CN109821559A - A kind of preparation method and applications of core-shell structure composite photoelectric material - Google Patents
A kind of preparation method and applications of core-shell structure composite photoelectric material Download PDFInfo
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- CN109821559A CN109821559A CN201910239486.7A CN201910239486A CN109821559A CN 109821559 A CN109821559 A CN 109821559A CN 201910239486 A CN201910239486 A CN 201910239486A CN 109821559 A CN109821559 A CN 109821559A
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- 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 discloses a kind of core-shell structure TiO2The preparation method of@CdSe composite photoelectric material and its application in visible light photoelectrocatalysis, the composite photoelectric material are the one-dimensional TiO prepared with hydro-thermal method2Nanometer stick array introduces CdSe as shell by electrochemical deposition method and is made as stratum nucleare.The preparation method of composite photoelectric material of the present invention is simple, easily operated, and it can be used as photo cathode, and under conditions of using 0.2 mol/L sodium sulfide solution as electrolyte, excellent photoelectric properties are showed under visible light action, is suitble to promote and apply.
Description
Technical field
The invention belongs to photoelectrocatalysimaterial material preparation fields, and in particular to a kind of core-shell structure TiO2@CdSe composite photoelectric
The preparation method and applications of material.
Background technique
Energy and environmental problem is the two large problems that the mankind are faced.Using semiconductor material as the photocatalysis skill of catalyst
Art restores greenhouse gases dioxy because that solar energy can be converted to chemical energy, photocatalytic hydrogen production by water decomposition and oxygen processed at room temperature
Change carbon and decomposing organic pollutant, it is considered to be most ideal and most promising technology.It found partly to lead for the first time from 1972
Body TiO2Since mono crystalline photovoltaic pole can split water into hydrogen and oxygen under the action of ultraviolet light, photocatalysis has become one
New branch of science, the favor by domestic and international every field researcher.However, so far due to the limitation of catalysis material, light
Catalysis technique not yet realizes large-scale commercial.So develop efficient, stable and cheap photocatalytic system, be it is current and
One of the forefront of the following photocatalysis research and most crucial problem.
Compared with powder photocatalytic, photoelectrocatalysis water decomposition have it is higher too can positive transformation efficiency, had always been considered as
Brighter industrial application prospect.Theoretically, one-dimensional (1D) structure has compared with the nano material of other dimensions
More continuous charge transmission channel and less granule boundary are more advantageous to the separation and transmission of space charge, so it is generated
Electron-transport speed it is faster than common nano material, and TiO2Have many advantages, such as that cheap, catalytic activity and stability are high,
Therefore one-dimensional TiO2Nanometer stick array is considered as one of most promising photo cathode material.From Liu(J. in 2009
Am. Chem. Soc., 131 (11), 39853990.) et al. one-dimensional single crystal TiO has been synthesized on transparent conductor FTO for the first time2
Since nanometer rods, with one-dimensional TiO2Nanotube, two dimension TiO2The TiO of nanometer sheet and three-dimensional2Nano particle is compared, one-dimensional single crystal
TiO2Nanometer rods have been shown one's talent as light anode most potential in dye-sensitized solar cells and photoelectrocatalysis field
Material.But rutile TiO2The forbidden bandwidth of nanometer stick array is larger, can only utilize in solar spectrum 4% or so ultraviolet light
Region, and low (1 cm of its electron mobility2/ V/s), the diffusion path in hole it is short (10-100 nm), limit photoproduction electricity
The separation of son-hole and transfer, result in its solar energy utilization ratio and incident photon-to-electron conversion efficiency is low.
CdSe is a kind of very important II-VI race semiconductor, its band gap is 1.75 eV, have in solar spectrum
The adaptable bandwidth of visible light wave range, and conduction band positions ratio TiO2Height convenient for the migration of photo-generated carrier be a kind of outstanding
Sensitizer.CdSe can effectively enhance TiO2The efficiency of light absorption of nano-tube array promotes the separation of photo-generated carrier and turns
It moves, and then the performance that its photoelectrocatalysis decomposes water is significantly increased.Meanwhile the CdSe of quantum dot form has bigger ratio table
Area and more active sites, and quantum size effect and the other physical effects derived, can make the band of semiconductor
Gap is broadening, to enhance its redox potential, promotes the driving force of catalysis reaction, and catalysis reaction can be promoted to go on smoothly.Cause
This, the present invention makes full use of one-dimensional TiO2The advantage of nanometer stick array introduces CdSe nanometers of materials by the method for electrochemical deposition
Material, constructs efficient TiO2@CdSe composite photoelectric anode material.
