CN107043222A - The preparation method of phosphorus doping graphite phase carbon nitride nano thin-film - Google Patents
The preparation method of phosphorus doping graphite phase carbon nitride nano thin-film Download PDFInfo
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- CN107043222A CN107043222A CN201710042164.4A CN201710042164A CN107043222A CN 107043222 A CN107043222 A CN 107043222A CN 201710042164 A CN201710042164 A CN 201710042164A CN 107043222 A CN107043222 A CN 107043222A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
- C03C17/3429—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating
- C03C17/3435—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials at least one of the coatings being a non-oxide coating comprising a nitride, oxynitride, boronitride or carbonitride
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- C03C2217/00—Coatings on glass
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- C03C2217/211—SnO2
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- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
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- C03C2217/24—Doped oxides
- C03C2217/241—Doped oxides with halides
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- C03C2217/00—Coatings on glass
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- C03C2218/10—Deposition methods
- C03C2218/17—Deposition methods from a solid phase
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Abstract
The invention discloses a kind of preparation method of the graphite phase carbon nitride nano thin-film of phosphorus doping, belong to semiconductor nano material preparing technical field.First by high molecular polymer 2,4 diaminourea 1,3,5 triazines and cyanuric acid hybrid reaction prepare the presoma of graphite phase carbon nitride, then the presoma is placed in FTO glass surfaces by the method for high-temperature calcination and prepares carbon nitride films, finally carbon nitride films are placed in magnetic boat, the graphite phase carbon nitride nano thin-film for obtaining phosphorus doping is calcined under nitrogen atmosphere using sodium hypophosphite as phosphorus source.The inventive method is using FTO electro-conductive glass as base material, and preparation process is simple, with low cost；Obtained phosphorus doping graphite phase carbon nitride nano thin-film form is good, purity is high, and overcomes the shortcoming of phosphorus doping graphite phase carbon nitride nano-powder material bad dispersibility, and photocatalytic activity is high；Generation without poisonous and harmful substances in whole preparation process, will not pollute to environment, will not also be detrimental to health, safety and environmental protection.
Description
Technical field
The invention belongs to semiconductor nano material preparing technical field, and in particular to a kind of phosphorus doping graphite phase carbon nitride is received
The preparation method of rice film.
Background technology
Graphite phase carbon nitride (C3N4) as a kind of ancient polymer, with density is low, chemical stability is high, biological simultaneous
The advantages of capacitive is good, wearability is strong, in high-performance abrasion-proof coating, membrane material, catalyst and catalyst carrier, metal nitride
The fields such as preparation have broad application prospects, and get more and more people's extensive concerning for a long time.C3N4It is that a kind of energy gap is
2.7 eV n-type semiconductor, is also a kind of good light-sensitive material, has very strong absworption peak at 460nm, and have
Good fluorescent characteristic.With nonmetalloid phosphorus to C3N4Its modified maximum absorption band there occurs obvious blue-shifted phenomenon, utilize
This blue-shifted phenomenon can be designed has the composite fully absorbed to visible ray.It is used as photochemical catalyst, the C of phosphorus doping3N4It is right
The organic dyestuff such as rhodamine have good photocatalytic Degradation.Meanwhile, nano level C3N4Due to by small-size effect,
The influence of macro quanta tunnel effect, skin effect, bulk effect etc., in terms of light absorbs, thermal resistance, fusing point, chemism
Special physical and chemical performance is shown, makes its application field more extensive：For example, showing high catalysis as catalysis material
Activity；As light-sensitive material application on a sensor；It can also be applied in terms of thermal conducting material and superconductor.
