Chemical vapor deposition device for improving surface resistance uniformity of montmorillonite material

Abstract

The invention relates to a chemical vapor deposition device for improving surface resistance uniformity of a montmorillonite material, the chemical vapor deposition device comprises a reaction chamber, a gas inlet device and a gas outlet device, the gas inlet device and the gas outlet device are respectively arranged at two sides of the reaction chamber, the reaction chamber is internally provided with an object placing plate for placing a substrate material, and two ends of the object placing plate are provided with blocking assemblies. The blocking assemblies comprise the first blocking assembly and the second blocking assembly, the first blocking assembly is arranged at the end, close to the air inlet device, of the storage plate, the second blocking assembly is arranged at the end, close to the air outlet device, of the storage plate, and the substrate material is placed between the first blocking assembly and the second blocking assembly. The assembly is short in design period, low in cost and easier to disassemble and assemble, and the final purpose can be effectively achieved from multiple angles.

Description

Technical Field

[0001] This invention relates to the field of chemical vapor deposition technology, and in particular to a chemical vapor deposition apparatus for improving the uniformity of surface resistivity of montmorillonite materials. Background Technology

[0002] There are various methods for preparing graphene materials. Among them, chemical vapor deposition (CVD) is considered a method for preparing high-quality graphene. Under certain growth temperatures and with appropriate hydrocarbon source ratios, high-quality, large-size, single-crystal, and ultra-clean graphene films can be prepared on various substrates. Because glass fiber materials lack catalytic activity in the CVD growth process of graphene, the CVD growth of graphene on glass fiber surfaces is very difficult, usually requiring high temperatures to accelerate the cracking rate and degree of the carbon source gas. However, higher reaction temperatures not only damage the internal structure of the glass fiber material, leading to a significant reduction in its mechanical properties, but also increase the temperature difference and heat exchange between the isothermal zone and the external environment, resulting in a shortened isothermal zone.

[0003] In addition, the current method for preparing large-sized montmorillonite glass materials requires an excessively large size, necessitating the extension of the heating zone of the equipment to prepare large-sized samples. This results in problems such as uneven surface resistance distribution in the prepared montmorillonite glass fiber materials. Alternatively, dynamic roll-to-roll preparation of large-sized samples can be achieved by widening the width of the equipment, but this method is not only too costly but also requires very high precision from the equipment. Summary of the Invention

[0004] Based on the above problems, the present invention improves the uniformity of the surface resistance of the CVD device by adding first and second blocking components on both sides of the reaction chamber. This not only enhances the uniformity of the surface resistance of the styrene fiberglass cloth in the airflow direction and expands the range of uniform surface resistance of the styrene fiberglass cloth in the airflow direction, thereby increasing the utilization rate of the equipment, but also makes it easier to disassemble and install, thus overcoming the above defects.

[0005] This invention provides a chemical vapor deposition apparatus for improving the surface resistivity uniformity of substrate materials, comprising a reaction chamber, an inlet device, and an outlet device, wherein the inlet device and the outlet device are respectively disposed on both sides of the reaction chamber. A placement plate for placing substrate material is disposed inside the reaction chamber, and blocking components are disposed at both ends of the placement plate. The blocking components include a first blocking component and a second blocking component. The first blocking component is disposed at the end of the placement plate near the inlet device, and the second blocking component is disposed at the end of the placement plate near the outlet device.

[0006] Furthermore, the placement plate divides the space inside the reaction chamber into two unconnected upper and lower parts.

[0007] Furthermore, the blocking components are detachable, and the positions of the first and second blocking components can be adjusted along the placement plate according to the specifications of the substrate material.

[0008] Furthermore, the material of the blocking component is at least one of metal, graphite, or porous aluminosilicate ceramic.

[0009] Furthermore, metallic materials include copper, silver, gold, iron, and aluminum; graphite materials include graphite, C60, carbon nanotubes, and graphene; porous aluminosilicate ceramic materials are selected from fine ceramic materials, high-silica silicate materials, aluminosilicate materials, and diatomaceous earth materials.

[0010] Furthermore, the surface of the barrier component is also provided with a catalytic layer. Preferably, the catalytic layer is a thin film layer formed by coating a metal material that can catalyze the cracking of carbon source gas onto the surface of the barrier component.

[0011] Furthermore, the material of the catalyst layer includes at least one selected from platinum, palladium, nickel, copper, and chromium.

