Carbon nanoelectrode production equipment, preparation method and annealing process

Abstract

The application discloses a carbon nano electrode production equipment, a preparation method and an annealing process. The production equipment comprises a heating cabin, a carbon heater is fixed in the center of the shell of the heating cabin, a protective gas inlet is arranged on the back plate of the shell, a water-cooling heat exchanger is arranged on the side of the shell, the protective gas inlet is connected with a protective gas source, a protective gas valve is arranged correspondingly, a lifting unit comprises a linear sliding table and a connecting rod arranged on the action end of the linear sliding table, a probe fixing clamp is arranged on the connecting rod, the probe fixing clamp holds a probe, the probe moves towards or away from the heating cabin along the length direction of the probe, a jack is arranged on the shell and corresponds to the probe, the end of the probe is connected with a carbon source or a vacuum pump, and a carbon source control valve is arranged on the hose corresponding to the carbon source, a control unit comprises a control circuit board and a switching power supply for providing electric energy, and the control action component moves according to preset parameters. The production equipment has the advantages of high automation and program control degree, good reproducibility, high safety and simple operation.

Description

Technical Field

[0001] This application relates to the field of micro-nano fabrication technology, and in particular to a carbon nanotube electrode production equipment, preparation method and annealing process. Background Technology

[0002] Carbon nanoelectrodes are electrochemical probes made of carbon materials with a size in the hundreds of nanometers in at least one dimension. They have the characteristics of high mass transfer rate, high signal-to-noise ratio, wide potential window, high temperature resistance and high conductivity, and have important applications in chemistry, life sciences, materials science and other fields.

[0003] Chemical vapor deposition using a bottom-up approach is a common method for preparing carbon nanoelectrodes. For example, carbon sources are introduced into quartz nanotubes and carbon nanoelectrodes are prepared by chemical vapor deposition. Another method is to selectively deposit carbon on the inner wall of quartz nanotubes using a spatial confinement mechanism to prepare smaller carbon nanoelectrodes. However, the above methods are difficult and time-consuming to prepare carbon nanoelectrodes, which cannot meet the current scientific research needs.

[0004] To achieve controllable fabrication of carbon nanoelectrodes, various fabrication devices have been developed. Based on the heating method, they are mainly divided into heater heating and open flame heating.

[0005] A carbon nanotube electrode fabrication device using a resistance wire as a heater controls the heating temperature by regulating the current flowing through the resistance wire, thermally reducing gaseous carbon source introduced into a quartz nanotube to carbon, thereby fabricating carbon nanotube electrodes. However, the heating temperature of the resistance wire is relatively low and it cannot operate stably under high-temperature conditions. The fabricated electrodes often have irregular carbon filling, requiring techniques such as focused ion beam cutting to process the electrode tips, making it difficult to obtain small-sized carbon nanotube electrodes. Furthermore, the instrument has low automation and programmability, is cumbersome to operate, and is unsuitable for processes such as electrode annealing.

[0006] This method employs open flame heating, such as a butane flame gun, to thermally decompose a gaseous carbon source introduced into a quartz micro / nano probe, causing carbon atoms to deposit on the inner wall of the probe and form a carbon electrode with a regular pointed morphology. However, this method requires open flame heating, which is not suitable for the operating environment of a typical laboratory; furthermore, the equipment has a low degree of automation and programmability, and requires advanced operating skills.

[0007] Therefore, in view of the above-mentioned technical problems, how to provide a safe, efficient, easy-to-operate, highly automated and programmable carbon nanoelectrode preparation and annealing equipment is a technical problem that needs to be solved by those skilled in the art. Summary of the Invention

[0008] The purpose of this application is to provide a carbon nanoelectrode production equipment, preparation method and annealing process, which has the advantages of high degree of automation and programmability, good reproducibility, high safety and simple operation, greatly reducing the operation difficulty of carbon nanoelectrode preparation, and has nanoelectrode ultrafast annealing technology to significantly extend the service life of the electrode.

[0009] To achieve the above objectives, this application provides an automated and programmable production equipment for carbon nanotube electrodes, comprising:

[0010] The heating chamber includes an outer shell and a quartz window disposed on the outer shell and forming a closed chamber with the outer shell. A carbon heater is fixed in the center of the closed chamber. A protective gas inlet is opened on the back plate of the outer shell. A water-cooled heat exchanger is disposed around the outer shell. The water-cooled heat exchanger is externally connected to a circulating water pump. The protective gas inlet is externally connected to a protective gas source through a hose, and a protective gas valve is provided on the hose.

[0011] The lifting unit includes a linear slide and a connecting rod located at the moving end of the linear slide. The connecting rod is provided with a probe fixing clamp, which holds the probe by clamping the nut. The probe moves toward or away from the heating chamber along its length. The outer shell is provided with an insertion hole corresponding to the probe, so that the tip of the probe can enter and exit the sealed chamber. The end of the probe is connected to a carbon source or a vacuum pump through a hose, and a carbon source control valve is provided on the hose corresponding to the carbon source.

[0012] The control unit includes a control circuit board and a switching power supply that provides power. The control circuit board is electrically connected to the power components of the circulating water pump, the protective gas valve, the vacuum pump, and the linear slide, respectively, to control the four components to operate according to preset parameters.

[0013] Preferably, it also includes a chassis structure, the chassis structure including a base plate and a main body disposed on the base plate, the lifting unit and the control unit being located inside the chassis structure, and the heating chamber being located outside the main body.

[0014] Preferably, the lifting unit further includes a first fixing plate and a second fixing plate disposed on the base plate, the linear slide is disposed on the first fixing plate, the back plate of the outer shell is fixed on the side of the second fixing plate away from the first fixing plate, and a through hole is provided on the main body corresponding to the position of the outer shell and exposing the outer shell. The second fixing plate and the main body are provided with corresponding strip holes, and the connecting rod passes through the strip holes to keep the probe and the insertion hole position aligned. The length direction of the strip holes is consistent with the movement direction of the probe.

[0015] Preferably, the water-cooled heat exchanger includes heating chamber heat exchangers disposed on both sides and / or the top of the outer shell and electrode heat exchangers disposed on the back plate of the outer shell, and the protective gas inlet is disposed on the back plate of the outer shell.

[0016] Preferably, the vacuum pump and the protective gas valve are mounted on the base plate and located inside the main body, the carbon source control valve is connected to the rotor flow meter via a hose, the rotor flow meter is connected to the protective gas source to monitor the flow rate of the protective gas, and the carbon source control valve and the rotor flow meter are mounted on the base plate and located outside the main body.

[0017] Preferably, the main body is provided with function buttons and a human-machine interface. The function buttons include a start button, a stop button, and an emergency stop button. Both the function buttons and the human-machine interface are connected to the control circuit board via signals.

[0018] Preferably, the main body is provided with a light-proof shield covering the outer periphery of the heating chamber. The light-proof shield is detachably connected to the main body. The main body is also provided with heat dissipation holes and a drying chamber. Protective gas enters the heating chamber after passing through the drying chamber.

