CN104498991A - NiO/CdSe/MoS2 laminar composite photocathode and preparation method thereof - Google Patents
NiO/CdSe/MoS2 laminar composite photocathode and preparation method thereof Download PDFInfo
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- CN104498991A CN104498991A CN201410840973.6A CN201410840973A CN104498991A CN 104498991 A CN104498991 A CN 104498991A CN 201410840973 A CN201410840973 A CN 201410840973A CN 104498991 A CN104498991 A CN 104498991A
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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
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Abstract
The invention discloses a NiO/CdSe/MoS2 laminar composite photocathode and a preparation method thereof. The preparation method comprises the following steps: (1) with ITO conductive glass as a base, preparing a uniform and consistent nickel oxide layer employing a hydrothermal process; (2) loading cadmium selenide on the surface of nickel oxide by adopting an ion alternate adsorption method; and (3) with a NiO/CdSe electrode as a cathode, and (NH4)2[MoS4] as a deposition liquid, depositing MoS2 particles on the surface of the NiO/CdSe electrode by adopting a light-assisted potentiostatic deposition method, so as to obtain a MoS2-modified electrode. According to the method for preparing the photocathode, the amounts of an absorption agent and a cocatalyst are controllable; and under visible light irradiation, the composite photocathode shows good photoelectrocatalytic activity and visible light response characteristics, is stable in performance, and can be effectively applied to the field of photoelectrocatalysis of water decomposition to produce hydrogen.
Description
Technical field
The present invention relates to semiconductor photoelectrocatalysielectrode and decompose aquatic products hydrogen technical field, particularly a kind of lamellar composite type electrode and preparation method thereof.
Background technology
As the energy carrier in a kind of future, hydrogen, due to its spatter property, receives extensive concern.One of efficient potential product hydrogen methods is photoelectric decomposition aquatic products hydrogen, and sun power can be caught and store to this method at the simplest chemical bond (H
2) in, and without any undesirable pollutent.Optoelectronic equipment is made up of two different electrodes: photo cathode and photocathode, and the oxidation and induction reaction of water occurs respectively.As the half-reaction of producing hydrogen, efficiently, at a low price, the structure of stable photocathode still faces huge challenge.
NiO is as the P-type semiconductor transmitting hole, there is wider band gap, good thermostability and chemical stability, and its valence band location is at 0.45V (vs NHE), for many photosensitizerss, be a kind of well electron donor, these characteristics have been doomed nickel oxide can become one of the most promising photoelectric cathode materials of one.CdSe, as the good light absorbing material of one, has low energy gap (about 1.7eV), can absorb large-scale visible ray.Therefore, the present invention with this bi-material construct a kind of novel with stable composite type photocathode for photoelectric decomposition aquatic products hydrogen, re-use MoS
2as promotor, improve the photoelectric properties of this electrode further.
Summary of the invention
The object of the present invention is to provide a kind of product hydrogen lamellar composite type photocathode NiO/CdSe/MoS
2and preparation method thereof, CdSe/NiO electrode has very high stability in long-time reaction process, and uses base metal MoS
2after promotor, the stability not only maintaining primary electrode substantially increases again the performance of this electrode.Under the impressed voltage of-0.131V (vsRHE), the hydrogen generation efficiency in buffered soln (pH=6) of the electrode after this modification can reach 0.519 μm of ol h
-1cm
-2, and faradic efficiency is close to 100%.The photoelectricity that the composite photocathode that the present invention obtains has efficient stable produces hydrogen effect, and preparation method is simple.
Object of the present invention can be achieved through the following technical solutions:
The present invention adopts hydrothermal method, and ion alternation absorption method and light assist electrodip process to prepare NiO/CdSe/MoS
2lamellar composite type electrode.