[0012] Furthermore, the first blocking component is provided with multiple through holes, preferably, the middle part is a large hole and the edge part is a small hole; the diameter of the large hole is usually 3mm to 5mm and the diameter of the small hole is usually 1mm to 3mm.

[0013] Furthermore, the blocking component is a baffle, which is circular or square.

[0014] The reaction chamber has an inner diameter of 20-30cm and a length of 250-300cm. The placement plate is a quartz plate with a length of 250-300cm and a width of 20-25cm.

[0015] Another inventive aspect of this invention is a montmorillonite glass fiber material, which is prepared using the apparatus described above.

[0016] Compared with the prior art, the advantages of the present invention are:

[0017] This invention provides a chemical vapor deposition apparatus for improving the uniformity of sheet resistivity of montmorillonite materials. The barrier components installed in the CVD equipment can slow down temperature dissipation; the barrier components can also increase gas reflux, increase uniformity, and improve the utilization rate of the equipment. The components of this invention have a short design cycle, low cost, and are easier to disassemble and install, and can effectively achieve uniform sheet resistivity distribution of montmorillonite glass fiber materials from multiple angles.

[0018] In addition, the special selection of materials and post-processing of the blocking components can catalyze the cracking of the gas source and accelerate the reaction; the structural design of the blocking components near the air intake device can adjust the gas flow distribution and improve uniformity. Attached Figure Description

[0019] Figure 1 A schematic diagram of a chemical vapor deposition apparatus for improving the uniformity of surface resistivity of montmorillonite materials;

[0020] Figure 2 Working principle diagram;

[0021] Figure 3 Front view of the first blocking component when it has a hole.

[0022] Reference numerals: 1-Heating furnace, 2-Reaction chamber, 3-Placement plate, 4-First blocking assembly, 5-Second blocking assembly, 6-Inlet device, 7-Outlet device, 8-Substrate material.

[0023] Specific implementation methods

[0024] To make the objectives, technical solutions, and advantages of this application clearer, a more detailed description is provided below. However, it should be understood that the description herein is merely for explaining this application and is not intended to limit its scope.

[0025] In the description of this invention, it should be understood that the terms "first", "second", "vertical", "horizontal", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0026] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of this application. All reagents and instruments used herein are commercially available, and the characterization methods involved can be found in relevant descriptions in the prior art, and will not be repeated here.

[0027] To further understand this application, the following detailed description is provided in conjunction with the preferred embodiments.

[0028] This invention provides a chemical vapor deposition apparatus for improving the uniformity of surface resistivity of a substrate material, comprising a reaction chamber 2, an inlet device 6, and an outlet device 7. The inlet device 6 and the outlet device 7 are respectively disposed on both sides of the reaction chamber 2. A placement plate 3 for placing a substrate material 8 is disposed within the reaction chamber 2. Blocking components are disposed at both ends of the placement plate 3, including a first blocking component 4 and a second blocking component 5. The first blocking component 4 is disposed near the inlet device 6, and the second blocking component 5 is disposed near the outlet device 7. The substrate material 8 is placed between the first blocking component 4 and the second blocking component 5. Figure 1 As shown.

[0029] In actual graphene CVD growth processes, the high temperature setting increases the temperature difference between the isothermal zone within the reaction chamber and the external environment, leading to stronger heat exchange. Specifically, the temperature is higher in the center of the isothermal zone and lower at the boundaries, resulting in less graphene growth at the edges of the substrate material and more growth in the middle, causing uneven resistance distribution. The design of this invention addresses this by using a blocking component to slow heat dissipation at the boundaries, improving temperature uniformity in the isothermal zone. Furthermore, the blocking component allows for gas recirculation at the boundaries, increasing gas flow and improving the graphene growth rate, ultimately resulting in a more uniform resistance distribution. (Recirculation is mentioned as an example.) Figure 2 As stated above.

[0030] In a further preferred embodiment, the placement plate 3 divides the reaction chamber 2 into two non-communicating upper and lower parts. This eliminates gaps between the placement plate and the inner wall of the reaction chamber, increasing gas reflux.

[0031] As a further preferred embodiment, the blocking components are detachable structures, and the positions of the first and second blocking components can be adjusted along the placement plate according to the specifications of the substrate material so that the substrate material is located between the first and second blocking components.

