CN110327959B - BiVO4@CdIn2S4/g-C3N4Visible light response photocatalyst and preparation method thereof - Google Patents
BiVO4@CdIn2S4/g-C3N4Visible light response photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 229910002915 BiVO4 Inorganic materials 0.000 title claims abstract description 30
- 230000004298 light response Effects 0.000 title claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 19
- 239000002243 precursor Substances 0.000 claims abstract description 11
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 48
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 27
- 238000000227 grinding Methods 0.000 claims description 21
- 239000000047 product Substances 0.000 claims description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 19
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 238000001354 calcination Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 15
- 239000007795 chemical reaction product Substances 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 12
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 10
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000004202 carbamide Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 5
- 150000001621 bismuth Chemical class 0.000 claims description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 5
- 150000001661 cadmium Chemical class 0.000 claims description 4
- 150000002471 indium Chemical class 0.000 claims description 4
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical group O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 239000002131 composite material Substances 0.000 abstract description 6
- 239000000969 carrier Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 15
- 239000001257 hydrogen Substances 0.000 description 15
- 229910052739 hydrogen Inorganic materials 0.000 description 15
- 239000010410 layer Substances 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002135 nanosheet Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 230000009286 beneficial effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 229910052976 metal sulfide Inorganic materials 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- PSCMQHVBLHHWTO-UHFFFAOYSA-K indium(iii) chloride Chemical compound Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 description 3
- 238000003760 magnetic stirring Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000001132 ultrasonic dispersion Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012429 reaction media Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- QYIGOGBGVKONDY-UHFFFAOYSA-N 1-(2-bromo-5-chlorophenyl)-3-methylpyrazole Chemical compound N1=C(C)C=CN1C1=CC(Cl)=CC=C1Br QYIGOGBGVKONDY-UHFFFAOYSA-N 0.000 description 1
- KKMOSYLWYLMHAL-UHFFFAOYSA-N 2-bromo-6-nitroaniline Chemical compound NC1=C(Br)C=CC=C1[N+]([O-])=O KKMOSYLWYLMHAL-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
-
- B01J35/39—
-
- B01J35/61—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/10—Catalysts for performing the hydrogen forming reactions
- C01B2203/1041—Composition of the catalyst
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention provides a BiVO4@CdIn2S4/g‑C3N4A visible light response photocatalyst and a preparation method thereof relate to the technical field of photocatalysis. Preparation of few-lamellar g-C3N4And CdIn in monolithic or minority layer2S4Then, g-C is added3N4And CdIn2S4Mixing in solvent, evaporating to obtain CdIn2S4/g‑C3N4Mixing; then adding CdIn2S4/g‑C3N4Mixture with BiVO4The precursor reacts for 3-5h at the temperature of 100-4@CdIn2S4/g‑C3N4The visible light is responsive to the photocatalyst. Through g-C3N4The multicomponent metallic sulfide CdIn2S4And BiVO4The heterojunction composite system can be constructed, the separation efficiency of photo-generated charges is improved, the service life of photo-generated carriers is prolonged, and the photocatalyst has a good photocatalytic effect and a wide application prospect.
Description
Technical Field
The invention relates to the technical field of photocatalysis, and in particular relates to BiVO4@CdIn2S4/g-C3N4Visible light responsive photocatalysisAn agent and a preparation method thereof.
Background
Energy shortage and environmental deterioration are two major problems facing human beings at present. With the rapid increase of energy demand, solar energy utilization technology is receiving more and more attention. Converting solar energy into chemical energy is a challenging task. The hydrogen is produced by water decomposition by using the photocatalytic material, so that organic pollutants can be degraded by using light on one hand, and solar energy is directly converted into hydrogen energy on the other hand. Hydrogen can be stored, the thermal efficiency is high, it is the ideal clean energy, also is the important chemical raw material. The hydrogen production by photolysis of water can avoid the generation of byproduct carbon dioxide in the existing hydrogen production method, and is more environment-friendly. Therefore, the photocatalytic material has double application prospects in the aspects of solving energy and environmental problems.
