CN110512260A - A kind of preparation method of complex light electrode - Google Patents
A kind of preparation method of complex light electrode Download PDFInfo
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- CN110512260A CN110512260A CN201910801174.0A CN201910801174A CN110512260A CN 110512260 A CN110512260 A CN 110512260A CN 201910801174 A CN201910801174 A CN 201910801174A CN 110512260 A CN110512260 A CN 110512260A
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- complex light
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- carbon nitride
- titanium dioxide
- phase carbon
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- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 129
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 126
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 78
- 239000010439 graphite Substances 0.000 claims abstract description 73
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 60
- 239000002127 nanobelt Substances 0.000 claims abstract description 33
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 32
- 238000001354 calcination Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000012545 processing Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 36
- 239000010936 titanium Substances 0.000 claims description 34
- 239000008367 deionised water Substances 0.000 claims description 31
- 229910021641 deionized water Inorganic materials 0.000 claims description 31
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 28
- 229910052719 titanium Inorganic materials 0.000 claims description 28
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 229910052697 platinum Inorganic materials 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000003792 electrolyte Substances 0.000 claims description 16
- 230000003647 oxidation Effects 0.000 claims description 15
- 238000007254 oxidation reaction Methods 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- 238000000151 deposition Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000002604 ultrasonography Methods 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 11
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000005498 polishing Methods 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 8
- 229920000877 Melamine resin Polymers 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 230000008021 deposition Effects 0.000 claims description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 7
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 6
- 238000004070 electrodeposition Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000012286 potassium permanganate Substances 0.000 claims description 6
- 230000035807 sensation Effects 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 244000137852 Petrea volubilis Species 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 2
- 239000002135 nanosheet Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- GTTYPHLDORACJW-UHFFFAOYSA-N nitric acid;sodium Chemical compound [Na].O[N+]([O-])=O GTTYPHLDORACJW-UHFFFAOYSA-N 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000005829 trimerization reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000003595 spectral effect Effects 0.000 abstract description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000011065 in-situ storage Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000004317 sodium nitrate Substances 0.000 description 5
- 235000010344 sodium nitrate Nutrition 0.000 description 5
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000002071 nanotube Substances 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 1
- SZUKQRSUJLZCFE-UHFFFAOYSA-N [Ti].O=[Si]=O Chemical compound [Ti].O=[Si]=O SZUKQRSUJLZCFE-UHFFFAOYSA-N 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000002048 anodisation reaction Methods 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000001808 coupling effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000012719 thermal polymerization Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
-
- B01J35/33—
-
- B01J35/39—
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
- C01B32/192—Preparation by exfoliation starting from graphitic oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
- C25D9/08—Electrolytic coating other than with metals with inorganic materials by cathodic processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Abstract
The invention discloses a kind of preparation methods of complex light electrode, belong to complex light electrode preparation field, include the following steps, prepare titanium dioxide nano-belts array photoelectric pole, and do calcination processing, prepare graphite phase carbon nitride nanometer sheet colloidal solution, prepare graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode, prepare the titanium dioxide nano-belts complex light electrode of graphite phase carbon nitride and graphene co-deposition, complex light electrode produced by the present invention is economic and environment-friendly, stability is good, operating process is easily controllable, the shortcomings that system overcomes titanium dioxide nano-belts array and graphite phase carbon nitride itself, spectral absorption range is widened, reduce the compound of photo-generate electron-hole, it is a kind of environmentally friendly material with visible light-responded highlight catalytic active.
Description
Technical field
The invention belongs to complex light electrode preparation fields, relate in particular to a kind of preparation method of complex light electrode.
