Continuous liquid injection tubular furnace and chemical vapor deposition device

Abstract

The utility model relates to the field of heating devices, and discloses a continuous liquid injection tube furnace and a chemical vapor deposition device. The continuous liquid injection tubular furnace comprises a heating furnace body and a reaction tube, the reaction tube is arranged in the heating furnace body, a reaction container used for containing to-be-deposited materials and a liquid guide tube used for continuously injecting liquid into the reaction tube are arranged in the reaction tube, and the tail end of the liquid guide tube is connected with a liquid drop prevention assembly used for containing injected liquid and vaporizing the injected liquid. And the anti-droplet assembly is positioned above the reaction container. The stable conditions such as the carbon source reaction atmosphere state and concentration can be met, the liquid carbon source utilization rate is maximized, and the carbon source atmosphere is effectively controlled to be uniform so as to achieve the optimal reaction effect.

Description

Technical Field

[0001] The utility model relates to the field of heating devices, in particular to a continuous liquid injection tubular furnace and a chemical vapor deposition device. Background Art

[0002] Tube furnaces are commonly used as equipment for depositing carbon materials (nanocarbon coating, growing carbon nanotubes, etc.) using chemical vapor deposition technology (CVD), and have been widely used in various new energy material fields such as catalytic materials and battery materials. In addition to commonly used gaseous carbon sources such as methane and acetylene, liquid carbon sources such as ethanol and ethylene glycol are also commonly used for CVD method deposition of carbon materials because of their high utilization rate, high safety, and the ability to form special nanocarbon structures. The current common method of using a liquid carbon source is to place it at one end of a tube furnace, evaporate it into a gaseous state by heating, and guide the carbon source vapor to the middle of the tube furnace through the atmosphere airflow introduced into the tube furnace to participate in the reaction. This method cannot accurately control the amount of liquid carbon source added, and the carbon source cannot be supplemented during the reaction, so the carbon source will be exhausted before the reaction ends, and the reaction cannot be fully carried out. Therefore, it is necessary to design a new type of tube furnace device that can continuously introduce a liquid carbon source.

[0003] In view of this, the present utility model is proposed. Utility Model Content

[0004] The utility model aims to provide a continuous liquid injection tubular furnace and a chemical vapor deposition device, which are used to solve the problems of insufficient liquid carbon source or inability to replenish when the carbon source is exhausted and inadequate reaction in the tubular furnace CVD reaction.

[0005] The embodiment of the utility model is achieved as follows:

[0006] In the first aspect, the utility model provides a continuous liquid injection tubular furnace, which includes a heating furnace body and a reaction tube, wherein the reaction tube is arranged in the heating furnace body, and the reaction tube is provided with a reaction container for placing a material to be deposited and a liquid guide tube for continuously injecting liquid into the reaction tube, and the end of the liquid guide tube is connected to a drip-proof component for receiving the injected liquid and vaporizing it, and the drip-proof component is located above the reaction container.

[0007] In an optional embodiment, the liquid guide tube includes an external liquid guide tube and an internal liquid guide tube, the external liquid guide tube is arranged outside the reaction tube, the internal liquid guide tube is arranged inside the reaction tube, one end of the internal liquid guide tube extends out of the reaction tube and communicates with the external liquid guide tube, and the other end is connected to the drip-proof component.

[0008] In an optional embodiment, the external liquid guiding tube is further provided with a flow regulating valve for controlling continuous liquid injection;

[0009] And / or, the internal catheter sleeve is provided with a heat insulating protective layer.

[0010] In an optional embodiment, the external liquid guiding tube is vertically arranged, and the direction from the inlet end to the outlet end of the internal liquid guiding tube is inclined downward.

[0011] In an optional embodiment, the inclination angle of the internal catheter is 5° to 30°.

[0012] In an optional embodiment, the droplet-proof component includes a drainage wire and a liquid grid, the two ends of the drainage wire are respectively connected to the end of the catheter and the liquid grid, and the liquid grid is suspended above the reaction container.

[0013] In an optional embodiment, the drainage wire is arranged vertically, the liquid placement grid is arranged horizontally, and the drainage wire and the liquid placement grid are detachably connected;

[0014] And / or, the drainage wire is a telescopic rod structure;

[0015] And / or, the aperture of the liquid placing grid is 300-1000 mesh.

