WO2013149572A1

WO2013149572A1 - Equipment for large-scale continuous preparation of two-dimensional nanometer thin film

Info

Publication number: WO2013149572A1
Application number: PCT/CN2013/073573
Authority: WO
Inventors: 徐明生
Original assignee: Xu Mingsheng
Priority date: 2012-04-02
Filing date: 2013-04-01
Publication date: 2013-10-10

Abstract

Disclosed is equipment for the large-scale continuous preparation of a two-dimensional nanometer thin film, which comprises a feeding chamber, a thin film preparation chamber, a balancing chamber, a chemical vapour deposition chamber, a discharging chamber, etc. A valve is arranged between every two chambers, and a sample is continuously transmitted between the chambers through a transmission device which is arranged in the whole system; the chamber is provided therein with a sample processing device, a heating device, a physical vapour deposition system and/or a chemical vapour deposition system, etc.; each chamber is connected to a gas connection port and is connected to a vacuum system; and the whole equipment is provided with an automation control system to control the ON/OFF of the valve between every two chambers, sample transmission, gas flow control, vacuum pumping, etc. The device can be applied to prepare two-dimensional nanometer thin films of graphene, transition metal chalcogenide, silicene, germanene or boron nitride, etc. The equipment has a simple structure and reliable operation, can conduct the large-scale continuous preparation of uniform high-quality two-dimensional nanometer thin films of graphene, metal chalcogenide, silicene, germanene or boron nitride, etc., and is suitable for the industrial preparation of two-dimensional nanometer thin films.

Description

Equipment for large-scale continuous preparation of two-dimensional nano-films

The present invention relates to a new material preparation apparatus, and more particularly to an apparatus for large-scale continuous preparation of novel two-dimensional nanomaterials such as graphene, metal chalcogenide, silene, terpene, and boron nitride. Background technique

Graphene is a honeycomb-like single carbon atom layer with a thickness of 0.334 nm. It has excellent two-dimensional electrical, optical, thermal, mechanical properties and chemical stability. Graphene is in ultrafast optoelectronic devices, clean energy, Sensors and other aspects have broad application prospects. The transmission speed of electrons in graphene is 150 times that of silicon. IBM and other famous companies have already prepared ultra-fast optoelectronic devices with speeds up to terahertz. The University of California uses graphene to develop optical modems, which is expected to increase the network speed by 10,000 times. The global demand for semiconductor crystalline silicon is about 2,500 tons per year. If graphene replaces one-tenth of crystalline silicon to make high-end integrated circuits such as RF circuits, the market capacity is at least 500 billion yuan. Because graphene has only 2.3% light absorption, this makes graphene useful for the preparation of flexible transparent electrodes for optoelectronic devices such as display devices, solar cells, touch panels, etc., thereby replacing expensive, resource-intensive, non-freely foldable indium-based components. ITO transparent conductive film; According to reports, the global demand for ITO conductive glass in 2011 is between 85 and 95 million pieces, so that the replacement space for graphene is huge. Due to the unique electron transport properties of graphene, as a sensor, it has single-molecule sensitivity; if graphene-based gene electronic sequencing technology can be realized, the sequencing cost of human whole-genome spectrometry will be about $100,000/person And it is greatly reduced to about $1,000/person, which helps biomedical innovation and helps to achieve personalized health care. After several years of rapid development, graphene products have emerged in touch screen applications. Therefore, the good commercial value of graphene and the broad market have already shown the dawn, the industrialization of graphene materials will be a revolutionary change in the materials, information, energy industry!

In addition to graphene, graphene-like new two-dimensional nanomaterials also have their unique photoelectron properties and have broad application prospects. New two-dimensional graphene-based material comprising a layered metal chalcogenide (metal chalcogenides), silicon-ene (sili _Cene), germanium-ene (germanene), BN (boron nitride) and the like.

However, there is currently no large-scale device for continuously preparing two-dimensional nano-films such as graphene. Chemical vapor deposition (CVD) and surface segregation methods are technical methods for preparing two-dimensional nano-films over a large area. Methods The apparatus for preparing two-dimensional nanofilms is basically a quartz tube high temperature furnace [Science 324, 1312-1314 (2009); Nature Nanotechnology 5, 574 (2010); Nano Lett. 11, 297-303 (2011)]. The high temperature furnace based on quartz tube only has the single function of synthesizing two-dimensional nano-film on the existing metal catalyst layer, that is, the surface of the substrate cannot be processed successively, and the catalysis required for preparing the two-dimensional nano-film on the substrate is prepared. Synthesis of layers and subsequent two-dimensional nanofilms. Moreover, the two-dimensional nano-film synthesized by quartz tube furnace has many structural defects, which leads to poor electron transport performance of the prepared film. The quartz tube furnace has severely restricted the application of two-dimensional nano-films such as graphene films, which is not suitable for scale. A two-dimensional nanofilm such as graphene is continuously prepared.

In order to realize the large-scale continuous preparation of two-dimensional nano-films, that is, the continuous process including the processing of the substrate, the preparation of the catalytic layer, and the preparation of the two-dimensional film, each chamber should be proprietary in the preparation process of the two-dimensional nano film. Unique functional role. Due to the structural characteristics of the two-dimensional film such as graphene and the requirements of the preparation technology, the conventional equipment of other industries cannot be used for the continuous controllable preparation of the high-quality graphene film; for example, the lining required for the synthesis of graphene and the like due to high temperature The effect of the mechanical properties of the bottom/catalytic layer, etc., roll-to-roll equipment is not possible to produce high quality graphene films [Applied Physics Letters 98, 133106 (2011)]; due to production process technology The difference between the current production process equipment for the preparation of ITO conductive glass is not suitable for the preparation of two-dimensional films such as graphene; so far, no special equipment has been developed for the large-scale continuous preparation of high-quality graphene films. Summary of the invention

In view of the deficiencies of the prior art, the present invention provides an apparatus capable of large-scale continuous preparation of two-dimensional nano-films such as graphene, metal chalcogenide, silene, terpene or boron nitride. In order to enable continuous preparation of a two-dimensional nanofilm, the apparatus is provided with a high temperature resistant sample transport device; in order to achieve balance and stability during continuous preparation, it is preferred to provide a transition between a specific chamber and the chamber. The balance chamber and the balance chamber have a stabilizing effect on the whole preparation process of the two-dimensional nano film; the functions of the film preparation chamber and the chemical vapor deposition chamber are mainly used for preparing the film and appropriately processing the prepared film, The film includes a catalytic layer, a precursor of a two-dimensional film, a two-dimensional film, and the like; the function of the processing chamber is mainly used to optimize the structure of the substrate, the catalytic layer, the precursor of the two-dimensional film, and the two-dimensional film, thereby being able to prepare The high-quality two-dimensional film; the device has the characteristics of simple structure, simple operation, good safety, etc. The process for preparing the two-dimensional nano film by the device is simple, the cost is low, and the prepared film has excellent structure and performance.

The physical vapor deposition system includes any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system. The chemical vapor deposition system comprises a chemical vapor deposition system composed of a chamber, a gas and a heater (ie, a thermal chemical vapor deposition system), a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, and an aerosol assist. Any one or a combination of two or more of a chemical vapor deposition system, an inductively coupled plasma chemical vapor deposition system.

Depending on the process for preparing the two-dimensional film, such as the substrate, the catalytic layer, and the source material of the synthetic two-dimensional film, continuous preparation of the two-dimensional film can be realized by selecting different device combinations or equipments.

For the sake of simplicity and clarity of the various embodiments, the present specification unifies various terminology.

According to the different preparation conditions of the two-dimensional film, the technical scheme adopted by the invention is as follows:

A scaled-up apparatus for continuously preparing a two-dimensional nanofilm, comprising a feed chamber, a first film preparation chamber, and a discharge chamber. The first film preparation chamber may also be referred to as a sample preparation chamber.

The feed chamber, the first film preparation chamber and the discharge chamber are each provided with a sample transfer device, and the sample can be transferred from the feed chamber to the first film preparation chamber through the sample transfer device, from the first The film preparation chamber is transported to the discharge chamber for continuous preparation of the two-dimensional nanofilm; the sample transfer device includes any one or a combination of two or more of a roller, a pulley and a conveyor belt.

The feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first film preparing chamber, and a valve is arranged between the first film preparing chamber and the discharging chamber. The material chamber is provided with a valve that communicates with the atmosphere.

At least one of the feeding chamber, the first film preparation chamber and the discharge chamber is provided with a heating device; the heating device may be a resistance wire heating device, an infrared heating device, a laser heating device or the like.

The feeding chamber, the first film preparing chamber and the discharging chamber are respectively provided with independent vacuuming devices, and each vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc. The vacuum device can maintain the vacuum of each chamber at a normal pressure to between 1.0 x 10 - 1 ^Q Pa.

At least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with one or more gas connection ports, and the gas connection port may be a gas connection port, a gas connection port It can also be connected to the gas mixing box, and the gas connection port is connected to the gas path; at least two or more gas paths are connected in parallel at the inlet of the gas mixing box, so that two or more gases can enter the gas mixing box at the same time; each gas path is It is equipped with a mass flow meter and an electromagnetic shut-off valve, so that the flow rate of the gas can be independently and precisely controlled; the gas to be introduced can be selected from an inert gas such as argon or nitrogen, a reducing gas such as hydrogen, an oxidizing gas such as oxygen, and a two-dimensional synthesis. The gaseous precursors required for the nanofilm are, for example, CH ₄ , C ₂ H ₄ , C ₂ H ₂ , NH ₃ , B ₃ N ₃ H ₆ or steam of ethanol.

At least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with a chemical vapor deposition system, including a plasma enhanced chemical vapor deposition system and a microwave plasma chemical vapor deposition system; Any one of the material chamber, the first film preparation chamber or the discharge chamber may form a chemical vapor deposition system with the heating device and the gas connection port, and the chemical vapor deposition system may be generally referred to as thermal chemical vapor deposition. system.

At least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with a physical vapor deposition system, and the physical vapor deposition system is a sputtering target thin film deposition system, an electron gun deposition system Any one or a combination of two or more of an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system.

Either one of the feed chamber, the first membrane preparation chamber or the discharge chamber may include both a chemical vapor deposition system and a physical vapor deposition system.

The temperature of at least one of the feed chamber, the first film preparation chamber or the discharge chamber is controlled at 20 to 1600 ° C;

Preferably, in order to concentrate heat at the sample and reduce transfer to a place where heat is not required, the chamber wall of at least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided Have a heat shielding system;

Preferably, in order to ensure safe and stable operation of the apparatus, the chamber wall of at least one of the feed chamber, the first film preparation chamber and the discharge chamber is provided with a cooling system, and the cooling system may be double-layer water-cooled system.

Preferably, the chamber is provided with a chamber of the heat shield system, while the chamber wall of the chamber is provided with a cooling system.

Preferably, the apparatus for large-scale continuous preparation of the two-dimensional nano-film of the present invention may further be provided with a control system including a sample transmission control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system. Any one or a combination of two or more.

The apparatus of the present invention can be used for growing a two-dimensional nano-film including graphene, metal chalcogenide, silicon dip, decene or boron nitride. According to the difference of the two-dimensional nano-film synthesized, the desired solid can be appropriately prepared. , precursors such as liquids or gases.

Preferably, the feed chamber serves as a surface treatment chamber, the first film preparation chamber serves as a preparation chamber for the substrate, the catalytic layer and the two-dimensional nano-film, and the discharge chamber serves as a cooling chamber or a two-dimensional nano-film. Processing chamber; the feed chamber is provided with a plasma surface processor, and the first film preparation chamber is provided with a thin film deposition system.

The basic process of large-scale continuous preparation of two-dimensional nano-films includes: placing a substrate material or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry, and transferring the sample transfer device to the first film through the feed chamber The chamber is prepared, and a two-dimensional nano-film is prepared by physical vapor deposition or chemical vapor deposition in the first film preparation chamber, and then the prepared two-dimensional nano film is sent from the sample transfer device to the discharge chamber.

The basic process of continuously preparing a two-dimensional nano film further includes: placing a substrate or a catalytic layer required for synthesizing a two-dimensional nano film on a loading gantry The sample transfer device is transferred to the feed chamber. Under a certain atmosphere, the substrate material or the catalytic layer is pretreated in the feed chamber, and then the substrate or catalytic layer is transferred to the first film by the sample transfer device. a catalytic layer, a carbon film or a two-dimensional nano-film is prepared by a physical vapor deposition or a chemical vapor deposition method in a first film preparation chamber; the film may be sent to a discharge chamber for heat treatment or processing by a sample transfer device. Surface optimization processing.

According to the different preparation conditions of the two-dimensional film, the technical solution adopted by the invention can also be as follows:

A scaled-up apparatus for continuously preparing a two-dimensional nanofilm includes a feed chamber, a first film preparation chamber, a first balance chamber, and a chemical vapor deposition chamber. In order to unify the terminology, the film preparation chamber is referred to as the first film preparation chamber, and the balance chamber is referred to as the first balance chamber. The balance chamber can serve as a transition, stable, and balanced sample during sample transfer. Functionality; The chemical vapor deposition chamber is also referred to as a thin film preparation chamber.

A sample transfer device is disposed between each of the feed chamber, the first thin film preparation chamber, the first balance chamber, and the chemical vapor deposition chamber, and the sample can be moved through the sample transfer device. The material chamber is continuously transferred to the first film preparation chamber, continuously transferred from the first film preparation chamber to the first balance chamber, and continuously transferred from the first balance chamber to the chemical vapor deposition chamber to realize the two-dimensional nano film Continuous preparation of the sample; the sample transfer device includes any one or a combination of two or more of a roller, a pulley, a conveyor belt, and the like.

The feed chamber is provided with a valve that communicates with the atmosphere, a valve is disposed between the feed chamber and the first film preparation chamber, and a valve is disposed between the first film preparation chamber and the first balance chamber. A valve is disposed between the first balance chamber and the chemical vapor deposition chamber, and the chemical vapor deposition chamber is provided with a valve that communicates with the atmosphere.

The feed chamber, the first film preparation chamber, the first balance chamber, and the chemical vapor deposition chamber are connected in one piece by a sample transfer device and a valve.

The first thin film preparation chamber is provided with a physical vapor deposition system including an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system. Any one or a combination of two or more of the systems.

The chemical vapor deposition chamber is provided with a heating device and a gas connection port;

The chemical vapor deposition chamber, the heating device and the gas connection port can constitute a simple chemical vapor deposition system;

Preferably, the chemical vapor deposition chamber is further provided with any one or a combination of two or more of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, and the like; The deposition chamber is provided with a valve that is open to the atmosphere, so the chemical vapor deposition chamber also functions as a discharge chamber.

At least one of the feed chamber, the first film preparation chamber and the first balance chamber is provided with a gas connection port; preferably, the feed chamber, the first film preparation chamber and the first balance The chambers are each provided with a gas connection port;

The gas connection port may be a gas connection port or a gas mixture box, and at least two or more gas paths may be connected in parallel to the inlet of the gas mixture box, so that two or more gases may be used. At the same time, the gas mixing box is entered; preferably, each gas path is independently connected with a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve, so that the flow rate of each gas can be independently and accurately controlled.