Preparation of the preparation method for the phosphorus doping graphite phase carbon nitride reported at present primarily directed to its powder.As authorized
Notification number discloses a kind of phosphorus doping graphite phase carbon nitride visible light catalyst for the B of CN 103769213 Chinese invention patent
Preparation method, by the way that melamine is scattered in dilute phosphoric acid solution, phosphoric acid molecules uniform adsorption is dispersed in melamine
Microparticle surfaces, then heating removes aqueous solvent, melamine is occurred pyrocondensation to 520 DEG C through temperature programming after abundant dry
Poly- reaction, product obtains phosphorus doping graphite phase carbon nitride visible light catalyst through cooling, grinding.Qing Han etc. provide one
Plant preparation method (the Qing Han.Phosphorus-Doped Carbon of the azotized carbon nano dusty material of phosphorus doping
Nitride Tubes with a Layered Micronanostructure for Enhanced Visible-Light
Photocatalytic Hydrogen Evolution. Angew. Chem. 2016,128,1862-1866), this method
It is that the aqueous solution stirring of melamine as the presoma and phosphoric acid of graphite phase carbon nitride is mixed finally to be placed in polytetrafluoroethyl-ne
In alkene reaction kettle, at 180 DEG C or more than 190 DEG C at a temperature of directly react 10 hours, then the reaction product is centrifuged, wash,
And under conditions of 60-80 DEG C dry, finally by the desciccate in tube furnace nitrogen protection under 500 DEG C, high temperature burn 4h, most
The graphite phase carbon nitride nanometer powder composite of phosphorus doping is obtained afterwards.But above method one side preparation process is complicated, time-consuming
Long, cost is higher, and on the other hand its powder body material water solubility prepared is bad, disperses uneven, can cause to urge during use
Change performance degradation.
The content of the invention
It is an object of the invention to provide a kind of simple, the with low cost phosphorus doping graphite phase carbon nitride nanometer thin of preparation process
The preparation method of film, to obtain good form, purity and the high phosphorus doping graphite phase carbon nitride nano thin-film of catalytic performance.
The purpose of the present invention is realized in the following way：First by high molecular polymer 2,4- diaminostilbenes, 3,5- tri-
Piperazine and cyanuric acid hybrid reaction prepare graphite phase carbon nitride presoma, and the presoma then is placed in into FTO glass surface high temperature
The method of calcining prepares graphite phase carbon nitride film, finally the graphite phase carbon nitride film is placed in magnetic boat, with ortho phosphorous acid
Sodium is calcined under nitrogen protection as phosphorus source obtains phosphorus doping graphite phase carbon nitride nano thin-film.Specifically include following steps：
（1）By high molecular polymer 2,4- diaminostilbenes, 3,5- triazines and cyanuric acid are dissolved in distilled water and concentration point are made
Not Wei 45mg/mL and 32.5mg/mL mixed solution, at room temperature stir 12-24h after suction filtration, filter residue at 60-80 DEG C dry
After obtain graphite phase carbon nitride presoma, grind standby；
（2）Clean FTO glass conduction is placed in crucible up, step is weighed（1）In graphite phase carbon nitride presoma
Powder is laid on FTO glass, calcines 4-5h in 500-550 DEG C under nitrogen protection, and 2.3-2.5 DEG C of heating rate/min is obtained
To the graphite phase carbon nitride film of yellow；
（3）By step（2）In graphite phase carbon nitride film it is ultrasonic together with FTO glass, remove surface impurity after be placed in magnetic
In boat；Sodium hypophosphite is placed in another magnetic boat as phosphorus source, and two magnetic boats are placed in into tube furnace 300-350 under nitrogen protection
1-2h is calcined at DEG C, 2.0-2.5 DEG C of heating rate/min takes out sample after tube furnace naturally cools to room temperature, with ethanol and
Distilled water flushing, drying obtain phosphorus doping graphite phase carbon nitride nano thin-film.
Above-mentioned steps（2）The amount of weighing of middle graphite phase carbon nitride precursor powder is controlled in 1.0-1.3g, sodium hypophosphite
Addition be 0.5-1g, to obtain, thickness is suitable, phosphorus doping graphite phase carbon nitride nano thin-film of good performance.
In order that the phosphorus doping reaction of graphite phase carbon nitride phosphorus film obtains optimal effect, it is of the invention by step（3）In
The magnetic boat for filling sodium hypophosphite is placed in tube furnace high-temperature region, and the magnetic boat for filling graphite phase carbon nitride film sample is placed in tube furnace
Downstream, and the distance of two magnetic boats is controlled for 7-8cm.
Relative to prior art, the invention has the advantages that：
（1）The present invention uses 2,4- diamino-1,3,5-triazines and cyanuric acid to prepare graphite phase carbon nitride presoma, through high temperature
Complete homogeneous graphite phase carbon nitride nano thin-film can be formed after calcining, cyanuric acid is solved as cannot be complete during presoma
The technical barrier of whole homogeneous graphite phase carbon nitride nano thin-film, and using sodium hypophosphite as phosphorus source, preferably to control phosphorus
Incorporation, make operation more easy.