[0016] In an optional embodiment, one end of the reaction tube is connected to an air inlet pipe for introducing protective gas, and the other end is connected to an air outlet pipe, and the air inlet pipe is provided with a pressure regulating valve and a pressure gauge.

[0017] In an optional embodiment, two ends of the reaction tube pass through opposite sides of the heating furnace body respectively, and sealing flanges are provided at two ends of the reaction tube respectively, and the air inlet pipe and the air outlet pipe pass through the sealing flanges respectively.

[0018] In a second aspect, the utility model provides a chemical vapor deposition device, which includes a continuous liquid injection tubular furnace as described in any one of the aforementioned embodiments.

[0019] The beneficial effects of the embodiments of the utility model are:

[0020] The continuous liquid injection tubular furnace provided by the utility model introduces a liquid guide tube and a liquid droplet prevention component above the reaction container. The liquid guide tube can directly introduce the liquid carbon source and drop it onto the liquid droplet prevention component. Since the liquid droplet prevention component is located above the reaction container and does not contact the reaction container, the liquid carbon source can directly react with the material to be deposited in the reaction container after evaporation and vaporization. The continuous liquid injection tubular furnace provided by the utility model can regulate and meet the stability of the carbon source reaction atmosphere state, concentration and other conditions, maximize the utilization rate of the liquid carbon source, and effectively control the carbon source atmosphere to be uniform to achieve the best reaction effect, avoiding the problems of insufficient reaction atmosphere, uncontrollable reaction concentration, low production efficiency, etc. caused by the traditional liquid carbon source end injection method. Using the continuous liquid injection tubular furnace provided in this embodiment to carry out chemical vapor deposition can obtain better reaction effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] In order to more clearly illustrate the technical solutions of the embodiments of the utility model, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the utility model and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other relevant drawings can be obtained based on these drawings without paying creative work.

[0022] Figure 1 A schematic diagram of the structure of a continuous liquid injection tubular furnace provided in an embodiment of the utility model;

[0023] Figure 2 A schematic diagram of the structure of a liquid droplet prevention assembly in a continuous liquid injection tubular furnace provided by an embodiment of the utility model;

[0024] Figure 3 A schematic structural diagram of a liquid placement grid of a liquid droplet prevention assembly in a continuous liquid injection tubular furnace provided in an embodiment of the utility model.

[0025] Icons: 100-continuous liquid injection tubular furnace; 110-heating furnace body; 120-reaction tube; 121-sealing flange; 122-inlet pipe; 123-outlet pipe; 124-pressure regulating valve; 125-pressure gauge; 126-reaction vessel; 130-liquid guide tube; 131-sealing ring; 132-external liquid guide tube; 133-internal liquid guide tube; 134-flow regulating valve; 135-insulation protective layer; 140-dripproof component; 141-drainage wire; 142-liquid placement grid. DETAILED DESCRIPTION

[0026] In order to make the purpose, technical scheme and advantages of the embodiments of the utility model clearer, the technical scheme in the embodiments of the utility model will be clearly and completely described below in conjunction with the drawings in the embodiments of the utility model. Obviously, the described embodiments are part of the embodiments of the utility model, not all of the embodiments. Generally, the components of the embodiments of the utility model described and shown in the drawings here can be arranged and designed in various different configurations.

[0027] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the present invention to be protected, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0029] In the description of the present utility model, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside", etc. indicate the orientation or position relationship based on the orientation or position relationship shown in the accompanying drawings, or the orientation or position relationship in which the utility model product is usually placed when in use, which is only for the convenience of describing the utility model and simplifying the description, and does not indicate or imply 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 utility model. In addition, the terms "first", "second", "third", etc. are only used to distinguish the description, and cannot be understood as indicating or implying relative importance.

[0030] In addition, the terms "horizontal", "vertical" and the like do not mean that the components are required to be absolutely horizontal or suspended, but can be slightly tilted. For example, "horizontal" only means that its direction is more horizontal than "vertical", and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0031] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set", "install", "connect", and "connect" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0032] Example

[0033] Please refer to Figure 1 This embodiment provides a continuous liquid injection tube furnace 100, which includes a heating furnace body 110, a reaction tube 120, a liquid guide tube 130 and a drip prevention component 140.

