CN107188178B - A kind of g-C3N4The preparation method of surface photovoltage signal enhancing - Google Patents
A kind of g-C3N4The preparation method of surface photovoltage signal enhancing Download PDFInfo
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- CN107188178B CN107188178B CN201710561992.9A CN201710561992A CN107188178B CN 107188178 B CN107188178 B CN 107188178B CN 201710561992 A CN201710561992 A CN 201710561992A CN 107188178 B CN107188178 B CN 107188178B
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- 230000002708 enhancing effect Effects 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 34
- 239000002608 ionic liquid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004202 carbamide Substances 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- 239000002563 ionic surfactant Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- -1 1- ethyl Chemical group 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 239000008118 PEG 6000 Substances 0.000 claims description 5
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims 2
- 239000005864 Sulphur Substances 0.000 claims 1
- 150000002500 ions Chemical class 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 5
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 42
- 230000000052 comparative effect Effects 0.000 description 31
- 235000019441 ethanol Nutrition 0.000 description 25
- 239000000047 product Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 13
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 12
- 238000005406 washing Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000003643 water by type Substances 0.000 description 9
- 239000006185 dispersion Substances 0.000 description 8
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- 229910021653 sulphate ion Inorganic materials 0.000 description 7
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- 238000007146 photocatalysis Methods 0.000 description 6
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- 238000012545 processing Methods 0.000 description 5
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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- 239000003208 petroleum Substances 0.000 description 1
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- 238000000634 powder X-ray diffraction Methods 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical group [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to chemical material preparation fields, especially field of photocatalytic material, specially a type graphite phase carbon nitride (g-C3N4) surface photovoltage signal enhancing preparation method.This method is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4；With the g-C prepared3N4To g-C under ionic liquid or surfactant auxiliary3N4Carry out hydro-thermal process, cooled to room temperature；It uses ethanol wash 1-2 times, powder taking-up is dispersed in alcohol, 60-80 DEG C is dried to obtain g-C again after powder is washed with deionized3N4.Class graphite phase carbon nitride (g-C through surfactant or ionic liquid auxiliary hydro-thermal process3N4) material has the surface photovoltage signal of enhancing, and has the advantages that preparation method simplicity, raw material are easy to get, are low in cost.
Description
Technical field
The present invention relates to chemical material preparation field, especially field of photocatalytic material, specially a kind of g-C3N4Surface light
The preparation method of voltage signal enhancing.
Background technique
With the development of the social economy, the problem of environmental pollution got worse has threatened the existence of the mankind.Meanwhile closely
The consumption of the resources such as coal, petroleum also brings immeasurable loss to the mankind over year, and there is an urgent need for a kind of sustainable developments for this
New technology.
It has been found that Photocatalitic Technique of Semiconductor has good potential application in protection environment and solar energy conversion aspect
Value, because its reaction condition is mild, low energy consumption, secondary pollution is few and has wide range of applications and has obtained extensive research.Photocatalysis
Agent (photocatalyst) can directly utilize sunlight as light source, preparation process also compares since itself is nontoxic and pollution-free
Simply, have many advantages, such as again while curbing environmental pollution for producing clean energy resource, for solve environmental pollution this all one's life
The problem of criticality is of great importance, so visible light photocatalysis technology is concerned.Efficient visible-light photocatalysis material should
Have the characteristics that low-energy zone, high-quantum efficiency, high stability, easily recycling, large specific surface area, easily recycling.
Carbonitride is a kind of very promising covalent compound, wherein class graphite phase carbon nitride (g-C3N4) it is at room temperature
Most stable of phase has properties such as nontoxic and visible light-responded (2.7 eV of semiconductor band gap), has it very in catalytic field
Have broad application prospects.g-C3N4With its photocatalytic activity is high, stability is good, cost of material is cheap, be especially free of metal this
One outstanding advantages make it a kind of novel photochemical catalyst.
