CN105289689A - Synthesis and application of nitrogen-doped graphene quantum dot/similar-graphene phase carbon nitride composite material - Google Patents
Synthesis and application of nitrogen-doped graphene quantum dot/similar-graphene phase carbon nitride composite material Download PDFInfo
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- CN105289689A CN105289689A CN201510748490.8A CN201510748490A CN105289689A CN 105289689 A CN105289689 A CN 105289689A CN 201510748490 A CN201510748490 A CN 201510748490A CN 105289689 A CN105289689 A CN 105289689A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention discloses synthesis of nitrogen-doped graphene quantum dot/similar-graphene phase carbon nitride composite material and research and application of photocatalytic decomposition of aquatic hydrogen performance. A catalyst is composed of a nitrogen-doped graphene quantum dot and similar-graphene phase carbon nitride. Under simulated sunlight, the catalyst can efficiently and stably achieve water photolysis to produce hydrogen. The synthesis and application have the advantages that the catalyst is completely composed of nonmetal elements and has the advantages of being environmentally friendly and low in cost; the light response range of the similar-graphene phase carbon nitride is enlarged due to the doping of the nitrogen-doped graphene quantum dot, and absorption under the visible light is increased; the photosensitization effect and the ultrastrong electron conduction capacity of the nitrogen-doped graphene quantum dot are utilized at the same time, photo-induced electron and hole composition is restrained, and meanwhile the light utilization rate is improved; the raw materials are low in cost and easy to obtain, the synthesis method is simple, the synthesis yield and purity are high, and experimental repeatability is good.
Description
Technical field
The present invention relates to synthesis and the photochemical catalyzing H2-producing capacity investigation and application of a kind of nitrogen-doped graphene quantum dot/class Graphene phase carbon nitride composite.
Background technology
21 century is the epoch that high and new technology develops, and the development of new material, information and biotechnology is the representative of new and high technology.Photocatalysis originates from the TiO of report in 1972
2carry out illumination as electrode material and can produce the report of hydrogen by decomposition water, therefore people start to pay close attention to this technology---photocatalyst.Compare with the method for traditional electrolyte, physics or chemistry, the easy and cheaper starting materials of the method for photocatalysis Decomposition, but catalytic efficiency is relatively low, therefore finds the catalyst that combined coefficient is high, photocatalysis performance is good, become the study hotspot in this field.And the key successfully realizing photochemical catalyzing finds suitable catalyst, most popular is at present semiconductor light-catalyst, but catalytic efficiency is on the low side, for improving the resolution ratio of water further, around the modification of traditional catalyst and the development of new catalyst, numerous research workers have carried out a large amount of research work.
Present stage, the conductor photocatalysis material of people's development can only absorb the ultraviolet light less than 5% in the sun power spectrum only accounting for and arrive at the earth mostly, and solar energy utilization ratio is lower.Therefore, finding also synthesizing efficient, visible light catalytic material that is stable, low cost is the key that decomposing water with solar energy hydrogen manufacturing is studied.
In recent years, the photocatalytic activity with the composite of inorganic non-metallic structure causes the attention of research workers.Research finds, inorganic non-metallic structural semiconductor material has special band structure and carrier transport characteristic, effectively can suppress the compound of photo-generated carrier in light-catalyzed reaction, thus improves quantum efficiency.
Graphite-like structure (lamellar graphite phase) carbonitride (g-C
3n
4) there is the particular semiconductor optical characteristics similar with Graphene, be applied in light-catalyzed reaction as visible light-responded catalyst, but its photocatalytic activity need further raising.Nitrogen-doped graphene quantum dot is as typical conductor photocatalysis material, and it can stablize effective photosensitizer and co-catalyst as one, has and has good auxiliary catalysis effect to photocatalysis Decomposition aquatic products hydrogen, but defect to be photostability slightly poor.Therefore we plan nitrogen-doped graphene quantum dot and class Graphene carbonitride carries out load, thus form the hetero-junctions of nitrogen-doped graphene quantum dot/class Graphene phase carbon nitride, realize effective separation of effective electrical conductivity and photo-generated carrier, improve Photocatalyzed Hydrogen Production efficiency and the stability of material, the catalysis material for light decomposition water provides source and the theoretical foundation of new material.
