CN116332160B - Synthesis device and synthesis method of carbon nano tube - Google Patents
Synthesis device and synthesis method of carbon nano tube Download PDFInfo
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- CN116332160B CN116332160B CN202310362392.5A CN202310362392A CN116332160B CN 116332160 B CN116332160 B CN 116332160B CN 202310362392 A CN202310362392 A CN 202310362392A CN 116332160 B CN116332160 B CN 116332160B
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Abstract
The application belongs to the technical field of carbon nano material synthesis devices, and particularly discloses a synthesis device and a synthesis method of a carbon nano tube. The catalyst is arranged in the material trays, the material trays are in one-to-one correspondence with the spray heads, and the heating pipes and the heat preservation layers are arranged outside the spray heads and the second transportation unit, so that an optimized airflow field and an optimized temperature field are provided, and the stable growth of the carbon nanotubes is ensured.
Description
Technical Field
The application belongs to the technical field of carbon nano material synthesis devices, and particularly relates to a synthesis device and a synthesis method of a carbon nano tube.
Background
In recent years, carbon nanotubes have been rapidly developed in the fields of electrothermal conversion slurry additives and functional master batch additives, particularly in the fields of lithium-ion conductive slurry additives, and the market space of the carbon nanotubes of the global lithium battery in 2025 is expected to reach 184 hundred million, and the market demand for the carbon nanotubes is expected to further rise. The main preparation methods of the carbon nano tube comprise an electric arc method, a chemical vapor deposition method, a laser method and the like, wherein the chemical vapor deposition method has the advantages of simple process, easy control of parameters, pure and controllable product and capability of realizing the macro-mass production of the carbon nano tube, so that the current industrialized synthesis method of the carbon nano tube mostly adopts the chemical vapor deposition, and a small test device of the industrialized synthesis method is usually a horizontal tube furnace or a vertical tube furnace. According to the principle of a vertical tube furnace, a fluidized bed growth system is designed by part of enterprises, so that batch preparation of carbon nanotubes can be realized, but the catalyst in the fluidized bed is disturbed by dynamic balance of air flow and gravity and is not suitable for stable growth of a compact carbon nanotube array; the horizontal tube furnace amplifying production equipment has the problems of uneven distribution of air flow fields and temperature fields, and the like. Aiming at the problems, the patent aims to provide a synthesis device and a synthesis method for carbon nanotubes, which can optimize the distribution of an air flow field and a temperature field and can be used for stably growing a carbon nanotube vertical array.
Disclosure of Invention
The application aims to provide a synthesis device and a synthesis method of carbon nanotubes, which are used for solving the problems of uneven distribution of an air flow field and a temperature field and inapplicability to stable growth of a compact carbon nanotube array caused by a horizontal tube furnace and a vertical tube furnace at present.
In order to achieve the above purpose, the technical scheme of the application is as follows: the utility model provides a synthesizer of carbon nanotube, includes feeding equipment, reaction unit and the discharging equipment that sets gradually, feeding equipment includes first control unit, feed chamber, first vacuum system, first protection gas system and locates the first unit and the first transportation unit of placing in the feed chamber, reaction unit includes second control unit, reaction chamber, second protection gas system, second vacuum system, reaction gas system and locates the second transportation unit and the heating unit in the reaction chamber, discharging equipment includes third control unit, discharge chamber, third vacuum system, third protection gas system and locates the third transportation unit and the second unit of placing in the discharge chamber; pressure gauges are arranged on the feeding chamber, the discharging chamber and the reaction chamber; the feeding chamber is provided with a first discharging hole close to one side of the reaction chamber, a first sealing connecting piece is arranged at the first discharging hole, a second discharging hole and a first feeding hole are respectively arranged at two sides of the reaction chamber, a second sealing connecting piece and a third sealing connecting piece are respectively arranged at the first discharging hole and the second discharging hole, a second feeding hole is arranged at one side of the discharging chamber close to the reaction chamber, a fourth sealing connecting piece is arranged at the second feeding hole, the first sealing connecting piece is connected with the second sealing connecting piece, the third sealing connecting piece is connected with the fourth sealing connecting piece, the first discharging hole is communicated with or isolated from the first feeding hole through the first sealing connecting piece and the second sealing connecting piece, and the second discharging hole is communicated with or isolated from the fourth sealing connecting piece through the third sealing connecting piece and the fourth sealing connecting piece; the first placing unit is used for placing a plurality of material trays filled with catalysts, the first transporting unit is used for transporting the material trays on the first placing unit to the second transporting unit in sequence, the second transporting unit is used for transporting the material trays towards the direction of the discharging chamber, and the third transporting unit is used for transporting the material trays on the second transporting unit to the second placing unit; the first vacuum system, the second vacuum system and the third vacuum system are respectively used for vacuumizing the feeding chamber, the reaction chamber and the discharging chamber; the first shielding gas system, the second shielding gas system and the third shielding gas system are respectively used for conveying shielding gas to the feeding chamber, the reaction chamber and the discharging chamber, and the reaction gas system is used for conveying preheated carbon source gas and carrier gas to the reaction chamber; the heating unit is used for heating the reaction chamber, the first control unit is used for controlling the first vacuum system, the first protective gas system, the first placing unit and the first transportation unit, and the second control unit is used for controlling the second vacuum system, the second protective gas system, the reaction gas system, the heating unit and the second transportation unit; the third control unit is used for controlling the third vacuum system, the third shielding gas system, the second placing unit and the third transportation unit; one side of the feeding chamber and one side of the discharging chamber are provided with openable door bodies; the quantity that feed chamber and ejection of compact room can hold the material tray is greater than the reaction chamber can hold the quantity of material tray.
