CN106148910B - A kind of preparation method of nitrogen-doped graphene film - Google Patents
A kind of preparation method of nitrogen-doped graphene film Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of nitrogen-doped graphene film, the method includes the steps: a substrate is provided first, the substrate is placed in dual temperature sound zone system, and places carbon nitrogen source in the dual temperature sound zone system, is heated to deposit the precursor layer to form nitrogen-doped graphene in the substrate surface；Gaseous carbon sources are then passed to, Carbon deposition reacts to form nitrogen-doped graphene film under hot conditions.The present invention introduces micro-molecular gas carbon source on the basis of solid-liquid carbon nitrogen source grows nitrogen-doped graphene method to improve precursor layer, so that defect is more in existing method, electrical properties are poor, the uncontrollable nitrogen-doped graphene film quality of doping concentration is improved, to obtain, electric property is outstanding, the controllable N-type graphene film of the less N doping of defect.
Description
Technical field
The present invention relates to materials to prepare manufacture field, more particularly to a kind of preparation method of nitrogen-doped graphene film.
Background technique
Graphene is the two-dimensional material made of a kind of single layer of carbon atom is arranged with hexagonal structure with honeycomb structure,
Since first passage micromechanics removing in 2004 is produced, because of its unique optics, electricity, calorifics and mechanical property, obtain
Extensive concern from researcher all over the world.These excellent performances make graphene in touch screen, field effect transistor
The numerous areas such as pipe, fast-response probe, solar battery, heavy-duty battery and super capacitor have potential application.However, intrinsic
The characteristics of zero band gap of graphene, also gives it to bring difficulty in the application of field of electronic devices, such as leakage current is big, on-off ratio is low,
Then how to obtain N-shaped and p-type graphene becomes its key in electrical application.Scientist develops more in response to this problem
Kind method and technology, wherein the doping of nitrogen is its important means changed to n-type semiconductor.
Graphene nitrogen-doping method mainly has chemical vapor deposition (CVD) method, hydrothermal synthesis method, gas ions sputtering technology at present
Etc., these method combined coefficienies and quality are generally lower, it would be highly desirable to improve.Wherein the CVD method of metal catalytic is in large area deposition
There are advantages for graphene film, therefore this method is also used to growth nitrogen-doped graphene film.Such as Liu Yun boundary, study group passes through
Use small gas molecule methane gas as carbon source, ammonia is as nitrogen source, in the copper film conduct of silicon substrate surface deposition 25nm thickness
Catalyst is kept for 10 minutes at a high temperature of 800 DEG C, a small number of several layers of nitrogen-doped graphenes has been made；In addition, solid-liquid carbon
Nitrogen source such as pyridine, melamine etc. are also used to growth nitrogen-doped graphene film, specially use carrier gas by solid-liquid carbon nitrogen source
Steam is brought into the metallic catalyst substrate under the conditions of being placed in certain temperature, and it is thin to obtain nitrogen-doped graphene in substrate surface deposition
Film.Although the graphene film simple process of above-mentioned CVD method preparation, still there are some problems, such as graphene defect
More, electrical properties are poor, and nitrogen doped concentration is not easy to control, and the film number of plies is difficult to control.Therefore seeking one kind can reduce stone
Defect in black alkene film, improve electrical properties high quality large area nitrogen-doped graphene film preparation method for present stone
Application of the black alkene in fields such as opto-electronic device, solar cells is of great significance.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of nitrogen-doped graphene films
Preparation method, for solving in the prior art, nitrogen-doped graphene film doping concentration is not easy to control, lattice defect is more, electrical property
The problems such as matter is poor.
