CN116393147B - Synthesis method of triangular flaky cadmium sulfide coated tungsten oxide composite material - Google Patents
Synthesis method of triangular flaky cadmium sulfide coated tungsten oxide composite material Download PDFInfo
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- CN116393147B CN116393147B CN202310387830.3A CN202310387830A CN116393147B CN 116393147 B CN116393147 B CN 116393147B CN 202310387830 A CN202310387830 A CN 202310387830A CN 116393147 B CN116393147 B CN 116393147B
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- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 44
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229910052980 cadmium sulfide Inorganic materials 0.000 title claims abstract description 39
- 238000001308 synthesis method Methods 0.000 title claims abstract description 5
- 239000002073 nanorod Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- 239000000758 substrate Substances 0.000 claims abstract description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 15
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- YKYOUMDCQGMQQO-UHFFFAOYSA-L cadmium dichloride Chemical compound Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000008098 formaldehyde solution Substances 0.000 claims description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 7
- 229910052753 mercury Inorganic materials 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 229910052793 cadmium Inorganic materials 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 229910052717 sulfur Inorganic materials 0.000 claims description 6
- 229910052721 tungsten Inorganic materials 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005253 cladding Methods 0.000 claims description 5
- 239000011593 sulfur Substances 0.000 claims description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 5
- 239000010937 tungsten Substances 0.000 claims description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 claims description 3
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 3
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 3
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 3
- KPGXUAIFQMJJFB-UHFFFAOYSA-H tungsten hexachloride Chemical compound Cl[W](Cl)(Cl)(Cl)(Cl)Cl KPGXUAIFQMJJFB-UHFFFAOYSA-H 0.000 claims description 3
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 230000004298 light response Effects 0.000 abstract description 5
- 238000012546 transfer Methods 0.000 abstract description 4
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000003115 biocidal effect Effects 0.000 abstract description 3
- 239000001569 carbon dioxide Substances 0.000 abstract description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000004332 deodorization Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 239000000446 fuel Substances 0.000 abstract description 3
- 229930195733 hydrocarbon Natural products 0.000 abstract description 3
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 230000006798 recombination Effects 0.000 description 4
- 238000005215 recombination Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 210000001624 hip Anatomy 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
-
- B01J35/23—
-
- B01J35/39—
-
- B01J35/397—
-
- 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
-
- 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 application relates to the technical field of photocatalysis composite materials, in particular to a synthesis method of a triangle flaky cadmium sulfide coated tungsten oxide composite material, which comprises the steps of preparing a tungsten oxide nano rod by a hydrothermal method, and carrying out directional coating growth on a substrate of the tungsten oxide nano rod to obtain the triangle flaky cadmium sulfide composite material coated with tungsten oxide. The synthesized cadmium sulfide coated tungsten oxide composite material has fluorescent characteristic, and a tightly combined heterostructure is formed in the composite material, so that separation and transfer of photo-generated electron-hole pairs can be promoted, an energy band structure can be regulated and controlled, visible light response is enhanced, and photocatalysis performance of the composite material is improved, and the composite material can be applied to aspects of hydrogen production by decomposing water by solar energy, reduction of carbon dioxide into hydrocarbon fuel, degradation of pollutants, antibiosis and deodorization and the like.
Description
Technical Field
The application relates to the technical field of photocatalysis composite materials, in particular to a method for synthesizing a triangle flaky cadmium sulfide coated tungsten oxide composite material.
Background
With the rapid development of industrialization and informatization, the problem of global energy shortage is increasingly severe, and meanwhile, the challenges of climate change are increasingly aggravated and the environment pollution is irreversible, so that the steps of research and development of renewable clean energy and environmental treatment are quickened for students around the world. The photocatalysis technology with the advantages of low cost, energy saving, sustainability, environmental protection and the like can effectively solve the energy and environmental problems, such as the aspects of hydrogen production by decomposing water by solar energy, reduction of carbon dioxide into hydrocarbon fuel, pollutant degradation, antibiosis and deodorization and the like.
At present, most semiconductor photocatalysts have the problems of insufficient solar energy utilization and high photo-generated electron-hole pair recombination rate, so that the photocatalysis efficiency is low. Tungsten oxide (WO) 3 ) The catalyst is a typical catalyst active component, has a band gap between 2.5eV and 3.0eV, has good absorption capacity to ultraviolet light and visible light, has excellent photoactivity, chemical stability and physical stability, and also has the problem that a photon-generated electron-hole pair commonly existing in a single semiconductor catalyst is easy to be compounded. Cadmium sulfide (CdS) is an ideal visible light responsive semiconductor material, simple to synthesize, and has a relatively narrow band gap of about 2.4eV, but it is susceptible to photo-etching in aqueous solution and its photo-generated electron-hole pairs are susceptible to recombination.
