CN102634769A - Equipment for continuously preparing two-dimensional nano thin film - Google Patents
Equipment for continuously preparing two-dimensional nano thin film Download PDFInfo
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- CN102634769A CN102634769A CN2012100959368A CN201210095936A CN102634769A CN 102634769 A CN102634769 A CN 102634769A CN 2012100959368 A CN2012100959368 A CN 2012100959368A CN 201210095936 A CN201210095936 A CN 201210095936A CN 102634769 A CN102634769 A CN 102634769A
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Abstract
The invention discloses equipment for continuously preparing a two-dimensional nano thin film, comprising a feeding chamber, a sample preparing chamber, a discharging chamber and the like, wherein a valve is arranged between every two chambers; a sample is transferred among the chambers through a sample conveying device including an idler wheel or a conveying belt and the like; all the chambers are respectively connected with independent vacuumizing devices and gas pipelines; a sample preparing chamber is provided with a physical vapor deposition system or a chemical vapor deposition system and the like; the feeding chamber is provided with a heating device or a surface treatment system of plasmas and the like; the discharging chamber is provided with the heating device and the like; the whole equipment is provided with an automation control system to control the opening and the closing of the valve between the chambers, the transportation of samples, the operation of a vacuum system, the control of an air flow and the like. The equipment has the advantages of simple structure, reliable work and can continuously prepare a uniform two-dimensional nano thin film of graphene, transition metal sulfide, silylene, germylene or boron nitride and the like, and is suitable for industrial preparation of the two-dimensional nano thin film.
Description
Technical field
The present invention relates to a kind of equipment of two-dimensional nano film preparation, particularly a kind of equipment of continuous preparation two-dimensional nano film.
Background technology
Graphene has remarkable two-dimentional electricity, optics, calorifics, mechanical property and chemicalstability, and Graphene is with a wide range of applications at aspects such as ultrafast opto-electronic device, clear energy sources, transmitters.Electronics transmission speed in Graphene is 150 times of silicon, and leading companys such as IBM have prepared the supper-fast opto-electronic device that speed can reach Terahertz, and California, USA university utilizes Graphene to be developed into the optical modulation detuner, is expected to network speed is improved 10,000 times; The demand of the annual semi-conductor crystal silicon in the whole world is about 2500 tons, if the crystal silicon of Graphene alternative 1/10th is processed high-end unicircuit such as radio circuit, market capacity is at least more than 5,000 hundred million yuan.Because Graphene has only 2.3% photoabsorption; This makes Graphene can be used for preparing the flexible and transparent electrode of opto-electronic device such as display device, solar cell, touch panel etc., thereby replaces cost costliness, resource scarcity, what can not freely fold is the ITO nesa coating of staple by indium.It is reported that the demand of global ITO nesa coating in 2011 is at 8,500 ten thousand-9,500 ten thousand, like this, the development space of the alternative ITO nesa coating of Graphene is huge.Because the electron transport property that Graphene is unique, as transmitter, it has monomolecular susceptibility; If the gene electronics sequencing technologies based on Graphene can be realized; The order-checking cost that human full gene spectrogram is measured will be reduced to about 1000 dollars/people greatly by present about 100,000 dollars/people; Thereby help biomedical innovation, help to realize personalized health care.Through fast development in recent years, the Graphene product appears on the touch-screen applications.Therefore, the Graphene good commercial is worth and vast market has represented dawn, and the industrialization of grapheme material will be the revolution property change to material, information, energy industry!
Except Graphene, the novel two-dimensional nano film of type Graphene also has its unique photoelectron performance, is with a wide range of applications.The novel two-dimensional nano film of class Graphene comprises lamellated metallizing sulfide (transition metal dichalcogenides), silene (silicene), germanium alkene (germanene), the SP 1 (boron nitride) etc. crossed
Chemical Vapor deposition process (CVD) and carbon segregation (surface segregation) method is the technological method of present large-area preparation graphene film, the equipment that adopts these two kinds of methods to prepare graphene film all be basically quartz tube furnace [
Science324,1312-1314 (2009);
Nature Nanotechnology5,574 (2010);
Nano Lett.11,297-303 (2011)].But quartz tube furnace only possesses the simple function of synthesizing graphite alkene film on existing metal catalytic layer, can not realize to substrate material surface treatment, on substrate required Catalytic Layer, the graphene film synthetic successive processes of preparation synthesizing graphite alkene.And, adopt quartz tube furnace synthetic graphene film to have textural defect, cause electronic transmission performance relatively poor, quartz tube furnace has seriously restricted the application of two-dimensional nano film such as graphene film.