In order to achieve the above objects and other related objects, the present invention provides a kind of preparation side of nitrogen-doped graphene film
Method, the preparation method include at least:
1) substrate is provided, the substrate is placed in dual temperature sound zone system, and place carbon nitrogen source in the dual temperature sound zone system,
Heating is to deposit the precursor layer to form nitrogen-doped graphene in the substrate surface；
2) gaseous carbon sources are passed through, Carbon deposition reacts to form nitrogen-doped graphene film under hot conditions.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention in the step 1), is put
Before setting carbon nitrogen source, further include the steps that making annealing treatment substrate under protective atmosphere.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the step 1) is middle to be used
Chemical vapor deposition process forms the precursor layer of nitrogen-doped graphene, comprising steps of
The carbon nitrogen source and substrate 1-1) are placed on the different zones of dual temperature sound zone system, and heated respectively, is passed through simultaneously
Carbon nitrogen source steam is introduced substrate region by carrier gas, is deposited；
1-2) stop heating, be cooled to room temperature, takes out the substrate that surface is deposited with nitrogen-doped graphene precursor layer.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the step 1-1) in carbon
The heating temperature range of nitrogen source is 50~200 DEG C.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the step 1-1) in base
The heating temperature range at bottom is 250~600 DEG C.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the step 1-1) in carry
Gas is the mixed gas of hydrogen or hydrogen and argon gas.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the middle deposition of the step 1)
Time is 10min~80min.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, carbon nitrogen in the step 1)
Source is nitrogen heteroaromatic compounds and its derivative.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the carbon nitrogen source are solid
Or liquid.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the base material are
One of Au, Co, Pt, Pd, Ir, Ru, Ni, Cu or a variety of alloy materials are coated with the above metal material or alloy material
Metal foil, silicon wafer, glass.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, select Au, Co, Pt, Pd,
When one of Ir, Ru, Ni, Cu or a variety of alloy materials are substrate, it is also necessary to handle substrate, processing mode includes
Chemical polishing is carried out using acetic acid, nitric acid or hydrochloric acid or carries out electrochemical polish under the conditions of phosphoric acid.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, the step 2) are at least wrapped
Include step:
2-1) substrate for being deposited with nitrogen-doped graphene precursor layer is put into high-temperature systems；
It 2-2) heats the high-temperature systems and is passed through hydrogen and micro-molecular gas carbon source, make nitrogen-doped graphene presoma knot
Crystalline substance go forward side by side single step reaction deposition；
2-3) stop heating, be cooled to room temperature, takes out the substrate for being deposited with nitrogen-doped graphene film.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, carbon source in the step 2)
For low carbon chain hydrocarbon.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, when the step 2) deposits
Between be 0.5~50min.
A kind of preferred scheme of preparation method as nitrogen-doped graphene film of the present invention, step 2) the heating temperature
Degree is 600 DEG C~1100 DEG C.
As described above, the preparation method of nitrogen-doped graphene film of the invention, have the advantages that the present invention with
Nitrogen-doped graphene film is grown to research object, improves for existing method, grows in existing solid-liquid carbon nitrogen source
The method that micro-molecular gas carbon source improves precursor layer is introduced on the basis of nitrogen-doped graphene method, so that in existing method
Defect is more, and the poor nitrogen-doped graphene film quality of electrical properties is improved, so that it is outstanding to obtain electric property, defect
Less nitrogen-doped graphene film.More importantly this method can be realized by the technology controlling and process of carbon nitrogen source deposition step
The N doping content of film forming is controllable.Meanwhile this method is completely suitable for the growth of large area nitrogen-doped graphene film, obtains
Uniformity of film is good, electric property is excellent.
Detailed description of the invention
Fig. 1 is the preparation method process flow chart of nitrogen-doped graphene film of the present invention.
Fig. 2 is dual temperature sound zone system schematic diagram of the present invention, wherein 1 is carbon nitrogen source region in reaction, and 2 be base in reaction
Bottom region.
Fig. 3 is the Raman spectrogram of nitrogen-doped graphene film prepared by the present invention.
Fig. 4 is the stereoscan photograph of nitrogen-doped graphene film prepared by the present invention.
Fig. 5 is the x-ray photoelectron spectroscopy of nitrogen-doped graphene film prepared by the present invention.
Fig. 6 is the peak the C comparison diagram of the x-ray photoelectron spectroscopy of nitrogen-doped graphene prepared by the present invention and pure graphene.
Fig. 7 is the peak N and its swarming figure of the x-ray photoelectron spectroscopy of nitrogen-doped graphene prepared by the present invention.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Please refer to attached drawing.It should be noted that only the invention is illustrated in a schematic way for diagram provided in the present embodiment
Basic conception, only shown in schema then with related component in the present invention rather than component count, shape when according to actual implementation
Shape and size are drawn, when actual implementation kenel, quantity and the ratio of each component can arbitrarily change for one kind, and its component cloth
Office's kenel may also be increasingly complex.
