CN107419294A - A kind of CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles - Google Patents
A kind of CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles Download PDFInfo
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- CN107419294A CN107419294A CN201710595922.5A CN201710595922A CN107419294A CN 107419294 A CN107419294 A CN 107419294A CN 201710595922 A CN201710595922 A CN 201710595922A CN 107419294 A CN107419294 A CN 107419294A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- 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
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- 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
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Abstract
The invention discloses a kind of CdS/MoS2The preparation method of/Mo bilayer core shell structure optoelectronic poles, step are as follows:Using molybdenum net as 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 and vulcanized, that is, obtains CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles.CdS/MoS prepared by the present invention2The electricity conversion of/Mo bilayer core shell structure optoelectronic poles is high, there is larger application prospect.Through experimental studies have found that CdS/MoS2/Mo bilayer core shell structure optoelectronic pole optical electro-chemistry H2-producing capacities, photoelectric current is more than three milliamperes in optical electro-chemistry test, in main absorbance region electricity conversion close to 20%, performance is better than the vulcanization cadmium electrode prepared on traditional FTO glass.
Description
Technical field
The present invention relates to PhotoelectrochemicalTechnique Technique field, more particularly to a kind of CdS/MoS2/ Mo bilayer core shell structure photoelectricity
Pole and its preparation method and application.
Background technology
The solar energy for the low-density for being difficult to collect can be changed into what high density easily utilized using semiconductor light-catalyst
Electric energy and chemical energy turn into 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 general principle of photodissociation aquatic products hydrogen is built upon on the basis of band theory, and its whole process can be divided into three
Part:(1) generation of carrier.When incident light photons energy is more than the band gap of semiconductor, electronics will be excited, from valence band
Conduction band is transitted to, while a positively charged hole is left in valence band;(2) separation and migration of carrier.Above-mentioned photoproduction
Electronics and hole are migrated to catalyst surface from body phase;(3) reaction of the surface carrier with water.When the valence band potential of semiconductor is high
In VO2/H2OWater will generate oxygen by Hole oxidation during=1.23V (vs.NHE, pH=7).When the potential of conduction band is less than VH+/H2
During=0V (vs.NHE, pH=7), water will be reduced to hydrogen by light induced electron.The quantum efficiency of photocatalytic water is mainly restricted in light
The light abstraction width of catalyst, carrier efficiently separate and three processes such as the redox reaction of surface water.
CdS is visible ray photocatalytic water catalyst the most typical, and its energy gap is 2.4eV, has preferable visible ray
Absorbent properties.Meanwhile CdS caused light induced electrons after excited by visible light can be transferred to material surface, there is stronger reduction
Ability, it smoothly can reduce hydrogen ion and produce hydrogen, therefore, good effect can be played on solving energy problem.But
One pack system CdS quantum efficiency is low, and light induced electron is easily compound with hole, greatly reduces the efficiency of its photocatalysis performance.For
Solve these problems, it is many study the preparation that concentrates on CdS materials and it is modified on, include different-shape and crystal formation CdS conjunction
Into 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 at the compound of co-catalyst to one pack system CdS.Transition metal, particularly some noble metals, are used frequently as
The co-catalyst of catalysis material.But because noble metal nature reserves are limited, it is expensive, the conjunction of photocatalytic system can be increased
Into 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 ratio 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.
The content of the invention
For above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of CdS/MoS2/ Mo bilayer nucleocapsid knots
Structure optoelectronic pole and preparation method thereof.The optoelectronic pole of the present invention has special CdS/MoS2/ Mo bilayer core shell structures, and to be formed
CdS/MoS2Hetero-junctions, hydrogen is produced available for for efficient optical electro-chemistry.
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of the first aspect of the present invention, there is provided CdS/MoS2The preparation method of/Mo bilayer core shell structure optoelectronic poles, 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, that is, obtains CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles.
In above-mentioned preparation method, molybdenum net is cleaned by ultrasonic with concentrated hydrochloric acid and concentrated alkali solution respectively, then uses deionized water again,
Ethanol, acetone are cleaned by ultrasonic.
In above-mentioned preparation method, the soluble cadmium salt is selected from cadmium nitrate, caddy or cadmium acetate.
In above-mentioned preparation method, it is online by way of controlling deposition voltage and sedimentation time cadmium metal to be deposited on into 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, there is provided above-mentioned CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles are in light hydrolytic hydrogen production
Application.
