CN219058558U - Heat treatment equipment - Google Patents
Heat treatment equipment Download PDFInfo
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- CN219058558U CN219058558U CN202223229413.6U CN202223229413U CN219058558U CN 219058558 U CN219058558 U CN 219058558U CN 202223229413 U CN202223229413 U CN 202223229413U CN 219058558 U CN219058558 U CN 219058558U
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Abstract
The present application relates to a heat treatment apparatus comprising: the furnace body is provided with at least one temperature measuring channel, and the temperature measuring channel extends into the furnace body; the heating mechanism is arranged in the furnace body; the temperature measuring mechanism comprises a first temperature measuring device and a second temperature measuring device, wherein the first temperature measuring device and the second temperature measuring device are alternately arranged in the temperature measuring channel, the temperature measuring range of the first temperature measuring device is 0-1800 ℃, and/or the temperature measuring range of the second temperature measuring device is 800-3200 ℃, the temperature of the low-temperature stage is measured through the first temperature measuring device, the temperature of the high-temperature stage is measured through the second temperature measuring device, and the heat conducting performance of the heat conducting composite film prepared at a high temperature through the high temperature of the application is improved through accurate measurement of the whole high-temperature process.
Description
Technical Field
The application belongs to the technical field of graphitization equipment, and particularly relates to heat treatment equipment.
Background
The existing heat-conducting composite film has the defects of low heat conductivity coefficient and huge difference from theoretical data, researchers are exploring an improved method, and the heat treatment process in the preparation process of the heat-conducting composite film is roughly divided into three steps: preheating, carbonizing and graphitizing, in the prior art, the raw materials are usually preheated in an oven at a low temperature below 1000 ℃, after the preheating is finished, the materials are cooled to room temperature and then taken out, then are placed in a carbonizing furnace for carbonizing, after the carbonizing is finished, the materials are cooled to room temperature and then are taken out, and finally, the materials are placed in the graphitizing furnace for graphitizing. At present, most researchers focus on improving a single heat treatment process, but little research is done on influencing relation among various heat treatment steps, how to reduce production cost and improvement of equipment, which directly results in high production cost, low through yield of products, high maintenance cost of equipment and lower performance of the products of the whole heat-conducting composite film, and is very unfavorable for improving the performance of the heat-conducting composite film, reducing the manufacturing cost and even developing the industry of the heat-conducting composite film.
Therefore, there is an urgent need to improve the thermal conductivity of the thermally conductive composite film.
Disclosure of Invention
In order to overcome the defects, the application provides heat treatment equipment, which can accurately measure the temperature of a low-temperature stage of 0-1800 ℃ and a high-temperature stage of 800-3200 ℃, does not need to replace other heat treatment equipment in the heat treatment process of the whole heating mechanism, does not have a cooling process, can improve the compactness of the internal molecular structure of the heat-conducting composite film, reduces the defects of a follow-up graphitization structure, and further improves the heat-conducting property of the heat-conducting composite film and reduces the production cost.
In a first aspect, embodiments of the present application provide a heat treatment apparatus, including:
the furnace body is provided with at least one temperature measuring channel, and the temperature measuring channel extends into the furnace body;
the heating mechanism is arranged in the furnace body;
the temperature measuring mechanism comprises a first temperature measuring device and a second temperature measuring device, the first temperature measuring device and the second temperature measuring device are alternately arranged in the temperature measuring channel, the temperature measuring range of the first temperature measuring device is 0-1800 ℃, and/or the temperature measuring range of the second temperature measuring device is 800-3200 ℃.
In some embodiments, the heat treatment apparatus further comprises a controller, an output of the controller is connected to the heating mechanism, an input of the controller is connected to the first and second thermometers, and the controller receives temperature data of the first and second thermometers and adjusts a heating temperature of the heating mechanism.
In some embodiments, the first temperature detector measures the temperature inside the furnace body in the preheating treatment and/or carbonization treatment stage, the second temperature detector measures the temperature inside the furnace body in the carbonization treatment and/or graphitization treatment stage, the temperature of the preheating treatment is 80 ℃ to 200 ℃, the temperature of the carbonization treatment is 800 ℃ to 1800 ℃, and the temperature of the graphitization treatment is 2800 ℃ to 3200 ℃.
