Preparation device of single-walled carbon nanotube

Abstract

The utility model discloses a preparation device of a single-walled carbon nanotube, and relates to the field of reaction devices, a reaction furnace tube is vertically placed, a gas-liquid feed pipe is arranged at the lower end of the reaction furnace tube, a material receiving tank is arranged at the upper end of the reaction furnace tube, a valve is arranged at the discharge end of the material receiving tank, and a material receiving shovel is movably arranged at the outlet end of the valve through a control mechanism. Therefore, the single-walled carbon nanotubes are generated in the receiving tank at the top in a bottom feeding and floating catalysis manner, so that the pollution of carbon impurities is avoided, the high-purity growth of the single-walled carbon nanotubes is realized, and the yield of high-quality single-walled carbon nanotubes is improved. And the material receiving tank is provided with a valve, a material receiving shovel and a control mechanism, so that sampling and quality detection can be carried out on the single-walled carbon nanotubes at any time more easily.

Description

Technical Field

[0001] The utility model relates to the field of reaction devices, in particular to a preparation device for single-walled carbon nanotubes. Background Art

[0002] Single-walled carbon nanotubes are nanotube-like structures composed of a layer of carbon atoms arranged in a spiral form. They have a high specific surface area, good electrical conductivity and mechanical strength, and therefore have broad application prospects in the field of nanotechnology. The methods for preparing single-walled carbon nanotubes mainly include chemical vapor deposition and arc discharge. Chemical vapor deposition uses the interaction between carbon atoms and metal catalysts at high temperatures to synthesize carbon nanotubes.

[0003] Chemical vapor deposition is a method in which an iron source catalyst is introduced into a reaction chamber through a feed pipe under atmospheric conditions to carry out a chemical reaction with one or more precursors of the desired material, and finally the desired thin film material is deposited on the surface of the substrate. Specifically, in the chemical vapor deposition process, metal catalysts such as nickel or iron are usually used to promote the conversion of reducing gases. First, metal catalyst particles are deposited on the substrate, and then the reducing gas is introduced into the reaction chamber and decomposed. Under the action of the catalyst, the generated carbon molecules are adsorbed and rearranged on the surface of the metal catalyst particles to form single-walled carbon nanotubes. This method can effectively prepare carbon nanotubes and has broad application prospects.

[0004] At present, there are two main devices for preparing single-walled carbon nanotubes by chemical vapor deposition, namely the top feeding device and the tubular furnace lateral feeding device. The tubular furnace lateral feeding device may be heated unevenly during the feeding process, thus affecting the heat conduction and reaction effect in the furnace. In addition, the gas is more likely to disperse to both ends, resulting in poor sample quality and difficulty in collection. The top feeding device is more common in the field of single-walled carbon nanotube preparation. During the preparation process, due to the low density of hydrogen, it is easy to stay at the top, which not only easily leads to unstable airflow in the furnace, but also makes it difficult for the sample at the bottom to contact with hydrogen during the deposition process, resulting in low yield and poor quality of carbon nanotubes. In addition, the bottom is prone to carbon impurities, and the prepared high-quality carbon nanotubes are easily contaminated by carbon impurities, further resulting in low yield, poor quality and difficulty in collection of high-quality single-walled carbon nanotubes. Summary of the invention

[0005] The purpose of the utility model is to provide a single-walled carbon nanotube preparation device, and its purpose is mainly to overcome the above-mentioned problems existing in the prior art.

[0006] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0007] A preparation device for single-walled carbon nanotubes comprises a material receiving tank, a reaction furnace tube and a gas-liquid feeding pipe. The reaction furnace tube is placed vertically, and the gas-liquid feeding pipe is arranged at the lower end thereof; the gas inlet end of the gas-liquid feeding pipe is connected with gas delivery pipe three and gas delivery pipe one, the liquid inlet end is connected with a syringe injector and is equipped with a syringe pump, and the liquid outlet end is provided with an atomizer; the feeding end of the material receiving tank is connected to the upper end of the reaction furnace tube, the gas inlet end is connected with gas delivery pipe two, and the material outlet end is provided with a valve.

