CN106148910A - A kind of preparation method of nitrogen-doped graphene thin film - Google Patents
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Abstract
The present invention provides the preparation method of a kind of nitrogen-doped graphene thin film, described method includes step: first provide a substrate, described substrate being placed in dual temperature sound zone system, and places carbon nitrogen source in described dual temperature sound zone system, heating is with the precursor layer at described substrate surface formation of deposits nitrogen-doped graphene；Then passing to gaseous carbon sources, under hot conditions, carbon laydown reaction forms nitrogen-doped graphene thin film.The present invention introduces micro-molecular gas carbon source on the basis of solid-liquid carbon nitrogen source growth nitrogen-doped graphene method and improves precursor layer, make defect in existing method more, electrical properties is poor, doping content uncontrollable nitrogen-doped graphene film quality is improved, thus it is outstanding to obtain electric property, the N-type graphene film that the less N doping of defect is controlled.
Description
Technical field
The present invention relates to material and prepare manufacture field, particularly relate to the preparation method of a kind of nitrogen-doped graphene thin film.
Background technology
Graphene is the two-dimensional material with alveolate texture that a kind of monolayer carbon atom is arranged with hexagonal structure, from 2004
Year first passage micromechanics has been peeled off since producing, because of optics, electricity, calorifics and the mechanical property of its uniqueness, obtained from
The extensive concern of research worker all over the world.The performance of these excellences makes Graphene at touch screen, field-effect transistor, sensitive
The numerous areas such as sensor, solaode, heavy-duty battery and super capacitor have potential application.But, intrinsic Graphene
The feature of zero band gap brings difficulty in the application of field of electronic devices also to it, and as big in leakage current, on-off ratio is low, the most such as
What obtains N-shaped and p-type Graphene becomes its key in electrical application.Scientist develops multiple method for this problem
With technology, wherein the doping of nitrogen element is its important means changed to n-type semiconductor.
Graphene nitrogen-doping method mainly has chemical gaseous phase deposition (CVD) method, hydrothermal synthesis method, gas ions sputtering technology etc. at present
Deng, these method combined coefficienies and quality are the most relatively low, it would be highly desirable to improve.Wherein the CVD of metal catalytic is at large area deposition stone
There is advantage in ink alkene thin film, therefore the method is also used to grow nitrogen-doped graphene thin film.If Liu Yun boundary seminar is by using
Little gas molecule methane gas is as carbon source, and ammonia is as nitrogen source, at copper film thick for silicon substrate surface deposition 25nm as catalysis
Agent, keeps 10 minutes under the high temperature of 800 DEG C, has prepared which floor nitrogen-doped graphene of minority；Additionally, solid-liquid carbon
Nitrogen source such as pyridine, tripolycyanamide etc. are also used to grow nitrogen-doped graphene thin film, are specially and use carrier gas to be steamed by solid-liquid carbon nitrogen source
Vapour is brought in the metallic catalyst substrate being placed under the conditions of uniform temperature, obtains nitrogen-doped graphene thin film in substrate surface deposition.
Although graphene film technique prepared by above-mentioned CVD method is simple, but still there are some problems, as more in Graphene defect,
Electrical properties is poor, and nitrogen doped concentration is wayward, and the thin film number of plies is difficult to control etc..Therefore seeking one, can to reduce Graphene thin
Defect in film, improve the preparation method of high-quality large area nitrogen-doped graphene thin film of electrical properties for present Graphene at light
The application in the field such as electronic device, solar cell is significant.
Summary of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide the preparation side of a kind of nitrogen-doped graphene thin film
Method, is used for solving in prior art that nitrogen-doped graphene film doping concentration is wayward, lattice defect is many, electrical properties is poor
Problem.
For achieving the above object and other relevant purposes, the present invention provides the preparation method of a kind of nitrogen-doped graphene thin film, described
Preparation method at least includes:
1) substrate is provided, described substrate is placed in dual temperature sound zone system, and in described dual temperature sound zone system, places carbon nitrogen source, heating
With the precursor layer at described substrate surface formation of deposits nitrogen-doped graphene；
2) being passed through gaseous carbon sources, under hot conditions, carbon laydown reaction forms nitrogen-doped graphene thin film.