（2）The inventive method is using FTO electro-conductive glass as base material, and preparation process is simple, with low cost；Obtained phosphorus is mixed
Miscellaneous graphite phase carbon nitride nano thin-film form is good, purity is high, and overcomes phosphorus doping graphite phase carbon nitride nano-powder material point
The shortcoming of property difference is dissipated, photocatalytic activity is high.
（3）Generation without poisonous and harmful substances in whole preparation process, will not pollute to environment, will not also endanger
Health.
Brief description of the drawings
Fig. 1 is the SEM figures of the graphite phase carbon nitride nano thin-film prepared using method in the embodiment of the present invention 1.
Fig. 2 is the SEM figures of the phosphorus doping graphite phase carbon nitride nano thin-film prepared using method in the embodiment of the present invention 1.
Fig. 3 is the graphite phase carbon nitride nano thin-film and phosphorus doping graphite-phase prepared using method in the embodiment of the present invention 1
The density of photocurrent figure of nano carbon nitride film.
Fig. 4 is the XRD spectrums of the phosphorus doping graphite phase carbon nitride nano thin-film prepared using method in the embodiment of the present invention 1
Figure.
Embodiment
For a better understanding of the present invention, the invention will be further described with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The preparation method of phosphorus doping graphite phase carbon nitride nano thin-film, comprises the following steps：
（1）Weigh 9g 2,4- diaminostilbenes, 3,5- triazines and 6.5g cyanuric acid solid powder are dissolved in 200mL distilled water
In, suction filtration after 18h is stirred at room temperature, and filter residue obtains graphite phase carbon nitride presoma after being dried at 80 DEG C, grinds standby；Take
Several pieces are placed in beaker 1.5 × 2.5 FTO glass, are respectively rinsed after 30min and to be dried up with nitrogen with running water, ethanol and distilled water,
It is standby；
（2）Clean FTO glass conduction is placed in crucible up, 1.3g steps are weighed（1）In graphite phase carbon nitride before
Drive body powder to be laid on FTO glass, calcine 4h, 2.3 DEG C/min of heating rate in 500 DEG C under nitrogen protection, obtain yellow
Graphite phase carbon nitride film；
（3）By step（2）In graphite phase carbon nitride film it is together ultrasonic together with FTO glass, be placed in and put after removing surface impurity
Put in the magnetic boat in tube furnace downstream；1g sodium hypophosphites are placed in another magnetic boat for being placed on tube furnace high-temperature region as phosphorus source
In, two magnetic boats are at a distance of 7cm；Two magnetic boats are placed at 300 DEG C of tube furnace under nitrogen protection and calcine 1h, 2.0 DEG C of heating rate/
Min, sample is taken out after tube furnace naturally cools to room temperature, and the graphite of phosphorus doping is obtained with ethanol and distilled water flushing, drying
Phase carbon nitride nano thin-film.
To above-mentioned steps（2）In obtained graphite phase carbon nitride film and step（3）In obtained phosphorus doping graphite-phase nitrogen
Change C film and carry out SEM Morphological Characterizations respectively, as a result as shown in Figure 1 and Figure 2.As can be seen from Figure 1, graphite phase carbon nitride film
Uniform macroreticular structure is showed, and after phosphorating treatment, the network structure of graphite phase carbon nitride film is covered by phosphorus,
Narrow and small and sparse, the favorable dispersibility that hole becomes, and the generation of soilless sticking phenomenon（Fig. 2）.Illustrate that this method is successfully prepared phosphorus doping
Graphite phase carbon nitride nano thin-film.
With CHI660 electrochemical workstations, using three-electrode system, to graphite phase carbon nitride film and phosphorus doping graphite
Phase carbon nitride film carries out LSV tests respectively, is respectively working electrode with the two, and Pt is that SCE is reference electrode to electrode；Electricity
The NaOH solution that liquid is 1mol/L is solved, potential window is -1V-1V, and test result is as shown in Figure 3.It can be seen that graphite
Phase carbon nitride shows very small photocurrent response, about 0.005mA/cm2, and P elements doping after photocurrent response
It is significantly improved, about 0.01mA/cm2（Relative to current density of the reversible hydrogen electrode potential in 1.23V）, with compared with
Good photoelectric response characteristic, photocatalytic activity is high.
Fig. 4 is the XRD spectra of phosphorus doping graphite phase carbon nitride nano thin-film, from the figure, it can be seen that the nano thin-film exists
27.5 ° have a very strong diffraction maximum, and this is consistent with the diffraction maximum of graphite phase carbon nitride, and go out without other diffraction maximums
It is existing, show that the present embodiment method is prepared for purity very high phosphorus doping graphite phase carbon nitride nano thin-film.