The feeding chamber, the first film preparing chamber, the first balancing chamber, and the chemical vapor deposition chamber are all provided with a vacuuming device, and each vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum By the vacuuming device, the vacuum of each chamber can be maintained at a normal pressure to between ^1.0 x 10 - ^{1 ()} Pa.

At least one of the feed chamber and the first film preparation chamber is provided with a sample processing device; preferably, the feed chamber and the first film preparation chamber are each provided with a sample processing device;

The sample processing device adopts a plasma surface processor, a wire ionizing or heating device for gas ionization, and the like, and the device for modifying the sample can be used under vacuum high frequency conditions. The ionization of the gas is realized; the heating device uses a resistance heating device, an infrared heating device, a laser heating device, and the like to realize heating of the sample.

Preferably, the temperature in the feed chamber, the first film preparation chamber and the chemical vapor deposition chamber can be controlled at 20 to 2000 ° C;

In order to concentrate heat at the sample, to reduce unnecessary heat transfer, at least one of the feed chamber, the first film preparation chamber and the chemical vapor deposition chamber is provided with an insulation shielding system; Only in the chamber where high temperature (such as higher than 40CTC) exists, there is an insulation shielding system.

In order to ensure safe and stable operation of the device, a cooling system is provided in the chamber wall of at least one of the feeding chamber, the first film preparation chamber and the chemical vapor deposition chamber, and the cooling system may be a double water cooling system or the like. Preferably, only the wall of the chamber in which a high temperature (e.g., 40 CTC) is present is provided with a cooling system.

Preferably, the apparatus for large-scale continuous preparation of two-dimensional nano-films of the present invention is further provided with a control system, and the control system comprises a sample transmission control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system. Any one or a combination of two or more.

Preferably, the feed chamber serves as a substrate and/or a chamber for processing the catalytic layer, the first film preparation chamber serves as a chamber for preparing a film of a two-dimensional nano film or a catalytic layer, and the chemical vapor deposition chamber serves as a cooling chamber. Or prepare a two-dimensional nano-film or a two-dimensional nano-film reprocessed chamber. The device of the invention can be used for growing various two-dimensional nano-films including graphene, metal chalcogenide, silicon thinner, germanium or boron nitride, and can be appropriately selected according to the difference of the two-dimensional nano film synthesized. Prepare the desired precursors such as solids, liquids or gases.

The basic process for continuously preparing a two-dimensional nano film comprises: placing a substrate and/or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry and transferring it from a sample transfer device to a feed chamber, in a certain atmosphere environment Substituting the substrate material and/or the catalytic layer in the feed chamber, and then transferring the substrate and/or the catalytic layer to the first thin film preparation chamber by the sample transfer device; utilizing in the first thin film preparation chamber The physical vapor deposition system prepares a two-dimensional nano-film or a catalytic layer film; the two-dimensional film preparation can also be prepared in a chemical vapor deposition chamber and then transferred to the atmosphere to complete the preparation.

An apparatus for continuously preparing a two-dimensional nano film by scale, characterized in that: a feeding chamber, a first processing chamber, a first balance chamber, a first film preparation chamber, and a second balance are sequentially disposed on a production line a chamber, a second processing chamber, and a discharge chamber. To unify the terminology, the film preparation chamber is referred to herein as the first film preparation chamber.

Wherein: the feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first processing chamber, and a valve is arranged between the first processing chamber and the first balancing chamber, the first balance a valve is disposed between the chamber and the first film preparation chamber, a valve is disposed between the first film preparation chamber and the second balance chamber, and a valve is disposed between the second balance chamber and the second processing chamber. a valve is disposed between the second processing chamber and the discharge chamber, and the discharge chamber is provided with a valve that is open to the atmosphere;

a sample transfer device, a sample, is provided between the feed chamber, the first processing chamber, the first balance chamber, the first thin film preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber Transfer from the atmosphere to the feed chamber by the sample transfer device, from the feed chamber to the first processing chamber, from the first processing chamber to the first balancing chamber, from the first balancing chamber to the first The film preparation chamber is transferred from the first film preparation chamber to the second balance chamber, from the second balance chamber to the second processing chamber, from the second processing chamber to the discharge chamber, and from the discharge The chamber is delivered to the atmosphere to effect continuous preparation of the two-dimensional nanofilm; the sample transport device includes any one or a combination of two or more of a roller, a pulley, and a conveyor belt. The balance chamber functions as a transition, stable, and balanced sample during sample transfer.

At least one of the feed chamber, the first processing chamber, the first membrane preparation chamber, the second processing chamber, and the discharge chamber is provided with a heating device to reach a certain temperature, such as 20 to 2000°. C _{; The} heating device may be a resistance heating device, an infrared heating device, a laser heating device, or the like.

At least one of the feed chamber, the first processing chamber, the first balancing chamber, the first membrane preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber is provided with one or a plurality of gas connection ports; the gas connection port may be a gas connection port, and the gas connection port may also be connected to the gas mixing box; the inlet of the gas mixture box has at least two or more gas paths connected in parallel, which may be two or The above gas enters the gas mixing box at the same time; the mass flow meter and the electromagnetic cut-off valve are used, so that each gas path can precisely control the flow rate of the gas; the gas to be introduced can be selected from inert gases such as Ar and N ₂ , reducing gas For example, H ₂ , an oxidizing gas such as 0 ₂ , a gas required for synthesizing a two-dimensional nano film such as CH ₄ , C ₂ H ₄ , C ₂ H ₂ , NH ₃ , B ₃ N ₃ H ₆ or a vapor of ethanol or the like.

The feed chamber, the first processing chamber, the first balance chamber, the first film preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber are respectively connected to independent vacuuming devices, each The vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be made to be between normal pressure and 1.0×10 ^{10 10} Pa by vacuuming.

For the purpose of better achieving the present invention, at least one of the first processing chamber, the first thin film preparation chamber, and the second processing chamber is provided with a physical vapor deposition system, the physical vapor deposition system Any one or a combination of two or more of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system is included.

For the purpose of better achieving the present invention, at least one of the first processing chamber, the first thin film preparation chamber, and the second processing chamber is provided with a chemical vapor deposition system including plasma enhanced chemical vapor deposition. System, aerosol-assisted chemical vapor deposition system, microwave plasma chemical vapor deposition system, etc.; any chamber (including first processing chamber, first membrane preparation chamber or second processing chamber), heating device and gas connection port Both can form a chemical vapor deposition system, which can be generally referred to as a thermal chemical vapor deposition system.

It is also possible to include both a chemical vapor deposition system and a physical vapor deposition system in the same chamber (the first thin film preparation chamber or the second processing chamber).

Various films can be prepared in the first film preparation chamber or the second processing chamber, such as a substrate material for synthesizing a two-dimensional nano film such as a graphene film, a catalytic layer material, a carbon film, and a two-dimensional nano film. The required precursors as well as two-dimensional nanofilms.

Preferably, in order to concentrate heat at the sample and reduce heat transfer to a place where heat is not required, at least one of the first processing chamber, the first film preparation chamber, and the second processing chamber The wall of the cavity is provided with a heat shielding system;

Preferably, in order to ensure safe and stable operation of the device, the cavity wall of at least one of the first processing chamber, the first film preparation chamber and the second processing chamber is provided with a cooling system, and the cooling system may be double Layer water cooling system.

Preferably, the first processing chamber is provided with a sample surface processor, and the surface processor may be a plasma surface processor, a thermal processor or the like. Preferably, the apparatus for continuously preparing a two-dimensional nano film of the present invention may further be provided with a control system, and the control system includes sample transmission control Any one or a combination of two or more of a system, a pneumatic control system, a vacuum control system, a valve control system, or a temperature control system. The apparatus of the present invention can be used to prepare two-dimensional nanofilms including graphene, metal chalcogenides, silenes, terpenes or boron nitride.

Preferably, the first processing chamber is used as a substrate surface processing chamber, the first thin film preparation chamber is used as a catalytic layer or a preparation chamber for a two-dimensional nano-film, and the second processing chamber is used as a cooling chamber for preparing a two-dimensional nano-film. Or a two-dimensional nanofilm reprocessing chamber.

The basic processes for preparing two-dimensional nano-films such as graphene films include, but are not limited to:

Using an automated control system, the substrate material or catalytic layer material required to synthesize a two-dimensional nanofilm such as a graphene film is placed on a carrier gantry, and from the feed chamber through the sample transfer device through the feed chamber and a valve of the processing chamber enters the first processing chamber; under a certain atmosphere, the substrate material or the catalytic layer material is first surface treated in the first processing chamber, and then passed through the first balancing chamber by the sample transfer device Transferring the substrate or catalytic layer material to the first thin film preparation chamber; preparing a catalytic layer, a carbon film, etc. for the two-dimensional nano-film by a physical deposition method or a chemical vapor deposition method in the first thin film preparation chamber; The transfer device is sent to the second balance chamber and then transferred to the second processing chamber. Under a certain atmosphere, the two-dimensional nano film is prepared in the second processing chamber; finally, the prepared two-dimensional nano film is sent by the sample transfer device. Discharge chamber. Depending on the function of each chamber, the two-dimensional nanofilm is either prepared in the first film preparation chamber or formed in the second processing chamber.

An apparatus for continuously preparing a two-dimensional nano film by scale, characterized in that: a feeding chamber, a first processing chamber, a first balance chamber, a first film preparation chamber, a second balance chamber, and a second film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a discharge chamber; in order to harmonize the terminology, the processing chamber is referred to herein as a first processing chamber; functionally, chemical vapor deposition The chamber may also be referred to as a thin film preparation chamber.

Wherein: the feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first processing chamber, and a valve is arranged between the first processing chamber and the first balancing chamber, the first balance a valve is disposed between the chamber and the first film preparation chamber, a valve is disposed between the first film preparation chamber and the second balance chamber, and a valve is disposed between the second balance chamber and the second film preparation chamber. a valve is disposed between the second film preparation chamber and the third balance chamber, a valve is disposed between the third balance chamber and the chemical vapor deposition chamber, and a chemical vapor deposition chamber is disposed between the discharge chamber and the discharge chamber The valve, the discharge chamber is provided with a valve that communicates with the atmosphere.

a feed chamber, a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a a sample transfer device is disposed in the chamber of the material chamber; the sample is transferred to the feed chamber through the sample transfer device, transferred from the feed chamber to the first processing chamber, and transferred from the first processing chamber to the first balance chamber Transfer from the first balance chamber to the first film preparation chamber, from the first film preparation chamber to the second balance chamber, from the second balance chamber to the second film preparation chamber, from the second The film preparation chamber is transferred to the third balance chamber, from the third balance chamber to the chemical vapor deposition chamber, and from the chemical vapor deposition chamber to the discharge chamber for continuous preparation of the two-dimensional nanofilm. The basic function of the feed chamber is to prepare the sample and enter the preparation device of the two-dimensional nano film, the first processing chamber realizes the pretreatment of the substrate or the catalytic layer, the first film preparation chamber and the second film preparation chamber It can be used to prepare substrates, catalytic layers, precursors of two-dimensional nano-films or two-dimensional nano-films required for the synthesis of two-dimensional nanomaterials. The chemical vapor deposition chamber can be used to prepare two-dimensional nano-films, and the equilibrium chamber is in the sample. It can function as a transition, stable, and balanced sample during transfer.

The sample transfer device includes any one or a combination of two or more of a roller, a pulley, a belt, and the like.

The entire apparatus passes the sample transfer device and the valve to the feed chamber, the first processing chamber, the first balance chamber, the first thin film preparation chamber, the second balance chamber, the second thin film preparation chamber, and the third balance chamber The chamber, the chemical vapor deposition chamber and the discharge chamber are connected in one piece.

a feed chamber, a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a At least one chamber in the material chamber is provided with a vacuuming device, and the vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be made to a normal pressure to 1.0 by a vacuuming device. Between x 10 - ^1Q Pa.

Preferably, the feed chamber, the first processing chamber, the first balance chamber, the first thin film preparation chamber, the second balance chamber, the second thin film preparation chamber, the third balance chamber, the chemical vapor deposition chamber The chamber and the discharge chamber are provided with independent vacuuming devices. Each vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be made at atmospheric pressure by the vacuuming device. To 1.0x l0 - ^1Q Pa.

A physical vapor deposition system is provided in a chamber of at least one of the first film preparation chamber and the second film preparation chamber for preparing a substrate, a catalytic layer, and a precursor of the two-dimensional nano film required for synthesizing the two-dimensional nano material The physical vapor deposition system includes any one or two of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system. More than one combination.

Chamber of a chemical vapor deposition chamber is provided with heating means in order to reach a certain temperature, for example 20 ~ 2000 ° _C; heating means may be resistance heating means, infrared heating means, laser heating means and the like.

a feed chamber, a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a At least one of the chambers is provided with one or more gas connections.

The gas connection port may be a gas connection port, and the gas connection port may also be connected to the gas mixing box; the inlet of the gas mixture box is connected at least in parallel Two or more gas paths allow two or more gases to enter the gas mixing chamber at the same time; preferably, each gas path is independently connected with a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve. In order to achieve independent and precise control of the flow rate of each gas.

The gas to be introduced may be selected from inert gases such as Ar and N ₂ , reducing gases such as H ₂ , oxidizing gases such as ₀₂ , and gases required to synthesize two-dimensional nanofilms such as CH ₄ , C ₂ H ₄ , C ₂ H ₂ , NH ₃ , B ₃ N ₃ H ₆ or steam of ethanol, etc., depending on the two-dimensional film to be synthesized, different gases can be appropriately selected.

The chemical vapor deposition chamber, the heating device and the gas connection port may constitute a chemical vapor deposition system; a chemical vapor deposition system may also be disposed in the chemical vapor deposition chamber, and the chemical vapor deposition system is plasma enhanced chemical vapor deposition Any one or a combination of two systems, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, and an inductively coupled plasma chemical vapor deposition system.

The first film preparation chamber, the second film preparation chamber or the first treatment chamber may be combined with the heating device and the gas connection port respectively to form a chemical vapor deposition system;

Preferably, both the chemical vapor deposition system and the physical vapor deposition system are provided in the first film preparation chamber, the second film preparation chamber, the first processing chamber or the chemical vapor deposition chamber.

Preferably, at least one of the first processing chamber, the first film preparation chamber and the second film preparation chamber is provided with heating means to reach a certain temperature, such as 20 to 2000 ° C; It may be a resistance heating device, an infrared heating device, a laser heating device, or the like.

Preferably, the first processing chamber is provided with a sample processing device, and the sample processing device is a plasma sample processing device, a wire enthalpy or a heating device for gas ionization, and the like, which can modify the sample. The wire enthalpy for gas ionization can realize ionization of gas under vacuum high-frequency conditions; the heating device is a device capable of heating the sample, such as a resistance heating device, an infrared heating device, and a laser heating device.

