CN104651802A - Method for directly synthesising nitrogen-doped graphene by simply using solid nitrogen source - Google Patents
Method for directly synthesising nitrogen-doped graphene by simply using solid nitrogen source Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation of carbon nanomaterials, and provides a novel method for synthesising nitrogen-doped graphene by taking melamine as a main nitrogen and carbon source and methane as an auxiliary carbon source through a chemical vapour deposition method under the normal-pressure condition. Other catalysts, except for a metal substrate, and a conventional gas or liquid nitrogen source are not used in the method; therefore, the method is low in cost, non-toxic, simple and convenient to operate and convenient in process application; furthermore, no specific requirement for equipment exists in the reaction process; other heating devices, except for a main heating device, are unnecessary; therefore, the method is high in operability and is applied to practical popularization; the temperature of copper is slowly increased in the low-temperature stage at first; a nitrogen source and a carbon source are simultaneously introduced into a tubular furnace for one time when the temperature of copper reaches reaction temperature; then, the temperature is rapidly decreased to room temperature after completing reaction; at the time, a layer of nitrogen doped graphene film is formed on the surface of metal; and structural regulation and control, such as the doping amount and doping type of nitrogen in graphene and the thickness and crystallization degree of graphene, can be realized through the parameters, such as the optimized nitrogen source amount, temperature matching of front and rear temperature areas, the reaction time and the reaction temperature.
Description
Technical field
The invention belongs to carbon nanomaterial preparation technology field, relating to a kind of is nitrogenous source with trimeric cyanamide, without the need to extra catalyst, one-step synthesis nitrating Graphene in CVD process, use instrument simple in reaction process, process is succinct, does not need the method for the CVD synthesizing graphite alkene of other heating installations except main heating installation.
Background technology
The rare sp as a kind of uniqueness of graphite
2the two-dimension single layer material of hydridization, its stable hexagonal lattice structure imparts the physics and chemistry character (Geim A K.science, 2009,324,1530.) of the rare many excellences of graphite.Such as its thermal conductivity (3000W/ (m K)) 10 times is to copper (397W/ (m K)), and Young's modulus reaches 1.0TPa, and hardness is greater than diamond, is the material that current nature is the hardest.In addition under room temperature, Graphene also has electronic mobility (the about 15000cm of superelevation
2/ (V s)) be greater than silicon single crystal, resistivity is about 10
-6Ω cm, lower than copper or silver, is the material that resistivity is minimum in the world at present.And single-layer graphene has good optical property, be only 2.3% at very wide wave band internal absorptance.This makes it all have broad application prospects in many high-tech areas, this also make the preparation of Graphene become recent research focus (Li Xu. material Leader, 2008,22 (8), 48.).
But Graphene also has two large weak points, first Graphene itself does not have band gap, which greatly limits the application of Graphene on electricity device.Secondly, the surface of Graphene does not have activating functional group, and be unfavorable for the compound with other materials (as metallics and organic functions small molecules), this also have impact on the research and extension of Graphene in a lot of Application Areas.Scientific research finds, Heteroatom doping is carried out in Graphene, can ensure under Graphene superior electrical performance prerequisite largely, introduce band gap, and graphenic surface reaction site is provided, strengthen the chemically reactive of Graphene, thus many electrochemical field can be applied to more easily, as fuel cell (Zheng B, et al.Electrochemistry Communications, 2013, 28, 24.), sensor (Guo H L, et al.Sensors and Actuators B:Chemical, 2014, 193, 623.), ultracapacitor (Su Peng. Acta PhySico-Chimica Sinica, 2012, 28, 2745.).
