CN104477903A - Preparation method of graphene film - Google Patents
Preparation method of graphene film Download PDFInfo
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- CN104477903A CN104477903A CN201410822933.9A CN201410822933A CN104477903A CN 104477903 A CN104477903 A CN 104477903A CN 201410822933 A CN201410822933 A CN 201410822933A CN 104477903 A CN104477903 A CN 104477903A
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Abstract
The invention provides a preparation method of a graphene film. The method comprises steps as follows: providing a substrate; forming a carbon source layer with the uniform thickness on the substrate in a controlled manner; heating the carbon source layer to enable the carbon source layer to have a chemical reaction to be converted into a graphene film layer. Therefore, the uniformity and the thickness of the graphene film can be controlled accurately through accurate control on the uniformity and the thickness of the carbon source layer; meanwhile, the high-quality graphene film can be obtained with the preparation method of the graphene film, and the method can be compatible with the existing CMOS technology and is suitable for mass production.
Description
Technical field
The present invention relates to technical field of integrated circuits, be specifically related to a kind of preparation method of graphene film.
Background technology
As a kind of Multifunction material, Graphene has many excellent specific properties, as the carrier mobility of superelevation, superelevation physical strength, high thermal conductivity, room temperature have quantum hall effect and ferromagnetic characteristic etc.These excellent machinery and photoelectric characteristics just, scientist generally predicts that Graphene has broad application prospects in fields such as electronics, information, the energy, material and biological medicines, is expected to start a new technological revolution in 21st century.
About the basic and applied research of Graphene, scientists has shown high enthusiasm, or even various countries also expand national Innovation Input all at this point, as there are special fund in the U.S., Japan, European Union etc. for Graphene technical study.At present, the preparation that a relatively more outstanding problem is exactly graphene film material is run in Graphene research.In existing research, the preparation method of Graphene mainly comprises mechanically peel method, SiC high-temperature decomposition, chemistry redox method, chemical Vapor deposition process etc., but these preparation methods are difficult to obtain controlled, the uniform high-quality graphene film of the number of plies.
Therefore, how accurately to control Graphene and form the difficult problem that the controlled uniform thin film of thickness is various countries research worker always, it affects the application of graphene film in high performance device field.
Summary of the invention
In order to overcome above problem, the present invention aims to provide a kind of preparation method of graphene film, thus reaches the thickness of graphene film and the object of homogeneity that accurately control to be formed.
To achieve these goals, the invention provides a kind of preparation method of graphene film, it comprises the following steps:
Step 01 a: substrate is provided;
Step 02: control on the substrate to form the uniform carbon source layer of thickness;
Step 03: heat described carbon source layer, makes described carbon source layer generation chemical reaction and changes graphene film layer into.
Preferably, described step 03 specifically comprises:
Step 31: depositing metal catalyst layer on described carbon source layer, to form the multilayered structure of metal catalyst layer-carbon source layer-substrate;
Step 32: carry out anneal to described multilayered structure, reacts to make described carbon source layer and forms graphene film;
Step 33: remove described metal catalyst, obtains pure graphene film.
Preferably, in described step 03, the material of described metal catalyst layer is Cu, Ni, Co, Fe or Pt.
Preferably, the thickness of described carbon source layer is 5-1000A, and the thickness of described metal catalyst layer is 150-250nm.
Preferably, in described step 03, the processing condition of described anneal are: adopt N
2or He protection of inert gas or adopt high vacuum environment, the annealing temperature adopted is 400-1200 DEG C.
Preferably, wet etching method or electrochemical method is adopted to remove described metal catalyst.
Preferably, in described step 02, the material of described carbon source layer is agraphitic carbon, silicon carbide or organic molecular film.
Preferably, described step 03 specifically comprises: under vacuum conditions, and the thermolysis of carbon source layer is obtained described graphene film.
Preferably, the carbon concentration of described substrate is lower than 0.5ppma.
Preferably, described substrate is silicon, silicon oxide, silicon nitride or silica glass substrate, or surface has the silicon base of silicon oxide film.