In some embodiments, the first temperature detector is any one of a ceramic temperature probe, a thermocouple, a thermistor, a resistive temperature detector, and a low temperature infrared temperature gun.
In some embodiments, the second temperature detector is any one of a laser infrared temperature probe, a high temperature infrared temperature gun and an infrared temperature detector.
In some embodiments, the temperature measuring channel is arranged at the side surface and/or the top of the furnace body.
In some embodiments, the interior of the thermometric channel is filled with a thermal insulation material.
In some embodiments, the temperature measuring channel is provided with a temperature measuring port, the temperature measuring port is arranged on the outer surface of the furnace body, and a heat insulation plug is detachably arranged in the temperature measuring port.
In some embodiments, the heat treatment apparatus further comprises a conveying component, an input end of the conveying component is connected with the controller, an output end of the conveying component is respectively connected with a first temperature detector and a second temperature detector, and the conveying component moves to enable the first temperature detector to be arranged inside the temperature measuring channel; or (b)
The conveying assembly is moved so that the second temperature detector is arranged inside the temperature measuring channel.
In some embodiments, the temperature measuring channel is made of any one of graphite, zirconia, alumina, corundum and yttria.
The technical scheme of the application has the following beneficial effects:
in the heat treatment equipment, the first temperature detector and the second temperature detector are alternately arranged in the temperature measuring channel, the temperature measuring range of the first temperature detector is 0-1800 ℃, and/or the temperature measuring range of the second temperature detector is 800-3200 ℃, so that the first temperature detector measures the temperature of the heating mechanism in the low-temperature stage furnace body, and the second temperature detector measures the temperature of the heating mechanism in the high-temperature stage furnace body, namely, the heat treatment equipment can accurately measure the temperature of the low-temperature stage of 0-1800 ℃ and the temperature of the high-temperature stage of 800-3200 ℃, other heat treatment equipment is not required to be replaced in the heat treatment process of the whole heating mechanism, the cooling process is not required, the compactness of the internal molecular structure of the heat conducting composite film prepared by the heat treatment equipment can be improved, the defect of a follow-up graphitization structure is reduced, and the heat conducting performance of the heat conducting composite film prepared by the heat treatment equipment is improved. In addition, the heat treatment equipment can continuously perform temperature measurement in a low-temperature stage and a high-temperature stage, so that gas generated by materials is automatically discharged when the temperature is raised, and the gas in the heat treatment equipment is little or even no gas, and can play a role in vacuum-like. The heat treatment equipment is simple in structure, the blank that the existing graphitization equipment cannot accurately measure the preheating treatment temperature is overcome, the application range of the heat treatment equipment is enlarged, and the production cost is reduced.
Drawings
The present application is further described below with reference to the drawings and examples.
FIG. 1 is a schematic view of a heat treatment apparatus of the present application;
FIG. 2 is a top view of the heat treatment apparatus of the present application;
fig. 3 is a schematic diagram showing electrical connection of a controller of the heat treatment apparatus of the present application.
Fig. 1 to 3 show:
1-a furnace body;
2-a temperature measuring channel;
3-a heating mechanism;
31-a first electrode;
32-a second electrode;
4-a temperature measuring mechanism;
41-a first temperature measurer;
42-a second temperature measurer;
5-a controller;
6-a thermal insulation plug.
Detailed Description
For a better understanding of the technical solutions of the present application, embodiments of the present application are described in detail below with reference to the accompanying drawings.
It should be understood that the described embodiments are merely some, but not all, of the embodiments of the present application. All other embodiments, based on the embodiments herein, which would be apparent to one of ordinary skill in the art without making any inventive effort, are intended to be within the scope of the present application.
