CN107419294B - A kind of CdS/MoS2/ Mo bilayer core-shell structure optoelectronic pole - Google Patents

A kind of CdS/MoS2/ Mo bilayer core-shell structure optoelectronic pole Download PDF

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CN107419294B
CN107419294B CN201710595922.5A CN201710595922A CN107419294B CN 107419294 B CN107419294 B CN 107419294B CN 201710595922 A CN201710595922 A CN 201710595922A CN 107419294 B CN107419294 B CN 107419294B
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cds
shell structure
optoelectronic pole
mos
cadmium
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CN107419294A (en
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黄柏标
朱相林
王朋
王泽岩
张晓阳
秦晓燕
刘媛媛
张倩倩
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Shandong University
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/01—Products
    • C25B1/02—Hydrogen or oxygen
    • C25B1/04—Hydrogen or oxygen by electrolysis of water
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00—Electrolytic production of inorganic compounds or non-metals
    • C25B1/50—Processes
    • C25B1/55—Photoelectrolysis
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/133—Renewable energy sources, e.g. sunlight

Abstract

The invention discloses a kind of CdS/MoS2The preparation method of/Mo bilayer core-shell structure optoelectronic pole, steps are as follows: using molybdenum net as substrate, using soluble cadmium salt as cadmium source, cadmium metal being deposited on to molybdenum is online, the molybdenum net deposited is placed in hydrogen sulfide atmosphere and is vulcanized to get to CdS/MoS2/ Mo bilayer core-shell structure optoelectronic pole.CdS/MoS prepared by the present invention2The incident photon-to-electron conversion efficiency of/Mo bilayer core-shell structure optoelectronic pole is high, there is biggish application prospect.Through experimental studies have found that CdS/MoS2/Mo bilayer core-shell structure optoelectronic pole optical electro-chemistry H2-producing capacity, photoelectric current is more than three milliamperes in optical electro-chemistry test, in main absorbance region incident photon-to-electron conversion efficiency close to 20%, performance is better than the vulcanization cadmium electrode prepared on tradition FTO glass.