Nitrating Graphene can be divided into three kinds according to the keyed jointing mode of C-N, i.e. graphite mould N, pyridine type N and pyrroles type N.Wherein affect the electrical property qualitative factor of nitrating Graphene, mainly nitrating mode and itrogen content of getter with nitrogen doped, and the relative proportion of each nitrating mode plays a leading role.Such as there are some researches show, the relative content of graphite mould N to play a leading role (Wang Z for nitrating Graphene electrocatalysis characteristic, et al.Journal of Materials Chemistry C, 2014,2,7396.), Wang seminar synthesis nitrating Graphene with report (Lu Y F before, et al.ACS Nano, 2013,7,6522.), the itrogen content of getter with nitrogen doped of the nitrating Graphene of Liang Ge seminar synthesis is 5.6%, but in the nitrating type of Wang, graphite mould nitrogen reaches more than 40%, and the electronic mobility of final nitrating Graphene is respectively 74cm
2v
-1s
-1and 5cm
2v
-1s
-1, the two difference is more.
The character investigation and application of nitrating Graphene depends on its cheap mass-producing preparation.Since Graphene is prepared by tape stripping method first, about the preparation of nitrating Graphene also along with people continue to bring out new method to the concern of its electro catalytic activity, such as: graphene oxide is hot method, chemical meteorology deposition method, hydrothermal method, plasma processing etc. altogether.
Wherein graphene oxide hot method altogether, needs in process to use the vitriol oil, then with NH
3(Zhang L.S, et al.PhysicalChemistry Chemical Physics, 2010,12,12055.) or organic nitrogen source (as trimeric cyanamide) (Sheng Z.H, et al.ACSNano, 2011,5,4350.) carry out common heat and obtain.Hydrothermal method often uses metal nitrogen salt and reactive organic molecule, as Li
3n/CCl
4(Deng D, et al.Chemistry of Materials, 2011,23,1188.).Plasma method uses graphene oxide and N
2(Shao Y, et al.Journal of Materials Chemistry, 2010,20,7491.) react obtained nitrating Graphene.
Because graphene oxide method needs to use the vitriol oil, the security of reaction limits the actual popularization of the method; Hydro-thermal rule limits its development because its cost is higher and circulation ratio is poor; Plasma processing requires higher to reaction unit, is unfavorable for practical application.Comparatively speaking, the research of chemical Vapor deposition process synthesis nitrating Graphene achieves great successes, is wherein the comparatively ripe of catalytic substrate research with copper, about the selection of nitrogenous source, is respectively gas nitrogenous source, liquid nitrogenous source and solid nitrogenous source.The research of gas nitrogenous source is with NH
3(Wei D, et al.Nano Letters, 2009,9,1752.) are more, and its concrete operations are for using NH
3with CH
4reaction unit is passed into after mixing; Liquid nitrogenous source mainly uses macromole nitrogenous compound, as used pyridine (Jin Z, et al.ACS Nano, 2011,5,4112.), the nitrating Graphene quality of this method synthesis is higher, but due to pyridine price higher and have certain toxicity, be unfavorable for producing and promote.
Study less at present about solid nitrogenous source, existing main achievement is: Sun seminar uses trimeric cyanamide to be dissolved in PMMA solution as carbon source, nitrogenous source, reaction process need be carried out under lower pressure, and after needing spin coating, use lithographic methods to assist synthesizing graphite alkene (Sun Z Z, et al.Nature, 2010,468,549.), synthesizing itrogen content of getter with nitrogen doped is 2%.Wang seminar uses trimeric cyanamide as nitrogenous source (Wang Z, et al.Journal of Materials Chemistry C, 2014,2,7396.), the itrogen content of getter with nitrogen doped of synthetic product is 5.6%, but process adopts lower pressure, and employ extra heating unit, process is more complicated.
This research directly uses trimeric cyanamide as nitrogenous source, do not need trimeric cyanamide is carried out to solvation, is coated on the special pre-treatment such as catalyst surface, reaction process is carried out at ambient pressure, reaction cost is cheap, do not need other heating installations except main heating installation, low to the requirement of reaction unit, and easy to operate, technique is simply easy to produce and promotes.
Summary of the invention
Synthesis nitrating Graphene adopts solid nitrogenous source method, simplifies reaction process, reduces costs, utilize cheap solid nitrogenous source trimeric cyanamide, utilize CVD process directly to synthesize nitrating Graphene in atmospheric conditions.Procedure is except the catalytic metal of graphene growth, without the need to extra catalyst, do not need to carry out special processing (be such as mixed with solution or be coated on additional catalytic material surface) to the trimeric cyanamide of solid, and except using main heating unit, do not need other heating installation.
