Heating Device and Material Heat Treatment Method

Abstract

The present application provides a heating device and a material heat treatment method, belonging to the field of heat treatment equipment. The heating device includes a heating table main body and a cover plate assembly. The heating table main body includes a mounting seat and a heat conducting block. There is a heating table cavity in the mounting seat, a ventilation channel communicating with the heating table cavity at the top, and first and second heating table connectors outside. The heat conducting block is installed on the mounting seat, and its top is located at the top of the mounting seat. A first channel penetrating through the top of the heat conducting block is provided inside the heat conducting block, and a connecting pipe is provided between the other end of the first channel and the first heating table connector. When the cover plate assembly covers the top of the mounting seat, there is a first cover plate cavity between the cover plate assembly and the top of the mounting seat; the ventilation channel and the first channel are both communicated with the first cover plate cavity; there is a first cover plate connector outside the cover plate assembly that communicates with the first cover plate cavity. The material heat treatment method uses the heating device for heating and annealing treatment, which can reduce the risk of the sample being damaged by contacting air after transfer and before annealing treatment.

Description

Technical Field

[0001] This application relates to the field of heat treatment equipment, and more particularly, to a heating device and a material heat treatment method. Background Art

[0002] In current material transfer equipment, such as in the transfer equipment for two-dimensional materials, heating devices such as sample heating tables are indispensable components, and their function is to heat samples such as two-dimensional materials to achieve the effect of melting the glue.

[0003] In the current process, after the heating and transfer process of the sample is completed, the sample often needs to be annealed to remove defects such as bubbles and wrinkles generated during the transfer process.

[0004] Regarding annealing treatment, the current conventional practice is to place the transferred sample in a vacuum annealing furnace for annealing under a certain atmosphere. When preparing some materials such as heterojunctions composed of water and oxygen sensitive materials, the entire transfer process needs to be carried out in a glove box; however, when taking the transferred sample out of the glove box and putting it into the vacuum annealing furnace, the sample may come into contact with air and thus be damaged. Summary of the Invention

[0005] The purpose of this application is to provide a heating device and a material heat treatment method, which can effectively reduce the risk of the sample being damaged when it comes into contact with air after the transfer is completed and before the annealing treatment.

[0006] The embodiments of this application are implemented as follows:

[0007] In a first aspect, an embodiment of this application provides a heating device, including a heating table main body and a cover plate assembly.

[0008] The heating table main body includes a mounting seat and a heat conducting block; the mounting seat has a heating table cavity inside, and the top of the mounting seat has a ventilation channel communicating with the heating table cavity; the outside of the mounting seat is provided with a first heating table joint and a second heating table joint communicating with the heating table cavity; the heat conducting block is installed on the mounting seat, and the top of the heat conducting block is located at the top of the mounting seat; a first channel is opened in the heat conducting block, one end of the first channel penetrates the top end face of the heat conducting block, and a connecting pipe is connected between the other end of the first channel and the first heating table joint;

[0009] When the cover plate assembly covers the top of the mounting seat, there is a first cover plate cavity between the cover plate assembly and the top of the mounting seat; the ventilation channel and the first channel are both communicated with the first cover plate cavity; the outside of the cover plate assembly is provided with a first cover plate joint communicating with the first cover plate cavity.

[0010] In the above technical solution, the heat conduction block of the heating table main body can adsorb the material to be processed on the top of the heat conduction block by connecting to negative pressure through the first heating table joint, which facilitates heating the material to be processed after the heat conduction block is heated up. The heating table main body and the cover plate assembly cooperate, and negative pressure and / or gas source can be connected through the second heating table joint, and the annealing atmosphere can be connected through the first cover plate cavity, which facilitates annealing treatment in a specific atmosphere and / or vacuum environment.

[0011] The heating device has both the functions of heating treatment and annealing treatment. After the heating and transfer of the material are completed, there is no need to take out the sample from the processing environment and place it in a vacuum annealing furnace for separate annealing. The material to be processed can remain under the preset environmental atmosphere conditions, which can effectively reduce the risk of the sample being damaged by contacting air after the transfer is completed and before the annealing treatment.

[0012] In some alternative embodiments, the first cover plate cavity is opened in the cover plate assembly and penetrates the bottom of the cover plate assembly. The first cover plate cavity penetrates the bottom of the cover plate assembly to form an observation hole, and an observation window corresponding to the observation hole is installed on the top of the cover plate assembly; when the cover plate assembly is covered on the top of the mounting base, the observation hole corresponds to the heat conduction block, and the ventilation channel and the first channel are both communicated with the first cover plate cavity through the observation hole.

[0013] In the above technical solution, the observation window corresponds to the observation hole, and the annealing process of the sample on the top of the heat conduction block corresponding to the observation hole can be observed. On the one hand, it is convenient to directly observe the progress of the sample annealing and save research time; on the other hand, the visual annealing process can also provide more experimental information for the research.

[0014] In some alternative embodiments, the top of the cover plate assembly has a mounting through hole communicated with the first cover plate cavity, and a mounting step is annularly provided on the circumference of the mounting through hole; the mounting step includes an annular step side wall and an annular step bottom wall, and the annular step bottom wall is connected to the inner side of the bottom of the annular step side wall; the observation window is arranged on the mounting step to close the mounting through hole, and an annular sealing ring is connected between at least one of the annular step side wall and the annular step bottom wall and the observation window.

[0015] In the above technical solution, the observation window is installed by setting the mounting step, so that the observation window can be better fitted in the cover plate assembly. The connection between the observation window and the mounting step is achieved through an annular sealing ring, which can better realize the connection and sealing between the two.