Further, the first unit of placing and the second unit of placing all include rotary driving piece, sprocket chain mechanism and a plurality of board of placing, sprocket chain mechanism installs one side of feeding chamber or ejection of compact room, rotary driving piece is used for driving sprocket chain mechanism operation, a plurality of place the board level in proper order evenly fix on sprocket chain mechanism's the chain.
Further, the first transporting unit is located below the first placing unit and is used for transporting the material tray on the placing plate at the lowest position of the first placing unit to the reaction chamber, and the third transporting unit is located above the second placing unit and is used for transporting the material tray in the reaction chamber to the material tray on the placing plate at the highest position of the second placing unit; the first conveying unit and the second conveying unit comprise a transverse driving piece, a clamping driving piece, two groups of vertical driving pieces, two groups of supporting plates and two groups of clamping jaws, wherein the transverse driving piece is used for transversely driving the clamping driving piece, the clamping driving piece is used for driving the two groups of supporting plates to be far away from or close to each other, the two groups of vertical driving pieces are respectively arranged on the two groups of supporting plates, the two groups of vertical driving pieces are respectively used for driving the two groups of clamping jaws to vertically move, and the clamping jaws can be contracted below the first placing unit or above the second placing unit by the vertical driving pieces; the material tray is in a round table structure with a large upper part and a small lower part; the two groups of clamping jaws are respectively used for clamping two sides of the material tray; the transverse driving piece of the first conveying unit is arranged at the bottom of the feeding chamber, and the transverse driving piece of the second conveying unit is arranged at the top of the discharging chamber.
Further, clamping jaw slope sets up, inclination and the outer wall phase-match of material tray.
Further, the heating unit comprises a heating pipe, a heat preservation layer and a temperature measuring element, the heating pipe is arranged outside the second transportation unit and the spraying mechanism, the heat preservation layer is arranged on the inner wall of the reaction chamber, and the temperature measuring element is used for measuring the temperature in the heating pipe.
Further, the reaction gas system comprises a gas mixing tank and a spraying mechanism, wherein the spraying mechanism is arranged in the reaction chamber and comprises an air inlet main pipe, a plurality of air inlet branch pipes and a plurality of spray heads, the air inlet main pipe is communicated with the gas mixing tank, the air inlet main pipe is provided with an air inlet valve, the air inlet branch pipes are respectively connected with the air inlet main pipe, the air inlet branch pipes are in one-to-one correspondence with the spray heads, and the spray heads are communicated with the air inlet branch pipes; the maximum number of trays for accommodating the materials in the reaction chamber is equal to the number of the spray heads; the reaction chamber is close to one side of the discharging chamber and is also provided with an air outlet pipe, the air inlet end of the air outlet pipe is positioned in the heating pipe, and the air outlet pipe is provided with an air outlet valve.
Further, the first sealing connecting piece, the second sealing connecting piece, the third sealing connecting piece and the third sealing connecting piece adopt flange type knife gate valves.