The terminology used in the embodiments of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be understood that the term "and/or" as used herein is merely one relationship describing the association of the associated objects, meaning that there may be three relationships, e.g., a and/or B, may represent: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
The existing heat-conducting composite film has the defects of low heat conductivity coefficient and huge difference from theoretical data, and the heat treatment process in the preparation process of the heat-conducting composite film is roughly divided into three steps: the parameters of preheating treatment, carbonization and graphitization are a critical link, the microstructure and heat conductivity of the composite film can be greatly influenced, most researchers focus on improving a certain heat treatment process, but the influence relation among various heat treatment steps, how to reduce the production cost and the improvement research of equipment are very few, so that the improvement effect is not ideal, and the large-scale batch production is difficult to realize.
Generally, the graphitization temperature is about 3000 ℃, the design of the existing graphitization furnace is mainly to facilitate the monitoring and heating of the temperature about 3000 ℃, the furnace body structure and the charging mode lead to the failure of accurate temperature monitoring of the low temperature section within 1000 ℃, therefore, the conventional practice is to firstly preheat the carbon-based raw material coating film in the oven below 1000 ℃, take out the carbon-based raw material coating film after cooling in the middle, and place the carbon-based raw material coating film in the carbonization furnace and the graphitization furnace for carbonization and graphitization, and the applicant finds that the heat treatment of each procedure in the preparation process of the heat-conducting composite film can be influenced mutually after a great deal of research on the relation between the heat treatment step and the performance of the composite film, and the influence of the low temperature Duan Jieduan within 1000 ℃ on the heat-conducting performance of the heat-conducting composite film is great. Specifically, during the cooling process among the preheating treatment, carbonization and graphitization processes, the carbon-based material fragments in the heat-conducting composite film can expand and shrink repeatedly along with the rise and the reduction of the temperature, and the impurities in the heat-conducting composite film are difficult to discharge in time, so that the energy threshold requirements of the rearrangement of the carbon-based material structure and the recombination of carbon-carbon bonds in the graphitization process are higher, more defects can exist on the structure, and thus the obtained heat-conducting composite film can have incoherence on the microstructure or connection disorder of the microstructure, and the heat-conducting property of the heat-conducting composite film is lower. If preheating treatment, carbonization treatment and heat treatment equipment are directly integrated into a whole for preparing the heat-conducting composite film, on one hand, vacuumizing treatment is needed for the integrated equipment, and then vacuum equipment is needed to be additionally arranged, so that the difficulty of equipment design is greatly increased; on the other hand, the collection of three devices occupies a large space and has high energy consumption, and the effect of reducing the cost and enhancing the efficiency cannot be achieved.
Therefore, based on the above research, the applicant thinks of designing a device, which can realize the preheating treatment, the carbonization treatment and the graphitization treatment in the device successively, and the material does not need to be taken out in the middle, and the temperature reduction process is not needed, and the precise temperature control of three stages can be realized, so that the structural defects caused by the temperature reduction process are avoided.
An embodiment of the present application provides a heat treatment apparatus, as shown in fig. 1 and 2, including:
the furnace body 1 is provided with at least one temperature measuring channel 2, and the temperature measuring channel 2 extends into the furnace body 1;
the heating mechanism 3 is arranged inside the furnace body 1;
the temperature measuring mechanism 4, the temperature measuring mechanism 4 comprises a first temperature measuring device 41 and a second temperature measuring device 42, the first temperature measuring device 41 and the second temperature measuring device 42 are alternately arranged in the temperature measuring channel 2, the temperature measuring range of the first temperature measuring device 41 is 0 ℃ to 1800 ℃, and/or the temperature measuring range of the second temperature measuring device 42 is 800 ℃ to 3200 ℃.