In order to solve the problems, the application adopts a method of cladding tungsten oxide by using the semiconductor cadmium sulfide with a narrow band gap, so that a tightly combined heterostructure is formed between the two semiconductors, photo-generated electrons are effectively transferred, the recombination probability of photo-generated electron-hole pairs is reduced, the energy band structure is regulated, in addition, the visible light response can be further enhanced, the photo-corrosion is slowed down, and the activity and stability of the catalyst are effectively improved.
Disclosure of Invention
The application aims to solve the defects in the prior art, and provides a synthesis method of a triangle flaky cadmium sulfide coated tungsten oxide composite material, which can effectively transfer photo-generated electrons, reduce the recombination rate of photo-generated electron-hole pairs, regulate and control an energy band structure, enhance visible light response, slow down photo-corrosion and improve photocatalysis efficiency.
In order to achieve the above purpose, the present application adopts the following technical scheme:
a method for synthesizing a triangle flaky cadmium sulfide coated tungsten oxide composite material comprises the following preparation steps:
step 1: preparing a tungsten oxide nano rod by a hydrothermal method;
step 2: and (3) carrying out directional cladding growth on the substrate of the tungsten oxide nano rod to obtain the triangular flaky cadmium sulfide composite material coated with the tungsten oxide.
Preferably, in step 1, the specific steps include: dissolving a tungsten source in deionized water, sequentially adding thiourea and hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12 hours, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and irradiating for 2-30 minutes under an ultraviolet high-pressure mercury lamp to obtain the blue tungsten oxide nano rod.
Preferably, in step 2, the specific steps include: dissolving a cadmium source in deionized water, adding mercaptopropionic acid, then adjusting the pH to 10-12 by using a 1mol/L NaOH solution, adding a mixed solution of a blue tungsten oxide nano rod and a sulfur source, heating and refluxing at 100 ℃, sampling at different reflux times respectively, and washing and drying the obtained sample.
Preferably, the tungsten source is one or more of sodium tungstate, tungsten hexachloride, and ammonium metatungstate.
Preferably, the cadmium source is one or more of cadmium chloride, cadmium nitrate, cadmium acetate and cadmium sulfate.
Preferably, the sulfur source is one or more of thiourea, sodium sulfide and thioacetamide.
Preferably, in step 2, the reflux time is 0.5 to 3 hours.
By adopting the technical scheme: the tungsten oxide nano rod is completely coated in the tungsten oxide nano rod by cadmium sulfide to form a tightly combined heterostructure; the shape of the cadmium sulfide coated tungsten oxide composite material is isosceles triangle nano-sheets, and the cadmium sulfide coated tungsten oxide composite material has certain thickness and fluorescence characteristic.
Compared with the prior art, the application has the following beneficial effects:
the application constructs the triangle flaky cadmium sulfide/tungsten oxide composite material with a tightly combined heterostructure through directional cladding growth, can effectively realize the separation and transfer of photo-generated electron-hole pairs, regulate and control the energy band structure, enhance the visible light response, slow the photo-corrosion and improve the photo-catalytic activity and stability.
Drawings
FIG. 1 shows a triangle-shaped flaky CdS/WO under 365nm ultraviolet irradiation 3 Fluorescence diagram of the composite material;
FIG. 2 is a diagram of WO in the present application 3 SEM image of nanorods;
FIG. 3 shows a triangle-shaped flaky CdS/WO with a reflow time of 1.5h in the present application 3 SEM images of the composite;
FIG. 4 shows a triangle-shaped flaky CdS/WO with a reflow time of 1.5h in the present application 3 EDS element distribution diagram of the composite material;
FIG. 5 shows a triangle sheet-like CdS/WO with a reflow time of 3h in the present application 3 SEM images of the composite;
FIG. 6 shows WO in the present application 3 Triangle flaky CdS/WO with nanorods and reflux time of 3h 3 XRD pattern of the composite material.