As shown in Figure 1, the present invention provides a kind of preparation method of nitrogen-doped graphene film, the nitrogen-doped graphene is thin
The preparation method of film at least includes the following steps:
S1 provides a substrate, and the substrate is placed in dual temperature sound zone system, and carbon nitrogen is placed in the dual temperature sound zone system
Source is heated to deposit the precursor layer to form nitrogen-doped graphene in the substrate surface；
S2 is passed through gaseous carbon sources, and Carbon deposition reacts to form nitrogen-doped graphene film under hot conditions.
Detailed introduction is done below with reference to preparation method of the specific attached drawing to nitrogen-doped graphene film of the invention.
Step S1 is first carried out, a substrate is provided, the substrate is placed in dual temperature sound zone system, and in the dual temperature sound zone system
Middle placement carbon nitrogen source is heated to deposit the precursor layer to form nitrogen-doped graphene in the substrate surface.
The base material is one of Au, Co, Pt, Pd, Ir, Ru, Ni, Cu or a variety of alloy materials or is coated with
The metal foil of the above metal material or alloy material, silicon wafer, glass etc..In the present embodiment, using copper foil as substrate.
As an example, when one of selection Au, Co, Pt, Pd, Ir, Ru, Ni, Cu or a variety of alloy materials are substrate,
It also needs to handle substrate, processing mode includes carrying out chemical polishing using acetic acid, nitric acid or hydrochloric acid etc. or in phosphoric acid item
Electrochemical polish is carried out under part.In the present embodiment, copper-based bottom is pre-processed using acetic acid.
To substrate the specific process is as follows: copper foil is put into beaker, successively with deionized water, acetone, EtOH Sonicate
Cleaning；Copper foil after having cleaned is put into acetic acid and is impregnated, is cleaned after taking-up with deionized water, N2Drying.
The structure of the two temperature system is respectively used to put as shown in Fig. 2, there are two different regions for setting in the system
Substrate and carbon nitrogen source are set, and substrate and carbon nitrogen source can be respectively heated.Wherein, it is placed close to the region 1 of carrier gas inlet
Substrate is placed in carbon nitrogen source, the region 2 far from carrier gas inlet, and two regions are utilized respectively resistance wire and are heated.
The carbon nitrogen source is nitrogen heteroaromatic compounds and its derivative.For example, it may be pyridine or azepine naphthalene compound.
Further, for example, it may be pyridine, penta chloropyridine, quinoline, melamine or 2, one kind of 3- benzodiazine etc..This implementation
In example, carbon nitrogen source can temporarily be selected as penta chloropyridine.The form of the carbon nitrogen source can be solid or liquid.
It, can be under the conditions of protective atmosphere, such as argon gas by substrate before carrying out first time chemical vapor deposition process
It is first made annealing treatment, the temperature of annealing can be within the scope of 800~1100 DEG C.
First time chemical vapor deposition, detailed process are carried out using dual temperature sound zone system later are as follows:
The carbon nitrogen source and substrate are placed on the different zones of dual temperature sound zone system, and heated respectively by the first step, are led to simultaneously
It crosses carrier gas and carbon nitrogen source steam is introduced into substrate region, deposited；
Second step stops heating, is cooled to room temperature, and takes out the substrate that surface is deposited with nitrogen-doped graphene precursor layer.
For example, copper foil is put into the position 2 in dual temperature area CVD system, then weighs 0.005~1g penta chloropyridine and be placed in
Position 1 in quartz ampoule, vacuumizes；Hydrogen is passed through as carrier gas, flow is chosen for 30~100sccm, while by liter at position 2
Temperature is to 250~600 DEG C；Etc. temperature stablize after will be warming up to 50~200 DEG C at position 1, respectively keep the temperature 10~80min；After cooling
Take out the copper foil for being deposited with nitrogen-doped graphene presoma.
In the present embodiment, the carrier gas being passed through is hydrogen.Certainly, in other embodiments, the carrier gas is also possible to hydrogen
It is unlimited herein with the mixed gas of argon gas or other suitable gases.
In the step, by the catalytic action of metallic substrates, mixed using chemical vapor deposition high-temperature service successful growth nitrogen
The precursor layer of miscellaneous graphene.