Summary of the invention
The object of the present invention is to provide a kind of novel photocatalyst and preparation method thereof, providing new material for solving energy problem.Photochemical catalyst of the present invention can split water into hydrogen and transform to the Green Chemistry energy, and this is not only conducive to alleviating energy crisis, simultaneously for environmental improvement provides new thinking.Material preparation manipulation of the present invention is simple, low production cost, synthesis productive rate higher, purity is high and reproducible, is applicable to the requirement that extension is produced.
The present invention is achieved like this, and a kind of nitrogen-doped graphene quantum dot/class Graphene phase carbon nitride composite, is characterized in that: the composite formed on class Graphene phase carbon nitride by the load of nitrogen-doped graphene quantum dot; Under simulated solar irradiation, the photochemical catalyzing that this composite has efficient stable produces hydrogen performance; When the load capacity of nitrogen-doped graphene quantum dot is 15%(mass ratio) time, expression formula is 15%N-GQDs/g-C
3n
4, be reduced to 15N-CNU, the catalytic effect of this material is best, and hydrogen-producing speed can reach 2.39mmol h
-1g
-1, hydrogen-producing speed is than pure g-C
3n
4improve 2.36 times.
The preparation method of photochemical catalyst of the present invention, is characterized in that method step is:
1, the synthesizing of nitrogen-doped graphene quantum dot: get 0.50 ~ 0.60 gram of citric acid and 0.45 ~ 0.65 gram of urea is dissolved in the deionized water of 10 ~ 15 milliliters, join in 50 milliliters of reactors after abundant dissolving, be placed in the air dry oven constant temperature 8 ~ 12 hours of 160 ~ 180 DEG C, be cooled to normal temperature and can obtain finely dispersed nitrogen-doped graphene quantum dot solution.
2, a kind of nitrogen-doped graphene quantum dot/class Graphene carbonitride complex light urges the synthetic method of agent to be:
(1) taking 6.3 ~ 6.8 grams of urea, to join capacity be in the porcelain crucible of 15 milliliters, and put into the Muffle furnace constant temperature 2 ~ 4 hours of 550 DEG C ~ 600 DEG C, obtains flaxen class Graphene phase carbon nitride.
(2) get 1 ~ 3 milliliter of nitrogen-doped graphene quantum dot dispersion liquid in 20 ~ 50 ml deionized water, after ultrasonic, obtain solution A;
(3) getting the class Graphene phase carbon nitride that 0.1 ~ 0.5 gram of step (1) obtains is dissolved in 10 ~ 20 ml waters, ultrasonic 1 ~ 5 hour, then solution A is slowly added, and stirs 15 ~ 20 hours, obtain turbid solution B under normal temperature condition;
(4) then turbid solution B is carried out filtering, washing and drying, obtain final catalyst.
Advantage of the present invention is: 1, catalyst of the present invention is the catalyst be made up of nonmetalloid completely, has the feature of environmental friendliness and low cost.2, the photoresponse scope of class Graphene phase carbon nitride has been expanded in the doping of nitrogen-doped graphene quantum dot, adds absorption under visible light; 3, make use of the optical sensibilization of nitrogen-doped graphene quantum dot and superpower electronic conduction ability simultaneously, not only inhibit the compound in light induced electron and hole, improve the utilization rate of light simultaneously; 4, cheaper starting materials of the present invention is easy to get, and synthetic method is simple, synthetic yield and purity higher, experimental repeatability is good, is applicable to the requirement that extension is produced.