Description

A kind of CdS/MoS2/ Mo bilayer core-shell structure optoelectronic pole
Technical field
The present invention relates to PhotoelectrochemicalTechnique Technique fields, more particularly to a kind of CdS/MoS2/ Mo bilayer core-shell structure photoelectricity Pole and its preparation method and application.
Background technique
The solar energy for being difficult to the low-density collected can be converted to what high density easily utilized using semiconductor light-catalyst Electric energy and chemical energy have become in recent years one of most active research field in the world.It is especially only in terms of optical electro-chemistry produces hydrogen Special advantage causes the extensive concern of countries in the world scientist, thus it is carried out extensive theoretical and experimental study will have it is non- Often important strategy and realistic meaning.
The basic principle of photodissociation aquatic products hydrogen is built upon on the basis of band theory, and whole process can be divided into three Part: (1) generation of carrier.When incident light photons energy is greater than the band gap of semiconductor, electronics will be excited, from valence Band transits to conduction band, while a positively charged hole is left in valence band；(2) separation and migration of carrier.Above-mentioned light Raw electrons and holes are mutually migrated from body to catalyst surface；(3) reaction of the surface carrier with water.When the valence band potential of semiconductor Higher than VO2/H2OWater will generate oxygen by Hole oxidation when=1.23V (vs.NHE, pH=7).When the potential of conduction band is lower than VH+/H2When=0V (vs.NHE, pH=7), water will be reduced to hydrogen by light induced electron.The quantum efficiency of photocatalytic water mainly restricts It is efficiently separated and three processes such as the redox reaction of surface water in the light abstraction width of photochemical catalyst, carrier.
CdS is visible light photocatalytic water catalyst the most typical, and forbidden bandwidth 2.4eV has preferable visible light Absorbent properties.Meanwhile the light induced electron that CdS is generated after excited by visible light can be transferred to material surface, have stronger reduction Ability smoothly can restore hydrogen ion and generate hydrogen, therefore, can play good effect on solving energy problem.But The quantum efficiency of one pack system CdS is low, and light induced electron is easy compound with hole, greatly reduces the efficiency of its photocatalysis performance.For Solve these problems, it is many study the preparation for concentrating on CdS material and it is modified on, conjunction including different-shape and crystal form CdS At the modification of material and the system design of photoelectrocatalysiwater water electrolysis, to improve photoelectric catalytically active.At present mainly by with its He optimizes modification to one pack system CdS at the compound of co-catalyst.Transition metal, especially some noble metals, is used frequently as The co-catalyst of catalysis material.It is expensive but since noble metal nature reserves are limited, it will increase the conjunction of photocatalytic system At cost；Also researcher utilizes MoS2As auxiliary agent, CdS/MoS is prepared for by high temperature sintering technique2Compound production hydrogen light is urged Agent, but the preparation method temperature is higher, is unfavorable for the structure regulating of catalyst and the further investigation of its architecture element.
To sum up, in all problems for restricting photocatalysis technology practical application at present, it is most important that improve photochemical catalyst pair The utilization efficiency of luminous energy.Wherein how to improve the carrier transport efficiency of photochemical catalyst is a research emphasis, is had critically important Theoretical and practical significance.
Summary of the invention
In view of the above shortcomings of the prior art, the purpose of the present invention is to provide a kind of CdS/MoS2/ Mo bilayer nucleocapsid knot Structure optoelectronic pole and preparation method thereof.Optoelectronic pole of the invention has special CdS/MoS2/ Mo bilayer core-shell structure, and to be formed CdS/MoS2Hetero-junctions can be used for producing hydrogen for efficient optical electro-chemistry.
To achieve the above object, the present invention adopts the following technical scheme:
The first aspect of the present invention provides a kind of CdS/MoS2The preparation method of/Mo bilayer core-shell structure optoelectronic pole, step It is as follows:
Using molybdenum net as substrate, using soluble cadmium salt as cadmium source, cadmium metal is deposited on to the molybdenum that molybdenum is online, will deposit Net, which is placed in hydrogen sulfide atmosphere, to be vulcanized to get CdS/MoS is arrived2/ Mo bilayer core-shell structure optoelectronic pole.
In above-mentioned preparation method, uses concentrated hydrochloric acid and concentrated alkali solution to be cleaned by ultrasonic respectively on molybdenum net, then uses deionized water again, Ethyl alcohol, acetone ultrasonic cleaning.
In above-mentioned preparation method, the solubility cadmium salt is selected from cadmium nitrate, caddy or cadmium acetate.
In above-mentioned preparation method, it is online by way of control deposition voltage and sedimentation time cadmium metal to be deposited on molybdenum.
In above-mentioned preparation method, it is preferred that the deposition voltage is -1.5 to -2.0V, sedimentation time 600-1200s.
In above-mentioned preparation method, the temperature of vulcanization is 300 DEG C -600 DEG C.
The second aspect of the present invention provides above-mentioned CdS/MoS2/ Mo bilayer core-shell structure optoelectronic pole is in light hydrolytic hydrogen production Application.
The third aspect of the present invention provides a kind of smooth hydrolytic hydrogen production system, and the smooth hydrolytic hydrogen production system is with above-mentioned CdS/MoS2As working electrode, platinum electrode is used as to electrode/Mo bilayer core-shell structure optoelectronic pole, is saturated silver/silver chloride electrode As reference electrode.
Further, also include in the smooth hydrolytic hydrogen production system: electrolyte solution；The electrolyte solution is preferred are as follows: 0.25 mol/L vulcanized sodium, 0.35 mol/L sodium sulfite.
Beneficial effects of the present invention:
(1) CdS/MoS of the invention2The preparation method of/Mo bilayer core-shell structure optoelectronic pole is simple, using molybdenum net as base Bottom forms cadmium metal layer in molybdenum deposited thereon by control deposition voltage and sedimentation time parameter；Then in hydrogen sulfide atmosphere Vulcanized, while CdS is generated, metal Mo is by partial vulcanization at MoS2, ultimately form CdS/MoS2/ Mo bilayer nucleocapsid knot Structure optoelectronic pole, preparation process are reacted without high temperature sintering.
