CN106185846A - The preparation method of graphite phase carbon nitride nanometer sheet, nano belt and quantum dot - Google Patents
The preparation method of graphite phase carbon nitride nanometer sheet, nano belt and quantum dot Download PDFInfo
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- CN106185846A CN106185846A CN201510232437.2A CN201510232437A CN106185846A CN 106185846 A CN106185846 A CN 106185846A CN 201510232437 A CN201510232437 A CN 201510232437A CN 106185846 A CN106185846 A CN 106185846A
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Abstract
The invention provides a kind of graphite phase carbon nitride nanometer sheet, nano belt and the preparation method of quantum dot.Described graphite phase carbon nitride nanometer sheet, nano belt and quantum dot can pass sequentially through following step and prepare: provides body phase graphite phase carbon nitride；Described body phase graphite phase carbon nitride is carried out heat treated so that described body phase graphite phase carbon nitride is peeled off thinning, obtains graphite phase carbon nitride nanometer sheet；Described graphite phase carbon nitride nanometer sheet concentrated acid is processed, destroys the C-N key connecting triazine ring network structure so that described graphite phase carbon nitride nanometer sheet is directivity fracture, obtains graphite phase carbon nitride nano belt；Described graphite phase carbon nitride nano belt is used hydrothermal treatment consists, makes the cutting of described graphite phase carbon nitride nano belt obtain particle diameter quantum dot within 10nm, and the described hydrothermal treatment consists reduction oxidized group of part.
Description
Technical field
The present invention is the preparation about nanometer sheet, nano belt and quantum dot, particularly relates to graphite phase carbon nitride and receives
Rice sheet, nano belt and the preparation method of quantum dot.
Background technology
Graphite phase carbon nitride (g-C3N4) there is the electronic structure of uniqueness and excellent chemical stability, make in recent years
It is widely used in photochemical catalyzing, degradable organic pollutant, organo-functional group for non-metal optical catalyst
The directions such as selectivity conversion, environment disinfected sterilization, gradually cause the pass of people at the energy and material association area
Note.
Optical, electrical and catalytic performance that quantum dot is special owing to its quantum size effect presents and photocatalysis,
The fields such as luminescence generated by light, phosphor, sensor have wide practical use.Such as in photocatalysis field, carbon
Quantum dot and graphene quantum dot apply the absorption model at Photocatalytic enhancement light because it has upper conversion performance
Enclose.Graphite phase carbon nitride has the structure similar with Graphene, will be prepared as having biocompatibility and optics
The quantum dot of performance, is expected to be applied to prepare biological fluorescent labeling, biosensor and environmental photocatlytsis.Cause
This, a kind of graphite phase carbon nitride nanometer sheet of research and development, nano belt and then obtain graphite phase carbon nitride quantum dot and show
Obtain particularly important.
Summary of the invention
It is an object of the invention to provide a kind of graphite phase carbon nitride nanometer sheet, nano belt and the preparation of quantum dot
Method, it is desirable to provide particle diameter is little, yield is high and the graphite phase carbon nitride nanometer sheet of good dispersion, nano belt
And quanta point material.
The present invention is achieved in that the preparation method of a kind of graphite phase carbon nitride nanometer sheet, including following step
Rapid:
Body phase graphite phase carbon nitride is provided；
Described body phase graphite phase carbon nitride is carried out heat treated so that described body phase graphite phase carbon nitride is peeled off
Thinning, obtain graphite phase carbon nitride nanometer sheet.
And, the preparation method of a kind of graphite phase carbon nitride nano belt, comprise the following steps:
Body graphite phase carbon nitride nanometer sheet is provided；
Described graphite phase carbon nitride nanometer sheet concentrated acid is processed, destroys the C-N connecting triazine ring network structure
Key so that described graphite phase carbon nitride nanometer sheet is directivity fracture, obtains graphite phase carbon nitride nano belt.
And, the preparation method of a kind of graphite phase carbon nitride quantum dot, comprise the following steps:
Graphite phase carbon nitride nano belt is provided；
Described graphite phase carbon nitride nano belt is used hydrothermal treatment consists, makes described graphite phase carbon nitride nano belt cut
Cut the quantum dot obtaining particle diameter within 10nm, and the described hydrothermal treatment consists reduction oxidized group of part.