The technical scheme that the present invention solves the employing of its technical problem is: utilize two temperature-area tubular furnace; trimeric cyanamide is placed in special quartz specimen boat in overdraught direction; in downstream direction; metal catalytic substrate (as Copper Foil) is placed on the quartzy pallet with magnetite handle; thereafter tube furnace two side flange is installed; open mixed gas system and regulate gas flow required in CVD successively; then under carrier gas protection; regulate temperature regulating device, by tube furnace with the ramp of 10-20 DEG C/min to temperature of reaction undetermined.In the method, in order to solve the hot volatilization problems of trimeric cyanamide, before arrival temperature of reaction, trimeric cyanamide sample is placed in outside, diamond heating district all the time, when being delivered in process furnace by sample after arrival preset temperature again.Utilize the air flow line of carrier gas/reaction gas, the catalytic metal substrate Carbon and nitrogen sources of gasification being transported to downstream direction realizes the decomposition of carbon source/nitrogenous source, carbon atom/nitrogen-atoms is in the process such as deposition, diffusion/dissolving, nucleation, growth of catalytic metal surface.After question response terminates, the catalytic metal of downstream direction (the second warm area) is shifted out heating warm area, with the speed fast cooling of 20-50 DEG C/min.To be cooledly to room temperature, take out metal base, now catalytic metal surface successfully synthesizes nitrating Graphene.
The invention has the beneficial effects as follows, reaction pressure is normal atmosphere, does not need other catalyzer beyond metal catalytic substrate in process, and does not use conventional gas or liquid nitrogenous source, and cost is low, nontoxic, easy and simple to handle, is convenient to process application.Particular requirement is not had to conversion unit, does not need other heating units beyond main heating unit, workable, be applicable to actual popularization.In Graphene, the doping of nitrogen and the structure regulating such as thickness, crystallization degree of doping type and Graphene all can be realized by the parameter such as Temperature Matching, reaction times, temperature of reaction of optimization nitrogenous source amount, front and back warm area.
Accompanying drawing explanation
Below in conjunction with accompanying drawing and example, the present invention is further described.
Fig. 1 is the reaction unit schematic diagram that the present invention synthesizes nitrating Graphene.
Fig. 2 is that the present invention synthesizes the temperature value schematic diagram of nitrating Graphene in different time sections.
Fig. 3 is first example take trimeric cyanamide as nitrogenous source, CH
4for carbon source, take Copper Foil as substrate, constant temperature 950 DEG C, H
2flow is that under 10sccm, reaction generates nitrating Graphene, is wherein warmed up to 1050 DEG C of annealing in reaction process, then cools to temperature of reaction reaction, and after question response completes, the nitrating Graphene that cooling generates rapidly is transferred to SiO through conventional wet chemistry method
2the opticmicroscope test picture on (thick 300nm)/Si surface and Raman spectrogram.
Fig. 4 is the condition according to first example, generates the XPS collection of illustrative plates of nitrogen-doped graphene.Confirm the synthesis utilizing this technology successfully to achieve nitrogen-doped graphene.
Fig. 5 is second example take trimeric cyanamide as nitrogenous source, CH
4for carbon source, Copper Foil is that substrate is at low temperature 500-1000 DEG C and reductibility carrier gas H
2effect under, the low-crystallinity Graphene that reaction generates is transferred to SiO through conventional wet chemistry method
2the opticmicroscope test picture on (thick 300nm)/Si surface and typical Raman spectrogram.
Fig. 6 the 3rd example take trimeric cyanamide as nitrogenous source, CH
4for carbon source, take Copper Foil as substrate, constant temperature 1000 DEG C, H
2under flow is respectively 10-50sccm, reaction generates nitrating Graphene, and when carbon source and nitrogenous source are introduced to when 1000 DEG C by temperature simultaneously, after question response completes, the nitrating Graphene that cooling generates rapidly is transferred to SiO through conventional wet chemistry method
2the opticmicroscope test picture on (thick 300nm)/Si surface and Raman spectrogram.
