The thermal conductivity data of water disclosed in the finite element simulation of this invention are shown in the embodiments of the present invention.

[0041] Among them, 101 is the reaction vessel, 102 is the heating component, 103 is the first temperature measuring component, 104 is the cooling component, and 105 is the driving component. Detailed Implementation

[0042] The core of this invention is to disclose a bulk amorphous alloy preparation apparatus to improve the cooling rate of bulk amorphous alloys and ensure the quality of bulk amorphous alloys.

[0043] Another core aspect of this invention is the disclosure of a method for preparing bulk amorphous alloys using the aforementioned bulk amorphous alloy preparation apparatus.

[0044] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0045] like Figures 4-5 As shown in the figure, an embodiment of the present invention discloses a bulk amorphous alloy preparation device, including a reaction vessel 101, a vacuum pumping assembly, a heating assembly 102, a cooling assembly 104, and a driving assembly 105.

[0046] The reaction vessel 101 is used to hold the sample for preparing the bulk amorphous alloy (hereinafter referred to as the preparation sample), and can be a quartz glass tube, such as... Figure 1As shown, in an embodiment, the quartz glass tube is in a cylindrical shape, with an inner diameter of 13 mm and a length of 200 mm. It should be noted that the size of the reaction container 101 is only an example, and the specific size can be selected according to actual needs.

[0047] The vacuum assembly is used to vacuumize and gas wash (inert gas) the reaction container 101. Specifically, the vacuum assembly includes a vacuum pump and an inert gas pressurizing device. The reaction container 101 is provided with a three-way pipe, and the vacuum pump and the inert gas pressurizing device are connected to the three-way pipe. The vacuum pump is used to vacuumize the reaction container 101, and the inert gas pressurizing device is used to gas wash the reaction container 101. The gas washing gas can be argon or nitrogen. The purpose of gas washing is to reduce the oxygen content in the reaction container 101 as much as possible. The gas washing usually includes three times of gas washing. The inert gas filled in the reaction container 101 protects the prepared sample from oxidation.

[0048] The heating assembly 102 is used to heat the reaction container 101. In order to ensure uniform heating, the heating assembly 102 is arranged on the outer periphery of the reaction container 101. The heating assembly 102 can be an electromagnetic induction coil or a laser heating device. The electromagnetic induction coil is preferred. The cooling assembly 104 is used to cool the reaction container 101. In order to improve the cooling rate, the cooling liquid of the cooling assembly 104 is a mixture of water and cement or water.

[0049] Specifically, when the cooling liquid is a mixture of water and cement, the ratio of water to cement is 1:1 (50% water and 50% cement). The thermal conductivity of water at room temperature is 0.59 W / (m·K), and the thermal conductivity of the mixture of water and cement is >1 W / (m·K). The thermal conductivity of the cement mortar (70% water, 20% cement, and 10% sand) is 0.7 W / (m·K)-1.5 W / (m·K), which is higher than that of traditional water cooling. Figures 7-8 As shown, Figure 7 The thermal conductivity data of the cement mortar (70% water, 20% cement, and 10% sand) is shown. Figure 8 The thermal conductivity data of water is shown. Assuming that the initial temperature is the same, within the same time, it can be seen from the figure that the thermal conductivity of the cement mortar is 2-2.5 times that of water. It can be seen that the cement mortar is more conducive to heat conduction than water, and can achieve rapid cooling.

[0050] When the metal liquid solidifies, the atomic arrangement changes from order to disorder. When the solidification rate is slow, the atomic arrangement has enough time to form a regular crystal structure. If the solidification rate is fast, the atomic arrangement does not have enough time to rearrange into a regular crystal, thereby forming an amorphous structure. The amorphous alloy refers to the atomic arrangement having a long-range disorder and a short-range order structure. Therefore, the cooling efficiency can ensure the quality of the bulk amorphous alloy.

