Carbon nanoelectrode production equipment, preparation method and annealing process

Abstract

The invention discloses carbon nanoelectrode 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 a shell of the heating cabin, a protective gas inlet is formed in a back plate of the shell, a water-cooling heat exchanger is arranged on the peripheral side of the shell, and the protective gas inlet is externally connected with a protective gas source and is correspondingly provided with a protective gas valve; the lifting unit comprises a linear sliding table and a connecting rod arranged at the action end of the linear sliding table, the connecting rod is provided with a probe fixing clamp, the probe fixing clamp clamps a probe, the probe moves towards or away from the heating cabin in the length direction of the probe, the shell is provided with an insertion hole corresponding to the probe, and the tail end of the probe is connected with a carbon source or a vacuum pump. A carbon source control valve is arranged on the hose corresponding to the carbon source; and the control unit comprises a control circuit board and a switching power supply for providing electric energy, and controls the action part to act according to preset parameters. The production equipment has the advantages of being high in automation and program control degree, good in reproducibility, high in safety and easy and convenient to operate.

Description

Technical Field

[0001] The present application relates to the field of micro-nano processing technology, and in particular to a carbon nanoelectrode production device, a preparation method and an annealing process. Background Art

[0002] Carbon nanoelectrodes refer to electrochemical probes made of carbon materials with a size of 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. They have important applications in chemistry, life sciences, materials science and other fields.

[0003] Chemical vapor deposition using the "bottom-up" method is a common method for preparing carbon nanoelectrodes. For example, a carbon source is introduced into a quartz nanotube to prepare a carbon nanoelectrode by chemical vapor deposition. Another example is to use a spatial confinement mechanism to selectively deposit carbon on the inner wall of a quartz nanotube to prepare a smaller carbon nanoelectrode. However, the above methods are difficult and time-consuming to prepare carbon nanoelectrodes, and can hardly meet current scientific research needs.

[0004] In order to achieve controllable preparation of carbon nanoelectrodes, people have developed a variety of carbon nanoelectrode preparation devices. According to the heating method, they are mainly divided into heater heating and open flame heating:

[0005] The carbon nanoelectrode preparation device uses a resistance wire as a heater. By controlling the current flowing through the resistance wire to adjust the heating temperature, the gaseous carbon source introduced into the quartz nanotube is thermally reduced to carbon, thereby preparing a carbon nanoelectrode. However, the heating temperature of the resistance wire is low, and it cannot work stably under high temperature conditions. The prepared electrode often has irregular carbon filling, and the electrode tip needs to be processed with the help of focused ion beam cutting and other technologies, making it difficult to obtain a small-sized carbon nanoelectrode. At the same time, the instrument has a low degree of automation and program control, and the operation is cumbersome, and it is not suitable for processes such as electrode annealing;

[0006] By using an open flame heating method such as a butane flame gun, the gaseous carbon source introduced into the quartz micro-nano probe is thermally decomposed at high temperature, so that carbon atoms are deposited on the inner wall of the quartz micro-nano probe to form a carbon electrode with a regular tip morphology. However, this solution requires the use of open flame heating, which does not meet the operating environment of ordinary laboratories; in addition, the equipment has a low degree of automation and program control, and requires high operating technology.

[0007] Therefore, in response to the above 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 technical personnel in this field need to solve. Summary of the invention

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

[0009] To achieve the above objectives, the present application provides an automated and program-controlled production device for carbon nanoelectrodes, comprising:

[0010] The heating chamber comprises a shell and a quartz window arranged on the shell and forming a closed chamber body with the shell, a carbon heater is fixedly arranged in the center of the closed chamber body, a protective gas inlet is opened on the back plate of the shell, a water-cooled heat exchanger is arranged on the peripheral side of the 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 arranged on the hose;

[0011] A lifting unit, comprising a linear slide and a connecting rod arranged at the action end of the linear slide, the connecting rod is provided with a probe fixing clamp, the probe fixing clamp holds the probe through a clamping nut, the probe moves toward or away from the heating chamber along its length direction, the housing is provided with a plug hole corresponding to the probe, so that the tip of the probe can enter and exit the closed 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 for providing electrical energy. The control circuit board is electrically connected to the power parts of the circulating water pump, the protective gas valve, the vacuum pump, and the linear slide, respectively, to control the four to act according to preset parameters.

[0013] Preferably, it further comprises a chassis structure, the chassis structure comprising a bottom plate and a main body arranged on the bottom plate, the lifting unit and the control unit are located in the chassis structure, and the heating cabin is located outside the main body.

[0014] Preferably, the lifting unit also includes a first fixed plate and a second fixed plate arranged on the base plate, the linear slide is arranged on the first fixed plate, the back plate of the shell is fixed on the side of the second fixed plate away from the first fixed plate, and a through hole corresponding to the position of the shell and exposing the shell is opened on the main body, the second fixed plate and the main body are provided with corresponding bar holes, the connecting rod passes through the bar hole to keep the probe corresponding to the position of the jack, and the length direction of the bar hole is consistent with the movement direction of the probe.

[0015] Preferably, the water-cooled heat exchanger includes a heating chamber heat exchanger arranged on both sides and / or the upper side of the shell and an electrode heat exchanger arranged on the back plate of the shell, and the protective gas inlet is arranged on the back plate of the shell.

[0016] Preferably, the vacuum pump and the protective gas valve are arranged on the bottom plate and located inside the main body, the carbon source control valve is connected to the rotor flowmeter through a hose, the rotor flowmeter is connected to the protective gas source to monitor the flow of the protective gas, and the carbon source control valve and the rotor flowmeter are arranged on the bottom plate and located outside the main body.

