CN112723349B - Mild discharge preparation method and device for fluorinated graphene - Google Patents
Mild discharge preparation method and device for fluorinated graphene Download PDFInfo
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Abstract
The invention discloses a method and a device for preparing fluorinated graphene through mild discharge, and relates to the technical field of graphene preparation. According to the invention, the electric field is utilized to carry out the chemical carbonization process and the physical stripping process, so that the binding force of the graphite layer is overcome, and the carbonized graphite carbon is successfully stripped into sheets, therefore, the method can be applied to almost all carbon-containing carbon sources, the high-efficiency high-quality preparation of the fluorinated graphene is ensured, meanwhile, the preparation raw materials of the fluorinated graphene are expanded to carbon-based substances, namely almost all carbon-containing substances can be used as the raw materials of the process, and the raw materials have wide sources and low cost. The active metal is used as a catalyst, the electric preheating is carried out firstly, the temperature of the carbon source and the active metal is increased, the metal activity is increased, the carbon source graphitization is realized by adding large voltage, the reaction is rapid, the reaction energy consumption is greatly reduced, the conversion rate is good, the efficiency for preparing the fluorinated graphene powder is high, the fluorinated graphene is prepared in a low-temperature environment, the low energy consumption is realized, and the preparation cost is reduced.
Description
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a mild discharge preparation method and device for fluorinated graphene.
Background
Graphene, a special allotrope of carbon, whose carbon atoms pass through sp2The hybrid orbit and the pi bond are closely and regularly linked to form a honeycomb-like shape, and have an ideal two-dimensional crystal structure. These unique knotsThe structure characteristics lead the graphite to have good electric conductivity and thermal conductivity in the layer, and the graphite has good application value in the fields of batteries, catalysis, special lubricants, powder metallurgy and the like. The fluorinated graphene is used as a novel derivative of graphene, and fluorine atoms are introduced on the basis of a two-dimensional planar structure of the graphene, so that a plurality of new electrical properties are obtained.
The nano-composite material has good hydrophobicity, electronic, optical and mechanical properties, and has incomparable potential application value in the fields of photoelectrons, electronics, friction-resistant and high-temperature-resistant coatings and the like. At present, researchers have explored some fluorinated graphene preparation processes.
Chinese patent publication No. CN111747401A discloses a method for obtaining fluorinated graphene by performing a functionalization treatment on graphene by using a carboxylation method to obtain carboxylated graphene, and then performing fluorine substitution on hydroxyl groups on carboxyl groups on the surface of graphene by using a decarboxylation substitution method to obtain fluorinated graphene. The fluorinated graphene prepared by the method has a complete surface, obvious structural damage does not occur, but the preparation period is long and needs about one week. Chinese patent publication No. CN111620326A discloses a preparation method of a fluorinated graphene material with adjustable fluorine content. The fluorine content of the product fluorinated graphene can be adjusted by adjusting the reaction time, but the problem of complex preparation operation needs to be solved urgently.
Disclosure of Invention
Aiming at the defects, the invention aims to provide a mild discharge preparation method and a mild discharge preparation device for fluorinated graphene, wherein a carbon source is processed by using a discharge technology, so that the preparation process is efficient, the carbon source is heated by low-pressure discharge, the fluorinated graphene is prepared in a low-temperature environment, the low energy consumption is realized, and the basic requirements of simple operation, high quality and high efficiency are realized on the basis of ensuring the high quality of the fluorinated graphene.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a mild discharge preparation method of fluorinated graphene, which comprises the following steps:
s1: mixing a carbon source, polytetrafluoroethylene powder and active metal with the melting point higher than 450 ℃, and then placing the mixture into a reaction tube;
s2: introducing inert gas into the reaction tube;
s3: preheating the mixture according to the set voltage value and the set capacitance value; after the preheating is finished, increasing the voltage value to perform electric discharge machining on the mixture;
s4: and (4) after the processing is finished, taking out the fluorinated graphene powder and filling the fluorinated graphene powder into a prepared container.
Further, in the step S1, the mass ratio of the carbon source, the polytetrafluoroethylene powder, and the active metal is: 10 parts of carbon source, 1 part of polytetrafluoroethylene and 0.5-1 part of active metal.