As a kind of preferred scheme of the preparation method of nitrogen-doped graphene thin film of the present invention, described step 1) in, place carbon
Before nitrogen source, it is additionally included under protective atmosphere the step that substrate is carried out to be made annealing treatment.
As a kind of preferred scheme of the preparation method of nitrogen-doped graphene thin film of the present invention, described step 1) middle employing chemistry
Gas-phase deposition forms the precursor layer of nitrogen-doped graphene, including step:
1-1) described carbon nitrogen source and substrate are placed on the zones of different of dual temperature sound zone system, and heat respectively, simultaneously will by carrier gas
Carbon nitrogen source steam introduces substrate region, deposits；
1-2) stopping heating, be cooled to room temperature, taking out surface deposition has the substrate of nitrogen-doped graphene precursor layer.
A kind of preferably scheme, described step 1-1 of preparation method as nitrogen-doped graphene thin film of the present invention) in carbon nitrogen source
Heating temperature range is 50～200 DEG C.
A kind of preferably scheme, described step 1-1 of preparation method as nitrogen-doped graphene thin film of the present invention) in the adding of substrate
Hot temperature range is 250～600 DEG C.
A kind of preferably scheme, described step 1-1 of preparation method as nitrogen-doped graphene thin film of the present invention) in carrier gas be hydrogen
Gas or hydrogen and the mixed gas of argon.
A kind of preferably scheme, the described step 1 of preparation method as nitrogen-doped graphene thin film of the present invention) in sedimentation time
For 10min～80min.
A kind of preferably scheme, the described step 1 of preparation method as nitrogen-doped graphene thin film of the present invention) in carbon nitrogen source be
Nitrogen heteroaromatic compounds and derivant thereof.
As a kind of preferably scheme of the preparation method of nitrogen-doped graphene thin film of the present invention, described carbon nitrogen source is solid or liquid
Body.
As a kind of preferably scheme of the preparation method of nitrogen-doped graphene thin film of the present invention, described base material is Au, Co,
The alloy material of one or more in Pt, Pd, Ir, Ru, Ni, Cu or be coated with the gold of above metal material or alloy material
Belong to paper tinsel, silicon chip, glass.
As a kind of preferably scheme of the preparation method of nitrogen-doped graphene thin film of the present invention, select Au, Co, Pt, Pd, Ir,
When the alloy material of one or more in Ru, Ni, Cu is substrate, in addition it is also necessary to process substrate, processing mode includes adopting
Carry out chemical polishing with acetic acid, nitric acid or hydrochloric acid or under the conditions of phosphoric acid, carry out electrochemical polish.
As a kind of preferred scheme of the preparation method of nitrogen-doped graphene thin film of the present invention, described step 2) at least include step
Rapid:
2-1) deposition have the substrate of nitrogen-doped graphene precursor layer put in high-temperature systems；
2-2) heat described high-temperature systems and be passed through hydrogen and micro-molecular gas carbon source, making the crystallization of nitrogen-doped graphene presoma go forward side by side
Single step reaction deposits；
2-3) stopping heating, be cooled to room temperature, taking out deposition has the substrate of nitrogen-doped graphene thin film.
A kind of preferably scheme, the described step 2 of preparation method as nitrogen-doped graphene thin film of the present invention) in carbon source be low
Carbochain Hydrocarbon.
A kind of preferably scheme, the described step 2 of preparation method as nitrogen-doped graphene thin film of the present invention) sedimentation time is
0.5～50min.