It will be appreciated, however, that g-C3N4The photocatalytic activity electron-hole high by its is compound to be influenced, to improve g-
C3N4Photocatalysis performance, people have carried out study on the modification to it to improve the separation effect of electron-hole.It is most of inorganization
G-C can be combined or be inserted by closing object and inorganic metal ion3N4In matrix, g-C can be effectively finely tuned3N4Structure and
Improve reactivity.The study found that by g-C3N4Modification, can expand the response range of its visible light, inhibit g-C3N4's
Compound, the raising g-C of light induced electron and hole3N4Photocatalytic activity and selectivity, improve surface property, this is to g-C3N4's
Industrial applications are significant.In terms of study on the modification, various methods, including g-C are used3N4Pattern, nonmetallic mix
Miscellaneous, metal-doped, semiconductors coupling, noble metal loading, dye sensitization and surface modification etc..Zhong Junbo etc. using infusion process and
Photoreduction met hod is prepared for SO4 2-、PO4 2-With the g-C of Ag modification3N4, the results showed that surface photovoltage significantly increases, photocatalytic activity
It improves.But there is the shortcomings that cumbersome, poor controllability in above method, be badly in need of improving g-C using easy means3N4Photoproduction
Separation of charge effect, to further increase photocatalysis performance.
In all factors for influencing photocatalytic activity, the separation effect of electron-hole plays vital effect.
After photochemical catalyst receives energy greater than the light of forbidden bandwidth, only photo-generate electron-hole efficiently separates, moves to catalyst surface
After could induce light-catalyzed reaction.It can be seen that the separation of research Photoinduced Charge discloses surface for improving photocatalysis efficiency
Light-catalyzed reaction essence has great theoretical and practical significance.The research of photogenerated charge metastatic rule is that building high-performance optical is urged
The core topic of change system.Therefore, g-C is improved3N4Efficiently separating for photochemical catalyst electron-hole is urgent and necessary.
g-C3N4Photochemical catalyst photo-generate electron-hole separation effect can indicate that surface photovoltage is believed using surface photovoltage
It is number stronger, indicate that photogenerated charge separation effect is better.
Summary of the invention
The present invention is based on the above technical problems, provide a kind of g-C3N4The preparation method of surface photovoltage signal enhancing.The system
Preparation Method is easy to operate, and raw material is cheap and easily-available；The g-C prepared using this preparation method3N4, surface photovoltage signal significantly increases
By force, solid foundation is established for its practice.
The specific technical solution of the present invention is as follows:
A kind of g-C that surface photovoltage signal significantly increases3N4Preparation method refers in g-C3N4And suspension
In, ionic liquid or surfactant are added, through washing the g- for obtaining surface photovoltage signal and significantly increasing after hydro-thermal process
C3N4.Specific step is as follows:
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4.Urea
For commercial product.
Second step, with the g-C prepared3N4To g-C under ionic liquid or surfactant auxiliary3N4Carry out water
Heat treatment.Specially take the g-C of 2-2.5g3N4It is dispersed in 40-60 mL deionized water, adds 0.05-0.5g ionic liquid
Or surfactant, 160-180 DEG C hydro-thermal process 0.5-2 hours, cooled to room temperature.The ionic liquid is 1- second
- 3 methylimidazolium nitrate of base, -3 methylimidazolium hydrogen sulphate salt of 1- ethyl, 1- ethyl -2,3- methylimidazole bromide, 1- ethyl -
Any one or a few mixture in 2,3- methylimidazole villaumite and 1- ethyl -2,3- methylimidazole salt compounded of iodine.It is described
Surfactant be PEG 6000 or CTAB.
Third step is used ethanol wash 1-2 times again after being washed with deionized, and powder taking-up is dispersed in alcohol, 60-80
DEG C it is drying to obtain product, test surfaces photovoltage.
A kind of g-C of surface photovoltage signal enhancing prepared by the present invention3N4, crystal phase is using X-ray powder diffraction table
Sign；Surface photovoltage test is tested on the surface photovoltaic spectroscopy that Jilin University assembles.Light source is xenon lamp, using lock-in amplifier
The signal of acquisition is amplified, sample is pressed between electro-conductive glass and oxide array on metallic copper substrate, wavelength measurement range 300-600 nm.
(1) g-C of surface photovoltage signal enhancing of the invention3N4, the preparation of catalyst only uses urine cheap and easy to get
Element, ethyl alcohol, so that catalyst of the invention has requirement cheap, suitable for mass production.
(2) g-C of surface photovoltage signal enhancing of the present invention3N4, easy to operate, the time is short, securely and reliably.