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

[0018] Preferably, the main body is provided with a light-proof shield covering the outer periphery of the heating chamber, and 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, and the protective gas enters the heating chamber after passing through the drying chamber.

[0019] A preparation method, which is implemented by using the above-mentioned carbon nanoelectrode automated and program-controlled production equipment, and the preparation method comprises:

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

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

[0022] Install the probe, adjust the opening of the carbon source control valve so that the gaseous carbon source evacuates the air in the corresponding hose, then seal the end of the probe on the hose, and fix the probe on the probe fixing 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 the center of the carbon heater through a linear slide;

[0023] Setting preparation parameters, setting 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, record that the tip of the quartz nanotube is located in the center of the carbon heater as the initial position, open the protective gas valve to purify the heating chamber, the carbon heater works according to the first preset heating calorific value, the quartz nanotube stays at 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 length of the rise is the heating length of the quartz nanotube, and heats at the top position according to the second preset heating calorific value and stays for a second preset time, after the heating is completed, the carbon heater stops working, and the quartz nanotube returns to the initial position or the origin position after the first preset heat dissipation time.

[0025] Preferably, the electrode preparation also includes a second stage of heating. When the quartz nanotube returns to the initial position after the first preset heat dissipation time, the second stage of heating is turned on, and the carbon heater heats according to a third preset heating calorific value and stays for a third preset time, and then rises to the top position at a preset speed. The preset length of the rise is the heating length of the quartz nanotube, and heats at the top position according to a fourth preset heating calorific value and stays for a fourth preset time. After the heating is completed, the carbon heater stops working, and the quartz nanotube exits the heating chamber after the second preset heat dissipation time and returns to the original position.

[0026] An annealing process, an annealing process implemented by the above-mentioned carbon nanoelectrode automation and program-controlled production equipment, the annealing process comprising:

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

[0028] Set the protective gas, select the "electrode annealing" mode in the human-computer interaction 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 fixing clamp, wherein the probe is a carbon nanoelectrode, start the vacuum pump to evacuate the carbon nanoelectrode, and adjust the tip of the carbon nanoelectrode to be located in the center of the carbon heater through a linear slide;

[0030] Setting annealing parameters, setting the heating calorific value of the carbon heater, the heating time and the heat dissipation time of the carbon nanoelectrode;

[0031] The electrode is annealed, the protective gas valve is opened to purify the heating chamber, and the carbon heater works according to the fifth preset heating calorific value and the preset heating time. After completion, the carbon heater stops working and exits the heating chamber after the third preset heat dissipation and returns to the value origin position.

[0032] Relative to the above background technology, the present application uses a linear slide to accurately control the spatial position of quartz nanotubes / carbon nanoelectrodes. The linear slide has a precisely controlled servo motor or stepper motor to achieve precise carbon nanoelectrode preparation and annealing processes; using the Joule heat principle, high-quality carbon nanoelectrodes are prepared by high-temperature thermal reduction method. The carbon heater has the advantages of high upper limit of heating temperature and fast heating and cooling rate. The carbon heater is used to perform high-temperature pyrolysis deposition on the gaseous carbon source in the high-temperature resistant micro-nano probe such as quartz to achieve the preparation and annealing of carbon nanoelectrodes. Carbon materials such as graphite have good thermal conductivity and high temperature resistance, can evenly distribute Joule heat, and are suitable for use as high-temperature heaters; compared with resistance wire heating, the carbon heater used in the present invention can achieve a higher heating temperature, and compared with traditional open flame heating, the method of heating with a heater is very safe, which can achieve carbon nanoelectrode preparation, carbon nanocone filling and ultra-fast annealing of nanoelectrodes.

[0033] In addition, the present application adjusts the circulating water pump and the protective air valve through the control unit to improve the service life and working stability of the equipment, and under the action of the control unit, the preparation process and annealing process can be automated and programmed, and the control unit can flexibly store and call adaptive program parameters to meet the standardized carbon nanoelectrode preparation requirements, and provide the possibility of highly reproducible manufacturing of carbon nanoelectrodes of different sizes and morphologies. Compared with the traditional solution, the present invention has the advantages of high automation and program control, good reproducibility, high safety, and simple operation, which greatly reduces the operational difficulty of carbon nanoelectrode preparation, reduces the operating threshold of experimenters, and has nanoelectrode ultrafast annealing technology to significantly extend the service life of the electrode. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0035] FIG1 is a schematic diagram of the three-dimensional structure of the front side of the carbon nanoelectrode production equipment provided in an embodiment of the present application;

[0036] FIG2 is a schematic diagram of the three-dimensional structure of the back side of the carbon nanoelectrode production equipment provided in an embodiment of the present application;

[0037] FIG3 is a schematic diagram of the structure of the carbon nanoelectrode production equipment provided in an embodiment of the present application after the main body is removed;

[0038] FIG4 is a schematic diagram of the three-dimensional structure of the lifting unit provided in an embodiment of the present application;

[0039] FIG5 is a human-computer interaction interface of a preparation procedure in a preparation method provided in an embodiment of the present application;

[0040] FIG6 is a cyclic voltammogram of a carbon nanodisk electrode in a first embodiment of the preparation method provided in an embodiment of the present application;

[0041] FIG7 is a SEM (scanning electron microscope) image of a carbon nanodisk electrode in a first embodiment of the preparation method provided in an embodiment of the present application;

[0042] FIG8 is a cyclic voltammogram of a carbon nanodisk electrode in a second embodiment of the preparation method provided in an embodiment of the present application;

[0043] FIG9 is a SEM (scanning electron microscope) image of a carbon nanodisk electrode in a second embodiment of the preparation method provided in an embodiment of the present application;

[0044] FIG10 is a human-computer interaction interface of an annealing procedure in an annealing process provided in an embodiment of the present application;

[0045] FIG11 is an optical microscopic image of a carbon nanoelectrode after being newly prepared, tip contaminated, and annealed and cleaned in the first embodiment of the annealing process provided in the embodiments of the present application;

[0046] FIG12 is a cyclic voltammogram of a carbon nanoelectrode before and after annealing in the first embodiment of the annealing process provided in the embodiments of the present application;

[0047] FIG. 13 is a SEM image of the Au nanoelectrode before and after annealing in the second embodiment of the annealing process provided in the embodiments of the present application.