A kind of preferably scheme, the described step 2 of preparation method as nitrogen-doped graphene thin film of the present invention) heating-up temperature is
600 DEG C～1100 DEG C.
As it has been described above, the preparation method of the nitrogen-doped graphene thin film of the present invention, have the advantages that the present invention mixes with nitrogen
Miscellaneous graphene film be grown to object of study, improve for existing method, existing solid-liquid carbon nitrogen source grow N doping
The method that micro-molecular gas carbon source improves precursor layer is introduced on the basis of Graphene method, so that defect is more in existing method,
The poor nitrogen-doped graphene film quality of electrical properties is improved, thus it is outstanding to obtain electric property, and the less nitrogen of defect is mixed
Miscellaneous graphene film.What is more important, the method can realize the N doping of film forming by the technology controlling and process of carbon nitrogen source deposition step
Content is controlled.Meanwhile, the method is completely suitable for the growth of large area nitrogen-doped graphene thin film, the uniformity of film obtained is good,
Electric property is excellent.
Accompanying drawing explanation
Fig. 1 is the preparation method process chart of nitrogen-doped graphene thin film of the present invention.
Fig. 2 is dual temperature sound zone system schematic diagram of the present invention, and wherein, 1 is carbon nitrogen source region in reaction, and 2 is substrate institute in reaction
In region.
Fig. 3 is the Raman spectrogram of nitrogen-doped graphene thin film prepared by the present invention.
Fig. 4 is the stereoscan photograph of nitrogen-doped graphene thin film prepared by the present invention.
Fig. 5 is the x-ray photoelectron power spectrum of nitrogen-doped graphene thin film prepared by the present invention.
Fig. 6 is the C peak comparison diagram of nitrogen-doped graphene prepared by the present invention and the x-ray photoelectron power spectrum of pure Graphene.
Fig. 7 is N peak and the swarming figure thereof of the x-ray photoelectron power spectrum of nitrogen-doped graphene prepared by the present invention.
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by disclosed by this specification
Content understand other advantages and effect of the present invention easily.The present invention can also be added by the most different detailed description of the invention
To implement or application, the every details in this specification can also be based on different viewpoints and application, in the essence without departing from the present invention
Various modification or change is carried out under god.
Refer to accompanying drawing.It should be noted that the diagram provided in the present embodiment illustrates that the present invention's is basic the most in a schematic way
Conception, the most graphic in component count, shape and size time only display with relevant assembly in the present invention rather than is implemented according to reality
Drawing, during its actual enforcement, the kenel of each assembly, quantity and ratio can be a kind of random change, and its assembly layout kenel is also
It is likely more complexity.
As it is shown in figure 1, the present invention provides the preparation method of a kind of nitrogen-doped graphene thin film, described nitrogen-doped graphene thin film
Preparation method at least comprises the following steps:
S1 a, it is provided that substrate, is placed in described substrate dual temperature sound zone system, and places carbon nitrogen source in described dual temperature sound zone system, add
Heat is with the precursor layer at described substrate surface formation of deposits nitrogen-doped graphene；
S2, is passed through gaseous carbon sources, and under hot conditions, carbon laydown reaction forms nitrogen-doped graphene thin film.
Below in conjunction with concrete accompanying drawing, the preparation method of the nitrogen-doped graphene thin film of the present invention is done detailed introduction.
Step S1 is first carried out, it is provided that a substrate, described substrate is placed in dual temperature sound zone system, and puts in described dual temperature sound zone system
Putting carbon nitrogen source, heating is with the precursor layer at described substrate surface formation of deposits nitrogen-doped graphene.
Described base material is the alloy material of one or more in Au, Co, Pt, Pd, Ir, Ru, Ni, Cu or plating
There are above metal material or the metal forming of alloy material, silicon chip, glass etc..In the present embodiment, use Copper Foil as substrate.
As example, selecting the alloy material of one or more in Au, Co, Pt, Pd, Ir, Ru, Ni, Cu is substrate
Time, in addition it is also necessary to processing substrate, processing mode includes using acetic acid, nitric acid or hydrochloric acid etc. to carry out chemical polishing or at phosphorus
Electrochemical polish is carried out under the conditions of acid.In the present embodiment, use acetic acid to carrying out pretreatment at the bottom of cuprio.