Preferably, in order to concentrate heat at the sample and reduce heat transfer to places where heat is not required, the first processing chamber, the first film preparation chamber, the second film preparation chamber, and the chemical vapor deposition chamber At least one chamber in the chamber is provided with a heat shield system; preferably, only a heat shield system is provided in the chamber where high temperature (e.g., above 400 °C) is present.

Preferably, in order to ensure safe and stable operation of the apparatus, the chamber walls of at least one of the first processing chamber, the first thin film preparation chamber, the second thin film preparation chamber and the chemical vapor deposition chamber are cooled. System; preferably, only the wall of the chamber in which a high temperature (e.g., above 40 CTC) is present is provided with a cooling system.

Preferably, the chamber of at least one of the first processing chamber, the first thin film preparation chamber, the second thin film preparation chamber and the chemical vapor deposition chamber is provided with a cavity of the heat shielding system. The chamber wall is also equipped with a cooling system.

Preferably, the complete set of equipment is further provided with a control system for controlling the equipment or the process, and the control system includes any one of a sample transfer control system, a gas path control system, a vacuum control system, a valve control system or a temperature control system. One or a combination of two or more.

The device of the invention can continuously prepare a two-dimensional nano film by scale, and the two-dimensional nano film comprises graphene, metal chalcogenide, silicon thinner, germanium or boron nitride film.

Preferably, the first processing chamber serves as a surface treatment chamber for the substrate and/or the catalytic layer, the first thin film preparation chamber serves as a preparation chamber for the catalytic layer, and the second thin film preparation chamber serves as a substrate and/or catalyst A preparation chamber for preparing a precursor for a two-dimensional nano-film on a layer, and a chemical vapor deposition chamber as a chamber for processing the precursor to form a two-dimensional nano-film.

In the preparation of two-dimensional nano-films, the functions of the chambers of the present invention vary depending on the preparation process conditions due to differences in the selected substrate, catalytic layer, and process, etc., in different preparation processes. Conditions may assume multiple functions at the same time, or may not assume specific functions.

Components disposed in or connected to the chambers such as valves, gas ports, sample processors, heaters, physical vapor deposition systems, chemical vapor deposition systems, thermal barrier systems, cooling systems, etc. may be prepared according to The specific process of the nano-film is set at different positions of each chamber, and the relevant components can be selectively selected according to a specific process.

A precursor of a two-dimensional nanomaterial refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, for preparing a graphene, the precursor includes an amorphous carbon, an amorphous carbon film, and a carbon target. Materials, carbon-containing polymers, etc.; for the synthesis of MoS ₂ as an example, the precursor includes a MoS ₂ target, a Mo target, a sulfur powder, and the like.

The basic processes for large-scale continuous preparation of two-dimensional nano-films include, but are not limited to:

The substrate and/or catalytic layer required for synthesizing the two-dimensional nanofilm is placed on the loading rack and transferred from the feeding chamber to the first processing chamber by the sample conveying device; under certain atmosphere, the lining The bottom and/or catalytic layer is processed in the first processing chamber, and then the substrate and/or catalytic layer is transported by the sample transfer device to the first thin film preparation chamber through the first balancing chamber; in the first thin film preparation chamber The catalytic layer required for the growth of the two-dimensional nano-film is prepared by a physical vapor deposition method or a chemical vapor deposition method; and then sent to the second thin film preparation chamber through the second balance chamber through the sample transfer device under a certain atmosphere Preparing a two-dimensional nanofilm on the substrate and/or the catalytic layer. After the two-dimensional nano-film is prepared in the second film preparation chamber, the two-dimensional nano-film preparation device is transported through the third balance chamber, the chemical vapor deposition chamber, and the discharge chamber. The basic process for preparing a two-dimensional nano film may also be: placing a substrate and/or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry and transferring it from the feed chamber to the first by a sample transfer device Processing the chamber; under a certain atmosphere, the substrate and/or the catalytic layer are processed in the processing chamber, and then the substrate and/or the catalytic layer are transported to the first film by the sample transfer device through the first balancing chamber. a chamber for preparing a catalytic layer required for growth of a two-dimensional nano-film by a physical vapor deposition method or a chemical vapor deposition method in a first film preparation chamber; and then passing through a second balance chamber and being sent to a second by a sample transfer device a thin film preparation chamber for preparing a precursor for growth of a two-dimensional nano-film on a substrate and/or a catalytic layer under a certain atmosphere; after the precursor is prepared, the sample transfer device is transported to the chemical through the third equilibrium chamber A two-dimensional nano-film is prepared by a vapor deposition chamber; after the preparation of the two-dimensional nano-film, a two-dimensional nano-film preparation device is transported through the discharge chamber.

In order to achieve control of the equipment or process of each chamber, the entire equipment is also provided with a control system, which includes a sample transfer control system, a pneumatic control system, a vacuum control system, a valve control system or a temperature control system. Any one or a combination of two or more.

The device of the invention is suitable for large-scale continuous preparation of all two-dimensional nano-films, including the graphene, the metal chalcogenide, the silene, the terpene or the boron nitride film, etc., according to the prepared Different from the nano-film, the solid, liquid or gas required for preparing the two-dimensional nano film can be appropriately selected.

Preparation of two-dimensional film must meet certain conditions: For example, a higher temperature, such as 400 ° C, is required. A certain catalytic layer, such as a graphene film, is required to use a transition metal such as Ni or Cu as a catalyst and a crystal structure of the catalytic layer. For optimization, it is necessary to control the atmosphere and vacuum degree of the preparation chamber; equipment for continuously preparing a two-dimensional film must satisfy these conditions or achieve these functions, and is an integrated device. However, the existing process equipment cannot meet these basic conditions, and therefore cannot be used to continuously prepare a high-quality two-dimensional film; the combination of each chamber and device in the equipment of the present invention can satisfy the continuous preparation of a two-dimensional film. Different process technology requirements enable continuous production of high quality 2D films.

Compared with the prior art, the beneficial effects of the invention are as follows: The whole equipment is provided with a sample transfer device capable of withstanding high temperature, and has the characteristics of large-scale continuous preparation of two-dimensional nano-films, and each chamber is in the whole process of preparing the two-dimensional nano-film. Take on its unique features. For example: The basic function of the feed chamber is to prepare the sample and enter the preparation device of the two-dimensional nano-film. The processing chamber is used to pre-treat the substrate or the catalytic layer. The thin film preparation chamber can be used to prepare the synthetic two-dimensional nano material. The required substrate, catalytic layer, precursor of two-dimensional nano-film or two-dimensional nano-film, chemical vapor deposition chamber can be used to prepare two-dimensional nano-film, balance chamber can be transition and stable during sample transfer , balance the function of the sample. The device of the invention can continuously prepare a two-dimensional nano film such as graphene, metal chalcogenide, silylene, decene or boron nitride film in a large area and large scale, and is suitable for industrial application, and is beneficial to realize two-dimensional nano film. Industrialization of technology.

BRIEF DESCRIPTION OF THE DRAWINGS:

1 is a schematic view showing the overall structure of a large-scale continuous preparation of a two-dimensional nano-film apparatus according to the present invention, wherein a first film preparation chamber is provided with a heating device;

2 is a schematic view showing the overall structure of a large-scale continuous preparation of a two-dimensional nano-film apparatus according to the present invention, wherein the first film preparation chamber and the discharge chamber are each provided with a heating device, and the discharge chamber is provided with a heat shielding system. And a cooling system, the discharge chamber is provided with a gas mixing box connection;

3 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, and the first film preparation chamber is provided with a vapor deposition system, a heating device, and a heat The shielding system and the cooling system, the discharge chamber is provided with a heating device; FIG. 4 is a schematic view of the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor and heating The first thin film preparation chamber is provided with a vapor deposition system, a heating device, a heat shielding system and a cooling system, and the discharge chamber is provided with a heating device;

5 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor and a heating device, and the first film preparation chamber is provided with a vapor deposition system and heating. The device, the heat shield system and the cooling system, the discharge chamber is provided with a surface processor, a heating device and a cooling system.

6 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention;

7 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feed chamber is provided with a sample processing device, and the first film preparation chamber is provided with a sample processing device and a cooling system, and chemistry The vapor deposition chamber is provided with a chemical vapor deposition system, an insulation shielding system and a cooling system;

8 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a sample processing device and a heat shielding system, and the first film preparation chamber is provided with heat shielding. The system, the cooling system, the gas mixing box connection port and the sample processing device, the chemical vapor deposition chamber is provided with a chemical vapor deposition system, an insulation shielding system and a gas mixing box connection port.

9 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor and a heating device, and the first processing chamber is provided with a heating device and a gas mixture. a box interface, the first film preparation chamber is provided with a heating device and a heat shielding device, and the second processing chamber is provided with a heating device, a heat shielding device, a cooling device and a gas mixing box interface;

10 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, and the first processing chamber is provided with a heating device, a heat shielding device and cooling Device, the first film preparation chamber is provided with a physical vapor deposition system, heating a device and a gas mixing box connection port, the second processing chamber is provided with a heating device, a heat shielding shielding device, a cooling device and a gas mixing box connection port, and the chamber is provided with a surface processor;

11 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, and the first processing chamber is provided with a heating device, a heat shielding device and cooling The first film preparation chamber is provided with a physical vapor deposition system, a heating device, a heat shielding device, a cooling device and a gas mixing box connection port, and the second processing chamber is provided with a heating device, a heat shielding device, and a cooling device. And a gas mixing box connection;

12 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the feeding chamber is provided with a surface processor, the first processing chamber is provided with a heating device, and the first film preparation chamber is provided. A physical vapor deposition system, a heating device and a gas mixing box connection port are provided, and the second processing chamber is provided with a heating device, a heat shielding device, a cooling device and a gas mixing box connection port, and the discharge chamber is provided with a surface treatment Figure 13 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment of the present invention, wherein the feeding chamber is provided with a surface processor, the first processing chamber is provided with a heating device, and the first film is prepared. The chamber is provided with a physical vapor deposition system, a heating device, a heat shielding device, a cooling device and a gas mixing box connection port, and the second processing chamber is provided with a heating device and a gas mixing box connection port.

14 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the first processing chamber is provided with a heating device, a heat shielding system and a cooling system, and the first film preparation chamber is provided a heating device and a physical vapor deposition system, the second film preparation chamber is provided with a heating device and a physical vapor deposition system, the chemical vapor deposition chamber is provided with a sample processing device, a heating device, a heat shielding system, a cooling system and a gas mixing box Interface

15 is a schematic view showing the overall structure of a large-scale continuous preparation of two-dimensional nano-film equipment according to the present invention, wherein the first processing chamber is provided with a heating device and a sample processing device, and the first film preparation chamber is provided with a physical vapor deposition system. The heating device, the heat shielding system and the gas mixing box connection port, the second film preparation chamber is provided with a heating device and a physical vapor deposition system, and the chemical vapor deposition chamber is provided with a chemical vapor deposition system, a heating device, and an insulation shielding system. , cooling system and air box interface;

16 is a schematic view showing the overall structure of a large-scale continuous preparation of a two-dimensional nano-film apparatus according to the present invention, wherein a first processing chamber is provided with a sample processing device, and a first thin film preparation chamber is provided with a physical vapor deposition system and a heating device. The second film preparation chamber is provided with a heating device, a heat shielding system, a cooling system and a physical vapor deposition system, and the chemical vapor deposition chamber is provided with a sample processing device, a heating device, a heat shielding system, a cooling system and a gas mixing box. Interface, the discharge chamber is provided with a sample processing device;

The figure shows:

Feed chamber 1, first processing chamber 2, first balance chamber 3, first film preparation chamber 4, second balance chamber 5, second film preparation chamber 6, third balance chamber 7, a chemical vapor deposition chamber 8, a second processing chamber 201, a discharge chamber 9;

Valves 10, 11, 12, 13, 14, 15, 16, 17, 18, 19;

Vacuuming device 20, 21, 22, 23, 24, 25, 26, 27, 28;

Loading platform 29;

Sample transfer device 30;

Physical vapor deposition system 33, 34, 35, 36;

Chemical vapor deposition system 38, 39;

Heating means 40, 41, 42, 43, 44;

Sample processing device 50, 51, 52;

Gas connection ports 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 78, 79, 80; air mixing boxes 85, 86, 87;

Cooling system 90, 91, 92;

Thermal insulation shielding system 96, 97, 98, 99;

Vapor deposition system 101, 102.

detailed description

In order to more clearly understand the technical effects produced by the present invention and the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

Example 1

Referring to Figure 1, a scaled continuous preparation of a two-dimensional nanofilm apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a roller 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 A valve 11 is disposed, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber is passed through the roller and the valve. The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.

A second heating device 40 is disposed in the first film preparation chamber 4. The feed chamber 1 is provided with a vacuuming device 20, the first film preparation chamber 4 is provided with a vacuuming device 21, and the discharge chamber 9 is provided with a vacuuming device 22. The feed chamber 1 is provided with a gas connection port 60, the first film preparation chamber 4 is provided with two gas connection ports 61, 62, and the discharge chamber 9 is provided with a gas connection port 63. In order to accurately control the flow rate of the gas, each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each of the mass flow meters is provided with an electromagnetic cut-off valve at both ends thereof, and the electromagnetic cut-off valve and the mass flow meter pass through the pipeline. Connected to the gas connection.

The first film preparation chamber 4, the second heating means 40 and the gas connection ports 61, 62 constitute a chemical vapor deposition system which is generally referred to as a thermal chemical vapor deposition system.

The basic process for continuously preparing a two-dimensional nano film is: placing a substrate material and/or a catalytic layer material required for synthesizing a two-dimensional nano film on a carrier gantry 29, and transferring the roller 30 through the feeding chamber 1 to the first A film preparation chamber 4 is prepared in the first film preparation chamber 4 by a chemical vapor deposition method, and the sample is prepared and sent to the discharge chamber 9 by the roller 30.

Example 2

Referring to FIG. 2, a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a pulley 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 a valve 11 is provided, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 which is open to the atmosphere; the feed chamber 1 is passed through the pulley and the valve, The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.

A second heating device 40 is disposed in the first film preparation chamber 4, and a third heating device 41 is disposed in the discharge chamber 9.

Since the temperature of the chamber of the discharge chamber 9 may be as high as several hundred degrees or even thousands of degrees, in order to improve the utilization of heat, a heat shielding system 96 is provided in the chamber, and a cooling system 90 is provided in the chamber wall to prevent the chamber wall from being overheated. .

The feeding chamber 1 is provided with a vacuuming device 20, the first film preparing chamber 4 is provided with a vacuuming device 21, and the discharging chamber 9 is provided with a vacuuming device 22. The feed chamber 1 is provided with a gas connection port 60, the first film preparation chamber 4 is provided with a gas connection port 61, and the discharge chamber 9 is provided with a gas connection port 68 connected to an air mixing box 85, the air mixing box The inlet of 85 is connected in parallel with two gas connection ports 66, 67; each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic shut-off valve, an electromagnetic cut-off valve and The mass flow meter is connected to the gas mixing box or the gas connection port through the pipeline, so that the flow rate of the gas can be precisely controlled.