A method for synthesizing carbon nanotubes comprises the following steps:
placing material trays filled with catalysts into a feeding chamber, placing m material trays on each placing plate, wherein the distance a between the centers of the material trays is equal to the distance between the centers of adjacent spray heads, the number of the spray heads is n, n is an integer multiple of m, closing a door body, connecting a first sealing connecting piece with a second sealing connecting piece, and connecting a fourth sealing connecting piece of an empty discharging chamber with a third sealing connecting piece;
opening the first sealing connecting piece and the second sealing connecting piece, driving the first conveying unit by the first control unit, and conveying m material trays on a placement plate at the lowest part of the first placement unit to the second conveying unit in the reaction chamber by the first conveying unit, wherein the m material trays just correspond to the spray heads one by one; then the first transport unit returns to the initial position, the first control unit drives the first placement unit to operate, the next group of placement plates are operated to the lowest position, meanwhile, the second control unit drives the second transport unit to operate, and the second transport unit drives m material trays to move by a distance of m x a towards the direction of the discharge chamber; the first control unit drives the first transport unit again to transport m material trays on the lowest placing plate, and the steps are repeated until the number of the material trays in the reaction chamber is equal to the number of the spray heads;
then closing the first sealing connecting piece and the second sealing connecting piece, opening the first vacuum system, the second vacuum system and the third vacuum system, respectively vacuumizing the feeding chamber, the reaction chamber and the discharging chamber, then opening the first protective gas system, the second protective gas system and the third protective gas system, and filling protective gas into the feeding chamber, the reaction chamber and the discharging chamber to one atmosphere;
the second control unit opens the heating unit, the heating unit heats the reaction chamber, after the temperature rises to the temperature required by the growth of the carbon nano tube, the second control unit opens the air inlet valve, the carbon source gas and the carrier gas preheated to 500 ℃ are conveyed to each spray head, and the tail gas is discharged through the air outlet valve;
after the growth time of the carbon nano tube is reached, closing the air inlet valve, and opening the first sealing connecting piece, the second sealing connecting piece, the third sealing connecting piece and the fourth sealing connecting piece; the third control unit starts the third transport unit to transport m material trays on the second transport unit to the uppermost placement plate of the second placement unit, then simultaneously starts the second placement unit, the second transport unit and the first transport unit, the second placement unit operates to enable the other empty placement plate to be placed at the uppermost position, the second transport unit drives the material trays to move by m a distance towards the direction of the discharge chamber, the first transport unit transports the m material trays on the lowermost placement plate of the first placement unit to the second transport unit, and the steps are repeated until all the material trays filled with carbon nanotubes are transported to the discharge chamber;
repeating the steps until the discharging chamber is full or all material trays in the feeding chamber are transported out; opening a first protective gas system or a third protective gas system, and pumping out the protective gas in the feeding chamber or the discharging chamber; then opening a door body on the feeding chamber or the discharging chamber, and disassembling the first sealing connecting piece or the fourth sealing connecting piece; and the production can be continued by replacing the feeding chamber filled with the material tray or the empty discharging chamber.
The beneficial effects of this technical scheme lie in:
(1) in this technical scheme catalyst splendid attire to the material tray in to every material tray corresponds a set of shower nozzle, still sets up heating pipe and heat preservation in the outside of shower nozzle and second transportation unit simultaneously, has provided comparatively optimized air flow field and temperature field, thereby guarantees the stable growth of carbon nanotube.
(2) According to the technical scheme, the discharging chamber and the feeding chamber are arranged, so that the organic isolation between the atmosphere environment and flammable and explosive gas required by the growth of the carbon nano tube is realized.
(3) According to the technical scheme, the catalyst and the carbon nanotube product materials can be continuously added and collected through reasonable matching of the first placing unit, the second placing unit, the first transporting unit, the second transporting unit and the third transporting unit.
(4) According to the technical scheme, through the connection of the first sealing connecting piece and the second sealing connecting piece, and the connection of the third sealing connecting piece and the fourth sealing connecting piece, the communication and isolation of the feeding chamber and the reaction chamber and the communication and isolation of the reaction chamber and the discharging chamber are realized, the detachable connection is realized, the timely supply and the transportation of the material tray filled with the catalyst and the material tray filled with the carbon nano tubes are ensured, the production efficiency is improved, the method is suitable for industrial production, and the method has good application prospects in the field of carbon nano tube synthesis.
Drawings
FIG. 1 is a schematic diagram showing the internal structure of a device for synthesizing carbon nanotubes according to the present application;
FIG. 2 is a front view of FIG. 1;
FIG. 3 is a schematic view of the feed chamber of FIG. 1;
FIG. 4 is a schematic view of the reaction chamber of FIG. 1;
FIG. 5 is a schematic view of the structure of FIG. 1 with the insulation layer removed;
FIG. 6 is a schematic view of the structure of FIG. 5 with the heating tube removed;
FIG. 7 is a schematic view of the discharge chamber of FIG. 1;
FIG. 8 is a scanning electron microscope image of a grown carbon nanotube in the first embodiment;
fig. 9 is a scanning electron microscope image of a grown carbon nanotube in the second embodiment.
Detailed Description
The following is a further detailed description of the embodiments:
reference numerals in the drawings of the specification include: the device comprises a feeding chamber 1, a reaction chamber 2, a discharging chamber 3, a first shielding gas inlet 4, a first shielding gas outlet 5, an air inlet main pipe 6, an air outlet pipe 7, a rotary driving piece 8, a chain wheel and chain mechanism 9, a placing plate 10, a transverse driving piece 11, a supporting plate 12, a vertical driving piece 13, a clamping jaw 14, a first discharging hole 15, a first feeding hole 16, an insulating layer 17, a first sealing connecting piece 18, a second sealing connecting piece 19, an air inlet branch pipe 20, a conveyor belt 21, a second discharging hole 22, a material tray 23, a spray head 24, a second transportation unit 25, a second feeding hole 26, a third shielding gas inlet 27, a third shielding gas outlet 28, a second shielding gas inlet 29, a second shielding gas outlet 30, a third sealing connecting piece 31, a fourth sealing connecting piece 32, a first placing unit 33, a first transportation unit 34, a second placing unit 35, a third transportation unit 36 and a heating pipe 37.