[0008] Furthermore, the material receiving tank is provided with a visual window.

[0009] Furthermore, it also includes steel cylinder 2 and steel cylinder 1; the above-mentioned gas pipe 1 and gas pipe 2 are connected to steel cylinder 1, and the above-mentioned gas pipe 3 is connected to steel cylinder 2.

[0010] Furthermore, it also includes a material collecting shovel and a control mechanism, and the material collecting shovel is movably arranged at the outlet end of the valve through the control mechanism.

[0011] Furthermore, the control mechanism includes an image acquisition unit, a control unit, a motor and a rack, the output shaft of the motor is connected to the rack through a gear transmission, and the material collecting shovel is fixed to one end of the rack; the image acquisition unit faces the visual window of the material collecting tank; the valve is an electrically controlled valve, and the electrically controlled valve, the image acquisition unit and the motor are all electrically connected to the control unit;

[0012] The control unit is used to open the valve and start the motor according to the image acquisition situation of the image acquisition unit, so as to transfer the single-walled carbon nanotubes inside the receiving tank to the receiving shovel.

[0013] Furthermore, it also includes a broadcasting unit, which is electrically connected to the control unit.

[0014] Compared with the prior art, the beneficial effects of the utility model are:

[0015] First, the utility model adopts bottom feeding and generates single-walled carbon nanotubes in a top receiving tank in a floating catalytic manner, which can improve the stability of the intake air flow, avoid the pollution of carbon impurities, achieve high-purity growth of single-walled carbon nanotubes, and increase the output of high-quality single-walled carbon nanotubes.

[0016] Secondly, the utility model adopts bottom feeding, and the receiving tank is equipped with valves, a receiving shovel and a control mechanism, which makes it easier to sample and detect the quality of the single-walled carbon nanotubes at any time, and avoids the single-walled carbon nanotubes from being carbonized for too long in the receiving tank, and being converted into carbon impurities such as graphite and carbon black, thereby reducing the purity of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a simple structural schematic diagram of the utility model.

[0018] Figure 2 for Figure 1 A partial enlarged schematic diagram of part A. DETAILED DESCRIPTION

[0019] The specific implementation of the present invention is described below with reference to the accompanying drawings. In order to fully understand the present invention, many details are described below, but for those skilled in the art, the present invention can be implemented without these details.

[0020] like Figure 1 and Figure 2 As shown, a single-walled carbon nanotube preparation device includes a material receiving tank 1, a reaction furnace tube 2 and a gas-liquid feed pipe 3, which are all common components of existing carbon nanotube preparation devices, and their specific structures are not repeated here. Among them, the reaction furnace tube 2 is placed vertically, and the lower end of the reaction furnace tube 2 is supported and fixed by a base 21. The lower end of the reaction furnace tube 2 is provided with a gas-liquid feed pipe 3, and the upper end is connected to the feed end 12 of the material receiving tank 1.

[0021] like Figure 1 and Figure 2 As shown, the lower end of the gas-liquid feed pipe 3 extends to the outside of the reaction furnace tube 2, and is provided with an air inlet end 31 and a liquid inlet end 32; the upper end of the gas-liquid feed pipe 3 extends to the inside of the reaction furnace tube 2, and is provided with a gas outlet end and a liquid outlet end. Among them, the gas inlet end 31 of the gas-liquid feed pipe 3 is connected with a gas delivery pipe 3 81 and a gas delivery pipe 1 71. And the gas delivery pipe 3 81 is connected to a steel cylinder 2 8 for storing reducing gas, and the gas delivery pipe 1 71 is connected to a steel cylinder 1 7 for storing protective gas. The liquid inlet end 32 of the gas-liquid feed pipe 3 is connected with a syringe injector 5 for storing the precursor solution, and is equipped with an injection pump 6 for controlling the injection speed of the syringe injector 5. The liquid outlet end 33 of the gas-liquid feed pipe 3 is provided with an atomizer 9.

[0022] like Figure 1 and Figure 2 As shown, the syringe 5 and the injection pump 6 are common components of the existing carbon nanotube preparation device, and their specific structures are not repeated here. The atomizer 9 includes but is not limited to the existing atomizing nozzle.