[0019] A preparation method, implemented using the automated and programmable production equipment for carbon nanoelectrodes described above, the preparation method comprising:

[0020] Start the equipment, turn on the switching power supply to power the control circuit board, the control circuit board controls the probe fixing clip to reset, and controls the start of the circulating water pump;

[0021] Set up the protective gas and carbon source, select the "electrode preparation" mode in the human-machine interface and open the protective gas valve, adjust the valve opening of the protective gas source to the preset flow rate, close the protective gas valve, and adjust the pressure reducing valve of the carbon source to the preset gas pressure.

[0022] Install the probe, adjust the opening of the carbon source control valve to purge the air from the corresponding hose of the gaseous carbon source, then seal the end of the probe on the hose and fix the probe on the probe clamp. The probe is a quartz nanotube. Adjust the carbon source control valve to the maximum opening and adjust the tip of the quartz nanotube to be in the center of the carbon heater by using a linear slide.

[0023] The preparation parameters are set, including the heating calorific value of the carbon heater, the heating time of the quartz nanotube, the heating length of the quartz nanotube, and the heat dissipation time of the quartz nanotube.

[0024] Electrode preparation: The initial position is recorded as the tip of the quartz nanotube being located in the center of the carbon heater. The protective gas valve is opened to purify the heating chamber. The carbon heater operates according to a first preset heating value. The quartz nanotube stays in the initial position for a first preset time for heating. Subsequently, the quartz nanotube rises to the apex position at a preset speed. The preset rising length is the heating length of the quartz nanotube. At the apex position, it is heated according to a second preset heating value and stays for a second preset time. After heating is completed, the carbon heater stops working. The quartz nanotube returns to the initial position or origin position after a first preset heat dissipation time.

[0025] Preferably, the electrode preparation further includes a second stage of heating. When the quartz nanotube returns to its initial position after a first preset heat dissipation time, the second stage of heating is activated. The carbon heater heats the quartz nanotube according to a third preset heating value and a third preset dwell time. Then, it rises to the top position at a preset speed, with the preset rising length being the heating length of the quartz nanotube. At the top position, it heats the quartz nanotube according to a fourth preset heating value and a fourth preset dwell time. After heating is completed, the carbon heater stops working, and the quartz nanotube exits the heating chamber and returns to its original position after a second preset heat dissipation time.

[0026] An annealing process, implemented using the aforementioned automated and programmable carbon nanotube electrode production equipment, the annealing process comprising:

[0027] Start the equipment, turn on the switching power supply to power the control circuit board, the control circuit board controls the probe fixing clip to reset, and controls the start of the circulating water pump;

[0028] Set the protective gas, select the "electrode annealing" mode in the human-machine interface and open the protective gas valve, adjust the valve opening of the protective gas source to the preset flow rate, and then close the protective gas valve.

[0029] Install the electrode to be annealed, seal the end of the probe on the hose, and fix the probe on the probe clamp. The probe is a carbon nanoelectrode. Turn on the vacuum pump to evacuate the carbon nanoelectrode, and adjust the tip of the carbon nanoelectrode to be in the center of the carbon heater by using a linear slide.

[0030] Set the annealing parameters, including the heating calorific value of the carbon heater, and the heating and cooling time of the carbon nanoelectrode.

[0031] Electrode annealing is performed, the protective gas valve is opened to purify the heating chamber, the carbon heater operates according to the fifth preset heating calorific value and preset heating time, after which the carbon heater stops working, and after the third preset heat dissipation, it exits the heating chamber and returns to the origin position.

[0032] Compared to the aforementioned background technology, this application precisely controls the spatial position of quartz nanotube / carbon nanoelectrodes using a linear slide stage. The linear slide stage is equipped with a precisely controlled servo motor or stepper motor to achieve precise carbon nanoelectrode preparation and annealing processes. Utilizing the Joule heating principle, high-quality carbon nanoelectrodes are prepared via a high-temperature thermal reduction method. The carbon heater has advantages such as a high upper limit for heating temperature and a fast heating / cooling rate. The carbon heater is used to perform high-temperature pyrolysis deposition of gaseous carbon sources within high-temperature resistant micro / nano probes such as quartz, thereby achieving the preparation and annealing of carbon nanoelectrodes. Carbon materials such as graphite have good thermal conductivity and high-temperature resistance, and can uniformly distribute Joule heat, making them suitable as high-temperature heaters. Compared to resistance wire heating, the carbon heater used in this invention can achieve higher heating temperatures. Furthermore, compared to traditional open flame heating, the heater heating method is very safe, enabling the preparation of carbon nanoelectrodes, carbon nanocone filling, and ultrafast annealing of nanoelectrodes.

[0033] Furthermore, this application improves equipment lifespan and operational stability by adjusting the circulating water pump and protective gas valve through a control unit. Under the control unit's operation, the preparation and annealing processes can be automated and programmed. The control unit can also flexibly store and recall suitable program parameters to meet the standardized requirements for carbon nanoelectrode preparation, enabling highly reproducible fabrication of carbon nanoelectrodes of different sizes and morphologies. Compared to traditional methods, this invention offers advantages such as high automation and programmability, good reproducibility, high safety, and ease of operation, significantly reducing the operational difficulty of carbon nanoelectrode preparation and lowering the operational threshold for researchers. It also incorporates ultrafast annealing technology for nanoelectrodes to substantially extend electrode lifespan. Attached Figure Description

[0034] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of this application. For those skilled in the art, other drawings can be obtained based on the provided drawings without creative effort.

[0035] Figure 1 This is a three-dimensional structural diagram of the carbon nanoelectrode production equipment provided in the embodiments of this application;

[0036] Figure 2 This is a three-dimensional structural diagram of the back of the carbon nanoelectrode production equipment provided in the embodiments of this application;

[0037] Figure 3 This is a schematic diagram of the structure of the carbon nanotube electrode production equipment after the main body has been removed, as provided in the embodiments of this application.

[0038] Figure 4This is a three-dimensional structural diagram of the lifting unit provided in the embodiments of this application;

[0039] Figure 5 This is the human-computer interaction interface for the preparation procedure in the preparation method provided in the embodiments of this application;

[0040] Figure 6 Cyclic voltammetry of carbon nanodisk electrode in the first embodiment of the preparation method provided in this application;

[0041] Figure 7 SEM (scanning electron microscope) image of the carbon nanodisk electrode in the first embodiment of the preparation method provided in this application;

[0042] Figure 8 Cyclic voltammetry of carbon nanodisc electrode in the second embodiment of the preparation method provided in this application;

[0043] Figure 9 SEM (scanning electron microscope) image of the carbon nanodisc electrode in the second embodiment of the preparation method provided in this application;

[0044] Figure 10 This is the human-computer interaction interface for the annealing procedure in the annealing process provided in the embodiments of this application;

[0045] Figure 11 The optical microscopic images of the carbon nanoelectrode after fresh preparation, tip contamination, and annealing cleaning provided in the first embodiment of the annealing process of this application are provided in the embodiments of this application.

[0046] Figure 12 Cyclic voltammetry diagrams of carbon nanoelectrodes before and after annealing in the first embodiment of the annealing process provided in this application;

[0047] Figure 13 The images provided in this application are SEM images of the Au nanoelectrode before and after annealing in a second embodiment of the annealing process.

