CN102747337B - Method for preparing amorphous carbon film with large area and high quality - Google Patents
Method for preparing amorphous carbon film with large area and high quality Download PDFInfo
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- CN102747337B CN102747337B CN201210223312.XA CN201210223312A CN102747337B CN 102747337 B CN102747337 B CN 102747337B CN 201210223312 A CN201210223312 A CN 201210223312A CN 102747337 B CN102747337 B CN 102747337B
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Abstract
The invention relates to a method for preparing an amorphous carbon film with a large area and a high quality. The method comprises a step of introducing reducing gas into a reaction system to completely remove a metal surface oxide layer of a reaction substrate at high temperature; a step of introducing a carbon-source gas into the reaction system, wherein, at high temperature, the carbon-source gas is pyrolyzed and carbon atoms are separated, and the carbon atoms are dissolved on the metal surface layer of the reaction substrate; a step of rapidly cooling the high-temperature reaction furnace to abruptly lower the temperature of the reaction system, so that the carbon atoms is rapidly separated out of the metal surface to form the amorphous carbon film, for the dissolvability of the carbon atoms in metal obviously reduces at low temperature; and a step of performing annealing processing for the amorphous carbon film on the reaction substrate under certain temperature so as to further improve the quality of the amorphous carbon film. The invention utilizes dissolution and precipitation effect of metal on the carbon atoms under different temperatures, has advantages of simple technology and convenient operation, and is suitable for preparing a large area with low cost.
Description
Technical field
The present invention relates to field of nano material preparation, relate to a kind of method of preparing large-area high-quality amorphous carbon film.
Background technology
Amorphous carbon (amorphous carbon, a-C) because the difference of its carbon hybrid state and hydrogen content has multiple isomer, as glass carbon, GLC, DLC, from composition and atomic structure, amorphous carbon can be regarded as diamond and graphite two-phase compound and form, its character is mainly by sp
3: sp
2content determine.
In general; amorphous carbon film is the semi-conductor of low mobility; its band gap variable (1-4eV); there is the fluorescent effect under room temperature, low electron affinity, good wear resistance, low-friction coefficient, the good excellent character such as heat conductance, good infrared breathability, high rigidity and unreactiveness; its wettability can large-scope change, thereby is widely used in the fields such as various supercoat, wear-resistant coating, optical window, magnetic memory device, mechanical workout, biomaterial, feds and solar cell.That prepares at present comparative maturity in the method for amorphous carbon film has ion beam assisted depositing method, radio-frequency magnetron sputter method and a vacuum cathode arc deposited method.
Amorphous carbon-film in process of growth, produces higher internal stress and film does not mate with substrate physical property the stress causing, this not only makes the bonding force of amorphous carbon-film and substrate poor, and limited thickness and the area of film, lack a kind of method of preparing large-area high-quality amorphous carbon film.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of method of preparing large-area high-quality amorphous carbon film is provided.
The inventive method comprises the following steps:
Step 1: pass into the gas with reducing property to reactive system, at high temperature the oxidation on metal surface layer at the bottom of reactive group is removed completely.
Step 2: pass into carbon-source gas to reactive system, wherein cracking isolate carbon atom under carbon-source gas high temperature, is dissolved in the matallic surface layer at the bottom of reactive group when carbon atom high temperature.
Step 3: cooling down high-temperature Reaktionsofen fast, make reactive system temperature decrease, under low temperature, the solvability of carbon atom in metal obviously reduces, and carbon atom is separated out rapidly formation amorphous carbon film in metallic surface.
Step 4: suprabasil reaction amorphous carbon film is carried out to flash annealing processing at a certain temperature, and the quality of amorphous carbon film further improves.
In such scheme, the gas of reducing property can be the gas mixture of hydrogen, hydrogen and argon gas or the gas mixture of hydrogen and nitrogen, and wherein carbon-source gas can be methane, acetylene or propylene, can be nickel foil, goldleaf or platinum foil at the bottom of reactive group.