Summary of the invention
Deficiency to prior art; The present invention provide a kind of can big area the equipment of the novel two-dimensional nano film of preparation continuously; Characteristics such as that this equipment has is simple in structure, simple to operate, security is good adopt this equipment to prepare that the technology of two-dimensional nano film is simple, cost film lower, that prepare has good structure and performance.
A kind of equipment of continuous preparation two-dimensional nano film comprises charging chamber, specimen preparation chamber and discharging chamber.
Described charging chamber, specimen preparation chamber and discharging chamber are equipped with device for transferring samples; Sample can be transferred to the specimen preparation chamber from the charging chamber through device for transferring samples; Be transferred to the discharging chamber from the specimen preparation chamber, so that realize the continuous preparation of two-dimensional nano film; Described device for transferring samples comprises any one or the combination more than two kinds in roller, pulley and the travelling belt.
Described charging chamber is provided with the valve with atmosphere, is provided with valve between charging chamber and the specimen preparation chamber, is provided with valve between specimen preparation chamber and the discharging chamber, and the discharging chamber is provided with the valve with atmosphere.
Have at least a chamber to be provided with heating unit in described charging chamber, specimen preparation chamber and the discharging chamber; Heating unit can be wire spiral heating unit, infrared heating device, laser heating device etc.
Described charging chamber, specimen preparation chamber and discharging chamber are respectively equipped with independently vacuum extractor; Each vacuum extractor comprises various vacuum pumps, vacuum pipe, vacuum valve, vacuumometer etc., can make the vacuum tightness of each chamber remain on normal pressure to 10 through vacuum extractor
-10Between the Pa.
At least one chamber in described charging chamber, specimen preparation chamber and the discharging chamber is provided with one or more gas communication ports, and the gas communication port can be a kind of communication port of gas, and the gas communication port also can be connected with gas mixing box; The inlet of gas mixing box is parallel with two or above gas circuit at least, can make two kinds or above gas get into gas mixing box simultaneously; Each gas circuit all is provided with mass flowmeter and electromagnet cut off valve etc., thus can be independently the accurate flow of pilot-gas; The gas that feeds can be selected from rare gas element such as argon gas or nitrogen, reducing gas such as hydrogen, oxidizing gas such as oxygen, synthetic required gasiform presoma such as the CH of two-dimensional nano film
4, C
2H
4, C
2H
2, NH
3, B
3N
3H
6Or alcoholic acid steam etc.
At least one chamber in described charging chamber, specimen preparation chamber and the discharging chamber is provided with chemical gas-phase deposition system, comprises plasma reinforced chemical vapor deposition system and microwave plasma chemical gas-phase deposition system etc.; Any one chamber in charging chamber, specimen preparation chamber or the discharging chamber all can constitute chemical gas-phase deposition system with heating unit and gas communication port.
At least one chamber in described charging chamber, specimen preparation chamber and the discharging chamber is provided with physics vapour deposition system, and described physics vapour deposition system is any one or the combination more than two kinds in sputtering target thin film deposition system, electron beam gun depositing system, ion gun depositing system, ion injection deposition system and the hot deposition system.
Any one chamber in charging chamber, specimen preparation chamber or the discharging chamber can both comprise chemical gas-phase deposition system, comprised physics vapour deposition system again.
The temperature of at least one chamber in described charging chamber, specimen preparation chamber or the discharging chamber is controlled at 20 ~ 1600 oC;
As preferably, in order heat to be concentrated on the sample place, and reduce to the place that does not need heat and transmit, the chamber wall of at least one chamber in described charging chamber, specimen preparation chamber and the discharging chamber is provided with heat shield system;
As preferably, in order to make the device security steady running, the chamber wall of at least one chamber in described charging chamber, specimen preparation chamber and the discharging chamber is provided with cooling system, and cooling system can be double-deck water-cooling system.