[0016] In some alternative embodiments, a ring-shaped protrusion is provided at the bottom of the cover plate assembly; the ring-shaped protrusion is located in the first cover plate cavity and surrounds the observation hole; the top of the ring-shaped protrusion is flush with the annular step bottom wall; the ring-shaped protrusion is provided with a connection channel for communicating the inner side and the outer side of the ring-shaped protrusion.

[0017] In the above technical solution, the annular protrusion flush with the bottom wall of the annular step of the installation step is used to cooperate with the bottom wall of the annular step to better support the observation window, which is beneficial to reducing the thickness of the observation window, thereby making the light transmittance of the observation window better and enabling better observation.

[0018] In some alternative embodiments, the cover assembly further has a second cover cavity inside, and a second cover joint communicating with the second cover cavity is provided on the outside; the second cover cavity is located outside the first cover cavity, and a second channel communicating with the second cover cavity is opened at the bottom of the cover assembly; when the cover assembly is covered on the top of the mounting base, the second channel corresponds to the top of the mounting base, and the top of the mounting base separates the first cover cavity and the second cover cavity.

[0019] In the above technical solution, the top of the mounting base separates the first cover cavity and the second cover cavity, so that the first cover cavity communicates with the inner cavity of the mounting base, and the second cover cavity communicates with the external environment of the mounting base. The second channel corresponds to the top of the mounting base, which facilitates the gas in the second cover cavity to be blown out through the second channel and purged onto the top of the mounting base, and can cool the top of the mounting base, which is beneficial to better annealing treatment.

[0020] In some alternative embodiments, in the cross-section of the cover assembly, the second channel extends along an arc path, and the central angle of the arc path is greater than 300°.

[0021] In the above technical solution, the second channel is a large-arc circular arc, which can better correspond to the top of the mounting base axially, so that the gas purged onto the top of the mounting base can exert a more sufficient and uniform cooling effect.

[0022] In some alternative embodiments, the ventilation channel is a ventilation gap between the top of the heat conducting block and the top of the mounting base; a plurality of communication holes communicating with the heating table cavity are penetrated through the top of the mounting base; when the cover assembly is covered on the top of the mounting base, the communication holes communicate with the first cover cavity.

[0023] In the above technical solution, the setting of the communication holes can reduce the cross-sectional area of the top of the mounting base, thereby reducing the transfer of the heat radiated by the heat conducting block, which is beneficial to reducing the heat loss of the heat conducting block.

[0024] In some alternative embodiments, an annular mounting groove is recessed in the top of the mounting base for detachably mounting an annular seal, so that when the cover assembly is covered on the top of the mounting base, the top of the annular seal is in sealing contact with the bottom of the cover assembly and separates the first cover cavity and the second cover cavity.

[0025] In the above technical solution, the annular mounting groove is provided for detachably mounting the annular seal, which can better achieve the sealing fit between the top of the mounting seat and the cover plate assembly. At the same time, the setting of the annular mounting groove can also reduce the cross-sectional area of the top of the mounting seat, thereby reducing the transfer of the heat radiated by the heat conducting block.

[0026] In some alternative embodiments, the heating table body further includes a heating sheet and a screw-type temperature probe. The heating sheet is attached to the bottom end face of the heat conducting block, and the screw-type temperature probe penetrates through the heating sheet and is connected to the bottom of the heat conducting block.

[0027] In the above technical solution, the form of the heating sheet has a large heat dissipation area, which is beneficial to reducing the temperature overshoot caused by the untimely heat dissipation of the heating components and their large self-energy storage. The screw-type temperature probe is convenient to be fixed on the heat conducting block for temperature detection and can also fix the heating sheet.

[0028] In some alternative embodiments, the heating device further includes a heat insulation table, which includes a heat insulation seat, a side reflective structure and a bottom reflective structure; the heat insulation seat is used to connect the mounting seat, and a heat insulation chamber for communicating with the cavity of the heating table is recessed at the top of the heat insulation seat; the side reflective structure surrounds the side wall of the heat insulation chamber, and the bottom reflective structure is arranged at the bottom of the heat insulation chamber.

[0029] In the above technical solution, the heat insulation table is used to separate the heating table body from the operation table surface; the side reflective structure and the bottom reflective structure inside the heat insulation seat can reflect the thermal radiation of the heating table body, which is beneficial to reducing the heat loss of the heating table body and the heat transferred to the outside.

[0030] In a second aspect, the embodiments of the present application provide a material heat treatment method, which is carried out by using the heating device provided in the embodiments of the first aspect, including, under preset ambient atmosphere conditions:

[0031] Place the material to be processed on the top of the heat conducting block and cover the opening of the first channel;

[0032] Connect the first heating table joint to negative pressure and heat the heat conducting block to a preset temperature to complete the heating treatment of the material to be processed;

[0033] Place the material to be processed after the heating treatment on the top of the heat conducting block;

[0034] And, connect the second heating table joint to negative pressure and connect the first cover plate joint to the annealing gas source, and then perform annealing treatment on the material to be processed.

[0035] In the above technical solution, a heating table main body is used to adsorb the material to be processed for heat treatment, and the heating table main body and the cover plate assembly are used in cooperation to provide a specific atmosphere and vacuum environment for the material to be processed for annealing treatment. After the material is heated and transferred, there is no need to take the sample out of the processing environment and place it in a vacuum annealing furnace for separate annealing. The material to be processed can remain in the preset environmental atmosphere conditions, which can effectively reduce the risk of the sample being damaged by contacting air after being transferred and before annealing treatment. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] To more clearly illustrate the technical solutions of the embodiments of the present application, the following will briefly introduce the drawings required to be used in the embodiments. It should be understood that the following drawings only show some embodiments of the present application, and therefore should not be regarded as limiting the scope. For those of ordinary skill in the art, without creative efforts, other relevant drawings can also be obtained based on these drawings.