Background technique
Titanium oxide is as a kind of traditional n-type semiconductor photochemical catalyst, due to its superior optics and Electronic Performance, physics
The advantages that chemical property is stablized, and has no toxic side effect, cheap and easy to get, is widely studied and applied in photocatalysis field, is
The most photocatalyst material of current research.However, titanium dioxide optical catalyst has the disadvantage in that light induced electron and hole
Recombination rate is higher；Since TiO2 forbidden bandwidth is wider (~3.2eV), make it that can only absorb energy greater than its forbidden bandwidth energy
Ultraviolet light causes the utilization rate of its sunlight lower.TiO2 photochemical catalyst is modified to improve disadvantages mentioned above, modified side
Method mainly has precious metal doping, nonmetal doping, semiconductors coupling and surface sensitization effect, comes relative to other method of modifying
It says, semiconductors coupling effect is much better, and complex method diversification.
There are five types of allotropes for carbonitride tool, and wherein graphite phase carbon nitride (g-C3N4) is most stable in five kinds of carbonitrides
One kind.It is environment-protecting and non-poisonous, cheap and easy to get, belongs to narrow gap semiconductor, and band gap width is about 2.7eV, maximum absorption wavelength
Near 460nm, this allows it effectively to absorb visible light, has higher utilization efficiency to sunlight.Meanwhile g-C3N4
Also have many advantages, such as good thermal stability, electronics and optical characteristics.According to a series of above-mentioned excellent characteristics, g-C3N4 is can
Cause greatly to pay close attention in terms of light-exposed lower degradable organic pollutant.However have by the graphite phase carbon nitride that thermal polymerization obtains
The disadvantages of light induced electron and fast hole-recombination, photocatalysis efficiency is still to be improved.By narrow gap semiconductor graphite phase carbon nitride with
Broad-band gap titanium dioxide is compound, can not only improve visible absorption range, promotes the migration of photo-generate electron-hole, at the same have compared with
High redox ability finally has superior photocatalytic redox performance.By the two dimension for introducing earth rich content
Conductive redox graphene (rGO) is used as effective electronic media, further promotes photo-generated carrier transfer.Theoretically
It says, rGO not only can increase connecing between two kinds of different semiconductors by creating new electron transmission bridge for Z- type charge recombination
Contacting surface product and compactness, and adsorption and kinetics can be substantially improved, to significantly increase photocatalytic activity.
Current is fewer to the research of graphene@graphite phase carbon nitride/titanium dioxide nano-belts array photoelectric pole, only
Research be concentrated mainly on graphene@graphite phase carbon nitride/titanium dioxide nanotube array photoelectrode and graphene@graphite-phase nitrogen
Change in the preparation of carbon/titania powder, is received by thermal polycondensation in-situ preparation Z-type graphene@graphite phase carbon nitride/titanium dioxide
Rice band array photoelectric pole yet there are no relevant report.Graphene@graphite phase carbon nitride/titanium dioxide nanotube array photoelectrode has
It is recycled to recycle and facilitates cheap advantage, but the graphite phase carbon nitride of graphene made from this method/titanium dioxide array
For optoelectronic pole there is also several respects disadvantage, the graphite phase carbon nitride of generation is deposited at the top of nanotube in the form of quantum dot, right
The utilization rate of visible light and the adsorbance of pollutant are low, so as to cause photocatalysis efficiency reduction；Anodizing and chemical gas
The graphite phase carbon nitride amount of phase deposition method to titanium dioxide photoelectrode is considerably less, absorption and light induced electron to visible light
It is not significantly improved with the separation rate in hole；Graphene@graphite phase carbon nitride/titania powder separates needs from suspension
Costly cost, this seriously hinders practical application of the technique in pollutant process.
Nano-band array optoelectronic pole at the top of bottom silicon dioxide titanium nanotube is made by adjusting altering anodization parameters in this technology,
Have many advantages, such as nanobelt+pipe array that large specific surface area, stability are high, PhotoelectrocatalytiPerformance Performance is good, orderly, further improves
The transference ability of stationary state titanium dioxide photoproduction electronics.By orderly titanium dioxide array and graphite phase carbon nitride, graphene
Semiconductor coupling is carried out, the position of the top of valence band and conduction band bottom energy level of titanium dioxide and graphite phase carbon nitride matches, when illumination
The two is capable of forming Z-type heterojunction structure, and the hole that the light induced electron and graphite phase carbon nitride that titanium dioxide generates generate is answered
It closes, last photohole is gathered in the conduction band of titanium dioxide, and light induced electron is then gathered in the valence band of graphite phase carbon nitride, leads to
It crosses graphene and conducts light induced electron to photoelectricity pole surface and reduction reaction occurs, extend the service life in light induced electron and hole, together
When also efficiently separate photo-generated carrier, be widen light abstraction width and promote separation of charge effective ways.