As preferably, be provided with the chamber of heat shield system in the chamber, the chamber wall of this chamber is provided with cooling system simultaneously.
As preferably; The equipment of continuous preparation two-dimensional nano film of the present invention can also be provided with system, and described system comprises any one or the combination more than two kinds in sample transmission control system, air-path control system, vacuum-control(led) system, valve control system or the temperature controlling system.
Equipment of the present invention can be used for growth and comprises Graphene, crosses two-dimensional nano films such as metallizing sulfide, silene, germanium alkene or SP 1; According to the difference of institute's synthetic two-dimensional nano film, can suitably select to prepare presomas such as required solid, liquid or gas.
As preferably, the charging chamber is as the surface treatment chamber, and the specimen preparation chamber is as the preparation chamber of substrate, Catalytic Layer and two-dimensional nano film, and the discharging chamber is as the treatment chamber again of cooling chamber or two-dimensional nano film; The charging chamber is provided with the Surface Treatment with Plasma device, and the specimen preparation chamber is provided with thin film deposition system.
The primary process of preparation two-dimensional nano film comprises continuously: will synthesize required substrate material of two-dimensional nano film or Catalytic Layer and be placed on the material containing stand; Be transferred to the specimen preparation chamber by device for transferring samples through the charging chamber; Utilize physical vapor deposition or chemical gaseous phase depositing process to prepare the two-dimensional nano film at the specimen preparation chamber, then the two-dimensional nano film for preparing is delivered to the discharging chamber by device for transferring samples.
Continuously the primary process of preparation two-dimensional nano film also comprises: will synthesize required substrate of two-dimensional nano film or Catalytic Layer and be placed on the material containing stand and be transferred to the charging chamber by device for transferring samples; Under certain atmosphere; Substrate material or Catalytic Layer are carried out pre-treatment at the charging chamber earlier, by device for transferring samples substrate or Catalytic Layer are transferred to the specimen preparation chamber then; In the specimen preparation chamber, utilize physical vapor deposition or chemical gaseous phase depositing process to prepare Catalytic Layer, carbon film or two-dimensional nano film; Can deliver to the discharging chamber by device for transferring samples after the film preparation heat-treats or carries out surface optimization and handle.
Equipment of the present invention has the characteristics of continuous preparation two-dimensional nano film; Can big area, scale preparation such as Graphene, cross two-dimensional nano films such as metallizing sulfide, silene, germanium alkene or SP 1; Help to realize the large-scale production of two-dimensional nano film, promote the application of two-dimensional nano film.
Description of drawings
Fig. 1 is the one-piece construction synoptic diagram of continuous preparation two-dimensional nano membrane equipment of the present invention, and wherein, the specimen preparation chamber is provided with heating unit;
Fig. 2 is the one-piece construction synoptic diagram of continuous preparation two-dimensional nano membrane equipment of the present invention, and wherein, specimen preparation chamber and discharging chamber are equipped with heating unit, and the discharging chamber is provided with heat shield system and cooling system, and the discharging chamber is provided with a gas mixing box communication port;
Fig. 3 is the one-piece construction synoptic diagram of continuous preparation two-dimensional nano membrane equipment of the present invention; Wherein, The charging chamber is provided with surface processor, and the specimen preparation chamber is provided with gas-phase deposition system, heating unit, heat shield system and cooling system, and the discharging chamber is provided with heating unit;
Fig. 4 is the one-piece construction synoptic diagram of continuous preparation two-dimensional nano membrane equipment of the present invention; Wherein, The charging chamber is provided with surface processor and heating unit, and the specimen preparation chamber is provided with gas-phase deposition system, heating unit, heat shield system and cooling system, and the discharging chamber is provided with heating unit;
Fig. 5 is the one-piece construction synoptic diagram of continuous preparation two-dimensional nano membrane equipment of the present invention; Wherein, The charging chamber is provided with surface processor and heating unit; The specimen preparation chamber is provided with gas-phase deposition system, heating unit, heat shield system and cooling system, and the discharging chamber is provided with surface processor, heating unit and cooling system.