The third aspect of the present invention, there is provided a kind of smooth hydrolytic hydrogen production system, the smooth hydrolytic hydrogen production system is with above-mentioned
CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles are used as to electrode, saturation silver/silver chloride electrode as working electrode, platinum electrode
As reference electrode.
Further, also included in the smooth hydrolytic hydrogen production system:Electrolyte solution;The electrolyte solution is preferably:
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 poles is simple, and base is used as using molybdenum net
Bottom, by controlling deposition voltage and sedimentation time parameter, cadmium metal layer is formed in molybdenum deposited thereon;Then in hydrogen sulfide atmosphere
Vulcanized, while CdS is generated, metal Mo is by partial vulcanization into MoS2, ultimately form CdS/MoS2/ Mo bilayer nucleocapsid knots
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 poles have 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 electricity conversion of/Mo bilayer core shell structure optoelectronic poles is high, has larger
Application prospect.Through experimental studies have found that CdS/MoS2/Mo bilayer core shell structure optoelectronic pole optical electro-chemistry H2-producing capacities, photoelectrochemical
Photoelectric current is more than three milliamperes in test, and in main absorbance region electricity conversion close to 20%, performance is better than traditional FTO glass
The vulcanization cadmium electrode prepared on glass.
Brief description of the drawings
The Figure of description for forming the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not form the improper restriction to 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
Fall the XPS after CdS;
Fig. 4 is photoelectric current comparison diagram of the present invention;
Fig. 5 is light photoelectric transformation efficiency comparison diagram of the present invention.
Embodiment
It is noted that described further below is all exemplary, it is intended to provides further instruction to the application.It is unless another
Indicate, all technologies used herein and scientific terminology are with 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 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 singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
It is most important in all problems for restricting photocatalysis technology practical application at present as background technology is introduced
It is to improve utilization ratio of the photochemical catalyst to luminous energy.Based on this, the present invention proposes a kind of CdS/MoS2/ Mo bilayer core shell structures
Optoelectronic pole and preparation method thereof.
In a kind of embodiment of the application, there is provided a kind of CdS/MoS2The system of/Mo bilayer core shell structure optoelectronic poles
Preparation Method, step are as follows:
(1) molybdenum net is cleaned by ultrasonic 10 hours with concentrated hydrochloric acid and concentrated alkali solution respectively, then with deionized water, ethanol, third
The surface-brightening of ketone ultrasonic cleaning;
(2) soluble cadmium salt is dissolved in deionized water;
(3) that cadmium metal is deposited on into molybdenum by way of controlling deposition voltage and sedimentation time is online;
(4) the molybdenum net deposited is placed in hydrogen sulfide atmosphere and can obtain desired photoelectricity in 300 DEG C of -600 DEG C of vulcanizations
Pole.
As preferable scheme, the soluble cadmium salt is cadmium nitrate, caddy or cadmium acetate.
As preferable scheme, the deposition voltage is -1.5 to -2.0V, sedimentation time 600-1200s.Deposition voltage
Cadmium metal can be influenceed in the online deposition effect of molybdenum with parameters such as sedimentation times, so as to influence the performance of the cadmium sulfide of generation, warp
Assay optimization is found, high-sequential, compact structure can be on the net prepared in molybdenum using the deposition voltage and sedimentation time of the application
Cadmium sulfide layer.
In order that the technical scheme of the application can clearly be understood by obtaining those skilled in the art, below with reference to tool
The embodiment of body describes the technical scheme of the application in detail.
Test material used is the conventional test material in this area in the embodiment of the present invention, can pass through commercial channel
It is commercially available.