The existing photocatalytic material is generally TiO2Material, TiO2Only ultraviolet light responds, the energy of the ultraviolet light only accounts for about 4% of the energy of the sunlight, and the energy of the visible light accounts for 43% of the energy of the sunlight. In a research of the last decade, visible light-responsive photocatalysts are favored, of which metal sulfides are a typical representative. The metal sulfide has narrow forbidden band width and good chemical stability, has stronger light absorption in a visible light region, and can effectively improve the utilization rate of light energy. But the photocatalytic activity of pure metal sulfides is low. The inventor researches and discovers that factors such as the microscopic morphology of the catalyst, the photo-generated electron-hole pair conductive carrier, the cocatalyst and the like play a great influence role in the water decomposition reaction besides the visible light absorption capacity.
Disclosure of Invention
The invention aims to provide a BiVO4@CdIn2S4/g-C3N4Preparation method of visible light response photocatalyst, g-C3N4The multicomponent metallic sulfide CdIn2S4And BiVO4A heterojunction composite system is constructed, and the photo-generated charge separation efficiency is improved, so that the photo-catalytic effect is good.
Another object of the present invention is to provide a BiVO4@CdIn2S4/g-C3N4The visible light responds to the photocatalyst, and the photocatalyst has good photocatalytic performance and high hydrogen production effect.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a BiVO4@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst comprises the following steps:
few-lamellar layer g-C3N4Preparation: calcining carbon nitride precursor to obtain low-sheet g-C3N4；
Monolithic or minority layer CdIn2S4Preparation: respectively dissolving divalent cadmium salt, trivalent indium salt and thioacetamide in a first solvent according to a molar ratio, mixing, heating at 140-200 ℃ for 22-30h, and separating, washing, drying and grinding to obtain a reaction product; placing the reaction product in a mixed solution, heating and refluxing for 1-3 h to obtain single-chip or few-chip CdIn2S4Wherein the mixed solution is an aqueous solution containing sodium bicarbonate, isopropanol and polyvinyl pyrrolidone;
CdIn2S4/g-C3N4preparation of a mixture: subjecting said g-C to3N4And the CdIn2S4Mixing the obtained product in a second solvent, evaporating the second solvent to dryness, and drying to obtain CdIn2S4/g-C3N4Mixing;
BiVO4@CdIn2S4/g-C3N4preparation: dissolving trivalent bismuth salt in an acetic acid solution to obtain a first solution, dissolving ammonium metavanadate in an ammonia water solution to obtain a second solution, and slowly mixing the first solution and the second solution to obtain a third solution; adjusting the pH value of the third solution to 7-8, stirring for 30-60 min, and adding the CdIn 2S4/g-C3N4Ultrasonically dispersing the mixture, reacting for 2-4h at 140-200 ℃, cooling, separating, washing, drying and grinding to obtain BiVO4@CdIn2S4/g-C3N4The visible light is responsive to the photocatalyst.
Further, in a preferred embodiment of the present invention, the step of calcining the carbon nitride precursor comprises:
heating to 500-550 ℃ at a first heating rate, calcining for 1-3 h, and cooling and grinding the obtained calcined product to obtain a first calcined substance; then, the user can use the device to perform the operation,
heating the first calcined substance to 500-550 ℃ at a second heating rate, calcining for 1-3 h, cooling and grinding the calcined product to obtain the few-lamellar g-C3N4。
Further, in a preferred embodiment of the present invention, the first temperature-raising speed is 1 to 2 ℃/min, and the second temperature-raising speed is 3 to 5 ℃/min.
Further, in a preferred embodiment of the present invention, the carbon nitride precursor is selected from one or more of urea, cyanamide, dicyandiamide and melamine.
Further, in a preferred embodiment of the present invention, the first solvent is an ethanol aqueous solution.
Further, in a preferred embodiment of the present invention, the concentration of the sodium bicarbonate in the mixed solution is 0.1 to 0.2g/ml, the volume concentration of the isopropanol is 8 to 12% v/v, and the concentration of the polyvinylpyrrolidone is 4 to 6 mg/ml.
Further, in a preferred embodiment of the present invention, the second solvent is one or more selected from the group consisting of absolute ethanol, polyethylene glycol and pyridine.