Beneficial effect of the present invention: the present invention utilizes metal dissolving to carbon atom and separate out effect under differing temps, and technique is simple, easy to operate, is applicable to the preparation of big area low cost.
Brief description of the drawings
Fig. 1 is the reactive system schematic diagram of preparing amorphous carbon film.
Fig. 2 is the amorphous carbon film Raman image of not doing anneal and annealed processing.
Fig. 3 is the SEM image of amorphous carbon film under 20000 magnifications.
Fig. 4 is the SEM image of amorphous carbon film under 10000 magnifications.
Fig. 5 is the SEM image of amorphous carbon film under 5000 magnifications.
Fig. 6 is the SEM image of amorphous carbon film under 2000 magnifications.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
The present invention mainly utilizes the carburizing of metal under differing temps to analyse carbon mechanism and prepares large-area high-quality amorphous carbon film, is applicable to large-scale production, especially demonstrates very strong advantage at the aspect such as preparation cost, thin film stability.
The step of the inventive method
Step 1: pass into the gas with reducing property to reactive system, at high temperature the oxidation on metal surface layer at the bottom of reactive group is removed completely.
Step 2: pass into carbon-source gas to reactive system, wherein cracking isolate carbon atom under carbon-source gas high temperature, is dissolved in the matallic surface layer at the bottom of reactive group when carbon atom high temperature.
Step 3: cooling down high-temperature Reaktionsofen fast, make reactive system temperature decrease, under low temperature, the solvability of carbon atom in metal obviously reduces, and carbon atom is separated out rapidly formation amorphous carbon film in metallic surface.
Step 4: suprabasil reaction amorphous carbon film is carried out to flash annealing processing at a certain temperature, and the quality of amorphous carbon film further improves.
Below provide specific embodiment:
Embodiment 1: utilize methane to make carbon source, nickel foil is done to prepare amorphous carbon film at the bottom of reactive group
Prepare the reactive system schematic diagram of amorphous carbon film as shown in Figure 1: be first that 4 centimetres of 4 cm x, thickness are that the nickel foil of 50 microns is put into high temperature reaction stove at the bottom of reactive group using area, utilize vacuum pump that vacuum tightness is adjusted to below 5mTorr; Then high temperature reaction stove is warming up to 950 degrees Celsius, passes into 50sccm hydrogen as reducing gas, first heat 50 minutes; Then pass into 20sccm methane as carbon source 950 degrees Celsius of lower cracking and be dissolved in nickel foil, high temperature continues to maintain 30 minutes; Secondly Reaktionsofen temperature is down to normal temperature in 3 minutes, closes source of the gas and open Reaktionsofen; Finally the nickel foil of taking-up is placed on and in the annealing furnace of 500 degrees Celsius, carries out flash annealing and process 1 hour, whole amorphous carbon film preparation process finishes.
Accompanying drawing 2 is amorphous carbon film Raman image of not doing anneal and annealed processing, finds both to exist 1603cm
-1(G peak) and 1374cm
-1(D peak) two characteristic peaks, 2D peak is wider and smooth, and intensity is starkly lower than G peak, illustrates that amorphous carbon layer content is very outstanding; After annealed processing, characteristic peak is more obvious, illustrates that flash annealing further improves the quality of amorphous carbon film.Accompanying drawing 3 is the SEM image of amorphous carbon film under 20000 magnifications, accompanying drawing 4 is the SEM image of amorphous carbon film under 10000 magnifications, accompanying drawing 5 is the SEM image of amorphous carbon film under 5000 magnifications, accompanying drawing 6 is the SEM image of amorphous carbon film under 2000 magnifications, the amorphous carbon film continuity excellence that as seen from the figure prepared by the present invention, difference in thickness is less.