Accompanying drawing explanation
Fig. 1 is g-C
3n
4and with the g-C of load 3%, 5%, 10%, 15%, 20% different proportion nitrogen-doped graphene quantum dot
3n
4x-ray powder diffraction comparison diagram.(in figure, CN-U, 3N-CNU, 5N-CNU, 10N-CNU, 15N-CNU, 20N-CNU represent pure g-C respectively
3n
4and the g-C of the nitrogen-doped graphene quantum dot of load 3%, 5%, 10%, 15%, 20% different proportion
3n
4).
Fig. 2 is the nitrogen-doped graphene quantum dot heterostructures transmission electron microscope picture of load 15%.(in figure, CN-U and 15N-CNU represents pure g-C respectively
3n
4and the g-C of the nitrogen-doped graphene quantum dot of load 15%
3n
4).
Fig. 3 is g-C
3n
4and the infrared spectrum comparison diagram of nitrogen-doped graphene quantum dot heterostructures with load 3%, 5%, 10%, 15%, 20% different proportion.(in figure, CN-U, 3N-CNU, 5N-CNU, 10N-CNU, 15N-CNU, 20N-CNU represent pure g-C respectively
3n
4and the g-C of the nitrogen-doped graphene quantum dot of load 3%, 5%, 10%, 15%, 20% different proportion
3n
4).
Fig. 4 is g-C
3n
4the XPS figure of load 15% nitrogen-doped graphene quantum dot heterostructures.(in figure, CN-U and 15N-CNU represents pure g-C respectively
3n
4and the g-C of load 15% nitrogen-doped graphene quantum dot
3n
4).
Fig. 5 is g-C
3n
4and the UV-Vis DRS figure of nitrogen-doped graphene quantum dot heterostructures with load 3%, 5%, 10%, 15%, 20% different proportion.(in figure, CN-U, 3N-CNU, 5N-CNU, 10N-CNU, 15N-CNU, 20N-CNU represent pure g-C respectively
3n
4and the g-C of the nitrogen-doped graphene quantum dot of load 3%, 5%, 10%, 15%, 20% different proportion
3n
4).
Fig. 6 is g-C
3n
4and the fluorogram of load 15% nitrogen-doped graphene quantum dot heterostructures.(in figure, CN-U and 15N-CNU represents pure g-C respectively
3n
4and the g-C of the nitrogen-doped graphene quantum dot of load 15%
3n
4).
Fig. 7 is g-C
3n
4and the photoelectricity flow graph of load 15% nitrogen-doped graphene quantum dot heterostructures.(in figure, CN-U and 15N-CNU represents pure g-C respectively
3n
4and the g-C of the nitrogen-doped graphene quantum dot of load 15%
3n
4).
Fig. 8 is for being g-C
3n
4and with load 3%, 5%, 10%, 15%, 20% different proportion nitrogen-doped graphene quantum dot heterostructures under the induction of simulated solar irradiation, the design sketch of Photocatalyzed Hydrogen Production.(in figure, CN-U, 3N-CNU, 5N-CNU, 10N-CNU, 15N-CNU, 20N-CNU represent pure g-C respectively
3n
4and the g-C of load 3%, 5%, 10%, 15%, 20% different proportion nitrogen-doped graphene quantum dot
3n
4).
Detailed description of the invention
1. the synthesis of catalyst
(1) preparation of class Graphene phase carbon nitride: take 6.5 grams of urea and join in the porcelain crucible of 15 milliliters, the slight compacting of medication spoon, covers crucible cover.Above-mentioned porcelain crucible is placed in the Muffle furnace constant temperature 2 hours of 550 DEG C, heating rate is 8 DEG C/min, obtains yellow product and is class Graphene phase carbon nitride (g-C
3n
4).
(2) nitrogen-doped graphene quantum dot preparation: get 0.5254 gram of citric acid and 0.6006 gram of urea is dissolved in the deionized water of 12 milliliters, join in the reactor of 50 milliliters after abundant dissolving, be placed in the air dry oven constant temperature 8 hours of 160 DEG C, obtain nitrogen-doped graphene quantum dot solution (N-GQDs).