Further, in a preferred embodiment of the present invention, CdIn2S4/g-C3N4In the step of preparing the mixture, the CdIn2S4And said g-C3N4The mass ratio of (A) to (B) is 0.3-0.8: 1.
Further, in the preferred embodiment of the present invention, BiVO4@CdIn2S4/g-C3N4In the preparation step, the CdIn2S4/g-C3N4The adding amount of the mixture in the third solution is 2-12 mg/ml.
The invention also provides BiVO4@CdIn2S4/g-C3N4The visible light response photocatalyst is prepared according to the preparation method.
BiVO of the embodiment of the invention4@CdIn2S4/g-C3N4The visible light response photocatalyst and the preparation method thereof have the beneficial effects that:
few-lamellar layer g-C3N4The photocatalyst is a polymer semiconductor visible light photocatalyst, has stable structure and hydrogen production performance by photocatalytic water decomposition, can be repeatedly used, and is environment-friendly. The few-lamellar structure provides a larger specific surface area for photocatalytic hydrolysis hydrogen production, and the quantum yield is high. Monolithic or minority layer CdIn2S4During preparation, the CdIn is effectively regulated and controlled by heating the reaction product in an aqueous solution containing sodium bicarbonate, isopropanol and polyvinyl pyrrolidone in a refluxing manner2S4The nucleation and growth of the catalyst are carried out, so that the metal sulfide with a single layer or less layers is formed, the formation of a blocky structure is avoided, and the hydrogen production efficiency is improved.
Furthermore, BiVO4The band gap is 2.40eV, the valence band and the conduction band are respectively positioned at +2.70eV and +0.30 eV, and the photo-generated electron-hole pair has stronger redox capability. Through in-situ compounding of BiVO4And CdIn2S4/g-C3N4The mixture can regulate and control the particle size of a product, construct a heterojunction composite system, improve the charge transmission capability, realize high photo-generated charge separation efficiency, prolong the service life of photo-generated carriers and ensure that the photocatalyst has a good photo-catalytic hydrogen production effect.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Following are embodiments of the present inventionBiVO (b)4@CdIn2S4/g-C3N4The visible light response photocatalyst and the preparation method thereof are concretely explained.
The embodiment of the invention provides a BiVO4@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst comprises the following steps:
s1, few layers g-C3N4Preparation: calcining carbon nitride precursor to obtain low-sheet g-C 3N4。
Further, in this step, the step of calcining the carbon nitride precursor is: heating to 500-550 ℃ at a first heating rate, calcining for 1-3 h, cooling the obtained calcined product, and grinding to obtain a first calcined product; then heating the first calcined substance to 500-550 ℃ at a second heating rate, calcining for 1-3 h, cooling the obtained calcined product, and grinding to obtain the few-lamellar g-C3N4。
Further, in the step, the first temperature rise speed is 1-2 ℃/min; the second temperature rise speed is 3-5 ℃/min. Firstly heating to 500-550 ℃ at a lower heating rate for calcination, cooling and grinding the calcined product, then heating to 500-550 ℃ at a higher heating rate for calcination again, and thus g-C can be calcined3N4The shape of the nano-sheet is regulated, so that the nano-sheet is beneficial to driving of a nano-sheet structure, separation and transfer of photon-generated carriers are facilitated, and the hydrogen production efficiency is improved.
Further, in this step, the carbon nitride precursor is selected from one or more of urea, cyanamide, dicyandiamide, and melamine. More preferably, the carbon nitride precursor is urea.
Further, in the step, after the calcined product is cooled, grinding the calcined product by adopting zirconia balls with a ball-to-material ratio of 1:7 for 0.5-1 h. The surface stress of the product can be removed by grinding after calcination, and the particles form a few-sheet structure through repeated crushing-cold welding-crushing processes, thereby being beneficial to the rapid transmission of charges and the compounding with other components.
S2, monolithic or minority layer CdIn2S4Preparation: respectively dissolving divalent cadmium salt, trivalent indium salt and thioacetamide in a first solvent according to a molar ratio, mixing, heating at 140-200 ℃ for 22-30h, and separating, washing, drying and grinding to obtain a reaction product; placing the reaction product in a mixed solution, heating and refluxing for 1-3 h to obtain single-chip or few-chip CdIn2S4Wherein the mixed solution is an aqueous solution containing sodium bicarbonate, isopropanol and polyvinyl pyrrolidone.