[0023] like Figure 1 and Figure 2 As shown, the receiving tank 1 is provided with a visual window 10 to facilitate observation of the single-walled carbon nanotubes inside the receiving tank 1 and prevent the single-walled carbon nanotubes from clogging the feed end 12 .

[0024] like Figure 1 and Figure 2As shown, the air inlet end 11 of the receiving tank 1 is connected to the cylinder 1 7 through the air delivery pipe 2 72. The discharge end 13 of the receiving tank 1 is provided with a valve 42. The valve 42 includes but is not limited to an existing electric control valve, such as an electric control ball valve. Of course, the receiving tank 1 is also provided with an exhaust end (not shown in the figure) to facilitate the discharge of exhaust gas. The exhaust end can be arranged at the bottom of the receiving tank 1 and is located beside the feed end 12.

[0025] like Figure 1 and Figure 2 As shown, as a preferred embodiment, the gas delivery pipe 3 81, the gas delivery pipe 1 71 and the gas delivery pipe 2 72 are all equipped with a gas flow meter 100. The receiving tank 1 is equipped with a pressure gauge 14 to facilitate monitoring the pressure of the receiving tank 1.

[0026] like Figure 1 and Figure 2 As shown, the general method of using the single-walled carbon nanotube preparation device is as follows:

[0027] The precursor solution in the syringe 5 is injected into the reaction furnace tube 2 through the atomizer 9 by the injection pump 6, and the protective gas in the cylinder 1 7 and the reducing gas in the cylinder 2 8 are injected into the reaction furnace tube 2; a high-temperature reaction is carried out in the reaction furnace tube 2, and single-walled carbon nanotubes are generated on the substrate surface inside the receiving tank 1. The single-walled carbon nanotubes are in an aerogel state when they are produced, and adhere to the collection tank 1 and the upper part of the feed end 12 in the form of a mass. When the valve 42 is opened to sample the single-walled carbon nanotubes, protective gas is introduced into the receiving tank 1 through the gas pipe 2 72 to prevent methane from directly contacting the air and burning or even exploding, and the ventilation flow is strictly controlled by the pressure gauge 14 and the gas flow meter 100.

[0028] The structure of the utility model of feeding at the bottom and depositing single-walled carbon nanotubes at the top avoids the pollution of carbon impurities, realizes the high-purity growth of single-walled carbon nanotubes, and improves the yield of high-quality single-walled carbon nanotubes. Based on the structure of the utility model of feeding at the bottom and depositing single-walled carbon nanotubes at the top, combined with the control of the catalyst composition, reaction conditions and deposition time during the preparation process, the yield of high-quality single-walled carbon nanotubes can be better improved.

[0029] like Figure 1 and Figure 2 As shown, the single-walled carbon nanotube preparation device further includes a collecting shovel 44 and a control mechanism, and the collecting shovel 44 is movably arranged at the side of the valve 42 toward the inside of the collecting tank 1 through the control mechanism. It should be noted that the bottom plate of the collecting shovel 44 is in the form of a thin sheet, and the shape is adapted to the inner wall of the collecting tank 1, so that the bottom plate of the collecting shovel 44 can move along the inner wall of the collecting tank 1, thereby better scraping the single-walled carbon nanotubes inside the collecting tank 1.

[0030] like Figure 1 and Figure 2 As shown, in a specific embodiment, the control mechanism includes a motor 43 and a rack 422. The output shaft of the motor 43 is connected to the rack 422 through a gear 431, and the material collecting shovel 44 is fixed to one end of the rack 422, so that the material collecting shovel 44 can be movably arranged beside the valve 42.

[0031] like Figure 1 and Figure 2 As shown, as a preference, the control mechanism further includes an image acquisition unit 41 and a control unit 40. The lens of the image acquisition unit 41 faces the visual window 10 of the material receiving tank 1; the electric control valve, the image acquisition unit 41 and the motor 43 are all electrically connected to the control unit 40. The control unit 40 is used to open the valve 42 and start the motor 43 according to the image acquisition situation of the image acquisition unit 41, so as to transfer the single-walled carbon nanotubes inside the material receiving tank 1 to the material receiving shovel 44 to realize automatic material collection. The image acquisition unit 41 includes but is not limited to a CCD camera.