Then step S2 is executed, is passed through gaseous carbon sources, Carbon deposition reacts to form nitrogen-doped graphene film under hot conditions.
Detailed process are as follows: firstly, the substrate for being deposited with nitrogen-doped graphene precursor layer is put into high-temperature systems；Then plus
Heat high-temperature systems, and be passed through micro-molecular gas carbon source and hydrogen is deposited, make the crystallization of nitrogen-doped graphene presoma with
Small molecule carbon source fills gap；Finally, stopping heating, it is cooled to room temperature, takes out the substrate for being deposited with nitrogen-doped graphene film.
For example, the copper foil for being deposited with nitrogen-doped graphene precursor layer is placed in CVD system, vacuumize；It is passed through H2As
Carrier gas, flow are chosen for 30~100sccm, while being warming up to 600~1100 DEG C；Etc. temperature reach setting value after be passed through carbon source
CH4, flow is chosen for 0.1~5sccm, 0.5~50min of time；The copper foil for covering with nitrogen-doped graphene film is taken out after cooling.
The carbon source is low carbon chain hydrocarbon.For example, methane, ethane, ethylene acetylene etc..In the present embodiment, institute
Stating carbon source is methane.
It, can also be with it should be noted that the implementation of step S2 can occur in dual temperature area high-temperature systems in step sl
Select single temperature zone high-temperature systems optionally to complete.If selecting single temperature zone system, need that nitrogen-doped graphene precursor layer will be deposited with
Substrate taken out from the dual temperature sound zone system in step S1, be placed in single temperature zone system, then be passed through gaseous carbon sources.
High temperature deposition mode is used in this step, high-temperature temperature is preferably 800 DEG C or more, in high-temperature deposition process, nitrogen
Doped graphene precursor layer crystallizes, and small molecule carbon source is filled in precursor layer, plays the role of repairing, and it is close to reduce defect
Degree.Next nitrogen-doped graphene film is transferred to SiO2/ Si on piece is characterized.If Fig. 3 is that nitrogen prepared by the present invention is mixed
The Raman spectrum of miscellaneous graphene film, it can be observed that the peak characteristic peak D, G, 2D of graphene, illustrates finally to prepare and obtain from Fig. 3
What is obtained is to have the graphene film of single layer structure, and defect is less.Fig. 4 is the electronics after film is transferred in silicon chip substrate
Microscope photo, as can be seen from Figure 4 the uniformity with integrality of film are good, and defect is few.The X of nitrogen-doped graphene film is penetrated
Photoelectron spectra is as shown in Fig. 5, Fig. 6 and Fig. 7.Fig. 5 is score, it can be seen that the apparent peak C, N；Fig. 6 indicates N doping graphite
The peak the C comparison diagram of alkene and pure graphene, there are the obvious peaks C-N for nitrogen-doped graphene；Fig. 7 indicates nitrogen-doped graphene X-ray light
The peak the N swarming figure of electron spectrum, N element is in doped graphene in the form of three kinds of nitrogen of pyrrolesization nitrogen, pyridine nitrogen and graphitization
In the presence of.It is can be achieved by technological parameter (amount, reaction temperature and the time of such as carbon nitrogen source) control of carbon nitrogen source deposition step
The N doping content of film is controllable, passes through nitrogen in the available prepared nitrogen-doped graphene film of the calculating of XPS spectrum diagram data
Content is 1~10%.Hall effect test shows it with N-type semiconductor characteristic.
In conclusion the present invention provides a kind of preparation method of nitrogen-doped graphene film, and the method includes the steps: it is first
One substrate is first provided, the substrate is placed in dual temperature sound zone system, and place carbon nitrogen source in the dual temperature sound zone system, heating with
The substrate surface deposits the precursor layer to form nitrogen-doped graphene；Then carbon source, high temperature are passed through into the dual temperature sound zone system
Under the conditions of Carbon deposition react to form nitrogen-doped graphene film.The present invention grows nitrogen-doped graphene method in solid-liquid carbon nitrogen source
On the basis of introduce micro-molecular gas carbon source and improve precursor layer so that defect is more in existing method, electrical properties compared with
The nitrogen-doped graphene film quality of difference is improved, and acquisition electric property is outstanding, the controllable N-type stone of the less N doping of defect
Black alkene film.