[0037] Figure 1 An exploded view of the heating device provided by an embodiment of the present application;

[0038] Figure 2 A cross-sectional view of the heating device provided by an embodiment of the present application;

[0039] Figure 3 A cross-sectional view of the heating table main body provided by an embodiment of the present application;

[0040] Figure 4 A structural diagram of the heating table main body provided by an embodiment of the present application;

[0041] Figure 5 An exploded view of the cover plate assembly provided by an embodiment of the present application;

[0042] Figure 6 A cross-sectional view of the cover plate assembly provided by an embodiment of the present application;

[0043] Figure 7 An exploded view of the heat insulation table provided by an embodiment of the present application.

[0044] Reference numerals: 10 - heating device;

[0045] 100 - heating table main body; 101 - mounting base; 110 - heat insulation ring; 111 - heating table cavity; 112 - first heating table joint; 113 - second heating table joint; 114 - vacuum aviation plug; 120 - mounting plate; 121 - ventilation channel; 122 - communication hole; 123 - annular mounting groove; 130 - heat conducting block; 131 - first channel; 132 - connecting pipe; 133 - heating sheet; 134 - screw type temperature probe; 135 - spring washer;

[0046] 200 - Cover plate assembly; 201 - Cover plate seat; 210 - Ring - shaped side plate of the seat; 211 - First cover plate cavity; 212 - First cover plate joint; 213 - Second cover plate cavity; 214 - Second cover plate joint; 220 - Seat bottom plate; 221 - Observation hole; 222 - Ring - shaped protrusion; 223 - Connection channel; 224 - Second channel; 230 - Observation window; 231 - Installation step; 232 - Side wall of the ring - shaped step; 233 - First ring - shaped sealing ring; 234 - Bottom wall of the ring - shaped step; 235 - Second ring - shaped sealing ring; 240 - Sealing cover plate

[0047] 300 - Annular seal

[0048] 400 - Heat - insulating platform; 410 - Heat - insulating seat; 411 - Heat - insulating chamber; 420 - Side reflective structure; 430 - Bottom reflective structure Detailed implementation manners

[0049] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of this application. Apparently, the described embodiments are some but not all of the embodiments of this application. Generally, the components of the embodiments of this application described and illustrated in the accompanying drawings here can be arranged and designed in various different configurations.

[0050] Therefore, the following detailed description of the embodiments of this application provided in the accompanying drawings is not intended to limit the scope of the claimed application, but merely represents selected embodiments of this application. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of this application without creative efforts fall within the scope of protection of this application.

[0051] It should be noted that: Similar reference numerals and letters denote similar items in the following drawings. Therefore, once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings.

[0052] In the description of this application, it should be noted that the orientation or positional relationship indicated by the terms "center", "upper", "lower", "vertical", "horizontal", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings or the orientation or positional relationship in which the product of this application is usually placed during use. It is only for the convenience of describing this application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as a limitation of this application.

[0053] Terms such as "vertical" and "parallel" do not mean that components must be absolutely vertical or parallel, but can be slightly inclined.

[0054] In addition, the terms "first", "second", etc. are only used for distinguishing descriptions and cannot be understood as indicating or implying relative importance.

[0055] In the description of this application, it should also be noted that unless otherwise clearly specified and limited, the terms "set", "installed", "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected, or indirectly connected through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific situations.

[0056] Embodiment

[0057] Please refer to Figure 1 and Figure 2 , an embodiment of this application provides a heating device 10, including a heating table main body 100 and a cover plate assembly 200.

[0058] Please refer to Figure 3 and Figure 4 , the heating table main body 100 includes a mounting base 101 and a heat conducting block 130. The mounting base 101 has a heating table cavity 111 inside, and the top of the mounting base 101 has a ventilation channel 121 communicating with the heating table cavity 111. On the outside of the mounting base 101, a first heating table joint 112 and a second heating table joint 113 communicating with the heating table cavity 111 are provided. The heat conducting block 130 is installed on the mounting base 101; the top of the heat conducting block 130 is located at the top of the mounting base 101. A first channel 131 is opened in the heat conducting block 130; one end of the first channel 131 penetrates the top end face of the heat conducting block 130; the other end of the first channel 131 penetrates the side wall or the bottom end face of the heat conducting block 130, and a connecting pipe 132 is connected between the other end of the first channel 131 and the first heating table joint 112.

[0059] As an example, the top of the heat conducting block 130 extends out of the top of the mounting base 101, which is convenient for placing the material to be processed on the top of the heat conducting block 130. As another example, the ventilation channel 121 is a ventilation gap between the top of the heat conducting block 130 and the top of the mounting base 101, which can reduce the heat transferred from the heat conducting block 130 to the mounting base 101 while realizing the communication function and reducing heat loss. Of course, in other implementation schemes, the ventilation channel 121 can also be opened through the top of the heat conducting block 130, for example, opened in the area near the heat conducting block 130 on the top of the heat conducting block 130, and it can be any regular or irregular shape.

[0060] In some alternative embodiments, the connecting pipe 132 is a thin-walled TC4 pipe. TC4 has low thermal conductivity and high strength, so the wall thickness can be made thin, reducing the cross-sectional area of heat conduction. Therefore, the temperature of the end of the connecting pipe 132 far from the heat conducting block 130 can be greatly reduced.

[0061] As an example, the sealing method at the end of the connecting pipe 132 connected to the heat conducting block 130 adopts interference fit, and the sealing method for the connection between the other end and the first heating table joint 112 is a fluororubber O-ring. This sealing method has one end fixed and the other end has a certain expansion space, so that it is not easy for the mounting base 101 to crack due to thermal expansion when the temperature rises.