Further, In the step, cadmium acetate is selected as a divalent cadmium salt, indium chloride is selected as a trivalent indium salt, and cadmium acetate, indium chloride and thioacetamide are respectively weighed according to the mass ratio of Cd to In to S being 1:2: 4.
Further, in this step, the first solvent is an aqueous ethanol solution. Under the action of alcoholic solution, a thin-layer nanosheet structure can be obtained, and the nanosheets are beneficial to separation and transfer of photon-generated carriers, so that the hydrogen production efficiency is improved.
Further, in the step, the concentration of the sodium bicarbonate in the mixed solution is 0.1-0.2 g/ml, the volume concentration of the isopropanol is 8-12% v/v, and the concentration of the polyvinylpyrrolidone is 4-6 mg/ml.
Further, in the step, the feed-liquid ratio of the reaction product to the mixed liquid is 1-10 mg/ml.
Further, in the step, the temperature of the reaction product in the mixed solution is heated and refluxed to be 80-110 ℃. The reaction product is heated and refluxed in the mixed solution, so that the sample morphology and the dispersion performance of the product are regulated and controlled, the aggregation growth of particles is avoided, and the obtained CdIn2S4The structure is a single-layer structure or a few-layer structure, the specific surface area is larger, and more reactive sites can be provided.
S3，CdIn2S4/g-C3N4Preparation of a mixture: subjecting said g-C to3N4And the CdIn2S4Mixing the obtained product in a second solvent, evaporating the second solvent to dryness, and drying to obtain CdIn2S4/g-C3N4And (3) mixing.
Further, in the step, the second solvent is one or more selected from the group consisting of absolute ethyl alcohol, polyethylene glycol and pyridine. More preferably, the second solvent is selected from anhydrous ethanol.
Further, in the step, a rotary evaporator is adopted to evaporate the second solvent to dryness, the rotary evaporation temperature is 40-50 ℃, and the second solvent is dried for 6 hours at the temperature of 60 ℃ after evaporation to dryness, so that the composite few-piece layer CdIn is obtained2S4/g-C3N4And (3) mixing.
Further, in this step, CdIn2S4And g-C3N4In a mass ratio of 0.3 to 0.8:1, more preferably, CdIn2S4And g-C3N4The mass ratio of (A) to (B) is 0.6: 1.
CdIn by rotary evaporation in absolute ethanol solution2S4And g-C3N4The process is simple, the solvent can be recovered, and the reaction condition is mild.
S4，BiVO4@CdIn2S4/g-C3N4Preparation: dissolving trivalent bismuth salt in an acetic acid solution to obtain a first solution, dissolving ammonium metavanadate in an ammonia water solution to obtain a second solution, and slowly mixing the first solution and the second solution to obtain a third solution; adjusting the pH value of the third solution to 7-8, stirring for 30-60 min, and adding the CdIn2S4/g-C3N4Ultrasonically dispersing the mixture, reacting for 2-4h at 140-200 ℃, cooling, separating, washing, drying and grinding to obtain BiVO4@CdIn2S4/g-C3N4The visible light is responsive to the photocatalyst.
Further, in this step, the trivalent bismuth salt is selected from one or more of bismuth nitrate, bismuth chloride, bismuth acetate, and bismuth citrate. More preferably, the trivalent bismuth salt is bismuth nitrate. The acetic acid solution is a mixed solution of acetic acid and water in a volume ratio of 1: 1. The concentration of bismuth nitrate in the acetic acid solution is 2-5 mol/L.
Further, in this step, the aqueous ammonia solution was a mixed solution of aqueous ammonia (containing 25 wt% of ammonia) and water in a volume ratio of 3: 1. The concentration of the ammonium metavanadate in the ammonia water solution is 2-5 mol/L.
Further, in the step, adjusting the pH value of the third solution to 7-8 by using ammonia water, specifically, adjusting the process as follows: and (3) firstly adding 20ml of ammonia water in the adjusting process, and then slowly dropwise adding the ammonia water until the pH value is 7-8.