Summary of the invention
Inventor is prepared by being modified using graphite phase carbon nitride and graphene titanium dioxide nano-belts array
There is the yield and separative efficiency of the raw electron hole of high light, higher visible light utility, to antibiotic to photochemical catalyst
The photocatalytic degradation of quadracycline (TC) has a significant effect, and is a kind of Z-type graphene@graphite-phase that green is stable nitridation
Carbon/titanium dioxide nano-belts array photoelectric pole preparation method.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of complex light electrode, comprising the following steps:
S1: titanium dioxide nano-belts array photoelectric pole is prepared, and does calcination processing；
S2: preparation graphite phase carbon nitride nanometer sheet colloidal solution；
S3: preparation graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode；
S4: the titanium dioxide nano-belts complex light electrode of preparation graphite phase carbon nitride and graphene co-deposition.
Preferably, in step S1, pretreated titanium sheet is as anode, using the platinized platinum of identical size as cathode, electrolysis
Matter is 0.25~0.75wt%NH4F and 90-99% ethylene glycol 100ml mixed solution, controls 15-25 DEG C of reaction temperature, and voltage is
55-65V is aoxidized 2-4h, and is stirred continuously with revolving speed 600-800rpm/min, the titanium dioxide nano-belts array after oxidation
Optoelectronic pole is placed in Muffle furnace, calcination processing.
Preferably, the pretreated step of titanium sheet includes but is not limited to cleaning, sanding and polishing and ultrasonic cleaning.
Preferably, Ti content > 99.9% in titanium sheet, titanium sheet specification are 100mm × 10mm × 0.2mm, the sand of sanding and polishing
Paper successively selects 600 mesh, 1000 mesh and 2000 mesh, ultrasonic in deionized water, acetone and alcohol mixeding liquid, deionized water respectively
10min is cleaned, the volume ratio of acetone and ethyl alcohol is 1:1 in the acetone and alcohol mixeding liquid, it places into deionized water and seals up for safekeeping,
.
Preferably, calcination temperature is 550 DEG C, calcination time 2h.
Preferably, in step S2, melamine is put into crucible with cover, 2h, heating rate 5 are calcined in Muffle furnace
DEG C/min, it is ground to no obvious granular sensation with agate mortar after calcining, can be prepared by body phase graphite phase carbon nitride；
3-5g body phase graphite phase carbon nitride is taken to be placed in the 50ml concentrated sulfuric acid, stirring is formed suspended under the conditions of 25 DEG C of temperature
Suspension is add to deionized water by liquid, and ultrasound removing 10-24h is washed to neutrality using the method for suction filtration, obtains graphite
Phase carbon nitride nanometer sheet by azotized carbon nano piece Ultrasonic Pulverization and is settled to 2-3L.
Preferably, the melamine is 10-15g, and calcination temperature is 450~550 DEG C, and mixing time 10-24h is gone
Ion water volume is 200-400ml, and the Ultrasonic Pulverization time is 2-3h.
Preferably, in step S3, taking graphite phase carbon nitride nanometer sheet colloidal solution obtained in 100ml step S2 is electrolysis
Cathode is made in liquid, titanium dioxide nano-belts array photoelectric pole, and platinized platinum makees anode, electrochemical deposition 30min under 1-6V voltage, and 101 DEG C
It is dried under the conditions of temperature.