Further, in the step 3, the temperature of the mixed carbon source, polytetrafluoroethylene powder and active metal in the preheating stage is 100-200 ℃, and the temperature of the mixed carbon source, polytetrafluoroethylene powder and active metal in the reaction stage is 200-400 ℃.
Further, in the step 3, the voltage value is 20-30V and the capacitance value is 20-40 mF in the preheating process.
Further, in the step 3, the voltage value in the reaction stage is two times or more than two times of the voltage value in the preheating process.
Further, in the step 3, the mixed carbon source, polytetrafluoroethylene powder and active metal are preheated for 1-3 times.
The invention also provides a mild discharge preparation device of the fluorinated graphene, which is applied to the mild discharge preparation method of the fluorinated graphene and comprises a vacuum working cavity and a discharge control system; the vacuum working cavity comprises a reaction cover, a reaction tube, an electrode, a cavity vessel, an air inlet pipe, an air outlet pipe, a first air valve and a second air valve; the reaction cover is arranged above the cavity vessel; the reaction tube is arranged inside the cavity vessel; the two electrodes are respectively inserted at two ends of the reaction tube; one end of the air inlet pipe is communicated to an inert gas source, and the other end of the air inlet pipe is communicated to the inside of the cavity vessel; one end of the air outlet pipe is communicated to the cavity vessel, and the other end of the air outlet pipe is communicated to the outside of the cavity vessel; the first air valve is arranged on the air inlet pipe, and the second air valve is arranged on the air outlet pipe; the discharge control system is used for transmitting power to the electrode.
Further, the discharge control system comprises a charging power supply, a capacitor, a bleeder resistor, a universal meter, an NPN type triode, a first diode, a relay, an LED lamp, a first load interface, a second load interface, an inductor and a second diode; the negative electrode of the charging power supply is grounded; a plurality of capacitors are connected in parallel to form a capacitor bank; the positive electrode of each capacitor is electrically connected with the positive electrode of the charging power supply; each capacitor is connected with one of the bleeder resistors in parallel in the same direction; the negative electrode of each capacitor and the positive electrode of the universal meter are respectively and electrically connected with the base electrode of the NPN type triode; the negative electrode of the multimeter and the emitting electrode of the NPN type triode are respectively grounded; the collector of the NPN type triode is electrically connected with the positive electrode of the coil of the relay; the negative electrode of the coil of the relay is electrically connected with the normally open contact of the relay; the common end of the relay is electrically connected with the first load connector; the common end of the relay is also electrically connected with the anode of the LED lamp; the cathode of the LED lamp is grounded; the anode of the first diode is electrically connected with the cathode of the coil of the relay, and the cathode of the first diode is electrically connected with the anode of the coil of the relay; the inductor is connected in parallel with the second diode; the cathode of the second diode is electrically connected with the second load interface; the anode of the second diode is grounded; the first load interface is electrically connected with an electrode at one end of the reaction tube; the second load interface is electrically connected with the electrode at the other end of the reaction tube.
Further, a first current limiting resistor is connected in series between the negative electrodes of the plurality of discharge resistors and the positive electrode of the multimeter and the base electrode of the NPN type triode; and a second current-limiting resistor is connected in series between the common end of the relay and the anode of the LED lamp.
Further, the discharge control system also comprises a cabinet body, wherein the cabinet body is horizontally provided with a first partition plate, a second partition plate, a third partition plate and a fourth partition plate from top to bottom; the charging power supply is arranged on the first partition plate; the multimeter is arranged on the second partition plate; a plurality of the capacitors are disposed on the third and fourth spacers.
The mild discharge preparation method and device for fluorinated graphene provided by the invention have the beneficial effects that:
1. through utilizing the electric field to carry out chemical carbonization process and physical stripping process, overcome graphite layer cohesion, make the graphite carbon after the carbonization successfully peel off into the lamella, consequently can be applicable to almost all carbonaceous carbon sources, realize guaranteeing graphite fluoride high efficiency high quality preparation simultaneously, make its preparation raw materials expand carbon group material, almost all carbonaceous materials all can regard as this technology raw materials promptly, the wide cost of raw materials source is cheap.