Further, in this step, CdIn2S4/g-C3N4The addition amount of the mixture in the third solution is 2-12 mg/ml, and more preferably, CdIn2S4/g-C3N4The adding amount of the mixture in the third solution is 8-10 mg/ml.
Further, in the step, the ultrasonic dispersion condition is that the ultrasonic dispersion is carried out for 1-2 hours under the power of 400-600W. Under the action of ultrasonic waves, the size of a product can be effectively reduced, and the product is degraded into a nano-sheet structure.
BiVO4The band gap is 2.40eV, the valence band and the conduction band are respectively positioned at +2.70eV and +0.30eV, and the photo-generated electron-hole pair has stronger redox capability. By hydrothermal reaction, in CdIn2S4/g-C3N4BiVO is coated on the surface of the mixture4Form BiVO4@CdIn2S4/g-C3N4The core-shell structure is more beneficial to charge transfer between interfaces, inhibits the recombination of photon-generated carriers and improves the photocatalytic activity.
The embodiment of the invention also provides BiVO4@CdIn2S4/g-C3N4The visible light response photocatalyst is prepared according to the preparation method.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
BiVO provided by the embodiment4@CdIn2S4/g-C3N4A visible light-responsive photocatalyst, prepared according to the steps of:
(1) 10g of urea was placed in an alumina crucible with a lid and placed in a muffle furnace at a rate of 1 ℃/min Heating to 550 deg.C, holding for 2h, naturally cooling to room temperature, grinding for 0.5h to obtain sample, placing into aluminum oxide crucible with cover, heating to 500 deg.C at 4 deg.C/min in muffle furnace, holding for 3h, naturally cooling to room temperature, grinding for 0.5h to obtain few-lamellar g-C3N4And (3) powder.
(2) Under the condition of room temperature, cadmium acetate, indium chloride and thioacetamide are weighed according to the mass ratio of Cd to In to S of 1:2:4 and are respectively dissolved In 30ml of ethanol water solution, the mixture is magnetically stirred for 30min, the mixture is transferred into a polytetrafluoroethylene lining, and then the polytetrafluoroethylene lining is placed into a stainless steel reaction kettle and is heated and reacted for 24h at the temperature of 180 ℃. After the reaction is finished, centrifuging at 1000rpm for 30min, washing with deionized water for 3 times, then washing with absolute ethyl alcohol for three times, drying at 60 ℃ for 12 hours, and grinding to obtain a reaction product A.
(3) Adding the reaction product A in the step (2) into a reflux device which is connected with a condensation pipe and a 500ml three-neck flask with a thermometer, adding 10g of sodium bicarbonate, 10ml of isopropanol, 0.5g of polyvinylpyrrolidone and 100ml of deionized water, placing on an electric heating sleeve with magnetic stirring for heating and refluxing for 2h, filtering, washing for 3 times by using the deionized water, then washing for three times by using absolute ethyl alcohol to obtain single-piece or few-piece layer CdIn 2S4And (3) powder.
(4) The obtained CdIn2S4And g-C3N4Mixing the sample in 50ml of absolute ethyl alcohol according to the mass ratio of 0.6:1, evaporating to dryness in a vacuum rotary evaporator, and drying in a drying oven at 60 ℃ for 6h to obtain the composite few-layer CdIn2S4/g-C3N4And (3) mixing.
(5) In volume ratio V(acetic acid)：V(Water)1: 1 preparing acetic acid solution, accurately weighing 1g of bismuth nitrate and dissolving in the acetic acid solution, and magnetically stirring for 20min to fully dissolve the bismuth nitrate. In volume ratio V(Ammonia water)：V(Water)3: 1 preparing an ammonia water solution, accurately weighing 0.2g of ammonium metavanadate and dissolving the ammonium metavanadate in the ammonia water solution, and completely dissolving the ammonium metavanadate by magnetic stirring for 20 min.