It is: Copper Foil is put in beaker to clean with deionized water, acetone, EtOH Sonicate successively the concrete processing procedure of substrate；
Copper Foil after having cleaned is put in acetic acid and is soaked, and cleans with deionized water, N after taking-up2Dry up.
The structure of described two temperature system, as in figure 2 it is shown, be provided with two different regions in this system, is respectively used to place base
The end and carbon nitrogen source, it is possible to substrate and carbon nitrogen source are respectively heated.Wherein, carbon nitrogen is placed in the region 1 near carrier gas inlet
Source, the region 2 away from carrier gas inlet places substrate, and two regions are utilized respectively resistance wire and heat.
Described carbon nitrogen source is nitrogen heteroaromatic compounds and derivant thereof.For example, it may be pyridine or azanaphthalene compound.More enter
One step, for example, it may be the one of pyridine, Pentachloropyridine, quinoline, tripolycyanamide or 2，3-benzodiazine etc..The present embodiment
In, carbon nitrogen source can elect Pentachloropyridine temporarily as.The form of described carbon nitrogen source can be solid or liquid.
Before carrying out first time chemical vapor deposition method, substrate first can be carried out under the conditions of such as argon at protective atmosphere
Annealing, the temperature of annealing can be in the range of 800～1100 DEG C.
Utilizing dual temperature sound zone system to carry out chemical gaseous phase deposition for the first time afterwards, its detailed process is:
The first step, is placed on described carbon nitrogen source and substrate the zones of different of dual temperature sound zone system, and heats respectively, simultaneously by carrying
Carbon nitrogen source steam is introduced substrate region by gas, deposits；
Second step, stops heating, is cooled to room temperature, and taking out surface deposition has the substrate of nitrogen-doped graphene precursor layer.
Such as, Copper Foil is put into the position 2 in dual temperature district CVD system, then weigh 0.005～1g Pentachloropyridine and be placed in quartz
Position 1 in pipe, evacuation；Being passed through hydrogen as carrier gas, flow is chosen for 30～100sccm, will heat up at position 2 simultaneously
To 250～600 DEG C；50～200 DEG C will be warming up at position 1, respectively insulation 10～80min after equitemperature is stable；Take out after cooling
Deposition has the Copper Foil of nitrogen-doped graphene presoma.
In the present embodiment, the carrier gas being passed through is hydrogen.Certainly, in other embodiments, described carrier gas can also be hydrogen and argon
The mixed gas of gas or other suitable gas, do not limit at this.
In this step, by the catalytic action of metallic substrates, utilize chemical gaseous phase depositing high temperature equipment successful growth N doping graphite
The precursor layer of alkene.
Then performing step S2, be passed through gaseous carbon sources, under hot conditions, carbon laydown reaction forms nitrogen-doped graphene thin film.
Detailed process is: first, and deposition has the substrate of nitrogen-doped graphene precursor layer put in high-temperature systems；Then institute is heated
State high-temperature systems, and be passed through micro-molecular gas carbon source and hydrogen deposits, make the crystallization of nitrogen-doped graphene presoma and little molecule
Carbon source fills space；Finally, stopping heating, be cooled to room temperature, taking out deposition has the substrate of nitrogen-doped graphene thin film.
Such as, deposition have the Copper Foil of nitrogen-doped graphene precursor layer be placed in CVD system, evacuation；It is passed through H2As load
Gas, flow is chosen for 30～100sccm, is warming up to 600～1100 DEG C simultaneously；Equitemperature is passed through carbon source CH after reaching setting value4,
Flow is chosen for 0.1～5sccm, the time 0.5～50min；The Copper Foil covering with nitrogen-doped graphene thin film is taken out after cooling.
Described carbon source is low carbon chain Hydrocarbon.Such as, methane, ethane, ethylene acetylene etc..In the present embodiment, described
Carbon source is methane.
It should be noted that the enforcement of step S2 can occur in dual temperature district high-temperature systems in step sl, it is also possible to alternative
Select single warm area high-temperature systems to complete.If selecting single warm area system, then need the substrate that deposition is had nitrogen-doped graphene precursor layer
Dual temperature sound zone system from step S1 takes out, be placed in single warm area system, then be passed through gaseous carbon sources.