[0062] Optionally, the O-ring is made of 246 fluororubber. 246 fluororubber can work continuously at a temperature of 300 °C and still maintain good elasticity after aging at 350 °C for 16 hours. The outer diameter of the O-ring is slightly larger than the inner diameter of the first heating table joint 112, and the inner diameter of the O-ring is slightly smaller than the outer diameter of the connecting pipe 132, so that the O-ring can maintain a certain elastic deformation after installation and play a good sealing role.

[0063] The cover plate assembly 200 is used to be detachably placed on the top of the mounting base 101, so that the cover plate assembly 200 has a first state of covering the top of the mounting base 101 and a second state of detaching from the top of the mounting base 101.

[0064] Please refer to Figure 5 and Figure 6 , when the cover plate assembly 200 is in the first state of covering the top of the mounting base 101, there is a first cover plate cavity 211 between the cover plate assembly 200 and the top of the mounting base 101; and in this state, the ventilation channel 121 and the first channel 131 are both communicated with the first cover plate cavity 211. A first cover plate joint 212 communicating with the first cover plate cavity 211 is provided on the outside of the cover plate assembly 200.

[0065] As an example, the first cover plate cavity 211 is opened in the cover plate assembly 200 and penetrates through the bottom of the cover plate assembly 200. In this way, it is convenient to open the first cover plate cavity 211 and it is also convenient for the first cover plate joint 212 to communicate with the first cover plate cavity 211. Of course, in other embodiments, the first cover plate cavity 211 is not limited to being opened in the cover plate assembly 200. For example, an annular side wall can also be convexly provided on the top of the mounting base 101, and the first cover plate cavity 211 is enclosed by the cover plate assembly 200 abutting against the top of the annular side wall in the first state.

[0066] In the present application, the heating stage main body 100 can be used for heating treatment of a sample to be processed; when the cover plate assembly 200 is cooperated with the heating stage main body 100 by covering the top of the mounting base 101, it can be used for annealing treatment of the sample to be processed.

[0067] In the heating treatment stage, the material to be processed is placed on the top of the heat conducting block 130 to cover the opening at the top end of the first channel 131. By connecting the first heating stage joint 112 to a negative pressure, the material to be processed can be adsorbed on the top of the heat conducting block 130, facilitating the heat conducting block 130 to be heated to a preset temperature and then completing the heating treatment of the material to be processed. In this annealing treatment stage, the material to be processed after the heating treatment is placed on the top of the heat conducting block 130. By connecting the second heating stage joint 113 to a negative pressure, an environment with a certain degree of vacuum is provided for the first cover plate cavity 211 where the material to be processed is located. By connecting the first cover plate joint 212 to an annealing gas source, a specific annealing atmosphere is provided for the first cover plate cavity 211 where the material to be processed is located, facilitating the annealing treatment in a specific atmosphere and vacuum environment.

[0068] The heating device 10 provided by the present application combines heating treatment and annealing treatment, facilitating the heating device 10 to be placed in a specific preset environmental atmosphere condition to sequentially perform heating transfer and annealing treatment. The specific preset environmental atmosphere condition is, for example, a glove box environment.

[0069] After the heating transfer of the material is completed, there is no need to take out the sample from the processing environment and place it in a vacuum annealing furnace for separate annealing. The material to be processed can remain in the preset environmental atmosphere condition, effectively reducing the risk of the sample being damaged by contacting air after the transfer and before the annealing treatment.

[0070] It should be noted that in the heating stage main body 100 of the present application, the function of the heat conducting block 130 is to conduct heat, and a heating element corresponding to the heat conducting block 130 needs to be configured to heat the heat conducting block 130. Further, in order to better monitor the heating situation, optionally, a temperature sensing device corresponding to the heat conducting block 130 is also provided.

[0071] Please continue to refer to Figure 3 , as an example, the heating stage main body 100 further includes a heating sheet 133 and a screw type temperature probe 134; optionally, the heating sheet 133 is a ceramic heating sheet 133. The heating sheet 133 is attached to the bottom end face of the heat conducting block 130, and the screw type temperature probe 134 penetrates through the heating sheet 133 and is connected to the bottom of the heat conducting block 130.

[0072] The heating element is in the form of a heating sheet 133, which has a large heat dissipation area, facilitating the reduction of temperature overshoot caused by untimely heat dissipation of the heating component and its large self-energy storage. The heating sheet 133 is attached to the bottom end face of the heat conducting block 130, which is convenient to set up and has a relatively uniform heat conduction effect on the top of the heat conducting block 130. Of course, in other embodiments, the heating element is not limited to being set as a sheet, for example, it can also be set as a heating rod; the heating element is not limited to being attached to the bottom of the heat conducting block 130, for example, it can be set on the side wall of the heat conducting block 130.

[0073] The screw type temperature probe 134 is convenient to be fixed on the heat conducting block 130 for temperature detection and can also fix the heating sheet 133. Of course, in other embodiments, the temperature sensing device can also be set in other common contact or non-contact forms.

[0074] Correspondingly, the heating table main body 100 is also provided with a vacuum aviation plug 114, which is exemplarily sealed and installed on the side wall of the heating table main body 100 through high-temperature resistant epoxy resin.

[0075] Furthermore, the heating table main body 100 further includes a spring washer 135. The spring washer 135 is attached to the bottom of the heating sheet 133. The screw type temperature probe 134 passes through the spring washer 135 and the heating sheet 133 in sequence and then is connected to the bottom of the heat conducting block 130.