[0034] The heating furnace body 110 is used to heat the reaction tube 120. The reaction tube 120 in this embodiment can be, for example, a common quartz tube. In this embodiment, the reaction tube 120 is arranged in the heating furnace body 110. The two ends of the reaction tube 120 pass through the opposite sides of the heating furnace body 110 respectively. The left and right ends of the reaction tube 120 are respectively provided with sealing flanges 121. The setting of the sealing flanges 121 can ensure the sealing of the reaction tube 120 as a whole. One end of the reaction tube 120 is connected to an inlet pipe 122 for passing a protective gas, and the other end is connected to an outlet pipe 123. The inlet pipe 122 and the outlet pipe 123 pass through the sealing flange 121 respectively. The protective gas can be selected from conventional inert gases, such as nitrogen, helium, etc. By passing the protective gas into the reaction tube 120, the entire reaction is carried out under the protection of the inert gas to avoid oxidation and the introduction of other impurities. Furthermore, the air inlet pipe 122 in this embodiment is provided with a pressure regulating valve 124 and a pressure gauge 125, and the flow rate of the protective gas entering the reaction tube 120 can be controlled by the arrangement of the pressure regulating valve 124 and the pressure gauge 125. A reaction container 126 for placing the material to be deposited is arranged in the reaction tube 120, and the arrangement position of the reaction container 126 is approximately located in the middle of the reaction tube 120. The reaction container 126 can be, for example, a reaction ark or a crucible, and the heating furnace body 110 heats the reaction tube 120, so that the material reaction in the reaction container 126 is carried out under the conditions of high temperature and protective gas.

[0035] The liquid guide tube 130 is arranged on the side of the reaction tube 120 close to the air inlet pipe 122. Specifically, the liquid guide tube 130 also needs to extend from the sealing flange 121, and the extended position is sealed by the sealing ring 131. The liquid guide tube 130 is used to realize continuous liquid injection into the reaction tube 120. In this embodiment, the liquid guide tube 130 includes an external liquid guide tube 132, an internal liquid guide tube 133 and a flow control valve 134. The external liquid guide tube 132 is arranged outside the reaction tube 120 and is arranged vertically. It should be understood that the vertical arrangement of the external liquid guide tube 132 is not absolutely vertical, and there may be a certain angle deviation. The flow control valve 134 is installed on the external liquid guide tube 132, and the internal liquid guide tube 133 is arranged in the reaction tube 120. One end of the internal liquid guide tube 133 extends out of the reaction tube 120 and communicates with the external liquid guide tube 132, and the other end is connected to the anti-drip assembly 140. In this embodiment, by introducing the liquid conduit 130, the liquid carbon source can be continuously input into the reaction container 126. At the same time, the setting of the flow control valve 134 can accurately control the input amount of the liquid carbon source, and the liquid carbon source can be replenished at any time during the reaction process to ensure sufficient reaction. The internal liquid conduit 133 is provided with an insulating protective layer 135. The setting of the insulating protective layer 135 is conducive to protecting the internal liquid conduit 133, avoiding damage to the internal liquid conduit 133 by high temperature, and also avoiding the liquid carbon source in the internal liquid conduit 133 from evaporating prematurely under high temperature conditions and affecting the reaction effect.

[0036] Furthermore, the direction from the inlet end to the outlet end of the internal liquid guiding tube 133 is inclined downward, and specifically, the inclination angle of the internal liquid guiding tube 133 is 5° to 30°. In this embodiment, by tilting the internal liquid guiding tube 133, and the inclination angle is adjustable, the flow rate of the droplets can be controlled by the inclination angle to avoid the droplets from being fed too fast or too slow, thereby satisfying the flow characteristics of different liquid carbon sources to achieve the best reaction effect.