(6) Slowly mixing the two solutions in the step (5), magnetically stirring for 1h, and adjusting pH to 7 with ammonia water (adding the solution during the adjustment process)20mL of ammonia water, slowly adding dropwise until the pH is 7), and adding CdIn after continuously stirring for 0.5h2S4/g-C3N4Ultrasonically dispersing the mixture for 1h, transferring the mixture into a high-pressure reaction kettle container containing a polytetrafluoroethylene lining, reacting for 3h at 160 ℃, cooling the sample to room temperature, taking out the sample, placing the sample into a centrifuge tube, centrifuging, repeatedly washing with distilled water and absolute ethyl alcohol for three times, drying at 60 ℃ for 18h, and grinding to obtain BiVO4@CdIn2S4/g-C3N4The visible light responds to the photocatalyst sample.
Example 2
BiVO provided by the embodiment4@CdIn2S4/g-C3N4A visible-light-responsive photocatalyst, which is different from example 1 in that:
the step (1) is as follows: putting 10g of urea into an alumina crucible with a cover, heating to 550 ℃ in a muffle furnace at the speed of 1 ℃/min, preserving heat for 5h, naturally cooling to room temperature, taking out and grinding for 1h to obtain g-C3N4And (3) powder.
Comparative example 1
This comparative example provides a CdIn2S4/g-C3N4Visible light-responsive photocatalyst, CdIn obtained according to the method of example 12S4/g-C3N4And (3) mixing.
Comparative example 2
This comparative example provides a visible light responsive photocatalyst, obtained according to the following steps:
(1) less lamellar g-C was obtained according to step (1) of example 13N4And (3) powder.
(2) The reaction product a was obtained according to the step (2) of example 1.
(3) The reaction products A and g-C obtained3N4Mixing the sample in 50ml of absolute ethyl alcohol, evaporating to dryness in a vacuum rotary evaporator, and drying in a drying oven at 60 ℃ for 6h to obtain the composite few-lamellar layer CdIn2S4/g-C3N4And (3) mixing.
(4) According to the procedure of the examples(5) And step (6) of obtaining BiVO4@CdIn2S4/g-C3N4The visible light responds to the photocatalyst sample.
Comparative example 3
This comparative example provides a visible light responsive photocatalyst, obtained according to the following steps:
(1) less lamellar g-C was obtained according to step (1) of example 1 3N4And (3) powder.
(2) The less lamellar CdIn was obtained according to the steps (2) and (3) of example 12S4And (3) powder.
(3) In volume ratio V(acetic acid)：V(Water)1: 1 preparing acetic acid solution, accurately weighing 1g of bismuth nitrate and dissolving in the acetic acid solution, and magnetically stirring for 20min to fully dissolve the bismuth nitrate. In volume ratio V(Ammonia water)：V(Water)3: 1 preparing an ammonia water solution, accurately weighing 0.2g of ammonium metavanadate and dissolving the ammonium metavanadate in the ammonia water solution, and completely dissolving the ammonium metavanadate by magnetic stirring for 20 min.
(4) Slowly mixing the two solutions in the step (3), magnetically stirring for 1h, adjusting the pH to 7 with ammonia water (adding 20mL of ammonia water during the adjustment process, then slowly dropwise adding until the pH is 7), and adding the few-lamellar g-C obtained in the step (1) after continuously stirring for 0.5h3N4Powder and the little-sheet layer CdIn obtained in the step (2)2S4Performing ultrasonic dispersion on the powder for 1h, transferring the powder into a high-pressure reaction kettle container with a polytetrafluoroethylene lining, reacting for 3h at 160 ℃, cooling the sample to room temperature, taking out the sample, placing the sample into a centrifuge tube, centrifuging, repeatedly washing with distilled water and absolute ethyl alcohol for three times, drying for 18h at 60 ℃, and grinding to obtain BiVO4@CdIn2S4/g-C3N4The visible light responds to the photocatalyst sample.