The discharge chamber 9, the third heating means 41 and the gas connection port 63, and the gas mixture tank 85 constitute a chemical vapor deposition system which is generally referred to as a thermal chemical vapor deposition system.

The basic process for continuously preparing a two-dimensional nano film is: placing a substrate material and/or a catalytic layer material required for synthesizing a two-dimensional nano film on a carrier gantry 29, and transferring it from the pulley 30 through the feeding chamber 1 a film preparation chamber 4, the substrate/catalyst layer is heat-treated in the first film preparation chamber 4, and then transported by the pulley 30 to the discharge chamber 9, and a two-dimensional nano film is prepared by chemical vapor deposition, and a two-dimensional nano film is prepared. After preparation, it is conveyed by the pulley sample conveying device to the outside of the discharge chamber 9.

Example 3

Referring to FIG. 3, a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a roller 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 a valve 11 is provided, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber 1 is fed through the roller and the valve, The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.

A first surface processor 50 is disposed in the feed chamber 1, a second heating device 40 is disposed in the first film preparation chamber 4, and a third heating device 41 is disposed in the discharge chamber 9.

The first film preparation chamber 4 is provided with two vapor deposition systems: a first vapor deposition system 101 and a second vapor deposition system 102, which may be any combination of a physical gas phase system and a chemical vapor deposition system.

The first vapor deposition system or the second vapor deposition system is a physical vapor deposition system, including any one of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system. Or a combination of two or more; the first vapor deposition system or the second vapor deposition system may also be a chemical vapor deposition system, including any one or two of a plasma enhanced chemical vapor deposition system and a microwave plasma chemical vapor deposition system. The combination above.

Since the temperature of the first film preparation chamber 4 may be as high as several hundred degrees or even thousands of degrees, in order to concentrate the heat in a desired place and reduce the transfer to a place where heat is not required, the first film preparation chamber is provided with heat. The system 96 is shielded while the chamber wall is provided with a cooling system 90, which may be a dual layer water cooling system.

The feed chamber 1 is provided with a vacuuming device 20, the first film preparation chamber 4 is provided with a vacuuming device 21, and the discharge chamber 9 is provided with a vacuuming device 22. The feed chamber 1 is provided with a gas connection port 60, and the discharge chamber 9 is provided with a gas connection port 63; the first film preparation chamber 4 is provided with two gas connection ports, one of which has a connection port of 61, the other The connection port 68 is connected to the air mixing box 85, and the inlet of the air mixing box 85 is connected in parallel with three gas connections. Ports 62, 64 and 65; In order to accurately control the flow rate of the gas, each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic cut-off valve, an electromagnetic cut-off valve And the mass flow meter is connected to the gas mixing box or the gas connection port through a pipeline.

The basic process for continuously preparing a two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the loading stage 29 and transferring it to the feeding chamber 1 by the roller 30, under a certain atmosphere, lining The bottom material is pretreated in the feed chamber 1, and then the substrate material is transferred by the roller 30 to the first film preparation chamber 4; the physical vapor phase is utilized in the first vapor deposition system 101 in the first film preparation chamber 4. The deposition method is prepared by electron gun deposition to prepare a catalytic layer, and then a second physical vapor deposition method such as ion implantation is used in the second vapor deposition system 102 to inject a precursor of the two-dimensional nano material into the catalytic layer, and then transferred to the discharge chamber. Chamber 9; In the discharge chamber 9, a sample implanted with a precursor of a two-dimensional nanomaterial is processed to form a two-dimensional nanofilm.

Example 4

Referring to FIG. 4, a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a roller 30 for conveying a sample; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, between the feed chamber 1 and the first film preparation chamber 4 a valve 11 is provided, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber 1 is fed through the roller and the valve, The first film preparation chamber 4 and the discharge chamber 9 are connected in one piece.

A first surface processor 50 and a first heating device 42 are disposed in the feed chamber 1, a second heating device 40 is disposed in the first film preparation chamber 4, and a third heating device 41 is disposed in the discharge chamber 9.

The first film preparation chamber 4 is provided with a first vapor deposition system 101, which is a physical vapor deposition system or/and a chemical vapor deposition system, and the physical vapor deposition system includes a sputtering target film deposition. Any one or a combination of two or more of a system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; the chemical vapor deposition system including a plasma enhanced chemical vapor deposition system and microwave plasma A chemical vapor deposition system or the like; a physical vapor deposition system and a chemical vapor deposition system can be arbitrarily combined.

The feeding chamber 1 is provided with a vacuuming device 20, the first film preparing chamber 4 is provided with a vacuuming device 21, and the discharging chamber 9 is provided with a vacuuming device 22. The feed chamber 1 is provided with a gas connection port 60, the discharge chamber 9 is provided with a gas connection port 63, and the first film preparation chamber 4 is provided with two gas connection ports 61, 62, each of which is connected to the gas connection port. There is a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic cut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through the pipeline.

The discharge chamber 9, the discharge chamber heating device 41, and the gas connection port 63 constitute a chemical vapor deposition system.

The basic process for continuously preparing a two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the loading stage 29 and transporting it by the roller 30 to the feeding chamber 1, under a certain atmosphere and temperature Next, the substrate material is pretreated in the feed chamber 1, and then the substrate material is transferred by the roller 30 to the first film preparation chamber 4; in the first film preparation chamber 4, a physical vapor deposition method or/and The catalytic layer is prepared by a chemical vapor deposition method and then transferred to a discharge chamber 9, where a two-dimensional nanofilm is prepared by chemical vapor deposition.

Example 5

Referring to Figure 5, a scaled continuous preparation of a two-dimensional nanofilm apparatus of the present invention comprises: a feed chamber 1, a first film preparation chamber 4, a discharge chamber 9; a complete set of equipment in the feed chamber 1, A film preparation chamber 4 and a discharge chamber 9 are each provided with a sample conveyor belt 30; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided. a valve 11, a valve 12 is disposed between the first film preparation chamber 4 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 13 that communicates with the atmosphere; the feed chamber 1 is fed through the conveyor belt and the valve, first The film preparation chamber 4 and the discharge chamber 9 are connected in one piece.

A first surface processor 50 and a first heating device 42 are disposed in the feed chamber 1, a second heating device 40 is disposed in the first film preparation chamber 4, and a second surface processor 51 is disposed in the discharge chamber 9. And a third heating device 41.

The first thin film preparation chamber 4 is provided with a first vapor deposition system 101, which is a physical vapor deposition system or/and a chemical vapor deposition system, and the physical vapor deposition system includes a sputtering target thin film deposition. Any one or a combination of two or more of a system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; the chemical vapor deposition system including a plasma enhanced chemical vapor deposition system and microwave plasma A chemical vapor deposition system or the like; a physical vapor deposition system and a chemical vapor deposition system can be arbitrarily combined.

A heat shield system 96 is provided in the first film preparation chamber 4 to reduce heat transfer to an undesired place, and the chamber wall is provided with a cooling system 90 to prevent overheating of the chamber wall.

The discharge chamber 9 is provided with a cooling system 90 due to the presence of high temperatures.

The feed chamber 1 is provided with a vacuuming device 20, the first film preparation chamber 4 is provided with a vacuuming device 21, and the discharge chamber 9 is provided with a vacuuming device 22. The feed chamber 1 is provided with a gas connection port 60, and the discharge chamber 9 is provided with a gas connection port 63; the first film preparation chamber 4 is provided with two a gas connection port, one of the connection ports is 61, the other connection port 68 is connected to the air mixing box 85, and the inlet of the air mixture box 85 is connected in parallel with three gas connection ports 62, 64 and 65; in order to precisely control the flow of the gas, each The gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided with an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter pass through the pipeline and the gas mixing box or the gas connection port. connection.

The feed chamber 1, the heating device 42 and the gas connection port 60 constitute a chemical vapor deposition system; the discharge chamber 9, the heating device 41 and the gas connection port 63 constitute a chemical vapor deposition system.

The basic process for continuously preparing a two-dimensional nano film is to place the substrate material required for synthesizing the two-dimensional nano film on the carrier gantry 29 and transport it to the feed chamber 1 by the conveyor belt 30, under a certain atmosphere and temperature. The substrate material is pretreated in the feed chamber 1, and then the substrate material is transferred by the conveyor belt 30 to the first film preparation chamber 4; the physical vapor deposition method or/and the chemistry is utilized in the first film preparation chamber 4. The catalytic layer is prepared by a vapor deposition method, and then a two-dimensional nano film is prepared by a chemical vapor deposition method; the prepared two-dimensional nano film is transported by a sample transfer device to a discharge chamber 9, which can be surface-treated in the discharge chamber 9. .

Example 6

Referring to FIG. 6, a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feeding chamber 1, a first film preparing chamber 4, a first balancing chamber 3, a chemical vapor deposition chamber 8, and a whole set of equipment. a sample transfer device 30 is disposed between each of the chambers of the feed chamber 1, the first thin film preparation chamber 4, the first balance chamber 3, and the chemical vapor deposition chamber 8 and the chamber; The device comprises any one or a combination of two or more of a roller, a pulley and a conveyor belt; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided a valve 12 is disposed between the first film preparation chamber 4 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the chemical vapor deposition chamber 8. The chemical vapor deposition chamber 8 is provided. A valve 14 is provided which is open to the atmosphere; the feed chamber 1, the first film preparation chamber 4, the first balance chamber 3 and the chemical vapor deposition chamber 8 are connected together by a sample transfer device and a valve.

The feeding chamber 1 is provided with a vacuuming device 21, the first film preparing chamber 4 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the chemical vapor deposition chamber 8 is provided with a vacuuming device 24; Each vacuuming device includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be maintained at a normal pressure to 1.0 x 10 - 1 ^Q Pa by a vacuuming device.

A sample processor device 51 is disposed in the first film preparation chamber 4, and the sample processing device may be a plasma surface processor, a wire ionizing device for gas ionization or a heating device, etc., capable of realizing modification of the sample. In the example, the sample processor device 51 is a heating device, and the heating device uses a resistance heater, an infrared heater, and a laser heater to implement a device for heating the sample; the first film preparation chamber 4 is further provided with a physical vapor deposition system. 33. The physical vapor deposition system comprises any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system.

The chemical vapor deposition chamber 8 is provided with a heating device 40 which is a device which can heat the sample by using an electric resistance heater, an infrared heater and a laser heater.

The feed chamber 1 is provided with a gas connection port 60, the first film preparation chamber 4 is provided with gas connection ports 61 and 62, the first balance chamber 3 is provided with a gas connection port 63, and the chemical vapor deposition chamber 8 is provided with a gas. The connecting ports 64 and 75, the gas connecting port 75 are connected to the air mixing box 85, and the air mixing box 85 is connected to the two gas connecting ports 66 and 67; each gas path is independently provided with a metering and flow regulating device such as a mass flow meter and an electromagnetic cut-off valve. Therefore, the flow rate of the gas is precisely controlled. For example, each gas connection port is connected with a mass flow meter to control the flow rate of each gas. Each of the mass flow meters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic cut-off valve and the mass flow meter pass The line is connected to the gas connection.

The chemical vapor deposition chamber 8, the heating device 40 and the gas connection ports 64 and/or 75 constitute a chemical vapor deposition system.

The first film preparation chamber 4, the sample processing device 51 and the gas connection ports 61 and/or 62 may also constitute a chemical vapor deposition system. The basic process for continuously preparing a two-dimensional nanofilm is: placing the substrate required for synthesizing the two-dimensional nanofilm and/or placing it on the carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1, and then transferring it to a first film preparation chamber 4; at a certain temperature, a catalytic layer is prepared on the substrate and/or the catalytic layer in the first film preparation chamber 4 by a physical vapor deposition system such as an electron beam deposition system 33, and then passes through the first The chamber 3 is transferred to the chemical vapor deposition chamber 8; a two-dimensional nano-film is prepared by a chemical vapor deposition system in the chemical vapor deposition chamber 8, and the two-dimensional film is prepared, and then passed through the valve 14 to the atmosphere to complete the two-dimensional film. A process for continuous preparation.

Example 7

Referring to FIG. 7, a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feeding chamber 1, a first film preparation chamber 4, a first balance chamber 3, a chemical vapor deposition chamber 8, and a whole set of equipment. a sample transfer device 30 is disposed between each of the chambers of the feed chamber 1, the first thin film preparation chamber 4, the first balance chamber 3, and the chemical vapor deposition chamber 8 and the chamber; The device comprises any one or a combination of two or more of a roller, a pulley and a conveyor belt; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided a valve 12 is disposed between the first film preparation chamber 4 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the chemical vapor deposition chamber 8. The chemical vapor deposition chamber 8 is provided. A valve 14 is provided which is open to the atmosphere; the feed chamber 1, the first film preparation chamber 4, the first balance chamber 3 and the chemical vapor deposition chamber 8 are connected together by a sample transfer device and a valve.

The feeding chamber 1 is provided with a vacuuming device 21, the first film preparing chamber 4 is provided with a vacuuming device 22, and the first balancing chamber 3 is provided with a vacuuming device 23, the chemical vapor deposition chamber 8 is provided with a vacuuming device 24; each vacuuming device comprises various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum degree of each chamber can be kept constant by the vacuuming device Press between 1.0x 10 - ^1Q Pa.

The feeding chamber 1 is provided with a sample processing device 50, which may be a plasma surface processor, a surface processor composed of a gas ionization coil, and a heating device capable of modifying the sample, and the heating device adopts a resistor. A device that can heat a sample, such as a heater, an infrared heater, and a laser heater.

A sample processor device 51 is disposed in the first film preparation chamber 4. The sample processing device may be a plasma surface processor, a device for modifying a sample such as a gas ionization coil or a heating device, where the sample is The processor device 51 is a heating device, and the heating device uses a device capable of heating the sample, such as a resistance heater, an infrared heater, and a laser heater; the first film preparation chamber 4 is further provided with physical vapor deposition systems 33 and 34, The physical vapor deposition system includes any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system; A cooling system 90 is also provided in the film preparation chamber 4.

The chemical vapor deposition chamber 8 is provided with a heating device 40, which is a device capable of heating a sample, such as a resistance heater, an infrared heater and a laser heater; the chemical vapor deposition chamber 8 is further provided with a chemical vapor deposition system 38, The chemical vapor deposition system includes any one or a combination of two or more of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, and an aerosol assisted chemical vapor deposition system; the chemical vapor deposition chamber 8 further An insulation shielding system 96 and a cooling system 91 are provided, and the cooling system may be a double water cooling system or the like.

In addition to the separate chemical vapor deposition system 38, the chemical vapor deposition chamber 8, the heating device 40 and the gas connections 64 and/or 75 may also constitute a simple chemical vapor deposition system.