[0048] In the diagram: 1-Heating chamber; 11-Outer shell; 12-Carbon heater; 13-Clamp; 14-Heating chamber heat exchanger; 15-Protective gas inlet; 16-Electrode heat exchanger; 17-Temperature sensor;

[0049] 2-Lifting unit; 21-Probe fixing clamp; 22-First fixing plate; 23-Linear slide; 24-Second fixing plate; 25-Connecting rod; 26-Probe; 27-Strip hole;

[0050] 3-Control unit; 31-Control circuit board; 32-Switching power supply;

[0051] 4-Chassis structure; 41-Base plate; 42-Main body; 43-Function buttons; 44-Human-machine interface; 45-Heat dissipation holes; 46-Shielded cover; 47-Drying chamber;

[0052] 5-Rotameter;

[0053] 6-Carbon source control valve;

[0054] 7-Vacuum pump;

[0055] 8-Protection valve. Detailed Implementation

[0056] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0057] It should be noted that in this embodiment, the orientation or positional relationship indicated by terms such as "upper," "lower," "front," and "rear" is based on the orientation or positional relationship shown in the accompanying drawings. It is used only for the convenience of describing this application and for simplifying the description, and does not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation of this application. Furthermore, "first," "second," "third," and "fourth" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0058] To enable those skilled in the art to better understand the present application, the present application will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0059] Explanation of relevant terms:

[0060] Carbon nanoelectrodes: Carbon nanoelectrodes are electrochemical probes made of carbon materials with a size in the hundreds of nanometers in at least one dimension. They have the characteristics of high mass transfer rate, high signal-to-noise ratio, wide potential window, high temperature resistance and high conductivity, and are widely used in electrochemical sensing, catalysis, energy storage and biomedicine.

[0061] Stepper motor: A stepper motor is an electric motor that converts electrical pulse signals into discrete mechanical motion. Its working principle is based on electromagnetic principles; it generates rotational or linear motion by controlling the energizing sequence of coils, achieving precise control and is widely used in mechanical systems requiring precise positioning.

[0062] Joule heating principle: The heating principle of Joule heating is the phenomenon that when an electric current passes through a conductor, the conductor converts electrical energy into heat energy due to its resistance, thereby increasing the temperature of the conductor. This process follows Joule's law, which states that the heat generated is directly proportional to the square of the current, the resistance, and the time it takes for the current to pass through the conductor.

[0063] High-temperature thermal reduction: High-temperature thermal reduction refers to the process of thermally decomposing a compound into its elemental form under high-temperature conditions. It can prepare high-purity carbon materials without the need for complex chemical reactions, making it very suitable for the preparation of carbon nanoelectrodes.

[0064] Electrode annealing: Electrode annealing refers to heating an electrode to a certain temperature and maintaining it for a period of time, and then slowly cooling it to remove impurities or oxide layers adsorbed on the surface, reduce the surface roughness of the electrode, thereby restoring the purity of the electrode surface and improving its electrochemical performance.

[0065] In related technologies, when using resistance wire as a heater, the upper limit of the heating temperature of the resistance wire is low; it can typically only operate stably within a temperature range below 1400℃. Above this temperature, the resistance wire is prone to oxidation, melting, or breakage. In the process of preparing carbon nanoelectrodes, the resistance wire heater cannot raise the electrode surface temperature above 1200℃, making it difficult to prepare carbon nanoelectrodes of large sizes. Using open flame heating poses certain risks. Although a nanoelectrode preparation platform has been built, its automation and programmability are low, requiring manual control throughout the preparation process. Experimenters need rigorous training and extensive practice to master the electrode preparation technology. If different sizes of electrodes are required, the firing conditions need to be explored separately, resulting in a high barrier to entry. Since the firing time and position are controlled by the experimenter, there is a certain degree of deviation, and the reproducibility of electrode preparation is highly dependent on the experimenter's skill. Based on the above, this embodiment provides an automated and programmable carbon nanoelectrode production equipment with a high degree of automation and programmability, good reproducibility, high safety, and simple operation.

[0066] like Figure 1As shown, the device includes a heating chamber 1, a lifting unit 2, and a control unit 3. The heating chamber 1 includes an outer shell 11 and a quartz window disposed on the outer shell 11 and forming a closed chamber with the outer shell 11. The quartz window is usually located on the front of the heating chamber 1 and is used to see the position of the probe 26 inside the heating chamber 1 and the heating status. A carbon heater 12 is provided in the closed chamber formed by the heating chamber 1. The carbon heater 12 can be a graphite heater, a graphite ring heater, etc. Compared with the resistance wire heater, the carbon heater can reach a stable heating temperature of more than 1400°C, while the resistance wire heating temperature has a low upper limit. It can usually only work stably in the temperature range below 1400°C. Above this temperature, the resistance wire is prone to oxidation, melting, or breakage. In the process of preparing carbon nanoelectrodes, the resistance wire heater cannot make the electrode surface temperature reach more than 1200°C, making it difficult to prepare carbon nanoelectrodes in a large range. The carbon heater 12 is fixed on both sides by clamps 13; while the back plate of the outer shell 11 is provided with a protective gas inlet 15. The back plate refers to the back panel opposite to the front of the outer shell 11. The protective gas inlet 15 is connected to the protective gas source through a hose, and a protective gas valve 8 is provided on the hose for introducing protective gas into the heating chamber 1.

[0067] Please refer to Figure 3 The heating chamber 1 also includes water-cooled heat exchangers disposed around the outer shell 11. These water-cooled heat exchangers include heating chamber heat exchangers 14 disposed on both sides and / or the top of the outer shell 11, and electrode heat exchangers 16 disposed on the back plate of the outer shell 11. Both the heating chamber heat exchangers 14 and the electrode heat exchangers 16 are externally connected to circulating water pumps, which enhance heat dissipation of the heating chamber 1. A temperature sensor 17 is also provided on the back plate of the outer shell 11 to monitor the heating temperature of the heating chamber 1 or the carbon heater 12.

[0068] Please refer to Figure 4 The lifting unit 2 includes a linear slide 23 and a connecting rod 25 located at the moving end of the linear slide 23. The linear slide 23 has a high-precision power component, such as a stepper motor or a servo motor, which can drive the moving end of the linear slide 23 to move precisely. The moving end can then drive the connecting rod 25 to move. The connecting rod 25 is equipped with a probe fixing clamp 21, which in turn drives the probe fixing clamp 21 to move precisely. The probe fixing clamp 21 holds the probe 26 by clamping the nut. The probe 26 moves along its length toward or away from the heating chamber 1. The outer shell 11 is provided with a corresponding insertion hole for the probe 26, so that the tip of the probe 26 can enter and exit the sealed chamber. Generally, the probe is located below the outer shell 11. When the probe 26 moves upward, it can smoothly enter the heating chamber 1 through the insertion hole.