Detailed Description
The following technical solutions in the embodiments of the present application will be clearly and completely described with reference to the accompanying drawings, so that those skilled in the art can better understand the advantages and features of the present application, and thus the protection scope of the present application is more clearly defined. The described embodiments of the present application are intended to be only a few, but not all embodiments of the present application, and all other embodiments that may be made by one of ordinary skill in the art without inventive faculty are intended to be within the scope of the present application.
Referring to fig. 1-6, a method for synthesizing a triangle-shaped flaky cadmium sulfide coated tungsten oxide composite material comprises the following preparation steps:
step 1: preparing a tungsten oxide nano rod by a hydrothermal method;
dissolving a tungsten source in deionized water, sequentially adding thiourea and hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12 hours, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and irradiating for 2-30 minutes under an ultraviolet high-pressure mercury lamp to obtain the blue tungsten oxide nano rod.
Step 2: directional cladding growth is carried out on a substrate of the tungsten oxide nano rod, so that a triangular flaky cadmium sulfide composite material coated with tungsten oxide is obtained;
dissolving a cadmium source in deionized water, adding mercaptopropionic acid, then adjusting the pH to 10-12 by using a 1mol/L NaOH solution, adding a mixed solution of a blue tungsten oxide nano rod and a sulfur source, heating and refluxing for 0.5-3 h at 100 ℃, and washing and drying the obtained sample.
Example 1:
dissolving 1.5mmol of sodium tungstate in 15mL of deionized water, sequentially adding 3mmol of thiourea and 5mmol of hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12h, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and irradiating for 5min under a 400W ultraviolet high-pressure mercury lamp to obtain the blue tungsten oxide nano rod.
Dissolving 2mmol of cadmium chloride in 100mL of deionized water, adding 2mmol of mercaptopropionic acid, then adjusting the pH value to 11 by using 1mol/LNaOH solution, adding the mixed solution of the blue tungsten oxide nanorod and 0.3mmol of thiourea, heating and refluxing for 1.5h at 100 ℃, washing the obtained sample with deionized water for 3 times, washing with absolute ethyl alcohol for one time, and drying in an oven at 60 ℃ for 5h to obtain the triangular flaky cadmium sulfide coated tungsten oxide composite material.
Wherein FIG. 1 is a schematic diagram showing CdS/WO under 365nm ultraviolet irradiation 3 Fluorescence pattern of the composite material, the prepared CdS/WO can be observed 3 The composite material has fluorescent properties. FIG. 2 is WO 3 SEM images of nanorods, which were approximately 3 μm long, were approximately 300nm in diameter. FIG. 3 is a CdS/WO with a reflux time of 1.5h 3 SEM pictures of composite material, cdS/WO can be observed 3 The composite material is in the form ofThe isosceles triangle has two waists of about 2 μm, a base of about 3 μm and a thickness of about 500nm. FIG. 4 is a CdS/WO with a reflux time of 1.5h 3 EDS element distribution diagram of the composite material can clearly observe that the triangular sheet sample consists of Cd, S, W, O, which proves that the cadmium sulfide coats the tungsten oxide to grow.
Example 2:
dissolving 1.5mmol of sodium tungstate in 15mL of deionized water, sequentially adding 3mmol of thiourea and 5mmol of hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12h, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and irradiating for 5min under a 400W ultraviolet high-pressure mercury lamp to obtain the blue tungsten oxide nano rod.
Dissolving 2mmol of cadmium chloride in 100mL of deionized water, adding 2mmol of mercaptopropionic acid, then adjusting the pH value to 11 by using 1mol/LNaOH solution, adding the mixed solution of the blue tungsten oxide nanorod and 0.3mmol of thiourea, heating and refluxing for 3 hours at 100 ℃, washing the obtained sample with deionized water for 3 times, washing with absolute ethyl alcohol for one time, and drying for 5 hours at 60 ℃ in an oven to obtain the triangular flaky cadmium sulfide coated tungsten oxide composite material.
FIG. 5 is a CdS/WO with a reflux time of 3h 3 SEM pictures of composite material, cdS/WO can be observed 3 The morphology and dimensions of the composite material are substantially identical to those of fig. 3. FIG. 6 is WO 3 CdS/WO with nanorods and reflow time of 3h 3 XRD patterns of composite materials, WO prepared in the patterns 3 Triclinic system WO corresponding to nanorod diffraction peak and standard card (JCPDS No. 00-002-0310) 3 Is matched with the characteristic diffraction peak of the (2); cdS/WO prepared 3 The diffraction peak of the composite material is matched with the characteristic diffraction peak of the hexagonal system CdS corresponding to the standard card (JCPDS No. 00-001-0780), and a triclinic system WO is observed 3 Is proved to be CdS/WO 3 A composite material.
