Apparatus for synthesizing continuous carbon nanotube aggregate by heating reaction liquid assisted CVD

Abstract

The utility model provides a device for synthesizing continuous carbon nanotube aggregate by heating reaction liquid assisted CVD, which comprises an injection pump, a furnace tube, a tube furnace and a cylinder heating part, wherein the inside of the tube furnace is coaxially provided with the furnace tube, the left end of the furnace tube is in communication with a nozzle located outside the tube furnace, the side wall of the nozzle is in communication with the bottom end of a liquid inlet column, the liquid inlet column is in communication with the output end of a liquid delivery long tube, the input end of the liquid delivery long tube is in communication with the output end of a pump cylinder in the injection pump, the inside of the pump cylinder is provided with a piston which is in reciprocating sliding cooperation with the pump cylinder, the outside of the piston is connected with the inner end of a piston rod, the outer end of the piston rod extends to the outside of the pump cylinder, the side wall of the pump cylinder is wrapped with the cylinder heating part, and in application, excessive ferrocene is first put into carbon source, then heated to improve the solubility of ferrocene in the reaction liquid, and finally the obtained reaction liquid is input into the pump cylinder for heat preservation to participate in subsequent reaction. The design not only can make the solubility of ferrocene higher, but also has better synthesis effect.

Description

Technical Field

[0001] This invention relates to an apparatus for synthesizing continuous carbon nanotube aggregates, belonging to the field of carbon nanotube aggregate fabrication, and particularly to an apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating a reaction solution. Background Technology

[0002] In existing technologies, when synthesizing continuous carbon nanotube aggregates using CVD, ferrocene is used as a catalyst, alcohol or acetone as a carbon source, and thiophene as a catalyst promoter. In practice, the ferrocene catalyst and thiophene promoter are first dissolved in small organic molecules such as alcohol or acetone to obtain a mixed reaction liquid. This reaction liquid is then injected into a nozzle and carried by the carrier gas introduced into the nozzle, and then introduced into a high-temperature furnace tube for catalytic pyrolysis to synthesize continuous carbon nanotube aggregates.

[0003] However, in the existing technology, the solubility of ferrocene as a catalyst in small organic molecules is limited, which cannot reach the designed reaction ratio and can only reach a minimum solubility standard. This limits the yield and quality of carbon nanotube aggregates synthesized in the reaction, and consequently limits the synthesis efficiency, resulting in poor synthesis effect.

[0004] The information disclosed in this background section is intended only to enhance understanding of the overall background of this application and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0005] The purpose of this invention is to overcome the defects and problems of low ferrocene solubility and poor synthesis effect in the prior art, and to provide a device for the heated reaction liquid-assisted CVD synthesis of continuous carbon nanotube aggregates with high ferrocene solubility and better synthesis effect.

[0006] To achieve the above objectives, the technical solution of the present invention is: an apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction liquid, comprising an injection pump, a furnace tube, and a tubular furnace. The furnace tube is coaxially arranged inside the tubular furnace. The left end of the furnace tube is connected to the output end of a nozzle located outside the tubular furnace. The side of the nozzle is connected to the bottom end of the liquid inlet column. The top or side of the liquid inlet column is connected to the output end of a long inlet tube. The input end of the long inlet tube is connected to the output end of the pump barrel in the injection pump. A piston is provided inside the pump barrel for reciprocating sliding cooperation. The outer side of the piston is connected to the inner end of the piston rod, and the outer end of the piston rod extends to the outside of the pump barrel.

[0007] The side circumference of the pump cylinder is covered with a cylinder heating element, which is a semi-cylindrical structure with an open top.

[0008] The cylinder heating element includes a cylinder protective arc layer, a cylinder heating arc layer, and a cylinder heat-conducting arc layer wrapped sequentially from the outside to the inside. The cylinder heat-conducting arc layer is wrapped around the outer side of the pump cylinder. The cylinder protective arc layer, the cylinder heating arc layer, and the cylinder heat-conducting arc layer are all open at the top.

[0009] The cylindrical heating arc layer includes a cylindrical carbon nanotube membrane and cylindrical electrode one and cylindrical electrode two connected to its two ends. The cylindrical carbon nanotube membrane has a circular arc structure, and cylindrical electrode one and cylindrical electrode two are connected to the positive and negative terminals of the external circuit respectively.

[0010] The infusion tube is wrapped with a tube heating element or a tube insulation element.

[0011] The tube heating element is a semi-cylindrical structure with an open top, comprising a tube protective arc layer, a tube heating arc layer, and a tube heat-conducting arc layer wrapped sequentially from the outside to the inside. The tube heat-conducting arc layer is wrapped around the outer side of the infusion tube. The tube protective arc layer, the tube heating arc layer, and the tube heat-conducting arc layer are all open-top structures.

[0012] The tube heating arc layer includes a tube carbon nanotube membrane and a tube electrode 1 and a tube electrode 2 connected to its two ends. The tube carbon nanotube membrane has a circular arc structure, and the tube electrode 1 and the tube electrode 2 are connected to the positive and negative terminals of the external circuit respectively.