[0048] In the figure: 1-heating chamber; 11-housing; 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-bottom plate; 42-main body; 43-function button; 44-human-computer interaction interface; 45-heat dissipation hole; 46-light-proof shield; 47-drying cabin;

[0052] 5-Rotameter;

[0053] 6-Carbon source control valve;

[0054] 7- Vacuum pump;

[0055] 8-Protect the gas valve. DETAILED DESCRIPTION

[0056] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.

[0057] It should be noted that in this embodiment, the directions or positional relationships indicated by "upper", "lower", "front", "back", etc. are based on the directions or positional relationships shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as limiting the present application. In addition, "first", "second", "third", and "fourth" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0058] In order to enable those skilled in the art to better understand the present application, the present application is further described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0059] Explanation of relevant terms:

[0060] Carbon nanoelectrode: Carbon nanoelectrode is an electrochemical probe made of carbon material with a size of hundreds of nanometers in at least one dimension. It has the characteristics of high mass transfer rate, high signal-to-noise ratio, wide potential window, high temperature resistance and high conductivity. It is 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 the principle of electromagnetism. It generates rotation or linear motion by controlling the energization timing of the coil to achieve precise control. It is widely used in mechanical systems that require precise positioning.

[0062] Joule heating principle: The heating principle of Joule heating is that when current passes through a conductor, the conductor converts electrical energy into heat energy due to the existence of resistance, thereby increasing the temperature of the conductor. This process follows Joule's law, that is, the heat is proportional to the square of the current, the resistance and the time it passes through the conductor.

[0063] High-temperature thermal reduction: High-temperature thermal reduction refers to the process of thermally decomposing a compound into a single substance under high temperature conditions. It can prepare high-purity carbon materials without complex chemical reactions and is very suitable for the preparation of carbon nanoelectrodes.

[0064] Electrode annealing: Electrode annealing refers to heating the 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 properties.

[0065] In the related art, when the resistance wire is used as a heater, the upper limit of the heating temperature of the resistance wire is low, and it can usually only work stably within a temperature range below 1400°C. If the temperature exceeds this, the resistance wire is easily oxidized, melted or broken; in the process of preparing carbon nanoelectrodes, the resistance wire heater cannot make the electrode surface temperature reach above 1200°C, and it is difficult to achieve the preparation of carbon nanoelectrodes in a large size range. When using open flame heating, there is a certain danger. Although a nanoelectrode preparation platform has been constructed, its automation and program control are low. The preparation process requires human control throughout the process. Experimenters need to undergo rigorous training and long-term practice to master the electrode preparation technology. If electrodes of different sizes need to be prepared, it is necessary to explore the firing conditions separately, and the threshold for use is high; because the firing time and firing position are controlled by the experimenter, there is a certain deviation, and the reproducibility of electrode preparation is highly dependent on the experimenter's technology. Based on the above situation, this embodiment provides a carbon nanoelectrode automation and program control production equipment with high automation and program control, good reproducibility, high safety, and easy operation.

[0066] As shown in Figure 1, the equipment 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 arranged on the outer shell 11 and forming a closed chamber body with the outer shell 11. The quartz window is usually located on the front of the heating chamber 1, and is used to penetrate the position of the probe 26 inside the heating chamber 1 and the heating condition; a carbon heater 12 is provided in the closed chamber body 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, and the upper limit of the heating temperature of the resistance wire is low. It can usually only work stably within the temperature range below 1400°C. If the temperature exceeds this, the resistance wire is easily oxidized, melted or broken. In the process of preparing carbon nanoelectrodes, the resistance wire heater cannot make the electrode surface temperature reach more than 1200°C, and it is difficult to achieve the preparation of carbon nanoelectrodes in a large size range. The carbon heater 12 is fixed on both sides by clamps 13; a protective gas inlet 15 is provided on the back plate of the outer shell 11, and the back plate refers to the back plate opposite to the front of the outer shell 11. The protective gas inlet 15 is connected to an external 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 FIG3 , the heating chamber 1 also includes a water-cooled heat exchanger arranged on the periphery of the shell 11, the water-cooled heat exchanger includes a heating chamber heat exchanger 14 arranged on both sides and / or the upper side of the shell 11 and an electrode heat exchanger 16 arranged on the back plate of the shell 11, the heating chamber heat exchanger 14 and the electrode heat exchanger 16 are externally connected to a circulating water pump, and both are used to enhance the heat dissipation of the heating chamber 1. A temperature sensor 17 is also provided on the back plate of the 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 provided at the action end of the linear slide 23. The linear slide 23 has a high-precision power part, such as a stepper motor or a servo motor. The power part can drive the action end of the linear slide 23 to move accurately, and the action end can drive the connecting rod 25 to move. The connecting rod 25 is provided with a probe fixing clamp 21, which in turn drives the probe fixing clamp 21 to move accurately. The probe fixing clamp 21 holds the probe 26 through a clamping nut. The probe 26 moves toward or away from the heating chamber 1 along its length. The outer shell 11 is provided with a socket corresponding to the probe 26 so that the tip of the probe 26 can enter and exit the closed chamber. Generally speaking, 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 socket.