[0069] A carbon source or vacuum pump 7 is connected to the end of probe 26 via a flexible tube. A carbon source control valve 6 is provided on the flexible tube corresponding to the carbon source. When probe 26 is sealed and connected to the carbon source, it corresponds to the preparation process of carbon nanoelectrode; when connected to vacuum pump 7, it corresponds to the annealing process of carbon nanoelectrode. It should be noted that the aforementioned flexible tube can be a silicone tube or a peristaltic pump tube; no further restrictions are imposed here, and both fall within the protection scope of this application.

[0070] Please refer to Figure 3 The control unit 3 includes a control circuit board 31 and a switching power supply 32 that provides power to it. The control circuit board 31 is electrically connected to the power components of the circulating water pump, the protective air valve 8, the vacuum pump 7, and the linear slide 23, as well as the temperature sensor 17. By setting the control parameters of the control circuit board 31, the power components of the circulating water pump, the protective air valve 8, the vacuum pump 7, and the linear slide 23 operate according to preset parameters. The temperature sensor 17 transmits temperature information to the control circuit board 31 and displays the reading through the human-machine interface 44. That is, the human-machine interface 44 is also connected to the control circuit board 31. The human-machine interface 44 can also be equipped with control buttons for controlling components such as the circulating water pump, the protective air valve 8, the vacuum pump 7, and the linear slide 23, so that the parameters of the above components can be adjusted and controlled through human-machine interaction.

[0071] The carbon nanotube electrode production equipment of this application also includes a chassis structure 4, please refer to... Figures 1 to 3 The chassis structure 4 includes a base plate 41 and a main body 42 mounted on the base plate 41. The lifting unit 2 and the control unit are located inside the chassis structure 4, and the heating chamber 1 is located outside the main body 42. Specifically, the heating chamber 1 is located at the left front or right front of the main body 42. An instrument switch can be installed on the main body 42 to control the switching power supply 32 to supply power to the control circuit board 31, thereby enabling the equipment to be turned on and off.

[0072] Further, please refer to Figure 4 The lifting unit 2 also includes a first fixed plate 22 and a second fixed plate 24 disposed on the base plate 41. A linear slide 23 is disposed on the first fixed plate 22. The moving end of the linear slide 23 moves vertically, and the probe 26 is also vertically disposed to drive the probe 26 to move. The back plate of the outer casing 11 is fixed to the side of the second fixed plate 24 away from the first fixed plate 22, and a through hole corresponding to the position of the outer casing 11 and exposing the outer casing 11 is provided on the main body 42. The second fixed plate 24 and the main body 42 are provided with corresponding strip holes 27. The connecting rod 25 passes through the strip hole 27 to keep the probe 26 and the insertion hole in the same position. The length direction of the strip hole 27 is consistent with the movement direction of the probe 26, so as to facilitate the smooth movement of the probe 26 and its insertion into the insertion hole.

[0073] Secondly, the vacuum pump 7 and the protective gas valve 8 can be mounted on the base plate 41 and located inside the main body 42. The vacuum pump 7 is used to evacuate the carbon nanotube electrode during electrode annealing. The carbon source control valve 6 is connected to the rotor flow meter 5 via a hose. The rotor flow meter 5 is connected to the protective gas source to monitor and control the flow rate of the protective gas entering the heating chamber 1. The carbon source control valve 6 and the rotor flow meter 5 are mounted on the base plate 41 and located outside the main body 42, which facilitates manual adjustment of the carbon source flow rate and easy observation of the flow meter reading. The carbon source control valve 6 is mainly used to control the flow rate of the carbon source, which is usually liquefied petroleum gas, including at least one or more of propane, butane, propylene, and butene.

[0074] The above indicates that a human-machine interface 44 is provided on the main body 42, and multiple function buttons 43 can also be provided on the main body 42, such as start button, stop button, emergency stop button, etc. The function buttons 43 can be located on the front of the main body 42 for easy pressing by personnel. The function buttons 43 can be connected to the control circuit board 31 for signal connection, so that the corresponding function can be started or stopped by personnel pressing it. As for other specific settings of the function buttons 43, no further restrictions are made here, and they all fall within the protection scope of this application.

[0075] It should be noted that the aforementioned carbon source control valve 6, protective gas valve 8, and other valve components can be solenoid valves, so that the control circuit board 31 can control them; of course, the carbon source control valve can also be a manual ball valve or other valve components, which can be selected according to the actual situation.

[0076] In addition, a light shield 46 is provided on the main body 42 to cover the outer perimeter of the heating chamber 1. The light shield 46 is detachably connected to the main body 42. When the carbon heater 12 starts to work, the light shield 46 is covered to reduce the damage to the eyes caused by the strong light emitted by the heater. After heating is completed or during the initial heating process, the light shield 46 can be removed to observe the internal condition of the heating chamber 1.

[0077] The main body 42 is also equipped with heat dissipation holes 45 and a drying chamber 47. The heat dissipation holes 45 can be located on the left and right sides of the main body 42 to improve the overall heat dissipation capacity of the main body 42 and ensure that the equipment is in a safe working environment. The drying chamber 47 is connected to the protective gas inlet 15 and the protective gas source via a hose. Please refer to [reference needed]. Figure 2 The protective gas passes through the drying chamber 47 and then enters the heating chamber 1.

[0078] In summary, this application precisely controls the spatial position of quartz nanotube / carbon nanoelectrodes using a linear slide 23. The linear slide 23 is equipped with a precisely controlled servo motor or stepper motor to achieve precise carbon nanoelectrode preparation and annealing processes. High-quality carbon nanoelectrodes are prepared using a high-temperature thermal reduction method based on the Joule heating principle. The carbon heater has advantages such as a high upper limit of heating temperature and a fast heating and cooling rate. The carbon heater 12 is used to perform high-temperature pyrolysis deposition of gaseous carbon sources within high-temperature resistant micro / nano probes such as quartz, thereby achieving the preparation and annealing of carbon nanoelectrodes. Carbon materials such as graphite have good thermal conductivity and high-temperature resistance, and can uniformly distribute Joule heat, making them suitable as high-temperature heaters. Compared with resistance wire heating, the carbon heater 12 used in this invention can achieve higher heating temperatures. Compared with traditional open flame heating, the method of heating with a heater is very safe, enabling the preparation of carbon nanoelectrodes, carbon nanocone filling, and ultrafast annealing of nanoelectrodes.

[0079] This application improves equipment lifespan and operational stability by regulating the circulating water pump and protective gas valve 8 through the control unit 3. Under the control unit 3, the preparation and annealing processes can be automated and programmed. Furthermore, the control unit 3 can flexibly store and recall suitable program parameters to meet the standardized requirements for carbon nanoelectrode preparation, making it possible to manufacture carbon nanoelectrodes of different sizes and morphologies with high reproducibility. Compared with traditional solutions, this invention has the advantages of high automation and programmability, good reproducibility, high safety, and simple operation, greatly reducing the operational difficulty of carbon nanoelectrode preparation, lowering the operational threshold for experimental personnel, and possessing ultrafast annealing technology for nanoelectrodes to significantly extend the electrode's lifespan.