In the above scheme, in the heat treatment device of the present application, the first temperature detector 41 and the second temperature detector 42 are alternately arranged in the temperature measurement channel 2, and the temperature measurement range of the first temperature detector 41 is 0 ℃ to 1800 ℃, and the temperature measurement range of the second temperature detector 42 is 800 ℃ to 3200 ℃, so that the first temperature detector 41 measures the temperature of the heating mechanism 3 in the low temperature stage furnace body 1, and the second temperature detector 42 measures the temperature of the heating mechanism 3 in the high temperature stage furnace body 1, namely, the heat treatment device of the present application can accurately measure the temperature of the low temperature stage of 0 ℃ to 1800 ℃ and the temperature of the high temperature stage of 800 ℃ to 3200 ℃, no other heat treatment devices need to be replaced in the heat treatment process of the whole heating mechanism 3, no cooling process exists, the compactness of the internal molecular structure of the heat conducting composite film can be improved, the defect of the subsequent graphitization structure is reduced, and the heat conducting performance of the heat conducting composite film prepared by the heat treatment device of the present application is improved. In addition, the heat treatment equipment can continuously perform temperature measurement in a low-temperature stage and a high-temperature stage, so that gas generated by materials is automatically discharged when the temperature is raised, and the gas in the heat treatment equipment is little or even no gas, and can play a role in vacuum-like. The heat treatment equipment is simple in structure, the blank that the existing graphitization equipment cannot accurately measure the preheating treatment temperature is overcome, the application range of the heat treatment equipment is enlarged, and the production cost is reduced.
In the present application, the temperature measurement range of the first temperature detector 41 is, for example, from 0 ℃ to 1800 ℃, and the temperature measurement range of the first temperature detector 41 may be, for example, 10 ℃, 50 ℃,100 ℃, 120 ℃, 200 ℃, 500 ℃, 800 ℃,1000 ℃, 1200 ℃, 1500 ℃, 1800 ℃, etc., but may be other values within the above range, and the present application is not limited thereto. The temperature measurement range of the second temperature measuring device 42 is 800 ℃ to 3200 ℃, and the temperature measurement range of the second temperature measuring device 42 may be, for example, 800 ℃,1000 ℃, 1200 ℃, 1500 ℃, 1800 ℃, 2500 ℃, 2800 ℃, 3000 ℃, 3100 ℃, 3200 ℃ or the like, but may be other values within the above range, and the present application is not limited thereto.
It will be appreciated that the preheating process uses the first temperature detector 41, the graphitizing process uses the second temperature detector 42, and the carbonization process may use either the first temperature detector 41 or the second temperature detector 42.
In some embodiments, the heat treatment apparatus further includes a controller 5, as shown in fig. 3, which is a schematic diagram of electrical connection of the controller 5, where an input end of the controller 5 is connected with the first temperature detector 41 and the second temperature detector 42 respectively to perform electrical connection, so that temperature data and a temperature rising rate detected by the first temperature detector 41 and the second temperature detector 42 are transferred to the controller 5, an output end of the controller 5 is electrically connected with the heating mechanism 3, and the controller 5 adjusts a heating temperature of the heating mechanism 3 according to the data transferred by the temperature detectors, thereby performing process parameters of the dynamic heat treatment apparatus to achieve an effect of controlling an internal temperature of the furnace body 1.
In some embodiments, the temperature measuring mechanism 4 includes at least one of a contact temperature measuring probe and an induction temperature measuring probe. The contact type temperature measuring probe can be a thermocouple, a thermistor, a contact type ceramic temperature measuring probe and the like. The inductive temperature measuring probe can be an infrared temperature measuring probe, an infrared temperature measuring gun, an infrared temperature sensor and the like. The temperature measurement precision of the temperature measurement mechanism 4 is +/-0.1-0.5 ℃.
In some embodiments, the first temperature detector 41 is any one of a ceramic temperature probe, a thermocouple, a thermistor, a resistive temperature detector, and a low temperature infrared temperature gun. Wherein, the low-temperature infrared temperature measuring gun refers to an infrared temperature measuring gun with the test temperature of 0-1800 ℃. Preferably, the first temperature detector 41 is a ceramic temperature detector, and the ceramic temperature detector is used for measuring the temperature of preheating treatment and/or carbonization treatment, and the ceramic temperature detector can resist high temperature, can keep higher stability at the temperature below 1800 ℃, and has high measurement accuracy.
In some embodiments, the second temperature detector 42 is any one of a laser infrared temperature probe, a high temperature infrared temperature gun, and an infrared thermometer. Wherein, the high-temperature infrared temperature measuring gun refers to an infrared temperature measuring gun with the testing temperature of 800-3200 ℃.