Preferably, in step S4, take 10~30mg graphite oxide in 1L water, it is 10 that 1~3h of ultrasound removing, which obtains concentration,
~30mg/L graphene oxide dispersion, using graphene oxide dispersion as electrolyte, graphite-phase nitrogen obtained in step S3
Change carbon doping titanium dioxide nano band array composite photoelectric extremely cathode, platinized platinum is as anode, deposition voltage 1-10V, deposition
1-10min.
Preferably, it is added in the concentrated sulfuric acid after graphite powder and sodium nitrate being mixed according to mass ratio 1:0.5, is stirred in ice bath
The potassium permanganate solid of 3~4 times of graphite powder quality is added in 30min, and reaction temperature is lower than 10 DEG C, stirs 8~10h, and water is added,
Under the conditions of 98 DEG C of temperature stirring 20~for 24 hours, be added 30% water simultaneously stir evenly, cleaned simultaneously with 5% HCl and deionized water
Centrifugal filtration can be prepared by graphite oxide.
The beneficial effects of the present invention are:
Combination electrode prepared by the present invention is economic and environment-friendly, and stability is good, and reaction condition is mild, and operating process is easily controllable,
Combination electrode obtained overcomes the shortcomings that titanium dioxide nano-belts array and graphite phase carbon nitride itself, has widened spectral absorption
Range reduces the compound of photo-generate electron-hole, is a kind of environmental-friendly profile with visible light-responded highlight catalytic active
Material has the yield and separative efficiency of the raw electron hole of high light, higher visible light utility, to antibiotic quadracycline
(TC) photocatalytic degradation has a significant effect.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one
A kind of preparation method of complex light electrode, is prepared according to the following steps:
One, titanium dioxide nano-belts array photoelectric pole is prepared, and does calcination processing.
Titanium sheet is cut into 100mm × 10mm × 0.2mm bar shaped paillon, Ti content > 99.9% in titanium sheet successively passes through hydrogen
Hydrofluoric acid cleaning, 600 mesh, 1000 mesh and 2000 mesh sand paper sanding and polishings, respectively in deionized water, acetone: ethyl alcohol=1:1 (vol)
Be cleaned by ultrasonic 10min in deionized water, be put into deionized water and seal up for safekeeping, obtained anodic oxidation prepares titanium dioxide nano-belts battle array
The base material of column.
Pretreated titanium sheet is as anode, using the platinized platinum of identical size as cathode, electrolyte 0.25wt%NH4F and
90% ethylene glycol 100ml mixed solution controls 15 DEG C of reaction temperature, voltage 55V, aoxidizes 2h, and in anode oxidation process
It is stirred continuously with 600rpm/min, in titanium plate surface in-situ preparation titanium dioxide nano-belts array photoelectric pole, oxidation is finished
Titanium sheet is placed at 550 DEG C of calcining 2h in Muffle furnace.
Two, graphite phase carbon nitride nanometer sheet colloidal solution is prepared.
10g melamine is put into crucible with cover, 450 DEG C of calcinings 2h, 5 DEG C/min of heating rate in Muffle furnace are placed in.
It is ground to no obvious granular sensation with agate mortar after calcining, body phase graphite phase carbon nitride is made.Take 3g body phase graphite-phase
Carbonitride is placed in the 50ml concentrated sulfuric acid, is stirred 10h at 25 DEG C, is obtained suspension.Suspension is added to 200ml deionized water
In, ultrasound removing 10h carries out being washed to neutrality, obtains graphite phase carbon nitride nanometer sheet using the method for suction filtration, then by carbonitride
Nanometer sheet Ultrasonic Pulverization 2h is simultaneously settled to 2L.
Three, preparation graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode.
Taking graphite phase carbon nitride nanometer sheet colloidal solution made from 100ml step 2 is electrolyte, titanium dioxide nano-belts
Cathode is made in array photoelectric pole, and platinized platinum makees anode, and the electrochemical deposition 30min under 1V voltage is placed in drying box and dries at 101 DEG C
It is dry.
Four, the titanium dioxide nano-belts complex light electrode of graphite phase carbon nitride and graphene co-deposition is prepared.