(2) CdS/MoS prepared by the present invention2/ Mo bilayer core-shell structure optoelectronic pole has special CdS/MoS2/ Mo is double-deck Core-shell structure, and form CdS/MoS2Hetero-junctions promotes carrier separation.
(3) CdS/MoS prepared by the present invention2The incident photon-to-electron conversion efficiency of/Mo bilayer core-shell structure optoelectronic pole is high, has biggish Application prospect.Through experimental studies have found that CdS/MoS2/Mo bilayer core-shell structure optoelectronic pole optical electro-chemistry H2-producing capacity, photoelectrochemical Learning photoelectric current in test is more than three milliamperes, and in main absorbance region incident photon-to-electron conversion efficiency close to 20%, performance is better than tradition FTO glass The vulcanization cadmium electrode prepared on glass.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the X ray picture of optoelectronic pole of the present invention；
Fig. 2 is that the SEM of optoelectronic pole of the present invention schemes；
Fig. 3 is that the XPS of optoelectronic pole of the present invention schemes；In figure, A is the XPS without HCl treatment surface, and B is that HCl treatment is molten XPS after falling CdS；
Fig. 4 is photoelectric current comparison diagram of the present invention；
Fig. 5 is light photoelectric conversion efficiency comparison diagram of the present invention.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
It is most important in all problems that restrict photocatalysis technology practical application at present as background technique is introduced It is to improve photochemical catalyst to the utilization efficiency of luminous energy.Based on this, the invention proposes a kind of CdS/MoS2/ Mo bilayer core-shell structure Optoelectronic pole and preparation method thereof.
In a kind of embodiment of the application, a kind of CdS/MoS is provided2The system of/Mo bilayer core-shell structure optoelectronic pole Preparation Method, steps are as follows:
(1) it uses concentrated hydrochloric acid and concentrated alkali solution to be cleaned by ultrasonic respectively 10 hours on molybdenum net, then uses deionized water, ethyl alcohol, third The surface-brightening of ketone ultrasonic cleaning；
(2) soluble cadmium salt is dissolved in deionized water；
(3) that cadmium metal is deposited on molybdenum by way of control deposition voltage and sedimentation time is online；
(4) the molybdenum net deposited is placed in hydrogen sulfide atmosphere can be obtained desired photoelectricity in 300 DEG C of -600 DEG C of vulcanizations Pole.
As a preferred option, the soluble cadmium salt is cadmium nitrate, caddy or cadmium acetate.
As a preferred option, the deposition voltage is -1.5 to -2.0V, sedimentation time 600-1200s.Deposition voltage It will affect the cadmium metal deposition effect online in molybdenum with parameters such as sedimentation times, so that the performance of the cadmium sulfide generated is influenced, warp Assay optimization discovery can prepare on the net high-sequential, compact structure in molybdenum using the deposition voltage and sedimentation time of the application Cadmium sulfide layer.
In order to enable those skilled in the art can clearly understand the technical solution of the application, below with reference to tool The technical solution of the application is described in detail in the embodiment of body.
Test material used in the embodiment of the present invention is the test material of this field routine, can pass through commercial channel It is commercially available.
Embodiment 1:CdS/MoS2The preparation of/Mo bilayer core-shell structure optoelectronic pole
(1) it uses concentrated hydrochloric acid and concentrated alkali solution to be cleaned by ultrasonic respectively 10 hours on molybdenum net, then uses deionized water, ethyl alcohol, third The surface-brightening of ketone ultrasonic cleaning；
(2) soluble cadmium salt is dissolved in deionized water；
(3) that cadmium metal is deposited on molybdenum by way of control deposition voltage and sedimentation time is online, and deposition voltage is- 1.8V, sedimentation time 1200s；
(4) the molybdenum net deposited is placed in hydrogen sulfide atmosphere can be obtained desired photoelectricity in 300 DEG C of -600 DEG C of vulcanizations Pole.
Structural analysis is carried out to optoelectronic pole manufactured in the present embodiment, as a result respectively as shown in Figure 1-3, wherein, Fig. 1 is this reality The X-ray diffractogram of optoelectronic pole obtained by example is applied, as seen from the figure, there is the cadmium sulfide of generation good crystallinity MoS do not occur2 With other apparent miscellaneous peaks.Fig. 2 is the SEM figure of optoelectronic pole obtained by the present embodiment, and as seen from the figure, electrode surface is by sheet CdS group Dress package shape.Fig. 3 is the figure of optoelectronic pole XPS obtained by the present embodiment, and Fig. 3 A is the XPS without HCl treatment surface, and Fig. 3 B is hydrochloric acid Processing dissolves away the XPS after CdS.Electrode surface only has CdS layer before handling known to XPS result, without the exposure of Mo substrate.At hydrochloric acid CdS is completely dissolved after reason post-processing, surface MoS2, still without the exposure of Mo substrate.It can conclude that electricity in conjunction with SEM and XPS It is great to have CdS/MoS2/ Mo bilayer core-shell structure.
Application examples 1: photoelectric activity test:
Using optoelectronic pole prepared by embodiment 1 as working electrode, platinum electrode is used as to electrode, is saturated silver/silver chloride electrode As reference electrode, 0.25 mol/L vulcanized sodium, for 0.35 mol/L sodium sulfite as electrolyte solution, light source is 300W xenon Lamp.Photoelectric activity is recorded by three-electrode electro Chemical work station.As a result as shown in Figure 4 and Figure 5.
Photoelectric activity test shows there is the CdS optoelectronic pole prepared on FTO glass relatively, and optoelectronic pole prepared by the present invention has Higher photoelectric conversion efficiency.
The comprehensive optoelectronic pole that the present embodiment obtains that demonstrates of above detection and analysis is that have efficient photoelectric conversion Efficiency.And there is application value in terms of optical electro-chemistry produces hydrogen.
Comparative example 1:
50 ml deionized waters, 1 mM of cadmium nitrate, 1 mM of thiocarbamide and 0.5 milli are added in ptfe autoclave Mole glutathione, by clean FTO glass it is conductive be put into then to react 10 hours under 180 degrees Celsius down obtain CdS/ FTO optoelectronic pole.
Investigate the incident photon-to-electron conversion efficiency of the material of optoelectronic pole prepared by the embodiment of the present invention 1 and comparative example 1, the results showed that, CdS/MoS of the invention2The incident photon-to-electron conversion efficiency of/Mo bilayer core-shell structure optoelectronic pole is apparently higher than the preparation of documents 1 CdS/FTO optoelectronic pole.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.