Shown in the figure:
1---roller, 2---the material containing stand, 4---the charging chamber;
5---the first surface treater, 6---first heating unit,
7---the specimen preparation chamber, 8---cooling system, 9---heat shield system;
11---second heating unit, 12---the discharging chamber, 13---the second surface treater;
14---the 3rd heating unit, 15---pulley, 16---gas valve;
17---gas path pipe, 18---gas mixing box, 20---travelling belt;
21---first gas-phase deposition system, 22---second gas-phase deposition system;
31,32,33---valve, 40,41,42,43,44,45,46,47---gas circuit;
50,51,52---vacuum extractor.
Embodiment
The technique effect that is produced in order more to be expressly understood the present invention and the present invention is done further explain below in conjunction with accompanying drawing to the present invention.
Embodiment 1:
Referring to Fig. 1, the equipment of continuous preparation two-dimensional nano film of the present invention comprises: charging chamber 4, specimen preparation chamber 7, discharging chamber 12; Whole plant is equipped with the roller 1 that transmits sample at charging chamber 4, specimen preparation chamber 7 and discharging chamber 12; Charging chamber 4 is provided with the valve 31 with atmosphere, is provided with valve 32 between charging chamber 4 and the specimen preparation chamber 7, is provided with valve 33 between specimen preparation chamber 7 and the discharging chamber 12, and discharging chamber 12 is provided with the valve 34 with atmosphere; Through roller and valve charging chamber 4, specimen preparation chamber 7 and discharging chamber 12 are connected into an integral body.
Be provided with second heating unit 11 in the specimen preparation chamber 7.
Charging chamber 4 is provided with vacuum extractor 50, and specimen preparation chamber 7 is provided with vacuum extractor 51, and discharging chamber 12 is provided with vacuum extractor 52.
Charging chamber 4 is provided with a gas communication port 40, and specimen preparation chamber 7 is provided with two gas communication ports 41,42, and discharging chamber 12 is provided with a gas communication port 43.Flow for accurate pilot-gas; Each gas communication port is connected with mass flowmeter and controls the flow of each gas; The two ends of each mass flowmeter respectively are provided with an electromagnet cut off valve, and electromagnet cut off valve is connected with the gas communication port through pipeline with mass flowmeter.
Specimen preparation chamber 7, second heating unit 11 and gas communication port 41,42 have constituted a chemical gas-phase deposition system.
The primary process of preparation two-dimensional nano film is continuously: will synthesize required substrate material of two-dimensional nano film and/or Catalytic Layer material and be placed on the material containing stand 2; Be transferred to specimen preparation chamber 7 by roller 1 through charging chamber 4; Utilize chemical gaseous phase depositing process to prepare the two-dimensional nano film at specimen preparation chamber 7, deliver to discharging chamber 12 by roller 1 after the specimen preparation.
Embodiment 2:
Referring to Fig. 2, the equipment of continuous preparation two-dimensional nano film of the present invention comprises: charging chamber 4, specimen preparation chamber 7, discharging chamber 12; Whole plant is equipped with the pulley 15 that transmits sample at charging chamber 4, specimen preparation chamber 7 and discharging chamber 12; Charging chamber 4 is provided with the valve 31 with atmosphere, is provided with valve 32 between charging chamber 4 and the specimen preparation chamber 7, is provided with valve 33 between specimen preparation chamber 7 and the discharging chamber 12, and discharging chamber 12 is provided with the valve 34 with atmosphere; With charging chamber 4, specimen preparation chamber 7 connects into an integral body with discharging chamber 12 through pulley and valve.
Be provided with second heating unit 11 in the specimen preparation chamber 7, discharging chamber 12 is provided with the 3rd heating unit 14.
Because the temperature of the chamber of discharging chamber 12 may in order to improve the utilization to heat, be provided with heat shield system 9 and chamber wall and be provided with cooling system 8 in case the chamber wall is overheated up to hundreds of degree even thousands of degree in the chamber.