[0080] This embodiment also provides a preparation method, namely, a preparation method implemented using the above-mentioned automated and programmable carbon nanoelectrode production equipment, the preparation method comprising:

[0081] S1. Start the equipment and turn on the instrument switch so that the switching power supply 32 supplies power to the control circuit board 31. The control circuit board 31 controls the probe fixing clip 21 to reset and controls the start of the circulating water pump.

[0082] S2. Set the protective gas and carbon source. In the human-machine interface 44, select the "electrode preparation" mode and open the protective gas valve 8. Please refer to... Figure 5 After adjusting the pressure reducing valve of the protective gas source to the preset flow rate, close the protective gas valve 8 and adjust the pressure reducing valve of the carbon source to the preset gas pressure.

[0083] S3. Install probe 26, adjust the opening of carbon source control valve 6 to purge the air from the corresponding hose by the gaseous carbon source, then seal the end of probe 26 on the hose and fix probe 26 on probe fixing clamp 21. At this time, probe 26 is a quartz nanotube. The quartz nanotube is hollow. The end of the quartz nanotube is inserted into the hose (the hose is connected to the gaseous carbon source). The gaseous carbon source can then enter the quartz nanotube. Adjust carbon source control valve 6 to the maximum opening and adjust the tip of the quartz nanotube to be in the center of carbon heater 12 by linear slide table 23.

[0084] S4. Set the preparation parameters, including the heating calorific value of the carbon heater 12, the heating time of the quartz nanotube, the heating length of the quartz nanotube, and the heat dissipation time of the quartz nanotube.

[0085] S5. Electrode preparation: Record the initial position of the quartz nanotube tip located in the center of the carbon heater 12. Open the protective gas valve 8 to purify the heating chamber 1. The carbon heater 12 operates according to the first preset heating value. The quartz nanotube stays in the initial position for a first preset time for heating. Then, the quartz nanotube rises to the top position at a preset speed. The preset rising length is the heating length of the quartz nanotube. At the top position, it is heated according to the second preset heating value and stays for a second preset time. After heating is completed, the carbon heater 12 stops working. The quartz nanotube returns to the initial position or origin position after the first preset heat dissipation time.

[0086] In step S5, electrode preparation also includes a second stage of heating. Of course, only the first stage of heating described above can be used. The first stage is a high-calorific-value rapid heating to form a thin layer of carbon on the inner wall of the quartz nanotube. Since the temperature required to grow carbon on carbon is lower than that required to grow carbon on quartz, the second stage is a low-calorific-value slow heating to fill the interior of the quartz nanotube with carbon at the tip to form a carbon nanodisc electrode. Here, one or two stages of heating can be selected according to the actual situation. The second stage of heating is started when the quartz nanotube returns to the initial position after the first preset heat dissipation time. The carbon heater 12 heats according to the third preset heating calorific value and stays for the third preset time. Then, it rises to the top position at a preset speed. The preset rising length is the heating length of the quartz nanotube. At the top position, it heats according to the fourth preset heating calorific value and stays for the fourth preset time. After the heating is completed, the carbon heater 12 stops working, and the quartz nanotube exits the heating chamber 1 and returns to the original position after the second preset heat dissipation time.

[0087] Generally speaking, in existing related technologies, the first and second preset heating calorific values ​​are the same in the first stage of heating, and the third and fourth preset heating calorific values ​​are the same in the second stage of heating. However, with the advancement of technology and the improvement of the preparation process, there may be situations where the first and second preset heating calorific values ​​are different, or the third and fourth preset heating calorific values ​​are different. These situations all fall within the protection scope of this application.

[0088] In step S5, the origin position is defined as the position of the tip of the quartz nanotube when it is fixed on the probe clamp 21. The vertex position is the highest point where the fixed quartz nanotube can rise in the heating chamber 1 under the control of the linear slide 23, or the highest point where the tip of the quartz nanotube rises according to the actual required heating length. Furthermore, the purpose of moving the quartz nanotube from the initial position to the vertex position in step S5 is to deposit carbon not only at the tip but also at a distance below the tip. This is because in subsequent experiments, the carbon nanoelectrode needs to connect the carbon to the electrode clamp via a metal wire. The portion of carbon deposited at the vertex position is used to contact the metal wire in subsequent experiments, increasing the contact length between the metal wire and the carbon and preventing accidental damage to the carbon nanoelectrode during the experiment.

[0089] In the first embodiment of the preparation method, a method for preparing a carbon nanodisk electrode with a diameter of 200 nm is provided, utilizing a carbon nanoelectrode production device, specifically including the following steps:

[0090] The first step is to use a P-2000 laser drawing machine to draw quartz capillaries (inner / outer diameter: 0.7 / 1.0mm) into quartz nanotubes with a tip diameter of about 200nm.

[0091] Step 2: Turn on the power to the device to reset the probe clamp 21, and at the same time the circulating water pump will start automatically.

[0092] Step 3: Select the "Electrode Preparation" mode, click "Protective Gas Valve" to turn on the protective gas, adjust the pressure divider valve of the protective gas source to 0.2 MPa, and adjust the flow rate of the rotor flowmeter to 1 L / min. -1 Close the protective gas valve 8, open the carbon source main valve and adjust the pressure reducing valve to 0.28MPa;

[0093] Step 4: Open part of the carbon source control valve 6 to purge the air from the corresponding hose. Then connect the end of the quartz nanotube to the hose (seal the interface with sealing film) and fix it on the probe clamp 21. Then adjust the carbon source control valve 6 to the maximum flow rate.

[0094] Step 5: Precisely adjust the position of the quartz nanotube tip using the linear slide 23 so that it is located in the center of the heater; this is the initial position.

[0095] Step 6: Set the calorific value, residence time I, rising speed, residence time II, and heat dissipation time for the two-stage heating process. The parameters for the first stage heating are: calorific value 320, residence time I 0.1s, and rising speed 5mm / s. -1 The residence time II is 0.1s, and the heat dissipation time is 5s; the parameters for the second stage heating are: calorific value 300, residence time I is 6s, and rising speed is 0.5mm / s. -1 The dwell time II is 1 second, and the heat dissipation time is 5 seconds.

[0096] Step 7: Cover the light shield 46, press the "Start" button, the protective air valve 8 will open automatically, and the cabin purification will begin;

[0097] Step 8, First Stage Heating: After the chamber purification is completed, the heater starts working with a calorific value of 320. The quartz nanotubes remain in their initial position for 0.1 seconds, and then move at a speed of 5 mm / s. -1 The speed moves upward to the peak, stays for 0.1s, then the heater stops working. After 5s of heat dissipation, the quartz nanotube returns to the initial position, and the first stage of heating ends.

[0098] Step 9, Second Stage Heating: The heater starts operating at a calorific value of 300, the quartz nanotube remains in its initial position for 6 seconds, and then moves at a speed of 0.5 mm / s. -1 The speed moves up to the peak, stays for 1 second, then the heater stops working. After 5 seconds of heat dissipation, the electrode returns to the origin, the protective gas valve 8 closes automatically, the second stage of heating ends, and finally the carbon source control valve 6 is manually closed to complete the preparation process.