[0051] The driving assembly 105 is in transmission connection with the reaction container 101, so that the reaction container 101 is switched between the heating assembly 102 and the cooling assembly 104, and further switched between the heating state and the cooling state. The specific type of the driving assembly 105 can adopt an up-down moving device, directly place the cooling assembly 104 below the reaction container 101, or adopt other types.

[0052] In use, the preparation sample is placed in the reaction container 101, and the reaction container 101 is repeatedly washed and vacuumized by the vacuumizing assembly. After the preparation sample is washed, the reaction container 101 is heated, and after the heating is completed, the driving assembly 105 drives the reaction container 101 to separate from the heating assembly 102, places the reaction container in the cooling assembly 104, cools the reaction container 101, and then passes the inert gas into the reaction container 101 through the vacuumizing assembly, so that the pressure in the reaction container 101 returns to the atmospheric pressure, and the bulk amorphous alloy is obtained.

[0053] The bulk amorphous alloy preparation device disclosed by the embodiment of the present application has simple structure and convenient operation, uses the cement mortar or the mixed liquid of water and cement as the cooling liquid for cooling, can improve the cooling rate, and ensures the quality of the bulk amorphous alloy. The heating assembly 102 is arranged at the outer periphery of the reaction container 101, so that the heating is more uniform, the driving assembly 105 drives the reaction container 101 to switch between the heating assembly and the cooling assembly, can improve the switching rate of the preparation sample between the heating state and the cooling state, and ensures the quality of the prepared bulk amorphous alloy. Meanwhile, the arrangement of the driving assembly 105 can avoid the safety problems caused by manual operation of the operator, ensures the personal safety of the operator, and improves the safety of the operation. Meanwhile, the preparation of the amorphous alloy can solve the problem of poor plasticity of the amorphous alloy at room temperature.

[0054] In one specific embodiment of the present invention, the cooling assembly 104 includes a coolant tank and a circulation pump connected to the coolant tank. The coolant tank has an inlet and an outlet; coolant enters the coolant tank through the inlet and flows out through the outlet to cool the reaction vessel 101. In another specific embodiment, a stirring device may also be provided in the coolant tank to ensure uniform temperature of the coolant. A second temperature measuring component is provided in the coolant tank to measure the temperature of the coolant. After a preset cooling time is reached, the drive assembly 105 can detach the reaction vessel 101 from the cooling assembly 104.

[0055] like Figures 4-5 As shown, in a specific embodiment of the present invention, the heating assembly 102 includes an electromagnetic induction coil wound around the outer periphery of the reaction vessel 101. The electromagnetic induction coil is made of copper wire, and the number of coils can be determined according to the actual situation. The winding method uses multiple strands connected in parallel, which can increase the heating area. The heating temperature of the electromagnetic induction coil can be precisely controlled by controlling parameters such as current, voltage, and electromagnetic induction intensity. The electromagnetic induction coil heats up quickly, allowing for rapid heating of the reaction vessel 101. The diameter of the electromagnetic induction coil is greater than 1 mm, but does not exceed the inner diameter of the reaction vessel 101.

[0056] In order to measure the heating temperature of the heating component 102 and simultaneously achieve automatic control of the heating component 102, in a specific embodiment of the present invention, a first temperature measuring component 103 is further included. The first temperature measuring component 103 is electrically connected to the heating component 102 and includes a thermocouple, which is disposed inside or outside the reaction vessel 101. Figure 5 The thermocouple shown is placed outside the reaction vessel 101. The thermocouple is electrically connected to an electromagnetic induction coil, and specifically, the thermocouple can measure the temperature of the reaction vessel 101 in real time.

[0057] In a specific embodiment of the present invention, a support component is also included. The support component can be an iron frame or other devices. The reaction vessel 101, the heating component 102 and the driving component 105 are all disposed on the support component, which provides support.