(3) different loads ratio nitrogen-doped graphene quantum dot/class Graphene phase carbon nitride (N-GQDs/g-C
3n
4) preparation:
I) preparation of 3N-CNU
Take the g-C that step (1) is obtained
3n
40.100 gram, sample is scattered in 10 ml waters, by ultrasonic for its mixed solution 5 minutes, the nitrogen-doped graphene quantum dot solution 0.0754 milliliter that solubility is 0.410 mg/ml can be added subsequently respectively, stirring at normal temperature 15 hours, filtration, washing, drying, obtain the class Graphene carbonitride composite photo-catalyst that nitrogen-doped graphene quantum dot load percentage is 3%, expression formula is 3%N-GQDs/g-C
3n
4, be reduced to 3N-CNU.
Ii) the preparation of 5N-CNU
Take the g-C that step (1) is obtained
3n
40.100 gram, sample is scattered in 10 ml waters, by ultrasonic for its mixed solution 5 minutes, the nitrogen-doped graphene quantum dot solution 0.128 milliliter that solubility is 0.410 mg/ml can be added subsequently respectively, stirring at normal temperature 15 hours, filtration, washing, drying, obtain the class Graphene carbonitride composite photo-catalyst that nitrogen-doped graphene quantum dot load percentage is 5%, expression formula is 5%N-GQDs/g-C
3n
4, be reduced to 5N-CNU.
Iii) the preparation of 10N-CNU
Take the g-C that step (1) is obtained
3n
40.100 gram, sample is scattered in 10 ml waters, by ultrasonic for its mixed solution 5 minutes, the nitrogen-doped graphene quantum dot solution 0.271 milliliter that solubility is 0.410 mg/ml can be added subsequently respectively, stirring at normal temperature 15 hours, filtration, washing, drying, obtain the class Graphene carbonitride composite photo-catalyst that nitrogen-doped graphene quantum dot load percentage is 10%, expression formula is 10%N-GQDs/g-C
3n
4, be reduced to 10N-CNU.
Iv) the preparation of .15N-CNU
Take the g-C that step (1) is obtained
3n
40.100 gram, sample is scattered in 10 ml waters, by ultrasonic for its mixed solution 5 minutes, the nitrogen-doped graphene quantum dot solution 0.0.441 milliliter that solubility is 0.410 mg/ml can be added subsequently respectively, stirring at normal temperature 15 hours, filtration, washing, drying, obtain the class Graphene carbonitride composite photo-catalyst that nitrogen-doped graphene quantum dot load percentage is 15%, expression formula is 15%N-GQDs/g-C
3n
4, be reduced to 15N-CNU.
V) the preparation of .20N-CNU
Take the g-C that step (1) is obtained
3n
40.100 gram, sample is scattered in 10 ml waters, by ultrasonic for its mixed solution 5 minutes, the nitrogen-doped graphene quantum dot solution 0.625 milliliter that solubility is 0.410 mg/ml can be added subsequently respectively, stirring at normal temperature 15 hours, filtration, washing, drying, obtain the class Graphene carbonitride composite photo-catalyst that nitrogen-doped graphene quantum dot load percentage is 20%, expression formula is 20%N-GQDs/g-C
3n
4, be reduced to 20N-CNU.