Embodiment 2
The preparation method of phosphorus doping graphite phase carbon nitride nano thin-film, comprises the following steps：
（1）Weigh 4.5g 2,4- diaminostilbenes, 3,5- triazines and 3.25g cyanuric acid solid powder are dissolved in 100mL distillations
In water, suction filtration after 18h is stirred at room temperature, and filter residue obtains graphite phase carbon nitride presoma after being dried under conditions of 70 DEG C, ground
Mill is standby；Using with implementing 1 step（1）In same method cleaning FTO glass it is standby；
（2）Clean FTO glass conduction is placed in crucible up, 1.2g steps are weighed（1）In graphite phase carbon nitride before
Drive body powder to be laid on FTO glass, calcine 4h, 2.4 DEG C/min of heating rate in 520 DEG C under nitrogen protection, obtain yellow
Graphite phase carbon nitride film；
（3）By step（2）In graphite phase carbon nitride film it is together ultrasonic together with FTO glass, be placed in and put after removing surface impurity
Put in the magnetic boat in tube furnace downstream；0.8g sodium hypophosphites are placed in another magnetic for being placed on tube furnace high-temperature region as phosphorus source
In boat, two magnetic boats are at a distance of 7cm；Two magnetic boats are placed at 325 DEG C of tube furnace under nitrogen protection and calcine 1.5h, heating rate 2.2
DEG C/min, sample is taken out after tube furnace naturally cools to room temperature, the stone of phosphorus doping is obtained with ethanol and distilled water flushing, drying
Black phase carbon nitride nano thin-film.
Embodiment 3
The preparation method of phosphorus doping graphite phase carbon nitride nano thin-film, comprises the following steps：
（1）Weigh 13.5g 2,4- diaminostilbenes, 3,5- triazines and 9.75g cyanuric acid solid powder are dissolved in 300mL distillations
In water, suction filtration after 24h is stirred at room temperature, and filter residue obtains graphite phase carbon nitride presoma after being dried under conditions of 60 DEG C, ground
Mill is standby；Take 1.5 × 2.5 FTO glass several pieces be placed in beaker, respectively rinsed after 30min and used with running water, ethanol and distilled water
Nitrogen is dried up, standby；Using with implementing 1 step（1）In same method cleaning FTO glass it is standby；
（2）Clean FTO glass conduction is placed in crucible up, 1.0g steps are weighed（1）In graphite phase carbon nitride before
Drive body powder to be laid on FTO glass, calcine 4h, 2.5 DEG C/min of heating rate in 550 DEG C under nitrogen protection, obtain yellow
Graphite phase carbon nitride film；
（3）By step（2）In graphite phase carbon nitride film it is together ultrasonic together with FTO glass, be placed in and put after removing surface impurity
Put in the magnetic boat in tube furnace downstream；0.5g sodium hypophosphites are placed in another magnetic for being placed on tube furnace high-temperature region as phosphorus source
In boat, two magnetic boats are at a distance of 8cm；Two magnetic boats are placed at 350 DEG C of tube furnace under nitrogen protection and calcine 2h, 2.5 DEG C of heating rate/
Min, sample is taken out after tube furnace naturally cools to room temperature, and the graphite of phosphorus doping is obtained with ethanol and distilled water flushing, drying
Phase carbon nitride nano thin-film.
Claims (4)
1. the preparation method of phosphorus doping graphite phase carbon nitride nano thin-film, it is characterised in that comprise the following steps：
（1）By high molecular polymer 2,4- diaminostilbenes, 3,5- triazines and cyanuric acid are dissolved in distilled water and concentration point are made
Not Wei 45mg/mL and 32.5mg/mL mixed solution, at room temperature stir 12-24h after suction filtration, filter residue at 60-80 DEG C dry
After obtain graphite phase carbon nitride presoma, grind standby；
（2）Clean FTO glass conduction is placed in crucible up, step is weighed（1）In graphite phase carbon nitride presoma
Powder is laid on FTO glass, calcines 4-5h in 500-550 DEG C under nitrogen protection, and 2.3-2.5 DEG C of heating rate/min is obtained
To the graphite phase carbon nitride film of yellow；
（3）By step（2）In graphite phase carbon nitride film it is ultrasonic together with FTO glass, remove surface impurity after be placed in magnetic
In boat；Sodium hypophosphite is placed in another magnetic boat as phosphorus source, and two magnetic boats are placed in into tube furnace 300-350 under nitrogen protection
1-2h is calcined at DEG C, 2.0-2.5 DEG C of heating rate/min takes out sample after tube furnace naturally cools to room temperature, with ethanol and
Distilled water flushing, drying obtain phosphorus doping graphite phase carbon nitride nano thin-film.