Charging chamber 4 is provided with vacuum extractor 50, and specimen preparation chamber 7 is provided with vacuum extractor 51, and discharging chamber 12 is provided with vacuum extractor 52.
Charging chamber 4 is provided with a gas communication port 40, and specimen preparation chamber 7 is provided with a gas communication port 41, and discharging chamber 12 is provided with a gas communication port 43 and a gas mixing box 18, two gas communication ports 46,47 of inlet parallel connection of gas mixing box 18; Each gas communication port is connected with mass flowmeter and controls the flow of each gas; The two ends of each mass flowmeter respectively are provided with an electromagnet cut off valve; Electromagnet cut off valve is connected with gas mixing box or gas communication port through pipeline with mass flowmeter, thus the accurate flow of pilot-gas.
The primary process of preparation two-dimensional nano film is continuously: will synthesize required substrate material of two-dimensional nano film and/or Catalytic Layer material and be placed on the material containing stand 2; Be transferred to specimen preparation chamber 7 by pulley 15 through charging chamber 4; Substrate/Catalytic Layer is heat-treated at specimen preparation chamber 7; Be sent to discharging chamber 12 by pulley 15 then; Utilize chemical gaseous phase depositing process to prepare the two-dimensional nano film, be sent to outside the discharging chamber 12 by the pulley device for transferring samples after the two-dimensional nano film preparation.
Embodiment 3:
Referring to Fig. 3, the equipment of continuous preparation two-dimensional nano film of the present invention comprises: charging chamber 4, specimen preparation chamber 7, discharging chamber 12; Whole plant is equipped with the roller 1 that transmits sample at charging chamber 4, specimen preparation chamber 7 and discharging chamber 12; Charging chamber 4 is provided with the valve 31 with atmosphere, is provided with valve 32 between charging chamber 4 and the specimen preparation chamber 7, is provided with valve 33 between specimen preparation chamber 7 and the discharging chamber 12, and discharging chamber 12 is provided with the valve 34 with atmosphere; With charging chamber 4, specimen preparation chamber 7 connects into an integral body with discharging chamber 12 through roller and valve.
Be provided with first surface treater 5 in the charging chamber 4, be provided with second heating unit 11 in the specimen preparation chamber 7, discharging chamber 12 is provided with the 3rd heating unit 14.
Specimen preparation chamber 7 is provided with two gas-phase deposition systems: first gas-phase deposition system 21 and second gas-phase deposition system 22 can be the arbitrary combination of physical vapor system and chemical gas-phase deposition system.
Described first gas-phase deposition system or second gas-phase deposition system are physics vapour deposition system, comprise any one or the combination more than two kinds in sputtering target thin film deposition system, electron beam gun depositing system, ion gun depositing system, ion injection deposition system and the hot deposition system; First gas-phase deposition system or second gas-phase deposition system can be chemical gas-phase deposition systems also, comprise any one or the combination more than two kinds in plasma reinforced chemical vapor deposition system and the microwave plasma chemical gas-phase deposition system.
Because the temperature of specimen preparation chamber 7 may be up to hundreds of degree even thousands of degree; Like this in order heat to be concentrated on required place; And reduce to the place that does not need heat and transmit; Be provided with heat shield system 9 in the specimen preparation chamber, the chamber wall is provided with cooling system 8 simultaneously, and cooling system can be double-deck water-cooling system.
Charging chamber 4 is provided with vacuum extractor 50, and specimen preparation chamber 7 is provided with vacuum extractor 51, and discharging chamber 12 is provided with vacuum extractor 52.
Charging chamber 4 is provided with a gas communication port 40, and discharging chamber 12 is provided with a gas communication port 43; Specimen preparation chamber 7 is provided with two gas communication ports, and one of them communication port is 41, and another communication port links to each other with gas mixing box 18, three gas communication ports 42,44 and 45 of inlet parallel connection of gas mixing box 18; Flow for accurate pilot-gas; Each gas communication port is connected with mass flowmeter and controls the flow of each gas; The two ends of each mass flowmeter respectively are provided with an electromagnet cut off valve, and electromagnet cut off valve is connected with gas mixing box or gas communication port through pipeline with mass flowmeter.