2. Compared with the prior art that a carbon source is calcined and heated to 3000K, the method has the advantages that the active metal is used as the catalyst, electricity is firstly conducted for preheating, the temperature of the carbon source and the active metal is increased, the activity of the metal is improved, the graphitization of the carbon source is realized by applying large voltage, the temperature can reach 400 ℃ within 500ms, 80-90 wt% of the carbon source is converted into the fluorinated graphene powder under the action of the active metal and the polytetrafluoroethylene powder, the reaction is rapid, the reaction energy consumption is greatly reduced, the conversion rate is good, the efficiency of preparing the fluorinated graphene powder is high, the fluorinated graphene is prepared under the low-temperature environment, the low energy consumption is realized, and the preparation cost is reduced.
3. The preparation of the fluorinated graphene powder can be completed by performing voltage control and capacitance control, the circuit stability is high, and the processing quality of the fluorinated graphene is favorably optimized.
Drawings
FIG. 1 is a schematic flow chart of a mild discharge preparation method of fluorinated graphene in the present invention;
FIG. 2 is a schematic diagram of a vacuum chamber according to an embodiment of the present invention;
FIG. 3 is a circuit diagram of a discharge control system in an embodiment of the present invention;
fig. 4 is a schematic structural diagram of a discharge control system in an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.
Referring to fig. 1, the invention discloses a mild discharge preparation method of fluorinated graphene, which comprises the following steps:
s1: the carbon source, polytetrafluoroethylene powder and reactive metal with a melting point higher than 450 ℃ are mixed and then placed in the reaction tube 102.
S2: an inert gas is introduced into the reaction tube 102. Specifically, an inert gas such as any of argon or nitrogen.
S3: preheating the mixture according to the set voltage value and the set capacitance value; after the preheating is finished, the voltage value is increased to perform electric discharge machining on the mixture.
S4: and (4) after the processing is finished, taking out the fluorinated graphene powder and filling the fluorinated graphene powder into a prepared container.
It is noted that the carbon source may be any carbon-based material, such as any one or a mixture of carbon powder, coal powder, plastic powder or scraps. The active metal is useful as a catalyst for this reaction because it has good activity and electron conductivity and reduces the tendency of the carbon-based raw material to transform into a graphite phase. However, the preparation method provided by the invention is completed under a certain temperature condition, and in order to avoid the melting of the active metal, the active metal with the melting point higher than 450 ℃ is selected, such as Pd (palladium), Ni (nickel), Co (cobalt), Mg (magnesium) and the like. It is worth mentioning that the melting point of the metal potassium is too low, so the preparation method provided by the invention can not use the metal potassium.
According to the mild discharge preparation method of fluorinated graphene, provided by the invention, in the discharge process of active metal assisted catalysis, a carbon source is firstly carbonized into graphite carbon and then peeled into graphene. And in the stripping process of the graphite carbon, fluorine elements in the polytetrafluoroethylene powder are heated and decomposed, and form carbon-fluorine bonds with carbon elements on the graphene, so that the fluorinated graphene is generated.
It should be noted that if the ratio of the polytetrafluoroethylene in the mixture is too high, the conductivity will be affected, and the discharge will be unsuccessful, therefore, in a preferred embodiment of the present invention, the mass ratio of the carbon source, the polytetrafluoroethylene powder, and the active metal is: 10 parts of carbon source, 1 part of polytetrafluoroethylene and 0.5-1 part of active metal. The mixture is ensured to have good conductivity, and the carbon source can be effectively converted into the fluorinated graphene powder.