[0099] Step 10: The experimenter, wearing electrostatic protection, removes the prepared carbon nanodisc electrode and places it in a solution containing 1 mmol L... -1 Ferrocene methanol (FcMeOH) and 1 mol L -1 In an aqueous solution of KCl, a two-electrode system was used, with a carbon nanodisc electrode as the working electrode, and Ag / AgCl (3 mol L) -1 KCl was used as the reference and counter electrode. Cyclic voltammetry tests were performed using an electrochemical workstation in a super-shielded chamber. Please refer to [link / reference] for details. Figure 6 According to the formula a = i / 4.64nFDc, where n is the number of electrons transferred by FcMeOH oxidation (n=1), a is the radius of the carbon nanodisk electrode, i is the limiting diffusion current of the carbon nanodisk electrode, and F is the Faraday constant (F=96485C mol). -1 D is the diffusion coefficient of FcMeOH in aqueous solution (D = 7.6 × 10⁻⁶). -6cm 2 s -1 c is the molar concentration of FcMeOH (c = 1 × 10⁻⁶). –3 mol L -1 The calculated diameter of the prepared carbon nanodisc electrode was 215 nm, which is consistent with... Figure 7 The results shown in the SEM images are consistent.

[0100] In a second embodiment of the preparation method, a method for preparing a carbon nanodisk electrode with a diameter of 600 nm is provided, utilizing a carbon nanoelectrode production device, specifically including the following steps:

[0101] The first step is to use a P-2000 laser drawing machine to draw quartz capillaries (inner / outer diameter: 0.7 / 1.0mm) into quartz nanotubes with a tip diameter of about 600nm.

[0102] Step 2: Turn on the power to the device to reset the probe clamp 21, and at the same time the circulating water pump will start automatically.

[0103] Step 3: Select the "Electrode Preparation" mode, click "Protective Gas Valve" to turn on the protective gas, adjust the pressure divider valve of the protective gas source to 0.2 MPa, and adjust the flow rate of the rotor flowmeter to 1 L / min. -1 Close the protective gas valve 8, open the carbon source main valve and adjust the pressure reducing valve to 0.26MPa;

[0104] Step 4: Open part of the carbon source control valve 6 to purge the air from the corresponding hose. Then connect the end of the quartz nanotube to the hose (seal the interface with a sealing film) and fix it on the probe clamp 21. Then adjust the carbon source control valve 6 to the maximum flow rate.

[0105] Step 5: Precisely adjust the position of the quartz nanotube tip using the linear slide 23 so that it is located in the center of the heater; this is the initial position.

[0106] Step 6: Set the calorific value, residence time I, rising speed, residence time II, and heat dissipation time for the two-stage heating process. The parameters for the first stage heating are: calorific value 320, residence time I 0.3s, and rising speed 5mm / s. -1 The residence time II is 0.1s, and the heat dissipation time is 8s; the parameters for the second stage heating are: calorific value 300, residence time I is 10s, and rising speed is 0.5mm / s. -1 The dwell time II is 1 second, and the heat dissipation time is 8 seconds;

[0107] Step 7: Cover the light shield 46, press the "Start" button, the protective air valve 8 will open automatically, and the cabin purification will begin;

[0108] Step 8, First Stage Heating: After the chamber purification is completed, the heater starts working with a calorific value of 320. The quartz nanotubes remain in their initial position for 0.3 seconds, and then move at a speed of 5 mm / s. -1 The speed moves upward to the peak, stays for 0.1s, then the heater stops working. After 8s of heat dissipation, the quartz nanotube returns to the initial position, and the first stage of heating ends.

[0109] Step 9, Second Stage Heating: The heater starts operating at a calorific value of 300, and the quartz nanotube remains in its initial position for 10 seconds, then moves at a speed of 0.5 mm / s. -1 The speed moves up to the peak, stays for 1 second, then the heater stops working. After 8 seconds of heat dissipation, the electrode returns to the origin, the protective gas valve 8 closes automatically, the second stage of heating ends, and finally the carbon source control valve 6 is manually closed to complete the preparation process.

[0110] Step 10: The experimenter, wearing electrostatic protection, removes the prepared carbon nanodisc electrode and places it in a solution containing 1 mmol L... -1 Ferrocene methanol (FcMeOH) and 1 mol L -1 In an aqueous solution of KCl, a two-electrode system was used, with a carbon nanodisc electrode as the working electrode, and Ag / AgCl (3 mol L) -1 KCl was used as the reference and counter electrode. Cyclic voltammetry tests were performed using an electrochemical workstation in a super-shielded chamber. Please refer to [link / reference] for details. Figure 8 According to the formula a = i / 4.64nFDc, where n is the number of electrons transferred by FcMeOH oxidation (n=1), a is the radius of the carbon nanodisk electrode, i is the limiting diffusion current of the carbon nanodisk electrode, and F is the Faraday constant (F=96485C mol). -1 D is the diffusion coefficient of FcMeOH in aqueous solution (D = 7.6 × 10⁻⁶). -6 cm 2 s -1 c is the molar concentration of FcMeOH (c = 1 × 10⁻⁶). –3 mol L -1 The calculated diameter of the prepared carbon nanodisc electrode was 624 nm, which is consistent with... Figure 9 The results shown in the SEM images are consistent.

[0111] In the embodiments of the two preparation methods described above, the rising speed is the speed at which the quartz nanotube moves from the initial position to the apex; the dwell time I is the time the quartz nanotube stays in the center of the heater when the heater is working; the dwell time II is the time the quartz nanotube stays at the apex when the heater is working; and the heat dissipation time is the time the quartz nanotube stays at the apex after the heater stops working.

[0112] This embodiment also provides an annealing process, namely an annealing process implemented using the above-mentioned automated and programmable production equipment for carbon nanotube electrodes, the annealing process including:

[0113] S1. Start the equipment and turn on the instrument switch so that the switching power supply 32 supplies power to the control circuit board 31. The control circuit board 31 controls the probe fixing clip 21 to reset and controls the start of the circulating water pump.

[0114] S2. Set the protective gas. In the human-machine interface 44, select the "Electrode Annealing" mode and click the "Protective Gas Valve" to turn on the protective gas. Please refer to... Figure 10 After adjusting the pressure reducing valve of the protective gas source to the preset flow rate, close the protective gas valve 8.

[0115] S3. Install the electrode to be annealed. Seal the end of the carbon nanotube electrode on the flexible tube and fix the carbon nanotube electrode on the probe clamp 21. Turn on the vacuum pump 7 to evacuate the carbon nanotube electrode. That is, the tip of the carbon nanotube electrode is solid, but only the tip is filled with carbon, while the end is still a hollow quartz tube. Evacuation is to remove the air in this part to prevent the carbon nanotube electrode from being oxidized by the air during the annealing process. Adjust the tip of the carbon nanotube electrode to be in the center of the carbon heater 12 by using the linear slide 23. This is the initial position of the carbon nanotube electrode.

[0116] S4. Set the annealing parameters, including the heating calorific value of the carbon heater 12, and the heating and cooling time of the carbon nanoelectrode.