(1) surface preparation of ITO conductive glass
Pretreated ITO conductive glass first successively at dehydrated alcohol, soak two hours in acetone, and then in the aqueous isopropanol of 2mol/L potassium hydroxide reflux 15min;
(2) hydrothermal method prepares NiO film
Ito glass is put into 0.25mol/L Ni (NO
3)
26H
2in the mixed aqueous solution of O and 0.25mol/L hexamethylenetetramine, 100 DEG C of heating 12min, take out, by washed with de-ionized water, dry, and to be placed in retort furnace 300 DEG C of calcining 30min, ITO/NiO;
(3) ion alternation absorption method is adopted to prepare the NiO combined electrode of cadmium selenide (CdSe) sensitization
ITO/NiO electrode is immersed 0.03mol/LCd successively
2+and 0.03mol/LSe
2-ethanolic soln in, immerse 30s at every turn, then use ethanol purge, immerse circulation execution 6 times, can ITO/NiO/CdSe be obtained;
(4) light assists galvanic deposit base metal MoS
2as promotor
Light is utilized to assist the method for galvanic deposit on ITO/NiO/CdSe, deposit one deck MoS
2, first configure deposit fluid, i.e. 0.10mmol/L (NH
4)
2[MoS
4] and 0.10mol/L KCl; Take ITO/NiO/CdSe as working electrode, deposition voltage is 0.6V (vs Ag/AgCl), and depositing time controls as 15min.
Remarkable advantage of the present invention is:
(1) after this composite photocathode adopts simple hydrothermal method to prepare NiO, then use ion alternation absorption method by CdSe load at NiO on the surface, finally use up again and assist electrodip process load MoS
2as promotor.Preparation method is simple.
(2) ion alternation absorption method can make optical absorbing agent CdSe directly contact with p-type semiconductor NiO, shortens the distance of transfer transport, is conducive to electric transmission; And light assists flexible MoS
2, compared with traditional method, can complete under low-temperature atmosphere-pressure, and can by regulation and control impressed voltage and light application time control MoS
2deposition.
(3) NiO is a kind of well P-type semiconductor, and has good thermostability and chemical stability.
(4) CdSe is a kind of well light absorbing material, has narrower energy gap, can effectively absorb large-scale visible ray.
(5) cheap base metal MoS is adopted
2replace traditional precious metals pt as promotor load at CdSe/NiO/ITO electrode surface, not only save cost, or a kind of catalyzer of efficient stable, can effectively improve photoelectrocatalysis H2-producing capacity.
(6) photocathode prepared by the present invention is used for the hydrogen manufacturing of photoelectrolysis water, and reaction is efficient, simple to operate, cheap practical, and the lamellar composite type photocathode of preparation has very high stability, has very high practical value and application prospect.
Accompanying drawing explanation
Fig. 1 be the made electrode of embodiment 1 ultraviolet-visible absorption spectroscopy comparison diagram (a) and at-0.222V vs Ag/AgCl, in the buffered soln that nitrogen is saturated, electric current changes correlation curve figure (b) in time.
Fig. 2 be the made electrode of embodiment 1 under the impressed voltage of-0.5V, the radiation of visible light current-time curvel (a) of 9 hours is in the saturated buffered soln of nitrogen (pH=6); B () be (0.1mol/L) in the Klorvess Liquid of air saturation.
Fig. 3 is ultraviolet-visible absorption spectroscopy comparison diagram (a) and the XPS spectrum figure of the made electrode of embodiment 2, (b) overall collection of illustrative plates, (c) Ni 2p, (d) O 1s, (e) Cd 3d, (f) Se 3d, (g) Mo 3d and (h) S 2p.
Fig. 4 is the made three kinds of Different electrodes electric currents of embodiment 2 change curve comparison diagrams in time; (a) NiO; (b) NiO/CdSe; (c) NiO/CdSe/MoS
2.
Fig. 5 is the made three kinds of Different electrodes short-circuit current comparison diagrams of embodiment 2; (a) NiO; (b) NiO/CdSe; (c) NiO/CdSe/MoS
2.
Fig. 6 is embodiment 3 laminate composite type photocathode NiO/CdSe and NiO/CdSe/MoS
2the contrast of photoelectricity H2-producing capacity at different conditions.
Fig. 7 is that embodiment 3 laminate combined electrode is for producing the mechanism schematic diagram of hydrogen experiment.
Embodiment
Embodiment 1
1. the preparation method of novel photoelectric negative electrode CdSe/NiO electrode, specifically prepares as follows:
(1) surface preparation of ITO conductive glass:
Pretreated ITO conductive glass first successively at dehydrated alcohol, soak two hours in acetone, and then in the aqueous isopropanol of 2mol/L potassium hydroxide reflux 15min.