The preparation method of graphite phase carbon nitride nanometer sheet, nano belt and quantum dot that the present invention provides,
The method utilizing heat treatment, chemical attack and hydro-thermal to combine first obtains a kind of graphite phase carbon nitride
Quantum dot, prepared quantum dot mean diameter is 6.7nm, yield height and good dispersion；
Graphite phase carbon nitride quantum dot prepared by the present invention has upper conversion performance, is expected to be applied to photocatalysis body
System strengthens the absorption region of light, thus strengthens the photocatalytic activity of system further, can be applicable to preparation biology
Fluorescent probe, biosensor and environmental photocatlytsis；
Quantum dot prepared by the present invention has stronger fluorescence property, can as fluorescent material for biological medicine,
Optical storage, field of electronic devices；
Preparation method of the present invention is simple, quick, optionally obtains graphite phase carbon nitride nanometer sheet, nanometer
Band and quantum dot, expanded the range of application of the method significantly.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of the graphite phase carbon nitride body phase material that the embodiment of the present invention 1 prepares；
Fig. 2 is the transmission electron microscope picture of the graphite phase carbon nitride nanometer sheet that the embodiment of the present invention 1 prepares；
Fig. 3 is the transmission electron microscope picture of the graphite phase carbon nitride nano belt that the embodiment of the present invention 2 prepares；
Fig. 4 is the transmission electron microscope picture of the graphite phase carbon nitride quantum dot that the embodiment of the present invention 3 prepares；
Fig. 5 is the high-resolution-ration transmission electric-lens of the single graphite phase carbon nitride quantum dot that the embodiment of the present invention 3 prepares
Figure；
Fig. 6 is the fluorescence spectrum figure of the graphite phase carbon nitride quantum dot that the embodiment of the present invention 3 prepares；
Fig. 7 is the up-conversion fluorescence spectrogram of the graphite phase carbon nitride quantum dot that the embodiment of the present invention 3 prepares.
Detailed description of the invention
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearer, with
Lower combination drawings and Examples, are further elaborated to the present invention.Should be appreciated that described herein
Specific embodiment only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide the preparation method of a kind of graphite phase carbon nitride nanometer sheet, comprise the following steps:
S01., body phase graphite phase carbon nitride is provided；
S02. described body phase graphite phase carbon nitride is carried out heat treated so that described body phase graphite phase carbon nitride
Peel off thinning, obtain graphite phase carbon nitride nanometer sheet.
Concrete, in above-mentioned steps S01, described body phase graphite phase carbon nitride preferably with cyanamide, cyanamid dimerization,
Tripolycyanamide, carbamide or thiourea, as raw material, obtain through Overheating Treatment calcining, the described body phase graphite obtained
Phase carbon nitride is the irregular three-dimensional block materials with layer structure.Wherein, the calcining of described heat treatment is excellent
Choosing is with programming rate 4-6 DEG C/min heated at constant temperature 1.5-2.5 hour at 500-600 DEG C, further, institute
State heat treatment to calcine preferably with 5 DEG C/min of programming rate heated at constant temperature 2 hours at 550 DEG C.
Described body phase graphite layers is with hydrogen bonded, can destroy hydrogen bond by heat treatment.Therefore by control
Temperature processed to the body phase graphite phase carbon nitride calcining obtained, can make its phased separation thinning, obtain further
Graphite phase carbon nitride nanometer sheet, its thickness is 2～3nm.As the presently preferred embodiments, in above-mentioned steps S02,
Described heat treated is 450-550 DEG C of heated at constant temperature 1.5-2.5 hour with programming rate 1.8-2.5 DEG C/min；
Further, described heat treated is preferably with 2 DEG C/min of programming rate 500 DEG C of heated at constant temperature 2 hours.
And, embodiments provide the preparation method of a kind of graphite phase carbon nitride nano belt, including with
Lower step:
Q01., graphite phase carbon nitride nanometer sheet is provided；
Q02. described graphite phase carbon nitride nanometer sheet concentrated acid is processed, destroy and connect triazine ring network structure
C-N key so that described graphite phase carbon nitride nanometer sheet is directivity fracture, obtains graphite phase carbon nitride nanometer
Band.
Concrete, in embodiment of the present invention above-mentioned steps Q01, described graphite phase carbon nitride nanometer sheet can be led to
The method crossing above-mentioned preparation graphite phase carbon nitride nanometer sheet obtains.Of course it is to be understood that other approach obtain
Described graphite phase carbon nitride nanometer sheet also can prepare graphite phase carbon nitride nano belt as the embodiment of the present invention
Raw material.
In above-mentioned steps Q02, described graphite phase carbon nitride nanometer sheet concentrated acid is processed, connection can be destroyed
The C-N key of triazine ring network structure, so that graphite phase carbon nitride nanometer sheet is the fracture of directivity, is formed
Nano belt.The concrete optional dense HNO of described concentrated acid3With dense H2SO4Mixed acid.As the presently preferred embodiments,
The width of described graphite phase carbon nitride nano belt is within 10nm.