[0013] The device also includes a pump base, the top two ends of which are fixedly connected to the bottom of the front fixed platform and the rear fixed platform, respectively. The right side of the rear fixed platform is provided with a rear outer hole, a rear middle hole, and a rear inner hole in sequence. The left side of the front fixed platform is provided with a front outer hole, a front middle hole, and a front inner hole in sequence. The rear outer hole is connected to the front outer hole through a slide rail, and the rear inner hole is connected to the front inner hole through another slide rail. A screw parallel to both slide rails is provided between the two slide rails. The right end of the screw is located in the front middle hole, and the left end of the screw passes through the rear middle hole and is connected to the drive handle.

[0014] A middle sliding platform is provided between the front fixed platform and the rear fixed platform, which slides relative to each other along the top surface of the pump base. The middle sliding platform has two parallel holes, a middle-middle hole and a middle inner hole. A slide rail passes through each of the middle outer hole and the middle inner hole, and a screw passes through the middle-middle hole.

[0015] The right side of the sliding platform is connected to the outer end of the piston rod, and the top of the front fixed platform is connected to the pump cylinder.

[0016] The top of the front fixed platform has a front groove to embed the lower part of the cylinder heating element. A pressure rod hole is provided on the top of the front fixed platform near the front groove. The pressure rod hole is threaded to the lower part of the pressure rod. The upper part of the pressure rod is perpendicularly connected to the inner end of the pressure plate. The outer end of the pressure plate extends outward.

[0017] When the projection of the pressure plate on the front fixed platform is perpendicular to the central axis of the front groove, the outer end of the pressure plate crosses the top groove opening of the front groove.

[0018] A front clamping plate is provided on the left side of the front fixed platform. The top of the front clamping plate has a front clamping opening that is directly opposite to the front groove. The middle of the front clamping plate has a front outer plate hole, a front middle plate hole, and a front inner plate hole that correspond one-to-one with the front outer hole, the front middle hole, and the front inner hole. The front and rear ends of the front clamping plate are respectively connected to the inner end of the front clamping plate. The outer end of the front clamping plate has a front fork. A single front bolt is inserted into the middle of a single front fork. The bottom end of the front bolt is threaded to the forward bolt hole opened on the side of the front fixed platform. The outer end of the front bolt is connected to the middle of the front rotating plate. The projection of the front rotating plate on its corresponding front fork covers the front fork.

[0019] The front clamp plate slides relative to the slide rail and screw passing through it, and a front clamping gap is formed between the front clamp plate and the left side of the front fixed platform to connect with the pump cylinder.

[0020] A ring surface is circumferentially attached to the outer side of the left end of the pump cylinder, and the bottom of the ring surface is inserted into the front clamping gap.

[0021] A middle clamping plate is provided on the right side of the middle sliding table. The middle clamping plate has a middle outer clamping hole, a middle middle clamping hole, and a middle inner clamping hole in the middle, which correspond one-to-one with the middle outer hole, the middle middle hole, and the middle inner hole. The front and rear ends of the middle clamping plate are respectively connected to the inner end of the middle clamping plate. A middle fork is provided on the outer end of the middle clamping plate. A middle bolt is inserted into the middle of a single middle fork. The bottom end of the middle bolt is threaded to the middle bolt hole provided on the side of the middle sliding table. The outer end of the middle bolt is connected to the middle of the middle rotating plate. The projection of the middle rotating plate on its corresponding middle fork covers the middle fork.

[0022] The middle clamp plate slides relative to the slide rail and screw that pass through it, and a middle clamp gap is formed between the middle clamp plate and the right side of the middle sliding table to connect with the outer end of the piston rod.

[0023] A rod ring surface is circumferentially connected to the outer side of the outer end of the piston rod, and the bottom of the rod ring surface is inserted into the interior of the clamping gap.

[0024] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0025] 1. The present invention discloses an apparatus for the CVD synthesis of continuous carbon nanotube aggregates assisted by a heated reaction solution, comprising an injection pump, a furnace tube, and a tubular furnace. The furnace tube is coaxially arranged inside the tubular furnace. The left end of the furnace tube is connected to the output end of a nozzle located outside the tubular furnace. The side of the nozzle is connected to the bottom end of an inlet column. The top or side of the inlet column is connected to the output end of a long delivery tube. The input end of the long delivery tube is connected to the output end of the pump barrel in the injection pump. A piston is reciprocatingly sliding with the pump barrel. The outer side of the plug is connected to the inner end of the piston rod, and the outer end of the piston rod extends to the outside of the pump barrel. A barrel heating element is wrapped around the side of the pump barrel. This barrel heating element is a semi-cylindrical structure with an open top. In application, excess ferrocene is first placed in the carbon source and then heated to increase the solubility of ferrocene in the reaction liquid. The resulting reaction liquid is then input into the pump barrel, and the barrel heating element further heats the pump barrel to ensure the temperature inside the barrel, thereby maintaining the high solubility of ferrocene in the reaction liquid and improving the synthesis effect. Alternatively, the carbon source and excess ferrocene can be directly placed into the pump barrel, and then the barrel heating element can be used to directly increase the solubility of ferrocene, thereby obtaining a reaction liquid with high ferrocene solubility and improving the synthesis effect. Therefore, this invention enables higher ferrocene solubility and better synthesis results.