Embodiment
The present invention first allows two temperature-area tubular furnace reach treat fixed temperature, passes into H in heat-processed
2be oxidized to prevent Copper Foil, in process, carbon source and nitrogenous source all do not pass into tube furnace, after fixed temperature, the nitrogen of warm area side, tube furnace overdraught direction, carbon source are introduced into tube furnace when reaching, utilize high temperature to make it decompose to dissociate the material of carbon containing, nitrogen, utilize carrier gas to be delivered to copper foil surface generation chemical reaction, utilize thereafter fast cooling to make copper foil surface generate nitrating Graphene.The metal base itself wherein used in CVD synthesis nitrating Graphene process serves as the effect of catalyzer, does not therefore need extra catalyst more here.And not using gas, liquid nitrogen source relative to traditional method, reaction process only needs a main heating installation just can complete, and do not need other heating installations, therefore our method is simpler, cheap, is applicable to promoting.
Described metal base all refers to the clean substrate after with acetic acid, acetone and Virahol successively ultrasonic 5min in the method for the invention; Described gas ratio is standard volume flow ratio;
Specifically, we with trimeric cyanamide for main nitrogen, carbon source, CH
4be that auxiliary carbon source uses the method example of CVD synthesizing graphite alkene to comprise the steps:
Be the present invention shown in Fig. 1 and Fig. 2 take trimeric cyanamide as nitrogenous source, CH
4for carbon source, the method for CVD synthesizing graphite alkene and main heating installation are at the schematic diagram of different time sections temperature value.T in figure
1be the slow temperature rise period before temperature, experimentally need thereafter to be divided into and annealing and unannealed process two kinds of situations are carried out to catalytic metal.Wherein, the situation of unannealed process is raised to T when warm area
1introduce nitrogenous source and carbon source, fast cooling after the reaction of experience for some time after temperature at once; The situation of anneal is at T by the catalytic metal of downstream side warm area
2to anneal at temperature certain hour, be cooled to temperature of reaction T
3after, introducing nitrogenous source and carbon source carry out the reaction of certain hour, then fast cooling.Wherein the carrier gas flux changing conditions of whole process is that carrier gas flux proportioning remains unchanged before starting the reaction, and carrier gas is only containing Ar and H
2gas mixture, when reaching step of reaction, carbon source and nitrogenous source are introduced to participate in simultaneously and react.This stage carrier gas is except Ar and H
2gas mixture outward also containing auxiliary carbon source CH
4, be the fast cooling stage after having reacted, now carrier gas flux proportioning is consistent with initial situation, namely only containing Ar and H
2gas mixture.By the method, we have successfully obtained nitrating Graphene.
Shown in Fig. 3 is an example of the nitrating Graphene generated by the experimentation shown in Fig. 2 after carrying out anneal to Copper Foil.This example carrier gas flux proportioning is Ar/H
2=50/1, temperature of reaction elects 950 DEG C as.Can find out, under this condition, there is good continuity result, and its Raman 2D peak is better by force, thus generates the good nitrating Graphene of quality.
Test by the XPS of the generation nitrating Graphene shown in Fig. 3 shown in Fig. 4.Test result is presented at and combines can be that the characteristic peak of N1s appear in the position of 399.34eV, and this fully shows to utilize this technology can successful synthetic nitrogen doped graphene.
Shown in Fig. 5 is by the annealing group example shown in Fig. 2.This example contains the impact of nitrating Graphene at differential responses temperature.Wherein a-e group Ar flow is 400-600sccm, H
2flow is 20sccm, and temperature of reaction is respectively 500,800,900,950,1000 DEG C, observes Raman spectrogram and can find out, due to 2D peak (2700cm
-1near) the strongest when being 1000 DEG C, 950 DEG C have more weak 2D peak, do not have the appearance at 2D peak when less than 900 DEG C.So the lower nitrating Graphene of crystallinity can be grown below 900 DEG C.Contrast opticmicroscope figure, when temperature of reaction is 1000 DEG C, continuity is poor, and 950 DEG C have good continuity.Therefore, our technology can obtain the nitrogen-doped graphene of different crystallization degree by the regulation and control of temperature.