Continuously the primary process of preparation two-dimensional nano film is: will synthesize the required substrate material of two-dimensional nano film and be placed on the material containing stand 2 and be transferred to charging chamber 4 by roller 1; Under certain atmosphere; Substrate material carries out pre-treatment at charging chamber 4, by roller 1 substrate material is transferred to specimen preparation chamber 7 then; Utilize physical gas-phase deposite method such as electron beam gun deposition preparation Catalytic Layer in first gas-phase deposition system 21 in specimen preparation chamber 7; In second gas-phase deposition system 22, utilize another kind of physical gas-phase deposite method such as ion implantation to inject the presoma of two-dimensional nano material in the Catalytic Layer then, be sent to discharging chamber 12 afterwards; At discharging chamber 12, the sample of the presoma that is injected with the two-dimensional nano material is handled and formed the two-dimensional nano film.
Embodiment 4:
Referring to Fig. 4, the equipment of continuous preparation two-dimensional nano film of the present invention comprises: charging chamber 4, specimen preparation chamber 7, discharging chamber 12; Whole plant is equipped with the roller 1 that transmits sample at charging chamber 4, specimen preparation chamber 7 and discharging chamber 12; Charging chamber 4 is provided with the valve 31 with atmosphere, is provided with valve 32 between charging chamber 4 and the specimen preparation chamber 7, is provided with valve 33 between specimen preparation chamber 7 and the discharging chamber 12, and discharging chamber 12 is provided with the valve 34 with atmosphere; With charging chamber 4, specimen preparation chamber 7 connects into an integral body with discharging chamber 12 through roller and valve.
Be provided with the first surface treater 5 and first heating unit 6 in the charging chamber 4, be provided with second heating unit 11 in the specimen preparation chamber 7, discharging chamber 12 is provided with the 3rd heating unit 14.
Specimen preparation chamber 7 is provided with first gas-phase deposition system 21; Described first gas-phase deposition system is a physics vapour deposition system or/and chemical gas-phase deposition system, and described physics vapour deposition system comprises any one or the combination more than two kinds in sputtering target thin film deposition system, electron beam gun depositing system, ion gun depositing system, ion injection deposition system and the hot deposition system; Described chemical gas-phase deposition system comprises plasma reinforced chemical vapor deposition system and microwave plasma chemical gas-phase deposition system etc.; Physics vapour deposition system and chemical gas-phase deposition system can arbitrary combination.
Because the temperature of specimen preparation chamber 7 may be up to hundreds of degree even thousands of degree; Like this in order heat to be concentrated on required place; And reduce to the place that does not need heat and transmit; Be provided with heat shield system 9 in the specimen preparation chamber, the chamber wall is provided with cooling system 8 simultaneously, and cooling system can be double-deck water-cooling system.
Charging chamber 4 is provided with vacuum extractor 50, and specimen preparation chamber 7 is provided with vacuum extractor 51, and discharging chamber 12 is provided with vacuum extractor 52.
Charging chamber 4 is provided with a gas communication port 40; Discharging chamber 12 is provided with a gas communication port 43; Specimen preparation chamber 7 is provided with two gas communication ports 41,42; Each gas communication port is connected with mass flowmeter and controls the flow of each gas, and the two ends of each mass flowmeter respectively are provided with an electromagnet cut off valve, and electromagnet cut off valve is connected with the gas communication port through pipeline with mass flowmeter.
Discharging chamber 12, discharging chamber heating unit 14 and gas communication port 43 constitute chemical gas-phase deposition system.
Continuously the primary process of preparation two-dimensional nano film is: will synthesize the required substrate material of two-dimensional nano film and be placed on the material containing stand 2 and be transferred to charging chamber 4 by roller 1; Under certain atmosphere and under the temperature; Substrate material carries out pre-treatment at charging chamber 4, by roller 1 substrate material is transferred to specimen preparation chamber 7 then; In specimen preparation chamber 7, utilize physical gas-phase deposite method, be sent to discharging chamber 12 then, adopt chemical gaseous phase depositing process to prepare the two-dimensional nano film at discharging chamber 12 or/and chemical gaseous phase depositing process prepares Catalytic Layer.