According to the mild discharge preparation method of the fluorinated graphene, provided by the invention, the chemical carbonization process and the physical stripping process are carried out by utilizing the electric field, the binding force of a graphite layer is overcome, and the carbonized graphite carbon is successfully stripped into a sheet layer, so that the method can be suitable for almost all carbon-containing carbon sources, the preparation raw materials of the fluorinated graphene are expanded to carbon-based substances while the efficient high-quality preparation of the fluorinated graphene is ensured, namely almost all the carbon-containing substances can be used as the raw materials of the process, and the raw materials are wide in source and low in cost. Compared with the prior art that a carbon source is calcined and heated to 3000K, the method has the advantages that the active metal is used as the catalyst, electricity is firstly conducted for preheating, the temperature of the carbon source and the active metal is increased, the activity of the metal is improved, the graphitization of the carbon source is realized by applying large voltage, the temperature can reach 400 ℃ within 500ms, 80-90 wt% of the carbon source is converted into the fluorinated graphene powder under the action of the active metal and the polytetrafluoroethylene powder, the reaction is rapid, the reaction energy consumption is greatly reduced, the conversion rate is good, the efficiency of preparing the fluorinated graphene powder is high, the fluorinated graphene is prepared under the low-temperature environment, the low energy consumption is realized, and the preparation cost is reduced. In addition, the preparation of the fluorinated graphene powder can be completed by performing voltage control and capacitance control, the circuit stability is high, and the processing quality of the fluorinated graphene is favorably optimized.
Specifically, in the step 3, the temperature of the mixed carbon source, polytetrafluoroethylene powder and active metal in the preheating stage is 100-200 ℃, and the temperature of the mixed carbon source, polytetrafluoroethylene powder and active metal in the reaction stage is 200-400 ℃. The mixed carbon source, polytetrafluoroethylene powder and active metal are preheated to 100-200 ℃, so that the temperature of the carbon source and the active metal is increased, the activity of the metal is improved, the metal activity of the carbon source is improved, the carbon source is carbonized into graphite carbon, and the graphite carbon is further peeled into graphene. The metal activity of the active metal is improved, so that the electron flow is facilitated, and the conductive heat transfer is realized. The carbon source, the polytetrafluoroethylene powder and the active metal which are mixed are preheated to 200-400 ℃, so that the carbon source is carbonized into graphite carbon in a low-temperature environment and then is peeled into graphene. And in the stripping process of the graphite carbon, fluorine elements in the polytetrafluoroethylene powder are heated and decomposed, and form carbon-fluorine bonds with carbon elements on the graphene, so that the fluorinated graphene is generated.
Specifically, in the step 3, the voltage value is 20-30V and the capacitance value is 20-40 mF in the preheating process. Therefore, the mixed carbon source, the polytetrafluoroethylene powder and the active metal are preheated under the condition of low energy consumption, and the preparation cost is reduced.
Specifically, in step 3, the voltage value in the reaction stage is two times or more than two times the voltage value in the preheating process. The temperature required by the graphene stripping stage is higher than that required by the preheating stage, and the joule heat generated in the electric discharge machining is in direct proportion to the voltage, so that the voltage value required by the graphene stripping stage is higher than that required by the preheating stage. Preferably, the voltage value in the reaction stage is set to be two times or more than two times the voltage value in the preheating process according to the temperature relationship between the temperature in the preheating stage and the temperature in the reaction stage.
Specifically, in the step 3, the mixed carbon source, polytetrafluoroethylene powder and active metal are preheated for 1-3 times. Therefore, the mode of preheating for multiple times is adopted, the carbon source, the polytetrafluoroethylene powder and the active metal after mixing are ensured to be uniformly preheated, the metal activity of the carbon source and the active metal is improved, the carbon source is favorably converted into the fluorinated graphene powder, and the conversion rate of the carbon source is improved.
The invention also discloses a mild discharge preparation device of the fluorinated graphene, which is applied to the mild discharge preparation method of the fluorinated graphene and comprises a vacuum working cavity and a discharge control system;
the vacuum working cavity comprises a reaction cover 101, a reaction tube 102, an electrode 103, a cavity dish 104, an air inlet tube 105, an air outlet tube 106, a first air valve 107 and a second air valve 108; the reaction hood 101 is arranged above the cavity vessel 104 in a covering manner; the reaction tube 102 is disposed inside the well 104; the two electrodes 103 are respectively inserted at two ends of the reaction tube 102; one end of the air inlet pipe 105 is communicated to an inert gas source, and the other end of the air inlet pipe 105 is communicated to the inside of the cavity dish 104; one end of the air outlet pipe 106 is communicated to the cavity vessel 104, and the other end of the air outlet pipe 106 is communicated to the outside of the cavity vessel 104; the first air valve 107 is arranged on the air inlet pipe 105, and the second air valve 108 is arranged on the air outlet pipe 106; the discharge control system is used to deliver power to the electrode 103 to effect discharge of the electrode 103.