The unannealed situation example be through shown in Fig. 2 shown in Fig. 6.This example contains the impact on the nitrating Graphene quality of synthesis under different carrier gas flux conditions of mixture ratios.Wherein in a-d figure, Ar flow is 400-600sccm, H
2be respectively 50,20,15,10sccm.After reaction, sample is through opticmicroscope figure and Raman spectrum test, and wherein Graphene transfer process is all utilized by Graphene wet type transfer method to transfer to SiO
2carry out behind (thick 300nm)/Si surface.From opticmicroscope figure, we can see, H
2flow generates a quality skim relatively preferably when 20sccm, work as H
2during change, the continuity of film is deteriorated.Observe Raman spectrogram, work as H
2from 50sccm to 10sccm, during change, all there is 2D peak (2700cm
-1near), and the carbon film generated all has certain D peak (1350cm
-1near), prove now to generate nitrating Graphene (Graphene of standard type can produce along with atom N enters Graphene lattice the D peak reacting defect level).And as can be seen from the color comparator of opticmicroscope, the thickness of produced film and continuity are subject to the impact of hydrogen flowing quantity very large.Therefore, our technology can obtain the nitrogen-doped graphene of different thickness by the regulation and control of the reaction conditionss such as hydrogen, is even expected to the nitrogen-doped graphene quantum dot of composition rule distribution.
Above-mentioned example and characterization result prove that the method that we invent can use trimeric cyanamide as solid nitrogenous source at a lower temperature, and reaction can generate nitrating Graphene.This technology, owing to using CVD technology, can realize the regulation and control of the doping of nitrogen in Graphene and the constitutional features such as thickness, crystallization degree of doping type and Graphene conveniently by the reaction parameter such as Temperature Matching, reaction times, temperature of reaction of optimization nitrogenous source amount, front and back warm area.
Claims (10)
1. one kind is the method that nitrogenous source synthesizes nitrating Graphene with trimeric cyanamide, it is characterized in that, under certain reaction pressure, do not use other catalyzer beyond metal base, do not need other heating installations beyond main heating installation, under the protection of the carrier gas of definite composition and flow, metal base is first allowed slowly to heat up, again by as the nitrogenous source outside heating zone after temperature of reaction to be achieved, carbon source is disposable to be introduced in reaction tube furnace simultaneously, the degradation production of trimeric cyanamide and carbon source are incorporated into the reaction of metal substrate surface generation nitrating Graphene under the effect of carrier gas, question response completes, be cooled to room temperature rapidly, now metal substrate surface has generated one deck nitrating Graphene.
2. certain reaction pressure according to claim 1 comprises the reaction pressure such as normal pressure, vacuum that chemical gaseous phase depositing process uses.
3. metal base according to claim 1 comprises chemical gaseous phase depositing process synthesizing graphite alkene metallic membrane used, tinsel, tinsel.
4. other catalyzer beyond metal base according to claim 1, comprise organism or the inorganics of the made trimeric cyanamide activation of any other form except the necessary metal base of nitrating Graphene is synthesized in chemical vapour deposition, or industrial and artificial Kaolinite Preparation of Catalyst.
5. other heating installations beyond main heating installation according to claim 1, comprise except providing chemical Vapor deposition process heating zone except the equipment of temperature, many temperature-area tubular furnaces must place any equipment that can provide heating function such as other warm area, heating jackets etc. beyond metal base.
6. temperature of reaction according to claim 1 comprises the temperature value being enough to make in the temperature range of trimeric cyanamide decomposition-reduction generation nitrating Graphene or agraphitic carbon, and makes the product after trimeric cyanamide thermolysis and carbon source generate the temperature value in the temperature range of nitrating Graphene at metallic catalyst surfaces.
7. the composition of carrier gas according to claim 1 and flow, composition comprises reactant gases, reducing gas, carrier gas or several mixture, and flow comprises the gas mixing ratio that the carbon product successful conversion that low temperature generates can be become nitrating Graphene.