Claims (9)

1. a kind of CdS/MoS2The preparation method of/Mo bilayer core-shell structure optoelectronic pole, which is characterized in that steps are as follows: with molybdenum net work For substrate, using soluble cadmium salt as cadmium source, cadmium metal is deposited on to molybdenum is online, the molybdenum net deposited is placed in hydrogen sulfide atmosphere In vulcanized to get to CdS/MoS2/ Mo bilayer core-shell structure optoelectronic pole.
2. preparation method according to claim 1, which is characterized in that the solubility cadmium salt is selected from cadmium nitrate, caddy Or cadmium acetate.
3. preparation method according to claim 1, which is characterized in that by way of control deposition voltage and sedimentation time It is online that cadmium metal is deposited on molybdenum.
4. preparation method according to claim 3, which is characterized in that the deposition voltage is -1.5 to -2.0V, when deposition Between be 600-1200s.
5. preparation method according to claim 1, which is characterized in that the temperature of vulcanization is 300 DEG C -600 DEG C.
6. the CdS/MoS that the described in any item methods of claim 1-5 are prepared2/ Mo bilayer core-shell structure optoelectronic pole.
7. CdS/MoS as claimed in claim 62Application of/Mo bilayer core-shell structure the optoelectronic pole in light hydrolytic hydrogen production.
8. a kind of smooth hydrolytic hydrogen production system, which is characterized in that the smooth hydrolytic hydrogen production system is with CdS/ as claimed in claim 7 MoS2As working electrode, platinum electrode is used as to electrode/Mo bilayer core-shell structure optoelectronic pole, is saturated silver/silver chloride electrode conduct Reference electrode.
9. light hydrolytic hydrogen production system as claimed in claim 8, which is characterized in that also include in the smooth hydrolytic hydrogen production system: Electrolyte solution；The electrolyte solution are as follows: 0.25 mol/L vulcanized sodium, 0.35 mol/L sodium sulfite.
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