Embodiment 5:
Referring to Fig. 5, the equipment of continuous preparation two-dimensional nano film of the present invention comprises: charging chamber 4, specimen preparation chamber 7, discharging chamber 12; Whole plant is equipped with sample travelling belt 20 at charging chamber 4, specimen preparation chamber 7 and discharging chamber 12; Charging chamber 4 is provided with the valve 31 with atmosphere, is provided with valve 32 between charging chamber 4 and the specimen preparation chamber 7, is provided with valve 33 between specimen preparation chamber 7 and the discharging chamber 12, and discharging chamber 12 is provided with the valve 34 with atmosphere; With charging chamber 4, specimen preparation chamber 7 connects into an integral body with discharging chamber 12 through travelling belt and valve.
Be provided with the first surface treater 5 and first heating unit 6 in the charging chamber 4, be provided with second heating unit 11 in the specimen preparation chamber 7, discharging chamber 12 is provided with second surface treater 13 and the 3rd heating unit 14.
Specimen preparation chamber 7 is provided with first gas-phase deposition system 21; Described first gas-phase deposition system is a physics vapour deposition system or/and chemical gas-phase deposition system, and described physics vapour deposition system comprises any one or the combination more than two kinds in sputtering target thin film deposition system, electron beam gun depositing system, ion gun depositing system, ion injection deposition system and the hot deposition system; Described chemical gas-phase deposition system comprises plasma reinforced chemical vapor deposition system and microwave plasma chemical gas-phase deposition system etc.; Physics vapour deposition system and chemical gas-phase deposition system can arbitrary combination.
Be provided with heat shield system 9 in the specimen preparation chamber 7 to reduce heat to unwanted local the transmission, the chamber wall is provided with cooling system 8 in order to avoid the chamber wall is overheated.
Because pyritous exists, discharging chamber 12 is provided with cooling system 8.
Charging chamber 4 is provided with vacuum extractor 50, and specimen preparation chamber 7 is provided with vacuum extractor 51, and discharging chamber 12 is provided with vacuum extractor 52.
Charging chamber 4 is provided with a gas communication port 40, and discharging chamber 12 is provided with a gas communication port 43; Specimen preparation chamber 7 is provided with two gas communication ports, and one of them communication port is 41, and another communication port links to each other with gas mixing box 18, three gas communication ports 42,44 and 45 of inlet parallel connection of gas mixing box 18; Flow for accurate pilot-gas; Each gas communication port is connected with mass flowmeter and controls the flow of each gas; The two ends of each mass flowmeter respectively are provided with an electromagnet cut off valve, and electromagnet cut off valve is connected with gas mixing box or gas communication port through pipeline with mass flowmeter.
Charging chamber 4, heating unit 6 constitute chemical gas-phase deposition system with gas communication port 40; Discharging chamber 12, heating unit 14 constitute chemical gas-phase deposition system with gas communication port 43.
Continuously the primary process of preparation two-dimensional nano film is: will synthesize the required substrate material of two-dimensional nano film and be placed on the material containing stand 2 and be transferred to charging chamber 4 by travelling belt 20; Under certain atmosphere and temperature; Substrate material carries out pre-treatment at charging chamber 4, by travelling belt 20 substrate material is transferred to specimen preparation chamber 7 then; In specimen preparation chamber 7, utilize physical gas-phase deposite method, adopt chemical gaseous phase depositing process to prepare the two-dimensional nano film then or/and chemical gaseous phase depositing process prepares Catalytic Layer; The two-dimensional nano film for preparing is sent to discharging chamber 12 by device for transferring samples, can carry out surface treatment to it at discharging chamber 12.
Though clearly displaying and reference example embodiment of the present invention have been described the present invention; But be understood by those skilled in the art that; Can not break away under the situation that the spirit and scope of the present invention that appended claims defines are arranged, to this paper do on the various forms with details on change.