Graphite oxide is prepared using Hummers method is improved, is added after graphite powder and sodium nitrate are mixed according to mass ratio 1:0.5
Enter in the concentrated sulfuric acid, 30min is stirred in ice bath, the potassium permanganate solid of 3 times of graphite powder quality is added, reaction temperature is lower than 10
DEG C, 8h is stirred, water is added, 20h is stirred under the conditions of 98 DEG C of temperature, 30%H is added2O2And stir evenly, with 5% HCl and
Deionized water cleaning and centrifugal filtration, can be prepared by graphite oxide.
Take 20mg graphite oxide in 1L water, it is 20mg/L graphene oxide dispersion that ultrasound removing 3h, which obtains concentration, with
Graphene oxide dispersion is as electrolyte, and graphite phase carbon nitride doping titanium dioxide nano band array obtained is multiple in step 3
Light combination electrode is cathode, and for platinized platinum as anode, deposition voltage is that 2V deposits 5min.
Embodiment two
A kind of preparation method of complex light electrode, is prepared according to the following steps:
One, titanium dioxide nano-belts array photoelectric pole is prepared, and does calcination processing.
Titanium sheet is cut into 100mm × 10mm × 0.2mm bar shaped paillon, Ti content > 99.9% in titanium sheet, hydrofluoric acid is clear
It washes, 600 mesh, 1000 mesh and 2000 mesh sand paper sanding and polishings is successively selected, respectively in deionized water, acetone: ethyl alcohol=1:1
(vol) it is cleaned by ultrasonic and in deionized water after 10min to be put into deionized water and seals up for safekeeping, obtains anodic oxidation and prepare titanium dioxide receiving
Base material of the rice with array.
Pretreated titanium sheet is as anode, using the platinized platinum of identical size as cathode, electrolyte 0.5wt%NH4F and
93% ethylene glycol 100ml mixed solution controls 28 DEG C of reaction temperature, voltage 58V, aoxidizes 2.5h, and in anodic oxidation
It is stirred continuously in journey with 700rpm/min, in titanium plate surface in-situ preparation titanium dioxide nano-belts array photoelectric pole, oxidation is tied
Titanium sheet after beam is placed in 550 DEG C of calcining 2h in Muffle furnace.
Two, graphite phase carbon nitride nanometer sheet colloidal solution is prepared.
12g melamine is put into crucible with cover, 490 DEG C of calcinings 2h, 5 DEG C/min of heating rate in Muffle furnace.It forges
It is ground to no obvious granular sensation with agate mortar after burning, body phase graphite phase carbon nitride is made.Take 3.5g body phase graphite-phase
Carbonitride is placed in the 50ml concentrated sulfuric acid, is stirred 10h at 25 DEG C, is obtained suspension.Suspension is added to 300ml deionized water
In, ultrasound removing 15h be washed to neutrality using the method for suction filtration and obtains graphite phase carbon nitride nanometer sheet, then by carbonitride
Nanometer sheet Ultrasonic Pulverization 2.2h is simultaneously settled to 2.2L.
Three, preparation graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode.
Taking graphite phase carbon nitride nanometer sheet colloidal solution made from 100ml step 2 is electrolyte, titanium dioxide nano-belts
Cathode is made in array photoelectric pole, and platinized platinum makees anode, and electrochemical deposition 30min, is placed in drying box under 3V voltage, in 101 DEG C of temperature
It is dried under the conditions of degree.
Four, the titanium dioxide nano-belts complex light electrode of graphite phase carbon nitride and graphene co-deposition is prepared.
Graphite oxide is prepared using Hummers method is improved, is added after graphite powder and sodium nitrate are mixed according to mass ratio 1:0.5
Enter in the concentrated sulfuric acid, 30min is stirred in ice bath, the potassium permanganate solid of 3.2 times of graphite powder quality is added, reaction temperature is lower than 10
DEG C, 9h is stirred, water is added, 22h is stirred under the conditions of 98 DEG C of temperature, 30%H is added2O2And stir evenly, with 5% HCl and
Deionized water cleaning and centrifugal filtration, can be prepared by graphite oxide.