Summary of the invention
The purpose of the present invention is to provide a kind of core-shell structure TiO2It the preparation method of@CdSe composite photoelectric material and its answers
With the TiO of gained one-dimensional nucleocapsid structure2@CdSe photoelectric material has visible light absorption capacity, and illustrates excellent photo electric
Energy.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of core-shell structure TiO2@CdSe composite photoelectric material is to prepare one-dimensional TiO using hydro-thermal method2Nanometer stick array, so
Afterwards with one-dimensional TiO2Nanometer stick array is stratum nucleare, introduces CdSe as shell structurre using electrochemical deposition method, the tool constructed
There is the TiO of one-dimensional nucleocapsid structure2@CdSe composite photoelectric material.
The core-shell structure TiO2The preparation method of@CdSe composite photoelectric material includes the following steps:
1) one-dimensional TiO2The preparation of nanometer stick array
FTO electro-conductive glass is sequentially placed in deionized water in acetone, absolute ethanol and deionized water, is cleaned by ultrasonic 20 min respectively, to clear
It is dried for standby after washing；Then the HCl solution that 15 mL volumetric concentrations are 37% is added in 50 mL ptfe autoclaves
With 15 mL deionized waters, persistently stirring 5 min at room temperature makes it after mixing, adds the titanium source of 1.5-5.8 mmol, holds
5 min of continuous stirring；Clean FTO electro-conductive glass is tiltedly placed in a kettle, keeps the conduction of FTO face-up, then reaction
Kettle moves into hydro-thermal reaction 4-6 h in 150-180 DEG C of baking oven, after reaction takes out FTO electro-conductive glass, is rushed with deionized water
It washes, dries at room temperature, then be placed on 400-500 DEG C of calcining 1-2 h in Muffle furnace, obtain the rutile TiO of one-dimentional structure2It receives
Rice stick array；
2) core-shell structure TiO2The preparation of@CdSe composite photoelectric anode
The DMF solution that 60 mL contain 10 mM cadmium sources and 5 mM selenium is prepared in the two mouth flask of 100 mL, then moves it into 125
DEG C thermostatical oil bath in, through TiO made from step 1)2For nanometer stick array as working electrode, Pt, which is used as, immerses two to electrode
In mouth flask, two electrode systems are constituted, -0.3 A/cm is added to two constructed electrode systems-2Constant current, continue 300-700s
Electrochemical deposition is carried out, to prepare core-shell structure TiO2@CdSe composite nanorod array.
Titanium source described in step 1) includes butyl titanate, isopropyl titanate, any one or a few in titanium tetrachloride.
Cadmium source described in step 2 is at least one of caddy, cadmium nitrate, cadmium acetate.
Obtained core-shell structure TiO2@CdSe composite photoelectric material, which can be used as photo cathode, to be applied and urges in visible light photoelectricity
Change in water oxygen, electrolyte used is the sodium sulfide solution of 0.2 mol/L.
Remarkable advantage of the invention is:
(1) present invention for existing photoelectrocatalysis decomposition water technology there are aiming at the problem that, especially TiO2There are light for optical anode material
The problems such as absorption region is narrow and photoelectric efficiency is low, provides a kind of TiO with core-shell structure2@CdSe composite photoelectric material.It should
Composite photoelectric material have uniform core-shell structure, using 0.2 mol/L sodium sulfide solution as electrolyte, can visible light (λ >=
420 nm) induction under show excellent photoelectric properties.
(2) preparation method of composite material of the present invention is simple, easily operated, is suitable for wide popularization and application.
Detailed description of the invention
Fig. 1 is TiO prepared by embodiment 12TiO prepared by nanometer stick array (A) and embodiment 22@CdSe composite nanorod
The SEM comparison diagram of array (B).
Fig. 2 is TiO prepared by embodiment 12TiO prepared by nanometer stick array (A, B) and embodiment 22@CdSe composite Nano
The TEM comparison diagram of stick array (C, D).
Fig. 3 is TiO prepared by embodiment 12The TiO prepared under different sedimentation times with embodiment 4,5,2,6,72@CdSe sample
The transient photocurrents response curve of product.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further, but the present invention is not limited only to this.