(2) hydrothermal method prepares NiO film
Ito glass is put into 0.25mol/L Ni (NO
3)
26H
2in the mixed aqueous solution of O and 0.25mol/L hexamethylenetetramine, 100 DEG C of heating 12min, take out, by washed with de-ionized water five times, dry, and are placed on 300 DEG C of calcining 30min in retort furnace, NiO/ITO electrode.
(3) ion alternation absorption method is adopted to prepare the NiO combined electrode of cadmium selenide (CdSe) sensitization
ITO/NiO electrode is immersed 0.03mol/LCd successively
2+with 0.03mol/L Se
2-ethanolic soln in, immerse 30sec at every turn, then use ethanol purge, immerse circulation execution 6 times.CdSe/NiO/ITO combined electrode can be obtained.
2. performance test
With 0.30mol/L hexamethylenetetramine, the mixed aqueous solution (pH=6) of 0.10mol/L hydrochloric acid and 0.20mol/L Repone K is electrolyte solution, the xenon lamp of 300W is analog light source, Ag/AgCl electrode is used as reference electrode, platinum guaze is as to electrode, CdSe/NiO electrode, as working electrode, CHI600D electrochemical instrument does photoelectric properties test.Result is as shown in Fig. 1 (b) He Fig. 2.
In Fig. 1 (b), black line represents independent NiO electrode current change curve in time; Red line represents the combined electrode CdSe/NiO electric current change curve in time after CdS-loaded e.Show when other are identical, adding of CdSe considerably increases the absorption of electrode in visible-range, thus substantially increases photoelectric current.
Fig. 2 be CdSe/NiO electrode under the impressed voltage of-0.5V, the radiation of visible light current-time curvel (a) of 9 hours is in the saturated buffered soln of nitrogen (pH=6); B () be (0.1mol/L) in the Klorvess Liquid of air saturation.As can be seen from the figure the electrode prepared by the present invention is used to react in general salts solution and buffered soln and can keep very high stability.
Embodiment 2
1. adopt MoS
2as promotor load at CdSe/NiO electrode surface, prepare more efficient photocathode MoS
2/ CdSe/NiO, specifically prepares as follows:
(1) surface preparation of ITO conductive glass:
Pretreated ITO conductive glass first successively at dehydrated alcohol, soak two hours in acetone, and then in the aqueous isopropanol of 2mol/L potassium hydroxide reflux 15min.
(2) hydrothermal method prepares NiO film
Ito glass is put into 0.25mol/L Ni (NO
3)
26H
2in the mixed aqueous solution of O and 0.25mol/L hexamethylenetetramine, 100 DEG C of heating 12min, take out, by washed with de-ionized water five times, dry, and are placed on 300 DEG C of calcining 30min in retort furnace, NiO/ITO electrode.
(3) ion alternation absorption method is adopted to prepare the NiO combined electrode of cadmium selenide (CdSe) sensitization
ITO/NiO electrode is immersed 0.03mol/LCd successively
2+and 0.03mol/LSe
2-ethanolic soln in, immerse 30sec at every turn, then use ethanol purge, immerse circulation execution 6 times.CdSe/NiO/ITO combined electrode can be obtained.
(4) light assists galvanic deposit base metal MoS
2as promotor
Light is utilized to assist the method for galvanic deposit to deposit one deck MoS on CdSe/NiO/ITO combined electrode
2, first configure deposit fluid, i.e. 0.10mmol/L (NH
4)
2[MoS
4] KCl (0.10mol/L) solution.Take CdSe/NiO/ITO as working electrode, Ag/AgCl (0.3M) is reference electrode, and platinum guaze is to electrode, and deposition voltage is 0.6V (vsAg/AgCl), and depositing time controls as 15min.
Fig. 3 is ultraviolet-visible absorption spectroscopy comparison diagram (a) and x-ray photoelectron power spectrum (XPS) figure (b) ~ (h) of made electrode.MoS can be found out from figure (a)
2after load, the absorbing ability of CdSe/NiO electrode has had a little reduction, thus proves MoS
2by successful load at CdSe/NiO electrode surface, and also can prove MoS from XPS spectrum figure
2, each component of CdSe, NiO existence.
2. performance test
With 0.30mol/L hexamethylenetetramine, the mixed aqueous solution (PH=6) of 0.10mol/L hydrochloric acid and 0.20mol/L Repone K is electrolyte solution, and the xenon lamp of 300W is analog light source, and Ag/AgCl electrode is used as reference electrode, platinum guaze as to electrode, MoS
2/ CdSe/NiO electrode, as working electrode, CHI600D electrochemical instrument does photoelectric properties test.Result as shown in Figure 4 and Figure 5.