[0058] In a specific embodiment of the present application, the driving assembly 105 comprises a motor and a screw nut transmission mechanism, the fixed end of the motor is arranged on the supporting assembly, the transmission end of the motor is in transmission connection with the screw nut transmission mechanism, and the screw nut transmission mechanism is in transmission connection with the reaction container 101. Specifically, the screw nut transmission mechanism comprises a screw rod and a transmission nut, the screw rod is in rotational connection with the supporting assembly, the reaction container 101 is fixedly connected with the transmission nut, the transmission nut is in threaded connection with the screw rod, the motor rotates in a first direction to drive the reaction container 101 to ascend, the motor rotates in a second direction to drive the reaction container 101 to descend, and the first direction is opposite to the second direction. The cooling liquid tank is arranged below the reaction container 101, after the reaction container 101 is heated, the heating assembly 102 can be closed, the reaction container 101 is driven to move downward by starting the motor and the screw nut transmission mechanism, so that the reaction container 101 is arranged below the electromagnetic induction coil and in the cooling liquid tank for cooling.

[0059] As shown in FIG. 1, Figures 2-3 In another specific embodiment of the present application, the driving assembly 105 comprises a driving cylinder connected with the supporting assembly, and the piston rod of the driving cylinder is connected with the reaction container 101 to realize the lifting movement of the reaction container 101. Specifically, the piston rod can be connected with the reaction container 101 through a clamping piece. Figure 2 As shown in FIG. 2, Figure 3 As shown in FIG. 3, the piston rod is in the extended state.

[0060] As shown in FIG. 4, Figure 6 The present application further discloses a bulk amorphous alloy preparation method, which is prepared by using the bulk amorphous alloy preparation device, and comprises the following steps:

[0061] S1: placing a sample for preparing a bulk amorphous alloy;

[0062] The sample for preparing the bulk amorphous alloy is placed in the reaction container 101, and the reaction container 101 is packaged;

[0063] S2: repeatedly washing and continuously vacuumizing the reaction container 101 by the vacuumizing assembly;

[0064] Specifically, 0.9 MPa of inert gas is filled in the last washing to prevent the sample from being oxidized.

[0065] S3: heating the reaction container 101;

[0066] The driving assembly 105 drives the reaction container 101 to be placed in the center of the electromagnetic induction coil, starts the heating assembly 102, turns on the electromagnetic induction coil, adjusts the heating power, and heats the reaction container 101 after the gas washing is completed, so as to heat the prepared sample in the reaction container 101; during the heating process, the electromagnetic induction coil can adjust the heating power according to the temperature measured by the first temperature measuring assembly 103, and control the heating rate;

[0067] S4: cooling the reaction container 101;

[0068] The heating assembly 102 is turned off, the reaction container 101 is driven by the driving assembly 105 to be separated from the heating assembly 102, and enters the cooling assembly 104 for cooling;

[0069] S5: filling the reaction container 101 with inert gas;

[0070] The inert gas is introduced into the reaction container 101 after the cooling is completed through the vacuum pumping assembly, until the pressure in the reaction container 101 returns to the atmospheric pressure, and the bulk amorphous alloy is generated.

[0071] The bulk amorphous alloy preparation method provided by the application simplifies the preparation process of the bulk amorphous alloy, can obtain the bulk amorphous alloy through a simple method, can reduce the preparation cost compared with the prior art, and can improve the safety of operation.

[0072] It should be noted that each embodiment in the specification adopts a progressive manner for description, and each embodiment focuses on the difference from other embodiments, and the same or similar parts between each embodiment can be referred to each other.

[0073] As shown in the present application and claims, unless the context clearly indicates otherwise, "one", "a", "an", and / or "the" do not refer to the singular, but can also include the plural. Generally, the terms "comprise" and "include" only indicate the inclusion of the steps and elements explicitly identified, and these steps and elements do not constitute an exclusive list, and the method or device can also include other steps or elements. The element defined by the statement "comprises one" does not exclude the presence of another same element in the process, method, product or device comprising the element.

