阅读说明：本技术 一种化学气相沉积装置与方法 (Chemical vapor deposition device and method ) 是由 祝巍 马萍萍 于 2020-04-20 设计创作，主要内容包括：本发明提供了一种化学气相沉积装置,包括反应腔体、阴极、阳极、电源、反应衬底、机械泵、加热装置和冷却装置；本申请还提供了利用化学气相沉积装置进行化学气相沉积的方法。本发明在化学气相沉积反应中直接采用直流辉光引入等离子体,一方面可以大幅提高化学气相沉积的效率,降低反应温度,降低成本,提高品质等；另一方面利用直流辉光产生等离子体既直接作用于反应区域,成本又低。因此本发明不仅适合于研究化学气相反应的机制,也适用于大规模生产,特别是石墨烯的生产。(The invention provides a chemical vapor deposition device, which comprises a reaction cavity, a cathode, an anode, a power supply, a reaction substrate, a mechanical pump, a heating device and a cooling device, wherein the reaction cavity is provided with a plurality of reaction holes; the application also provides a method for carrying out chemical vapor deposition by using the chemical vapor deposition device. The invention directly adopts direct current glow to introduce plasma in the chemical vapor deposition reaction, on one hand, the efficiency of the chemical vapor deposition can be greatly improved, the reaction temperature is reduced, the cost is reduced, the quality is improved, and the like; on the other hand, the direct current glow is utilized to generate plasma, which directly acts on the reaction area and has low cost. Therefore, the method is not only suitable for researching the mechanism of the chemical gas phase reaction, but also suitable for large-scale production, in particular to the production of graphene.)

1. A chemical vapor deposition device comprises a reaction cavity, a cathode, an anode, a power supply, a reaction substrate, a mechanical pump, a heating device and a cooling device;

the cathode, the anode and the reaction substrate are arranged in the reaction cavity; the cathode and the anode are used for generating plasma, the cathode is arranged opposite to the anode, and the reaction substrate is arranged between the cathode and the anode;

the power supply is connected with the cathode and the anode;

the mechanical pump is connected with the reaction cavity;

the heating device is used for heating the reaction cavity;

the cooling device is used for cooling the reaction cavity.

2. The chemical vapor deposition apparatus of claim 1, wherein the cathode and the anode are both hollow structures.

3. The chemical vapor deposition apparatus according to claim 1, wherein the heating device is a heating wire or a heating jacket disposed outside the reaction chamber, or disposed inside the reaction chamber.

4. The chemical vapor deposition apparatus of claim 1, wherein the cooling device is a copper tube surrounding the reaction chamber.

5. A chemical vapor deposition apparatus according to claim 1, wherein the chemical vapor deposition apparatus is further provided with an infrared thermometer or a thermocouple for measuring the temperature of the reaction substrate.

6. The chemical vapor deposition apparatus of claim 1, wherein the reaction chamber is a metal pipe or a non-metal pipe.

7. The chemical vapor deposition apparatus of claim 1, wherein the reaction substrate is a silicon wafer, sapphire, nickel foil, copper foil, or the reaction chamber itself.

8. A method of chemical vapor deposition using the chemical vapor deposition apparatus of claim 1, comprising the steps of:

and vacuumizing and heating the reaction cavity, introducing reaction atmosphere, applying voltage to generate plasma, and introducing a reaction source to perform chemical vapor deposition.

9. The method of claim 8, wherein the reactive source is a gaseous reactive source, a solid reactive source, or a liquid reactive source, and the gaseous reactive source is methane, ethane, or ethylene; the reaction atmosphere is hydrogen, argon or oxygen.

10. The method of claim 9, wherein the product of the chemical vapor deposition is graphene, molybdenum sulfide, tungsten sulfide, or phosphorus.

Technical Field

The invention relates to the technical field of chemical vapor deposition, in particular to a chemical vapor deposition device and a chemical vapor deposition method.

Background

Chemical Vapor Deposition (CVD) is a process that uses chemical reactions to vaporize a gas or solid/liquid source to produce a desired product, typically under a vacuum environment and at a certain temperature, which is typically deposited on a specific substrate. Through the development of many years, the CVD method is not only a very important scientific research means, but also has a certain scale in the aspect of industrial production; particularly, in recent years, growth of graphene is an important method for producing high-quality graphene.