According to the mild discharge preparation device for fluorinated graphene, provided by the invention, after the mixed carbon source, polytetrafluoroethylene powder and active metal are placed in the reaction tube 102, the reaction cover 101 is hermetically covered on the cavity 104, and the first air valve 107 and the second air valve 108 are opened, so that the air inlet tube 105 is communicated with the air outlet tube 106. Inert gas is introduced to fill the reaction hood 101 with inert gas, and the first gas valve 107 and the second gas valve 108 are closed. And finally, transmitting electricity to the electrode 103 through a discharge control system to realize preheating and discharge machining of the mixed carbon source, polytetrafluoroethylene powder and active metal.
Specifically, the material of the reaction tube 102 is an inert material, which is a material that does not chemically react with the active metal, such as a silicon nitride material.
Preferably, the electrode 103 may be a carbon material such as carbon or graphite, and may be a noble metal material such as platinum, palladium, or iridium.
Preferably, the reaction hood 101 and the vessel 104 have good sealing performance to prevent heat radiation from being generated to the outside during the electrical discharge machining, and simultaneously, prevent raw materials and air from reacting to generate other impurities during the reaction stage. Specifically, the material of the reaction hood 101 may be one of glass or acrylic, so as to facilitate observation. The thickness of the reaction hood 101 is 5-10 mm to ensure safety in the preparation process. The walls of the vessel 104 are made of a high temperature material, such as a metal steel plate, a quartz plate, or a high strength substrate with a high temperature resistant coating material.
It should be noted that, as shown in fig. 3, the discharge control system includes a charging power supply 201, a capacitor 202, a bleeder resistor 203, a multimeter 204, an NPN-type triode 205, a first diode 206, a relay 207, an LED lamp 208, a first load interface 209, a second load interface 210, an inductor 211, and a second diode 212; the negative electrode of the charging power supply 201 is grounded; a plurality of capacitors 202 are connected in parallel to form a capacitor bank; the positive electrode of each capacitor 202 is electrically connected to the positive electrode of the charging power supply 201; each capacitor 202 is connected in parallel with one of the bleeder resistors 203 in the same direction; the negative electrode of each capacitor 202 and the positive electrode of the multimeter 204 are respectively electrically connected with the base electrode of the NPN type triode 205; the negative electrode of the multimeter 204 and the emitter of the NPN triode 205 are respectively grounded; the collector of the NPN transistor 205 is electrically connected to the positive electrode of the coil of the relay 207; the negative electrode of the coil of the relay 207 is electrically connected with the normally open contact of the relay 207; the common end of the relay 207 is electrically connected with the first load connector; the common end of the relay 207 is also electrically connected with the positive electrode of the LED lamp 208; the cathode of the LED lamp 208 is grounded; the anode of the first diode 206 is electrically connected to the cathode of the coil of the relay 207, and the cathode of the first diode 206 is electrically connected to the anode of the coil of the relay 207; the inductor 211 is connected in parallel with the second diode 212; the cathode of the second diode 212 is electrically connected to the second load interface 210; the anode of the second diode 212 is grounded; the first load interface 209 is electrically connected with the electrode 103 at one end of the reaction tube 102; the second load port 210 is electrically connected to the electrode 103 at the other end of the reaction tube 102.