The first film preparation chamber 4, the sample processing device 51 and the gas connection ports 61 and/or 62 may also constitute a chemical vapor deposition system. The basic process for continuously preparing a two-dimensional nano film is: placing a substrate and/or a catalytic layer required for synthesizing a two-dimensional nano film on a carrier gantry 29, and transferring it from the sample transfer device 30 to the feed chamber 1; The feed chamber 1 processes the surface of the sample by the sample processing device 50, and after surface treatment, transfers to the first film preparation chamber 4; at a certain temperature, the first film preparation chamber 4 utilizes a physical vapor deposition system such as The thermal evaporation deposition system 33 prepares a catalytic layer on the substrate and/or the catalytic layer, and then injects a precursor required for preparing the two-dimensional nano film into the catalytic layer by a physical vapor deposition system such as an ion implantation deposition system 34, and then passes through The first balance chamber 3 is transferred to the chemical vapor deposition chamber 8; the precursor of the two-dimensional nano-film is converted into a two-dimensional nano-film by heat treatment in the chemical vapor deposition chamber 8, and the two-dimensional film is prepared and passed through the valve 14 A process for the continuous preparation of a two-dimensional film to the atmosphere. The precursor of the two-dimensional nano material is a compound containing an element constituting the two-dimensional nano material, and the synthesis of graphene includes, for example, an amorphous carbon, an amorphous carbon film, a carbon-containing polymer, etc.; to synthesize MoS ₂ As an example, the precursor includes MoS ₂ powder, Mo powder, and the like.

The basic process of continuously preparing the two-dimensional nano film may also be: placing the substrate and/or the catalytic layer required for synthesizing the two-dimensional nano film on the loading stage 29, and transferring it from the sample conveying device 30 to the feeding chamber 1 The surface of the sample is processed in the feed chamber 1 by the sample processing device 50, and then surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, physical vapor deposition is performed in the first film preparation chamber 4. A system such as laser deposition system 33 prepares a catalytic layer on the substrate and/or catalytic layer, which is then passed through first diffusion chamber 3 to chemical vapor deposition chamber 8; in chemical vapor deposition chamber 8, a chemical vapor deposition system is employed. A two-dimensional nanofilm is prepared by a microwave plasma chemical vapor deposition technique. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process for continuous preparation of the two-dimensional film.

The basic process for continuously preparing a two-dimensional nano film may also be: placing a substrate required for synthesizing a two-dimensional nano film on a carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1; in the feed chamber The chamber 1 processes the surface of the sample by the sample processing device 50, and is surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, the first film preparation chamber 4 is deposited by a physical vapor deposition system such as sputtering. Systems 33 and 34 prepare a catalytic layer on the substrate and/or catalytic layer, which is then passed through a first balancing chamber 3 to a chemical vapor deposition chamber 8; in a chemical vapor deposition chamber 8, a chemical vapor deposition system such as an aerosol is employed. A two-dimensional nanofilm is prepared by an auxiliary chemical vapor deposition technique. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process of continuous preparation of the two-dimensional film.

Example 8

Referring to FIG. 8, a scaled continuous preparation two-dimensional nano film apparatus of the present invention comprises: a feeding chamber 1, a first film preparing chamber 4, a first balancing chamber 3, a chemical vapor deposition chamber 8, and a whole set of equipment. a sample transfer device 30 is disposed between each of the chambers of the feed chamber 1, the first thin film preparation chamber 4, the first balance chamber 3, and the chemical vapor deposition chamber 8 and the chamber; The device comprises any one or a combination of two or more of a roller, a pulley and a conveyor belt; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, and between the feed chamber 1 and the first film preparation chamber 4 is provided a valve 11, a first valve preparation chamber 4 and a first balance chamber 3 are provided with a valve 12, a first balance chamber 3 and a chemical vapor deposition chamber Between the 8 is provided a valve 13, the chemical vapor deposition chamber 8 is provided with a valve 14 which is open to the atmosphere; the feed chamber 1, the first film preparation chamber 4, and the first balance chamber 3 are passed through the sample transfer device and the valve It is connected to the chemical vapor deposition chamber 8 as a whole.

The feeding chamber 1 is provided with a sample processing device 50 and a heat insulating shielding system 98, and the sample processing device may be a plasma surface processor, a gas ionization wire surface processor and a heating device, etc., which can modify the sample. The heating device uses a resistance heater, an infrared heater, and a laser heater to heat the sample.

A sample processor device 51 is disposed in the first film preparation chamber 4, and the sample processing device may be a plasma surface processor, a device for gas ionization, or a heating device, such as a device capable of modifying a sample. The sample processor device 51 is a heating device using a resistance heater, an infrared heater, a laser heater or the like to enable heating of the sample; the first film preparation chamber 4 is provided with physical vapor deposition systems 33 and 34. The physical vapor deposition system includes any one or a combination of two or more of an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system; A film preparation chamber 4 is provided with a cooling system 90 and an insulation shielding system 97.

The chemical vapor deposition chamber 8 is provided with a heating device 40, which is a device capable of heating a sample by using an electric resistance heater, an infrared heater and a laser heater; and a chemical vapor deposition system 38 is disposed in the chemical vapor deposition chamber 8. And 39, the chemical vapor deposition system comprises any one or a combination of two or more of an ion-enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, and an aerosol-assisted chemical vapor deposition system; a chemical vapor deposition chamber There is an insulation shielding system 96 in the 8th.

The feeding chamber 1 is provided with a gas connection port 60, the first film preparation chamber 4 is provided with gas connection ports 61 and 76, 76 is connected to the air mixing box 86, and the air mixing box 86 is connected to the two gas connection ports 69 and 70, A balance chamber 3 is provided with a gas connection port 63, a chemical vapor deposition chamber 8 is provided with gas connection ports 64 and 75, a gas connection port 75 is connected to the gas mixture box 85, and a gas mixing box 85 is connected to the three gas connection ports 66, 67. And 68; each gas path is independently equipped with a metering and flow regulating device such as a mass flow meter and an electromagnetic shut-off valve, so as to accurately control the flow rate of the gas, for example, each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each Each of the mass flowmeters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic shut-off valve and the mass flowmeter are connected to the gas connection port through the pipeline.

The chemical vapor deposition chamber 8, the heating device 40 and the gas connection ports 64 and/or 75 may also constitute a chemical vapor deposition system.

The first film preparation chamber 4, the sample processing device 51 and the gas connection ports 61 and/or 76 may also constitute a chemical vapor deposition system. The basic process for continuously preparing a two-dimensional nanofilm is: placing a substrate required for synthesizing a two-dimensional nanofilm on a carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1; in the feed chamber 1 The surface of the sample is processed by the sample processing device 50, and then surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, a physical deposition system such as a thermal evaporation deposition system is utilized in the first film preparation chamber 4. Preparing a first catalytic layer on the substrate, and then preparing a second catalytic layer using a physical deposition system such as sputter deposition system 34, and then passing through the first balancing chamber 3 to the chemical vapor deposition chamber 8; The deposition chamber 8 uses a chemical vapor deposition system 38 and 39 to prepare a two-dimensional nanofilm. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process for continuous preparation of the two-dimensional film. In this embodiment, the first catalytic layer and the second catalytic layer may also be deposited simultaneously to achieve blending.

The basic process for continuously preparing the two-dimensional nano film may also be: placing the substrate required for synthesizing the two-dimensional nano film and/or placing it on the loading stage 29, and transferring it to the feeding chamber 1 by the sample conveying device 30; The feed chamber 1 processes the surface of the sample by the sample processing device 50, and is surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, a physical deposition system such as a laser is used in the first film preparation chamber 4. The deposition system 33 prepares a catalytic layer on the substrate and/or the catalytic layer, and then deposits a precursor required for synthesizing the two-dimensional nano-film on the catalytic layer by a physical deposition system such as an ion beam deposition system 34; after deposition, after the first The chamber 3 is transferred to the chemical vapor deposition chamber 8. Under certain circumstances, the precursor of the two-dimensional nano-film is converted into a two-dimensional nano-film in the chemical vapor deposition chamber 8. After the two-dimensional film is prepared, the valve is passed through the valve. 14 is passed to the atmosphere to complete a process for the continuous preparation of a two-dimensional film. The precursor of the two-dimensional nanomaterial is a compound containing an element constituting the two-dimensional nano material, and the synthetic precursor includes a carbonaceous polymer such as methane, ethylene or ethanol.

The basic process for continuously preparing a two-dimensional nano film may also be: placing a substrate required for synthesizing a two-dimensional nano film on a carrier gantry 29, transferring it from the sample transfer device 30 to the feed chamber 1; in the feed chamber The chamber 1 processes the surface of the sample by the sample processing device 50, and is surface-treated and transferred to the first film preparation chamber 4; at a certain temperature, a physical deposition system such as a sputter deposition system is used in the first film preparation chamber 4. 33 and 34 prepare a catalytic layer on the substrate and/or the catalytic layer, and then pass through the first balancing chamber 3 to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, a chemical vapor deposition system such as aerosol assist A two-dimensional nanofilm is prepared by chemical vapor deposition technology. After the two-dimensional film is prepared, it is passed through the valve 14 to the atmosphere to complete a process for continuous preparation of the two-dimensional film.

Example 9

Referring to FIG. 9, a scaled continuous preparation of two-dimensional nano-film equipment of the present invention includes sequentially providing a feeding chamber 1 on a production line, the first place a chamber 2, a first balance chamber 3, a first membrane preparation chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with an atmosphere a valve 10 is disposed between the feed chamber 1 and the first processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 is A valve 13 is disposed between the first film preparation chambers 4, and a valve 14 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and between the second balance chamber 5 and the second processing chamber 201. a valve 15 is disposed, a valve 16 is disposed between the second processing chamber 201 and the discharge chamber 9, and the discharge chamber 9 is provided with a valve 17 that communicates with the atmosphere; the entire device is in the feeding chamber 1, the first treatment The chamber 2, the first balance chamber 3, the first film preparation chamber 4, the second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a roller conveyor 30 for conveying samples; The device will feed the chamber 1 through the roller conveyor and the valve, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second balancing chamber 5, The processing chamber 201 and a discharge chamber 9 is connected into a whole.

The feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balancing chamber 5 is provided with a vacuuming device 25, the second processing chamber 201 is provided with a vacuuming device 26, and the discharging chamber 9 is provided with a vacuuming device 27.

The feeding chamber 1 is provided with a gas connection port 61, the first processing chamber 2 is provided with two gas connection ports 62 and 80, the gas connection port 80 is connected to the air mixing box 86, and the air mixing box 86 is connected to the two gas connection ports 76. And 77, the first balance chamber 3 is provided with a gas connection port 64, the first film preparation chamber 4 is provided with a gas connection port 78, the second balance chamber 5 is provided with a gas connection port 68, and the second process chamber 201 is provided. There are two gas connection ports 69 and 79, a gas connection port 79 is connected to the air mixing box 85, a gas mixing box 85 is connected to the three gas connection ports 71, 72 and 73, and the discharge chamber 9 is provided with a gas connection port 74; The road can precisely control the flow of gas. For this purpose, the mass flow meter and the electromagnetic cut-off valve are included. Each gas connection port is connected with a mass flow meter to control the flow rate of the gas. Each mass flow meter has one end at each end. The electromagnetic shut-off valve, the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.

The feeding chamber 1 is provided with a surface processor 50 and a heating device 40. The first processing chamber 2 is provided with a heating device 41, and the first film preparation chamber 4 is provided with a heating device 42 and a heat insulating shielding device 97, and the second processing The chamber 201 is provided with heating means 43 and 44, a cooling means 90 and a heat insulating shield 96.

The first processing chamber 2, the heating device 41 and the gas connection ports 62 and/or 80 constitute a chemical vapor deposition system.

The first film preparation chamber 4, the heating device 42 and the gas connection port 78 constitute a chemical vapor deposition system.

The second processing chamber 201, the heating means 43 and/or 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system. The basic process for continuously preparing a two-dimensional nano film is: placing a substrate material/catalyst layer required for preparing a two-dimensional nano film on a carrier gantry 29, and transporting it by a roller conveyor 30 to a feed chamber 1; At a certain temperature, the substrate material/catalyst layer is surface-treated in the feed chamber 1 by the surface processor 50, and then transferred to the first film preparation chamber through the first processing chamber 2 and the first balance chamber 3. Room 4; under a certain atmosphere, the substrate/catalyst layer is heat-treated in the first film preparation chamber 4, and then transferred to the second processing chamber 201 via the second balance chamber 5; in the second processing chamber 201 uses a microwave plasma chemical vapor deposition system to prepare a two-dimensional nano-film on the substrate/catalyst layer. The two-dimensional nano-film is prepared and transported out of the device through the discharge chamber 9 to complete the preparation of the two-dimensional nano-film.

Example 10

Referring to FIG. 10, a scaled continuous preparation of a two-dimensional nano-film apparatus of the present invention includes sequentially providing a feed chamber 1, a first processing chamber 2, a first balance chamber 3, and a first film preparation chamber on a production line. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed. A valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201. The second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4. The second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a roller for conveying samples. The feeding device 30; the whole device passes through the roller conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparing chamber 4, the second balancing chamber 5, the second The processing chamber 201 and the discharge chamber 9 are connected in one piece.

The feed chamber 1 is provided with a gas connection port 61, the first process chamber 2 is provided with two gas connection ports 62 and 63, the first balance chamber 3 is provided with a gas connection port 64, and the first film preparation chamber 4 is provided. The gas connection port 80, the gas connection port 80 is connected to the air mixing box 86, the air mixing box 86 is connected to the two gas connection ports 66 and 67, the second balance chamber 5 is provided with a gas connection port 68, and the second processing chamber 201 is provided. There are two gas connection ports 69 and 79, a gas connection port 79 is connected to the air mixing box 85, a gas mixing box 85 is connected to the three gas connection ports 71, 72 and 73, and the discharge chamber 9 is provided with two gas connection ports 74 and 75; The gas connection port is connected to the gas path, and each gas path can precisely control the flow rate of the gas. For this purpose, a mass flow meter and an electromagnetic cut-off valve are included, and each gas connection port is connected with a mass flow meter to control the flow rate of each gas. Each of the mass flowmeters is provided with an electromagnetic shut-off valve at both ends, and the electromagnetic shut-off valve and the mass flowmeter are connected to the gas connection port through the pipeline. The feeding chamber 1 is provided with a surface processor 50. The first processing chamber 2 is provided with a heating device 41, a cooling device 91 and a heat insulating shielding device 98. The first film preparing chamber 4 is provided with a heating device 42 and physical vapor deposition. Systems 33 and 34, second processing chamber 201 are provided with heating means 43 and 44, cooling means 90 and thermal barrier means 96, and discharge chamber 9 is provided with a surface processor 51.

The first processing chamber 2, the heating device 41 and the gas connection ports 62 and/or 63 constitute a chemical vapor deposition system.

The first film preparation chamber 4, the heating device 42 and the gas connection port 80 constitute a chemical vapor deposition system.