As shown in Fig. 1-Fig. 7, show through X-ray powder diffraction test result, the nitrogen-doped graphene quantum dot load g-C of different proportion in the present invention
3n
4the diffraction pattern of hetero-junctions and g-C
3n
4completely the same, illustrate that the load of Graphene does not affect g-C
3n
4crystal formation.15% prepared nitrogen-doped graphene quantum dot load g-C is found out from XPS
3n
4the peak of catalyst and g-C
3n
4peak completely the same, although there is no the diffraction peak-to-peak of nitrogen-doped graphene quantum dot in XRD, in XPS figure, there is the characteristic peak of nitrogen-doped graphene quantum dot, illustrated and successfully nitrogen-doped graphene quantum dot has been loaded to g-C
3n
4on.Can find out that the nitrogen-doped graphene quantum dot of 15% is at g-C from transmission electron microscope
3n
4on be uniformly distributed, and particle diameter is between 4-8 nanometer.Can find from UV-Vis DRS spectrogram, after load nitrogen-doped graphene quantum dot amount, material is absorbed with obvious enhancing to visible ray, and its maximum absorption wavelength also there occurs red shift, and this is all conducive to the raising of photocatalysis effect.As can be seen from fluorogram, after doping 15% is nitrogen-doped graphene quantum dot, the photoelectron intensity of catalyst adds twice.As can be seen from photoelectricity flow graph we, photo-current intensity adds three times, and the mixing of surface quantum point can be good at the electric transmission effect improving catalyst.Under an airtight glass light reaction system simulated solar irradiation, when the load capacity of nitrogen-doped graphene quantum dot is 15%, expression formula is 15%N-GQDs/g-C
3n
4, be reduced to 15N-CNU, now the catalytic effect of material is best, and hydrogen-producing speed can reach 2.39mmol h
-1g
-1, hydrogen generation efficiency is than pure g-C
3n
4improve 2.36 times.
The composite catalyst of the class Graphene carbonitride of nitrogen-doped graphene quantum dot of the present invention load is under simulated solar irradiation, there is good product hydrogen effect, achieve the effective combination by photochemical catalytic oxidation and photo catalytic reduction technology, substantially increase the utilization rate of sunshine.Water photocatalysis Decomposition is become hydrogen by catalyst of the present invention, alleviates energy crisis, and provides new approaches for environmental improvement, problem of energy crisis.
Claims (2)
1. nitrogen-doped graphene quantum dot/class Graphene phase carbon nitride composite, is characterized in that: the composite formed on class Graphene phase carbon nitride by the load of nitrogen-doped graphene quantum dot; Under simulated solar irradiation, the photochemical catalyzing that this composite has efficient stable produces hydrogen performance; When the load capacity of nitrogen-doped graphene quantum dot is 15%(mass ratio) time, the catalytic effect of this material is best, and hydrogen-producing speed can reach 2.39mmol h
-1g
-1.
2. a preparation method for a kind of nitrogen-doped graphene quantum dot as claimed in claim 1/class Graphene phase carbon nitride composite, is characterized in that method step is:
(1) taking 6.3 ~ 6.8 grams of urea, to join capacity be in the porcelain crucible of 15 milliliters, and put into the Muffle furnace constant temperature 2 ~ 4 hours of 550 DEG C ~ 600 DEG C, obtains flaxen class Graphene phase carbon nitride;
(2) get 1 ~ 3 milliliter of nitrogen-doped graphene quantum dot dispersion liquid in 20 ~ 50 ml deionized water, after ultrasonic, obtain solution A;
(3) getting the class Graphene phase carbon nitride that 0.1 ~ 0.5 gram of step (1) obtains is dissolved in 10 ~ 20 ml waters, ultrasonic 1 ~ 5 hour, then solution A is slowly added, and stirs 15 ~ 20 hours, obtain turbid solution B under normal temperature condition;
(4) then turbid solution B is carried out filtering, washing and drying, obtain final catalyst.
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| CN105964286A (en) * | 2016-05-18 | 2016-09-28 | 江苏理工学院 | Nitrogen-doped graphene quantum dot and graphite-phase carbon nitride composite photocatalyst and preparation method thereof |
| CN106475127A (en) * | 2016-08-30 | 2017-03-08 | 武汉理工大学 | A kind of nitrogen-doped graphene quantum dot/mesopore titania photocatalyst and preparation method thereof |
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