[0032] Substrate materials can include a wide variety of materials, such as some fibrous materials (e.g., glass fiber materials) and fibrous fabric materials (e.g., glass fiber cloth).

[0033] As a further preferred embodiment, the material of the blocking component includes at least one of metal, graphite, and porous aluminosilicate ceramic materials.

[0034] As a further preferred embodiment, the metallic material is selected from copper, silver, gold, iron, and aluminum; the graphite material is selected from at least one of graphite, C60, carbon nanotubes, and graphene; and the porous aluminosilicate ceramic material is selected from fine ceramic materials, high-silica silicate materials, aluminosilicate materials, and diatomaceous earth materials.

[0035] As a further preferred embodiment, the surface of the barrier component is further provided with a catalytic layer, which is a thin film layer formed by coating a metal material capable of catalyzing the cracking of carbon source gas onto the surface of the barrier component.

[0036] In a further preferred embodiment, the catalyst layer is made of at least one of platinum, palladium, nickel, copper, and chromium. It can catalyze the cracking of carbon source gas and accelerate the CVD reaction.

[0037] In a further preferred embodiment, the first blocking component is provided with multiple through holes, preferably, the middle portion is a large hole and the edge portions are small holes, such as... Figure 3 As shown, the diameter of the large holes is typically 3mm to 5mm, and the diameter of the small holes is typically 1mm to 3mm. When the substrate material (e.g., glass fiber cloth) is wound into a roll, the axis of the roll is parallel to the flow direction of the process gas. By setting large holes in the middle and small holes at the edges, the process gas flows more in the middle and less at the edges. This distribution of airflow results in less external airflow and more internal airflow, which can effectively improve the overall deposition uniformity of the rolled substrate material.

[0038] In a further preferred embodiment, the blocking component is a baffle, including but not limited to a circular baffle and a square baffle. The shape of the baffle needs to be adapted to the shape of the reaction chamber and the shape of the substrate material. For example, when the reaction chamber is tubular, the baffle is preferably circular; when the substrate material is wound into a roll, the baffle is preferably circular, and the size of the baffle is larger than the cross-sectional size of the rolled substrate material.

[0039] In a further preferred embodiment, a gap is formed between the blocking component and the inner wall of the reaction chamber to allow gas to flow through the gap. The width of the gap is set according to the required gas flow rate and the size of the substrate material, and is not specifically limited here.

[0040] In a further preferred embodiment, the blocking component is fixed to the shelf, and there are various ways to fix it. For example, the shelf can be designed with multiple slots horizontally from the center to both ends. The width of the slots is slightly larger than the thickness of the blocking component, the depth is 1-3mm, and the length of the slots is the width of the shelf. This allows the blocking component to be placed directly in the slots. Alternatively, several slots can be evenly arranged on the shelf, with the width of the slots slightly larger than the thickness of the blocking component. Of course, depending on the actual situation, other fixing methods can be selected.

[0041] In a further preferred embodiment, the reaction chamber may be a quartz tube with an inner diameter of 20-30 cm and a length of 250-300 cm. The shelf may be a quartz plate with a length of 250-300 cm, a width of 20-25 cm, and a thickness of 4-6 mm.

[0042] The substrate material placed on the quartz plate is in the form of a roll with a total length of 10cm to 1100cm. There are sufficient gaps between the layers to allow for surface CVD growth of graphene. The outer diameter of the roll is 3 to 6cm. Preferably, the substrate material is glass fiber cloth.

[0043] Furthermore, the temperature of the heating furnace is set to 700–1200°C to ensure that graphene can be CVD grown on the surface of the glass fiber cloth at a higher temperature.

[0044] Experimental Example 1

[0045] The chemical vapor deposition apparatus provided by this invention uses a quartz tube with an inner diameter of 25cm and a length of 260cm, a quartz plate with a length of 260cm and a width of 23cm. A graphite baffle, i.e., the first blocking component, is fixed to one end of the quartz plate near the inlet device. A glass fiber cloth, in a roll shape, is placed on the quartz plate with a total length of 900cm and a width of 100cm. It is wound into a roll shape with an outer diameter of 5cm and an inner diameter of 1cm. The glass fiber cloth roll is placed close to and to the right of the first blocking component. Then, a baffle, i.e., the second blocking component, is fixed to one end of the quartz plate near the outlet device.