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
The embodiment is basically as shown in the accompanying figures 1-7: as shown in fig. 1 and 2, the synthesis device of the carbon nanotube comprises a feeding device, a reaction device and a discharging device which are sequentially arranged, wherein the feeding device comprises a first control unit, a feeding chamber 1, a first vacuum system, a first protective gas system, a first placement unit 33 and a first transport unit 34 which are arranged in the feeding chamber 1, the reaction device comprises a second control unit, a reaction chamber 2, a second protective gas system, a second vacuum system, a reaction gas system, a second transport unit 25 and a heating unit which are arranged in the reaction chamber 2, and the discharging device comprises a third control unit, a discharging chamber 3, a third vacuum system, a third protective gas system, a third transport unit 36 and a second placement unit 35 which are arranged in the discharging chamber 3; and the feeding chamber 1, the discharging chamber 3 and the reaction chamber 2 are respectively provided with a pressure gauge, and the pressure gauges are used for detecting the pressure in the corresponding chambers. One side of the feeding chamber 1 and one side of the discharging chamber 3 are provided with openable door bodies, sealing layers are arranged on the door bodies, and the sealing layers seal the whole feeding chamber 1 and the whole discharging chamber 3 when the door bodies are closed.
As shown in fig. 2 and 3, a first discharge port 15 is arranged on one side of the feeding chamber 1, which is close to the reaction chamber 2, and a first sealing connecting piece 18 is welded at the first discharge port 15. As shown in fig. 2 and 6, two sides of the reaction chamber 2 are respectively provided with a second discharge port 22 and a first feed port 16, and the first feed port 16 and the second discharge port 22 are respectively welded with a second sealing connector 19 and a third sealing connector 31. As shown in fig. 2 and 7, a second feeding port 26 is arranged on one side of the discharging chamber 3 close to the reaction chamber 2, and a fourth sealing connecting piece 32 is arranged at the second feeding port 26. As shown in fig. 2, the first sealing connector 18 is connected with the second sealing connector 19, the third sealing connector 31 is connected with the fourth sealing connector 32, the first discharge port 15 and the first feed port 16 are communicated or isolated through the first sealing connector 18 and the second sealing connector 19, the second discharge port 22 and the second feed port 26 are communicated or isolated through the third sealing connector 31 and the fourth sealing connector 32, specifically, the first sealing connector 18, the second sealing connector 19, the third sealing connector 31 and the third sealing connector 31 adopt flange type knife gate valves, the connecting holes on the flanges are threaded holes, through holes corresponding to the threaded holes are formed on one side, close to the reaction chamber 2, of the discharge chamber 3 and the feed chamber 1, after the bolts pass through the through holes, the bolts are in threaded connection with the threaded holes on the two flanges, connection between the first sealing connector 18 and the second sealing connector 19, the third sealing connector 31 and the fourth sealing connector 32 is achieved, and flange gaskets are further arranged between the first sealing connector 18 and the second sealing connector 19, the third sealing connector 31 and the fourth sealing connector 32.
The first placing unit 33 is used for placing a plurality of material trays 23 filled with catalysts, the first transporting unit 34 is used for transporting the material trays 23 on the first placing unit 33 to the second transporting unit 25 in sequence, the second transporting unit 25 is used for transporting the material trays 23 towards the discharging chamber 3, and the third transporting unit 36 is used for transporting the material trays 23 on the second transporting unit 25 to the second placing unit 35.
As shown in fig. 3 and 7, the first placing unit 33 and the second placing unit 35 each include a rotary driving member 8, a sprocket chain mechanism 9 and a plurality of placing plates 10, the sprocket chain mechanism 9 is installed at one side of the feeding chamber 1 or the discharging chamber 3, the rotary driving member 8 is used for driving the sprocket chain mechanism 9 to operate, and the plurality of placing plates 10 are sequentially and horizontally and uniformly fixed on the chain of the sprocket chain mechanism 9. The rotary driving member 8 employs a servo motor. The placing plate 10 is printed with positioning circles or provided with positioning grooves for positioning the material trays 23.
The first transporting unit 34 is located below the first placing unit 33, and is used for transporting the material tray 23 on the placing plate 10 at the lowest position of the first placing unit 33 to the reaction chamber 2, and the second transporting unit 25 is located above the second placing unit 35, and is used for transporting the material tray 23 in the reaction chamber 2 to the material tray 23 on the placing plate 10 at the highest position of the second placing unit 35. As shown in fig. 3 and 7, the first transporting unit 34 and the second transporting unit 25 each include a transverse driving member 11, a clamping driving member, two sets of vertical driving members 13, two sets of support plates 12 and two sets of clamping jaws 14, the transverse driving member 11 is used for driving the two sets of support plates 12 away from or close to each other, the two sets of vertical driving members 13 are respectively disposed on the two sets of support plates 12, the two sets of vertical driving members 13 are respectively used for driving the two sets of clamping jaws 14 to move vertically, and the clamping jaws 14 can be retracted below the first placing unit 33 or above the second placing unit 35 by the vertical driving members 13. Specifically, the transverse driving piece 11 may be a translation stage, the clamping driving piece is a bidirectional linear motor or a bidirectional air cylinder, and the vertical driving piece 13 is a linear motor or an air cylinder. As shown in fig. 6, the material tray 23 has a truncated cone structure with a large top and a small bottom; the two groups of clamping jaws 14 are respectively used for clamping two sides of the material tray 23, the clamping jaws 14 are obliquely arranged, and the inclination angle is matched with the outer wall of the material tray 23. The transverse drive 11 of the first transport unit 34 is arranged at the bottom of the inlet chamber 1 and the transverse drive 11 of the third transport unit 36 is arranged at the top of the outlet chamber 3. The number of material trays 23 that can be accommodated in the feed chamber 1 and the discharge chamber 3 is greater than the number of material trays 23 that can be accommodated in the reaction chamber 2.