The embodiment of the present invention additionally provides the preparation method of a kind of graphite phase carbon nitride quantum dot, including following step
Rapid:
T01., graphite phase carbon nitride nano belt is provided；
T02. described graphite phase carbon nitride nano belt is used hydrothermal treatment consists, make described graphite phase carbon nitride nanometer
Band cutting obtains particle diameter quantum dot within 10nm, and the described hydrothermal treatment consists reduction oxidized group of part.
Concrete, in embodiment of the present invention above-mentioned steps T01, described graphite phase carbon nitride nano belt can be led to
The method crossing above-mentioned preparation graphite phase carbon nitride nano belt obtains.Of course it is to be understood that other approach obtain
Described graphite phase carbon nitride nano belt also can prepare graphite phase carbon nitride quantum dot as the embodiment of the present invention
Raw material.
As the presently preferred embodiments, the width of described graphite phase carbon nitride nano belt is within 10nm.
In above-mentioned steps T02, as the presently preferred embodiments, the reaction temperature of described hydrothermal treatment consists is 180-220 DEG C,
Response time is 8-12 hour.As particular preferred embodiment, the reaction temperature of described hydrothermal treatment consists is
200 DEG C, the response time is 10 hours.
The preparation method of graphite phase carbon nitride nanometer sheet, nano belt and quantum dot that the embodiment of the present invention provides,
Utilize heat treatment, chemical attack and hydro-thermal to combine first, be former with graphite phase carbon nitride body phase material
Material, is directly peeled off as two-dimensional nano sheet, 1-dimention nano band, is finally obtained zero-dimensional quantum dots, prepared
Quantum point grain diameter homogeneous, mean diameter is 6.7nm, yield is high, good dispersion and water solublity high, it is molten
Liquid ambient temperatare is put 1 year and is had no that precipitation produces, and has the highest stability；
Meanwhile, graphite phase carbon nitride quantum dot prepared by the embodiment of the present invention has upper conversion performance, and being expected to should
Strengthen the absorption region of light for photocatalysis system, thus strengthen the photocatalytic activity of system further, can answer
For preparing biological fluorescent labeling, biosensor and environmental photocatlytsis；
Quantum dot prepared by the embodiment of the present invention has stronger fluorescence property, can be used for giving birth to as fluorescent material
Thing medicine, optical storage, field of electronic devices；
Preparation method of the present invention is simple, quick, optionally obtains graphite phase carbon nitride nanometer sheet, nanometer
Band and quantum dot, expanded the range of application of the method significantly.
Below by specific embodiment, the present invention is described further.
Embodiment 1
5g thiourea is placed in crucible, in 550 DEG C of heated at constant temperature 2 hours (5 DEG C/min of programming rate), treats
After temperature cooling, sample is ground to form yellow powder, obtains graphite phase carbon nitride body phase material.After grinding
Body phase graphite phase carbon nitride be placed in the flat crucible of opening, with 2 DEG C/min of programming rate at 500 DEG C of constant temperature
Heat 2 hours, obtain faint yellow graphite phase carbon nitride nanometer sheet ultra-thin materials.Fig. 1 is prepared graphite-phase
The transmission electron microscope picture of carbonitride body phase material, shows irregular block structure.Fig. 2 is the graphite-phase obtained
The transmission electron microscope picture of azotized carbon nano sheet, illustrating that body phase graphite phase carbon nitride is successfully peeled off by heat treatment is
Nanometer sheet.
Embodiment 2
The graphite phase carbon nitride nanometer sheet obtained by 0.05g adds dense H2SO4(10mL) with dense HNO3(30
ML), in, then mixture is placed in ultrasonic machine with ultrasonic 16 hours of smaller power (500W, 40kHz),
Obtain the solution of a kind of clarification, obtain a kind of cotton-shaped suspended after this solution is diluted with 200mL deionized water
Liquid, more i.e. obtain graphite phase carbon nitride nano belt after the washing of this suspension 0.45-μm micro-pore-film filtration.
Fig. 3 is the transmission electron microscope picture of prepared graphite phase carbon nitride nano belt.