[0076] The inventor's research found that during repeated heating and cooling processes, the heat conducting block 130 will expand and contract repeatedly. In the case where the spring washer 135 is not provided, as the use time prolongs, it is easy to occur that the connection between the screw type temperature probe 134 and the heat conducting block 130 is not tight, and then the temperature detection is inaccurate as the use time prolongs. The setting of the spring washer 135 is beneficial to keeping the screw type temperature probe 134 tightly connected to the heat conducting block 130, thus being beneficial to ensuring the accuracy of temperature detection.

[0077] Optionally, the material of the spring washer 135 is TC4 titanium alloy. In the embodiment where the spring washer 135 is provided, the spring washer 135 abuts between the heating sheet 133 and the screw type temperature probe 134. Since the contact area of the spring washer 135 itself with the heating sheet 133 and the screw type temperature probe 134 is relatively small, and a material with low thermal conductivity is adopted, the interference of the heating sheet 133 on the screw type temperature probe 134 can be reduced, making the temperature measured by the temperature probe closer to the actual temperature of the heat conducting block 130.

[0078] It can be understood that in the embodiments of the present application, the setting manners of the heating stage main body 100 and the cover plate assembly 200 are not limited, as long as the mentioned functional parts are provided; it can be set as an integrally formed structure, or can be obtained by assembling multiple components; it can be in a regular shape or an irregular shape.

[0079] Regarding the mounting seat 101 of the heating stage main body 100:

[0080] Please continue to refer to Figure 3 , in some exemplary embodiments, the mounting seat 101 includes a heat insulation ring 110 and a mounting plate 120.

[0081] The heat insulation ring 110 is exemplarily arranged in a circular ring shape, and its annular side wall encloses a heating stage cavity 111. The first heating stage connector 112, the second heating stage connector 113, and the vacuum aviation plug 114 are all arranged outside the heat insulation ring 110.

[0082] As an example, the material of the heat insulation ring 110 is TC4 titanium alloy. Since the thermal conductivity of TC4 is 7.955 W / m·K, which is only about 50% of the thermal conductivity of stainless steel; and the density of TC4 is smaller than that of stainless steel, the heat transferred from the heat conducting block 130 to the heat insulation ring 110 can be reduced. Further, the inner surface of the heat insulation ring 110 is silver-plated and polished, which can reflect the heat radiated from the heating sheet 133 and the heat conducting block 130 in all directions, further reducing the transfer of energy to the heat insulation ring 110. On this basis, the load of the ceramic heating sheet 133 can be greatly reduced, so a smaller heating power can be used, which is beneficial to reducing the temperature overshoot and thus reducing the risk of sample damage.

[0083] The mounting plate 120 is connected to the heat insulation ring 110 and closes the top of the heating stage cavity 111. A mounting hole is penetrated through the middle of the mounting plate 120, and a plurality of countersunk holes are also provided around the mounting hole. Correspondingly, the top of the heat conducting block 130 is inserted through the mounting hole with a gap, and the gap between the mounting plate 120 and the top of the heat conducting block 130 is the ventilation channel 121. Two mounting arms protrude outward from the side wall of the heat conducting block 130, for example, three mounting arms are evenly distributed circumferentially, and the mounting arms are locked in the countersunk holes by fasteners to realize the installation of the heat conducting block 130 on the mounting plate 120.

[0084] As an example, the material of the mounting plate 120 is quartz. Compared with metal materials, quartz has a lower thermal conductivity, which can reduce the heat dissipation of the heat conducting block 130; and compared with materials such as polytetrafluoroethylene, pvc, and acrylic, quartz has good high-temperature resistance and allows the heat conducting block 130 to be heated to a higher temperature, such as up to 400 °C.

[0085] Please refer to Figure 4, optionally, a plurality of communication holes 122 communicating with the heating table cavity 111 are formed through the top of the mounting base 101, that is, a plurality of communication holes 122 communicating with the heating table cavity 111 are formed through the mounting plate 120. When the cover plate assembly 200 is covered on the top of the mounting base 101, the communication holes 122 communicate with the first cover plate cavity 211. The arrangement of the communication holes 122 can reduce the cross-sectional area of the top of the mounting base 101, thereby reducing the transfer of the heat radiated to the heat conducting block 130, which is beneficial to reducing the low heat dissipation of the heat conducting block 130.

[0086] Further, the heating device 10 further includes an annular seal 300, and the annular seal 300 is, for example, an annular sealing ring. An annular mounting groove 123 is recessed in the top of the mounting base 101, that is, an annular mounting groove 123 is recessed in the top of the mounting plate 120, for detachably mounting the annular seal 300.

[0087] When the cover plate assembly 200 is covered on the top of the mounting base 101, the bottom end opening of the first cover plate cavity 211 is located inside the annular seal 300, and the ventilation channel 121 and the communication holes 122 are located inside the annular seal 300, so as to realize that both the ventilation channel 121 and the communication holes 122 communicate with the first cover plate cavity 211.

[0088] In the above setting method, the annular mounting groove 123 is provided for detachably mounting the annular seal 300, and the top of the annular seal 300 is in sealing fit with the bottom of the cover plate assembly 200, which can preferably realize the sealing fit between the top of the mounting base 101 and the cover plate assembly 200, so as to preferably separate the bottom end opening of the first cover plate cavity 211, the ventilation channel 121 and the communication holes 122 from the environment outside the annular seal 300. At the same time, the arrangement of the annular mounting groove 123 can also reduce the cross-sectional area of the mounting plate 120 at the top of the mounting base 101, thereby reducing the transfer of the heat radiated to the heat conducting block 130.