[0032] like Figure 1 and Figure 2 As shown, the general working principle of the control mechanism is further explained:

[0033] The control unit 40 mainly includes a control module and an image processing module. The image acquisition unit 41 acquires images of the inside of the material receiving tank 1 through the visual window 10, and transmits the image acquisition data to the control unit 40. The image processing module processes and analyzes the image acquisition data. If there are more single-walled carbon nanotubes deposited inside the material receiving tank 1 (such as the distribution density of single-walled carbon nanotubes exceeds the preset value), the control module starts the motor 43, opens the valve 42, and moves the material receiving shovel 44 to the inner wall of the material receiving tank 1 through the valve 42, scrapes the wall carbon nanotubes inside the material receiving shovel 44, and realizes automatic sampling of single-walled carbon nanotubes. After the sampling is completed, the control unit 40 resets the material receiving shovel 44 and the valve 42.

[0034] like Figure 1 and Figure 2 As shown, the above-mentioned control mechanism also includes a broadcast unit 45, which is electrically connected to the control unit 40. The broadcast unit 45 includes but is not limited to a speaker, and is mainly used to broadcast information related to the working status of the preparation device, so that the staff can understand the working status of the preparation device in time.

[0035] The above is only a specific implementation method of the utility model, but the design concept of the utility model is not limited to this. Any non-substantial changes to the utility model using this concept shall be deemed as an infringement of the protection scope of the utility model.

Claims

1. A single-walled carbon nanotube preparation device, comprising a material receiving tank (1), a reaction furnace tube (2) and a gas-liquid feeding tube (3), characterized in that: The reaction furnace tube (2) is placed vertically, and the gas-liquid feed pipe (3) is arranged at its lower end; the gas inlet end (31) of the gas-liquid feed pipe (3) is connected to the gas delivery pipe three (81) and the gas delivery pipe one (71), the liquid inlet end (32) is connected to the syringe injector (5) and is equipped with a syringe pump (6), and the liquid outlet end (33) is provided with an atomizer (9); the feed end (11) of the material receiving tank (1) is connected to the upper end of the reaction furnace tube (2), the gas inlet end (12) is connected to the gas delivery pipe two (72), and the discharge end (13) is provided with a valve (42).

2. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: The material receiving tank (1) is provided with a visual window (10).

3. The single-walled carbon nanotube preparation device according to claim 1, characterized in that: It also includes a second steel cylinder (8) and a first steel cylinder (7); the first gas pipe (71) and the second gas pipe (72) are connected to the first steel cylinder (7), and the third gas pipe (81) is connected to the second steel cylinder (8).

4. A single-walled carbon nanotube preparation device according to any one of claims 1 to 3, characterized in that: It also includes a material collecting shovel (44) and a control mechanism, wherein the material collecting shovel (44) is movably arranged at the outlet end of the valve (42) through the control mechanism.

5. The device for preparing single-walled carbon nanotubes according to claim 4, characterized in that: The control mechanism comprises an image acquisition unit (41), a control unit (40), a motor (43) and a rack (422); the output shaft of the motor (43) is connected to the rack (422) through a gear (431); the material collecting shovel (44) is fixedly arranged at one end of the rack (422); the image acquisition unit (41) faces a visual window (10) of the material collecting tank (1); the valve (42) is an electrically controlled valve, and the electrically controlled valve, the image acquisition unit (41) and the motor (43) are all electrically connected to the control unit (40); The control unit (40) is used to open the valve (42) and start the motor (43) according to the image acquisition situation of the image acquisition unit (41), so as to transfer the single-walled carbon nanotubes inside the reaction furnace tube (2) to the receiving shovel (44).

6. The device for preparing single-walled carbon nanotubes according to claim 5, characterized in that: It also includes a broadcasting unit (45), which is electrically connected to the control unit (40).

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