[0117] S5. Electrode annealing, open the protective gas valve 8 to purify the heating chamber 1, the carbon heater 12 works according to the fifth preset heating heat value and preset heating time, after completion the carbon heater 12 stops working, and after the third preset heat dissipation, it exits the heating chamber 1 and returns to the original position.

[0118] In the annealing process described above, the origin position is defined as the position of the tip of the carbon nanoelectrode when it is fixed on the probe clamp 21.

[0119] In a first embodiment of the annealing process, a method for cleaning carbon nanodisc electrodes using an annealing process is provided, utilizing carbon nanodisc electrode production equipment, specifically including the following steps:

[0120] Step 1: Prepare carbon nanodisc electrodes using the above method. Observe the newly prepared carbon nanodisc electrodes under a microscope. The electrode surface is clean and free of dust. Please refer to... Figure 11 At 1 mmol L -1 Ferrocene methanol (FcMeOH) and 1 mol L -1 In a KCl electrolyte solution, a two-electrode system was used, with a carbon nanodisc electrode as the working electrode, and the Ag / AgCl ratio was 3 mol / L.-1 Using KCl as the reference and counter electrodes, the cyclic voltammetric characteristics of the newly prepared carbon nanodisc electrode were tested. Please refer to [reference needed]. Figure 12 The carbon nanodisk electrode with a diameter of 210 nm was obtained.

[0121] The second step involves exposing the newly prepared carbon nanodisc electrode to air. After a period of time, dust contamination was observed at the electrode tip under an optical microscope. Please refer to [reference needed]. Figure 11 ;

[0122] Third, turn on the power to the equipment to reset the probe fixing clip 21, and at the same time the circulating water pump will start automatically.

[0123] Step 4: Select the "Electrode Annealing" mode, click the "Protective Gas Valve" to turn on the protective gas, adjust the pressure divider valve of the protective gas source to 0.2 MPa, and adjust the flow rate of the rotor flowmeter to 1 L / min. -1 Close the protective gas valve 8;

[0124] Step 5: Connect the electrode tip to the flexible tube (seal the interface with sealing film) and fix it on the probe clamp 21. Click "vacuum pump" to start evacuating the vacuum. Use the linear slide 23 to precisely adjust the position of the electrode tip so that it is in the center of the heater.

[0125] Step 6: Set the parameters: heater heat value is 250, heating time is 3 seconds, and heat dissipation time is 5 seconds.

[0126] Step 7: Cover the light shield 46, press the "Start" button, the protective air valve 8 will open automatically, after the cabin is purified, the heater will work at a calorific value of 250 for 3 seconds, and then the heater will stop working.

[0127] Step 8: After the electrode stays in the heating chamber 1 for 5 seconds, it returns to its original position. Then the protective gas valve 8 and vacuum pump 7 automatically close, completing the annealing process.

[0128] Step 9: The experimenter, wearing electrostatic protection, removes the annealed electrodes and observes them under an optical microscope. The electrode tips are found to be clean and free of dust. Please refer to... Figure 11 At 1 mmol L -1 Ferrocene methanol (FcMeOH) and 1 mol / L -1 To test the cyclic voltammetric characteristics of the annealed carbon nanodisc electrode in a KCl electrolyte solution, please refer to [reference needed]. Figure 12 Compared with the newly prepared carbon nanoelectrode, the cyclic voltammetry curves of the annealed electrode are basically the same, indicating that the annealing successfully cleaned the surface of the carbon nanoelectrode without affecting the morphology and electrochemical performance of the electrode itself.

[0129] In a second embodiment of the annealing process, a method for reducing the surface roughness of Au nanoelectrodes using an annealing process is provided, specifically including the following steps:

[0130] Step 1: Prepare carbon nanodisc electrodes using the above preparation method, in a solution containing 25 μmol L... -1 HAuCl4 and 0.1 mol L -1 In an aqueous solution of HCl, a two-electrode system was used, with a carbon nanodisc electrode as the working electrode, and Ag / AgCl (3 mol / L) -1 Using KCl as the reference and counter electrodes, the electrodeposition of Au nanoparticles was performed in an electrochemical workstation within a super-shielded chamber. Please refer to [reference needed]. Figure 13 SEM images show that the Au nanoparticles deposited at the electrode tip are about 750 nm in diameter and have a large number of grains on their surface, which need to be reduced by annealing.

[0131] Step 2: Turn on the power to the device to reset the probe clamp 21, and at the same time the circulating water pump will start automatically.

[0132] Step 3: Select the "Electrode Annealing" mode, click the "Protective Gas Valve" to turn on the protective gas, adjust the pressure divider valve of the protective gas source to 0.2MPa, and adjust the flow rate of the rotor flowmeter to 1L / min. -1 Close the protective gas valve 8.

[0133] Step 4: Connect the electrode tip to the flexible tube (seal the interface with sealing film) and fix it on the probe clamp 21. Click "vacuum pump" to start evacuating the vacuum. Use the linear slide 23 to precisely adjust the position of the electrode tip so that it is in the center of the heater.

[0134] Step 5: Set the parameters: heater heat value is 275, heating time is 2s, and heat dissipation time is 5s.

[0135] Step 6: Cover with the light shield 46, press the "Start" button, the protective gas valve 8 will open automatically, and after the cabin purification is completed, the heater will operate at a calorific value of 275 for 2 seconds, after which the heater will stop working;

[0136] Step 7: After the electrode stays in the heating chamber 1 for 5 seconds, it returns to its original position. Then the protective gas valve 8 and vacuum pump 7 automatically close, completing the annealing process.

[0137] Step 8: Perform SEM characterization on the annealed Au nanoelectrode. Please refer to [reference needed]. Figure 13 SEM images show that the Au nanoparticles at the electrode tip after annealing have a diameter of approximately 650 nm, and the surface grains are reduced, indicating that annealing reduces the surface roughness of the Au nanoparticles.

[0138] It should be noted that in this specification, relational terms such as first and second are used only to distinguish one entity from several other entities, and do not necessarily require or imply any such actual relationship or order between these entities.

[0139] This document uses specific examples to illustrate the principles and implementation methods of this application. The descriptions of the embodiments above are only for the purpose of helping to understand the method and core ideas of this application. It should be noted that those skilled in the art can make several improvements and modifications to this application without departing from the principles of this application, and these improvements and modifications also fall within the protection scope of the claims of this application.

Claims

1. An automated and programmable production equipment for carbon nanotube electrodes, characterized in that, include: The heating chamber (1) includes an outer shell (11) and a quartz window disposed on the outer shell (11) and forming a closed chamber with the outer shell (11). A carbon heater (12) is fixedly disposed in the center of the closed chamber. A protective gas inlet (15) is provided on the back plate of the outer shell (11). A water-cooled heat exchanger is provided around the outer shell (11). The water-cooled heat exchanger is connected to a circulating water pump. The protective gas inlet (15) is connected to a protective gas source through a hose, and a protective gas valve (8) is provided on the hose. The lifting unit (2) includes a linear slide (23) and a connecting rod (25) located at the moving end of the linear slide (23). The connecting rod (25) is provided with a probe fixing clip (21). The probe fixing clip (21) holds the probe (26) by clamping the nut. The probe (26) moves toward or away from the heating chamber (1) along its length. The outer shell (11) is provided with an insertion hole corresponding to the probe (26) so that the tip of the probe (26) can enter and exit the closed chamber. The end of the probe (26) is connected to a carbon source or a vacuum pump (7) through a hose, and a carbon source control valve (6) is provided on the hose corresponding to the carbon source. The control unit (3) includes a control circuit board (31) and a switching power supply (32) that provides power. The control circuit board (31) is electrically connected to the power components of the circulating water pump, the protective gas valve (8), the vacuum pump (7), and the linear slide (23) to control the four components to operate according to preset parameters.