Thus, the discharge control system is realized to transmit electricity to the electrode 103, and the current is enabled to flow through the mixed carbon source, polytetrafluoroethylene powder and active metal for preheating and processing. The electromagnetic relay 207 is composed of the NPN transistor 205, the first diode 206, and the relay 207, and the remote switch can control the switch inside the relay 207 by using radio waves, so that the on/off of the control circuit is realized, and the preheating and the electric discharge machining are conveniently controlled. Multimeter 204 is used to detect the amount of charge remaining in the capacitor bank, and also to record the rate and time of discharge. Further, the first diode 206 is used to reversely freewheel, so that the first diode 206 provides a bleeding path for the current voltage in the coil of the relay 207 when the NPN transistor 205 is turned off from conduction, i.e., after the circuit is turned off. Meanwhile, the residual voltage of each capacitor 202 after discharge is discharged through the discharge resistor 203 connected thereto, so as to realize rapid discharge of the internal charge of the capacitor 202, thereby preventing the potential difference between the two ends of the capacitor 202 and the electric field generated by the charge from increasing, and reducing the work required to withstand the electric field. In addition, the inductor 211 and the second diode 212 are connected in parallel to form a protection circuit, consuming the reverse electromotive force generated by the relay 207 at the moment of power-off. Residual current and voltage in the circuit are consumed, the circuit is greatly protected, and the stability of the circuit is improved, so that the processing quality of the fluorinated graphene is optimized.
Preferably, a first current limiting resistor 213 is connected in series between the negative electrodes of the plurality of bleeder resistors 203 and the positive electrode of the multimeter 204 and the base of the NPN transistor 205; therefore, the current flowing through the NPN transistor 205 is limited by the first current limiting resistor 213, so as to reduce the power consumption of the NPN transistor 205, and prevent the NPN transistor 205 from being burned out due to an excessive current, thereby implementing a protection circuit. A second current limiting resistor 214 is connected in series between the common terminal of the relay 207 and the anode of the LED lamp 208. Therefore, the current flowing through the LED lamp 208 is limited by the second current limiting resistor 214, so that the LED lamp 208 is prevented from being burnt out due to excessive current, and a protection circuit is realized.
More preferably, the resistance value of the bleeder resistor 203 is 3000-4000 Ω. If the leakage resistance 203 is lower than 3000 Ω, the current will be too large and the circuit will be damaged. And the leakage resistor 203 higher than 4000 Ω causes too small leakage current and slow leakage, which affects the processing efficiency. Therefore, the discharging resistor 203 with a resistance value of 3000 to 4000 Ω is preferable, so that the electric charge in the capacitor 202 can be rapidly discharged, the current can be controlled to be less than 1.5mA, electric shock can be prevented, the capacitor 202 can be protected, the loss of the charging power supply 201 can be reduced, and the experimental safety can be ensured.
In some embodiments, the discharge control system further includes a cabinet 220, and the cabinet 220 is horizontally provided with a first partition 221, a second partition 222, a third partition 223, and a fourth partition 224 from top to bottom; the charging power supply 201 is disposed on the first partition 221; the multimeter 204 is disposed on the second partition 222; a plurality of the capacitors 202 are disposed on the third barrier 223 and the fourth barrier 224. In this way, by disposing the charging power supply 201 on the first partition 221 and disposing the plurality of capacitors 202 on the third partition 223 and the fourth partition 224, the charging power supply 201 is separated from the group of capacitors 202 to ensure safe operation.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (3)
1. A mild discharge preparation device of fluorinated graphene is applied to a mild discharge preparation method of fluorinated graphene, and the method comprises the following steps:
s1: mixing a carbon source, polytetrafluoroethylene powder and active metal with the melting point higher than 450 ℃, and then placing the mixture in a reaction tube, wherein the mass ratio of the carbon source to the polytetrafluoroethylene powder to the active metal is as follows: 10 parts of carbon source, 1 part of polytetrafluoroethylene and 0.5-1 part of active metal;
s2: introducing inert gas into the reaction tube;
s3: preheating the mixture for 1-3 times according to a set voltage value and a set capacitance value, wherein the voltage value is 20-30V, the capacitance value is 20-40 mF, and the temperature in the preheating stage is 100-200 ℃; after the preheating process is finished, increasing the voltage value to perform electric discharge machining on the mixture, wherein the voltage value in the reaction stage is two times or more than the voltage value in the preheating process, and the temperature in the reaction stage is 200-400 ℃;