[0026] 2. In the apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction liquid of the present invention, the cylindrical heating element comprises a cylindrical protective arc layer, a cylindrical heating arc layer, and a cylindrical thermally conductive arc layer wrapped sequentially from the outside to the inside. The cylindrical thermally conductive arc layer wraps around the outer perimeter of the pump cylinder. The cylindrical protective arc layer, the cylindrical heating arc layer, and the cylindrical thermally conductive arc layer are all open-top structures. The cylindrical heating arc layer includes a cylindrical carbon nanotube membrane and a cylindrical electrode one and a cylindrical electrode two connected to its two ends. The cylindrical carbon nanotube membrane has a circular arc structure, and the cylindrical electrode one and the cylindrical electrode two are connected to the positive and negative terminals of an external circuit. In application, the external circuit containing the cylindrical electrode one and the cylindrical electrode two is first turned on to energize and heat the cylindrical carbon nanotube membrane. The generated heat will pass through the cylindrical thermally conductive arc layer. The heat is transferred to the pump barrel, thereby increasing the internal temperature of the pump barrel and ensuring a reaction liquid with high ferrocene solubility. Simultaneously, the carbon nanotube membrane in the barrel is made of carbon nanotubes, which not only simplifies operation and accelerates heating, but also allows the use of the final carbon nanotube aggregates, or even defective products, reducing manufacturing costs. Furthermore, the barrel heating element, defined as a semi-cylindrical structure with an open top, not only securely clamps the pump barrel, facilitating heat transfer, but also allows direct observation of the heating status of the liquid inside the barrel (if the liquid is overheated and boiling, it is detrimental to injection) and the injection progress from the top opening, improving controllability and thus enhancing the injection effect and synthesis effect (the effect of the subsequent tube heating element is similar to that of the barrel heating element). Therefore, this invention not only has a good heating effect and low manufacturing cost, but also strong controllability and good synthesis effect.

[0027] 3. In the apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction liquid of the present invention, the apparatus further includes a pump base and a front fixed platform, a middle sliding platform, and a rear fixed platform disposed thereon. The right side of the middle sliding platform is connected to the outer end of the piston rod, and the top of the front fixed platform is connected to the pump cylinder. In application, the drive handle is first rotated to drive the screw to rotate, so that the screw moves back and forth reciprocally, thereby driving the middle sliding platform to move back and forth reciprocally, and then driving the piston rod to move back and forth reciprocally inside the pump cylinder, so as to sequentially input the reaction liquid into the nozzle through the long infusion tube and the infusion column. The operation is very convenient. Moreover, when the middle sliding platform moves back and forth, its two ends slide along two slide rails, which can improve the stability of the movement and facilitate precise liquid delivery. Therefore, the present invention is not only easy to operate, but also has high precision.

[0028] 4. In the apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction liquid of the present invention, a front clamping plate is preferably provided on the left side of the front fixed stage, or / and a middle clamping plate is provided on the right side of the middle sliding stage, to form a front clamping gap and a middle clamping gap respectively, thereby clamping the cylinder annular surface on the pump barrel and the rod annular surface on the piston rod, thus facilitating the reciprocating motion of the middle sliding stage to deliver the reaction liquid. In addition, the width of the middle clamping gap and the width of the front clamping gap can be adjusted by the combination of the middle fork, the middle bolt, and the middle rotating plate, to adapt to cylinder annular surfaces and rod annular surfaces of different thicknesses, and even other fixing structures on the cylinder or piston rod, expanding the applicable range of the injection pump that the present invention can be used with, and facilitating the promotion and application of the present invention. Therefore, the present invention has strong adjustability and a wide range of applications. Attached Figure Description

[0029] Figure 1 This is a schematic diagram of the structure of the present invention.

[0030] Figure 2 yes Figure 1 A schematic diagram showing the connection between the nozzle and the tubular furnace.

[0031] Figure 3 yes Figure 2 A sectional view.

[0032] Figure 4 This is a schematic diagram of the structure of the injection pump in this invention.

[0033] Figure 5 This is a side view of the heating element in the cylinder of the present invention.

[0034] Figure 6 This is a schematic diagram showing the connection between the infusion tube and the tube heating element in this invention.

[0035] Figure 7This is a schematic diagram of the pump base in this invention.

[0036] Figure 8 This is a schematic diagram of the structure of the middle card plate and the front card plate in this invention.

[0037] Figure 9 This is a schematic diagram showing the relative positions of the rear fixed platform, the middle sliding platform, and the front fixed platform in this invention.

[0038] Figure 10 This is a schematic diagram of the conductivity of the carbon nanotube membrane in this invention.

