CN108355698A - A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder - Google Patents
A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder Download PDFInfo
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- CN108355698A CN108355698A CN201810148643.9A CN201810148643A CN108355698A CN 108355698 A CN108355698 A CN 108355698A CN 201810148643 A CN201810148643 A CN 201810148643A CN 108355698 A CN108355698 A CN 108355698A
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- 239000000843 powder Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 28
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims description 23
- 229910021641 deionized water Inorganic materials 0.000 claims description 23
- 238000001354 calcination Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 150000007974 melamines Chemical class 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- -1 After mixing Chemical compound 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a kind of preparation methods of O doped graphites phase carbon nitride nanometer sheet powder, make raw material with melamine, hydrogen peroxide and water, and modified cyanurotriamide presoma is prepared using hydrogen peroxide auxiliary hydro-thermal process melamine;Then the melamine of above-mentioned modification is subjected to high-temperature calcination, you can obtain broad stopband O doping g C3N4Nanometer sheet powder.Obtained O doping g C3N4Nanometer sheet powder compares body phase g C3N4With higher specific surface area, while O is incorporated into g C3N4Conventional bulk phase g C are changed in skeleton3N4Electronic structure so that energy gap significantly increases, while overcoming it to light induced electron and hole easily quick compound, disadvantage that photo-quantum efficiency is low, to improve g C3N4Photocatalysis performance.And the method for the present invention have the advantages that reaction process it is simple, it is easily controllable, low using cost of material, to equipment without particular/special requirement, be suitble to large-scale industrial production.
Description
Technical field
The invention belongs to catalysis material preparing technical fields, and in particular to a kind of O doped graphites phase carbon nitride nanometer sheet
The preparation method of powder.
Background technology
Graphite phase carbon nitride (g-C3N4) make a kind of novel polymer semiconductor's photochemical catalyst and closed extensively by people
Note.Numerous studies show at present:g-C3N4With lamellar structure, suitable band structure and goodization similar to graphene
Stability is learned, therefore in photocatalytic pollutant degradation, decomposition aquatic products hydrogen and reduction CO2Field has a good application prospect.So
And conventional bulk phase g-C3N4Specific surface area is small and photo-generated carrier is easy and fast to compound disadvantage and significantly limits its light to urge
Change performance.
g-C3N4Physical and chemical performance and its microstructure and electronic structure it is closely related.Conventional g-C3N4Catalysis material
Modification mode includes mainly:Morphological control, carried noble metal and metal/non-metal doping.In particular, doping vario-property passes through two
Tie up stratiform g-C3N4Layer in and interlayer introduce heteroatom so that foreign atom track and g-C3N4Original molecular orbit hair
Raw Orbit revolutionary, can cause the change of electronic structure, lead to g-C3N4Material is realized in the variation of valence band and conduction level position
Visible light utilization efficiency and photocatalytic redox potential optimization, and then improve its photocatalysis performance.In recent years, O adulterates g-
C3N4It gets more and more people's extensive concerning, the increase of photocatalytic redox potential may be implemented in element doping strategy, to effectively carry
The photocatalysis performance of high material.However, related broad stopband O adulterates g-C at present3N4The still rare document report of research.
Therefore, the present invention provides a kind of modifies preparation O of forerunner to adulterate g-C3N4Strategy selects melamine, double first
Oxygen water and water make raw material, and modified cyanurotriamide presoma is prepared using hydrogen peroxide auxiliary hydro-thermal process melamine;Then
The melamine of above-mentioned modification is subjected to high-temperature calcination, you can obtain broad stopband O and adulterate g-C3N4Nanometer sheet powder.
Invention content
The object of the present invention is to provide a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder, solve existing
There is g-C3N4To the easily quick problem compound, photo-quantum efficiency is low in light induced electron and hole, and improve its energy gap.
The technical solution adopted in the present invention is a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder, tool
Body is implemented according to the following steps:
Step 1, the preparation of modified presoma:
Melamine, hydrogen peroxide, deionized water are added in reaction kettle, stirred evenly, it is anti-to be put into progress hydro-thermal in baking oven
It answers, obtains solidliquid mixture;Then solidliquid mixture washed, dried, obtain modified presoma;
Step 2, O adulterates g-C3N4The preparation of nanometer sheet powder:
The modification presoma obtained to step 1 carries out high-temperature calcination to get to g-C3N4Nanometer sheet powder.
Feature of the present invention also resides in,
Melamine and the mass volume ratio of deionized water are 1 in step 1:60~1:1, the body of hydrogen peroxide and deionized water
Product is than being 1:60~1:1.
The mass concentration of hydrogen peroxide is 30% in step 1.
Hydrothermal temperature is 120~200 DEG C in step 1, and the time is 12~96h.
It is washed in step 1, specially:Eccentric cleaning is distinguished 3~6 times using deionized water and absolute ethyl alcohol.
Drying temperature is 50~90 DEG C in step 1, and the time is 12~36h.