s4: after the processing is finished, taking out the fluorinated graphene powder and putting the fluorinated graphene powder into a prepared container;
the device is characterized in that the mild discharge preparation device of the fluorinated graphene comprises a vacuum working cavity and a discharge control system;
the vacuum working cavity comprises a reaction cover, a reaction tube, an electrode, a cavity vessel, an air inlet pipe, an air outlet pipe, a first air valve and a second air valve;
the reaction cover is arranged above the cavity vessel; the reaction tube is arranged inside the cavity vessel; the two electrodes are respectively inserted at two ends of the reaction tube; one end of the air inlet pipe is communicated to an inert gas source, and the other end of the air inlet pipe is communicated to the inside of the cavity vessel; one end of the air outlet pipe is communicated to the cavity vessel, and the other end of the air outlet pipe is communicated to the outside of the cavity vessel; the first air valve is arranged on the air inlet pipe, and the second air valve is arranged on the air outlet pipe; the discharge control system is used for transmitting power to the electrode;
the discharge control system comprises a charging power supply, a capacitor, a bleeder resistor, a universal meter, an NPN type triode, a first diode, a relay, an LED lamp, a first load interface, a second load interface, an inductor and a second diode;
the negative electrode of the charging power supply is grounded; a plurality of capacitors are connected in parallel to form a capacitor bank; the positive electrode of each capacitor is electrically connected with the positive electrode of the charging power supply; each capacitor is connected with one of the bleeder resistors in parallel in the same direction; the negative electrode of each capacitor and the positive electrode of the universal meter are respectively and electrically connected with the base electrode of the NPN type triode; the negative electrode of the multimeter and the emitting electrode of the NPN type triode are respectively grounded; the collector of the NPN type triode is electrically connected with the positive electrode of the coil of the relay; the negative electrode of the coil of the relay is electrically connected with the normally open contact of the relay; the common end of the relay is electrically connected with the first load connector; the common end of the relay is also electrically connected with the anode of the LED lamp; the cathode of the LED lamp is grounded; the anode of the first diode is electrically connected with the cathode of the coil of the relay, and the cathode of the first diode is electrically connected with the anode of the coil of the relay; the inductor is connected in parallel with the second diode; the cathode of the second diode is electrically connected with the second load interface; the anode of the second diode is grounded; the first load interface is electrically connected with an electrode at one end of the reaction tube; the second load interface is electrically connected with the electrode at the other end of the reaction tube.
2. The mild discharge preparation device for fluorinated graphene according to claim 1, wherein: a first current limiting resistor is connected in series between the negative electrodes of the plurality of discharge resistors and the positive electrode of the multimeter and the base electrode of the NPN type triode; and a second current-limiting resistor is connected in series between the common end of the relay and the anode of the LED lamp.
3. The mild discharge preparation device for fluorinated graphene according to claim 1, wherein: the discharge control system also comprises a cabinet body, wherein the cabinet body is horizontally provided with a first partition plate, a second partition plate, a third partition plate and a fourth partition plate from top to bottom; the charging power supply is arranged on the first partition plate; the multimeter is arranged on the second partition plate; a plurality of the capacitors are disposed on the third and fourth spacers.
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| CN104071774A (en) * | 2013-03-29 | 2014-10-01 | 中国科学院兰州化学物理研究所 | Method for preparing fluorinated graphene |
| CN104993145A (en) * | 2015-05-29 | 2015-10-21 | 深圳好电科技有限公司 | Electrode with fluorinated graphene as conductive agent and application in lithium ion batteries |
| CN104986750A (en) * | 2015-06-26 | 2015-10-21 | 浙江大学 | Preparation method for fluorinated graphene |
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| CN103283084A (en) * | 2011-01-11 | 2013-09-04 | 巴特尔纪念研究院 | Graphene-based battery electrodes having continuous flow paths |
| CN104071774A (en) * | 2013-03-29 | 2014-10-01 | 中国科学院兰州化学物理研究所 | Method for preparing fluorinated graphene |
| CN104993145A (en) * | 2015-05-29 | 2015-10-21 | 深圳好电科技有限公司 | Electrode with fluorinated graphene as conductive agent and application in lithium ion batteries |
| CN104986750A (en) * | 2015-06-26 | 2015-10-21 | 浙江大学 | Preparation method for fluorinated graphene |
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