The preparation method of graphene film of the present invention, first control to form the uniform carbon source layer of thickness in substrate, then make carbon source layer be heated and change graphene film into, like this, by accurately controlling homogeneity and the thickness of carbon source layer, can accurately control graphene film homogeneity and thickness; Meanwhile, the preparation method of Graphene of the present invention can obtain high-quality graphene film, and it can be mutually compatible with existing CMOS technology, is suitable for scale operation.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the preparation method of the Graphene of embodiments of the invention one
Fig. 2 is the schematic flow sheet of the preparation method of the Graphene of embodiments of the invention two
Embodiment
For making content of the present invention clearly understandable, below in conjunction with Figure of description, content of the present invention is described further.Certain the present invention is not limited to this specific embodiment, and the general replacement known by those skilled in the art is also encompassed in protection scope of the present invention.
The preparation method of graphene film of the present invention, it comprises: provide a substrate; Substrate controls the carbon source layer forming certain uniform thickness; Heating carbon source layer, makes carbon source layer generation chemical reaction and changes graphene film layer into.Thus the accurate control that can realize graphene film thickness and homogeneity.
Embodiment one
Preparation method below in conjunction with accompanying drawing 1 and specific embodiment a pair graphene film of the present invention is described in further detail.It should be noted that, accompanying drawing all adopt simplify very much form, use non-ratio accurately, and only in order to object that is convenient, that clearly reach aid illustration the present embodiment.
Refer to Fig. 1, the preparation method of the graphene film of the present embodiment comprises the following steps:
Step 11 a: substrate is provided;
Here, the carbon concentration of the substrate provided requires extremely low, high if any the carbon concentration in substrate, when follow-up anneal, can cause the precipitation of carbon in substrate, thus destroys thickness and the homogeneity of the carbon source layer accurately controlled.The carbon concentration of substrate is lower than 0.5ppma; Substrate can be silicon, silicon oxide, silicon nitride or silica glass substrate, or surface has the silicon base etc. of silicon oxide film, in the present embodiment, adopts surface and has 3000A thickness SiO
2the Si substrate of film, carbon concentration is lower than 0.3ppma.
Step 12: control to form the uniform carbon source layer of thickness in substrate;
Here, ald, molecular beam epitaxy, chemical vapour deposition or Langmuir-Blodgett technique can be adopted accurately to control thickness and the homogeneity of carbon source layer.The material of carbon source layer can be agraphitic carbon, silicon carbide or organic molecular film; The thickness of carbon source layer can be 5-1000A.In the present embodiment, adopt atom layer deposition process in substrate, complete the deposition in five cycles, thus form the agraphitic carbon active layer with 30A uniform thickness.By this step 12, the controlled and uniform carbon source layer of thickness can be formed.
Step 13: depositing metal catalyst layer on carbon source layer, to form the multilayered structure of metal catalyst layer-carbon source layer-substrate;
Here, the thickness of metal catalyst layer can be 150-250nm, and metal catalyst layer is transition metal, such as, can be Cu, Ni, Co, Fe or Pt etc.The physical gas-phase deposite methods such as sputtering, electron beam evaporation, pulsed laser deposition can be adopted to prepare metal catalyst layer.In the present embodiment, adopt physical vaporous deposition at amorphous carbon layer/SiO
2/ Si substrate deposits the Cu metal catalyst of 200nm, thus form Cu metal catalyst layer/amorphous carbon layer/SiO
2/ Si structure.
Step 14: carry out anneal to multilayered structure, reacts to make carbon source layer and forms graphene film;
Here, anneal can adopt the technique such as boiler tube, quick anneal oven, laser annealing, adopts N
2or He protection of inert gas or carry out anneal under high vacuum environment, the annealing temperature of employing can be 400-1200 DEG C.After annealing, carbon source layer is according to the principle of metal catalytic under the effect of metal catalyst, and in metal catalytic with high temperature induction process, carbon atom becomes key to arrange again, changes graphene film into; In the present embodiment, annealing temperature is 800 DEG C, and the time is 30 minutes, and under the effect of Cu metal catalyst, rear agraphitic carbon of having annealed changes into graphene film completely, forms metal catalyst/graphene film/SiO
2/ Si structure.