Embodiment 3
Graphite phase carbon nitride nano belt obtained above is scattered in 16mL deionized water again, then seals
It is contained in politef hydrothermal reaction kettle (20mL), is placed in baking oven and carries out hydro-thermal reaction (200 DEG C, 10 is little
Time), i.e. obtain graphite phase carbon nitride quantum dot solution.Fig. 4 is the saturating of prepared graphite phase carbon nitride quantum dot
Radio mirror figure, its mean diameter is 6.7nm.Fig. 5 is the high-resolution-ration transmission electric-lens figure of single quantum dot, card
Its spacing of lattice real is 0.336nm, matches with body phase graphite phase carbon nitride material (002) crystal face.Fig. 6 and
The fluorescence spectrum figure of the graphite phase carbon nitride quantum dot that Fig. 7 respectively prepares and upconversion emission figure, wherein,
In Fig. 6, excitation wavelength is respectively as follows: 340nm, 360nm, 380nm, 400nm, 420nm from left to right；
In Fig. 7, from left to right excitation wavelength be respectively as follows: 705nm, 725nm, 750nm, 778nm, 800nm,
853nm、862nm；Fig. 6 and Fig. 7 confirms that this quantum dot has stronger blue fluorescent emissions performance, and
And it is found that on it, dress changes optical property first.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all at this
Any amendment, equivalent and the improvement etc. made within bright spirit and principle, should be included in the present invention
Protection domain within.
Claims (10)
1. a preparation method for graphite phase carbon nitride nanometer sheet, comprises the following steps:
Body phase graphite phase carbon nitride is provided；
Described body phase graphite phase carbon nitride is carried out heat treated so that described body phase graphite phase carbon nitride is peeled off
Thinning, obtain graphite phase carbon nitride nanometer sheet.
2. the preparation method of graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that institute
The thickness stating graphite phase carbon nitride nanometer sheet is 2-3nm.
3. the preparation method of graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that institute
State body phase graphite phase carbon nitride using cyanamide, cyanamid dimerization, tripolycyanamide, carbamide or thiourea as raw material, warp
Overheating Treatment calcining obtains.
4. the preparation method of graphite phase carbon nitride nanometer sheet as claimed in claim 1, it is characterised in that institute
Stating heat treated is 450-550 DEG C of heated at constant temperature 1.5-2.5 hour with programming rate 1.8-2.5 DEG C/min.
5. the preparation method of graphite phase carbon nitride nanometer sheet as claimed in claim 4, it is characterised in that institute
State heat treated for 2 DEG C/min of programming rate 500 DEG C of heated at constant temperature 2 hours.
6. a preparation method for graphite phase carbon nitride nano belt, comprises the following steps:
Graphite phase carbon nitride nanometer sheet is provided；
Described graphite phase carbon nitride nanometer sheet concentrated acid is processed, destroys the C-N connecting triazine ring network structure
Key so that described graphite phase carbon nitride nanometer sheet is directivity fracture, obtains graphite phase carbon nitride nano belt.
7. the preparation method of graphite phase carbon nitride nano belt as claimed in claim 6, it is characterised in that institute
State the width of nano belt within 10nm.
8. a preparation method for graphite phase carbon nitride quantum dot, comprises the following steps:
Body graphite phase carbon nitride nano belt is provided；
Described graphite phase carbon nitride nano belt is used hydrothermal treatment consists, makes described graphite phase carbon nitride nano belt cut
Cut the quantum dot obtaining particle diameter within 10nm, and the described hydrothermal treatment consists reduction oxidized group of part.
9. the preparation method of graphite phase carbon nitride quantum dot as claimed in claim 8, it is characterised in that institute
The reaction temperature stating hydrothermal treatment consists is 180-220 DEG C, and the response time is 8-12 hour.
10. the preparation method of graphite phase carbon nitride quantum dot as claimed in claim 9, it is characterised in that
The reaction temperature of described hydrothermal treatment consists is 200 DEG C, and the response time is 10 hours.
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| CN106622331A (en) * | 2017-01-06 | 2017-05-10 | 广西民族大学 | Preparation method of high-specific-surface-area graphite phase carbon nitride photocatalyst |
| CN106669760A (en) * | 2016-12-28 | 2017-05-17 | 广州中国科学院沈阳自动化研究所分所 | Sulfur-doped carbon nitride photocatalyst as well as preparation method and application thereof |
| CN107744824A (en) * | 2017-04-19 | 2018-03-02 | 华中科技大学 | A kind of g C of modification3N4Base visible-light photocatalyst, its preparation method and application |
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| CN115159478B (en) * | 2022-06-17 | 2023-09-08 | 河海大学 | Method for preparing ultrathin porous graphite phase carbon nitride nanosheets in large scale |
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Application publication date: 20161207 |