Using high temperature deposition mode in this step, high-temperature temperature is preferably more than 800 DEG C, in high-temperature deposition process, N doping
Graphene precursor layer crystallizes, and little molecule carbon source is filled in precursor layer, plays repairing effect, reduces defect concentration.
Next nitrogen-doped graphene thin film is transferred to SiO2Characterize on/Si sheet.If Fig. 3 is N doping graphite prepared by the present invention
The Raman spectrum of alkene thin film, it is observed that characteristic peak D, G, 2D peak of Graphene from Fig. 3, illustrates finally to prepare
Be the graphene film with single layer structure, and defect is less.Fig. 4 is the electronic display after thin film is transferred in silicon chip substrate
Micro mirror photo, as can be seen from Figure 4 the uniformity of thin film is good with integrity, and defect is few.The X of nitrogen-doped graphene thin film penetrates
Photoelectron spectra is as shown in Fig. 5, Fig. 6 and Fig. 7.Fig. 5 is score, it can be seen that significantly C, N peak；Fig. 6 represents that nitrogen is mixed
Miscellaneous Graphene and the C peak comparison diagram of pure Graphene, there is obvious C-N peak in nitrogen-doped graphene；Fig. 7 represents nitrogen-doped graphene
The N peak swarming figure of x-ray photoelectron power spectrum, N element in doped graphene with pyrrolesization nitrogen, pyridine nitrogen and graphitization nitrogen
Three kinds of forms exist.Controlled by the technological parameter (such as amount, reaction temperature and the time etc. of carbon nitrogen source) of carbon nitrogen source deposition step
The N doping content that can realize film forming is controlled, can obtain prepared nitrogen-doped graphene by the calculating of XPS spectrum diagram data thin
In film, nitrogen content is 1～10%.Hall effect test shows that it has N-type semiconductor characteristic.
In sum, the present invention provides the preparation method of a kind of nitrogen-doped graphene thin film, and described method includes step: first carry
For a substrate, described substrate being placed in dual temperature sound zone system, and places carbon nitrogen source in described dual temperature sound zone system, heating is with described
The precursor layer of substrate surface formation of deposits nitrogen-doped graphene；Then in described dual temperature sound zone system, it is passed through carbon source, under hot conditions
Carbon laydown reaction forms nitrogen-doped graphene thin film.The present invention is on the basis of solid-liquid carbon nitrogen source growth nitrogen-doped graphene method
Introduce micro-molecular gas carbon source and improve precursor layer, so that defect is more in existing method, the N doping that electrical properties is poor
Graphene film quality is improved, it is thus achieved that electric property is outstanding, the N-type graphene film that the less N doping of defect is controlled.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The principle of above-described embodiment only illustrative present invention and effect thereof, not for limiting the present invention.Any it is familiar with this skill
Above-described embodiment all can be modified under the spirit and the scope of the present invention or change by the personage of art.Therefore, such as
All that in art, tool usually intellectual is completed under without departing from disclosed spirit and technological thought etc.
Effect is modified or changes, and must be contained by the claim of the present invention.
Claims (15)
1. the preparation method of a nitrogen-doped graphene thin film, it is characterised in that described preparation method at least includes:
1) substrate is provided, described substrate is placed in dual temperature sound zone system, and in described dual temperature sound zone system, places carbon nitrogen source, heating
With the precursor layer at described substrate surface formation of deposits nitrogen-doped graphene；
2) being passed through gaseous carbon sources, under hot conditions, carbon laydown reaction forms nitrogen-doped graphene thin film.
The preparation method of nitrogen-doped graphene thin film the most according to claim 1, it is characterised in that: described step 1) in, put
Before putting carbon nitrogen source, it is additionally included under protective atmosphere the step that substrate is carried out to be made annealing treatment.