Step 2 high temperature calcination temperature is 500~600 DEG C, and soaking time is 0.5~6h.
Heating rate is 0.1~10 DEG C/min in calcination process.
The invention has the advantages that the present invention makees raw material, hydrothermal treatment and height with melamine, hydrogen peroxide and water
Temperature calcining obtains broad stopband O doping g-C3N4Nanometer sheet powder.Used hydrogen peroxide auxiliary hydro-thermal process presoma strategy at
Realize g-C to work(3N4The band structure of powder is modified, and the O of acquisition adulterates g-C3N4Nanometer sheet powder compares body phase g-C3N4Tool
There is higher specific surface area, while O is incorporated into g-C3N4Conventional bulk phase g-C is changed in skeleton3N4Electronic structure so that prohibit
Bandwidth significantly increases, while overcoming it to light induced electron and hole easily quick compound, disadvantage that photo-quantum efficiency is low, from
And improve g-C3N4Photocatalysis performance.And the method for the present invention is simple, easily controllable with reaction process, uses cost of material
It is low, to equipment without particular/special requirement the advantages of, fully catered to the industrial scale applications of simple and environmentally-friendly low cost instantly, be suitble to extensive
Industrialized production.
Description of the drawings
Fig. 1 is O doping g-C prepared by the embodiment of the present invention 13N4The transmission electron micrograph of nanometer sheet powder;
Fig. 2 is O doping g-C prepared by the embodiment of the present invention 23N4The transmission electron micrograph of nanometer sheet powder.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
A kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder of the present invention, with melamine, hydrogen peroxide and water
Make raw material, modified cyanurotriamide presoma is prepared using hydrogen peroxide auxiliary hydro-thermal process melamine;Then change above-mentioned
Property melamine carry out high-temperature calcination, you can obtain broad stopband O adulterate g-C3N4Nanometer sheet powder.
It is specifically implemented according to the following steps:
Step 1, the preparation of modified presoma:
Melamine is weighed, is put it into clean polytetrafluoroethyllining lining, addition mass concentration is 30% hydrogen peroxide,
After mixing, deionized water is added, the mass ratio of melamine and deionized water is 1:60~1:1, hydrogen peroxide and deionized water
Volume ratio is 1:60~1:1, it is to be mixed uniform, it closes the lid and moves it into corresponding stainless steel cauldron housing, in an oven
120~200 DEG C of 12~96h of heat preservation, the presoma solidliquid mixture deionized water and absolute ethyl alcohol that are obtained are centrifuged respectively
Cleaning 3~6 times, what is obtained is deposited in 50~90 DEG C of dry 12~36h, you can obtains the melamine forerunner that hydrogen peroxide is modified
Body.
Step 2, O adulterates g-C3N4The preparation of nanometer sheet powder:
The melamine presoma that the hydrogen peroxide that step 1 is obtained is modified, is put into alumina crucible, closes the lid;With
500 DEG C in air atmosphere~600 DEG C 0.5~6h of calcining of Muffle furnace, calcining heating rate is 0.1~10 DEG C/min.It can obtain
It obtains O and adulterates g-C3N4Nanometer powder.
The present invention is using a kind of low cost, controllability and the good liquid and solid phase reaction method of operability and solid sintering technology phase
In conjunction with strategy, using hydrogen peroxide auxiliary hydro-thermal process presoma successfully realize g-C3N4The band structure of powder is modified, and is led to
The volume ratio of hydrogen peroxide and deionized water in adjustment and control system is crossed, the O with different doping O contents can be prepared and adulterate g-C3N4
Nanometer sheet powder improves conventional bulk phase g-C3N4Powder is easy to reunite and the unconspicuous structural disadvantages of two-dimensional structure.It is obtained
The O doping g-C obtained3N4Nanometer sheet powder compares body phase g-C3N4With higher specific surface area, while O is incorporated into g-C3N4
Conventional bulk phase g-C is changed in skeleton3N4Electronic structure so that energy gap significantly increases, at the same overcome its to photoproduction electricity
Son and the easily quick disadvantage compound, photo-quantum efficiency is low in hole, to improve g-C3N4Photocatalysis performance.System of the present invention
The O obtained adulterates g-C3N4Hydrogen-producing speed (1050.3 μm of olg of nanometer sheet-1·h-1) more unmodified melamine dinectly bruning institute
The body phase g-C of acquisition3N4Hydrogen-producing speed (98.2 μm of olg-1·h-1) improve nearly 10.7 times.
And the method for the present invention have reaction process it is simple, it is easily controllable, low using cost of material, to equipment without particular/special requirement
The advantages of, the industrial scale applications of simple and environmentally-friendly low cost instantly have fully been catered to, large-scale industrial production is suitble to.