(3) g-C of the present invention under ionic liquid or surfactant auxiliary after hydrothermal treatment3N4Relatively be not added with from
The g-C of sub- liquid or surfactant auxiliary hydro-thermal process3N4, on the section 300-450 nm surface, photoelectric signal significantly increases
By force.
Detailed description of the invention
Fig. 1 is that the XRD of 1 products obtained therefrom of comparative example schemes
Fig. 2 is the surface photovoltage signal contrast figure of 1 products obtained therefrom of comparative example 1 and embodiment
Fig. 3 is the surface photovoltage signal contrast figure of 2 products obtained therefrom of comparative example 1 and embodiment
Fig. 4 is the surface photovoltage signal contrast figure of 3 products obtained therefrom of comparative example 1 and embodiment
Fig. 5 is the surface photovoltage signal contrast figure of 4 products obtained therefrom of comparative example 1 and embodiment
Fig. 6 is the surface photovoltage signal contrast figure of 5 products obtained therefrom of comparative example 1 and embodiment
Fig. 7 is the surface photovoltage signal contrast figure of 6 products obtained therefrom of comparative example 1 and embodiment
Fig. 8 is the surface photovoltage signal contrast figure of 7 products obtained therefrom of comparative example 1 and embodiment
Fig. 9 is the surface photovoltage signal contrast figure of 8 products obtained therefrom of comparative example 1 and embodiment
Figure 10 is the surface photovoltage signal contrast figure of 9 products obtained therefrom of comparative example 1 and embodiment
Specific embodiment
The present invention is further explained with comparative example combined with specific embodiments below.It will be appreciated that these embodiments are only used for
Illustrate the present invention rather than limits the scope of the invention.It should also be understood that be, after reading the content taught by the present invention,
Those skilled in the art can make various modifications or changes to the present invention, and such equivalent forms equally fall within right appended by the application
Claim limited range.
The alcohol recorded in present specification uses the standard of medicinal alcohol.
Comparative example 1
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, to the g-C prepared3N4Carry out hydro-thermal process.Specially take 2.5 g g-C3N4It is dispersed in 60 mL
In deionized water, 180 DEG C hydro-thermal process 2 hours, cooled to room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
Fig. 1 is that the XRD spectrogram that comparative example 1 obtains sample apparent diffraction occurs at 27.4 ° as seen from the figure
Peak, this shows that sample is class graphite phase carbon nitride.
Embodiment 1
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, the g-C that will be prepared3N4To g-C under surfactant auxiliary3N4Carry out hydro-thermal process.Specially
Take 2.5 g g-C3N4It is dispersed in 60 mL deionized waters, 0.05g PEG6000 is then added, it is small in 180 DEG C of hydro-thermal process 2
When, cooled to room temperature.
Third step is used ethanol wash 1-2 times again after substance obtained in second step is washed with deionized, powder is taken
It is dispersed in alcohol out, 80 DEG C are dried to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, Surfactant PEG 6000 is added in embodiment 1.
Fig. 2 is that the surface photovoltage signal of 1 products obtained therefrom of comparative example 1 and embodiment compares figure.As can be seen that through second step
After Surfactant PEG 6000 assists hydro-thermal process, g-C3N4Surface photovoltage signal significantly increases.
Embodiment 2
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under surfactant auxiliary3N4Carry out hydro-thermal process.Specially
Take 2.5 g g-C3N4Be dispersed in 40 mL deionized waters, be added 0.05g CTAB, 160 DEG C hydro-thermal process 2 hours, natural cooling
To room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, Surfactant CTAB is added in embodiment 2, and hydrothermal temperature is 160 DEG C, and water dispersion volume is
40 mL.
Fig. 3 is that the surface photovoltage signal of 2 products obtained therefrom of comparative example 1 and embodiment compares figure.As can be seen that through second step
After Surfactant CTAB assists hydro-thermal process, g-C3N4Surface photovoltage signal significantly increases.