Step 15: remove metal catalyst, obtain pure graphene film.
Here, wet etching method or electrochemical method can be adopted to remove metal catalyst.In the present embodiment, adopt 1mol/L FeCl3 solution to be removed completely by Cu, to obtain being attached to suprabasil graphene film, last structure is graphene film/SiO
2/ Si structure.Existing technology can be adopted to be stripped down by graphene film, here repeat no more.
Embodiment two
The preparation process of the graphene film of the present embodiment two is identical with the cardinal principle in embodiment one, difference is: in the present embodiment two, do not adopt metal catalyst to form graphene film, but under high vacuum environment, adopt and direct for carbon source layer pyrolytic decomposition is obtained graphene film; Like this, the material of the carbon source layer in the present embodiment two need have high temperature thermal decomposition characteristic, adopts silicon carbide here.Concrete, refer to Fig. 2, the graphene preparation method of the present embodiment two specifically comprises the following steps:
Step 21, provides a substrate; Here, SiO is adopted
2/ Si substrate; This step can the step 11 in See Examples one specifically describe;
Step 22, substrate controls form the uniform carbon source layer of thickness; Here be the silicon carbide layer of 3nm thickness; Thus form silicon carbide layer/SiO
2/ Si structure; Here, can be, but not limited to adopt molecular beam epitaxy; Can also the description of the formation method of carbon source layer in step 12 in See Examples one;
Step 23, under high vacuum environment, direct heating carbon source layer/underlying structure, makes carbon source layer generation thermolysis change into graphene film; Here, to silicon carbide layer/SiO
2/ Si is heated to 900-1200 DEG C, preferably, is 1000 DEG C.Thus form graphene film/SiO
2/ Si structure.
Embodiment three
The preparation process of the graphene film of the present embodiment three and identical in embodiment one, difference is: in the present embodiment, Langmuir-Blodgett (LB) embrane method is adopted to be coated in equably in substrate by liquid carbon source toluene molecule, form toluene molecule film/underlying structure, and then utilize the step S13-S15 identical with embodiment one to form graphene film/underlying structure.
In sum, the preparation method of graphene film of the present invention, first control to form the uniform carbon source layer of thickness in substrate, then carbon source layer is graphene film by thermal response, like this, by accurately controlling homogeneity and the thickness of carbon source layer, can accurately control graphene film homogeneity and thickness; Meanwhile, the preparation method of Graphene of the present invention can obtain high-quality graphene film, and it can be mutually compatible with existing CMOS technology, is suitable for scale operation.
Although the present invention discloses as above with preferred embodiment; right described embodiment is citing for convenience of explanation only; and be not used to limit the present invention; those skilled in the art can do some changes and retouching without departing from the spirit and scope of the present invention, and the protection domain that the present invention advocates should be as the criterion with described in claims.
Claims (10)
1. a preparation method for graphene film, is characterized in that, comprises the following steps:
Step 01 a: substrate is provided;
Step 02: control on the substrate to form the uniform carbon source layer of thickness;
Step 03: heat described carbon source layer, makes described carbon source layer generation chemical reaction and changes graphene film layer into.
2. the preparation method of graphene film according to claim 1, is characterized in that, described step 03 specifically comprises:
Step 31: depositing metal catalyst layer on described carbon source layer, to form the multilayered structure of metal catalyst layer-carbon source layer-substrate;
Step 32: carry out anneal to described multilayered structure, reacts to make described carbon source layer and forms graphene film;
Step 33: remove described metal catalyst, obtains pure graphene film.
3. the preparation method of graphene film according to claim 2, is characterized in that, in described step 03, the material of described metal catalyst layer is Cu, Ni, Co, Fe or Pt.
4. the preparation method of graphene film according to claim 2, is characterized in that, the thickness of described carbon source layer is 5-1000A, and the thickness of described metal catalyst layer is 150-250nm.