[0039] In the diagram: 1. Tube furnace; 2. Furnace tube; 21. Nozzle; 211. Nozzle insulation layer; 22. Inlet column; 221. Column insulation layer; 3. Injection pump; 31. Pump barrel; 32. Piston; 33. Piston rod; 34. Barrel annular surface; 35. Rod annular surface; 4. Infusion tube; 5. Barrel heating element; 51. Barrel protective arc layer; 52. Barrel heating arc layer; 52. Barrel electrode 1; 522. Barrel carbon nanotube membrane; 523. Barrel electrode 2; 53. Barrel thermally conductive arc layer; 6. Tube heating element; 61. Tube protective arc layer; 62. Tube heating arc layer; 621. Tube electrode 1; 622. Tube carbon nanotube membrane; 623. Tube electrode 2; 63. Tube thermally conductive arc layer; 7. Rear fixed platform; 71. Rear outer hole; 72. Rear middle hole; 73. Rear inner hole; 8. Middle sliding platform; 80. Middle clamping gap; 81. Middle outer hole; 82. Middle middle hole; 83. Middle inner hole; Hole 83, middle clamping plate 84, middle outer clamping hole 841, middle middle clamping hole 842, middle inner clamping hole 843, middle clamping plate 85, middle fork 86, middle bolt 861, middle inlet bolt hole 862, middle rotating plate 863, middle clamping opening 87, front fixed platform 9, front clamping gap 90, front outer hole 91, front middle hole 92, front inner hole 93, front groove 94, top groove opening 941, pressure rod hole 95, pressure rod 951, pressure plate 952, front clamping plate 96, front outer plate hole 961, front middle plate hole 962, front inner plate hole 963, front clamping plate 97, front fork 971, front bolt 972, inlet bolt hole 973, front rotating plate 974, front clamping opening 964, pump base 10, slide rail 11, screw 12, drive handle 13, power supply 14, controller 15. Detailed Implementation

[0040] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0041] See Figure 1 — Figure 10An apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction liquid includes an injection pump 3, a furnace tube 2, and a tubular furnace 1. The furnace tube 2 is coaxially arranged inside the tubular furnace 1. The left end of the furnace tube 2 is connected to the output end of a nozzle 21 located outside the tubular furnace 1. The side of the nozzle 21 is connected to the bottom end of a liquid inlet column 22. The top or side of the liquid inlet column 22 is connected to the output end of a long inlet tube 4. The input end of the long inlet tube 4 is connected to the output end of a pump barrel 31 in the injection pump 3. A piston 32 is arranged inside the pump barrel 31 and reciprocates therewith. The outer side of the piston 32 is connected to the inner end of a piston rod 33. The outer end of the piston rod 33 extends to the outside of the pump barrel 31.

[0042] The pump cylinder 31 is surrounded by a cylinder heating element 5, which is a semi-cylindrical structure with an open top.

[0043] The cylinder heating element 5 includes a cylinder protective arc layer 51, a cylinder heating arc layer 52, and a cylinder heat-conducting arc layer 53 wrapped in layers from the outside to the inside. The cylinder heat-conducting arc layer 53 is wrapped around the outer side of the pump cylinder 31. The cylinder protective arc layer 51, the cylinder heating arc layer 52, and the cylinder heat-conducting arc layer 53 are all open-top structures.

[0044] The cylindrical heating arc layer 52 includes a cylindrical carbon nanotube membrane 522 and a cylindrical electrode 521 and a cylindrical electrode 523 connected to its two ends. The cylindrical carbon nanotube membrane 522 has an arc structure, and the cylindrical electrode 521 and the cylindrical electrode 523 are connected to the positive and negative terminals of the external circuit respectively.

[0045] The infusion tube 4 is wrapped with a tube heating element 6 or a tube insulation element.

[0046] The tube heating element 6 is a semi-cylindrical structure with an open top, including a tube protection arc layer 61, a tube heating arc layer 62, and a tube heat conduction arc layer 63 wrapped from the outside to the inside. The tube heat conduction arc layer 63 is wrapped around the outer side of the infusion tube 4. The tube protection arc layer 61, the tube heating arc layer 62, and the tube heat conduction arc layer 63 are all open-top structures.

[0047] The tube heating arc layer 62 includes a tube carbon nanotube film 622 and a tube electrode 621 and a tube electrode 623 connected to its two ends. The tube carbon nanotube film 622 has a circular arc structure, and the tube electrode 621 and the tube electrode 622 are connected to the positive and negative terminals of the external circuit respectively.

[0048] The device also includes a pump base 10, the top two ends of which are fixedly connected to the bottom of the front fixed platform 9 and the rear fixed platform 7 respectively. The right side of the rear fixed platform 7 is provided with a rear outer hole 71, a rear middle hole 72 and a rear inner hole 73 in sequence. The left side of the front fixed platform 9 is provided with a front outer hole 91, a front middle hole 92 and a front inner hole 93 in sequence. The rear outer hole 71 is connected to the front outer hole 91 through a slide rail 11, and the rear inner hole 73 is connected to the front inner hole 93 through another slide rail 11. A screw 12 parallel to both slide rails 11 is provided between the two slide rails 11. The right end of the screw 12 is located in the front middle hole 92, and the left end of the screw 12 passes through the rear middle hole 72 and is connected to the drive handle 13.

[0049] A middle sliding platform 8 is provided between the front fixed platform 9 and the rear fixed platform 7, which slides relative to each other along the top surface of the pump base 10. The middle sliding platform 8 has two parallel holes: a middle outer hole 81, a middle middle hole 82, and a middle inner hole 83. A slide rail 11 passes through each of the middle outer hole 81 and the middle inner hole 83, and a screw 12 passes through the middle middle hole 82.

[0050] The right side of the sliding platform 8 is connected to the outer end of the piston rod 33, and the top of the front fixed platform 9 is connected to the pump cylinder 31.