The second processing chamber 201, the heating means 43 and/or 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system. The physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; a chemical vapor deposition system, Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems and microwave plasma chemical vapor deposition systems.

The basic process for continuously preparing a two-dimensional nano film is: placing a substrate material required for synthesizing a two-dimensional nano film on a carrier gantry 29, which is transported by a roller conveyor 30 to a feed chamber 1; The surface of the feed chamber 1 is surface treated by the surface processor 50, then transferred to the first processing chamber 2 for heat treatment, and then transferred to the first film preparation chamber 4 via the first balance chamber 3; A catalytic layer film is prepared on the surface of the substrate by a physical vapor deposition system such as a sputtering target thin film deposition system 33 and 34 in an atmosphere environment and temperature; after the catalytic layer is prepared, it is transferred to the second processing chamber through the second balance chamber 5. 201; preparing a two-dimensional nano film on the substrate/catalyst layer by using a plasma enhanced chemical vapor deposition system in the second processing chamber 201, and preparing the two-dimensional nano film through the discharge chamber 9 to complete the two-dimensional nanometer Preparation of the film.

Example 11

Referring to FIG. 11, a large-scale continuous preparation of two-dimensional nano-film equipment of the present invention includes sequentially providing a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, and a first film preparation chamber on a production line. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed. A valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201. The second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4. The second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a roller for conveying samples. The feeding device 30; the whole device passes through the roller conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparing chamber 4, the second balancing chamber 5, the second The processing chamber 201 and the discharge chamber 9 are connected in one piece.

The feed chamber 1 is provided with a gas connection port 61, the first process chamber 2 is provided with a gas connection port 62, the first balance chamber 3 is provided with a gas connection port 64, and the first film preparation chamber 4 is provided with two gases. The connecting ports 80 and 78, the gas connecting port 80 are connected to the air mixing box 86, the air mixing box 86 is connected to the two gas connecting ports 66 and 67, the second balancing chamber 5 is provided with a gas connecting port 68, and the second processing chamber 201 is provided. There are two gas connection ports 69 and 79, a gas connection port 79 is connected to the air mixing box 85, a gas mixing box 85 is connected to the two gas connection ports 71 and 72, and the discharge chamber 9 is provided with a gas connection port 74; The gas path, each gas path can precisely control the flow of gas, including mass flow meters and electromagnetic shut-off valves, etc. Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, two of each mass flow meter Each end is provided with an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.

The feeding chamber 1 is provided with a surface processor 50. The first processing chamber 2 is provided with a heating device 41, a cooling device 91 and a heat insulating shielding device 98. The first film preparing chamber 4 is provided with a heating device 42 and physical vapor deposition. The systems 33 and 34, the cooling device 92 and the thermal shield 96, the second processing chamber 201 are provided with a heating device 43, a cooling device 90 and a thermal barrier 96.

The first processing chamber 2, the heating device 41 and the gas connection port 62 constitute a chemical vapor deposition system.

The first film preparation chamber 4, the heating device 42 and the gas connection ports 80 and/or 78 constitute a chemical vapor deposition system.

The second processing chamber 201, the heating means 43, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.

The physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implantation deposition system, and a thermal evaporation system; a chemical vapor deposition system, Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems and microwave plasma chemical vapor deposition systems.

The basic process for continuously preparing a two-dimensional nano film is: placing a substrate material required for synthesizing a two-dimensional nano film on a carrier gantry 29, which is transported by a roller conveyor 30 to a feed chamber 1; The surface of the feed chamber 1 is surface treated by the surface processor 50, then transferred to the first processing chamber 2 for heat treatment, and then transferred to the first film preparation chamber 4 via the first balance chamber 3; The catalytic layer is prepared on the substrate by a physical vapor deposition system such as an electron gun deposition system 33 in an atmosphere environment and temperature, and then a precursor of the two-dimensional nanomaterial is injected into the catalytic layer by a physical vapor deposition system such as an ion implanter 34, after which Passing through the second balance chamber 5 to the second processing chamber 201; The processing chamber 201 processes a sample in which a precursor of a two-dimensional nanomaterial is injected into the catalytic layer. After the heat treatment, the sample is transferred to the discharge chamber 9 for cooling to complete the preparation of the two-dimensional nanofilm.

Example 12

Referring to FIG. 12, a scaled continuous preparation of two-dimensional nano-film equipment of the present invention includes sequentially providing a feed chamber 1, a first processing chamber 2, a first balance chamber 3, and a first film preparation chamber on a production line. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed. A valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201. The second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4. The second balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are each provided with a transfer of the transport sample. Conveying device 30; the entire device passes through the conveyor belt and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second balancing chamber 5, the second The processing chamber 201 and the discharge chamber 9 are connected in one piece.

The feed chamber 1 is provided with a gas connection port 61, the first process chamber 2 is provided with two gas connection ports 62 and 63, the first balance chamber 3 is provided with a gas connection port 64, and the first film preparation chamber 4 is provided. There is a gas connection port 80, a gas connection port 80 is connected to the air mixing box 86, the air mixing box 86 is provided with two gas connection ports 66 and 67, and the second balance chamber 5 is provided with a gas connection port 68, and the second processing chamber is provided. 201 is provided with two gas connection ports 69 and 79, a gas connection port 79 is connected to the gas mixing box 85, the gas mixing box 85 is connected to three gas connection ports 71, 72 and 73, and the discharge chamber 9 is provided with a gas connection port 74; Each gas path can precisely control the flow rate of the gas. For this purpose, a mass flow meter and an electromagnetic shut-off valve are included. Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and each end of each mass flow meter is provided. There is an electromagnetic shut-off valve, and the electromagnetic shut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.

The feeding chamber 1 is provided with a surface processor 50, the first processing chamber 2 is provided with a heating device 41, the first film preparation chamber 4 is provided with a physical vapor deposition system 33 and a heating device 42, and the second processing chamber 201 is provided There are heating means 43 and 44, a cooling means 90 and a heat insulating shield 96, and the discharge chamber 9 is provided with a surface processor 51.

The second processing chamber 201, the heating means 43 and/or 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system. The physical vapor deposition system includes any one or a combination of a sputtering target thin film deposition system, an electron gun deposition system, an ion gun deposition system, an ion implanter deposition system, and a thermal evaporation system; a chemical vapor deposition system Including plasma enhanced chemical vapor deposition systems, aerosol assisted chemical vapor deposition systems, and microwave plasma chemical vapor deposition systems.

The basic process for continuously preparing a two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the carrier gantry 29, and transferring it to the feeding chamber 1 by the conveyor belt conveying device 30; The material chamber 1 is surface-treated by the surface processor 50, and then transferred to the first film preparation chamber 4 through the first processing chamber 2 and the first balance chamber 3; under a certain atmosphere, the substrate is The first film preparation chamber 4 is subjected to heat treatment, and then transferred to the second processing chamber 201 via the second balance chamber 5; a two-dimensional nano-film is prepared on the substrate by using a chemical vapor deposition system in the second processing chamber 201, After the two-dimensional nano film is prepared, it is conveyed to the discharge chamber 9; in the discharge chamber 9, the prepared two-dimensional nano film is subjected to surface modification treatment, and then processed and transferred to the device to complete the preparation of the two-dimensional nano film.

Example 13

Referring to FIG. 13, a scaled continuous preparation of two-dimensional nano-film equipment comprises a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, and a first film preparation chamber. a chamber 4, a second balance chamber 5, a second processing chamber 201 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 communicating with the atmosphere, the feed chamber 1 and the first processing chamber 2 A valve 11 is disposed between the first processing chamber 2 and the first balance chamber 3, and a valve 13 is disposed between the first balance chamber 3 and the first film preparation chamber 4, and the first film is disposed. A valve 14 is disposed between the preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second processing chamber 201. The second processing chamber 201 and the discharge chamber 9 are provided. Between the valve 16 is provided, the discharge chamber 9 is provided with a valve 17 which is open to the atmosphere; the whole set of equipment is in the feed chamber 1, the first balance chamber 3, the second balance chamber 5 and the discharge chamber 9 a pulley conveying device 30 for conveying a sample; a first processing chamber 2, a first film preparation chamber 4 and a second The processing chamber 201 is provided with a roller conveying device 30; the entire device passes through the sample conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second The balance chamber 5, the second processing chamber 201 and the discharge chamber 9 are connected in one piece.

The feeding chamber 1 is provided with a vacuuming device 21, the first processing chamber 2 is provided with a vacuuming device 22, the first balancing chamber 3 is provided with a vacuuming device 23, and the first film preparation chamber 4 is provided with a vacuuming device 24, the second balance chamber 5 is provided with a vacuuming device 25, and the second processing chamber 201 is provided with a vacuum At 26, the discharge chamber 9 is provided with a vacuuming device 27.

The feed chamber 1 is provided with a gas connection port 61, the first process chamber 2 is provided with gas connection ports 62 and 63, the first balance chamber 3 is provided with a gas connection port 64, and the first film preparation chamber 4 is provided with two The gas connection ports 80 and 78, the gas connection port 80 are connected to the air mixing box 86, the air mixing box 86 is connected to the two gas connection ports 66 and 67, and the second balance chamber 5 is provided with a gas connection port 68, and the second processing chamber 201 is provided with two gas connection ports 69 and 79, a gas connection port 79 is connected to the air mixing box 85, a gas mixing box 85 is connected to the two gas connection ports 71 and 72, and the discharge chamber 9 is provided with two gas connection ports 74 and 75; Each gas path can precisely control the flow of gas, including mass flow meters and electromagnetic shut-off valves, etc. Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and both ends of each mass flow meter Each has an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.

The feeding chamber 1 is provided with a surface processor 50, the first processing chamber 2 is provided with a heating device 41, and the first film preparation chamber 4 is provided with heating means 42 and physical vapor deposition systems 33 and 34, cooling means 92 and partition The heat shielding device 97, the second processing chamber 201 is provided with a heating device 44.

The first processing chamber 2, the heating device 41, and the gas connection ports 62 and/or 63 constitute a chemical vapor deposition system.

The first film preparation chamber 4, the heating means 42, and the gas connection ports 80 and/or 78 constitute a chemical vapor deposition system.

The second processing chamber 201, the heating device 44, and the gas connection ports 69 and/or 79 constitute a chemical vapor deposition system.

The basic process for continuously preparing the two-dimensional nano film is: placing the substrate material required for synthesizing the two-dimensional nano film on the loading stage 29, and transferring it to the feeding chamber 1 by the transfer pulley conveying device 30; The surface treatment is performed in the feed chamber 1 by the surface processor 50, and then transferred to the first processing chamber 2 for heat treatment. After the heat treatment, it is transferred to the first balance chamber 3 by the roller conveyor 30, and then, A balance chamber 3 is transferred to the first film preparation chamber 4; a catalytic layer is prepared on the substrate by a physical vapor deposition system such as a thermal evaporation system 33 under a certain atmosphere and temperature, and then physical vapor deposition is employed. A system such as ion gun deposition system 34 ionizes the precursor of the two-dimensional nanomaterial onto the catalytic layer, and thereafter, is transported to the second processing chamber 201 via the second balancing chamber 5; A sample of a precursor of a two-dimensional nanomaterial deposited on the catalytic layer is processed, and after the heat treatment, the sample is transferred to the discharge chamber 9 for cooling to complete the preparation of the two-dimensional nanofilm.Example 14

Referring to FIG. 14, a large-scale continuous preparation two-dimensional nano film device of the present invention is sequentially provided with a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, a first film preparing chamber 4, and a first a second balance chamber 5, a second thin film preparation chamber 6, a third balance chamber 7, a chemical vapor deposition chamber 8 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 connected to the atmosphere, feeding A valve 11 is disposed between the chamber 1 and the first processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 and the first thin film preparation chamber A valve 13 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second film preparation chamber 6. A valve 16 is disposed between the second film preparation chamber 6 and the third balance chamber 7, and a valve 17 is disposed between the third balance chamber 7 and the chemical vapor deposition chamber 8, and the chemical vapor deposition chamber 8 and the discharge are provided. A valve 18 is arranged between the chambers 9, and the discharge chamber 9 is provided with a valve 19 which is open to the atmosphere; Material chamber 1, first processing chamber 2, first balance chamber 3, first thin film preparation chamber 4, second balance chamber 5, second thin film preparation chamber 6, third balance chamber 7, chemistry The sample delivery device 30 is disposed in the chambers of the vapor deposition chamber 8 and the discharge chamber 9; the sample delivery device 30 includes any one or a combination of two or more of a roller, a pulley, and a conveyor belt; The apparatus will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first thin film preparation chamber 4, the second balance chamber 5, and the second thin film preparation chamber 6 through the sample transfer device and the valve The third balance chamber 7, the chemical vapor deposition chamber 8 and the discharge chamber 9 are connected in one piece.

The first processing chamber 2 is provided with a heating device 40, and the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 ° C; Cooling system 90.

The first processing chamber 2, the heating device 40 and the gas connection port 61 or 62 may constitute a thermal chemical vapor deposition system.

The first film preparation chamber 4 is provided with a physical vapor deposition system 33 and a heating device 41; the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion Any one or a combination of two or more of the injection systems; the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 °C. The first film preparation chamber 4, the heating means 41 and the gas connection port 64 may constitute a thermal chemical vapor deposition system.

The second thin film preparation chamber 6 is provided with a physical vapor deposition system 34 and a heating device 42; the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion Any one or a combination of two or more of the injection systems; the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be adjusted between 20 and 2000 °C. The second film preparation chamber 6, the heating device 42, and the gas connection port 66 may constitute a thermal chemical vapor deposition system.

The chemical vapor deposition chamber 8 is provided with a sample processing device 51, a heating device 43, a cooling system 91 and a heat insulating shielding system 97; the sample processing device 51 may be a plasma sample processing device, a wire enthalpy or heating for gas ionization. a device capable of modifying a sample, such as a device, The wire enthalpy for gas ionization can realize ionization of gas under high-frequency conditions of vacuum; the heating device can be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature can be adjusted between 20 and 2000 ° C. .

The feed chamber 1 is provided with a gas connection port 60, the first process chamber 2 is provided with two gas connection ports 61 and 62, the first balance chamber 3 is provided with a gas connection port 63, and the first film preparation chamber 4 is provided. There is a gas connection port 64, a second balance chamber 5 is provided with a gas connection port 65, a second film preparation chamber 6 is provided with a gas connection port 66, and a third balance chamber 7 is provided with a gas connection port 67, a chemical vapor deposition chamber The chamber is provided with gas connection ports 68 and 69, the gas connection port 69 is connected to the air mixing box 87, the air mixing box 87 is connected to the three gas connection ports 76, 77 and 78, and the discharge chamber is connected with two gas connection ports 70 and 71. Each gas path can precisely control the flow of gas, and can include metering and flow regulating devices such as mass flow meters and electromagnetic shut-off valves. Each gas connection port is connected with a mass flow meter to control the flow rate of each gas. Each mass flow meter Each end of the two ends is provided with an electromagnetic shut-off valve, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through the pipeline.