In some embodiments, the first temperature detector 41 measures the temperature inside the furnace body in the preheating treatment and/or carbonization treatment stage, the second temperature detector 42 measures the temperature inside the furnace body in the carbonization treatment and/or graphitization treatment stage, the preheating treatment temperature is 80 ℃ to 200 ℃, and the preheating treatment temperature may be 80 ℃,100 ℃, 120 ℃, 150 ℃, 180 ℃, 200 ℃ or the like, and other values within the above range are of course possible, and the application is not limited herein. The carbonization temperature is 800 to 1800 ℃, and is exemplified by 800 ℃,1000 ℃, 1200 ℃, 1500 ℃, 1800 ℃ and the like, but other values within the above range are also possible, and the present application is not limited thereto. The graphitization treatment temperature is 2800 ℃ to 3200 ℃, and the graphitization treatment temperature is 2800 ℃, 2900 ℃, 3000 ℃, 3100 ℃ and 3200 ℃ and the like, but other values within the above range are also possible, and the present application is not limited thereto. Specific:
the preheating treatment comprises the following steps: the first temperature detector 41 is extended into the furnace body 1 through the temperature measuring channel 2, the temperature of the heat treatment equipment is raised to 80-200 ℃, the temperature raising rate is 0.01-2 ℃/min, and the heat is preserved for 100-480 min. The temperature of the preheating process is monitored in real time by the first temperature detector 41.
The carbonization treatment comprises: the temperature of the heat treatment equipment is continuously increased to 800-1800 ℃, the temperature increasing rate is 0.2-1.2 ℃/min, the temperature is kept for 30-240 min, in some embodiments, the temperature in the furnace body 1 is measured by a first temperature detector 41 below 1000 ℃ and the temperature in the furnace body 1 is measured by a second temperature detector 42 above 1000 ℃ in the heating process. In other embodiments, only the first temperature detector 41 is used to measure the temperature inside the furnace body 1 during the whole carbonization process.
The graphitization treatment comprises: continuously heating the heat treatment equipment to 2800-3200 ℃, preserving heat for 100-900 min, stopping power transmission, and naturally cooling the heat treatment equipment to room temperature. The temperature in the furnace body 1 is monitored in real time by the second temperature detector 42 in the whole graphitization treatment stage.
In some embodiments, the temperature measuring channel 2 is an inner hollow channel, and the temperature measuring channel 2 extends into the furnace body 1 through the surface of the furnace body 1, and further may extend into the furnace core in the furnace body 1 to measure the temperature in the furnace body 1. Because the temperature measuring channel 2 is communicated with the inside of the furnace body 1, the temperature measuring channel 2 is required to be prepared from refractory materials so as to meet the high temperature resistant requirement. The temperature measuring channel is made of any one of graphite, zirconia, alumina, corundum and yttria. The material of the temperature measuring channel can be any one of graphite, refractory bricks, zirconia bricks, alumina hollow sphere bricks, corundum bricks, yttria bricks, corundum bricks, low-sodium corundum bricks, high-purity corundum bricks, fused corundum bricks and light corundum bricks.
In some embodiments, at least one temperature measuring channel 2 is provided, preferably, 6 to 10 temperature measuring channels 2 are generally provided to improve the accuracy of temperature measurement, as shown in fig. 1, 6 temperature measuring channels 2 are provided, and it can be understood that the number of temperature measuring channels 2 is consistent with the number of temperature measuring mechanisms 4.
In some embodiments, the thermometric channels 2 are provided at the top and/or sides of the furnace body 1. When the temperature measuring channels 2 are arranged in a plurality, the temperature measuring channels 2 can be arranged at the top of the furnace body 1 and can also be arranged at the side face of the furnace body 1 so as to improve the accuracy of measuring the temperature.
In some embodiments, the temperature measuring channel 2 is filled with a heat insulating material, and in the process of taking out the first temperature measuring device 41 or the second temperature measuring device 42 from the temperature measuring channel 2, the heat insulating material is filled to reduce the dissipation of heat in the furnace body 1 near the temperature measuring channel 2, so that the problem of nonuniform internal temperature can be solved.