2. the preparation method of phosphorus doping graphite phase carbon nitride nano thin-film according to claim 1, it is characterised in that：Step
（2）Described in graphite phase carbon nitride precursor powder the amount of weighing be 1.0-1.3g.
3. the preparation method of phosphorus doping graphite phase carbon nitride nano thin-film according to claim 2 is characterized in that：Step
（3）Described in sodium hypophosphite amount be 0.5-1g.
4. the preparation method of phosphorus doping graphite phase carbon nitride nano thin-film according to claim 1, it is characterised in that：Step
（3）Described in fill sodium hypophosphite magnetic boat be located at tube furnace high-temperature region, fill the magnetic boat of graphite phase carbon nitride film sample
Positioned at tube furnace downstream, two magnetic boats are at a distance of 7-8cm.
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Cited By (11)
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| CN108408700A (en) * | 2018-04-04 | 2018-08-17 | 南京工业大学 | A kind of method that non-solvent in-situ carburization prepares blue-fluorescence carbon nitrogen nanometer sheet on a large scale |
| CN108435229A (en) * | 2018-04-25 | 2018-08-24 | 华东理工大学 | A kind of phosphorus doping multistage pore canal azotized carbon nano piece and preparation method thereof |
| CN108906105A (en) * | 2018-06-28 | 2018-11-30 | 湘潭大学 | A kind of metal is monatomic/preparation method of phosphorus doping carbon nitride photocatalyst |
| CN109261211A (en) * | 2018-10-25 | 2019-01-25 | 福州大学 | A kind of nitrogen modification covalent triazine organic polymer visible-light photocatalyst and its preparation and application |
| CN109580452A (en) * | 2018-11-30 | 2019-04-05 | 西北师范大学 | It is a kind of to study the infiltrative method of amino functional silica nanometer channel selecting with scan-type electrochemical microscope |
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| CN108408700A (en) * | 2018-04-04 | 2018-08-17 | 南京工业大学 | A kind of method that non-solvent in-situ carburization prepares blue-fluorescence carbon nitrogen nanometer sheet on a large scale |
| CN108435229A (en) * | 2018-04-25 | 2018-08-24 | 华东理工大学 | A kind of phosphorus doping multistage pore canal azotized carbon nano piece and preparation method thereof |
| CN108435229B (en) * | 2018-04-25 | 2020-07-31 | 华东理工大学 | Phosphorus-doped hierarchical pore carbon nitride nanosheet and preparation method thereof |
| CN108906105A (en) * | 2018-06-28 | 2018-11-30 | 湘潭大学 | A kind of metal is monatomic/preparation method of phosphorus doping carbon nitride photocatalyst |
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| CN110813343B (en) * | 2018-08-07 | 2020-12-01 | 上海交通大学 | Preparation method of doped graphite-like carbon nitride material |
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| CN109627012B (en) * | 2018-12-17 | 2021-06-22 | 福州大学 | Preparation method of self-supporting graphite phase carbon nitride film |
| CN109627012A (en) * | 2018-12-17 | 2019-04-16 | 福州大学 | A kind of preparation method of self-supporting graphite phase carbon nitride film |
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| CN114032578A (en) * | 2021-10-11 | 2022-02-11 | 三峡大学 | Preparation method of boron or phosphorus doped graphite phase carbon nitride film electrode |
| CN115385420A (en) * | 2022-07-29 | 2022-11-25 | 江苏理工学院 | In-situ controllable preparation method and application of phosphorus-doped carbon nitride electrode |
| CN115385420B (en) * | 2022-07-29 | 2023-11-03 | 江苏理工学院 | In-situ controllable preparation method and application of phosphorus-doped carbon nitride electrode |
| CN115475632A (en) * | 2022-09-13 | 2022-12-16 | 东南大学 | CN/Mn 2 O 3 Preparation method of/FTOp-n heterojunction material, product and application thereof |
| CN115475632B (en) * | 2022-09-13 | 2024-04-05 | 东南大学 | CN/Mn 2 O 3 Preparation method of/FTOp-n heterojunction material, and product and application thereof |
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