[0069] 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; when the probe 26 is sealed and connected to the carbon source, it corresponds to the preparation process of the carbon nanoelectrode, and when it is connected to the vacuum pump 7, it corresponds to the annealing process of the carbon nanoelectrode. It should be noted that the above-mentioned hose can be a silicone tube or a peristaltic pump tube, and no further restrictions are made here, and all 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 switch power supply 32 for providing electrical energy thereto, wherein the control circuit board 31 is electrically connected to the circulating water pump, the protective gas valve 8, the vacuum pump 7, the power parts of the linear slide 23 and the temperature sensor 17 respectively, and the circulating water pump, the protective gas valve 8, the vacuum pump 7, the power parts of the linear slide 23 are operated according to the preset parameters by setting the control parameters of the control circuit board 31. The temperature sensor 17 transmits the temperature information to the control circuit board 31, and displays the reading through the human-machine interaction interface 44, that is, the human-machine interaction interface 44 is also connected to the control circuit board 31 signal, and the human-machine interaction interface 44 can also be provided with control buttons for controlling the circulating water pump, the protective gas valve 8, the vacuum pump 7, the linear slide 23 and other components, and the parameter adjustment and control of the above components are realized through human-machine interaction.

[0071] The carbon nanoelectrode production equipment of the present application also includes a chassis structure 4. Please refer to Figures 1 to 3. The chassis structure 4 includes a bottom plate 41 and a main body 42 arranged on the bottom plate 41. The lifting unit 2 and the control unit are located in the chassis structure 4, and the heating cabin 1 is located on the outside of the main body 42; specifically, the heating cabin 1 is located at the left front or right front of the main body 42, and an instrument switch can be set on the main body 42 to control the switch power supply 32 to supply power to the control circuit board 31 to realize the opening and closing of the equipment.

[0072] Further, please refer to FIG. 4 , the lifting unit 2 also includes a first fixed plate 22 and a second fixed plate 24 disposed on the bottom plate 41, and the linear slide 23 is disposed on the first fixed plate 22. The action end of the linear slide 23 moves vertically, and the probe 26 is correspondingly disposed vertically to drive the probe 26 to move. The back plate of the housing 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 housing 11 and exposing the housing 11 is provided on the main body 42, and a bar hole 27 corresponding to the position is provided on the second fixed plate 24 and the main body 42, and a connecting rod 25 passes through the bar hole 27 to keep the probe 26 corresponding to the position of the jack, and the length direction of the bar hole 27 is consistent with the movement direction of the probe 26, so that the probe 26 can move smoothly and be inserted into the jack.

[0073] Secondly, the vacuum pump 7 and the protective gas valve 8 can be arranged on the bottom plate 41 and located in the main body 42. The vacuum pump 7 is used to evacuate the carbon nanoelectrode during electrode annealing. The carbon source control valve 6 is connected to the rotor flowmeter 5 through a hose. The rotor flowmeter 5 is connected to the protective gas source to monitor and control the flow of the protective gas into the heating chamber 1. The carbon source control valve 6 and the rotor flowmeter 5 are arranged on the bottom plate 41 and located outside the main body 42, which is convenient for manually adjusting the carbon source flow and observing the flowmeter reading. The carbon source control valve 6 is mainly used to control the flow of the carbon source, which is usually liquefied petroleum gas, including at least one or more of propane, butane, propylene, and butene.

[0074] It is pointed out above that a human-computer interaction interface 44 is provided on the main body 42, and a plurality of function buttons 43 may also be provided on the main body 42, such as a start button, a stop button, an emergency stop button, etc. The function button 43 may be provided on the front of the main body 42 for convenience of pressing by personnel, and the function button 43 may be connected to the signal of the control circuit board 31, so that the corresponding function can be started or closed by pressing by personnel. As for other specific settings of the function button 43, no excessive restrictions will be made here, and they all fall within the protection scope of this application.

[0075] It should be pointed out that the valve components such as the carbon source control valve 6 and the protective gas valve 8 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 actual conditions.

[0076] In addition, a light-proof shield 46 covering the outer periphery of the heating chamber 1 is provided on the main body 42. The light-proof shield 46 is detachably connected to the main body 42. When the carbon heater 12 starts to work, the light-proof shield 46 is covered to reduce the damage to the eyes caused by the strong light emitted by the heater. After the heating is completed or in the early stage of heating, the light-proof shield 46 can be removed to observe the internal situation of the heating chamber 1.

[0077] The main body 42 is also provided 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 through a hose, please refer to Figure 2, so that the protective gas passes through the drying chamber 47 and enters the heating chamber 1.

[0078] In summary of the above embodiments, the present application uses a linear slide 23 to accurately control the spatial position of the quartz nanotube / carbon nanoelectrode. The linear slide 23 has a precisely controlled servo motor or stepper motor to achieve accurate carbon nanoelectrode preparation and annealing processes; using the Joule heat principle, high-quality carbon nanoelectrodes are prepared by high-temperature thermal reduction method. The carbon heater has the advantages of high upper limit of heating temperature and fast heating and cooling rate. The carbon heater 12 is used to perform high-temperature pyrolysis deposition on the gaseous carbon source in the high-temperature resistant micro-nano probe such as quartz to achieve the preparation and annealing of the carbon nanoelectrode. Carbon materials such as graphite have good thermal conductivity and high temperature resistance, can evenly distribute Joule heat, and are suitable for use as high-temperature heaters; compared with resistance wire heating, the carbon heater 12 used in the present invention can achieve a higher heating temperature, and compared with traditional open flame heating, the method of using a heater for heating is very safe, and can achieve carbon nanoelectrode preparation, carbon nanocone filling, and ultra-fast annealing of nanoelectrodes.