In some embodiments, the temperature measuring channel 2 is provided with a temperature measuring port, the temperature measuring port is arranged on the outer surface of the furnace body 1, and a heat insulation plug 6 is detachably arranged in the temperature measuring port. When no temperature measuring mechanism is arranged in the temperature measuring channel 2, the temperature measuring channel 2 is plugged through the heat insulation plug 6, so that the temperature reduction of the heat treatment equipment inside the furnace body 1 close to the temperature measuring channel 2 after the temperature measuring mechanism is taken out is avoided, the heat insulation function is achieved, and the heat conduction performance of the heat conduction composite film prepared by the heat treatment equipment is reduced.
In some embodiments, referring to fig. 2, the heating mechanism 3 includes a first electrode 31 and a second electrode 32 disposed at two ends inside the furnace body 1, where the first electrode 31 and the second electrode 32 are graphite electrodes, the first electrode 31 is an anode electrode, the second electrode 32 is a cathode electrode, and the first electrode 31 and the second electrode 32 are respectively externally connected with a power supply device, and the first electrode 31 and the second electrode 32 with high resistance are heated by high current generated by the power supply device, so that a higher temperature is generated inside the furnace body 1, thereby realizing heat treatment of materials in the furnace body 1.
In some embodiments, the heat treatment apparatus further includes a conveying assembly (the conveying assembly is not shown in the drawings), an input end of the conveying assembly is connected to the controller, an output end of the conveying assembly is connected to the first temperature detector 41 and the second temperature detector 42, respectively, the conveying assembly is moved so that the first temperature detector 41 or the second temperature detector 42 is disposed inside the temperature measuring channel 2, and the conveying assembly is a module commonly used in the art for controlling the position movement by the controller, which is not limited in this application. This application adopts conveying component to drive first thermoscope 41 or second thermoscope 42 and removes to make first thermoscope 41 or second thermoscope 42 set up in temperature measurement passageway 2, can be convenient for change use of first thermoscope 41 and second thermoscope 42, improve the operating efficiency, can avoid the manual work to change first thermoscope 41 and second thermoscope 42 simultaneously, improve operating personnel's safety in utilization.
In some embodiments, the controller 5 of the present application adopts an industrial personal computer as a core control unit of the device, and controls the execution unit through a compatible drive control card, an I/O card, an image acquisition card, and the like, for example, the movement of the conveying mechanism, the heating temperature of the heating structure, and the opening and closing of the first temperature detector 41 and the second temperature detector 42 are controlled in real time, and the man-machine interaction function and the visual operation window can set the heating temperature and the heating rate, store data, print data, and establish communication through a local area network and a service for data transmission, downloading and remote control.
Example 1
Referring to fig. 1-3, the heat treatment equipment of the application comprises a furnace body 1, a heating mechanism 3 is arranged in the furnace body 1, the heating mechanism 3 is connected with the output end of a controller 5, 6 temperature measuring channels 2 are arranged on the furnace body 1, the temperature measuring channels 2 extend into the furnace core in the furnace body 1, wherein three temperature measuring channels 2 are arranged at the top of the furnace body 1, three temperature measuring channels 2 are arranged on the side face of the furnace body 1, ceramic temperature measuring probes are uniformly distributed in the 6 temperature measuring channels 2, the 6 ceramic temperature measuring probes are respectively connected with the input end of the controller 5, and the controller 5 is used for controlling the heating mechanism 3 to start heat treatment of room temperature to 3200 ℃ on a graphene coating film in the furnace body 1.
In the heat treatment process at room temperature to 1000 ℃, the temperature rising curve is as follows: the room temperature is up to 90 ℃, the temperature and the heating rate are monitored by a ceramic temperature measuring probe, the heating rate is controlled to be 0.1 ℃/min, and the temperature is kept at 90 ℃ for 240min; then heating from 90 ℃ to 1000 ℃ at a heating rate of 0.3 ℃/min; after the internal temperature of the furnace body 1 reaches 1000 ℃, taking out the ceramic temperature measuring probes from the temperature measuring channels 2, placing 6 laser infrared temperature measuring probes into 6 temperature measuring channels 2, continuously heating to 1500 ℃ and preserving heat for 120min; heating from 1500 to 2500 ℃ at a rate of 0.3 ℃/min; then the temperature is raised from 2500 ℃ to 3000 ℃ at a speed of 1.0 ℃/min; then, the temperature is kept at the temperature of 3200 ℃ from 3000 ℃ to 0.6 ℃/min, the temperature is kept at the temperature of 3200 ℃ for 360min, after the heat preservation is finished, the laser infrared temperature measuring probe is taken out, the heat preservation plug 6 is plugged into the temperature measuring channel 2, then the power is cut off for natural cooling, and when the furnace temperature is cooled to the room temperature, the graphite crucible and the fluffy graphene film in the graphite crucible are taken out.