The first vacuum system, the second vacuum system and the third vacuum system are respectively used for vacuumizing the feeding chamber 1, the reaction chamber 2 and the discharging chamber 3; the first shielding gas system, the second shielding gas system and the third shielding gas system are respectively used for conveying shielding gas to the feeding chamber 1, the reaction chamber 2 and the discharging chamber 3, as shown in fig. 1, a first shielding gas inlet 4 and a first shielding gas outlet 5 are arranged on the feeding chamber 1, a second shielding gas inlet 29 and a second shielding gas outlet 30 are arranged on the reaction chamber 2, and a third shielding gas inlet 27 and a third shielding gas outlet 28 are arranged on the discharging chamber 3.
The reaction gas system is used for conveying preheated carbon source gas and carrier gas into the reaction chamber 2; as shown in fig. 6, the reaction gas system comprises a gas mixing tank and a spraying mechanism, the spraying mechanism is arranged in the reaction chamber 2, the spraying mechanism comprises a gas inlet main pipe 6, a plurality of gas inlet branch pipes 20 and a plurality of spray heads 24, the gas inlet main pipe 6 is communicated with the gas mixing tank, gas inlet valves are arranged on the gas inlet main pipe 6, the gas inlet branch pipes 20 are respectively connected with the gas inlet main pipe 6, the gas inlet branch pipes 20 are in one-to-one correspondence with the spray heads 24, and the spray heads 24 are communicated with the gas inlet branch pipes 20; the maximum number of trays 23 for holding materials in the reaction chamber 2 is equal to the number of nozzles 24; one side of the reaction chamber 2 close to the discharging chamber 3 is also provided with an air outlet pipe 7, the air inlet end of the air outlet pipe 7 is positioned in the heating pipe 37, and the air outlet pipe 7 is provided with an air outlet valve.
As shown in fig. 4 and 5, the heating unit is used for heating the reaction chamber 2, the heating unit includes a heating pipe 37, an insulating layer 17 and a temperature measuring element, the heating pipe 37 is arranged outside the second transportation unit 25 and the spraying mechanism, the insulating layer 17 is arranged on the inner wall of the reaction chamber 2, the insulating layer 17 is arranged outside the heating pipe 37, the temperature measuring element is used for measuring the temperature in the heating pipe 37, and the temperature measuring element specifically adopts a thermocouple. The second transporting unit 25 employs a conveyor belt 21.
The first control unit is used for controlling the first vacuum system, the first shielding gas system, the first placing unit 33 and the first transporting unit 34, and the second control unit is used for controlling the second vacuum system, the second shielding gas system, the reaction gas system, the heating unit and the second transporting unit 25; the third control unit is for controlling the third vacuum system, the third shielding gas system, the second placing unit 35 and the third transporting unit 36.
A method for synthesizing carbon nanotubes comprises the following steps:
s1, placing material trays 23 filled with catalysts into a feeding chamber 1, placing m (for example, two) material trays 23 on each placing plate 10, wherein the distance a between the centers of the material trays 23 is equal to the distance between the centers of adjacent spray heads 24, the number of the spray heads 24 is n, n is an integer multiple of m, closing a door body, connecting a first sealing connecting piece 18 with a second sealing connecting piece 19, and connecting a fourth sealing connecting piece 32 of an empty discharging chamber 3 with a third sealing connecting piece 31;
s2, opening the first sealing connecting piece 18 and the second sealing connecting piece 19, wherein the first control unit drives the first conveying unit 34, and the first conveying unit 34 conveys m material trays 23 on the lowest placing plate 10 of the first placing unit 33 to the second conveying unit 25 in the reaction chamber 2, and the m material trays 23 are just in one-to-one correspondence with the spray heads 24; the first transport unit 34 is then returned to the initial position, and the first transport unit 34 is specifically configured to: opening the vertical driving piece 13, the vertical driving piece 13 drives the clamping jaw 14 to move upwards until two sides of m material trays 23 are clamped, then starting the transverse driving piece 11, the transverse driving piece 11 drives the material trays 23 to move towards the second conveying unit 25, after being conveyed to the upper side of the second conveying unit 25 and being opposite to the spray nozzle 24, the vertical driving piece 13 drives the clamping jaw 14 and the material trays 23 to move downwards until the material trays 23 are positioned on the second conveying unit 25, then starting the clamping driving piece, the clamping driving piece drives the supporting plates 12 to be far away from each other, the clamping jaw 14 is far away from the material trays 23, finally the transverse driving piece 11 drives the clamping jaw 14 to return to the initial position, and the vertical driving piece 13 and the clamping moving piece also return to the original position. Then the first control unit drives the first placing unit 33 to operate, the next group of placing plates 10 are operated to the lowest position, meanwhile, the second control unit drives the second transporting unit 25 to operate, and the second transporting unit 25 drives the m material trays 23 to move by a distance of m x a towards the direction of the discharging chamber 3; the first control unit drives the first transport unit 34 again to transport m material trays 23 on the lowest placing plate 10, and the steps are repeated until the number of the material trays 23 in the reaction chamber 2 is equal to the number of the spray heads 24;