Take 15mg graphite oxide in 1L water, it is 15mg/L graphene oxide dispersion that ultrasound removing 3h, which obtains concentration, with
Graphene oxide dispersion is as electrolyte, and graphite phase carbon nitride doping titanium dioxide nano band array obtained is multiple in step 3
Light combination electrode is cathode, and for platinized platinum as anode, deposition voltage is that 2V deposits 5min.
Embodiment three
A kind of preparation method of complex light electrode, is prepared according to the following steps:
One, titanium dioxide nano-belts array photoelectric pole is prepared, and does calcination processing.
Titanium sheet is cut into 100mm × 10mm × 0.2mm bar shaped paillon, Ti content > 99.9% in titanium sheet successively passes through
Hydrofluoric acid clean, 600 mesh, 1000 mesh and 2000 mesh sand paper sanding and polishings, respectively in deionized water, acetone: ethyl alcohol=1:1
(vol) and in deionized water it is cleaned by ultrasonic 10min, is put into deionized water and seals up for safekeeping, obtained anodic oxidation prepares titanium dioxide and receives
Base material of the rice with array.
Pretreated titanium sheet is as anode, using the platinized platinum of identical size as cathode, electrolyte 0.6wt%NH4F and
95% ethylene glycol 100ml mixed solution, control 20 DEG C of reaction temperature, voltage 60V, aoxidize 3h, in anode oxidation process with
750rpm/min is stirred continuously, in titanium plate surface in-situ preparation titanium dioxide nano-belts array photoelectric pole, after oxidation
Titanium sheet is placed in Muffle furnace, 550 DEG C of calcining 2h.
Two, graphite phase carbon nitride nanometer sheet colloidal solution is prepared.
13g melamine is put into crucible with cover, is placed in Muffle furnace 520 DEG C, calcines 2h, 5 DEG C/min of heating rate,
It is ground to no obvious granular sensation with agate mortar after calcining, body phase graphite phase carbon nitride is made.
It takes 4g body phase graphite phase carbon nitride to be placed in the 50ml concentrated sulfuric acid, stirs 10h at 25 DEG C, obtain suspension.It will be suspended
Liquid is added in 350ml deionized water, and ultrasound removing 20h carries out being washed to neutrality obtaining graphite-phase nitrogen using the method for suction filtration
Change carbon nanosheet, by azotized carbon nano piece Ultrasonic Pulverization 2.5h and is settled to 2.5L.
Three, preparation graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode.
Taking graphite phase carbon nitride nanometer sheet colloidal solution made from 100ml step 2 is electrolyte, titanium dioxide nano-belts
Cathode is made in array photoelectric pole, and platinized platinum makees anode, and the electrochemical deposition 30min under 5V voltage is placed in 101 DEG C of temperature strips in drying box
It is dried under part.
Four, the titanium dioxide nano-belts complex light electrode of graphite phase carbon nitride and graphene co-deposition is prepared.
Graphite oxide is prepared using Hummers method is improved, is added after graphite powder and sodium nitrate are mixed according to mass ratio 1:0.5
Enter in the concentrated sulfuric acid, 30min is stirred in ice bath, the potassium permanganate solid of 3.5 times of graphite powder quality is added, reaction temperature is lower than 10
DEG C, 9.5h is stirred, water is added, 23h is stirred under the conditions of 98 DEG C of temperature, 30%H is added2O2And stir evenly, with 5% HCl
With deionized water cleaning and centrifugal filtration, graphite oxide can be prepared by.
Take 20mg graphite oxide in 1L water, it is 20mg/L graphene oxide dispersion that ultrasound removing 3h, which obtains concentration, with
Graphene oxide dispersion is as electrolyte, and graphite phase carbon nitride doping titanium dioxide nano band array obtained is multiple in step 3
Light combination electrode is cathode, and platinized platinum deposits 5min as anode, deposition voltage 2V.