Embodiment 1
Step 1, it is 1 according to melamine and deionized mass ratio:10, mass concentration be 30% hydrogen peroxide and go from
The volume ratio of sub- water is 1:60, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed,
It stirs evenly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 140 DEG C
12h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 3 times with deionized water and absolute ethyl alcohol, finally exists
Dry 36h in 50 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 600 DEG C of isothermal holdings
2h, calcining heating rate are 0.5 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
The O that the present embodiment obtains adulterates g-C3N4Powder TEM photos, as shown in Figure 1, it can be seen that it is apparent nanometer
Chip architecture.
Embodiment 2
Step 1, it is 1 according to melamine and deionized mass ratio:1, mass concentration be 30% hydrogen peroxide and go from
The volume ratio of sub- water is 1:1, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, stirred
It mixes uniformly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 180 DEG C
36h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 6 times with deionized water and absolute ethyl alcohol, finally exists
Dry 12h in 90 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 550 DEG C of isothermal holdings
3h, calcining heating rate are 3 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
The O that the present embodiment obtains adulterates g-C3N4Powder TEM photos, as shown in Figure 2, it can be seen that it is apparent nanometer
Chip architecture.
Embodiment 3
Step 1, it is 1 according to melamine and deionized mass ratio:5, mass concentration be 30% hydrogen peroxide and go from
The volume ratio of sub- water is 1:10, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed,
It stirs evenly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 200 DEG C
For 24 hours, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 4 times with deionized water and absolute ethyl alcohol, finally exists
Dry 18h in 70 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 500 DEG C of isothermal holdings
6h, calcining heating rate are 10 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
Embodiment 4
Step 1, it is 1 according to melamine and deionized mass ratio:30, mass concentration be 30% hydrogen peroxide and go from
The volume ratio of sub- water is 1:5, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed, stirred
It mixes uniformly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 120 DEG C
96h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 3 times with deionized water and absolute ethyl alcohol, finally exists
Dry 15h in 60 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 530 DEG C of isothermal holdings
4h, calcining heating rate are 5 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
Embodiment 5
Step 1, it is 1 according to melamine and deionized mass ratio:60, mass concentration be 30% hydrogen peroxide and go from
The volume ratio of sub- water is 1:10, melamine, hydrogen peroxide, deionized water are added in clean polytetrafluoroethyllining lining and are mixed,
It stirs evenly;Above-mentioned polytetrafluoroethyllining lining is fitted into corresponding stainless steel outer sleeve, is tightened, baking oven is put into, is kept the temperature at 160 DEG C
72h, after furnace cooling, the solidliquid mixture that will be obtained distinguishes eccentric cleaning 5 times with deionized water and absolute ethyl alcohol, finally exists
Dry 30h in 60 DEG C of baking ovens, you can obtain modified cyanurotriamide presoma.
Step 2, presoma step 1 obtained, is put into alumina crucible, closes the lid;In 580 DEG C of isothermal holdings
0.5h, calcining heating rate are 0.1 DEG C/min, you can obtain O and adulterate g-C3N4Powder.
Claims (8)
1. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder, which is characterized in that specifically real according to the following steps
It applies:
Step 1, the preparation of modified presoma:
Melamine, hydrogen peroxide, deionized water are added in reaction kettle, is stirred evenly, is put into baking oven and carries out hydro-thermal reaction, obtain
To solidliquid mixture;Then solidliquid mixture washed, dried, obtain modified presoma;
Step 2, O adulterates g-C3N4The preparation of nanometer sheet powder:
The modification presoma obtained to step 1 carries out high-temperature calcination to get to g-C3N4Nanometer sheet powder.
2. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In melamine and the mass ratio of deionized water are 1 in the step 1:60~1:1, the volume ratio of hydrogen peroxide and deionized water
It is 1:60~1:1.
3. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In the mass concentration of hydrogen peroxide is 30% in the step 1.
4. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In hydrothermal temperature is 120~200 DEG C in the step 1, and the time is 12~96h.
5. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In being washed in the step 1, specially:Eccentric cleaning is distinguished 3~6 times using deionized water and absolute ethyl alcohol.
6. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In drying temperature is 50~90 DEG C in the step 1, and the time is 12~36h.
7. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1, feature exist
In the step 2 high temperature calcination temperature is 500~600 DEG C, and soaking time is 0.5~6h.
8. a kind of preparation method of O doped graphites phase carbon nitride nanometer sheet powder according to claim 1 or claim 7, feature
It is, heating rate is 0.1~10 DEG C/min in the calcination process.
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CN109607500A (en) * | 2018-12-29 | 2019-04-12 | 广西大学 | A kind of g-C3N4The preparation method of ultrathin nanometer piece |
CN110201698A (en) * | 2019-06-03 | 2019-09-06 | 肇庆市华师大光电产业研究院 | A kind of preparation method of polynary nonmetal doping carbon nitride photocatalyst |
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CN112547109A (en) * | 2020-12-24 | 2021-03-26 | 江苏大学 | Preparation method of wide-spectrum response type three-dimensional carbon nitride photocatalyst for carbon and oxygen co-doping by introducing polymer molecules |
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