The chemical vapor deposition chamber 8, the heating device 43 and the gas connection ports 68 and/or 69 may constitute a thermal chemical vapor deposition system.

The chemical vapor deposition chamber 8 may also be provided with any one or two of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, and an inductively coupled plasma chemical vapor deposition system. The combination above.

The feeding chamber 1 is provided with a vacuuming device 20, the first processing chamber 2 is provided with a vacuuming device 21, the first balancing chamber 3 is provided with a vacuuming device 22, and the first film preparation chamber 4 is provided with a vacuuming device 23, the second balance chamber 5 is provided with a vacuuming device 24, the second film preparation chamber 6 is provided with a vacuuming device 25, the third balancing chamber 7 is provided with a vacuuming device 26, and the chemical vapor deposition chamber 8 is provided The vacuuming device 27, the discharge chamber 9 is provided with a vacuuming device 28. Each individual evacuating device include various vacuum pumps, vacuum lines, vacuum valves, vacuum meter, etc., can make the degree of vacuum in the chambers between 1.0x l0- ^1Q Pa to atmospheric pressure by the evacuating device.

The basic process for the continuous preparation of a two-dimensional nanofilm on a large scale may be: placing a substrate/catalyst layer required for preparing a two-dimensional nanofilm on a carrier gantry 29, which is conveyed by the sample transfer device 30 through the feed chamber 1 The first processing chamber 2; the substrate/catalytic layer is heat treated in the first processing chamber 2 by the heating device 40, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; The preparation chamber 4 deposits a precursor of the two-dimensional nano-film on the substrate/catalyst layer by means of a physical vapor deposition system 33 such as a sputter deposition system, and then passes through the second balance chamber 5 by the sample transfer device 30, The two thin film deposition chambers 6 and the third balance chamber 7 are transferred to the chemical vapor deposition chamber 8; the precursor of the two-dimensional nano material is chemically vapor deposited in the chemical vapor deposition chamber 8 under a certain atmosphere. Conversion into a two-dimensional nano-film; Finally, the prepared two-dimensional nano-film is transported out of the preparation device via the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano-film.

A precursor of a two-dimensional nanomaterial refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene including an amorphous carbon, an amorphous carbon film, and a carbon-containing material. A polymer of an element or the like; taking MoS ₂ as an example, the precursor includes a MoS ₂ target, a Mo target, and the like.

The basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate/catalyst layer required for preparing a two-dimensional nano film on a carrier gantry 29, and transporting it through the sample chamber 30 through the feed chamber 1 Arriving at the first processing chamber 2·' The substrate/catalyst layer is heat treated by the heating device 40 in the first processing chamber 2, and then passed through the second balancing chamber 5 and the second thin film deposition chamber 6 from the sample transport device 30. And the third balance chamber 7 is transferred to the chemical vapor deposition chamber 8; the two-dimensional nano-film is prepared by using a chemical vapor deposition system in the chemical vapor deposition chamber 8; finally, the prepared two-dimensional nano-film is transported through the discharge chamber 9. The preparation device is prepared to complete the continuous preparation of the two-dimensional nano film.

Example 15

Referring to FIG. 15, a large-scale continuous preparation two-dimensional nano film device of the present invention is sequentially provided with a feeding chamber 1, a first processing chamber 2, a first balancing chamber 3, a first film preparing chamber 4, and a first a second balance chamber 5, a second thin film preparation chamber 6, a third balance chamber 7, a chemical vapor deposition chamber 8 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 connected to the atmosphere, feeding A valve 11 is disposed between the chamber 1 and the first processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 and the first thin film preparation chamber A valve 13 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second film preparation chamber 6. A valve 16 is disposed between the second film preparation chamber 6 and the third balance chamber 7, and a valve 17 is disposed between the third balance chamber 7 and the chemical vapor deposition chamber 8, and the chemical vapor deposition chamber 8 and the discharge are provided. A valve 18 is arranged between the chambers 9, and the discharge chamber 9 is provided with a valve 19 which is open to the atmosphere; Material chamber 1, first processing chamber 2, first balance chamber 3, first thin film preparation chamber 4, second balance chamber 5, second thin film preparation chamber 6, third balance chamber 7, chemistry a sample transfer device 30 is disposed in the chambers of the vapor deposition chamber 8 and the discharge chamber 9; the sample transfer device 30 includes any one or a combination of two or more of a roller, a pulley, and a conveyor belt; The feed chamber 1, the first processing chamber 2, the first balance chamber 3, the first film preparation chamber 4, the second balance chamber 5, and the second film preparation chamber 6 are passed through the sample transfer device and the valve. The third balance chamber 7, the chemical vapor deposition chamber 8 and the discharge chamber 9 are connected in one piece.

The first processing chamber 2 is provided with a sample processing device 50 and a heating device 40; the sample processing device may be a plasma processor, a wire enthalpy for gas ionization, a heating device, etc.; the heating device may be a resistance heating device, an infrared heating device, For laser heating devices, etc., the temperature can be adjusted between 20 and 2000 °C.

The first processing chamber 2, the heating device 40 and the gas connection port 61 or 62 may constitute a thermal chemical vapor deposition system. The first film preparation chamber 4 is provided with physical vapor deposition systems 33 and 35, a heating device 41 and an insulation shielding system 98; the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, Any one or a combination of two or more of a thermal evaporation deposition system, a laser deposition system, and an ion implantation system; the heating device 41 may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be 20 to 2000°. Adjust between C. The first film preparation chamber 4, the heating means 41 and the gas connection port 64 may constitute a thermal chemical vapor deposition system.

The second thin film preparation chamber 6 is provided with a physical vapor deposition system device 34 and a heating device 42; the physical vapor deposition system 34 includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, and a laser deposition system. Any one or a combination of two or more of the ion implantation systems; the heating device 42 may be a resistance heating device, an infrared heating device, a laser heating device, or the like, and the temperature may be adjusted between 20 and 2000 °C. The second film preparation chamber 6, heating means 42 and gas connection port 66 may constitute a thermal chemical vapor deposition system.

The chemical vapor deposition chamber 8 is provided with a chemical vapor deposition system 38, a heating device 43, a cooling system 91 and an insulation shielding system 97; the chemical vapor deposition system 38 comprises a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor phase Any one or a combination of two or more of a deposition system, an aerosol-assisted chemical vapor deposition system, and an inductively coupled plasma chemical vapor deposition system.

The discharge chamber 9 is provided with a sample processing device 52, which may be a plasma processor, a coil for gas ionization, a heating device, and the like. The feed chamber 1 is provided with a gas connection port 60, the first process chamber 2 is provided with two gas connection ports 61 and 62, the first balance chamber 3 is provided with a gas connection port 63, and the first film preparation chamber 4 is provided. There is a gas connection port 64, a gas connection port 64 is connected to the air mixing box 85, a gas mixing box 85 is connected to the two gas connection ports 72 and 73, a second balance chamber 5 is provided with a gas connection port 65, and a second film preparation chamber 6 is provided. The gas connection port 66 is provided, the gas connection port 66 is connected to the air mixing box 86, the air mixing box 86 is connected to the two gas connection ports 74 and 75, and the third balance chamber 7 is provided with a gas connection port 67, and the chemical vapor deposition chamber is provided. There are gas connection ports 68 and 69, a gas connection port 69 is connected to the air mixing box 87, a gas mixing box 87 is connected to the three gas connection ports 76, 77 and 78, and the discharge chamber is connected with two gas connection ports 70 and 71; A gas path can precisely control the flow of gas, and can include metering and flow regulating devices such as mass flow meters and electromagnetic shut-off valves. Each gas connection port is connected with a mass flow meter to control the flow rate of each gas, and two of each mass flow meter. One at each end The electromagnetic shut-off valve, the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through a pipeline.

The chemical vapor deposition chamber 8, the heating device 43 and the gas connection ports 68 and/or 69 may constitute a chemical vapor deposition system.

The feeding chamber 1 is provided with a vacuuming device 20, the first processing chamber 2 is provided with a vacuuming device 21, the first balancing chamber 3 is provided with a vacuuming device 22, and the first film preparation chamber 4 is provided with a vacuuming device 23, the second balance chamber 5 is provided with a vacuuming device 24, the second film preparation chamber 6 is provided with a vacuuming device 25, the third balancing chamber 7 is provided with a vacuuming device 26, and the chemical vapor deposition chamber 8 is provided The vacuuming device 27, the discharge chamber 9 is provided with a vacuuming device 28. Each of the independent vacuuming devices includes various vacuum pumps, vacuum pipes, vacuum valves, vacuum gauges, etc., and the vacuum of each chamber can be made to be between normal pressure and 1.0x 10- ^1Q Pa by vacuuming.

The basic process for the continuous preparation of the two-dimensional nano-film on a large scale may be: placing the substrate required for preparing the two-dimensional nano film on the carrier gantry 29, and the substrate is transported by the sample transfer device 30 through the feed chamber 1 to reach the first a processing chamber 2; at a certain temperature, the substrate is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; in the first thin film preparation chamber The chamber 4 is prepared on the substrate by physical vapor deposition systems 33 and 35, such as an electron beam deposition system, and then passed through the second balancing chamber 5, to the second thin film deposition chamber 6; in the second thin film preparation chamber a chamber 6, using a physical vapor deposition system 34 such as an ion beam deposition system to ionize the precursor of the two-dimensional nano-film onto the catalytic layer, and then through the third balance chamber 7, is transferred to the chemical vapor deposition chamber 8; The vapor deposition chamber 8 processes the sample to form a two-dimensional nano film; finally, the prepared two-dimensional nano film is transported out of the preparation device through the discharge chamber 9 to complete the two-dimensional nano film. Continued preparation.

The precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing graphene, the precursor includes methane, ethanol, etc.; taking MoS ₂ as an example The precursor includes H ₂ S and the like.

The basic process for the continuous preparation of a two-dimensional nanofilm on a large scale may also be: placing a substrate required for preparing a two-dimensional nanofilm on a carrier gantry 29, which is conveyed by the sample transfer device 30 through the feed chamber 1 First processing chamber 2; at a certain temperature, the substrate is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; in the first film preparation The chamber 4 simultaneously deposits two different catalytic layer materials on the substrate by physical vapor deposition systems 33 and 35, such as an electron beam deposition system and a sputter deposition system, and then passes through the second balance chamber 5, and is transferred to the first a second thin film deposition chamber 6; in the second thin film preparation chamber 6, a precursor of the two-dimensional nano-film is deposited onto the catalytic layer by a physical vapor deposition system 34 such as a thermal evaporation deposition system, and then passes through the third balance chamber 7 , is transferred to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, the sample is processed to form a two-dimensional nano film; finally, the prepared two-dimensional nano film is transmitted through the discharge chamber 9 Preparation of the apparatus, thereby continuously producing two-dimensional film is completed.

The precursor of the two-dimensional nano material refers to a compound containing an element constituting a two-dimensional nano material or an element containing a two-dimensional nano material, for example, preparing a graphene, the precursor including graphite powder, carbon black, etc.; to prepare MoS ₂ As an example, the precursor includes MoS ₂ powder and the like.

The basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate required for preparing a two-dimensional nano film on a loading stage 29, which is conveyed by the sample conveying device 30 through the feeding chamber 1 First processing chamber 2; at a certain temperature, the substrate is in the first processing chamber 2 Pre-processing is carried out, and then transferred to the first film preparation chamber 4 through the first balance chamber 3; on the substrate is prepared in the first film preparation chamber 4 by using physical vapor deposition systems 33 and 35 such as an electron beam deposition system. The first catalytic layer is then passed through the second balancing chamber 5 to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, the second is formed by a physical vapor deposition system 34 such as a sputter deposition system The catalytic layer is deposited on the first catalytic layer and then passed through the third equilibrium chamber 7 to be transferred to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, the chemical vapor deposition system 38 is used to enhance the chemical vapor phase. The deposition system prepares a two-dimensional nano film on the catalytic layer; finally, the prepared two-dimensional nano film is transported out of the preparation device through the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano film.

The basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate/catalyst layer required for preparing a two-dimensional nano film on a carrier gantry 29, which is transported by the sample transfer device 30 through the feed chamber. 1. The first processing chamber 2 and the first balancing chamber 3 reach the first film preparation chamber 4; the substrate/catalyst layer is surface treated in the first film preparation chamber 4, and then passes through the second balance chamber 5 The second thin film deposition chamber 6 and the third balance chamber 7 are transferred from the sample transfer device 30 to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, using a chemical vapor deposition system 38 such as microwave plasma chemical vapor deposition The system prepares a two-dimensional nano film; finally, the prepared two-dimensional nano film is transferred to the atmosphere through the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano film.

Example 16

Referring to FIG. 16, a large-scale continuous preparation two-dimensional nano film device of the present invention is sequentially provided with a feeding chamber 1, a first processing chamber 2, a first balance chamber 3, a first film preparation chamber 4, and a first a second balance chamber 5, a second thin film preparation chamber 6, a third balance chamber 7, a chemical vapor deposition chamber 8 and a discharge chamber 9; the feed chamber 1 is provided with a valve 10 connected to the atmosphere, feeding A valve 11 is disposed between the chamber 1 and the processing chamber 2, and a valve 12 is disposed between the first processing chamber 2 and the first balancing chamber 3, and the first balancing chamber 3 and the first thin film preparation chamber 4 A valve 13 is disposed between the first film preparation chamber 4 and the second balance chamber 5, and a valve 15 is disposed between the second balance chamber 5 and the second film preparation chamber 6. A valve 16 is disposed between the film preparation chamber 6 and the third balance chamber 7, and a valve 17, a chemical vapor deposition chamber 8 and a discharge chamber are disposed between the third balance chamber 7 and the chemical vapor deposition chamber 8. Between 9 is provided a valve 18, the discharge chamber 9 is provided with a valve 19 which is open to the atmosphere; the whole set of equipment is in the feed chamber Room 1, first processing chamber 2, first balancing chamber 3, first film preparation chamber 4, second balance chamber 5, second film preparation chamber 6, third balance chamber 7, chemical vapor deposition A sample transfer device 30 is disposed in the chamber of the chamber 8 and the discharge chamber 9; the sample transfer device 30 includes any one or a combination of two or more of a roller, a pulley, a conveyor belt, and the like; The conveying device and the valve will feed the chamber 1, the first processing chamber 2, the first balancing chamber 3, the first film preparation chamber 4, the second balance chamber 5, the second film preparation chamber 6, and the third The balance chamber 7, the chemical vapor deposition chamber 8 and the discharge chamber 9 are connected in one piece.

The first processing chamber 2 is provided with a sample processing device 50; the sample processing device may be a plasma processor, a wire enthalpy for gas ionization, and a heating device.

The first processing chamber 2, the sample processing unit 50 and the gas connection port 61 or 62 may constitute a thermal chemical vapor deposition system.