[0037] Please refer to Figure 1 , Figure 2 and Figure 3The anti-drip assembly 140 is connected to the end of the liquid conduit 130 to receive the injected liquid and vaporize it. The anti-drip assembly 140 includes a drainage wire 141 and a liquid grid 142. The two ends of the drainage wire 141 are respectively connected to the end of the liquid conduit 130 and the liquid grid 142. The liquid grid 142 is suspended above the reaction container 126. The drainage wire 141 is vertically arranged, and the liquid grid 142 is horizontally arranged. It should be understood that the vertical arrangement of the drainage wire 141 and the horizontal arrangement of the liquid grid 142 are not absolutely vertical and horizontal, and there may be a certain angle deviation. In this embodiment, the arrangement of the anti-drip assembly 140 is conducive to preventing the liquid carbon source from being introduced too much and not having time to evaporate and directly dripping into the reaction crucible, which seriously affects the reaction effect. In this embodiment, the liquid carbon source discharged from the liquid guide tube 130 is first discharged into the liquid grid 142 through the drainage wire 141. The liquid carbon source on the liquid grid 142 is fully evaporated and vaporized under the high temperature of the reaction tube 120, and directly reacts with the material to be deposited in the reaction container 126 in gaseous form.

[0038] Since different liquid carbon sources have different viscosities and surface tensions, liquid placing grids 142 with different apertures are required to prevent the liquid from falling and accelerate surface evaporation. Therefore, in this embodiment, the drainage wire 141 and the liquid placing grid 142 are detachably connected. Such a setting facilitates replacement of different liquid placing grids 142 according to different liquid carbon sources. The aperture of the liquid placing grid 142 is 300 mesh to 1000 mesh, which has a wide selection range and can be applied to a variety of liquid carbon sources.

[0039] Furthermore, the drainage wire 141 in this embodiment is a telescopic rod structure, and the structural design of the telescopic rod makes the length of the drainage wire 141 adjustable. It should be understood that after the length of the drainage wire 141 is adjusted to a suitable position, it needs to be fixed by a fixing device, such as a conventional snap structure, locking structure or screw structure, etc., provided on the telescopic rod to achieve fixation. By adjusting the length of the drainage wire 141, the drainage wire 141 can be coordinated with the position and height of the reaction container 126 below, avoiding contact between the liquid grid 142 and the reaction container 126, and realizing that the liquid grid 142 is suspended above the reaction container 126.

[0040] Please refer to Figure 1 , Figure 2 and Figure 3The working principle of the continuous liquid injection tubular furnace 100 is as follows: the continuous liquid injection tubular furnace 100 provided in this embodiment introduces a liquid guide tube 130 above the reaction vessel 126. The liquid guide tube 130 can be divided into an external liquid guide tube 132 and an internal liquid guide tube 133. The liquid carbon source directly enters from the external liquid guide tube 132 and flows obliquely downward along the internal liquid guide tube 133. The liquid carbon source in the internal liquid guide tube 133 can remain in liquid state under the protection of the insulation protective layer 135, and will not evaporate prematurely. Then, it falls onto the liquid placement grid 142 through the drainage wire 141. Since the liquid grid 142 is located above the reaction vessel 126 and does not contact the reaction vessel 126, the liquid carbon source can directly react with the material to be deposited in the reaction vessel 126 after evaporation and vaporization. In this embodiment, by tilting the internal liquid guide tube 133 downward at a certain angle and cooperating with the flow regulating valve 134, the flow rate and addition amount of the liquid carbon source entering the reaction tube 120 can be accurately controlled. The continuous liquid injection tubular furnace 100 provided in this embodiment satisfies the stability of the carbon source reaction atmosphere state, concentration and other conditions, maximizes the utilization rate of the liquid carbon source, effectively controls the carbon source atmosphere to be uniform to achieve the best reaction effect, and avoids the problems of insufficient reaction atmosphere, uncontrollable reaction concentration, low production efficiency, etc. caused by the traditional liquid carbon source end injection method. The problem of insufficient liquid carbon source or inability to replenish when the carbon source is exhausted and insufficient reaction in the tubular furnace CVD reaction is solved.

[0041] In addition, the utility model also provides a chemical vapor deposition device, which includes the above-mentioned continuous liquid injection tube furnace 100. By using the continuous liquid injection tube furnace 100 provided in this embodiment to perform chemical vapor deposition, better reaction effects can be obtained.