Embodiment 1:CdS/MoS2The preparation of/Mo bilayer core shell structure optoelectronic poles
(1) molybdenum net is cleaned by ultrasonic 10 hours with concentrated hydrochloric acid and concentrated alkali solution respectively, then with deionized water, ethanol, third
The surface-brightening of ketone ultrasonic cleaning;
(2) soluble cadmium salt is dissolved in deionized water;
(3) that cadmium metal is deposited on into molybdenum by way of controlling deposition voltage and sedimentation time is online, deposition voltage for-
1.8V, sedimentation time 1200s;
(4) the molybdenum net deposited is placed in hydrogen sulfide atmosphere and can obtain 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 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 obvious miscellaneous peaks.Fig. 2 is the SEM figures of optoelectronic pole obtained by the present embodiment, and as seen from the figure, electrode surface is by sheet CdS groups
Dress parcel shape.Fig. 3 is optoelectronic pole XPS figures obtained by the present embodiment, and Fig. 3 A are the XPS without HCl treatment surface, and Fig. 3 B are hydrochloric acid
Processing dissolves away the XPS after CdS.Understand that before processing electrode surface only has CdS layer by XPS results, exposed without Mo substrates.At hydrochloric acid
CdS is completely dissolved after reason post processing, surface MoS2, still exposed without Mo substrates.Electricity is can conclude that with reference to SEM and XPS
Has CdS/MoS2/ Mo bilayer core shell structures.
Application examples 1:Photoelectric activity is tested:
Using optoelectronic pole prepared by embodiment 1 as working electrode, platinum electrode is used as to electrode, saturation 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 xenons
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 are the CdS optoelectronic poles prepared on FTO glass relatively, and optoelectronic pole prepared by the present invention has
Higher photoelectric transformation efficiency.
Detection and the analysis integrated optoelectronic pole that the present embodiment obtains that demonstrates above is that have efficient opto-electronic 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 down then 180 degrees Celsius under react 10 hours and obtain CdS/
FTO optoelectronic poles.
Investigate the electricity conversion of the material of optoelectronic pole prepared by the embodiment of the present invention 1 and comparative example 1, the results showed that,
The CdS/MoS of the present invention2What the electricity conversion of/Mo bilayer core shell structure optoelectronic poles was prepared apparently higher than documents 1
CdS/FTO optoelectronic poles.
The preferred embodiment of the application is the foregoing is only, is not limited to the application, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
- A kind of 1. CdS/MoS2The preparation method of/Mo bilayer core shell structure optoelectronic poles, it is characterised in that step is as follows:Using molybdenum net as substrate, using soluble cadmium salt as cadmium source, cadmium metal is deposited on to molybdenum is online, the molybdenum net deposited is put Vulcanized in hydrogen sulfide atmosphere, that is, obtain CdS/MoS2/ Mo bilayer core shell structure optoelectronic poles.
- 2. preparation method according to claim 1, it is characterised in that by molybdenum net respectively with concentrated hydrochloric acid and concentrated alkali solution ultrasound Cleaning, then uses deionized water, ethanol again, and acetone is cleaned by ultrasonic.
- 3. preparation method according to claim 1, it is characterised in that the soluble cadmium salt is selected from cadmium nitrate, caddy Or cadmium acetate.
- 4. preparation method according to claim 1, it is characterised in that by way of controlling deposition voltage and sedimentation time It is online that cadmium metal is deposited on molybdenum.
- 5. preparation method according to claim 4, it is characterised in that the deposition voltage is -1.5 to -2.0V, during deposition Between be 600-1200s.
- 6. preparation method according to claim 1, it is characterised in that the temperature of vulcanization is 300 DEG C -600 DEG C.
- 7. the CdS/MoS that the method described in claim any one of 1-6 is prepared2/ Mo bilayer core shell structure optoelectronic poles.
- 8. the CdS/MoS described in claim 72/ Mo bilayer core shell structure optoelectronic poles are in the application in light hydrolytic hydrogen production.
- 9. a kind of smooth hydrolytic hydrogen production system, it is characterised in that the smooth hydrolytic hydrogen production system is with the CdS/ described in claim 7 MoS2/ Mo bilayer core shell structure optoelectronic poles are used as to electrode, saturation silver/silver chloride electrode conduct as working electrode, platinum electrode Reference electrode.
- 10. light hydrolytic hydrogen production system as claimed in claim 9, it is characterised in that also included in the smooth hydrolytic hydrogen production system: Electrolyte solution;The electrolyte solution is:0.25 mol/L vulcanized sodium, 0.35 mol/L sodium sulfite.
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Cited By (2)
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CN108906080A (en) * | 2018-07-11 | 2018-11-30 | 中国科学技术大学 | A kind of CdS/Cu2S/Co base photoelectrocatalysimaterial material and preparation method thereof |
CN112221518A (en) * | 2020-10-21 | 2021-01-15 | 广东工业大学 | CdS/MoSxComposite material and one-step electrochemical deposition preparation method and application thereof |
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