[0051] The top of the front fixed platform 9 is provided with a front groove 94 to embed the lower part of the cylinder heating element 5. The top of the front fixed platform 9 is provided with a pressure rod hole 95 near the front groove 94. The pressure rod hole 95 is threaded to the lower part of the pressure rod 951. The upper part of the pressure rod 951 is vertically connected to the inner end of the pressure plate 952. The outer end of the pressure plate 952 extends outward.

[0052] When the projection of the pressure plate 952 on the front fixed platform 9 is perpendicular to the central axis of the front groove 94, the outer end of the pressure plate 952 crosses the top groove opening 941 of the front groove 94.

[0053] A front clamping plate 96 is provided on the left side of the front fixed platform 9. The top of the front clamping plate 96 is provided with a front clamping opening 964 that is directly opposite to the front groove 94. The middle part of the front clamping plate 96 is provided with a front outer plate hole 961, a front middle plate hole 962, and a front inner plate hole 963, which correspond one-to-one with the front outer hole 91, the front middle hole 92, and the front inner hole 93. The front and rear ends of the front clamping plate 96 are respectively connected to the inner end of the front clamping plate 97. The outer end of the front clamping plate 97 is provided with a front fork 971. A single front bolt 972 is inserted into the middle of a single front fork 971. The bottom end of the front bolt 972 is threadedly connected to the forward bolt hole 973 provided on the side of the front fixed platform 9. The outer end of the front bolt 972 is connected to the middle of the front rotating plate 974. The projection of the front rotating plate 974 on its corresponding front fork 971 covers the front fork 971.

[0054] The front clamping plate 96 slides relative to the slide rail 11 and screw 12 that pass through it, and the front clamping plate 96 and the left side of the front fixed platform 9 are clamped together to form a front clamping gap 90 that is connected to the pump cylinder 31.

[0055] A ring surface 34 is circumferentially attached to the outer side of the left end of the pump cylinder 31, and the bottom of the ring surface 34 is inserted into the front clamping gap 90.

[0056] A middle clamping plate 84 is provided on the right side of the middle sliding table 8. The middle clamping plate 84 has a middle outer clamping hole 841, a middle middle clamping hole 842, and a middle inner clamping hole 843 in the middle, which correspond one-to-one with the middle outer hole 81, the middle middle hole 82, and the middle inner hole 83. The front and rear ends of the middle clamping plate 84 are respectively connected to the inner end of the middle clamping plate 85. A middle fork 86 is provided on the outer end of the middle clamping plate 85. A middle bolt 861 is inserted into the middle of a single middle fork 86. The bottom end of the middle bolt 861 is threaded to the middle bolt hole 862 provided on the side of the middle sliding table 8. The outer end of the middle bolt 861 is connected to the middle of the middle rotating plate 863. The projection of the middle rotating plate 863 on its corresponding middle fork 86 covers the middle fork 86.

[0057] The middle clamping plate 84 slides relative to the slide rail 11 and screw 12 that pass through it, and the middle clamping plate 84 and the right side of the middle sliding table 8 form a middle clamping gap 80 that connects to the outer end of the piston rod 33.

[0058] A rod ring surface 35 is circumferentially connected to the outer side of the outer end of the piston rod 33, and the bottom of the rod ring surface 35 is inserted into the interior of the clamping gap 80.

[0059] The principle of this invention is explained as follows:

[0060] See Figure 10 This figure illustrates the energization and heating of the cylinder heating element 5 in this invention (the tube heating element 6 is similar). As shown in the figure, when heating is required, the controller 15 first activates the circuit containing the power supply 14, cylinder electrode 521, cylinder electrode 523, and cylinder carbon nanotube membrane 522. The cylinder carbon nanotube membrane 522 acts as the energized heating element. After the circuit is activated, the cylinder carbon nanotube membrane 522 generates heat, which is then transferred to the pump cylinder 31 via the cylinder thermally conductive arc layer 53, thereby heating and maintaining the temperature of the reaction liquid. The controller 15 can not only control the on / off state of the circuit (like a switch), but also further control the magnitude of the current.

[0061] Example 1:

[0062] See Figure 1 — Figure 10An apparatus for the CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction solution includes an injection pump 3, a furnace tube 2, and a tubular furnace 1. The furnace tube 2 is coaxially arranged inside the tubular furnace 1. The left end of the furnace tube 2 is connected to the output end of a nozzle 21 located outside the tubular furnace 1. The side of the nozzle 21 is connected to the bottom end of a liquid inlet column 22. The top or side of the liquid inlet column 22 is connected to the output end of a long inlet tube 4. The input end of the long inlet tube 4 is connected to the output end of a pump barrel 31 in the injection pump 3. A piston 32 is disposed inside the pump barrel 31 and reciprocates therewith. The outer side of the piston 32 is connected to the inner end of a piston rod 33. The outer end of the piston rod 33 extends to the outside of the pump barrel 31. A cylinder heating element 5 is wrapped around the side of the pump barrel 31. The cylinder heating element 5 is a semi-cylindrical structure with an open top.

