Three-temperature calcination preparation device for experimental carbon nanotube material
By designing a three-temperature calcination preparation device for experimental carbon nanotube materials that can perform carbon nanotube preparation experiments under multiple different temperatures or multiple different carbon source conditions at the same time, the problem that existing equipment cannot perform multi-condition experiments at the same time is solved, and efficient carbon nanotube preparation experiments are achieved.
Patent Information
- Application Number
- CN202520278468.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-21
- Publication Date
- 2025-05-09
- Estimated Expiration
- 2035-02-21
AI Technical Summary
Existing laboratory equipment cannot simultaneously conduct carbon nanotube preparation experiments under multiple different temperatures or multiple different carbon source conditions, which greatly affects the experimental efficiency.
A three-temperature calcination preparation device for experimental carbon nanotube materials can be designed, which can simultaneously perform calcination under three different temperatures or three different carbon source conditions. The device includes three side-by-side calcining chambers, each with a quartz tube and heating assembly, and multiple conditions are achieved simultaneously control through the PLC control panel.
This device can greatly improve the experimental efficiency of carbon nanotube preparation, shorten the cooling time, simplify the experimental process, and improve the flexibility and efficiency of the experiment.
Smart Images
Figure CN222849764U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the field of carbon nanotube preparation equipment, in particular to a three-temperature calcination preparation device for experimental carbon nanotube materials. Background Art
[0002] Faced with increasingly severe global climate and energy issues, the demand for new energy storage / conversion materials continues to increase. Carbon nanotubes (CNTs) have shown great application potential due to their unique structure, excellent mechanical properties, electrical conductivity, thermal conductivity, chemical stability and flexibility, and are expected to play a key role in mechanical energy storage and electrochemical energy storage.
[0003] Carbon nanotubes are composed of carbon atoms sp 2 Hybrid mainly, mixed with sp 3 The ideal structure formed by hybridization, carbon nanotubes can be regarded as a "cylinder" rolled up by sheet graphene skin, so it must have many excellent intrinsic characteristics of graphite. Carbon nanotubes have excellent performance due to their unique structure. It has extremely high mechanical strength and ideal elasticity, and its Young's modulus is equivalent to that of diamond, about 1TPa, which is about 5 times that of steel. The excellent properties of carbon nanotubes make their application prospects broad, but the realization of mass production of carbon nanotubes is still the focus of research.
[0004] When preparing carbon nanotubes by chemical vapor deposition, the carbon sources that can be used include methane, propylene, liquefied gas, etc., and the catalysts that can be used include nickel-based catalysts, iron-molybdenum catalysts, etc., and they are generally prepared by calcination in a tubular furnace. Studies have shown that the carbon source, catalyst and calcination temperature have an important influence on the morphological characteristics, number of tube wall layers, tube diameter distribution and specific surface area of carbon nanotube products. Therefore, in the experimental process of carbon nanotube preparation, in order to seek the best carbon source, catalyst, calcination temperature and other factors, it is necessary to conduct experiments with different carbon sources, different catalysts and different calcination temperatures. However, the tubular furnace currently used in the laboratory is usually a single quartz tube, which cannot simultaneously carry out carbon nanotube preparation experiments under multiple calcination temperatures or multiple carbon source conditions, which greatly affects the experimental efficiency. Utility Model Content
[0005] The purpose of the utility model is to provide a three-temperature calcination preparation device for experimental carbon nanotube materials in view of the shortcomings of the prior art in the above-mentioned background technology, which can simultaneously carry out calcination preparation experiments of carbon nanotubes under three different temperatures or three different carbon source conditions.
[0006] In order to achieve the above purpose, the technical solution adopted by the utility model is as follows:
[0007] The utility model provides a three-temperature calcination preparation device for experimental carbon nanotube materials, comprising an upper shell and a lower shell which are sealed and connected to each other, a sealed cavity is formed between the upper shell and the lower shell, a first partition is arranged in the sealed cavity, the first partition divides the sealed cavity into a heating cavity and a cooling cavity, a second partition and a third partition are arranged in the heating cavity, the second partition and the third partition divide the heating cavity into three calcination chambers arranged side by side, a quartz tube and a group of heating components are arranged in each calcination chamber, and the heating components are fixed on the first partition;
[0008] Three quartz tubes are arranged side by side and located between the upper shell and the lower shell. Two ends of the quartz tubes are respectively passed through the sealed cavity and fixedly connected to the first flange and the second flange. The first flange on each quartz tube is fixedly connected to the first cover, and the second flange on each quartz tube is fixedly connected to the second cover.
[0009] The first cover is provided with three carbon source gas inlets, and the second cover is provided with three exhaust ports. The three carbon source gas inlets and the three exhaust ports are connected to the three quartz tubes in a one-to-one correspondence.