[0079] The present application adjusts the circulating water pump and the protective gas valve 8 through the control unit 3 to improve the service life and working stability of the equipment, and under the action of the control unit 3, the automation and program-controlled operation of the preparation process and annealing process can be realized, and the control unit 3 can flexibly store and call the adaptive program parameters to meet the standardized carbon nanoelectrode preparation requirements, and provide the possibility for highly reproducible manufacturing of carbon nanoelectrodes of different sizes and morphologies. Compared with the traditional scheme, the present invention has the advantages of high automation and program control, good reproducibility, high safety, and simple operation, which greatly reduces the operational difficulty of carbon nanoelectrode preparation, reduces the operating threshold of experimenters, and has nanoelectrode ultrafast annealing technology to greatly extend the service life of the electrode.

[0080] In this embodiment, a preparation method is also provided, that is, a preparation method implemented by using the above-mentioned carbon nanoelectrode automated and program-controlled production equipment, the preparation method comprising:

[0081] S1, start the equipment, turn on the instrument switch to enable the switch power supply 32 to power the control circuit board 31, the control circuit board 31 controls the probe fixing clamp 21 to reset, and controls the start of the circulating water pump;

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

[0083] S3, install the probe 26, adjust the opening of the carbon source control valve 6 so that the gaseous carbon source evacuates 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. At this time, the probe 26 is a quartz nanotube, which is hollow. The end of the quartz nanotube is inserted into the hose (the hose is connected to the gaseous carbon source), and the gaseous carbon source can be passed into the 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 through the linear slide 23;

[0084] S4, setting the preparation parameters, setting the heating calorific value of the carbon heater 12, the heating time of the quartz nanotubes, the heating length of the quartz nanotubes, and the heat dissipation time of the quartz nanotubes;

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

[0086] In step S5, the electrode preparation also includes a second stage of heating. Of course, only the first stage of heating mentioned 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 the temperature required to grow carbon on quartz, the second stage is a low calorific value slow heating in order to fill the carbon at the tip of the quartz nanotube to form a carbon nanodisk electrode. Here, one or two stages of heating can be selected according to actual conditions; the second stage of heating is to start the second stage of heating when the quartz nanotube returns to the initial position after the first preset heat dissipation time, and the carbon heater 12 heats according to the third preset heating calorific value and stays for the third preset time, and then rises to the top position at the preset speed. The preset length of the rise is the heating length of the quartz nanotube, and at the top position, it is heated 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 the existing related technologies, the first preset heating calorific value and the second preset heating calorific value in the first stage heating are the same, and the third preset heating calorific value and the fourth preset heating calorific value in the second end heating are the same. However, with the advancement of science and technology and the improvement of the preparation process, it is possible that the first preset heating calorific value is different from the second preset heating calorific value, and the third preset heating calorific value is different from the fourth preset heating calorific value. These situations all fall within the protection scope of the present application.

[0088] Among them, the origin position in the above step S5 is when the quartz nanotube is fixed on the probe fixing clamp 21, and the position of the tip of the quartz nanotube at this time is defined as the origin position; the vertex position is the highest point that the fixed quartz nanotube can rise in the heating chamber 1 under the control of the linear slide 23, or the highest point that the tip of the quartz nanotube rises according to the actual required heating length. In addition, the purpose of the quartz nanotube moving from the initial position to the vertex position in step S5 is that in addition to depositing carbon at the tip of the quartz nanotube, carbon also needs to be deposited at a distance below the tip, because in the subsequent experimental process, the carbon nanoelectrode needs to be connected to the electrode clamp by a metal wire, and the part of carbon deposited at the vertex position is used to contact the metal wire in the subsequent experimental process, thereby increasing the contact length between the metal wire and the carbon and preventing accidental damage to the carbon nanoelectrode during the experiment.

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

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

[0091] Step 2: Turn on the power of the device to reset the probe fixing clamp 21 and the circulating water pump will start automatically;

[0092] Step 3: Select the "Electrode Preparation" mode, click "Protective Gas Valve" to open the protective gas, adjust the partial pressure valve of the protective gas source to 0.2MPa, and adjust the flow rate of the rotor flowmeter 5 to 1L 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 exhaust the air in the corresponding hose, then connect the end of the quartz nanotube to the hose (the interface is sealed with a sealing film), and fix it on the probe fixing clamp 21, and then adjust the carbon source control valve 6 to the maximum flow rate;

[0094] Step 5: Use the linear slide 23 to accurately adjust the position of the quartz nanotube tip so that it is located in the center of the heater, which is the initial position;

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

[0096] Step 7: Cover the light-proof shield 46, press the "start" button, the protective air valve 8 automatically opens, and the cabin purification begins;

[0097] Step 8. First stage of heating: After the cabin is purified, the heater starts working at a calorific value of 320°. The quartz nanotubes stay at the initial position for 0.1 s and then heat up at a rate of 5 mm s -1 The quartz nanotube moves up to the top at a speed of , stays for 0.1s, and 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 working at a heating value of 300, and the quartz nanotube stays at the initial position for 6 seconds, then heats up at a rate of 0.5 mm s -1 The electrode moves up to the top point at a speed of 1 second, and then the heater stops working. After heat dissipation for 5 seconds, 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 wore an electrostatic protection device, removed the prepared carbon nanodisk electrode, and placed it in a solution containing 1 mmol L -1 Ferrocenemethanol (FcMeOH) and 1 mol L -1 In aqueous solution of KCl, a two-electrode system was used, with the carbon nanodisk electrode as the working electrode and Ag / AgCl (3 mol L -1 KCl) was used as the reference electrode and counter electrode, and the cyclic voltammetry test was performed in a super shielding box using an electrochemical workstation. For details, please refer to Figure 6. According to the formula a=i / 4.64nFDc, where n is the electron transfer number of 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 cm 2 s -1 ), c is the molar concentration of FcMeOH (c = 1 × 10 –3 mol L -1 ), the calculated diameter of the prepared carbon nanodisk electrode is 215 nm, which is consistent with the result shown in the SEM image in Figure 7.