5. the preparation method of graphene film according to claim 2; it is characterized in that; in described step 03, the processing condition of described anneal are: adopt N2 or He protection of inert gas or adopt high vacuum environment, the annealing temperature adopted is 400-1200 DEG C.
6. the preparation method of graphene film according to claim 2, is characterized in that, adopts wet etching method or electrochemical method to remove described metal catalyst.
7. the preparation method of graphene film according to claim 1, is characterized in that, in described step 02, the material of described carbon source layer is agraphitic carbon, silicon carbide or organic molecular film.
8. the preparation method of graphene film according to claim 1, is characterized in that, described step 03 specifically comprises: under vacuum conditions, and the thermolysis of carbon source layer is obtained described graphene film.
9. the preparation method of the graphene film according to claim 1-8 any one, is characterized in that, the carbon concentration of described substrate is lower than 0.5ppma.
10. the preparation method of graphene film according to claim 9, is characterized in that, described substrate is silicon, silicon oxide, silicon nitride or silica glass substrate, or surface has the silicon base of silicon oxide film.
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Cited By (10)
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| CN104828808A (en) * | 2015-04-14 | 2015-08-12 | 北京化工大学 | Graphene film preparation method |
| CN104828772A (en) * | 2015-05-08 | 2015-08-12 | 华东师范大学 | Method for growing graphene in silicon micro-channel plate |
| CN105609323A (en) * | 2016-03-17 | 2016-05-25 | 北京理工大学 | Porous nanocarbon slice |
| CN107365959A (en) * | 2017-06-14 | 2017-11-21 | 中国地质大学（北京） | A kind of method of the growth in situ graphene sensor matrix on hard alloy |
| CN108046247A (en) * | 2017-12-25 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | The method for improving carborundum pyrolytic graphite alkene thin layer number uniformity |
| CN108314019A (en) * | 2018-03-19 | 2018-07-24 | 西北大学 | A kind of preparation method of the uniform large-area high-quality graphene film of the number of plies |
| CN109867276A (en) * | 2017-12-01 | 2019-06-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | The method of graphene is directly prepared on substrate |
| CN109950549A (en) * | 2019-04-16 | 2019-06-28 | 中国科学院过程工程研究所 | A kind of lithium ion battery collector and preparation method thereof |
| CN113445030A (en) * | 2020-03-25 | 2021-09-28 | 北京石墨烯研究院 | Method for improving cleanliness of graphene film |
| EP4002007A1 (en) * | 2020-11-11 | 2022-05-25 | Korea Electronics Technology Institute | Multilayer graphene direct growth method and method for manufacturing pellicle for extreme ultraviolet lithography using the same |
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| CN104828808A (en) * | 2015-04-14 | 2015-08-12 | 北京化工大学 | Graphene film preparation method |
| CN104828772A (en) * | 2015-05-08 | 2015-08-12 | 华东师范大学 | Method for growing graphene in silicon micro-channel plate |
| CN105609323A (en) * | 2016-03-17 | 2016-05-25 | 北京理工大学 | Porous nanocarbon slice |
| CN107365959A (en) * | 2017-06-14 | 2017-11-21 | 中国地质大学（北京） | A kind of method of the growth in situ graphene sensor matrix on hard alloy |
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| CN108046247A (en) * | 2017-12-25 | 2018-05-18 | 中国电子科技集团公司第五十五研究所 | The method for improving carborundum pyrolytic graphite alkene thin layer number uniformity |
| CN108314019A (en) * | 2018-03-19 | 2018-07-24 | 西北大学 | A kind of preparation method of the uniform large-area high-quality graphene film of the number of plies |
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| CN109950549A (en) * | 2019-04-16 | 2019-06-28 | 中国科学院过程工程研究所 | A kind of lithium ion battery collector and preparation method thereof |
| CN113445030A (en) * | 2020-03-25 | 2021-09-28 | 北京石墨烯研究院 | Method for improving cleanliness of graphene film |
| EP4002007A1 (en) * | 2020-11-11 | 2022-05-25 | Korea Electronics Technology Institute | Multilayer graphene direct growth method and method for manufacturing pellicle for extreme ultraviolet lithography using the same |
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