The one-dimensional TiO of embodiment 12The preparation of nanometer stick array
FTO electro-conductive glass is sequentially placed in deionized water in acetone, absolute ethanol and deionized water, is cleaned by ultrasonic 20 min respectively, to clear
It is dried for standby after washing；Then the HCl solution that 15 mL volumetric concentrations are 37% is added in 50 mL ptfe autoclaves
With 15 mL deionized waters, persistently stirring 5 min at room temperature makes it after mixing, adds the butyl titanate of 1.5 mmol,
Persistently stir 5 min；Clean FTO electro-conductive glass is tiltedly placed in a kettle, keeps the conduction of FTO face-up, then anti-
It answers kettle to move into 5 h of hydro-thermal reaction in 170 DEG C of baking ovens, FTO electro-conductive glass is taken out after reaction, is rinsed with deionized water, room
It is dried under temperature, then is placed on 400 DEG C of 2 h of calcining in Muffle furnace, obtain the rutile TiO of one-dimentional structure2Nanometer stick array is compiled
Number be 1.
Embodiment 2
1) one-dimensional TiO2The preparation of nanometer stick array
FTO electro-conductive glass is sequentially placed in deionized water in acetone, absolute ethanol and deionized water, is cleaned by ultrasonic 20 min respectively, to clear
It is dried for standby after washing；Then the HCl solution that 15 mL volumetric concentrations are 37% is added in 50 mL ptfe autoclaves
With 15 mL deionized waters, persistently stirring 5 min at room temperature makes it after mixing, adds the butyl titanate of 1.5 mmol,
Persistently stir 5 min；Clean FTO electro-conductive glass is tiltedly placed in a kettle, keeps the conduction of FTO face-up, then anti-
It answers kettle to move into 5 h of hydro-thermal reaction in 170 DEG C of baking ovens, FTO electro-conductive glass is taken out after reaction, is rinsed with deionized water, room
It is dried under temperature, then is placed on 400 DEG C of 2 h of calcining in Muffle furnace, obtain the rutile TiO of one-dimentional structure2Nanometer stick array；
2) core-shell structure TiO2The preparation of@CdSe complex light anode
60 mL are prepared in the two mouth flask of 100 mL containing 10 mM(0.1370g) caddy and 5 mM (0.0237g) selenium
Then DMF solution moves it into 125 DEG C of thermostatical oil bath, by TiO obtained2Nanometer stick array is as working electrode, Pt
It is immersed in two mouth flask as to electrode, two electrode systems is constituted, by Shanghai Chen Hua CHI660E electrochemical workstation to institute's structure
Two electrode systems built add -0.3 A/cm-2Constant current, continue 500s carry out electrochemical deposition, to prepare core-shell structure
TiO2@CdSe composite photoelectric anode, number 2.
Embodiment 3
1) one-dimensional TiO2The preparation of nanometer stick array
FTO electro-conductive glass is sequentially placed in deionized water in acetone, absolute ethanol and deionized water, is cleaned by ultrasonic 20 min respectively, to clear
It is dried for standby after washing；Then the HCl solution that 15 mL volumetric concentrations are 37% is added in 50 mL ptfe autoclaves
With 15 mL deionized waters, persistently stirring 5 min at room temperature makes it after mixing, adds the butyl titanate of 1.5 mmol,
Persistently stir 5 min；Clean FTO electro-conductive glass is tiltedly placed in a kettle, keeps the conduction of FTO face-up, then anti-
It answers kettle to move into 3 h of hydro-thermal reaction in 180 DEG C of baking ovens, FTO electro-conductive glass is taken out after reaction, is rinsed with deionized water, room
It is dried under temperature, then is placed on 500 DEG C of 1 h of calcining in Muffle furnace, obtain the rutile TiO of one-dimentional structure2Nanometer stick array；
2) core-shell structure TiO2The preparation of@CdSe complex light anode
60 mL are prepared in the two mouth flask of 100 mL containing 10 mM(0.1370g) caddy and 5 mM (0.0237g) selenium
Then DMF solution moves it into 125 DEG C of thermostatical oil bath, by TiO obtained2Nanometer stick array is as working electrode, Pt
It is immersed in two mouth flask as to electrode, two electrode systems is constituted, by Shanghai Chen Hua CHI660E electrochemical workstation to institute's structure
Two electrode systems built add -0.3 A/cm-2Constant current, continue 300s carry out electrochemical deposition, to prepare core-shell structure
TiO2@CdSe composite photoelectric anode, number 3.