Example IV
A kind of preparation method of complex light electrode, is prepared according to the following steps:
One, titanium dioxide nano-belts array photoelectric pole is prepared, and does calcination processing.
Titanium sheet is cut into 100mm × 10mm × 0.2mm bar shaped paillon, Ti content > 99.9% in titanium sheet successively passes through
Hydrofluoric acid clean, 600 mesh, 1000 mesh and 2000 mesh sand paper sanding and polishings, respectively in deionized water, acetone: ethyl alcohol=1:1
(vol) and in deionized water it is cleaned by ultrasonic 10min, is put into deionized water and seals up for safekeeping, obtained anodic oxidation prepares titanium dioxide and receives
Base material of the rice with array.
Pretreated titanium sheet is as anode, using the platinized platinum of identical size as cathode, electrolyte 0.75wt%NH4F
With 99% ethylene glycol 100ml mixed solution, 25 DEG C of reaction temperature, voltage 65V are controlled, aoxidizes 4h, and in anodic oxidation
It is stirred continuously in journey with 800rpm/min, in titanium plate surface in-situ preparation titanium dioxide nano-belts array photoelectric pole, will have been aoxidized
Complete titanium sheet is placed in Muffle furnace 550 DEG C, calcines 2h.
Two, graphite phase carbon nitride nanometer sheet colloidal solution is prepared.
15g melamine is put into crucible with cover, 550 DEG C of calcinings 2h, 5 DEG C/min of heating rate in Muffle furnace are placed in.
It is ground to no obvious granular sensation with agate after calcining, body phase graphite phase carbon nitride is made.
It takes 5g body phase graphite phase carbon nitride to be placed in the 50ml concentrated sulfuric acid, stirs 10h at 25 DEG C, obtain suspension.It will be suspended
Liquid is added in 400ml deionized water, and ultrasound removing for 24 hours, is washed to neutrality using the method for suction filtration and obtains graphite phase carbon nitride
Nanometer sheet by azotized carbon nano piece Ultrasonic Pulverization 3h and is settled to 3L.
Three, preparation graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode.
Taking graphite phase carbon nitride nanometer sheet colloidal solution made from 100ml step 2 is electrolyte, titanium dioxide nano-belts
Cathode is made in array photoelectric pole, and platinized platinum makees anode, and the electrochemical deposition 30min under 5V voltage is placed in 101 DEG C of temperature strips in drying box
Under part, drying.
Four, the titanium dioxide nano-belts complex light electrode of graphite phase carbon nitride and graphene co-deposition is prepared.
Graphite oxide is prepared using Hummers method is improved, is added after graphite powder and sodium nitrate are mixed according to mass ratio 1:0.5
Enter in the concentrated sulfuric acid, 30min is stirred in ice bath, the potassium permanganate solid of 4 times of graphite powder quality is added, reaction temperature is lower than 10
DEG C, 10h is stirred, water is added, is stirred under the conditions of 98 DEG C of temperature for 24 hours, 30%H is added2O2And stir evenly, with 5% HCl
With deionized water cleaning and centrifugal filtration, graphite oxide can be prepared by.
Take 30mg graphene oxide in 1L water, it is 30mg/L graphene oxide dispersion that ultrasound removing 3h, which obtains concentration,
Using graphene oxide dispersion as electrolyte, graphite phase carbon nitride doping titanium dioxide nano band array obtained in step 3
Composite photoelectric extremely cathode, platinized platinum deposit 5min as anode, deposition voltage 2V.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (10)
1. a kind of preparation method of complex light electrode, which comprises the following steps:
S1: titanium dioxide nano-belts array photoelectric pole is prepared, and does calcination processing；
S2: preparation graphite phase carbon nitride nanometer sheet colloidal solution；
S3: preparation graphite phase carbon nitride doping titanium dioxide nano band array complex light electrode；
S4: the titanium dioxide nano-belts complex light electrode of preparation graphite phase carbon nitride and graphene co-deposition.