[0010] Furthermore, a pull rod is arranged coaxially in the quartz tube, one end of the pull rod is connected to the quartz boat, and the other end of the pull rod slides out and passes through the first cover.
[0011] Furthermore, the heating assembly includes an upper heating element and a lower heating element, the quartz tube is located between the upper heating element and the lower heating element, and the upper heating element and the lower heating element are both inserted from the cooling cavity into the heating cavity.
[0012] Preferably, the upper heating element and the lower heating element are both made of U-shaped silicon molybdenum rods.
[0013] Furthermore, the calcination chamber is also provided with an upper insulation layer and a lower insulation layer, the upper insulation layer is fixed to the inner wall of the upper shell, and the lower insulation layer is fixed to the inner wall of the lower shell. The upper heating element, the lower heating element and the quartz tube are all located in the calcination cavity surrounded by the upper insulation layer and the lower insulation layer.
[0014] Furthermore, a protection box is provided on the outer side of the installation end of the heating component, and the protection box is fixed on the first partition plate at one side of the cooling chamber.
[0015] Furthermore, a cooling medium inlet and a cooling medium outlet are symmetrically arranged on the side wall of the upper shell, and the cooling medium inlet and the cooling medium outlet are both connected to the cooling cavity.
[0016] Furthermore, a first solenoid valve is provided on the carbon source gas inlet, and a second solenoid valve is provided on the cooling medium inlet. The first solenoid valve, the second solenoid valve, the upper heating element, and the lower heating element are all electrically connected to a PLC control panel fixedly installed on the outer wall of the upper shell.
[0017] Furthermore, three temperature transmitters are provided on the top of the upper shell, the three temperature transmitters correspond to the three quartz tubes one by one, the lower ends of the temperature transmitters extend into the calcining chamber, and the temperature transmitters are electrically connected to the PLC control panel.
[0018] Compared with the prior art, the beneficial technical effects of the utility model are:
[0019] 1. The three-temperature calcination preparation device for experimental carbon nanotube materials of the utility model can simultaneously carry out calcination preparation experiments of carbon nanotubes under three different temperatures or three different carbon source conditions, which greatly improves the experimental efficiency of carbon nanotube preparation.
[0020] 2. The three-temperature calcination preparation device for experimental carbon nanotube materials of the utility model introduces cooling medium through the cooling medium inlet, actively cools down the carbon nanotube materials in the quartz tube and the quartz boat inside it, shortens the cooling time, and further improves the experimental efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 It is a three-dimensional diagram of a three-temperature calcination preparation device for an experimental carbon nanotube material of the utility model;
[0022] Figure 2 This is a left view of a three-temperature calcination preparation device for an experimental carbon nanotube material of the utility model;
[0023] Figure 3 It is a right view of a three-temperature calcination preparation device for experimental carbon nanotube materials of the utility model;
[0024] Figure 4 It is a top view of a three-temperature calcination preparation device for an experimental carbon nanotube material of the utility model;
[0025] Figure 5 for Figure 4 Middle AA section view;
[0026] Figure 6 for Figure 4 Middle BB section view;
[0027] Figure 7 This is a rear view of a three-temperature calcination preparation device for an experimental carbon nanotube material of the utility model;
[0028] Figure 8 This is a front view of a three-temperature calcination preparation device for experimental carbon nanotube materials of the utility model;
[0029] Fig. 9 for Figure 8 Middle CC section view;
[0030] Fig.10 for Figure 8 Middle DD section view;
[0031] Figure markings: 1-upper shell, 2-lower shell, 3-first partition, 4-second partition, 5-third partition, 6-quartz tube, 7-first flange, 8-second flange, 9-first cover, 10-second cover, 11-quartz boat, 12-pull rod, 13-upper heating element, 14-lower heating element, 15-upper insulation layer, 16-lower insulation layer, 17-carbon source gas inlet, 18-exhaust port, 19-first solenoid valve, 20-cooling medium inlet, 21-cooling medium outlet, 22-second solenoid valve, 23-protective box, 24-temperature transmitter sensor, 25-PLC control panel. DETAILED DESCRIPTION
[0032] In order to make the purpose, technical solution and advantages of the utility model more clear, the utility model is further described in detail in combination with the embodiments below. It should be understood that the specific embodiments described here are only used to explain the utility model, and are not used to limit the utility model.
[0033] In the description of the present utility model, it should be understood that the terms "center", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the present application. The terms "first" and "second" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of the present utility model, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined. It should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", and "set" should be understood in a broad sense, for example, they can be fixedly connected or set, or detachably connected or set, or integrally connected or set, they can be directly connected, or indirectly connected through an intermediate medium, or they can be internally connected between two components. For ordinary technicians in this field, the specific meanings of the above terms in this utility model can be understood according to specific circumstances.
