CN102747337A - 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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- CN102747337A CN102747337A CN201210223312XA CN201210223312A CN102747337A CN 102747337 A CN102747337 A CN 102747337A CN 201210223312X A CN201210223312X A CN 201210223312XA CN 201210223312 A CN201210223312 A CN 201210223312A CN 102747337 A CN102747337 A CN 102747337A
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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 for preparing the large-area high-quality amorphous carbon film.
Background technology
Amorphous carbon (amorphous carbon; A-C) because of its carbon hybrid state and hydrogen content different multiple isomer is arranged; Like glass carbon, GLC, DLC; From composition and atomic structure, it is mutually compound and constitute that amorphous carbon can be regarded as diamond and graphite two, and its character mainly is by sp
3: sp
2Content determine.
In general; Amorphous carbon film is the semi-conductor of low mobility; Its band gap variable (1-4eV); Have excellent character such as fluorescent effect under the room temperature, low electron affinity, good wear resistance, low-friction coefficient, good heat conductance, good infrared breathability, high firmness and unreactiveness; Its wettability can large-scope change, thereby is widely used in fields such as various supercoat, wear-resistant coating, optical window, magnetic memory device, mechanical workout, biomaterial, feds and solar cell.What prepare 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 produces the stress that higher internal stress and film and substrate rerum natura do not match and cause in process of growth; This not only makes the bonding force of amorphous carbon-film and substrate poor; And limited the thickness and the area of film, lack a kind of method for preparing the large-area high-quality amorphous carbon film.
Summary of the invention
The present invention is directed to the deficiency of prior art, a kind of method for preparing the large-area high-quality amorphous carbon film is provided.
The inventive method may further comprise the steps:
Step 1: feed gas to reactive system, at high temperature the oxidation on metal surface layer at the bottom of the reactive group is removed fully with reducing property.
Step 2: feed carbon-source gas to reactive system, wherein cracking and isolate carbon atom under the carbon-source gas high temperature is dissolved in the matallic surface layer at the bottom of the reactive group during carbon atom high temperature.
Step 3: quick cooling down high-temperature Reaktionsofen, make the reactive system temperature decrease, the solvability of carbon atom in metal obviously reduces under the low temperature, and carbon atom is separated out the formation amorphous carbon film rapidly in the metallic surface.
Step 4: will react suprabasil amorphous carbon film and carry out the flash annealing processing at a certain temperature, the quality of amorphous carbon film further improves.
In the 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 the reactive group.
Beneficial effect of the present invention: the present invention utilize metal under differing temps to the dissolving of carbon atom with separate out effect, technology is simple, and is easy to operate, is fit to the low-cost preparation of big area.
Description of drawings
Fig. 1 is the reactive system synoptic diagram of preparation amorphous carbon film.
Fig. 2 is not for making the amorphous carbon film raman image of 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 present invention is described further.
The present invention mainly utilizes the carburizing of metal under differing temps to analyse carbon mechanism and prepares the large-area high-quality amorphous carbon film, is applicable to large-scale production, especially demonstrates very strong advantage at aspects such as preparation cost, thin film stabilities.
The step of the inventive method
Step 1: feed gas to reactive system, at high temperature the oxidation on metal surface layer at the bottom of the reactive group is removed fully with reducing property.
Step 2: feed carbon-source gas to reactive system, wherein cracking and isolate carbon atom under the carbon-source gas high temperature is dissolved in the matallic surface layer at the bottom of the reactive group during carbon atom high temperature.
Step 3: quick cooling down high-temperature Reaktionsofen, make the reactive system temperature decrease, the solvability of carbon atom in metal obviously reduces under the low temperature, and carbon atom is separated out the formation amorphous carbon film rapidly in the metallic surface.
Step 4: will react suprabasil amorphous carbon film and carry out the flash annealing processing at a certain temperature, the quality of amorphous carbon film further improves.
Below provide specific embodiment:
Embodiment 1: utilize methane to make carbon source, nickel foil do reaction substrate preparation amorphous carbon film
The reactive system synoptic diagram of preparation amorphous carbon film is shown in accompanying drawing 1: be that 4 centimetres of 4 cm x, thickness are that 50 microns nickel foil is put into high temperature reaction stove at the bottom of as reactive group with area at first, utilize vacuum pump that vacuum tightness is adjusted to below the 5mTorr; Then high temperature reaction stove is warming up to 950 degrees centigrade, feeds 50sccm hydrogen as reducing gas, first heat 50 minutes; Feed then 20sccm methane as carbon source 950 degrees centigrade of following cracking and be dissolved in the nickel foil, high temperature continued to keep 30 minutes; Secondly the Reaktionsofen temperature is reduced to normal temperature in 3 minutes, close source of the gas and open Reaktionsofen; At last the nickel foil that takes out is placed on and carries out flash annealing in 500 degrees centigrade the lehre and handled 1 hour, whole amorphous carbon film prepares end of processing.