s3, closing the first sealing connecting piece 18 and the second sealing connecting piece 19, opening the first vacuum system, the second vacuum system and the third vacuum system, vacuumizing the feeding chamber 1, the reaction chamber 2 and the discharging chamber 3 respectively, opening the first protective gas system, the second protective gas system and the third protective gas system, and filling protective gas into the feeding chamber 1, the reaction chamber 2 and the discharging chamber 3 to one atmosphere;
s4, the second control unit opens the heating unit, the heating pipe 37 heats the reaction chamber 2, the temperature in the reaction chamber 2 is observed through the temperature measuring element, after the temperature rises to the temperature required by the growth of the carbon nano tube, the second control unit opens the air inlet valve, the carbon source gas and the carrier gas preheated to 500 ℃ are conveyed to each spray head 24, and the tail gas is discharged through the air outlet valve;
s5, closing the air inlet valve and opening the first sealing connector 18, the second sealing connector 19, the third sealing connector 31 and the fourth sealing connector 32 after the growth time of the carbon nano tube is reached; the third control unit starts the third transport unit 36 to transport m material trays 23 on the second transport unit 25 to the uppermost placing plate 10 of the second placing unit 35, then starts the second placing unit 35, the second transport unit 25 and the first transport unit 34 simultaneously, the second placing unit 35 operates to enable the other empty placing plate 10 to be placed at the uppermost, the second transport unit 25 drives the material trays 23 to move by m a distance towards the discharging chamber 3, the first transport unit 34 transports m material trays 23 on the lowermost placing plate 10 of the first placing unit 33 to the second transport unit 25, and the steps are repeated until all the material trays 23 filled with carbon nanotubes are transported to the discharging chamber 3;
s6, repeating the steps until the discharging chamber 3 is full or all the material trays 23 in the feeding chamber 1 are transported out; opening a first protective gas system or a third protective gas system to pump out the protective gas in the feeding chamber 1 or the discharging chamber 3; then opening the door body on the feeding chamber 1 or the discharging chamber 3, and detaching the first sealing connecting piece 18 or the fourth sealing connecting piece 32; the production can be continued by replacing the feeding chamber 1 filled with the material tray 23 or the empty discharging chamber 3.
The following test was performed on the carbon nanotubes after production according to two specific examples:
embodiment one: the retention time of the material tray in the reaction chamber 2 is 30min, the reaction temperature is 650 ℃, the catalyst in the material tray and the catalyst in the material tray are 5g of cobalt-based hydrotalcite, the synthesized carbon nano tube is subjected to electron microscope scanning, the electron microscope scanning diagram is shown in figure 8, and the internal appearance completely meets the requirements.
Embodiment two: the retention time of the material tray in the reaction chamber 2 is 60min, the reaction temperature is 650 ℃, the catalyst in the material tray and the catalyst in the material tray are 5g of cobalt-based hydrotalcite, the synthesized carbon nano tube is subjected to electron microscope scanning, the electron microscope scanning diagram is shown in figure 9, and the internal appearance completely meets the requirements.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The foregoing is merely an embodiment of the present application, and a specific structure and characteristics of common knowledge in the art, which are well known in the scheme, are not described herein, so that a person of ordinary skill in the art knows all the prior art in the application date or before the priority date, can know all the prior art in the field, and has the capability of applying the conventional experimental means before the date, and a person of ordinary skill in the art can complete and implement the present embodiment in combination with his own capability in the light of the present application, and some typical known structures or known methods should not be an obstacle for a person of ordinary skill in the art to implement the present application. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present application, and these should also be considered as the scope of the present application, which does not affect the effect of the implementation of the present application and the utility of the patent. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (8)
1. A synthesis device of carbon nanotubes is characterized in that: the device comprises a feeding device, a reaction device and a discharging device which are sequentially arranged, wherein the feeding device comprises a first control unit, a feeding chamber (1), a first vacuum system, a first protective gas system, a first placement unit (33) and a first transportation unit (34) which are arranged in the feeding chamber (1), the reaction device comprises a second control unit, a reaction chamber (2), a second protective gas system, a second vacuum system, a reaction gas system, a second transportation unit (25) and a heating unit which are arranged in the reaction chamber (2), and the discharging device comprises a third control unit, a discharging chamber (3), a third vacuum system, a third protective gas system, a third transportation unit (36) and a second placement unit (35) which are arranged in the discharging chamber (3); pressure gauges are arranged on the feeding chamber (1), the discharging chamber (3) and the reaction chamber (2); a first discharging hole (15) is formed in one side, close to the reaction chamber (2), of the feeding chamber (1), a first sealing connecting piece (18) is arranged at the first discharging hole (15), a second discharging hole (22) and a first feeding hole (16) are respectively formed in two sides of the reaction