[0089] Regarding the heat conducting block 130 of the heating table main body 100:

[0090] In some exemplary embodiments, the first channel 131 is L-shaped, which includes a first section channel extending in the vertical direction and a second section channel extending in the horizontal direction. The first section channel is arranged near the top of the heat conducting block 130, and the top end of the first section channel penetrates through the top end face of the heat conducting block 130; the second section channel is arranged near the bottom of the heat conducting block 130, one end of which is connected to the bottom end of the first section channel, and the other end of which is connected to the first heating table joint 112 through a connecting pipe 132.

[0091] As an example, the material of the heat conduction block 130 is aluminum. Compared with copper, the product of the specific heat capacity and density of aluminum is smaller than that of copper, that is, for the same volume of aluminum and copper heated to a certain temperature, aluminum consumes less heat. In particular, the inventor has found through research that copper is prone to oxidation at high temperatures, forming a layer of fragile oxide skin. This oxide skin is easy to peel off, and the peeled oxide skin is easily sucked into the vacuum pump when the first heating stage joint 112 is connected to a negative pressure structure such as a vacuum pump, which affects the service life of the vacuum pump; moreover, the oxide skin will also contaminate the environment where the sample is located. Aluminum will form a dense oxide film at high temperatures, and this oxide film will not fall off, so the above problems can be effectively avoided.

[0092] Regarding the cover plate assembly 200:

[0093] Please continue to refer to Figure 5 and Figure 6 , as an example, the cover plate assembly 200 includes a cover plate base 201 and an observation window 230, and the observation window 230 is exemplarily a quartz plate.

[0094] The cover plate base 201 includes a base body bottom plate 220 and a base body annular side plate 210. The base body annular side plate 210 encloses a first cover plate cavity 211, and the base body bottom plate 220 is connected to the base body annular side plate 210. The first cover plate cavity 211 penetrates through the base body bottom plate 220 at the bottom of the cover plate assembly 200 to form an observation hole 221. The top of the cover plate assembly 200 has a mounting through hole communicating with the first cover plate cavity 211, and an observation window 230 corresponding to the observation hole 221 is installed in the mounting through hole.

[0095] When the cover plate assembly 200 is covered on the top of the mounting base 101, the observation hole 221 corresponds to the heat conduction block 130, and both the ventilation channel 121 and the first channel 131 communicate with the first cover plate cavity 211 through the observation hole 221.

[0096] In the above technical solution, the observation window 230 corresponds to the observation hole 221, and the annealing process of the sample on the top of the heat conduction block 130 corresponding to the observation hole 221 can be observed. On the one hand, it is convenient to directly observe the progress of sample annealing and save research time; on the other hand, the visual annealing process can also provide more experimental information for research.

[0097] In some exemplary embodiments, a mounting step 231 is annularly provided on the circumference of the mounting through hole. The mounting step 231 includes an annular step side wall 232 and an annular step bottom wall 234, and the annular step bottom wall 234 is connected to the inner side of the bottom of the annular step side wall 232; the observation window 230 is arranged on the mounting step 231 to close the mounting through hole. In the above setting method, the observation window 230 is installed by setting the mounting step 231, so that the observation window 230 can be better fitted in the cover plate assembly 200.

[0098] Further, an annular sealing ring is connected between at least one of the annular step sidewall 232 and the annular step bottom wall 234 and the observation window 230. The annular sealing ring is, for example, accommodated in an annular groove recessed in the annular step sidewall 232 and the annular step bottom wall 234.

[0099] As an example, the annular step sidewall 232 is recessed with a sidewall groove, in which a first annular sealing ring 233 is installed. The first annular sealing ring 233 serves a sealing function; secondly, it provides a fixing function to clamp the observation window 230; thirdly, it provides a buffering function. When the temperature rises, due to the different materials and expansion coefficients of the observation window 230 and the cover plate base 201, when adhesively connecting with rigid epoxy resin glue, when the observation window 230 is relatively thin, cracks are likely to appear in the observation window 230, while the buffering function of the first annular sealing ring 233 can effectively prevent cracks from appearing in the observation window 230. The annular step bottom wall 234 is recessed with a bottom wall groove, in which a second annular sealing ring 235 is installed for tightly connecting with the bottom wall of the observation window 230.

[0100] Further, an annular protrusion 222 is provided at the bottom of the cover plate assembly 200, that is, the upper surface of the seat body bottom plate 220 is convex with an annular protrusion 222. The annular protrusion 222 is located in the first cover plate cavity 211 and surrounds the observation hole 221. The top of the annular protrusion 222 is flush with the annular step bottom wall 234, and is used to cooperate with the annular step bottom wall 234 to better support the observation window 230, which is beneficial to reducing the thickness of the observation window 230. The thickness of the observation window 230 can be reduced to about 1.5 mm, so that the light transmittance of the observation window 230 is better; it can also reduce the minimum working distance required by the objective lens, so as to achieve better observation.

[0101] The annular protrusion 222 is provided with a connection channel 223 for communicating the inside and outside of the annular protrusion 222. After introducing the annealing atmosphere gas through the first cover plate joint 212, the annealing atmosphere gas can enter the inner cavity of the annular protrusion 222 from the outer cavity of the annular protrusion 222, so as to provide an annealing atmosphere for the material to be processed at the top of the heat conducting block 130 corresponding to the observation hole 221.

[0102] Please continue to refer to Figure 5 and Figure 6 , in some alternative embodiments, the cover plate assembly 200 further has a second cover plate cavity 213, which is opened in the seat body annular side plate 210 and penetrates through the top of the seat body annular side plate 210. The cover plate base 201 further includes a sealing cover plate 240 for closing the opening of the second cover plate cavity 213 at the top of the seat body annular side plate 210.

[0103] On the outer side of the cover plate assembly 200, there is also a second cover plate joint 214 communicating with the second cover plate cavity 213. The second cover plate joint 214 is arranged on the outer wall of the annular side plate. The second cover plate cavity 213 is located outside the first cover plate cavity 211, and a second channel 224 communicating with the second cover plate cavity 213 is provided at the bottom of the cover plate assembly 200.