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

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

[0102] Step 2: Turn on the power of the device to reset the probe fixing clamp 21 and the circulating water pump will start automatically;

[0103] Step 3: Select the "Electrode Preparation" mode, click "Protective Gas Valve" to open the protective gas, adjust the partial pressure valve of the protective gas source to 0.2MPa, and adjust the flow rate of the rotor flowmeter 5 to 1L 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 exhaust the air in the corresponding hose, then connect the end of the quartz nanotube to the hose (the interface is sealed with a sealing film), and fix it on the probe fixing clamp 21, and then adjust the carbon source control valve 6 to the maximum flow rate.

[0105] Step 5: Use the linear slide 23 to accurately adjust the position of the quartz nanotube tip so that it is located in the center of the heater, which is the initial position;

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

[0107] Step 7: Cover the light-proof shield 46, press the "start" button, the protective air valve 8 automatically opens, and the cabin purification begins;

[0108] Step 8. First stage of heating: After the cabin is purified, the heater starts working at a calorific value of 320°. The quartz nanotubes stay at the initial position for 0.3 seconds and then heat up at a rate of 5 mm s -1 The quartz nanotube moves up to the top at a speed of , stays for 0.1s, and then the heater stops working. After heat dissipation for 8s, the quartz nanotube returns to the initial position, and the first stage of heating ends.

[0109] Step 9, second stage heating: The heater starts working at a heating value of 300, and the quartz nanotube stays at the initial position for 10 seconds, then heats up at a rate of 0.5 mm s -1 The electrode moves up to the top point at a speed of 1 second, and then the heater stops working. After heat dissipation for 8 seconds, 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 wore an electrostatic protection device, removed the prepared carbon nanodisk electrode, and placed it in a solution containing 1 mmol L -1 Ferrocenemethanol (FcMeOH) and 1 mol L -1 In aqueous solution of KCl, a two-electrode system was used, with the carbon nanodisk electrode as the working electrode and Ag / AgCl (3 mol L -1 KCl) was used as the reference electrode and counter electrode, and the cyclic voltammetry test was performed in a super shielding box using an electrochemical workstation. For details, please refer to Figure 8. According to the formula a=i / 4.64nFDc, where n is the electron transfer number of 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 cm2 s -1 ), c is the molar concentration of FcMeOH (c = 1 × 10 –3 mol L -1 ), the calculated diameter of the prepared carbon nanodisk electrode is 624 nm, which is consistent with the result shown in the SEM image in Figure 9.

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

[0112] In this embodiment, an annealing process is also provided, that is, an annealing process implemented by the above-mentioned carbon nanoelectrode automation and program-controlled production equipment, and the annealing process includes:

[0113] S1, start the equipment, turn on the instrument switch to enable the switch power supply 32 to power the control circuit board 31, the control circuit board 31 controls the probe fixing clamp 21 to reset, and controls the start of the circulating water pump;

[0114] S2. Set the protective gas. Select the "electrode annealing" mode in the human-machine interaction interface 44, click "protective gas valve" to turn on the protective gas. Please refer to FIG. 10, adjust the opening of the pressure reducing valve of the protective gas source to the preset flow rate, and then close the protective gas valve 8;

[0115] S3, install the electrode to be annealed, seal the end of the carbon nanoelectrode on the hose, and fix the carbon nanoelectrode on the probe fixing clamp 21, turn on the vacuum pump 7 to evacuate the carbon nanoelectrode, that is, the tip of the carbon nanoelectrode is solid, but only the tip is filled with carbon, and the end is still a hollow quartz tube. The vacuum is to extract the air in this part to prevent the carbon nanoelectrode from being oxidized by air during the annealing process. The tip of the carbon nanoelectrode is adjusted to be located in the center of the carbon heater 12 by the linear slide 23, which is the initial position of the carbon nanoelectrode;

[0116] S4, setting annealing parameters, setting the heating calorific value of the carbon heater 12, the heating time of the carbon nanoelectrode and the heat dissipation time;

[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 calorific value and the preset heating time, and after completion, the carbon heater 12 stops working and exits the heating chamber 1 after the third preset heat dissipation and returns to the value origin position.

[0118] In the above annealing process, the origin position is when the carbon nanoelectrode is fixed on the probe fixing clamp 21 , and the position of the tip of the carbon nanoelectrode at this time is defined as the origin position.

[0119] In a first embodiment of the annealing process, a method for cleaning a carbon nanoplate electrode using an annealing process is provided, using a carbon nanoplate electrode production device, specifically comprising the following steps:

[0120] The first step is to prepare a carbon nanodisk electrode by the above preparation method. The newly prepared carbon nanodisk electrode is observed under a microscope. The electrode surface is clean and free of dust, as shown in Figure 11. -1 Ferrocenemethanol (FcMeOH) and 1 mol L -1 In the electrolyte solution of KCl, a two-electrode system was used, with the carbon nanodisk electrode as the working electrode and Ag / AgCl (3 mol L -1 KCl) was used as the reference electrode and the counter electrode to test the cyclic voltammetric characteristics of the newly prepared carbon nanodisk electrode. Please refer to FIG12 , and the diameter of the carbon nanodisk electrode was found to be 210 nm.