Embodiment 3
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under ionic liquid auxiliary3N4Carry out hydro-thermal process.Specially take
2.0 g g-C3N4It is dispersed in 50 mL deionized waters, addition -3 methylimidazolium nitrate of 0.1g 1- ethyl, at 170 DEG C of hydro-thermals
Reason 1 hour, cooled to room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, -3 methylimidazolium nitrate of ionic liquid 1- ethyl, hydrothermal temperature 170 is added in embodiment 3
DEG C, water dispersion volume be 50 mL, hydro-thermal process 1 hour.
Fig. 4 is the surface photovoltage signal graph of 3 products obtained therefrom of comparative example 1 and embodiment.As can be seen that through second step 1- second
Resulting catalyst surface photoelectric signal obviously sharply enhances after -3 methylimidazolium nitrate of base auxiliary hydro-thermal process.In addition,
The section 400-450nm surface photoelectric signal enhances after adding -3 methylimidazolium nitrate of 1- ethyl, this is conducive to improve visible
Photolytic activity.
Embodiment 4
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under ionic liquid auxiliary3N4Carry out hydro-thermal process.Specially take
2.0 g g-C3N4It is dispersed in 55 mL deionized waters, -3 methylimidazolium hydrogen sulphate salt of 0.2g 1- ethyl, 175 DEG C of hydro-thermals is added
Processing 1.5 hours, cooled to room temperature, test surfaces photovoltage.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, -3 methylimidazolium hydrogen sulphate salt of ionic liquid 1- ethyl is added in embodiment 4, and hydrothermal temperature is
175 DEG C, water dispersion volume be 55 mL, hydro-thermal process 1.5 hours.
Fig. 5 is the surface photovoltage signal graph of 4 products obtained therefrom of comparative example 1 and embodiment.As can be seen that through second step 1- second
Resulting catalyst surface photoelectric signal obviously sharply enhances after -3 methylimidazolium hydrogen sulphate salt of base auxiliary hydro-thermal process.
Embodiment 5
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under ionic liquid auxiliary3N4Carry out hydro-thermal process.Specially take
2.0 g g-C3N4It is dispersed in 50 mL deionized waters, 0.3g 1- ethyl -2,3- methylimidazole bromide, 175 DEG C of hydro-thermals is added
Processing 2 hours, cooled to room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, ionic liquid 1- ethyl -2,3- methylimidazole bromide is added in embodiment 5, and hydrothermal temperature is
175 DEG C, water dispersion volume be 50 mL, hydro-thermal process 2 hours.
Fig. 6 is the surface photovoltage signal graph of 5 products obtained therefrom of comparative example 1 and embodiment.As can be seen that through second step 1- second
Resulting catalyst surface photoelectric signal obviously sharply enhances after base -2,3- methylimidazole bromide auxiliary hydro-thermal process.This
Outside, g-C after addition 1- ethyl -2,3- methylimidazole bromide3N4In the section 400-500nm, surface photovoltage signal significantly increases
By force, this is conducive to improve visible light catalysis activity.
Embodiment 6
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under ionic liquid auxiliary3N4Carry out hydro-thermal process.Specially take
2.0 g g-C3N4It is dispersed in 45 mL deionized waters, 0.5g 1- ethyl -2,3- methylimidazole villaumite, 160 DEG C of hydro-thermals is added
Processing 0.5 hour, cooled to room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 70 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, ionic liquid 1- ethyl -2,3- methylimidazole villaumite is added in embodiment 4, and hydrothermal temperature is
160 DEG C, water dispersion volume be 45 mL, hydro-thermal process 0.5 hour.
Fig. 7 is the surface photovoltage signal graph of 6 products obtained therefrom of comparative example 1 and embodiment.As can be seen that through second step 1- second
Resulting catalyst surface photoelectric signal obviously sharply enhances after base -2,3- methylimidazole villaumite auxiliary hydro-thermal process.
Embodiment 7
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under ionic liquid auxiliary3N4Carry out hydro-thermal process.Specially take
2.0 g g-C3N4It is dispersed in 50 mL deionized waters, 0.4g 1- ethyl -2,3- methylimidazole salt compounded of iodine, 180 DEG C of hydro-thermals is added
Processing 2 hours, cooled to room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 60 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, ionic liquid 1- ethyl -2,3- methylimidazole villaumite is added in embodiment 7, and hydrothermal temperature is
160 DEG C, water dispersion volume be 45 mL, hydro-thermal process 0.5 hour.
Fig. 8 is the surface photovoltage signal graph of 7 products obtained therefrom of comparative example 1 and embodiment.As can be seen that through second step hydro-thermal
Resulting catalyst surface photoelectric signal obviously sharply enhances after heat treatment.