chamber (2), a second sealing connecting piece (19) and a third sealing connecting piece (31) are respectively arranged at the first feeding hole (16) and the second discharging hole (22), a second feeding hole (26) is formed in one side, close to the reaction chamber (2), of the discharging chamber (3), a fourth sealing connecting piece (32) is arranged at the second feeding hole (26), the first sealing connecting piece (18) is connected with the second sealing connecting piece (19), the third sealing connecting piece (31) is connected with the fourth sealing connecting piece (32), the first discharging hole (15) is communicated with the second sealing connecting piece (19) or the second sealing connecting piece (32) is communicated with the second sealing connecting piece (22) or the fourth sealing connecting piece (32); the first placing unit (33) is used for placing a plurality of material trays (23) filled with catalysts, the first transporting unit (34) is used for sequentially transporting the material trays (23) on the first placing unit (33) to the second transporting unit (25), the second transporting unit (25) is used for transporting the material trays (23) towards the direction of the discharging chamber (3), and the third transporting unit (36) is used for transporting the material trays (23) on the second transporting unit (25) to the second placing unit (35); the first vacuum system, the second vacuum system and the third vacuum system are respectively used for vacuumizing the feeding chamber (1), the reaction chamber (2) and the discharging chamber (3); the first protective gas system, the second protective gas system and the third protective gas system are respectively used for conveying protective gas to the feeding chamber (1), the reaction chamber (2) and the discharging chamber (3), and the reaction gas system is used for conveying preheated carbon source gas and carrier gas into the reaction chamber (2); the heating unit is used for heating the reaction chamber (2), the first control unit is used for controlling the first vacuum system, the first protective gas system, the first placing unit (33) and the first transportation unit (34), and the second control unit is used for controlling the second vacuum system, the second protective gas system, the reaction gas system, the heating unit and the second transportation unit (25); the third control unit is used for controlling the third vacuum system, the third shielding gas system, the second placing unit (35) and the third transporting unit (36); one side of the feeding chamber (1) and one side of the discharging chamber (3) are provided with openable door bodies; the number of the material trays (23) which can be contained in the feeding chamber (1) and the discharging chamber (3) is larger than the number of the material trays (23) which can be contained in the reaction chamber (2).
2. The apparatus for synthesizing carbon nanotubes according to claim 1, wherein: the first placing unit (33) and the second placing unit (35) comprise a rotary driving piece (8), a chain wheel chain mechanism (9) and a plurality of placing plates (10), the chain wheel chain mechanism (9) is installed on one side of the feeding chamber (1) or the discharging chamber (3), the rotary driving piece (8) is used for driving the chain wheel chain mechanism (9) to operate, and the plurality of placing plates (10) are sequentially and horizontally and uniformly fixed on a chain of the chain wheel chain mechanism (9).
3. The apparatus for synthesizing carbon nanotubes according to claim 2, wherein: the first transporting unit (34) is located below the first placing unit (33) and is used for transporting the material tray (23) on the placing plate (10) at the lowest part of the first placing unit (33) to the reaction chamber (2), and the third transporting unit (36) is located above the second placing unit (35) and is used for transporting the material tray (23) in the reaction chamber (2) to the material tray (23) on the placing plate (10) at the highest part of the second placing unit (35); the first transporting unit (34) and the second transporting unit (25) comprise a transverse driving piece (11), a clamping driving piece, two groups of vertical driving pieces (13), two groups of supporting plates (12) and two groups of clamping jaws (14), the transverse driving piece (11) is used for transversely driving the clamping driving piece, the clamping driving piece is used for driving the two groups of supporting plates (12) to be far away from or close to each other, the two groups of vertical driving pieces (13) are respectively arranged on the two groups of supporting plates (12), the two groups of vertical driving pieces (13) are respectively used for driving the two groups of clamping jaws (14) to vertically move, and the clamping jaws (14) can be contracted below the first placing unit (33) or above the second placing unit (35); the material tray (23) is in a round table structure with a large upper part and a small lower part; the two groups of clamping jaws (14) are respectively used for clamping two sides of the material tray (23); the transverse driving piece (11) of the first conveying unit (34) is arranged at the bottom of the feeding chamber (1), and the transverse driving piece (11) of the second conveying unit (25) is arranged at the top of the discharging chamber (3).
4. A device for synthesizing carbon nanotubes according to claim 3, wherein: the clamping jaw (14) is obliquely arranged, and the inclination angle is matched with the outer wall of the material tray (23).
5. The apparatus for synthesizing carbon nanotubes according to claim 4, wherein: the heating unit comprises a heating pipe (37), an insulating layer (17) and a temperature measuring element, wherein the heating pipe (37) is arranged outside the second conveying unit (25) and the spraying mechanism, the insulating layer (17) is arranged on the inner wall of the reaction chamber (2), and the temperature measuring element is used for measuring the temperature in the heating pipe (37).