[0063] In application, the catalyst, auxiliary agent, and excess ferrocene are first added to a carbon source (such as any one of ethanol, acetone, ethylene glycol, n-hexane, benzene, toluene, xylene, diethyl ether, or acetic acid) to obtain a mixed liquid. Excess refers to the amount of ferrocene added exceeding its solubility at room temperature; for example, the solubility of ferrocene in ethanol is 2.3. Adding more than 2.3 wt.% ferrocene will cause excess ferrocene to precipitate in ethanol. The mixed liquid is then heated to increase the solubility of ferrocene in the carbon source. As the temperature rises, the amount of ferrocene dissolved in the carbon source gradually increases until the temperature before the carbon source boils is stopped (greater than or equal to 60℃, generally 60 to 80℃; therefore, any existing material for the pump cylinder 31 is suitable, such as plastic, glass, or metal). The temperature is then maintained at a constant level. At this point, the amount of ferrocene dissolved in the carbon source reaches its maximum, yielding a reaction liquid. This reaction liquid is then loaded into the pump cylinder 31, and the pump cylinder 31 is heated by the cylinder heating element 5 to maintain a constant temperature and prevent damage to the solubility of ferrocene in the reaction liquid. The reaction liquid is then sequentially fed through the long delivery tube 4, the inlet column 22, and finally into the nozzle 21 to participate in the CVD synthesis of continuous carbon nanotubes, thereby improving production efficiency.

[0064] The yield of synthesized carbon nanotubes increased by at least 100%, while the quality was also improved!

[0065] Example 2:

[0066] The basic content is the same as in Example 1, except that:

[0067] The cylinder heating element 5 includes a cylinder protective arc layer 51, a cylinder heating arc layer 52, and a cylinder heat-conducting arc layer 53, which are wrapped layer by layer from the outside to the inside. The cylinder heat-conducting arc layer 53 is wrapped around the outer side of the pump cylinder 31. The cylinder protective arc layer 51, the cylinder heating arc layer 52, and the cylinder heat-conducting arc layer 53 are all open at the top. The cylinder heating arc layer 52 includes a cylinder carbon nanotube membrane 522 and a cylinder electrode 521 and a cylinder electrode 523 connected to its two ends. The cylinder carbon nanotube membrane 522 is an arc structure, and the cylinder electrode 521 and the cylinder electrode 523 are connected to the positive and negative terminals of the external circuit respectively.

[0068] Example 3:

[0069] The basic content is the same as in Example 1, except that:

[0070] The infusion tube 4 is externally wrapped with a tube heating element 6 or a tube insulation element. Generally, the tube insulation element is sufficient for heat preservation, but for the best application effect, a tube heating element 6 can also be set to heat the tube for heat preservation.

[0071] The preferred tube heating element 6 is a semi-cylindrical structure with an open top, comprising a tube protective arc layer 61, a tube heating arc layer 62, and a tube heat-conducting arc layer 63 wrapped sequentially from the outside to the inside. The tube heat-conducting arc layer 63 is wrapped around the outer side of the infusion tube 4. The tube protective arc layer 61, the tube heating arc layer 62, and the tube heat-conducting arc layer 63 are all open-top structures. The tube heating arc layer 62 includes a carbon nanotube membrane 622 and a tube electrode 621 and a tube electrode 623 connected to its two ends. The carbon nanotube membrane 622 has an arc structure, and the tube electrode 621 and the tube electrode 622 are connected to the positive and negative terminals of the external circuit respectively.

[0072] Example 4:

[0073] The basic content is the same as in Example 1, except that:

[0074] The device also includes a pump base 10, the top two ends of which are fixedly connected to the bottom of the front fixed platform 9 and the rear fixed platform 7, respectively. The right side of the rear fixed platform 7 has a rear outer hole 71, a rear middle hole 72, and a rear inner hole 73 sequentially formed. The left side of the front fixed platform 9 has a front outer hole 91, a front middle hole 92, and a front inner hole 93 sequentially formed. The rear outer hole 71 is connected to the front outer hole 91 via a slide rail 11, and the rear inner hole 73 is connected to the front inner hole 93 via another slide rail 11. A screw 12 parallel to both slide rails 11 is provided between the two slide rails 11, with the right end of the screw 12 located at the front... Inside the central hole 92, the left end of the screw 12 passes through the rear central hole 72 and connects to the drive handle 13; between the front fixed platform 9 and the rear fixed platform 7, a central sliding platform 8 is provided that slides relative to each other along the top surface of the pump base 10. The interior of the central sliding platform 8 has two parallel central outer holes 81, a central middle hole 82, and a central inner hole 83. A slide rail 11 passes through each of the central outer holes 81 and the central inner hole 83, and a screw 12 passes through the central middle hole 82; the right side of the central sliding platform 8 is connected to the outer end of the piston rod 33, and the top of the front fixed platform 9 is connected to the pump cylinder 31.