Embodiment 8
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under surfactant auxiliary3N4Carry out hydro-thermal process.Specially
Take 2.5 g g-C3N4Be dispersed in 40 mL deionized waters, be added 0.05 g CTAB, 150 DEG C hydro-thermal process 2 hours, it is naturally cold
But to room temperature.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, Surfactant CTAB, g-C is added in embodiment 83N 4Mass ratio with CTAB is 2.5:
0.05.Hydrothermal temperature is 150 DEG C, and water dispersion volume is 40 mL.
Fig. 9 is that the surface photovoltage signal of 8 products obtained therefrom of comparative example 1 and embodiment compares figure.As can be seen that through second step
After Surfactant CTAB assists hydro-thermal process, g-C3N4Surface photovoltage signal does not enhance.
Embodiment 9
The first step is roasted 3 hours at 550 DEG C using current semiclosed method using urea as raw material and obtains g-C3N4。
Second step, with the g-C prepared3N4To g-C under ionic liquid auxiliary3N4Carry out hydro-thermal process.Specially take
2.0 g g-C3N4It is dispersed in 55 mL deionized waters, -3 methylimidazolium hydrogen sulphate salt of 0.6 g 1- ethyl, 175 DEG C of hydro-thermals is added
Processing 1.5 hours, cooled to room temperature, test surfaces photovoltage.
Third step is used ethanol wash 1-2 times again after deionized water washing, and powder taking-up is dispersed in alcohol, and 80 DEG C dry
It is dry to obtain sample, test surfaces photovoltage.
It is compared with comparative example 1, -3 methylimidazolium hydrogen sulphate salt of ionic liquid 1- ethyl, g-C is added in embodiment 93N 4With from
The mass ratio of sub- liquid be 2.0:0.06, hydrothermal temperature be 175 DEG C, water dispersion volume be 55 mL, hydro-thermal process 1.5 hours.
Figure 10 is the surface photovoltage signal graph of 9 products obtained therefrom of comparative example 1 and embodiment.As can be seen that through second step 1-
Resulting catalyst surface photoelectric signal does not enhance after -3 methylimidazolium hydrogen sulphate salt of ethyl auxiliary hydro-thermal process.
Example described above is only the preferred embodiment of this patent, but the protection scope of this patent is not limited thereto.
It should be pointed out that for those skilled in the art, under the premise of not departing from this patent principle, specially according to this
The technical solution and its inventional idea of benefit, can also make several improvements and modifications, these improvements and modifications also should be regarded as this specially
The protection scope of benefit.
Claims (2)
1. a kind of method for the class graphene for preparing surface photovoltage signal enhancing, it is characterised in that include the following steps:
Step 1: being roasted 3 hours using semiclosed method at 550 DEG C using urea as raw material and obtaining g-C3N4；
Step 2: with the g-C prepared3N4To g-C under the auxiliary of ionic liquid or surfactant3N4It carries out at hydro-thermal
Reason, cooled to room temperature；The ionic liquid is -3 methylimidazole sulphur of -3 methylimidazolium nitrate of 1- ethyl and 1- ethyl
The mixture of any one or two kinds in sour hydrogen salt；The surfactant is PEG 6000 or CTAB；g-C3N4With ion
The mass ratio of liquid is 2-2.5:0.05-0.5；g-C3N4Mass ratio with surfactant is 2-2.5:0.05-0.5；
Step 3: by g-C3N4Powder is used ethanol wash 1-2 times again after being washed with deionized, by g-C3N4Powder taking-up is dispersed in
In alcohol, it is drying to obtain in 60-80 DEG C.
2. a kind of method for the class graphene for preparing surface photovoltage signal enhancing according to claim 1, it is characterised in that:
The specific steps of second step are as follows: the first step is prepared to the g-C of 2-2.5g3N 4It is dispersed in 40-60 mL deionized water, then
Ionic liquid or surfactant is added, in 160-180 DEG C hydro-thermal process 0.5-2 hours, cooled to room temperature.
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