[0074] Hereinafter, the terms "first" and "second" are only used for description purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of indicated technical features. Therefore, the features defined with "first" and "second" can explicitly or implicitly include one or more of the features.

[0075] The principles and implementations of the present application are described in the specific examples in this article, and the above examples are only used to help understand the core idea of the present application. It should be pointed out that for ordinary skilled persons in the art, without departing from the principles of the present application, the present application can be improved and modified, and these improvements and modifications also fall within the protection scope of the claims of the present application.

Claims

1. An apparatus for producing bulk amorphous alloys, comprising: The application relates to a preparation device for preparing bulk amorphous alloys, which comprises the following components: a reaction container (101) for containing a sample of the bulk amorphous alloy; a vacuumizing assembly in communication with the reaction container (101); a heating assembly (102) arranged at the periphery of the reaction container (101) to heat the reaction container (101); a cooling assembly (104) comprising cooling liquid, which is cement mortar or a mixture of water and cement; the mixture of water and cement has a water-cement ratio of 1:1 and a thermal conductivity greater than 1 W / (m.K); the cement mortar has a water-cement-sand ratio of 7:2:1 and a thermal conductivity of 0.7-1.5 W / (m.K); a driving assembly (105) in driving connection with the reaction container (101) to switch the reaction container (101) between the heating assembly (102) and the cooling assembly (104); the driving assembly (105) is connected to the top of the reaction container (101). The cooling assembly (104) comprises a cooling liquid tank for containing the cooling liquid and a circulating pump in communication with the cooling liquid tank. The heating assembly (102) comprises an electromagnetic induction coil wound around the periphery of the reaction container (101). The application further comprises a first temperature measuring assembly (103) in electric connection with the heating assembly (102). The first temperature measuring assembly (103) comprises a thermocouple arranged inside or outside the reaction container (101). The application further comprises a supporting assembly, and the reaction container (101), the heating assembly (102) and the driving assembly (105) are arranged on the supporting assembly.

2. The bulk amorphous alloy production device of claim 1 wherein, The driving assembly (105) comprises a motor and a screw nut transmission mechanism, the fixed end of the motor is arranged on the supporting assembly, the transmission end of the motor is in driving connection with the screw nut transmission mechanism, and the screw nut transmission mechanism is in driving connection with the reaction container (101).

3. The bulk amorphous alloy production device of claim 2 wherein, The application further comprises the following steps: placing a sample of the bulk amorphous alloy in the reaction container (101); repeatedly washing and vacuumizing the reaction container (101) through the vacuumizing assembly; heating the reaction container (101) by starting the heating assembly (102); cooling the reaction container (101) by driving the reaction container (101) to separate from the heating assembly (102) and enter the cooling assembly (104) to be cooled; filling the reaction container (101) with inert gas by introducing inert gas into the reaction container (101) after cooling through the vacuumizing assembly until the pressure in the reaction container (101) returns to atmospheric pressure.

4. The bulk amorphous alloy production device of claim 3 wherein, ​ ​ 5. The bulk amorphous alloy production device of claim 4 wherein, ​ 6. The bulk amorphous alloy production device of claim 5 wherein, ​ 7. A method for producing a bulk amorphous alloy using the apparatus for producing a bulk amorphous alloy according to claim 6, characterized by: ​ ​ ​ ​ ​ ​ 8. The bulk metallic glass alloy production method of claim 7, wherein, The reaction container (101) is filled with inert gas at 0.9 MPa during the last purging of the reaction container (101) in the repeated purging and vacuumizing steps by the vacuumizing assembly.

9. The bulk metallic glass alloy production method of claim 7, wherein the alloy is produced by a method comprising: The heating assembly (102) can adjust the heating power according to the temperature measured by the first temperature measuring assembly (103) during the heating of the reaction container (101).

10. The method for preparing bulk amorphous alloy as described in claim 8, characterized in that, The driving assembly (105) drives the reaction container (101) to be placed in the center of the heating assembly (102) during the heating of the reaction container (101).

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