Example 3:
dissolving 0.125mmol of ammonium metatungstate in 15mL of deionized water, sequentially adding 3mmol of thiourea and 5mmol of hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12h, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and illuminating for 30min under a 400W ultraviolet high-pressure mercury lamp to obtain the blue tungsten oxide nano rod.
Dissolving 1mmol of cadmium acetate in 100mL of deionized water, adding 1mmol of mercaptopropionic acid, then adjusting the pH value to 10 by using 1mol/LNaOH solution, adding the mixed solution of the blue tungsten oxide nanorod and 0.15mmol of sodium sulfide, heating and refluxing for 1h at 100 ℃, washing the obtained sample with deionized water for 3 times, washing with absolute ethyl alcohol for one time, and drying for 5h at 60 ℃ in an oven to obtain the triangular flaky cadmium sulfide coated tungsten oxide composite material.
Example 4:
dissolving 1.5mmol of tungsten hexachloride in 15mL of deionized water, sequentially adding 3mmol of thiourea and 5mmol of hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12h, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and irradiating for 15min under a 400W ultraviolet high-pressure mercury lamp to obtain the blue tungsten oxide nano rod.
2mmol of cadmium nitrate is dissolved in 100mL of deionized water, 2mmol of mercaptopropionic acid is added, then the pH value is adjusted to 11 by using 1mol/LNaOH solution, the mixed solution of the blue tungsten oxide nanorod and 0.3mmol of thioacetamide is added, the mixture is placed at 100 ℃ for heating reflux for 2 hours, the obtained sample is washed by the deionized water for 3 times, the obtained sample is washed by absolute ethyl alcohol for one time, and the obtained sample is placed in an oven for drying at 60 ℃ for 5 hours, so that the triangular flaky cadmium sulfide coated tungsten oxide composite material can be obtained.
In conclusion, the cadmium sulfide coated tungsten oxide composite material synthesized by the method has fluorescent characteristic, a tightly combined heterostructure is formed in the composite material, separation and transfer of photo-generated electron-hole pairs can be promoted, an energy band structure is regulated and controlled, visible light response is enhanced, photocatalytic performance of the composite material is improved, and the composite material can be applied to aspects of hydrogen production by decomposing water by solar energy, reduction of carbon dioxide into hydrocarbon fuel, pollutant degradation, antibiosis and deodorization and the like.
The description and practice of the application disclosed herein will be readily apparent to those skilled in the art, and may be modified and adapted in several ways without departing from the principles of the application. Accordingly, modifications or improvements may be made without departing from the spirit of the application and are also to be considered within the scope of the application.
Claims (1)
1. The synthesis method of the triangle flaky cadmium sulfide coated tungsten oxide composite material is characterized by comprising the following preparation steps:
step 1: preparing a tungsten oxide nano rod by a hydrothermal method;
step 2: directional cladding growth is carried out on a substrate of the tungsten oxide nano rod, so that a triangular flaky cadmium sulfide composite material coated with tungsten oxide is obtained;
in step 1, the specific steps include: dissolving a tungsten source in deionized water, sequentially adding thiourea and hydroxylamine hydrochloride, fully mixing, transferring to a high-pressure reaction kettle, heating at 200 ℃ for 12 hours, cooling to room temperature, washing for several times to obtain a tungsten oxide nano rod, placing the tungsten oxide nano rod in formaldehyde solution for ultrasonic dispersion, and irradiating for 2-30 min under an ultraviolet high-pressure mercury lamp to obtain a blue tungsten oxide nano rod;
in step 2, the specific steps include: dissolving a cadmium source in deionized water, adding mercaptopropionic acid, then adjusting the pH to 10-12 by using a 1mol/L NaOH solution, adding a mixed solution of a blue tungsten oxide nano rod and a sulfur source, heating and refluxing at 100 ℃, sampling at different reflux times respectively, and washing and drying the obtained sample;
the tungsten source is one or more of sodium tungstate, tungsten hexachloride and ammonium metatungstate;
the cadmium source is one or more of cadmium chloride, cadmium nitrate, cadmium acetate and cadmium sulfate;
the sulfur source is one or more of thiourea, sodium sulfide and thioacetamide;
in the step 2, the reflux time is 0.5-3 h.
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