[0121] Step 2: Expose the newly prepared carbon nanodisk electrode to the air. After a period of time, it is observed under an optical microscope that the tip of the electrode is contaminated by dust, as shown in FIG11 .

[0122] Step 3: Turn on the power of the device to reset the probe fixing clamp 21, and the circulating water pump will automatically start at the same time;

[0123] Step 4. Select the "Electrode Annealing" mode, click "Protective Gas Valve" to turn on the protective gas, adjust the partial pressure valve of the protective gas source to 0.2MPa, and adjust the rotor flowmeter 5 flow rate to 1 L min -1 , close the protective gas valve 8;

[0124] Step 5. Connect the end of the electrode to the hose (the interface is sealed with a sealing film), and fix it on the probe fixing clamp 21. Click "vacuum pump" to start vacuuming. Use the linear slide 23 to accurately adjust the position of the electrode tip so that it is located in the center of the heater.

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

[0126] Step 7: Cover the light-proof shield 46, press the "start" button, and the protective gas valve 8 will automatically open. After the cabin purification is completed, 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 the original position, and then the protective gas valve 8 and the vacuum pump 7 are automatically closed, completing the annealing process;

[0128] Step 9: The experimenter wears an electrostatic protection device, removes the annealed electrode, and observes the electrode under an optical microscope. It is found that the tip of the electrode is clean and free of dust, as shown in Figure 11. -1 Ferrocenemethanol (FcMeOH) and 1 molL -1 The cyclic voltammetry characteristics of the annealed carbon nanodisk electrode were tested in a KCl electrolyte solution, as shown in 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 and did not affect the morphology and electrochemical properties of the electrode itself.

[0129] In a second embodiment of the annealing process, a method for reducing the surface roughness of the Au nanoelectrode by using the annealing process is provided, which specifically includes the following steps:

[0130] The first step is to prepare a carbon nanodisk electrode using the above preparation method. -1 HAuCl4 and 0.1 mol L -1 In the aqueous solution of HCl, a two-electrode system was used, with the carbon nanodisk electrode as the working electrode and Ag / AgCl (3 molL -1 KCl) was used as the reference electrode and the counter electrode, and an electrochemical workstation was used in a super shielding box to conduct an experiment of electrodepositing Au nanoparticles. Please refer to the SEM image in Figure 13. The diameter of the Au nanoparticles deposited at the tip of the electrode is about 750nm, and there are a large number of grains on its surface, which need to be annealed to reduce the surface roughness;

[0131] Step 2: Turn on the power of the device to reset the probe fixing clamp 21 and the circulating water pump will start automatically;

[0132] Step 3: Select the "electrode annealing" mode, click "protective gas valve" to open the protective gas, adjust the partial pressure valve of the protective gas source to 0.2MPa, and adjust the rotor flowmeter 5 flow rate to 1L min -1 , close the protective gas valve 8.

[0133] Step 4: Connect the end of the electrode to the hose (the interface is sealed with a sealing film), and fix it on the probe fixing clamp 21, click "vacuum pump" to start vacuuming, and use the linear slide 23 to accurately adjust the position of the electrode tip so that it is located in the center of the heater;

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

[0135] Step 6: Cover the light-proof shield 46, press the "start" button, and the protective gas valve 8 will automatically open. After the cabin purification is completed, the heater will work at a calorific value of 275 for 2 seconds, and then the heater will stop working;

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

[0137] Step 8. Perform SEM characterization on the annealed Au nanoelectrode. Please refer to FIG. 13 . The SEM image shows that the diameter of the Au nanoparticles at the tip of the electrode after annealing is about 650 nm, and the grain size on the surface is 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 merely used to distinguish one entity from other entities, but do not necessarily require or imply any actual relationship or order between these entities.

[0139] Specific examples are used herein to illustrate the principles and implementation methods of the present application, and the description of the above embodiments is only used to help understand the method and core ideas of the present application. It should be pointed out that for ordinary technicians in this technical field, without departing from the principles of the present application, several improvements and modifications can be made to the present application, and these improvements and modifications also fall within the scope of protection of the claims of the present application.

Claims

1. An automated and program-controlled production device for carbon nanoelectrodes, characterized in that: include: A heating chamber (1) comprises an outer shell (11) and a quartz window arranged on the outer shell (11) and forming a closed chamber body with the outer shell (11); a carbon heater (12) is fixedly arranged at the center of the closed chamber body; a protective gas inlet (15) is opened on the back plate of the outer shell (11); a water-cooled heat exchanger is arranged on the peripheral side of the outer shell (11); the water-cooled heat exchanger is externally connected to a circulating water pump; the protective gas inlet (15) is connected to an external protective gas source through a hose, and a protective gas valve (8) is arranged on the hose; A lifting unit (2) comprises a linear slide (23) and a connecting rod (25) arranged at an action end of the linear slide (23), wherein a probe fixing clamp (21) is arranged on the connecting rod (25), wherein the probe fixing clamp (21) holds a probe (26) via a clamping nut, wherein the probe (26) moves along its length direction toward or away from the heating chamber (1), wherein a plug hole corresponding to the probe (26) is arranged on the housing (11) so that the tip of the probe (26) can enter and exit the closed chamber, wherein the end of the probe (26) is connected to a carbon source or a vacuum pump (7) via a hose, and a carbon source control valve (6) is arranged on the hose corresponding to the carbon source; A control unit (3) comprises a control circuit board (31) and a switch power supply (32) for providing electric energy, wherein 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) respectively, so as to control the four components to operate according to preset parameters.