The first film preparation chamber 4 is provided with a physical vapor deposition system device 33 and a heating device 41; the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, an electron beam deposition system, a thermal evaporation deposition system, a laser deposition system, Any one or a combination of two or more of the ion implantation systems; the heating device may be a resistance heating device, an infrared heating device, a laser heating device, or the like, and the temperature may be adjusted between 20 and 2000 °C. The first film preparation chamber 4, the heating means 41 and the gas connection port 64 may constitute a thermal chemical vapor deposition system.

The second film preparation chamber 6 is provided with physical vapor deposition system devices 34 and 36, a heating device 42, a cooling system 92, and a heat shield system 99; the physical vapor deposition system includes an ion beam deposition system, a sputter deposition system, and electron beam deposition. Any one or a combination of two or more of a system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system; the heating device may be a resistance heating device, an infrared heating device, a laser heating device, etc., and the temperature may be 20 to 2000. Adjust between °C. The second film preparation chamber 6, the heating means 42 and the gas connection port 74 or 75 may constitute a thermal chemical vapor deposition system.

The chemical vapor deposition chamber 8 is provided with a sample processing device 51, a heating device 43, a cooling system 91 and a heat shield system 97; the chemical vapor deposition chamber 8, the heating device 43, and the gas connection port 68 or 69 constitute a thermal chemical vapor deposition The chemical vapor deposition chamber 8 may also be provided with any one of a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, an aerosol assisted chemical vapor deposition system, an inductively coupled plasma chemical vapor deposition system, or Two or more combinations.

The discharge chamber 9 is provided with a sample processing device 52, which may be a plasma processor, a wire enthalpy for gas ionization, a heating device, and the like. The feed chamber 1 is provided with a gas connection port 60, the first process chamber 2 is provided with two gas connection ports 61 and 62, the first balance chamber 3 is provided with a gas connection port 63, and the first film preparation chamber 4 is provided. There is a gas connection port 64, a second balance chamber 5 is provided with a gas connection port 65, a second film preparation chamber 6 is provided with gas connection ports 74 and 75, and a third balance chamber 7 is provided with a gas connection port 67, a chemical vapor phase The deposition chamber is provided with gas connection ports 68 and 69, the gas connection port 69 is connected to the gas mixing box 87, the gas mixing box 87 is connected to the three gas connection ports 76, 77 and 78, and the discharge chamber is connected with two gas connection ports 70. And 71; each gas path can precisely control the flow of gas, including metering and flow regulating devices such as mass flow meters and electromagnetic shut-off valves, each gas connection port is connected with a mass flow meter to control the flow of each gas, each mass An electromagnetic shut-off valve is arranged at each end of the flow meter, and the electromagnetic cut-off valve and the mass flow meter are connected to the gas connection port through the pipeline. The chemical vapor deposition chamber 8, the heating device 43 and the gas connection ports 68 and/or 69 may constitute a chemical vapor deposition system. The feeding chamber 1 is provided with a vacuuming device 20, the first processing chamber 2 is provided with a vacuuming device 21, the first balancing chamber 3 is provided with a vacuuming device 22, and the first film preparation chamber 4 is provided with a vacuuming device 23, the second balance chamber 5 is provided with a vacuuming device 24, the second film preparation chamber 6 is provided with a vacuuming device 25, the third balancing chamber 7 is provided with a vacuuming device 26, and the chemical vapor deposition chamber 8 is provided The vacuuming device 27, the discharge chamber 9 is provided with a vacuuming device 28. Each individual evacuating device include various vacuum pumps, vacuum lines, vacuum valves, vacuum meter, etc., can make the degree of vacuum in the chambers between 1.0x l0- ^1Q Pa to atmospheric pressure by the evacuating device.

The basic process for the continuous preparation of the two-dimensional nano-film can be: placing the substrate required for preparing the two-dimensional nano film on the loading stage 29, passing through the feeding chamber 1, and transferring the substrate to the first processing chamber 2; the substrate is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3; in the first thin film preparation chamber 4 using the physical vapor deposition system 33 such as The electron beam deposition system prepares the catalytic layer on the substrate and then passes through the second balancing chamber 5 to be transferred to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, using the physical vapor deposition systems 34 and 36 A precursor of the two-dimensional nano-film is deposited on the catalytic layer by a sputter deposition system, and then transferred to the chemical vapor deposition chamber 8 through the third balance chamber 7, and chemical vapor deposition is performed in the chemical vapor deposition chamber 8. The method comprises preparing a two-dimensional nano film; finally, the prepared two-dimensional nano film is sent out through a discharge chamber 9 to prepare a device, thereby completing continuous preparation of the two-dimensional nano film.

The basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate and/or a catalytic layer required for preparing a two-dimensional nano film on a loading stage 29, passing through a feeding chamber 1, a substrate, and / or the catalytic layer is transported to the first processing chamber 2; the substrate and / or catalytic layer is pretreated in the first processing chamber 2, and then transferred to the first thin film preparation chamber 4 through the first balancing chamber 3 Depositing a precursor of the two-dimensional nanomaterial on the substrate and/or the catalytic layer in the first thin film preparation chamber 4 using a physical vapor deposition system 33 such as an electron beam deposition system, and then passing through the second balance chamber 5, Is transferred to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, a precursor of another two-dimensional nano-film is deposited onto the substrate by physical vapor deposition systems 34 and 36 such as a thermal evaporation deposition system and And / or on the catalytic layer, then through the third balance chamber 7, is transferred to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, the sample is processed to form a two-dimensional nano-film; finally, the two-dimensional preparation Nano thin Transmitted via the discharging chamber manufacturing apparatus 9, thereby continuously producing two-dimensional film is completed.

The basic process of continuously preparing a two-dimensional nano film in a large scale may also be: placing a substrate and/or a catalytic layer required for preparing a two-dimensional nano film on a loading stage 29, passing through a feeding chamber 1, a substrate, and / or the catalytic layer is transported to the first processing chamber 2; the substrate and / or the catalytic layer is pretreated in the first processing chamber 2, and then passes through the first balancing chamber 3, the first thin film preparation chamber 4, The second balance chamber 5 is transferred to the second thin film deposition chamber 6; in the second thin film preparation chamber 6, the precursor deposition of the two-dimensional nano-film is implanted by the physical vapor deposition systems 34 and 36, such as an ion implantation deposition system. Into the substrate and / or the catalytic layer, then through the third balance chamber 7, is transferred to the chemical vapor deposition chamber 8; in the chemical vapor deposition chamber 8, the sample is processed to form a two-dimensional nano-film; The prepared two-dimensional nano film is transferred to the atmosphere through the discharge chamber 9, thereby completing the continuous preparation of the two-dimensional nano film.

While the invention has been shown and described with reference to the exemplary embodiments of the embodiments of the invention This article makes various changes in form and detail.

Claims

Claim

1. Scaled equipment for continuously preparing two-dimensional nanofilms, including a feed chamber, a first film preparation chamber, and a discharge chamber, characterized by:

The feed chamber, the first film preparation chamber and the discharge chamber are each provided with a sample transfer device;

The feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first film preparing chamber, and a valve is arranged between the first film preparing chamber and the discharging chamber. The material chamber is provided with a valve that is open to the atmosphere;

At least one of the feeding chamber, the first film preparation chamber and the discharge chamber is provided with a heating device; the feeding chamber, the first film preparing chamber and the discharging chamber respectively Connecting a separate evacuation device; at least one of the feed chamber, the first membrane preparation chamber, and the discharge chamber is provided with one or more gas connections.

2. The apparatus for continuously preparing a two-dimensional nano film according to claim 1, wherein: at least one of the feeding chamber, the first film preparing chamber, and the discharging chamber is provided There is a chemical vapor deposition system.

3. The apparatus for continuously preparing a two-dimensional nano film according to claim 1, wherein: at least one of the feeding chamber, the first film preparing chamber, and the discharging chamber is provided. There is a physical vapor deposition system.

4. The apparatus for large-scale continuous preparation of a two-dimensional nanofilm according to claim 1, wherein: at least one of said feed chamber, said first film preparation chamber, and said discharge chamber The temperature is controlled at 20~1600 °C.

5. Apparatus for continuously preparing a two-dimensional nanofilm in a large scale, comprising a feed chamber, a first film preparation chamber, a first balance chamber, and a chemical vapor deposition chamber, characterized by:

The sample chamber, the first film preparation chamber, the first balance chamber and the chemical vapor deposition chamber are each provided with a sample transfer device;

The feed chamber is provided with a valve that communicates with the atmosphere, a valve is disposed between the feed chamber and the first film preparation chamber, and a valve is disposed between the first film preparation chamber and the first balance chamber. a valve is disposed between the first balance chamber and the chemical vapor deposition chamber, and the chemical vapor deposition chamber is provided with a valve that is open to the atmosphere;

The first film preparation chamber is provided with a physical vapor deposition system;

The feed chamber, the first film preparation chamber, the first balance chamber, and the chemical vapor deposition chamber are each provided with a vacuuming device.

6. The apparatus for continuously preparing a two-dimensional nano film according to claim 5, wherein: at least one of the feeding chamber, the first film preparing chamber, and the first balancing chamber With a gas connection.

7. The apparatus for continuously producing a two-dimensional nanofilm according to claim 5, wherein: at least one of the feed chamber and the first film preparation chamber is provided with a sample processing device.

8. The apparatus for continuously preparing a two-dimensional nano film in a large scale, comprising sequentially providing a feeding chamber, a first processing chamber, a first balance chamber, a first film preparation chamber, a second balance chamber, a second processing chamber and a discharge chamber, wherein: the feeding chamber is provided with a valve that communicates with the atmosphere, and a valve is disposed between the feeding chamber and the first processing chamber, the first processing chamber and the first A valve is disposed between the balance chambers, a valve is disposed between the first balance chamber and the first film preparation chamber, and a valve is disposed between the first film preparation chamber and the second balance chamber, and the second balance chamber a valve is disposed between the chamber and the second processing chamber, a valve is disposed between the second processing chamber and the discharge chamber, and the discharge chamber is provided with a valve that is open to the atmosphere;

a sample transfer device is provided in the feed chamber, the first processing chamber, the first balance chamber, the first film preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber;

At least one of the feed chamber, the first processing chamber, the first membrane preparation chamber, the second processing chamber, and the discharge chamber is provided with a heating device;

At least one of the feed chamber, the first processing chamber, the first balancing chamber, the first membrane preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber is provided with one or Multiple gas connections;

The feed chamber, the first processing chamber, the first balancing chamber, the first film preparation chamber, the second balance chamber, the second processing chamber, and the discharge chamber are each connected to a separate vacuuming device.

9. The apparatus for continuously preparing a two-dimensional nano film according to claim 8, wherein: at least one of the first processing chamber, the first film preparation chamber, and the second processing chamber The chamber is equipped with a chemical vapor deposition system.

10. The apparatus for continuously preparing a two-dimensional nano film according to claim 8, wherein: at least one of the first processing chamber, the first film preparation chamber, and the second processing chamber The chamber is equipped with a physical vapor deposition system.

11. An apparatus for continuously preparing a two-dimensional nano film in a large scale, characterized in that: a feeding chamber, a first processing chamber, and a first a balance chamber, a first film preparation chamber, a second balance chamber, a second film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a discharge chamber, wherein:

The feeding chamber is provided with a valve communicating with the atmosphere, a valve is arranged between the feeding chamber and the first processing chamber, and a valve is arranged between the first processing chamber and the first balancing chamber, the first balancing chamber a valve is disposed between the first film preparation chamber and the second balance chamber, and a valve is disposed between the second balance chamber and the second film preparation chamber, a valve is disposed between the film preparation chamber and the third balance chamber, a valve is disposed between the third balance chamber and the chemical vapor deposition chamber, and a valve is disposed between the chemical vapor deposition chamber and the discharge chamber. The discharge chamber is provided with a valve that is open to the atmosphere;

a feed chamber, a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor deposition chamber, and a a sample transfer device is disposed in the chamber of the material chamber; a feed chamber, a first processing chamber, a first balance chamber, a first film preparation chamber, a second balance chamber, a second film preparation chamber, a chamber of at least one of the third balance chamber, the chemical vapor deposition chamber and the discharge chamber is provided with a vacuuming device; and a chamber of at least one of the first film preparation chamber and the second film preparation chamber is provided Physical vapor deposition system; a feed chamber, a first processing chamber, a first balance chamber, a first thin film preparation chamber, a second balance chamber, a second thin film preparation chamber, a third balance chamber, a chemical vapor phase At least one of the deposition chamber and the discharge chamber is provided with one or more gas connections;

A heating device is provided in the chamber of the chemical vapor deposition chamber.

12. The apparatus for continuously producing a two-dimensional nano film according to claim 11, wherein: at least one of the first processing chamber, the first film preparation chamber, and the second film preparation chamber A heating device is arranged in the chamber.

13. The apparatus for continuously preparing a two-dimensional nanofilm according to claim 11, wherein: the first processing chamber is provided with a sample processing device.

14. The apparatus for continuously preparing a two-dimensional nano film according to claim 5 or 11, wherein the chemical vapor deposition chamber further comprises a plasma enhanced chemical vapor deposition system, a microwave plasma chemical vapor deposition system, Any one or a combination of two or more of an aerosol-assisted chemical vapor deposition system and an inductively coupled plasma chemical vapor deposition system.

15. The apparatus for continuously preparing a two-dimensional nanofilm according to claim 3, 5, 10 or 11, wherein: the physical vapor deposition system comprises an ion beam deposition system, a sputtering deposition system, and an electron beam Any one or a combination of two or more of a deposition system, a thermal evaporation deposition system, a laser deposition system, and an ion implantation system.

16. The apparatus for large scale continuous preparation of a two-dimensional nanofilm according to any one of claims 1 to 15, characterized in that: a cavity wall of at least one of the chambers constituting the equipment is provided with a cooling system Preferably, at least one of the feed chamber, the first processing chamber, the first thin film preparation chamber, the second thin film preparation chamber, the third balance chamber, and the chemical vapor deposition chamber The chamber wall is provided with a cooling system.

The apparatus for large-scale continuous preparation of a two-dimensional nano film according to any one of claims 1 to 15, characterized in that: at least one of the chambers constituting the equipment is provided with a heat shielding system; Preferably, the at least one cavity of the feeding chamber, the first processing chamber, the first film preparation chamber, the second film preparation chamber, the third balance chamber, and the chemical vapor deposition chamber There is a heat shield system in the room.

The apparatus for large-scale continuous preparation of a two-dimensional nano film according to any one of claims 1 to 15, characterized in that: the equipment is further provided with a control system, and the control system comprises a sample transfer control system, Any one or a combination of two or more of a pneumatic control system, a vacuum control system, a valve control system, or a temperature control system.

The apparatus for continuously producing a two-dimensional nano film according to any one of claims 1 to 15, characterized in that: the sample conveying device comprises any one or more of a roller, a conveyor belt and a pulley. The combination.

The apparatus for continuously preparing a two-dimensional nano film according to any one of claims 1 to 15, wherein: the two-dimensional nano film comprises graphene, a metal chalcogenide, a silicon thinner, and a thinner Or boron nitride.