The CVD method needs to be decomposed by heating, but many reaction sources need to be heated to a high temperature (such as more than 1000 ℃) to be decomposed, and the decomposition efficiency is low, so that the common CVD method has low efficiency and high cost. In order to improve the efficiency, plasma is introduced in the chemical vapor deposition process to improve the decomposition efficiency of gas, so that the growth rate of products can be greatly improved, and the growth temperature of some products can be reduced. There are many ways to generate plasma, such as high temperature, high voltage, microwave, plasma gun, etc.

Although plasma can effectively enhance the efficiency of chemical vapor deposition, the generation of plasma also increases the new cost, and a low-cost and high-efficiency plasma enhanced chemical vapor deposition apparatus and method are not seen.

Disclosure of Invention

The invention aims to provide a chemical vapor deposition device which can realize chemical vapor deposition with high efficiency and low cost.

In view of the above, the present application provides a chemical vapor deposition apparatus, which includes a reaction chamber, a cathode, an anode, a power supply, a reaction substrate, a mechanical pump, a heating device, and a cooling device;

the cathode, the anode and the reaction substrate are arranged in the reaction cavity; the cathode and the anode are used for generating plasma, the cathode is arranged opposite to the anode, and the reaction substrate is arranged between the cathode and the anode;

the power supply is connected with the cathode and the anode;

the mechanical pump is connected with the reaction cavity;

the heating device is used for heating the reaction cavity;

the cooling device is used for cooling the reaction cavity.

Preferably, the cathode and the anode are both of a hollow structure.

Preferably, the heating device is a heating wire or a heating sleeve arranged outside the reaction cavity body, or is arranged inside the reaction cavity body.

Preferably, the cooling device is a copper pipe externally wound around the reaction cavity.

Preferably, the chemical vapor deposition apparatus is further provided with an infrared thermometer or a thermocouple for measuring the temperature of the reaction substrate.

Preferably, the reaction chamber is a metal pipe or a non-metal pipe.

Preferably, the reaction substrate is a silicon wafer, sapphire, nickel foil, copper foil or the reaction chamber itself.

The application also provides a method for carrying out chemical vapor deposition by using the chemical vapor deposition device, which comprises the following steps:

and vacuumizing and heating the reaction cavity, introducing reaction atmosphere, applying voltage to generate plasma, and introducing a reaction source to perform chemical vapor deposition.

Preferably, the reaction source is a gas reaction source, a solid reaction source or a liquid reaction source, and the gas reaction source is methane, ethane or ethylene; the reaction atmosphere is hydrogen, argon or oxygen.

Preferably, the product of the chemical vapor deposition is graphene, molybdenum sulfide, tungsten sulfide or phosphorus.

The application provides a chemical vapor deposition device, which comprises a reaction cavity, a cathode, an anode, a power supply, a reaction substrate, a mechanical pump, a heating device and a cooling device; the chemical vapor deposition device provided by the application generates direct current glow through the arrangement of the anode and the cathode, and the decomposition efficiency of reaction gas is improved by plasma generated by the direct current glow; on the other hand, the cost of the direct current glow generated plasma is low, and the method is suitable for large-scale use.

Drawings

FIG. 1 is a schematic structural view of a CVD deposition apparatus according to the present invention;

fig. 2 is a photograph of graphene prepared by using a chemical vapor deposition apparatus according to example 1 of the present invention;

fig. 3 is a scanning electron micrograph and a raman spectrum of graphene produced in example 1 of the present invention.

Detailed Description

For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.

In view of the current situation of the chemical vapor deposition method, the application provides a chemical vapor deposition device which utilizes direct current glow plasma to enable the chemical vapor deposition method to have the characteristics of high efficiency and low cost. Specifically, the embodiment of the invention discloses a chemical vapor deposition device, which comprises a reaction cavity, a cathode, an anode, a power supply, a reaction substrate, a mechanical pump, a heating device and a cooling device, wherein the reaction cavity is provided with a plurality of reaction holes;

the cathode, the anode and the reaction substrate are arranged in the reaction cavity; the cathode and the anode are used for generating plasma, the cathode is arranged opposite to the anode, and the reaction substrate is arranged between the cathode and the anode;

the power supply is connected with the cathode and the anode;

the mechanical pump is connected with the reaction cavity;

the heating device is used for heating the reaction cavity;

the cooling device is used for cooling the reaction cavity.