2. The carbon nanoelectrode automation and program-controlled production equipment according to claim 1, characterized in that: The invention also comprises a chassis structure (4), wherein the chassis structure (4) comprises a bottom plate (41) and a main body (42) arranged on the bottom plate (41), the lifting unit (2) and the control unit (3) are located in the chassis structure (4), and the heating chamber (1) is located outside the main body (42).

3. The carbon nanoelectrode automation and program-controlled production equipment according to claim 2, characterized in that: The lifting unit (2) further comprises a first fixing plate (22) and a second fixing plate (24) which are arranged on the bottom plate (41); the linear slide (23) is arranged on the first fixing plate (22); the back plate of the housing (11) is fixed on the side of the second fixing plate (24) which faces away from the first fixing plate (22); a through hole corresponding to the position of the housing (11) and exposing the housing (11) is opened on the main body (42); corresponding strip holes (27) are arranged on the second fixing plate (24) and the main body (42); the connecting rod (25) passes through the strip hole (27) to keep the probe (26) corresponding to the position of the jack; the length direction of the strip hole (27) is consistent with the movement direction of the probe (26).

4. The carbon nanoelectrode automation and program-controlled production equipment according to claim 1, characterized in that: The water-cooled heat exchanger comprises a heating chamber heat exchanger (14) arranged on both sides and / or the upper side of the outer shell (11) and an electrode heat exchanger (16) arranged on the back plate of the outer shell (11), and the protective gas inlet (15) is arranged on the back plate of the outer shell (11).

5. The carbon nanoelectrode automation and program-controlled production equipment according to claim 2, characterized in that: The vacuum pump (7) and the protective gas valve (8) are arranged on the bottom plate (41) and located inside the main body (42); the carbon source control valve (6) is connected to a rotor flow meter (5) via a hose; the rotor flow meter (5) is connected to a protective gas source to monitor the flow of the protective gas; the carbon source control valve (6) and the rotor flow meter (5) are arranged on the bottom plate (41) and located outside the main body (42).

6. The carbon nanoelectrode automation and program-controlled production equipment according to claim 2, characterized in that: The main body (42) is provided with function buttons (43) and a human-machine interaction interface (44); the function buttons (43) include a start button, a stop button, and an emergency stop button; the function buttons (43) and the human-machine interaction interface (44) are both signal-connected to the control circuit board (31).

7. The carbon nanoelectrode automation and program-controlled production equipment according to claim 2, characterized in that: The main body (42) is provided with a light-proof shield (46) covering the outer periphery of the heating chamber (1); the light-proof 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 preparation method, characterized in that: A preparation method using the carbon nanoelectrode automated and program-controlled production equipment according to any one of claims 1 to 7, the preparation method comprising: Starting the device, turning on the switch power supply (32) to supply power to the control circuit board (31), wherein the control circuit board (31) controls the probe fixing clamp (21) to reset, and controls the start of the circulating water pump; Setting the protective gas and the carbon source, selecting the "electrode preparation" mode on the human-machine interaction interface (44) and opening the protective gas valve (8), adjusting the valve opening of the protective gas source to a preset flow rate, closing the protective gas valve (8), and adjusting the pressure reducing valve of the carbon source to a preset gas pressure; Installing a probe (26), adjusting the opening of the carbon source control valve (6) so that the gaseous carbon source evacuates the air in the corresponding hose, then sealing and installing the end of the probe (26) on the hose, and fixing the probe (26) on the probe fixing clamp (21), wherein the probe (26) is a quartz nanotube, adjusting the carbon source control valve (6) to a maximum opening, and adjusting the tip of the quartz nanotube to be located at the center of the carbon heater (12) through a linear slide (23); Setting preparation parameters, setting 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, recording that the tip of the quartz nanotube is located at the center of the carbon heater (12) as the initial position, opening the protective gas valve (8) to purify the heating chamber (1), the carbon heater (12) operates according to a first preset heating calorific value, the quartz nanotube stays at the initial position for a first preset time to be heated, 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, and is heated at the top position according to a second preset heating calorific value and stays for a second preset time, after the heating is completed, the carbon heater (12) stops working, and the quartz nanotube returns to the initial position or the origin position after the first preset heat dissipation time.

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

10. An annealing process, characterized in that: The annealing process implemented by the carbon nanoelectrode automated and program-controlled production equipment according to any one of claims 1 to 7 comprises: Starting the device, turning on the switch power supply (32) to supply power to the control circuit board (31), wherein the control circuit board (31) controls the probe fixing clamp (21) to reset, and controls the start of the circulating water pump; Setting the protective gas, selecting the "electrode annealing" mode on the human-machine interaction interface (44) and opening the protective gas valve (8), adjusting the valve opening of the protective gas source to a preset flow rate, and then closing the protective gas valve (8); The electrode to be annealed is installed, the end of the probe (26) is sealed and installed on the hose, and the probe (26) is fixed on the probe fixing clamp (21), wherein the probe (26) is a carbon nanoelectrode, the vacuum pump (7) is turned on to evacuate the carbon nanoelectrode, and the tip of the carbon nanoelectrode is adjusted to be located at the center of the carbon heater (12) through the linear slide (23); Setting annealing parameters, setting the heating calorific value of the carbon heater (12), the heating time and the heat dissipation time of the carbon nanoelectrode; The electrode is annealed, the protective gas valve (8) is opened to purify the heating chamber (1), and the carbon heater (12) works according to a fifth preset heating calorific value and a preset heating time. After completion, the carbon heater (12) stops working and exits the heating chamber (1) after a third preset heat dissipation and returns to the value origin position.

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