[0075] Example 5:

[0076] The basic content is the same as in Example 4, except that:

[0077] The top of the front fixed platform 9 has a front groove 94 for embedding the lower part of the cylindrical heating element 5. The top of the front fixed platform 9 has a pressure rod hole 95 near the front groove 94. The pressure rod hole 95 is threaded to the lower part of the pressure rod 951. The upper part of the pressure rod 951 is perpendicularly connected to the inner end of the pressure plate 952. The outer end of the pressure plate 952 extends outward. When the projection of the pressure plate 952 on the front fixed platform 9 is perpendicular to the central axis of the front groove 94, the outer end of the pressure plate 952 crosses the top groove opening 941 of the front groove 94. A front clamping plate 96 is provided on the left side of the front fixing platform 9. The top of the front clamping plate 96 has a front clamping opening 964 that is directly opposite to the front groove 94. The middle part of the front clamping plate 96 has a front outer plate hole 961, a front middle plate hole 962, and a front inner plate hole 963, which correspond one-to-one with the front outer hole 91, the front middle hole 92, and the front inner hole 93. The front and rear ends of the front clamping plate 96 are respectively connected to the inner ends of the front clamping plate 97. The outer end of the front clamping plate 97 has a front fork 971, and a single front screw is inserted into each front fork 971. The bottom end of the front bolt 972 is threadedly connected to the forward bolt hole 973 on the side of the front fixed platform 9 at the middle of the bolt 972. The outer end of the front bolt 972 is connected to the middle of the front rotating plate 974. The projection of the front rotating plate 974 on its corresponding front fork 971 covers the front fork 971. The front clamping plate 96 slides relative to the slide rail 11 and screw 12 that pass through it. The front clamping plate 96 and the left side of the front fixed platform 9 form a front clamping gap 90 that is connected to the pump cylinder 31. A cylindrical annular surface 34 is circumferentially connected to the outer side of the left end of the pump cylinder 31. The bottom of the cylindrical annular surface 34 is inserted into the interior of the front clamping gap 90.

[0078] Example 6:

[0079] The basic content is the same as in Example 4, except that:

[0080] A central clamping plate 84 is provided on the right side of the sliding table 8. The central clamping plate 84 has an outer clamping hole 841, a middle clamping hole 842, and an inner clamping hole 843 in its center, corresponding one-to-one with the outer clamping hole 81, the middle clamping hole 82, and the inner clamping hole 83. The front and rear ends of the central clamping plate 84 are connected to the inner ends of a central locking plate 85. A central fork 86 is provided on the outer end of the central locking plate 85. A single central bolt 861 is inserted into the center of each central fork 86. The bottom end of the bolt 861 is threadedly connected to the central bolt hole 862 on the side of the central sliding table 8. The outer end of the central bolt 861 is connected to the middle part of the central transfer plate 863. The projection of the central transfer plate 863 on its corresponding central fork 86 covers the central fork 86. The central clamping plate 84 slides relative to the slide rail 11 and the screw 12 that pass through it. The central clamping plate 84 and the right side of the central sliding table 8 form a central clamping gap 80 that connects to the outer end of the piston rod 33. A rod ring surface 35 is circumferentially connected to the outer side of the outer end of the piston rod 33. The bottom of the rod ring surface 35 is inserted into the interior of the central clamping gap 80.

[0081] The above description is only a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiments. Any equivalent modifications or changes made by those skilled in the art based on the content disclosed in the present invention should be included within the scope of protection set forth in the claims.

Claims

1. An apparatus for the CVD synthesis of continuous carbon nanotube aggregates assisted by heating a reaction solution, characterized in that: The device includes an injection pump (3), a furnace tube (2) and a tubular furnace (1). The furnace tube (2) is coaxially arranged inside the tubular furnace (1). The left end of the furnace tube (2) is connected to the output end of a nozzle (21) located outside the tubular furnace (1). The side of the nozzle (21) is connected to the bottom end of an inlet column (22). The top or side of the inlet column (22) is connected to the output end of a long infusion tube (4). The input end of the long infusion tube (4) is connected to the output end of a pump barrel (31) in the injection pump (3). A piston (32) is provided inside the pump barrel (31) and reciprocates therewith. The outer side of the piston (32) is connected to the inner end of a piston rod (33). The outer end of the piston rod (33) extends to the outside of the pump barrel (31). The side of the pump cylinder (31) is covered with a cylinder heating element (5), which is a semi-cylindrical structure with an open top. The infusion tube (4) is wrapped with a tube heating element (6) or a tube insulation element; The device also includes a pump base (10), the top two ends of which are fixedly connected to the bottom of the front fixed platform (9) and the rear fixed platform (7), respectively. The right side of the rear fixed platform (7) is provided with a rear outer hole (71), a rear middle hole (72), and a rear inner hole (73). The left side of the front fixed platform (9) is provided with a front outer hole (91), a front middle hole (92), and a front inner hole (93). The rear outer hole (71) is connected to the front outer hole (91) through a slide rail (11), and the rear inner hole (73) is connected to the front inner hole (93) through another slide rail (11). A screw (12) is provided between the two slide rails (11) and parallel to them. The right end of the screw (12) is located in the front middle hole (92), and the left end of the screw (12) passes through the rear middle hole (72) and is connected to the drive handle (13). A middle sliding platform (8) is provided between the front fixed platform (9) and the rear fixed platform (7) for relative sliding along the top surface of the pump base (10). The middle sliding platform (8) has two parallel outer holes (81), a middle hole (82), and a middle inner hole (83). A slide rail (11) passes through each of the outer holes (81) and the middle inner hole (83), and a screw (12) passes through the middle hole (82). The right side of the middle sliding platform (8) is connected to the outer end of the piston rod (33), and the top of the front fixed platform (9) is connected to the pump cylinder (31). The top of the front fixing platform (9) is provided with a front groove (94) to embed the lower part of the cylinder heating element (5). A pressure rod hole (95) is provided on the top of the front fixing platform (9) near the front groove (94). The pressure rod hole (95) is threaded to the lower part of the pressure rod (951). The upper part of the pressure rod (951) is vertically connected to the inner end of the pressure plate (952). The outer end of the pressure plate (952) extends outward. When the projection of the pressure plate (952) on the front fixed platform (9) is perpendicular to the central axis of the front groove (94), the outer end of the pressure plate (952) crosses the top groove opening (941) of the front groove (94). A front clamping plate (96) is provided on the left side of the front fixing platform (9). The top of the front clamping plate (96) is provided with a front clamping opening (964) that is directly opposite to the front groove (94). The middle part of the front clamping plate (96) is provided with a front outer plate hole (961), a front middle plate hole (962), and a front inner plate hole (963) that correspond one-to-one with the front outer hole (91), the front middle hole (92), and the front inner hole (93). The front and rear ends of the front clamping plate (96) are respectively connected to the inner ends of the front clamping plate (97). The front fork (971) is opened at the outer end of the front plate (97). A single front bolt (972) is inserted into the middle of each front fork (971). The bottom end of the front bolt (972) is threaded to the forward bolt hole (973) opened on the side of the front fixed platform (9). The outer end of the front bolt (972) is connected to the middle of the front rotating plate (974). The projection of the front rotating plate (974) on its corresponding front fork (971) covers the front fork (971). The front clamp (96) slides relative to the slide rail (11) and screw (12) that pass through it, and the front clamp (96) and the left side of the front fixed platform (9) are clamped together to form a front clamp gap (90) that is connected to the pump cylinder (31). A cylindrical annular surface (34) is circumferentially attached to the outer side of the left end of the pump cylinder (31), and the bottom of the cylindrical annular surface (34) is inserted into the interior of the front clamping gap (90).