6. The apparatus for synthesizing carbon nanotubes according to claim 5, wherein: the reaction gas system comprises a gas mixing tank and a spraying mechanism, wherein the spraying mechanism is arranged in the reaction chamber (2), the spraying mechanism comprises an air inlet main pipe (6), a plurality of air inlet branch pipes (20) and a plurality of spray heads (24), the air inlet main pipe (6) is communicated with the gas mixing tank, the air inlet main pipe (6) is provided with an air inlet valve, the air inlet branch pipes (20) are respectively connected with the air inlet main pipe (6), the air inlet branch pipes (20) are in one-to-one correspondence with the spray heads (24), and the spray heads (24) are communicated with the air inlet branch pipes (20); the maximum number of material trays (23) accommodated in the reaction chamber (2) is equal to the number of spray heads (24); one side of the reaction chamber (2) close to the discharging chamber (3) is also provided with an air outlet pipe (7), the air inlet end of the air outlet pipe (7) is positioned in the heating pipe (37), and the air outlet pipe (7) is provided with an air outlet valve.
7. The apparatus for synthesizing carbon nanotubes according to claim 6, wherein: the first sealing connecting piece (18), the second sealing connecting piece (19), the third sealing connecting piece (31) and the third sealing connecting piece (31) adopt flange type knife gate valves.
8. A method for synthesizing carbon nanotubes is characterized in that: a synthesis apparatus for carbon nanotubes according to claim 7, comprising the steps of:
placing material trays (23) filled with catalysts into a feeding chamber (1), placing m material trays (23) on each placing plate (10), wherein the distance a between the centers of the material trays (23) is equal to the distance between the centers of adjacent spray heads (24), the number of the spray heads (24) is n, n is an integer multiple of m, closing a door body, connecting a first sealing connecting piece (18) with a second sealing connecting piece (19), and connecting a fourth sealing connecting piece (32) of an empty discharging chamber (3) with a third sealing connecting piece (31);
opening a first sealing connecting piece (18) and a second sealing connecting piece (19), wherein the first control unit drives a first transportation unit (34) to transport m material trays (23) on a lowest placement plate (10) of a first placement unit (33) to a second transportation unit (25) in a reaction chamber (2), and the m material trays (23) are just in one-to-one correspondence with spray heads (24); then the first transport unit (34) returns to the initial position, the first control unit drives the first placing unit (33) to operate, the next group of placing plates (10) are operated to the lowest position, meanwhile, the second control unit drives the second transport unit (25) to operate, and the second transport unit (25) drives m material trays (23) to move by m x a distance towards the direction of the discharge chamber (3); the first control unit drives the first transportation unit (34) to transport m material trays (23) on the lowest placement plate (10) again, and the steps are repeated until the number of the material trays (23) in the reaction chamber (2) is equal to the number of the spray heads (24);
then closing the first sealing connecting piece (18) and the second sealing connecting piece (19), opening the first vacuum system, the second vacuum system and the third vacuum system, vacuumizing the feeding chamber (1), the reaction chamber (2) and the discharging chamber (3) respectively, opening the first protective gas system, the second protective gas system and the third protective gas system, and filling protective gas into the feeding chamber (1), the reaction chamber (2) and the discharging chamber (3) to one atmosphere;
the second control unit opens the heating unit, the heating unit heats the reaction chamber (2), after the temperature rises to the temperature required by the growth of the carbon nano tube, the second control unit opens the air inlet valve, the carbon source gas and the carrier gas preheated to 500 ℃ are conveyed to each spray head (24), and the tail gas is discharged by the air outlet valve;
closing the air inlet valve after the growth time of the carbon nano tube is reached, and opening the first sealing connecting piece (18), the second sealing connecting piece (19), the third sealing connecting piece (31) and the fourth sealing connecting piece (32); the third control unit starts the third transport unit (36) to transport m material trays (23) on the second transport unit (25) to the uppermost placement plate (10) of the second placement unit (35), then simultaneously starts the second placement unit (35), the second transport unit (25) and the first transport unit (34), the second placement unit (35) operates to enable the other empty placement plate (10) to be placed at the uppermost position, the second transport unit (25) drives the material trays (23) to move by m a distance towards the discharge chamber (3), and the first transport unit (34) transports the m material trays (23) on the placement plate (10) at the lowermost position of the first placement unit (33) to the second transport unit (25), and the steps are repeated until all the material trays (23) filled with carbon nanotubes are transported to the discharge chamber (3);
repeating the steps until the discharging chamber (3) is full or all the material trays (23) in the feeding chamber (1) are transported out; opening a first protective gas system or a third protective gas system to pump out the protective gas in the feeding chamber (1) or the discharging chamber (3); then opening a door body on the feeding chamber (1) or the discharging chamber (3), and disassembling the first sealing connecting piece (18) or the fourth sealing connecting piece (32); the production can be continued by replacing the feeding chamber (1) filled with the material tray (23) or the empty discharging chamber (3).
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