2. The automated and programmable production equipment for carbon nanotube electrodes according to claim 1, characterized in that, It also includes a chassis structure (4), which includes a base plate (41) and a main body (42) disposed on the base plate (41). The lifting unit (2) and the control unit (3) are located inside the chassis structure (4), and the heating chamber (1) is located outside the main body (42).

3. The automated and programmable production equipment for carbon nanotube electrodes according to claim 2, characterized in that, The lifting unit (2) further includes a first fixing plate (22) and a second fixing plate (24) disposed on the base plate (41). The linear slide (23) is disposed on the first fixing plate (22). The back plate of the outer shell (11) is fixed on the side of the second fixing plate (24) away from the first fixing plate (22). A through hole corresponding to the position of the outer shell (11) and exposing the outer shell (11) is provided on the main body (42). The second fixing plate (24) and the main body (42) are provided with corresponding strip holes (27). The connecting rod (25) passes through the strip hole (27) to keep the probe (26) and the insertion hole in the same position. The length direction of the strip hole (27) is consistent with the movement direction of the probe (26).

4. The automated and programmable production equipment for carbon nanotube electrodes according to claim 1, characterized in that, The water-cooled heat exchanger includes a heating chamber heat exchanger (14) disposed on both sides and / or the top of the outer shell (11) and an electrode heat exchanger (16) disposed on the back plate of the outer shell (11), and the protective gas inlet (15) is disposed on the back plate of the outer shell (11).

5. The automated and programmable production equipment for carbon nanotube electrodes according to claim 2, characterized in that, The vacuum pump (7) and the protective gas valve (8) are located on the base plate (41) and inside the main body (42). The carbon source control valve (6) is connected to the rotor flow meter (5) through a hose. The rotor flow meter (5) is connected to the protective gas source to monitor the flow rate of the protective gas. The carbon source control valve (6) and the rotor flow meter (5) are located on the base plate (41) and outside the main body (42).

6. The automated and programmable production equipment for carbon nanotube electrodes according to claim 2, characterized in that, The main body (42) is provided with function buttons (43) and human-machine interface (44). The function buttons (43) include a start button, a stop button and an emergency stop button. Both the function buttons (43) and the human-machine interface (44) are connected to the control circuit board (31) via signals.

7. The automated and programmable production equipment for carbon nanotube electrodes according to claim 2, characterized in that, The main body (42) is provided with a light shield (46) covering the outer periphery of the heating chamber (1). The light shield (46) is detachably connected to the main body (42). The main body (42) is also provided with heat dissipation holes (45) and a drying chamber (47). The protective gas enters the heating chamber (1) after passing through the drying chamber (47).

8. A method for preparing a carbon nanoelectrode, characterized in that, The preparation method using the automated and programmable production equipment for carbon nanoelectrodes according to any one of claims 1-7, the preparation method comprising: Start the device and turn on the switching power supply (32) to supply power to the control circuit board (31). The control circuit board (31) controls the probe fixing clip (21) to reset and controls the start of the circulating water pump. Set up the protective gas and carbon source, select the "electrode preparation" mode in the human-machine interface (44) and open the protective gas valve (8), adjust the valve opening of the protective gas source to the preset flow rate, close the protective gas valve (8), and adjust the pressure reducing valve of the carbon source to the preset gas pressure. Install the probe (26), adjust the opening of the carbon source control valve (6) to allow the gaseous carbon source to vent the air in the corresponding hose, then seal the end of the probe (26) on the hose, and fix the probe (26) on the probe fixing clamp (21). The probe (26) is a quartz nanotube. Adjust the carbon source control valve (6) to the maximum opening, and adjust the tip of the quartz nanotube to be located in the center of the carbon heater (12) by using the linear slide (23). Set the preparation parameters, including the heating calorific value of the carbon heater (12), the heating time of the quartz nanotube, the heating length of the quartz nanotube, and the heat dissipation time of the quartz nanotube; Electrode preparation: The initial position is recorded as the tip of the quartz nanotube being located in the center of the carbon heater (12). The protective gas valve (8) is opened to purify the heating chamber (1). The carbon heater (12) operates according to the first preset heating value. The quartz nanotube stays in the initial position for a first preset time for heating. Then, the quartz nanotube rises to the top position at a preset speed. The preset rising length is the heating length of the quartz nanotube. At the top position, it is heated according to the second preset heating value and stays for a second preset time. After heating is completed, the carbon heater (12) stops working. The quartz nanotube returns to the initial position or origin position after the first preset heat dissipation time.

9. The method for preparing the carbon nanoelectrode according to claim 8, characterized in that, The electrode preparation also includes a second stage of heating. When the quartz nanotube returns to its initial position after the first preset heat dissipation time, the second stage of heating is activated. The carbon heater (12) heats according to the third preset heating calorific value and stays for the third preset time. Then it rises to the top position at a preset speed. The preset rising length is the heating length of the quartz nanotube. At the top position, it heats according to the fourth preset heating calorific value and stays for the fourth preset time. After the heating is completed, the carbon heater (12) stops working. The quartz nanotube exits the heating chamber (1) and returns to its original position after the second preset heat dissipation time.

10. An annealing process for carbon nanoelectrodes, characterized in that, The annealing process implemented using the automated and programmable production equipment for carbon nanotube electrodes according to any one of claims 1-7, the annealing process comprising: Start the device and turn on the switching power supply (32) to supply power to the control circuit board (31). The control circuit board (31) controls the probe fixing clip (21) to reset and controls the start of the circulating water pump. Set the protective gas, select the "electrode annealing" mode in the human-machine interface (44) and open the protective gas valve (8), adjust the valve opening of the protective gas source to the preset flow rate, and then close the protective gas valve (8). Install the electrode to be annealed, seal the end of the probe (26) on the hose, and fix the probe (26) on the probe fixing clamp (21). The probe (26) is a carbon nanoelectrode. Turn on the vacuum pump (7) to evacuate the carbon nanoelectrode, and adjust the tip of the carbon nanoelectrode to be in the center of the carbon heater (12) by using the linear slide (23). Set annealing parameters, set the heating calorific value of the carbon heater (12), and set the heating time and heat dissipation time of the carbon nanoelectrode; Electrode annealing, opening the protective gas valve (8) to purify the heating chamber (1), the carbon heater (12) working according to the fifth preset heating heat value and preset heating time, after completion the carbon heater (12) stops working, and after the third preset heat dissipation, exits the heating chamber (1) and returns to the value origin position.

Images