Fig. 4 is load MoS
2front and back electric current curve comparison figure over time; Fig. 5 is load MoS
2front and back short-circuit current comparison diagram.Show when other are identical, MoS
2add the transport velocity greatly increasing electronics between interface, inhibit the compound in electronics and hole, thus substantially increase the photoelectric current of combined electrode.
Embodiment 3
Lamellar composite type photocathode NiO/CdSe and NiO/CdSe/MoS
2the contrast of photoelectricity H2-producing capacity at different conditions and the photoelectrocatalysis H_2-producing mechanism proposed.
With 0.30mol/L hexamethylenetetramine, the mixed aqueous solution (pH=6) of 0.10mol/L hydrochloric acid and 0.20mol/L Repone K is electrolyte solution, and the xenon lamp of 300W is analog light source, and Ag/AgCl electrode is used as reference electrode, platinum guaze as to electrode, prepared CdSe/NiO and MoS
2/ CdSe/NiO electrode, as working electrode, CHI600D electrochemical instrument does photoelectricity and produces hydrogen experiment.Photoelectrocatalysis produces the amount of hydrogen by the gas chromatographic detection containing thermal conductivity detector.Composite type photocathode CdSe/NiO and MoS of the present invention
2the contrast of/CdSe/NiO photoelectricity H2-producing capacity at different conditions as shown in Figure 6.
As can be seen from Fig. 6 (a), light is being only had to deposit in case, CdSe/NiO and MoS
2the equal no hydrogen of/CdSe/NiO two electrodes produces; When only having electric, CdSe/NiO electrode no hydrogen produces, MoS
2/ CdSe/NiO electric shock there is a small amount of hydrogen to produce; And under light and the simultaneous situation of electricity, two electrodes have hydrogen to produce, and load MoS
2electrode hydrogen generation efficiency the highest.Show to use MoS from Fig. 6 (b)
2after promotor, the stability not only maintaining primary electrode substantially increases again the performance of this electrode.Under the impressed voltage of-0.131V (vsRHE), the hydrogen generation efficiency in buffered soln (PH=6) of the electrode after this modification can reach 0.519 μm of ol h
-1cm
-2, and faradic efficiency is close to 100%.Its efficiency is 0.519 μm of ol h-1cm
-2at-0.131V vsRHE, than 0.108 μm of ol h-1cm of unmodified
-2high, and its faradic efficiency is close to 100%.
Inquire into the Photocatalyzed Hydrogen Production mechanism of made electrode as shown in Figure 7: radiation of visible light is at electrode surface, optical absorbing agent CdSe absorb photons, reductibility electronics and oxidisability hole is produced respectively at conduction band and valence band location, electrode base is transferred to by nickel oxide in hole, is then consumed by the electron institute of external circuit; Meanwhile, the electronics of reductibility is by MoS
2transfer to rapidly its surface, cause H
+rapid reduction produces H
2, inhibit again the compound in electronics and hole.