[0034] Example
[0035] like Figure 1-10As shown, the present embodiment provides a three-temperature calcination preparation device for experimental carbon nanotube materials, comprising an upper shell 1 and a lower shell 2 which are sealed and connected to each other, a sealed cavity is formed between the upper shell 1 and the lower shell 2, a first partition 3 is arranged in the sealed cavity, the first partition 3 divides the sealed cavity into a heating cavity and a cooling cavity, a second partition 4 and a third partition 5 are arranged in the heating cavity, the second partition 4 and the third partition 5 divide the heating cavity into three calcination chambers arranged side by side, a quartz tube 6 and a group of heating components are arranged in each calcination chamber, and the heating components are fixed on the first partition 3; three The quartz tubes 6 are arranged side by side and located between the upper shell 1 and the lower shell 2. The two ends of the quartz tubes 6 pass through the sealed cavity and are fixedly connected to the first flange 7 and the second flange 8 respectively. The first flange 7 on each quartz tube 6 is fixedly connected to the first cover 9, and the second flange 8 on each quartz tube 6 is fixedly connected to the second cover 10. The first cover 9 is provided with three carbon source gas inlets 17, and the second cover 10 is provided with three exhaust ports 18. The three carbon source gas inlets 17 and the three exhaust ports 18 are connected to the three quartz tubes 6 in a one-to-one correspondence.
[0036] Specifically, in order to flexibly adjust the position of the quartz boat 11 in the quartz tube 6, a pull rod 12 is coaxially arranged in the quartz tube 6, one end of the pull rod 12 is connected to the quartz boat 11, and the other end slides out of the first cover 9. By pushing or pulling the pull rod 12, the quartz boat 11 is placed in the heating chamber or the cooling chamber, which is convenient for heating and cooling.
[0037] Specifically, the heating assembly includes an upper heating element 13 and a lower heating element 14, and the quartz tube 6 is located between the upper heating element 13 and the lower heating element 14, and the upper heating element 13 and the lower heating element 14 are inserted from the cooling cavity into the heating cavity; in this embodiment, the upper heating element 13 and the lower heating element 14 are both U-shaped silicon molybdenum rods. The upper heating element 13 and the lower heating element 14 are arranged horizontally and parallel to the quartz tube 6. The upper heating element 13 and the lower heating element 14 heat the quartz tube 6 from the upper side and the lower side respectively, so as to improve the uniformity of heating the quartz tube 6.
[0038] Specifically, in order to ensure the thermal insulation performance of the heating chamber and reduce heat loss, the calcination chamber is also provided with an upper thermal insulation layer 15 and a lower thermal insulation layer 16. The upper thermal insulation layer 15 is fixed to the inner wall of the upper shell 1, and the lower thermal insulation layer 16 is fixed to the inner wall of the lower shell 2. The upper heating element 13, the lower heating element 14 and the quartz tube 6 are all located in the calcination chamber surrounded by the upper thermal insulation layer 15 and the lower thermal insulation layer 16.
[0039] Specifically, a protection box 23 is provided on the outer side of the installation end of the heating component, and the protection box 23 is fixed on the first partition plate 3 and is located on one side of the cooling chamber.
[0040] Specifically, in order to improve the cooling effect, a cooling medium inlet 20 and a cooling medium outlet 21 are symmetrically provided on the side wall of the upper shell 1. The cooling medium inlet 20 and the cooling medium outlet 21 are both connected to the cooling cavity. In this embodiment, the cooling medium is air or water.
[0041] Specifically, a first solenoid valve 19 is provided on the carbon source gas inlet 17, and a second solenoid valve 22 is provided on the cooling medium inlet 20. The first solenoid valve 19, the second solenoid valve 22, the upper heating element 13, and the lower heating element 14 are all electrically connected to a PLC control panel 25 fixedly provided on the outer wall of the upper shell 1.
[0042] Specifically, three temperature sensors 24 are provided on the top of the upper shell 1 , and the three temperature sensors 24 correspond to the three quartz tubes 6 one by one. The lower ends of the temperature sensors 24 extend into the calcining chamber, and the temperature sensors 24 are electrically connected to the PLC control panel 25 .
[0043] Working principle and usage of this utility model:
[0044] When the same carbon source is used, such as methane as the carbon source gas, after the nickel-based catalyst is placed in the three quartz boats 11, the first flange 7 is bolted to the first cover 9, the pull rod 12 is pushed to make the quartz boat 11 in the middle position in the quartz tube 6, and the vacuum machine is connected to the exhaust port 18 for vacuuming. The vacuum machine is turned off, and then the heating temperatures of the three groups of heating components are set to 700°C, 730°C, and 760°C respectively through the PLC control panel 25. Then the first solenoid valve 19 is opened, and methane is respectively introduced into the three quartz tubes 6 through the three carbon source gas inlets 17. After calcining for a period of time, the heating is stopped, and the pull rod 12 is pulled to make the quartz boat 11 in the cooling chamber. The temperature is gradually reduced by air cooling or water cooling, and finally carbon nanotube powders under three different temperature conditions are obtained, which are respectively recorded as CNTs-Ni-700, CNTs-Ni-730, and CNTs-Ni-760.