In the heating process, the temperature in the furnace body 1 is monitored at any time through the controller 5 so as to be convenient for judging whether the heating temperature in the furnace body 1 is equal to the preset heating curve 2, so that the heating temperature in the furnace body 1 is adjusted by using the controller 5 to reach the preset heating curve.
Compacting the fluffy graphene film under a vacuum platen press to obtain the graphene heat conduction composite film with the thickness of 35 mu m. The thermal diffusivity of the composite film was tested using LFA-467, test data 1043.243mm 2 /s, density of 2.182g/cm 3 The thermal conductivity is 1934.903W/mK.
Wherein, the vacuum degree of the vacuum platen press is-0.1 MPa, and the press pressure is 24MPa.
Comparative example 1
Placing the graphene coating film into an Acheson graphitizing furnace, and performing heat treatment on the graphene coating film by adopting the Acheson graphitizing furnace, wherein the temperature rise curve is as follows: the temperature is kept between room temperature and 90 ℃, the heating rate is 0.1 ℃/min, and the temperature is kept at 90 ℃ for 240min; then preserving heat for 120min from 90 ℃ to 1500 ℃; heating from 1500 to 2500 ℃ at a rate of 0.3 ℃/min; then the temperature is raised from 2500 ℃ to 3000 ℃ at a speed of 1.0 ℃/min; then, the temperature is kept at the temperature of between 3000 and 3200 ℃ for 360 minutes at the temperature of 3200 ℃ at the heating rate of 0.6 ℃/min, after the heat preservation is finished, the power is cut off, the temperature is naturally lowered, and when the furnace temperature is lowered to the room temperature, the graphite crucible and the fluffy graphene film in the graphite crucible are taken out.
In the heating treatment process, because the Acheson graphitizing furnace has no temperature measuring component, the temperature in the furnace is calculated at intervals by controlling the voltage and the current of power transmission, the accurate temperature measurement and the temperature control of the whole process cannot be realized, and the temperature of the whole heating process cannot be accurately measured and controlled.
And compacting the fluffy graphene film treated by the graphitizing furnace under vacuum and flat pressure to obtain the calendered graphene composite film. The thermal diffusivity of the composite film was tested using LFA-467, test data 675.516mm 2 Per s, density of 2.063g/cm 3 The thermal conductivity is 1184.551W/mK.
As can be seen from the comparison of example 1 and comparative example 1: the heat treatment equipment can realize accurate measurement and control of temperature in the process of heating from room temperature to 3200 ℃ so that the heat conduction performance of the composite film prepared by the heat treatment equipment is far better than that of the composite film prepared by adopting an Acheson graphitization furnace in comparative example 1.
Comparative example 2
Placing the graphene coating film into a blast oven for preheating treatment, wherein the temperature rise curve is as follows: the temperature is kept between room temperature and 90 ℃, the heating rate is 0.1 ℃/min, and the temperature is kept at 90 ℃ for 240min; naturally cooling to room temperature; placing the graphene coating film into a carbonization furnace, and preserving heat for 120min from room temperature to 1500 ℃; naturally cooling to room temperature; placing the graphene coating film into a graphitization furnace, and heating from room temperature to 2500 ℃ at a rate of 0.3 ℃/min; then the temperature is raised from 2500 ℃ to 3000 ℃ at a speed of 1.0 ℃/min; then, the temperature is kept at the temperature of between 3000 and 3200 ℃ for 360 minutes at the temperature of 3200 ℃ at the heating rate of 0.6 ℃/min, after the heat preservation is finished, the power is cut off, the temperature is naturally lowered, and when the furnace temperature is lowered to the room temperature, the graphite crucible and the fluffy graphene film in the graphite crucible are taken out.