Embodiment 4
Time used in electrodeposit reaction in embodiment 2 is changed to 300 s by 500 s, remaining step obtains TiO with embodiment 22@
CdSe composite photoelectric anode, number 4.
Embodiment 5
Time used in electrodeposit reaction in embodiment 2 is changed to 400 s by 500 s, remaining step obtains TiO with embodiment 22@
CdSe composite photoelectric anode, number 5.
Embodiment 6
Time used in electrodeposit reaction in embodiment 2 is changed to 600 s by 500 s, remaining step obtains TiO with embodiment 22@
CdSe composite photoelectric anode, number 6.
Embodiment 7
Time used in electrodeposit reaction in embodiment 2 is changed to 700 s by 500 s, remaining step obtains TiO with embodiment 22@
CdSe composite photoelectric anode, number 7.
Embodiment 8
Caddy used in embodiment 2 is changed to the cadmium nitrate of equimolar amounts, remaining step obtains TiO with embodiment 22@CdSe is multiple
Close photo cathode, number 8.
Embodiment 9
Caddy used in embodiment 2 is changed to the cadmium acetate of equimolar amounts, remaining step obtains TiO with embodiment 22@CdSe is multiple
Close photo cathode, number 9.
Embodiment 10
Butyl titanate used in embodiment 2 is changed to isometric isopropyl titanate, remaining step obtains TiO with embodiment 22@CdSe
Composite photoelectric anode, number 10.
Embodiment 11
Butyl titanate used in embodiment 2 is changed to isometric titanium tetrachloride, remaining step obtains TiO with embodiment 22@CdSe
Composite photoelectric anode, number 11.
Embodiment 12
Time used in electrodeposit reaction in embodiment 3 is changed to 500 s by 300 s, remaining step obtains TiO with embodiment 32@
CdSe composite photoelectric anode, number 12.
Fig. 1 is TiO prepared by embodiment 12TiO prepared by nanometer stick array (A) and embodiment 22@CdSe composite nanorod
The SEM comparison diagram of array (B).As seen from Figure 1, pure TiO2Surface it is very smooth, and TiO after electro-deposition 500s2Sample surfaces are rich
A large amount of nano particle is collected, and rough pattern is presented.
Fig. 2 is TiO prepared by embodiment 12TiO prepared by nanometer stick array (A, B) and embodiment 22@CdSe composite Nano
The TEM comparison diagram of stick array (C, D).TiO is clearly demonstrated in figure2The lattice fringe of shell CdSe is 0.37 nm, is belonged to
CdSe(100) crystal face illustrates TiO2@CdSe complex light anode material is successfully synthesized.
Fig. 3 is TiO2With the TiO of different sedimentation times preparation2The transient photocurrents response curve of@CdSe sample, wherein
TiO2(a), TC-300(b), TC-400(c), TC-500(d), TC-600(e) and TC-700(f) respectively correspond embodiment 1,4,
5,2,6 and 7.As seen from Figure 3, corresponding density of photocurrent is 0.09,0.11,0.97,2.14,1.62 and 0.99 mA/
cm2, illustrate the TiO that electrodeposition time is 500s2The density of photocurrent value of@CdSe sample is maximum, and photoelectric properties are best.
Visible light photoelectrocatalysis water oxygen performance evaluation
Electrochemical Characterization test is tested with occasion China electrochemical workstation (CHI660E).Survey photoelectric current and linear surface sweeping relationship
What the photoelectric test system of curve was made of three-electrode system, wherein Pt piece is as being as ginseng to electrode and Ag/AgCl
Than electrode, 0.2 mol/L vulcanized sodium is as electrolyte.It the results are shown in Table 1.
1 difference TiO of table2The current density of@CdSe composite photoelectric anode
Seen from table 1, when using butyl titanate as titanium source, caddy as cadmium source, electrodeposition time is 500s's
TiO2The density of photocurrent value of@CdSe sample is maximum, reaches 2.14 mA/cm2.And when titanium source and cadmium source is raw materials used changes
When, the TiO that is prepared using isopropyl titanate as titanium source, caddy as cadmium source2The density of photocurrent value of@CdSe sample is maximum, reaches
To 2.17 mA/cm2, photoelectric properties are best.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (8)
1. a kind of core-shell structure TiO2The preparation method of@CdSe composite photoelectric material, it is characterised in that: using hydro-thermal method preparation one
Tie up TiO2Nanometer stick array, then with one-dimensional TiO2Nanometer stick array is stratum nucleare, introduces CdSe as shell using electrochemical deposition method
Layer structure, constructs the TiO with one-dimensional nucleocapsid structure2@CdSe composite photoelectric material.