In the chemical vapor deposition apparatus provided in the present application, the reaction chamber may be a tube furnace structure (horizontal type), or a cylindrical chamber structure (vertical type), and there is no particular limitation to this application; similarly, the material of the reaction chamber is not particularly limited in the present application, and the reaction chamber may be a metal reaction chamber or a non-metal reaction chamber. In order to realize the cooling of the reaction cavity, a copper pipe can be wound outside the reaction cavity for water cooling, or a stainless steel reaction cavity with a double-layer water cooling cavity wall is directly adopted. In order to accurately control the amount of the reaction gas, the chemical vapor deposition device is also provided with a flow meter, and the flow of the gas entering the reaction cavity is controlled by a multi-path metering flow meter. The pressure of the reaction can be controlled between several Pa and several tens of thousands Pa, and the pressure is matched with the voltage between the electrodes according to actual needs. The reaction substrate may be heated by means of external heating, such as heating wires, heating jackets, etc.; electrode heating can also be directly introduced into the cavity; the plasma may be used to heat the substrate even when the plasma-generating cathode or anode is used as the substrate end. The reaction substrate is not particularly limited in this application, and may be a silicon wafer, sapphire, nickel foil, or copper foil, or may be a reaction chamber wall itself.

In order to ensure that the equipment stably runs for a long time, the cathode and the anode which generate plasma need to be cooled, so that the cathode and the anode need to be made into a hollow structure, and cooling water is conveniently introduced for cooling. For the convenience of observation, the reaction cavity of the tube furnace can adopt a quartz tube, and an observation window needs to be reserved in the stainless steel cavity. The substrate temperature can be measured by an infrared thermometer, or by setting the temperature of the heating wire or by installing a thermocouple directly under the substrate.

The chemical vapor deposition device provided by the application can finish chemical vapor deposition at a lower temperature or higher efficiency by utilizing the direct current glow plasma generated by the counter electrode, so that the chemical vapor deposition efficiency can be greatly improved, and the product quality is improved; meanwhile, the equipment has the characteristics of low cost, high reliability and the like.

The application also provides a method for carrying out chemical vapor deposition by using the chemical vapor deposition device, which comprises the following steps:

and vacuumizing and heating the reaction cavity, introducing reaction atmosphere, applying voltage to generate plasma, and introducing a reaction source to perform chemical vapor deposition.

More specifically, firstly, a mechanical pump is adopted to vacuumize the reaction cavity, then buffer gas is introduced, voltage is applied to the electrode to generate plasma, and the reaction cavity or the substrate is heated (or not heated); finally, reaction gas is introduced to react, and a required product can be deposited on the substrate.

In the chemical vapor deposition process, the reaction source is a gas reaction source, a solid reaction source or a liquid reaction source, and the gas reaction source is methane, ethane or ethylene; the reaction atmosphere is hydrogen, argon or oxygen; the product of the chemical vapor deposition is graphene, molybdenum sulfide, tungsten sulfide or phosphorus.

The device that this application provided utilizes the supplementary chemical vapor deposition method of direct current glow plasma can effectually utilize the plasma that the direct current glow produced to improve reaction gas's decomposition efficiency, can adjust plasma's intensity through control reaction pressure and voltage simultaneously, and the temperature of substrate can be adjusted through heating or control plasma heating. Compared with other plasma-assisted chemical vapor deposition methods, the method has the advantages that on one hand, generated plasmas directly act on a reaction area, and the effect is better; on the other hand, the cost of the direct current glow generated plasma is low, and the method is suitable for large-scale use.

For further understanding of the present invention, the chemical vapor deposition apparatus and method provided by the present invention are described in detail with reference to the following examples, and the scope of the present invention is not limited by the following examples.