[0046] Before CVD growth begins, a vacuum is drawn, the equipment is turned on for heating, and the temperature of the heating furnace reaches the growth temperature of 900℃. The carbon source methane is introduced at a flow rate of 500 sccm, the carrier gas hydrogen at a flow rate of 100 sccm, and the pressure is set to 700 Pa. The CVD growth process begins. After 200 minutes, the growth is completed, and montmorillonite glass fiber cloth is obtained.

[0047] To test the sheet resistivity of the montmorillonite glass fiber cloth, a 100cm x 100cm section of the cloth was cut from its center. Sheet resistivity was measured at points every 20cm along the width of the cloth and every 10cm along its length. The average, variance, and coefficient of variation of the sheet resistivity for each column were calculated. The experimental results can be determined or characterized by the coefficient of variation along the length; a smaller coefficient of variation indicates a more uniform distribution of sheet resistivity and better results. The uniformity of the entire cloth is also determined by the coefficient of variation of the entire cloth.

[0048] The sheet resistivity distribution of the montmorillonite glass fiber cloth prepared in Experiment Example 1 is shown in Table 1.

[0049] Table 1. Surface resistance information for Experiment Example 1 (Ω / sq)

[0050]

[0051]

[0052] Comparative Example 1

[0053] No baffles were used, and all other conditions were the same as in Experiment 1.

[0054] The surface resistivity of the montmorillonite glass fiber cloth was measured, and the surface resistivity distribution of the montmorillonite glass fiber cloth is shown in Table 2.

[0055] Table 2 Comparative Example 1: Surface Resistance Information (Ω / sq)

[0056]

[0057] As can be seen from the above test examples and comparative examples, the present application has a significant overall effect by setting two baffles (i.e. blocking components) on the placement plate. The resulting montmorillonite glass fiber cloth has a small overall surface resistivity variation coefficient and the surface resistivity uniformity in different places is greatly improved.

[0058] The above description is merely a preferred embodiment of this application and is not intended to limit this application. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. A chemical vapor deposition apparatus for improving the uniformity of surface resistivity of montmorillonite materials, comprising a reaction chamber (2), an inlet device (6), and an outlet device (7), wherein the inlet device (6) and the outlet device (7) are respectively disposed on both sides of the reaction chamber, characterized in that, The reaction chamber is provided with a placement plate (3) for placing substrate material (8). At both ends of the placement plate (3) are blocking components, which include a first blocking component (4) and a second blocking component (5). The first blocking component (4) is located at the end of the placement plate (3) near the air inlet device (6), and the second blocking component (5) is located at the end of the placement plate (3) near the air outlet device (7).

2. The apparatus according to claim 1, characterized in that, The placement plate divides the reaction chamber into upper and lower parts.

3. The apparatus according to claim 1, characterized in that, The blocking components are detachable, and the positions of the first and second blocking components can be adjusted along the placement plate according to the specifications of the substrate material.

4. The apparatus according to claim 1, characterized in that, The material of the blocking component is at least one of metal, graphite, or porous aluminosilicate ceramic materials.

5. The apparatus according to claim 4, characterized in that, Metallic materials include copper, silver, gold, iron, and aluminum; graphite materials include graphite, C60, carbon nanotubes, and graphene; porous aluminosilicate ceramic materials include fine ceramic materials, high-silica silicate materials, aluminosilicate materials, and diatomaceous earth materials.

6. The apparatus according to any one of claims 1-5, characterized in that, The surface of the barrier component is further provided with a catalytic layer. Preferably, the catalytic layer is a thin film layer formed by coating a metal material capable of catalyzing the cracking of carbon source gas onto the surface of the barrier component. Preferably, the material of the catalyst layer includes at least one selected from platinum, palladium, nickel, copper, and chromium.

7. The apparatus according to claim 1, characterized in that, The first blocking component is provided with multiple through holes, preferably, the middle part is a large hole and the edge part is a small hole; Preferably, the diameter of the large hole is usually 3mm to 5mm, and the diameter of the small hole is usually 1mm to 3mm.

8. The apparatus according to claim 1, characterized in that, The blocking component is a baffle, which is circular or square.

9. The apparatus according to claim 1, characterized in that, The inner diameter of the reaction chamber is 20-30 cm, and the length is 250-300 cm; The shelf is a quartz plate with a length of 250-300cm and a width of 20-25cm.

10. A montmorillonite glass fiber material, which is prepared using the apparatus described in any one of claims 1-9.

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