2. core-shell structure TiO according to claim 12The preparation method of@CdSe composite photoelectric material, it is characterised in that:
Include the following steps:
1) one-dimensional TiO2The preparation of nanometer stick array
FTO electro-conductive glass is sequentially placed in deionized water in acetone, absolute ethanol and deionized water, is cleaned by ultrasonic 20 min respectively, to clear
It is dried for standby after washing；Then the HCl solution and 15 that 15 mL volumetric concentrations are 37% is added in ptfe autoclave
ML deionized water, persistently stirring 5 min at room temperature makes it after mixing, adds the titanium source of 1.5-5.8 mmol, persistently stirs
Mix 5 min；Clean FTO electro-conductive glass is tiltedly placed in a kettle, the conduction for making FTO up, then moves reaction kettle
Enter and carry out hydro-thermal reaction in baking oven, FTO electro-conductive glass is taken out after reaction, is rinsed with deionized water, is dried at room temperature, then
It is placed on 400-500 DEG C of calcining 1-2 h in Muffle furnace, obtains the rutile TiO of one-dimentional structure2Nanometer stick array；
2) core-shell structure TiO2The preparation of@CdSe composite photoelectric anode
DMF solution of 60 mL containing 10 mM cadmium sources and 5 mM selenium is moved into 125 DEG C of thermostatical oil bath, then, with step 1)
TiO obtained2Nanometer stick array is as working electrode, and Pt, which is used as, constitutes two electrode systems to electrode, to two constructed electrodes
System adds -0.3 A/cm-2Constant current carry out electrochemical deposition, to prepare core-shell structure TiO2@CdSe composite nanorod
Array.
3. core-shell structure TiO according to claim 22The preparation method of@CdSe composite photoelectric material, it is characterised in that: step
It is rapid 1) described in titanium source include butyl titanate, isopropyl titanate, any one or a few in titanium tetrachloride.
4. core-shell structure TiO according to claim 22The preparation method of@CdSe composite photoelectric material, it is characterised in that: step
It is rapid 1) described in hydro-thermal reaction temperature be 150-180 DEG C, the reaction time be 4-6 hours.
5. core-shell structure TiO according to claim 22The preparation method of@CdSe composite photoelectric material, it is characterised in that: step
It is rapid 2) described in cadmium source be at least one of caddy, cadmium nitrate, cadmium acetate.
6. core-shell structure TiO according to claim 22The preparation method of@CdSe composite photoelectric material, it is characterised in that: step
It is rapid 2) described in electrochemical deposition duration be 300-700s.
7. core-shell structure TiO made from a kind of method as claimed in claim 1 or 22@CdSe composite photoelectric material is in visible light light
Application in electro-catalysis.
8. core-shell structure TiO according to claim 72The application of@CdSe composite photoelectric material, it is characterised in that: use institute
State core-shell structure TiO2@CdSe composite photoelectric material is as photo cathode, using 0.2 mol/ sodium sulfide solution as electrolyte.
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| CN112086289A (en) * | 2020-08-12 | 2020-12-15 | 华东师范大学 | Sunlight-driven electricity-oxygen co-production seawater battery and preparation method thereof |
| CN113846342A (en) * | 2021-10-13 | 2021-12-28 | 浙江工业大学 | Inorganic-organic core-shell framework loaded low-dose noble metal palladium material, preparation thereof and application thereof in electrocatalytic dechlorination and hydrogenation reaction |
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| CN112086289A (en) * | 2020-08-12 | 2020-12-15 | 华东师范大学 | Sunlight-driven electricity-oxygen co-production seawater battery and preparation method thereof |
| CN113846342A (en) * | 2021-10-13 | 2021-12-28 | 浙江工业大学 | Inorganic-organic core-shell framework loaded low-dose noble metal palladium material, preparation thereof and application thereof in electrocatalytic dechlorination and hydrogenation reaction |
| CN113846342B (en) * | 2021-10-13 | 2023-09-05 | 浙江工业大学 | Inorganic-organic core-shell skeleton loaded low-dose noble metal palladium material, preparation thereof and application thereof in electrocatalytic dechlorination hydrogenation reaction |
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