2. The apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction solution according to claim 1, characterized in that: The cylinder heating element (5) includes a cylinder protective arc layer (51), a cylinder heating arc layer (52), and a cylinder heat-conducting arc layer (53) wrapped from the outside to the inside. The cylinder heat-conducting arc layer (53) is wrapped around the outer side of the pump cylinder (31). The cylinder protective arc layer (51), the cylinder heating arc layer (52), and the cylinder heat-conducting arc layer (53) are all open at the top. The cylindrical heating arc layer (52) includes a cylindrical carbon nanotube membrane (522) and a cylindrical electrode (521) and a cylindrical electrode (523) connected to its two ends. The cylindrical carbon nanotube membrane (522) has a circular arc structure, and the cylindrical electrode (521) and the cylindrical electrode (523) are connected to the positive and negative terminals of the external circuit respectively.

3. The apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction solution according to claim 1, characterized in that: The tube heating element (6) is a semi-cylindrical structure with an open top, including a tube protection arc layer (61), a tube heating arc layer (62), and a tube heat conduction arc layer (63) wrapped layer by layer from the outside to the inside. The tube heat conduction arc layer (63) is wrapped around the outer side of the infusion tube (4). The tube protection arc layer (61), the tube heating arc layer (62), and the tube heat conduction arc layer (63) are all open-top structures. The tube heating arc layer (62) includes a tube carbon nanotube film (622) and a tube electrode (621) and a tube electrode (623) connected to its two ends. The tube carbon nanotube film (622) has a circular arc structure, and the tube electrode (621) and the tube electrode (622) are connected to the positive and negative terminals of the external circuit respectively.

4. The apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction solution according to claim 1, characterized in that: A middle clamping plate (84) is provided on the right side of the middle sliding table (8). The middle clamping plate (84) has a middle outer clamping hole (841), a middle middle clamping hole (842), and a middle inner clamping hole (843) in the middle to correspond one-to-one with the middle outer hole (81), the middle middle hole (82), and the middle inner hole (83). The front and rear ends of the middle clamping plate (84) are respectively connected to the inner end of the middle clamping plate (85). A middle fork (86) is opened on the outer end of the middle clamping plate (85). A middle bolt (861) is inserted into the middle of a single middle fork (86). The bottom end of the middle bolt (861) is threaded to the middle bolt hole (862) opened on the side of the middle sliding table (8). The outer end of the middle bolt (861) is connected to the middle of the middle rotating plate (863). The projection of the middle rotating plate (863) on its corresponding middle fork (86) covers the middle fork (86). The middle clamping plate (84) slides relative to the slide rail (11) and screw (12) that pass through it. The middle clamping plate (84) and the right side of the middle sliding table (8) are clamped together to form a middle clamping gap (80) that connects to the outer end of the piston rod (33).

5. The apparatus for CVD synthesis of continuous carbon nanotube aggregates assisted by heating reaction solution according to claim 4, characterized in that: A rod ring surface (35) is circumferentially attached to the outer side of the outer end of the piston rod (33), and the bottom of the rod ring surface (35) is inserted into the interior of the clamping gap (80).

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