[0042] In summary, the continuous liquid injection tubular furnace 100 provided by the utility model introduces a liquid guide tube 130 above the reaction vessel 126, and the liquid guide tube 130 can directly introduce the liquid carbon source, and the liquid carbon source falls onto the liquid placement grid 142 through the drainage wire 141. Since the liquid placement grid 142 is located above the reaction vessel 126 and does not contact the reaction vessel 126, the liquid carbon source can directly react with the material to be deposited in the reaction vessel 126 after evaporation and vaporization. The continuous liquid injection tubular furnace 100 provided by the utility model satisfies the stability of the carbon source reaction atmosphere state, concentration and other conditions, maximizes the utilization rate of the liquid carbon source, effectively controls the carbon source atmosphere to be uniform to achieve the best reaction effect, and avoids the problems of insufficient reaction atmosphere that cannot be supplemented, insufficient reaction, low production efficiency, etc. caused by the traditional liquid carbon source end injection method. The continuous liquid injection tubular furnace 100 provided by this embodiment is used for chemical vapor deposition to obtain better reaction effects.

[0043] The above description is only the preferred embodiment of the utility model, and is not intended to limit the utility model. For those skilled in the art, the utility model can have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model shall be included in the protection scope of the utility model.

Claims

1. A continuous liquid injection tube furnace, characterized in that: It includes a heating furnace body and a reaction tube, wherein the reaction tube is arranged in the heating furnace body, wherein a reaction container for placing materials to be deposited and a liquid guide tube for continuously injecting liquid into the reaction tube are arranged in the reaction tube, and the end of the liquid guide tube is connected with a drip-proof component for receiving the injected liquid and vaporizing it, and the drip-proof component is located above the reaction container.

2. The continuous liquid injection tube furnace according to claim 1, characterized in that: The liquid guide tube includes an external liquid guide tube and an internal liquid guide tube. The external liquid guide tube is arranged outside the reaction tube, and the internal liquid guide tube is arranged inside the reaction tube. One end of the internal liquid guide tube extends out of the reaction tube and communicates with the external liquid guide tube, and the other end is connected to the drip-proof component.

3. The continuous liquid injection tube furnace according to claim 2, characterized in that: The external liquid guiding tube is also provided with a flow regulating valve for controlling continuous liquid injection; And / or, the internal catheter sleeve is provided with a heat insulating protective layer.

4. The continuous liquid injection tube furnace according to claim 2, characterized in that: The external liquid guiding tube is arranged vertically, and the direction from the inlet end to the outlet end of the internal liquid guiding tube is arranged obliquely downward.

5. The continuous liquid injection tube furnace according to claim 4, characterized in that: The inclination angle of the internal liquid guiding tube is 5° to 30°.

6. The continuous liquid injection tube furnace according to claim 1, characterized in that: The anti-drip assembly comprises a drainage wire and a liquid placement grid. The two ends of the drainage wire are respectively connected to the end of the liquid guide tube and the liquid placement grid. The liquid placement grid is suspended above the reaction container.

7. The continuous liquid injection tube furnace according to claim 6, characterized in that: The drainage wire is arranged vertically, the liquid placement grid is arranged horizontally, and the drainage wire and the liquid placement grid are detachably connected; And / or, the drainage wire is a telescopic rod structure; And / or, the aperture of the liquid placing grid is 300-1000 mesh.

8. The continuous liquid injection tube furnace according to any one of claims 1 to 7, characterized in that: One end of the reaction tube is connected to an air inlet pipe for introducing protective gas, and the other end is connected to an air outlet pipe. The air inlet pipe is provided with a pressure regulating valve and a pressure gauge.

9. The continuous liquid injection tube furnace according to claim 8, characterized in that: Both ends of the reaction tube pass through opposite sides of the heating furnace body respectively, and sealing flanges are respectively arranged at both ends of the reaction tube, and the air inlet pipe and the air outlet pipe pass through the sealing flanges respectively.

10. A chemical vapor deposition device, characterized in that: It comprises the continuous liquid injection tube furnace as described in any one of claims 1-9.

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