8. cooling according to claim 1 comprises the quick and slow cooling carried out with given pace, and the method that different time is lowered the temperature with different rates time variable control.
9. according to claim 1 is that the concrete grammar of nitrogenous source chemical vapour deposition synthesis nitrating Graphene comprises the steps: with trimeric cyanamide
1) clean metal catalytic substrate is placed in heating installation reaction chamber, passes into carrier gas.
2) utilize heating installation that temperature is elevated to temperature range according to claim 6, while keeping carrier gas to pass into, pass into trimeric cyanamide, CH
4keep for some time at such a temperature with reducing gas, metal catalytic substrate makes the nitrogen containing species after trimeric cyanamide thermolysis to react Formed nitrogen compound.
3) temperature range described in right 6, keeps for some time fully to react.
4) use certain cooling method that the temperature of metal catalytic substrate is down to normal temperature as required.
10. carrier gas according to claim 1 comprises: reductibility carrier gas such as hydrogen, ammonia etc. have the gas of reductibility; The gas that rare gas element is as comparatively stable in character such as argon gas, nitrogen, neons; The mixed gas of reductibility carrier gas and inert carrier gas.
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Cited By (8)
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| CN105417530A (en) * | 2015-12-14 | 2016-03-23 | 哈尔滨工业大学 | Large-scale preparation method of nitrogen-doped graphene |
| CN106148910A (en) * | 2015-04-03 | 2016-11-23 | 中国科学院上海高等研究院 | A kind of preparation method of nitrogen-doped graphene thin film |
| CN107311125A (en) * | 2017-07-25 | 2017-11-03 | 江苏大学 | A kind of nitrogen carbide nanometer sheet and its preparation method and application |
| CN107403658A (en) * | 2017-07-17 | 2017-11-28 | 北京大学 | A kind of high conductivity graphene film and preparation method thereof |
| CN107601473A (en) * | 2017-09-30 | 2018-01-19 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) for the grapheme material for preparing uniformity |
| 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 |
| CN112517044A (en) * | 2020-12-22 | 2021-03-19 | 盐城工学院 | Carbon nitride quantum dot/oxide nanofiber composite photocatalytic material and preparation method thereof |
| CN112875659A (en) * | 2021-03-11 | 2021-06-01 | 北京大学 | Method for realizing uniform fluorine doping of hexagonal boron nitride in situ |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106148910A (en) * | 2015-04-03 | 2016-11-23 | 中国科学院上海高等研究院 | A kind of preparation method of nitrogen-doped graphene thin film |
| CN106148910B (en) * | 2015-04-03 | 2019-01-04 | 中国科学院上海高等研究院 | A kind of preparation method of nitrogen-doped graphene film |
| CN105417530A (en) * | 2015-12-14 | 2016-03-23 | 哈尔滨工业大学 | Large-scale preparation method of nitrogen-doped graphene |
| CN107403658A (en) * | 2017-07-17 | 2017-11-28 | 北京大学 | A kind of high conductivity graphene film and preparation method thereof |
| CN107311125A (en) * | 2017-07-25 | 2017-11-03 | 江苏大学 | A kind of nitrogen carbide nanometer sheet and its preparation method and application |
| CN107311125B (en) * | 2017-07-25 | 2019-10-01 | 江苏大学 | A kind of nitrogen carbide nanometer sheet and its preparation method and application |
| CN107601473A (en) * | 2017-09-30 | 2018-01-19 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) for the grapheme material for preparing uniformity |
| CN107601473B (en) * | 2017-09-30 | 2019-08-27 | 中国电子科技集团公司第十三研究所 | A kind of modified chemical vapor deposition process (MCVD) preparing uniform grapheme material |
| 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 |
| CN112517044A (en) * | 2020-12-22 | 2021-03-19 | 盐城工学院 | Carbon nitride quantum dot/oxide nanofiber composite photocatalytic material and preparation method thereof |
| CN112875659A (en) * | 2021-03-11 | 2021-06-01 | 北京大学 | Method for realizing uniform fluorine doping of hexagonal boron nitride in situ |
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Application publication date: 20150527 |