[0104] When the cover plate assembly 200 is covered on the top of the mounting seat 101, the second channel 224 corresponds to the top of the mounting seat 101, and the top of the mounting seat 101 separates the first cover plate cavity 211 and the second cover plate cavity 213. In an embodiment where an annular seal 300 is provided between the cover plate assembly 200 and the top of the mounting seat 101, the second channel 224 is located outside the annular seal 300, and the annular seal 300 separates the first cover plate cavity 211 and the second cover plate cavity 213.

[0105] In the above technical solution, the top of the mounting seat 101 separates the first cover plate cavity 211 and the second cover plate cavity 213, so that the first cover plate cavity 211 communicates with the inner cavity of the mounting seat 101, and the second cover plate cavity 213 communicates with the external environment of the mounting seat 101. The second channel 224 corresponds to the top of the mounting seat 101, which facilitates the gas in the second cover plate cavity 213 to be blown out through the second channel 224 and then purged onto the top of the mounting seat 101, which can cool the top of the mounting seat 101 and is beneficial for better annealing treatment.

[0106] Optionally, in the cross-section of the cover plate assembly 200, the second channel 224 extends along an arc path, and the central angle of the arc path is greater than 300°.

[0107] In the above setting method, the second channel 224 is a large-arc circular arc, which is similar to a C-shaped structure, and can better correspond to the top of the mounting seat 101 in the axial direction, so that the gas purged onto the top of the mounting seat 101 can achieve a more sufficient and uniform cooling effect.

[0108] Furthermore, in the cross-section of the cover plate assembly 200, the second cover plate cavity 213 and the sealing cover plate 240 are circular arcs corresponding to the second channel 224; the number of the second cover plate joints 214 is two, and they are respectively communicated with both ends of the second cover plate cavity 213 in the circular arc extension direction. This setting method can more conveniently provide a gas source for the second channel 224.

[0109] Correspondingly, the first cover plate joint 212 is arranged between the two second cover plate joints 214, and it communicates with the first cover plate cavity 211 through a channel that radially penetrates the seat body annular side plate 210 along the seat body annular side plate 210.

[0110] It is understood that in other embodiments, the second channel 224 can be arranged in any way. For example, it can also be arranged in multiple numbers and distributed at intervals along the circumferential direction of the annular side plate 210 of the base body in the form of circular through holes. The arrangement of the second cover cavity 213 is not limited either. For example, it can also be arranged in multiple numbers and distributed at intervals along the circumferential direction of the annular side plate 210 of the base body in the form of cylinders.

[0111] To better achieve the installation and heat insulation of the heating table main body 100, as an example, the heating device 10 further includes a heat insulation table 400.

[0112] Please refer to Figure 7 , the heat insulation table 400 includes a heat insulation seat 410, a side reflective structure 420 and a bottom reflective structure 430; the heat insulation seat 410 is used to connect the mounting seat 101, and a heat insulation chamber 411 for communicating with the heating table cavity 111 is recessed at the top of the heat insulation seat 410; the side reflective structure 420 surrounds the side wall of the heat insulation chamber 411, and the bottom reflective structure 430 is arranged at the bottom of the heat insulation chamber 411. Optionally, the side reflective structure 420 and the bottom reflective structure 430 are mirror structures with a silver-plated layer on the inner side, which are used to reflect the thermal radiation of the heating table main body 100, which is beneficial to reducing the heat loss of the heating table main body 100 and the heat transferred to the outside.

[0113] The embodiment of the present application provides a material heat treatment method, which is carried out by using the above-mentioned heating device 10, and includes performing the following operations under preset environmental atmosphere conditions, and the preset environmental atmosphere conditions are provided, for example, by placing the heating device 10 in a glove box.

[0114] S1. Place the material to be processed on the top of the heat conduction block 130 and cover the opening of the first channel 131.

[0115] S2. Connect the first heating table joint 112 to negative pressure, for example, connect it to a vacuum pump, so that negative pressure is generated in the first channel 131 to adsorb and fix the material to be processed on the top of the heat conduction block 130.

[0116] S3. Heat the heat conduction block 130 to a preset temperature to complete the heat treatment of the material to be processed. The material to be processed is, for example, a two-dimensional material. During the heat treatment, turn on the heating device and set the heating temperature to a specific temperature required for transferring the two-dimensional material, and start preparing the two-dimensional material heterojunction.

[0117] After the heat treatment is completed, stop heating and disconnect the negative pressure connection of the first heating table joint 112.

[0118] S4. Place the heat-treated material to be processed on the top of the heat conduction block 130.

[0119] S5. Connect the second heating stage joint 113 to negative pressure and connect the first cover plate joint 212 to the annealing gas source. The second heating stage joint 113 is connected to a negative pressure, for example, by connecting to a vacuum pump. Then, turn on the heating device and set the heating temperature to a specific temperature required for annealing, and start the annealing process for the material to be processed.

[0120] In the present application, the heating stage main body 100 of the heating device 10 is used to adsorb the material to be processed for heating, and the heating stage main body 100 and the cover plate assembly 200 are used in cooperation to provide a specific atmosphere and vacuum environment for the material to be processed for annealing. After the heating and transfer of the material are completed, there is no need to take the sample out of the processing environment and place it in a vacuum annealing furnace for separate annealing. The material to be processed can remain in the preset environmental atmosphere conditions, which can effectively reduce the risk of the sample being damaged when it comes into contact with air after the transfer and before the annealing process.