And compacting the fluffy graphene film treated by the graphitizing furnace under vacuum and flat pressure to obtain the calendered graphene composite film. The thermal diffusivity of the composite film was tested using LFA-467, test data 630.815mm 2 Per s, density of 2.092g/cm 3 The thermal conductivity is 1121.715W/mK.
Comparison of example 1 and comparative example 2 shows that: the temperature reduction process is carried out in each heat treatment stage in comparative example 2, and the obtained composite film has poorer heat conduction performance than the composite film obtained in the example, which indicates that the heat conduction performance of the heat conduction composite film can be improved by preparing the heat conduction composite film by the heat treatment equipment.
The foregoing has outlined a detailed description of a heat treatment apparatus provided herein, wherein specific examples have been provided to illustrate the principles and embodiments of the present application, the above examples being provided only to assist in understanding the method of the present application and the core ideas thereof; meanwhile, as those skilled in the art will have modifications in the specific embodiments and application scope in accordance with the ideas of the present application, the present description should not be construed as limiting the present application in view of the above.
Claims (10)
1. A heat treatment apparatus, characterized by comprising:
the furnace body is provided with at least one temperature measuring channel, and the temperature measuring channel extends into the furnace body;
the heating mechanism is arranged in the furnace body;
the temperature measuring mechanism comprises a first temperature measuring device and a second temperature measuring device, wherein the first temperature measuring device and the second temperature measuring device are alternately arranged in the temperature measuring channel, the temperature measuring range of the first temperature measuring device is 0-1800 ℃, and/or the temperature measuring range of the second temperature measuring device is 800-3200 ℃.
2. The heat treatment apparatus according to claim 1, further comprising a controller, an output of the controller being connected to the heating mechanism, an input of the controller being connected to the first temperature detector and the second temperature detector, the controller receiving temperature data of the first temperature detector and the second temperature detector and adjusting a heating temperature of the heating mechanism.
3. The heat treatment apparatus according to claim 1, wherein the first temperature detector measures an internal temperature of a furnace body in a preheating treatment and/or a carbonization treatment stage, the second temperature detector measures an internal temperature of a furnace body in a carbonization treatment and/or a graphitization treatment stage, the preheating treatment temperature is 80 ℃ to 200 ℃, the carbonization treatment temperature is 800 ℃ to 1800 ℃, and the graphitization treatment temperature is 2800 ℃ to 3200 ℃.
4. The heat treatment apparatus according to claim 1, wherein the first temperature detector is any one of a ceramic temperature probe, a thermocouple, a thermistor, a resistance temperature detector, and a low temperature infrared temperature measuring gun.
5. The heat treatment apparatus of claim 1, wherein the second temperature detector is any one of a laser infrared temperature probe, a high temperature infrared temperature gun, and an infrared temperature detector.
6. The heat treatment apparatus according to claim 1, wherein the temperature measuring channel is provided at a side and/or top of the furnace body.
7. The heat treatment apparatus according to claim 1, wherein the interior of the thermometric channel is filled with a thermal insulation material.
8. The heat treatment apparatus according to claim 1, wherein the temperature measuring channel has a temperature measuring port provided on an outer surface of the furnace body, and a heat insulating plug is detachably provided in the temperature measuring port.
9. The heat treatment apparatus according to claim 2, further comprising a conveying assembly, wherein an input end of the conveying assembly is connected to the controller, and an output end of the conveying assembly is connected to the first temperature detector and the second temperature detector, respectively, and the conveying assembly is moved so that the first temperature detector is disposed inside the temperature measurement channel; or (b)
The conveying assembly is moved so that the second temperature detector is arranged inside the temperature measuring channel.
10. The heat treatment apparatus according to claim 1, wherein the temperature measuring channel is made of any one of graphite, zirconia, alumina, corundum and yttria.
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| CN202223229413.6U CN219058558U (en) | 2022-12-02 | 2022-12-02 | Heat treatment equipment |
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| CN202223229413.6U CN219058558U (en) | 2022-12-02 | 2022-12-02 | Heat treatment equipment |
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