Accompanying drawing 2 is amorphous carbon film raman image of not doing anneal and annealed processing, finds that there is 1603cm in the both
-1(G peak) and 1374cm
-1(D peak) two characteristic peaks, 2D peak broad and smooth, intensity is starkly lower than the G peak, explains that amorphous carbon layer content is very outstanding; After the annealed processing, characteristic peak is more obvious, explains that flash annealing makes the quality of amorphous carbon film further improve.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, but excellent by the amorphous carbon film continuity of figure knowledge capital invention preparation, difference in thickness is less.
Embodiment 2: utilize acetylene to make carbon source, goldleaf do reaction substrate preparation amorphous carbon film
Be that 4 centimetres of 4 cm x, thickness are that 25 microns goldleaf is put into high temperature reaction stove at the bottom of as reactive group at first, utilize vacuum pump that vacuum tightness is adjusted to below the 5mTorr area; Then high temperature reaction stove is warming up to 850 degrees centigrade, feeds 75sccm hydrogen as reducing gas, first heat 60 minutes; Feed then 15sccm acetylene as carbon source 850 degrees centigrade of following cracking and be dissolved in the goldleaf, high temperature continued to keep 40 minutes; Secondly the Reaktionsofen temperature is reduced to normal temperature in 3 minutes, close source of the gas and open Reaktionsofen; At last the goldleaf that takes out is placed on and carries out flash annealing in 450 degrees centigrade the lehre and handled 1 hour, whole amorphous carbon film prepares end of processing.
Embodiment 3: utilize propylene to make carbon source, platinum foil do reaction substrate preparation amorphous carbon film
Be that 4 centimetres of 4 cm x, thickness are that 100 microns platinum foil is put into high temperature reaction stove at the bottom of as reactive group at first, utilize vacuum pump that vacuum tightness is adjusted to below the 5mTorr area; Then high temperature reaction stove is warming up to 1600 degrees centigrade, feeds 100sccm hydrogen as reducing gas, first heat 60 minutes; Feed then 45sccm acetylene as carbon source 1600 degrees centigrade of following cracking and be dissolved in the platinum foil, high temperature continued to keep 80 minutes; Secondly the Reaktionsofen temperature is reduced to normal temperature in 5 minutes, close source of the gas and open Reaktionsofen; At last the platinum foil that takes out is placed on and carries out flash annealing in 800 degrees centigrade the lehre and handled 1 hour, whole amorphous carbon film prepares end of processing.
Claims (4)
1. method for preparing the large-area high-quality amorphous carbon film is characterized in that this method may further comprise the steps:
Step 1: feed gas to reactive system, at high temperature the oxidation on metal surface layer at the bottom of the reactive group is removed fully with reducing property;
Step 2: feed carbon-source gas to reactive system, wherein cracking and isolate carbon atom under the carbon-source gas high temperature is dissolved in the matallic surface layer at the bottom of the reactive group during carbon atom high temperature;
Step 3: quick cooling down high-temperature Reaktionsofen, make the reactive system temperature decrease to normal temperature, the solvability of carbon atom in metal obviously reduces under the low temperature, and carbon atom is separated out the formation amorphous carbon film rapidly in the metallic surface;
Step 4: will react suprabasil amorphous carbon film and under design temperature, carry out the flash annealing processing, the quality of amorphous carbon film further improves.
2. preparation large-area high-quality amorphous carbon film preparation method according to claim 1 is characterized in that: the gas of the described reducing property of step 1 can be the gas mixture of gas mixture, hydrogen and the nitrogen of hydrogen, hydrogen and argon gas.
3. preparation large-area high-quality amorphous carbon film preparation method according to claim 1 is characterized in that: can be nickel foil, goldleaf or platinum foil at the bottom of the described reactive group of step 1.
4. preparation large-area high-quality amorphous carbon film preparation method according to claim 1 is characterized in that: the described carbon-source gas of step 2 can be methane, acetylene or propylene.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643217A (en) * | 2013-11-28 | 2014-03-19 | 华中科技大学 | Method for preparing self-supporting graphite porous amorphous carbon thin 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 |
| CN115268555A (en) * | 2022-07-27 | 2022-11-01 | 成都振芯科技股份有限公司 | Second-order temperature compensation band gap reference voltage circuit and differential circuit |
Citations (4)
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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 |
| CN102051589A (en) * | 2010-11-25 | 2011-05-11 | 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 |
-
2012
- 2012-06-27 CN CN201210223312.XA patent/CN102747337B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102051589A (en) * | 2010-11-25 | 2011-05-11 | 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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103643217A (en) * | 2013-11-28 | 2014-03-19 | 华中科技大学 | Method for preparing self-supporting graphite porous amorphous carbon thin film |
| 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 |
| CN115268555A (en) * | 2022-07-27 | 2022-11-01 | 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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| CN102747337B (en) | 2014-06-11 |
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