Test examples measurement of Hydrogen production Performance
The products obtained in examples 1-2 and comparative examples 1-3 were used as catalysts for photocatalytic reactions carried out in a 500mL Pyrex reactor system at a temperature of 25 ℃. The photocatalyst was added to an aqueous solution containing methanol as a reaction medium. The reaction medium is placed in a photoreactor. After the reaction system was purged with argon for 30min, the system was illuminated with visible light (420< lambda < 800nm) for 4h using a 300W xenon lamp (fitted with a filter) that surrounded the side of the photoreactor. Condensed water is introduced in the reactor in an external circulation manner. The photocatalytic effects of the five samples are shown in table 1:
TABLE 1
| Sample (I) | Average hydrogen production rate (first use) | Average hydrogen production rate (after 20 times of use) |
| Example 1 | 519.2μmol/(h·g) | 488.0μmol/(h·g) |
| Example 2 | 457.4μmol/(h·g) | 416.2μmol/(h·g) |
| Comparative example 1 | 361.3μmol/(h·g) | 130.1μmol/(h·g) |
| Comparative example 2 | 422.5μmol/(h·g) | 219.7μmol/(h·g) |
| Comparative example 3 | 417.6μmol/(h·g) | 186.2μmol/(h·g) |
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. BiVO4@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized by comprising the following steps:
few-lamellar layer g-C3N4Preparation: calcining carbon nitride precursor to obtain low-sheet g-C3N4；
Monolithic or minority layer CdIn2S4Preparation: respectively dissolving divalent cadmium salt, trivalent indium salt and thioacetamide in a first solvent according to a molar ratio, mixing, heating at 140-200 ℃ for 22-30h, and separating, washing, drying and grinding to obtain a reaction product; placing the reaction product in a mixed solution, heating and refluxing for 1-3 h to obtain single-chip or few-chip CdIn 2S4Wherein the mixed solution is an aqueous solution containing sodium bicarbonate, isopropanol and polyvinyl pyrrolidone;
CdIn2S4/g-C3N4preparation of a mixture: subjecting said g-C to3N4And the CdIn2S4Mixing the obtained product in a second solvent, evaporating the second solvent to dryness, and drying to obtain CdIn2S4/g-C3N4Mixing;
BiVO4@CdIn2S4/g-C3N4preparation: dissolving trivalent bismuth salt in acetic acid solutionDissolving ammonium metavanadate in an ammonia water solution to obtain a second solution, and slowly mixing the first solution and the second solution to obtain a third solution; adjusting the pH value of the third solution to 7-8, stirring for 30-60 min, and adding the CdIn2S4/g-C3N4Ultrasonically dispersing the mixture, reacting for 2-4h at 140-200 ℃, cooling, separating, washing, drying and grinding to obtain BiVO4@CdIn2S4/g-C3N4The visible light is responsive to the photocatalyst.
2. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that the step of calcining the carbon nitride precursor comprises the following steps:
heating to 500-550 ℃ at a first heating rate, calcining for 1-3 h, and cooling and grinding the obtained calcined product to obtain a first calcined substance; then, the user can use the device to perform the operation,
heating the first calcined substance to 500-550 ℃ at a second heating rate, calcining for 1-3 h, cooling and grinding the calcined product to obtain the few-lamellar g-C 3N4。
3. BiVO according to claim 24@CdIn2S4/g-C3N4The preparation method of the visible-light-responsive photocatalyst is characterized in that the first temperature rise speed is 1-2 ℃/min, and the second temperature rise speed is 3-5 ℃/min.
4. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that the carbon nitride precursor is selected from one or more of urea, cyanamide, dicyandiamide and melamine.
5. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that the first solvent is ethanol water solution.
6. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that in the mixed solution, the concentration of the sodium bicarbonate is 0.1-0.2 g/ml, the volume concentration of the isopropanol is 8-12% v/v, and the concentration of the polyvinylpyrrolidone is 4-6 mg/ml.
7. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that the second solvent is one or more selected from absolute ethyl alcohol, polyethylene glycol and pyridine.
8. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that CdIn 2S4/g-C3N4In the step of preparing the mixture, the CdIn2S4And said g-C3N4The mass ratio of (A) to (B) is 0.3-0.8: 1.
9. BiVO according to claim 14@CdIn2S4/g-C3N4The preparation method of the visible light response photocatalyst is characterized in that BiVO4@CdIn2S4/g-C3N4In the preparation step, the CdIn2S4/g-C3N4The adding amount of the mixture in the third solution is 2-12 mg/ml.
10. BiVO4@CdIn2S4/g-C3N4Visible light-responsive photocatalyst, characterized in that it is according to any one of claims 1 to 9The preparation method is characterized by comprising the following steps.
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