Claims (10)
1. an equipment for preparing the two-dimensional nano film continuously comprises charging chamber (4), specimen preparation chamber (7), and discharging chamber (12) is characterized in that:
Described charging chamber (4), specimen preparation chamber (7) and discharging chamber (12) are equipped with device for transferring samples;
Described charging chamber (4) is provided with the valve (31) with atmosphere; Be provided with valve (32) between charging chamber (4) and the specimen preparation chamber (7); Be provided with valve (33) between specimen preparation chamber (7) and the discharging chamber (12), discharging chamber (12) is provided with the valve (34) with atmosphere;
Have at least a chamber to be provided with heating unit in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12);
Described charging chamber (4), specimen preparation chamber (7) and discharging chamber (12) are connected independently vacuum extractor respectively;
At least one chamber in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12) is provided with one or more gas communication ports.
2. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that at least one chamber in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12) is provided with chemical gas-phase deposition system.
3. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that at least one chamber in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12) is provided with physics vapour deposition system.
4. the equipment of continuous preparation two-dimensional nano film according to claim 3 is characterized in that described physics vapour deposition system is any one or the combination more than two kinds in sputtering target thin film deposition system, electron beam gun depositing system, ion gun depositing system, ion injection deposition system and the hot deposition system.
5. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that the temperature of at least one chamber in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12) is controlled at 20 ~ 1600 oC.
6. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that the chamber wall of at least one chamber in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12) is provided with cooling system (8).
7. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that being provided with heat shield system (9) at least one chamber in described charging chamber (4), specimen preparation chamber (7) and the discharging chamber (12).
8. the equipment of continuous preparation two-dimensional nano film according to claim 1; It is characterized in that it also is provided with system, described system comprises any one or the combination more than two kinds in sample conveying control system, air-path control system, vacuum-control(led) system, valve control system or the temperature controlling system.
9. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that described device for transferring samples comprises any one or the combination more than two kinds in roller, pulley and the travelling belt.
10. the equipment of continuous preparation two-dimensional nano film according to claim 1 is characterized in that described two-dimensional nano film comprises Graphene, crosses metallizing sulfide, silene, germanium alkene or SP 1.
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CN2012100959368A CN102634769A (en) | 2012-04-02 | 2012-04-02 | Equipment for continuously preparing two-dimensional nano thin film |
PCT/CN2013/073573 WO2013149572A1 (en) | 2012-04-02 | 2013-04-01 | Equipment for large-scale continuous preparation of two-dimensional nanometer thin film |
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103011139A (en) * | 2012-11-13 | 2013-04-03 | 重庆绿色智能技术研究院 | Preparation method and device for graphene |
CN103074580A (en) * | 2012-12-25 | 2013-05-01 | 王奉瑾 | PVD equipment adopting electromagnetic heating |
WO2013149572A1 (en) * | 2012-04-02 | 2013-10-10 | Xu Mingsheng | Equipment for large-scale continuous preparation of two-dimensional nanometer thin film |
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CN103668453A (en) * | 2012-09-21 | 2014-03-26 | 浙江大学 | Two-dimensional silylene film and preparation method thereof |
CN103011139A (en) * | 2012-11-13 | 2013-04-03 | 重庆绿色智能技术研究院 | Preparation method and device for graphene |
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CN103074580A (en) * | 2012-12-25 | 2013-05-01 | 王奉瑾 | PVD equipment adopting electromagnetic heating |
CN103643287A (en) * | 2013-11-14 | 2014-03-19 | 中国科学院物理研究所 | Germanium olefine two-dimensional atom crystal material and its preparation method |
CN103643287B (en) * | 2013-11-14 | 2016-05-25 | 中国科学院物理研究所 | A kind of preparation method of germanium alkene two dimension atomic crystal material |
CN105314625A (en) * | 2014-08-05 | 2016-02-10 | 常州二维碳素科技股份有限公司 | Graphene growth equipment and method for preparing graphene by graphene growth equipment |
CN105314625B (en) * | 2014-08-05 | 2018-05-25 | 常州二维碳素科技股份有限公司 | A kind of graphene growth equipment and its method for preparing graphene |
CN107732249A (en) * | 2017-09-11 | 2018-02-23 | 张洪 | Copper foil graphene collector and preparation method |
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