[0121] In some exemplary embodiments, the heating stage main body 100 of the heating device 10 is further provided with a three-way structure (not shown in the figure), and the three-way structure is, for example, a three-way butterfly valve. Two of the connecting ends of the three-way structure are respectively communicated with the first heating stage joint 112 and the second heating stage joint 113, and the remaining one connecting end is used to connect to a negative pressure structure such as a vacuum pump, which is convenient for switching the passage communicated with the negative pressure structure during the heating process and the annealing process.

[0122] In the embodiment where the cover plate assembly 200 further has a second cover plate cavity 213 and a second cover plate joint 214, in step S5, it further includes: connecting the second heating stage joint 113 to the ambient gas source, so that the ambient gas source is introduced into the second cover plate cavity 213 and blown out from the second channel 224 during the annealing process, to realize purging and cooling of the top of the mounting base 101.

[0123] In the embodiment where the cover plate assembly 200 further has an observation window 230, in step S5, it further includes: after starting the annealing process, adjusting the heating device 10 and / or the microscope so that the material to be processed observed from the observation window 230 is in the center of the microscope field of view, which is convenient for observing the annealing process.

[0124] The above are only the preferred embodiments of the present application and are not used to limit the present application. For those skilled in the art, the present application can have various changes and modifications. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A heating device, characterized in that, it includes: a heating table main body, including a mounting base and a heat conducting block; a heating table cavity is provided inside the mounting base, and a ventilation passage communicating with the heating table cavity is provided at the top of the mounting base; a first heating table joint and a second heating table joint communicating with the heating table cavity are provided outside the mounting base; the heat conducting block is mounted on the mounting base, and the top of the heat conducting block is located at the top of the mounting base; a first channel is opened in the heat conducting block, one end of the first channel penetrates the top end face of the heat conducting block, and a connecting pipe is connected between the other end of the first channel and the first heating table joint; a cover plate assembly, when covering the top of the mounting base, has a first cover plate cavity between it and the top of the mounting base; the ventilation passage and the first channel both communicate with the first cover plate cavity; a first cover plate joint communicating with the first cover plate cavity is provided outside the cover plate assembly; a second cover plate cavity is further provided inside the cover plate assembly, and a second cover plate joint communicating with the second cover plate cavity is provided outside; the second cover plate cavity is located outside the first cover plate cavity, and a second channel communicating with the second cover plate cavity is provided at the bottom of the cover plate assembly; when the cover plate assembly covers the top of the mounting base, the second channel corresponds to the top of the mounting base, and the top of the mounting base separates the first cover plate cavity and the second cover plate cavity; an installation through hole communicating with the first cover plate cavity is provided at the top of the cover plate assembly, and an installation step is annularly provided on the circumference of the installation through hole; a ring-shaped protrusion is provided at the bottom of the cover plate assembly; a connecting channel is opened in the ring-shaped protrusion for communicating the inside and outside of the ring-shaped protrusion.

2. The heating device according to claim 1, characterized in that, the first cover plate cavity is opened in the cover plate assembly and penetrates the bottom of the cover plate assembly, the first cover plate cavity penetrates the bottom of the cover plate assembly to form an observation hole, and an observation window corresponding to the observation hole is installed at the top of the cover plate assembly; when the cover plate assembly covers the top of the mounting base, the observation hole corresponds to the heat conducting block, and the ventilation passage and the first channel both communicate with the first cover plate cavity through the observation hole.

3. The heating device according to claim 2, characterized in that, the installation step includes an annular step side wall and an annular step bottom wall, and the annular step bottom wall is connected to the inner side of the bottom of the annular step side wall; the observation window is arranged on the installation step to close the installation through hole, and an annular sealing ring is connected between at least one of the annular step side wall and the annular step bottom wall and the observation window.

4. The heating device according to claim 3, characterized in that, the ring-shaped protrusion is located in the first cover plate cavity and surrounds the observation hole; the top of the ring-shaped protrusion is flush with the annular step bottom wall.

5. The heating device according to claim 1, characterized in that, in the cross-section of the cover plate assembly, the second channel extends along an arc path, and the central angle of the arc path is greater than 300°.

6. The heating device according to claim 1, wherein, the ventilation channel is a ventilation gap between the top of the heat conducting block and the top of the mounting base; a plurality of communication holes communicating with the cavity of the heating table are also formed through the top of the mounting base; when the cover plate assembly covers the top of the mounting base, the communication holes communicate with the first cover plate cavity.

7. The heating device according to any one of claims 1 to 6, wherein, the heating table body further includes a heating sheet and a screw type temperature probe, the heating sheet is attached to the bottom end surface of the heat conducting block, and the screw type temperature probe penetrates through the heating sheet and is connected to the bottom of the heat conducting block.

8. The heating device according to any one of claims 1 to 6, wherein, the heating device further includes a heat insulation table, and the heat insulation table includes a heat insulation seat, a side surface light reflecting structure and a bottom surface light reflecting structure; the heat insulation seat is used for connecting the mounting base, and a heat insulation chamber communicating with the cavity of the heating table is recessed at the top of the heat insulation seat; the side surface light reflecting structure surrounds the side wall of the heat insulation chamber, and the bottom surface light reflecting structure is arranged at the bottom of the heat insulation chamber.

9. A material heat treatment method, wherein, it is carried out by using the heating device according to any one of claims 1 to 8, and includes, under preset ambient atmosphere conditions: placing the material to be treated on the top of the heat conducting block and covering the opening of the first channel; connecting the first heating table joint to negative pressure and heating the heat conducting block to a preset temperature to complete the heating treatment of the material to be treated; placing the material to be treated after the heating treatment on the top of the heat conducting block; and connecting the second heating table joint to negative pressure and connecting the first cover plate joint to an annealing gas source to carry out annealing treatment on the material to be treated.

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