2. a kind of preparation method of complex light electrode according to claim 1, which is characterized in that in step S1, pretreatment
Titanium sheet afterwards is as anode, and using the platinized platinum of identical size as cathode, electrolyte is 0.25~0.75wt%NH4F and 90-99%
Ethylene glycol 100ml mixed solution controls 15-25 DEG C of reaction temperature, voltage 55-65V, aoxidizes 2-4h, and with revolving speed 600-
800rpm/min is stirred continuously, and the titanium dioxide nano-belts array photoelectric pole after oxidation is placed in Muffle furnace, calcination processing,
.
3. a kind of preparation method of complex light electrode according to claim 2, which is characterized in that the pretreated step of titanium sheet
Including but not limited to cleaning, sanding and polishing and ultrasonic cleaning.
4. a kind of preparation method of complex light electrode according to claim 3, which is characterized in that Ti content in titanium sheet >
99.9%, titanium sheet specification is 100mm × 10mm × 0.2mm, and the sand paper of sanding and polishing successively selects 600 mesh, 1000 mesh and 2000
Mesh, is cleaned by ultrasonic 10min in deionized water, acetone and alcohol mixeding liquid, deionized water respectively, and the acetone is mixed with ethyl alcohol
The volume ratio of acetone and ethyl alcohol is 1:1 in liquid, places into deionized water and seals up for safekeeping.
5. a kind of preparation method of complex light electrode according to claim 2, which is characterized in that calcination temperature is 550 DEG C,
Calcination time is 2h.
6. a kind of preparation method of complex light electrode according to claim 2, which is characterized in that in step S2, by trimerization
Cyanamide is put into crucible with cover, and 2h is calcined in Muffle furnace, and 5 DEG C/min of heating rate is ground after calcining with agate mortar
To unobvious granular sensation, body phase graphite phase carbon nitride can be prepared by；
3-5g body phase graphite phase carbon nitride is taken to be placed in the 50ml concentrated sulfuric acid, stirring forms suspension under the conditions of 25 DEG C of temperature, will
Suspension is add to deionized water, and ultrasound removing 10-24h is washed to neutrality using the method for suction filtration, obtains graphite-phase nitridation
Carbon nanosheet by azotized carbon nano piece Ultrasonic Pulverization and is settled to 2-3L.
7. a kind of preparation method of complex light electrode according to claim 6, which is characterized in that the melamine is
10-15g, calcination temperature are 450~550 DEG C, mixing time 10-24h, and deionized water volume is 200-400ml, Ultrasonic Pulverization
Time is 2-3h.
8. a kind of preparation method of complex light electrode according to claim 2, which is characterized in that in step S3, take 100ml
Graphite phase carbon nitride nanometer sheet colloidal solution obtained is electrolyte in step S2, and yin is made in titanium dioxide nano-belts array photoelectric pole
Pole, platinized platinum make anode, electrochemical deposition 30min under 1-6V voltage, dry under the conditions of 101 DEG C of temperature.
9. a kind of preparation method of complex light electrode according to claim 2, which is characterized in that in step S4, take 10~
30mg graphite oxide is in 1L water, and it is 10~30mg/L graphene oxide dispersion that 1~3h of ultrasound removing, which obtains concentration, with oxidation
Graphene dispersing solution is as electrolyte, graphite phase carbon nitride doping titanium dioxide nano band array complex light obtained in step S3
Electrode is cathode, and platinized platinum deposits 1-10min as anode, deposition voltage 1-10V.
10. a kind of preparation method of complex light electrode according to claim 9, which is characterized in that by graphite powder and nitric acid
Sodium is added in the concentrated sulfuric acid after mixing according to mass ratio 1:0.5, and 30min is stirred in ice bath, and 3~4 times of graphite powder quality are added
Potassium permanganate solid, reaction temperature be lower than 10 DEG C, stir 8~10h, be added water, under the conditions of 98 DEG C of temperature stir 20~
For 24 hours, 30%H is added2O2And stir evenly, simultaneously centrifugal filtration is cleaned with 5% HCl and deionized water, can be prepared by oxidation stone
Ink.
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