[0045] When different carbon sources are used, such as methane, liquefied gas, and propylene as carbon source gases, respectively, after nickel-based catalysts, Fe-Mo-Al (FMA) catalysts, and LDH catalysts are placed in three quartz boats 11, respectively, the first flange 7 is bolted to the first cover 9, the pull rod 12 is pushed to make the quartz boat 11 in the middle position in the quartz tube 6, and a vacuum pump is connected to the vacuum pump through the exhaust port 18 to evacuate, and the vacuum pump is turned off. Then, the heating temperature of the three groups of heating components is set to 730° C. through the PLC control panel 25, and then the first solenoid valve 19 is opened, and methane, liquefied gas, and propylene are respectively introduced into the corresponding quartz tube 6 through the three carbon source gas inlets 17. After calcining for a period of time, the heating is stopped, and the pull rod 12 is pulled to make the quartz boat 11 in the cooling chamber. The temperature is gradually reduced by air cooling or water cooling, and finally carbon nanotube powders under the same temperature and different carbon source conditions are obtained, which are respectively recorded as CNTs-Ni-730, CNTs-FMA-730, and CNTs-LDH-730.
[0046] The above is a preferred embodiment of the utility model, which is used to explain the technical solution of the utility model in more detail, so that those skilled in the art can understand and use the utility model well. Those skilled in the art can also make routine modifications, equivalent substitutions and improvements within the spirit and principles of the utility model.
Claims
1. A three-temperature calcination preparation device for experimental carbon nanotube materials, comprising an upper shell and a lower shell that are sealed and connected to each other, and a sealed cavity is formed between the upper shell and the lower shell, characterized in that: A first partition is arranged in the sealed chamber, the first partition divides the sealed chamber into a heating chamber and a cooling chamber, a second partition and a third partition are arranged in the heating chamber, the second partition and the third partition divide the heating chamber into three calcining chambers arranged side by side, a quartz tube and a group of heating components are arranged in each calcining chamber, and the heating components are fixed on the first partition; Three quartz tubes are arranged side by side and located between the upper shell and the lower shell. Two ends of the quartz tubes are respectively passed through the sealed cavity and fixedly connected to the first flange and the second flange. The first flange on each quartz tube is fixedly connected to the first cover, and the second flange on each quartz tube is fixedly connected to the second cover. The first cover is provided with three carbon source gas inlets, and the second cover is provided with three exhaust ports. The three carbon source gas inlets and the three exhaust ports are connected to the three quartz tubes in a one-to-one correspondence.
2. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 1, characterized in that: A pull rod is arranged coaxially in the quartz tube, one end of the pull rod is connected to the quartz boat, and the other end of the pull rod slides out and passes through the first cover.
3. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 2, characterized in that: The heating assembly comprises an upper heating element and a lower heating element. The quartz tube is located between the upper heating element and the lower heating element. The upper heating element and the lower heating element are both inserted from the cooling cavity into the heating cavity.
4. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 3, characterized in that: The upper heating element and the lower heating element are both made of U-shaped silicon molybdenum rods.
5. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 4, characterized in that: The calcining chamber is also provided with an upper insulation layer and a lower insulation layer. The upper insulation layer is fixed to the inner wall of the upper shell, and the lower insulation layer is fixed to the inner wall of the lower shell. The upper heating element, the lower heating element and the quartz tube are all located in the calcining cavity surrounded by the upper insulation layer and the lower insulation layer.
6. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 5, characterized in that: A protection box is provided on the outer side of the installation end of the heating component, and the protection box is fixed on the first partition plate and located on one side of the cooling cavity.
7. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 6, characterized in that: A cooling medium inlet and a cooling medium outlet are symmetrically arranged on the side wall of the upper shell, and the cooling medium inlet and the cooling medium outlet are both communicated with the cooling cavity.
8. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 7, characterized in that: A first solenoid valve is provided on the carbon source gas inlet, and a second solenoid valve is provided on the cooling medium inlet. The first solenoid valve, the second solenoid valve, the upper heating element, and the lower heating element are all electrically connected to a PLC control panel fixedly arranged on the outer wall of the upper shell.
9. The three-temperature calcination preparation device for experimental carbon nanotube materials according to claim 8, characterized in that: The top of the upper shell is provided with three temperature transmitters, which correspond to the three quartz tubes one by one. The lower ends of the temperature transmitters extend into the calcining chamber, and the temperature transmitters are electrically connected to the PLC control panel.