The preparation method of nitrogen-doped graphene thin film the most according to claim 1, it is characterised in that: described step 1) middle employing
Chemical vapor deposition method forms the precursor layer of nitrogen-doped graphene, including step:
1-1) described carbon nitrogen source and substrate are placed on the zones of different of dual temperature sound zone system, and heat respectively, pass through carrier gas simultaneously
Carbon nitrogen source steam is introduced substrate region, deposits；
1-2) stopping heating, be cooled to room temperature, taking out surface deposition has the substrate of nitrogen-doped graphene precursor layer.
The preparation method of nitrogen-doped graphene thin film the most according to claim 3, it is characterised in that: described step 1-1) in carbon
The heating temperature range in nitrogen source is 50～200 DEG C.
The preparation method of nitrogen-doped graphene thin film the most according to claim 3, it is characterised in that: described step 1-1) in base
The heating temperature range at the end is 250～600 DEG C.
The preparation method of nitrogen-doped graphene thin film the most according to claim 3, it is characterised in that: described step 1-1) middle load
Gas is hydrogen or hydrogen and the mixed gas of argon.
The preparation method of nitrogen-doped graphene thin film the most according to claim 1, it is characterised in that: described step 1) middle deposition
Time is 10min～80min.
The preparation method of nitrogen-doped graphene thin film the most according to claim 1, it is characterised in that: described step 1) in carbon nitrogen
Source is nitrogen heteroaromatic compounds and derivant thereof.
The preparation method of nitrogen-doped graphene thin film the most according to claim 1, it is characterised in that: described carbon nitrogen source be solid or
Person's liquid.
The preparation method of nitrogen-doped graphene thin film the most according to claim 1, it is characterised in that: described base material be Au,
The alloy material of one or more in Co, Pt, Pd, Ir, Ru, Ni, Cu or be coated with above metal material or alloy
The metal forming of material, silicon chip, glass.
The preparation method of 11. nitrogen-doped graphene thin film according to claim 10, it is characterised in that: select Au, Co, Pt,
When the alloy material of one or more in Pd, Ir, Ru, Ni, Cu is substrate, in addition it is also necessary to substrate is processed, place
Reason mode includes using acetic acid, nitric acid or hydrochloric acid carry out chemical polishing or carry out electrochemical polish under the conditions of phosphoric acid.
The preparation method of 12. nitrogen-doped graphene thin film according to claim 1, it is characterised in that: described step 2) at least
Including step:
2-1) deposition have the substrate of nitrogen-doped graphene precursor layer put in high-temperature systems；
2-2) heat described high-temperature systems, and be passed through micro-molecular gas carbon source and hydrogen, make nitrogen-doped graphene presoma crystallize also
Reactive deposition further；
2-3) stopping heating, be cooled to room temperature, taking out deposition has the substrate of nitrogen-doped graphene thin film.
The preparation method of 13. graphene films according to claim 1, it is characterised in that: described step 2) in carbon source be low
Carbochain Hydrocarbon.
The preparation method of 14. graphene films according to claim 1, it is characterised in that: described step 2) sedimentation time is
0.5～50min.
The preparation method of 15. graphene films according to claim 1, it is characterised in that: described step 2) heating-up temperature is
600 DEG C～1100 DEG C.
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| CN109019571A (en) * | 2017-06-12 | 2018-12-18 | 中国科学院上海高等研究院 | The preparation method of the controllable nitrogen-doped graphene of the number of plies |
| 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 |
| CN109534328A (en) * | 2017-09-22 | 2019-03-29 | 天津大学 | A kind of two dimension 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 |
| CN114032525A (en) * | 2021-11-04 | 2022-02-11 | 西南科技大学 | Diamond-multilayer graphene composite cathode material and preparation method thereof |
| CN114032525B (en) * | 2021-11-04 | 2023-09-12 | 西南科技大学 | Diamond-multilayer graphene composite cathode material and preparation method thereof |
| CN114249316A (en) * | 2021-12-07 | 2022-03-29 | 厦门大学 | Method and device for synthesizing metal-doped fullerene material at high temperature in double temperature zones |
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