Embodiment 2: utilize acetylene to make carbon source, goldleaf is done to prepare amorphous carbon film at the bottom of reactive group
First be that 4 centimetres of 4 cm x, thickness are that the goldleaf of 25 microns is put into high temperature reaction stove at the bottom of reactive group using area, utilize vacuum pump that vacuum tightness is adjusted to below 5mTorr; Then high temperature reaction stove is warming up to 850 degrees Celsius, passes into 75sccm hydrogen as reducing gas, first heat 60 minutes; Then pass into 15sccm acetylene as carbon source 850 degrees Celsius of lower cracking and be dissolved in goldleaf, high temperature continues to maintain 40 minutes; Secondly Reaktionsofen temperature is down to normal temperature in 3 minutes, closes source of the gas and open Reaktionsofen; Finally the goldleaf of taking-up is placed on and in the annealing furnace of 450 degrees Celsius, carries out flash annealing and process 1 hour, whole amorphous carbon film preparation process finishes.
Embodiment 3: utilize propylene to make carbon source, platinum foil is done to prepare amorphous carbon film at the bottom of reactive group
First be that 4 centimetres of 4 cm x, thickness are that the platinum foil of 100 microns is put into high temperature reaction stove at the bottom of reactive group using area, utilize vacuum pump that vacuum tightness is adjusted to below 5mTorr; Then high temperature reaction stove is warming up to 1600 degrees Celsius, passes into 100sccm hydrogen as reducing gas, first heat 60 minutes; Then pass into 45sccm acetylene as carbon source 1600 degrees Celsius of lower cracking and be dissolved in platinum foil, high temperature continues to maintain 80 minutes; Secondly Reaktionsofen temperature is down to normal temperature in 5 minutes, closes source of the gas and open Reaktionsofen; Finally the platinum foil of taking-up is placed on and in the annealing furnace of 800 degrees Celsius, carries out flash annealing and process 1 hour, whole amorphous carbon film preparation process finishes.
Claims (1)
1. prepare a method for large-area high-quality amorphous carbon film, it is characterized in that the method comprises the following steps:
Step 1: pass into the gas with reducing property to reactive system, at high temperature the oxidation on metal surface layer at the bottom of reactive group is removed completely;
Step 2: pass into carbon-source gas to reactive system, wherein cracking isolate carbon atom under carbon-source gas high temperature, is dissolved in the matallic surface layer at the bottom of reactive group when carbon atom high temperature;
Step 3: cooling down high-temperature Reaktionsofen fast, make reactive system temperature decrease to normal temperature, under low temperature, the solvability of carbon atom in metal obviously reduces, and carbon atom is separated out rapidly formation amorphous carbon film in metallic surface;
Step 4: suprabasil reaction amorphous carbon film is carried out to flash annealing processing under design temperature, and the quality of amorphous carbon film further improves;
The gas of the reducing property described in step 1 can be the gas mixture of gas mixture, hydrogen and the nitrogen of hydrogen, hydrogen and argon gas;
At the bottom of reactive group described in step 1, can be nickel foil, goldleaf or platinum foil;
Carbon-source gas described in step 2 can be methane, acetylene or propylene.
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| CN103643217B (en) * | 2013-11-28 | 2016-08-17 | 华中科技大学 | A kind of preparation method of self-supporting class graphite porous amorphous carbon film |
| CN109136827A (en) * | 2018-08-20 | 2019-01-04 | 北京科技大学 | The method for improving deepsea mining system components anticorrosion antiwear from growth carbonaceous membrane |
| CN115268555B (en) * | 2022-07-27 | 2024-05-28 | 成都振芯科技股份有限公司 | Second-order temperature compensation band gap reference voltage circuit and differential circuit |
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| US5474816A (en) * | 1993-04-16 | 1995-12-12 | The Regents Of The University Of California | Fabrication of amorphous diamond films |
| CN101831633A (en) * | 2010-04-21 | 2010-09-15 | 清华大学 | Method for preparing composite film of graphene and amorphous carbon |
| CN102051589B (en) * | 2010-11-25 | 2013-01-02 | 南京理工大学 | Method for preparing amorphous silicon carbide film and epitaxial film at low temperature |
| CN102220566A (en) * | 2011-06-09 | 2011-10-19 | 无锡第六元素高科技发展有限公司 | Method for preparing single-layer or multi-layer graphene through chemical vapor deposition |
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