So the present invention effectively overcomes various shortcoming in the prior art and has high industrial utilization value.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (13)
1. a kind of preparation method of nitrogen-doped graphene film, which is characterized in that the preparation method includes at least:
1) substrate is provided, the substrate is placed in dual temperature sound zone system, and place carbon nitrogen source in the dual temperature sound zone system, is heated
To deposit the precursor layer to form nitrogen-doped graphene in the substrate surface, specifically include:
The carbon nitrogen source and substrate 1-1) are placed on the different zones of dual temperature sound zone system, and heated respectively, while passing through carrier gas
Carbon nitrogen source steam is introduced into substrate region, is deposited；
1-2) stop heating, be cooled to room temperature, takes out the substrate that surface is deposited with nitrogen-doped graphene precursor layer；
2) gaseous carbon sources are passed through, Carbon deposition reacts to form nitrogen-doped graphene film under hot conditions, it specifically includes:
2-1) substrate for being deposited with nitrogen-doped graphene precursor layer is put into high-temperature systems；
The high-temperature systems 2-2) are heated, and are passed through micro-molecular gas carbon source and hydrogen, crystallize nitrogen-doped graphene presoma
Single step reaction of going forward side by side deposition；
2-3) stop heating, be cooled to room temperature, takes out the substrate for being deposited with nitrogen-doped graphene film.
2. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: in the step 1),
Before placing carbon nitrogen source, further include the steps that making annealing treatment substrate under protective atmosphere.
3. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: the step 1-1) in
The heating temperature range of carbon nitrogen source is 50~200 DEG C.
4. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: the step 1-1) in
The heating temperature range of substrate is 250~600 DEG C.
5. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: the step 1-1) in
Carrier gas is the mixed gas of hydrogen or hydrogen and argon gas.
6. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: sink in the step 1)
The product time is 10min~80min.
7. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: carbon in the step 1)
Nitrogen source is nitrogen heteroaromatic compounds and its derivative.
8. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: the carbon nitrogen source is solid
Body or liquid.
9. the preparation method of nitrogen-doped graphene film according to claim 1, it is characterised in that: the base material is
One of Au, Co, Pt, Pd, Ir, Ru, Ni, Cu or a variety of alloy materials are coated with the above metal material or alloy material
Metal foil, silicon wafer, glass.
10. the preparation method of nitrogen-doped graphene film according to claim 9, it is characterised in that: select Au, Co, Pt,
When one of Pd, Ir, Ru, Ni, Cu or a variety of alloy materials are substrate, it is also necessary to handle substrate, processing mode
Including carrying out chemical polishing using acetic acid, nitric acid or hydrochloric acid or carrying out electrochemical polish under the conditions of phosphoric acid.
11. the preparation method of graphene film according to claim 1, it is characterised in that: carbon source is in the step 2)
Low carbon chain hydrocarbon.
12. the preparation method of graphene film according to claim 1, it is characterised in that: the step 2) sedimentation time
For 0.5~50min.
13. the preparation method of graphene film according to claim 1, it is characterised in that: the step 2) heating temperature
It is 600 DEG C~1100 DEG C.
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| WO2013160719A1 (en) * | 2012-04-26 | 2013-10-31 | Indian Institute Of Technology Madras | Metal-alloy graphene nanocomposites and methods for their preparation and use |
| CN109019571B (en) * | 2017-06-12 | 2022-01-21 | 中国科学院上海高等研究院 | Preparation method of nitrogen-doped graphene with controllable layer number |
| CN109534328B (en) * | 2017-09-22 | 2022-06-24 | 天津大学 | Two-dimensional nitrogen-doped graphene and preparation method thereof |
| CN108609614A (en) * | 2018-05-28 | 2018-10-02 | 天津大学 | A kind of preparation method of blue, purple fluorescent single nitrogen-doped graphene |
| CN110155991A (en) * | 2019-04-24 | 2019-08-23 | 华东师范大学 | A kind of preparation method of redox graphene and nitrogen-doped graphene |
| CN114032525B (en) * | 2021-11-04 | 2023-09-12 | 西南科技大学 | Diamond-multilayer graphene composite cathode material and preparation method thereof |
| CN114249316B (en) * | 2021-12-07 | 2023-06-06 | 厦门大学 | Method and device for synthesizing metal doped fullerene material at high temperature in double temperature areas |
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