Claims (1)
1. a NiO/CdSe/MoS
2lamellar composite type photocathode and preparation method thereof, is characterized in that this lamellar composite type photocathode is sequentially from top to bottom successively: ITO Conducting Glass, NiO layer, CdSe layer, MoS
2layer, under photocathode can be used for visible ray, photoelectrocatalysis produces hydrogen, and preparation method is as follows:
(1) ito glass is put into 0.25mol/L Ni (NO
3)
26H
2in the mixed aqueous solution of O and 0.25mol/L hexamethylenetetramine, 100 DEG C heating 12min, take out, by washed with de-ionized water, dry, 300 DEG C calcining 30min, ITO/NiO;
(2) ITO/NiO is immersed 0.03mol/L Cd successively
2+with 0.03mol/L Se
2-ethanolic soln in, immerse 30s at every turn, then use ethanol purge, immerse circulation 6 times, can ITO/NiO/CdSe be obtained;
(3) light is utilized to assist the method for galvanic deposit on ITO/NiO/CdSe, deposit one deck MoS
2, first configure deposit fluid, i.e. 0.10mmol/L (NH
4)
2[MoS
4] and 0.10mol/L KCl; Take ITO/NiO/CdSe as working electrode, deposition voltage is 0.6V (vs Ag/AgCl), and depositing time controls as 15min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104862758A (en) * | 2015-04-29 | 2015-08-26 | 江南大学 | Method for preparing NiS/Ni(OH)2 electrocatalyst used for decomposing water to generate hydrogen |
| CN105225841A (en) * | 2015-10-09 | 2016-01-06 | 河南大学 | A kind of preparation method of DSSC NiO photocathode |
| CN105336498A (en) * | 2015-10-21 | 2016-02-17 | 江南大学 | Novel and stable g-C3N4/NiO photoelectric cathode preparation method |
| CN108716006A (en) * | 2018-05-21 | 2018-10-30 | 江南大学 | A kind of preparation method of the cobaltosic oxide photocathode of cadmium selenide sensitization |
| CN106449142B (en) * | 2016-10-11 | 2019-02-01 | 东华大学 | A kind of molybdenum sulfide/nickel oxide composite material and its preparation method and application |
| CN109908921A (en) * | 2019-03-11 | 2019-06-21 | 三峡大学 | A kind of MoS2/ NiO hollow microspheres, preparation method and application |
| CN112458493A (en) * | 2020-12-02 | 2021-03-09 | 江南大学 | NixP/CuO/NiO photoelectric cathode modified by tannic acid-cobalt complex and preparation method thereof |
| CN114188428A (en) * | 2021-12-13 | 2022-03-15 | 湘潭大学 | Photoelectric device made of germanium selenide composite material and preparation method thereof |
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| CN102437206B (en) * | 2011-12-15 | 2014-05-07 | 湖北大学 | ZnO/CdSe/CdTe nanorod array photoelectrode and preparation method thereof |
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| ALBU-YARON ET AL: "influence of the electrochemical deposition parameters on the microstructure of MoS2 thin films", <THIN SOLID FILMS> * |
| GUANG-LI WANG ET AL.: "A new approach to light up the application of semiconductor nanomaterials for photoelectrochemical biosensors: Using self-operating photocathode as a highly selective enzyme sensor", <BIOSENSORS AND BIOELECTRONICS> * |
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| CN104862758A (en) * | 2015-04-29 | 2015-08-26 | 江南大学 | Method for preparing NiS/Ni(OH)2 electrocatalyst used for decomposing water to generate hydrogen |
| CN105225841A (en) * | 2015-10-09 | 2016-01-06 | 河南大学 | A kind of preparation method of DSSC NiO photocathode |
| CN105225841B (en) * | 2015-10-09 | 2017-07-28 | 河南大学 | A kind of preparation method of DSSC NiO photocathodes |
| CN105336498A (en) * | 2015-10-21 | 2016-02-17 | 江南大学 | Novel and stable g-C3N4/NiO photoelectric cathode preparation method |
| CN105336498B (en) * | 2015-10-21 | 2018-01-23 | 江南大学 | A kind of g C3N4The preparation method of/NiO photocathodes |
| CN106449142B (en) * | 2016-10-11 | 2019-02-01 | 东华大学 | A kind of molybdenum sulfide/nickel oxide composite material and its preparation method and application |
| CN108716006A (en) * | 2018-05-21 | 2018-10-30 | 江南大学 | A kind of preparation method of the cobaltosic oxide photocathode of cadmium selenide sensitization |
| CN109908921A (en) * | 2019-03-11 | 2019-06-21 | 三峡大学 | A kind of MoS2/ NiO hollow microspheres, preparation method and application |
| CN109908921B (en) * | 2019-03-11 | 2022-02-01 | 三峡大学 | MoS2NiO blankCore microsphere material, preparation method and application |
| CN112458493A (en) * | 2020-12-02 | 2021-03-09 | 江南大学 | NixP/CuO/NiO photoelectric cathode modified by tannic acid-cobalt complex and preparation method thereof |
| CN112458493B (en) * | 2020-12-02 | 2021-10-29 | 江南大学 | NixP/CuO/NiO photoelectric cathode modified by tannic acid-cobalt complex and preparation method thereof |
| CN114188428A (en) * | 2021-12-13 | 2022-03-15 | 湘潭大学 | Photoelectric device made of germanium selenide composite material and preparation method thereof |
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