CN106222685B - A kind of WO of photoelectrocatalysis water decomposition3The preparation method of-LDH laminated films - Google Patents

A kind of WO of photoelectrocatalysis water decomposition3The preparation method of-LDH laminated films Download PDF

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CN106222685B
CN106222685B CN201610698073.1A CN201610698073A CN106222685B CN 106222685 B CN106222685 B CN 106222685B CN 201610698073 A CN201610698073 A CN 201610698073A CN 106222685 B CN106222685 B CN 106222685B
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conductive glass
ldh
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laminated films
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CN106222685A (en
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范晓莉
何建平
王涛
高斌
黄现礼
郭虎
薛海荣
龚浩
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Nanjing University of Aeronautics and Astronautics
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B9/00Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
    • C25B9/70Assemblies comprising two or more cells
    • C25B9/73Assemblies comprising two or more cells of the filter-press type
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
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    • C25B1/02Hydrogen or oxygen
    • C25B1/04Hydrogen or oxygen by electrolysis of water
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/50Processes
    • C25B1/55Photoelectrolysis
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    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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Abstract

The present invention relates to a kind of WO of photoelectrocatalysis water decomposition3‑LDH(Layered double hydroxide, layered double-hydroxide)The preparation method of laminated film, comprises the steps of:Ammonium tungstate and concentrated hydrochloric acid is soluble in water, it is transferred to after stirring in autoclave liner, it is inserted into the electro-conductive glass FTO that will have been pre-processed, then solvent thermal reaction is carried out, cooled to room temperature, after electro-conductive glass washing, drying, in air atmosphere, 450 550 DEG C of heat treatment at least 1 h, obtain WO3Film;Again with WO3Film is working electrode, and the aqueous solution of nickel nitrate and ferric nitrate is electrolyte, in WO3Film surface galvanostatic deposition NiFe LDH, finally obtain WO3LDH laminated films;Product produced by the present invention is higher than electricity conversion, and photooxidation water take-off potential is low, has broad application prospects in fields such as photocatalytic degradation, photoelectrocatalysis water decomposition, artificial photosynthesis, light auxiliary energy storage batteries.

Description

A kind of WO of photoelectrocatalysis water decomposition3The preparation method of-LDH laminated films
Technical field
The present invention relates to field of inorganic nonmetallic material, especially a kind of WO of photoelectrocatalysis water decomposition3-LDH (Layered double hydroxide)The preparation method of laminated film.
Background technology
Last century 70, increasing environmental pollution and energy shortage problem have allowed it was recognized that the two are latent Global crisis.For the sustainable development of human society, the pollution-free technology of development environment close friend and alternative cleaning The energy is extremely urgent.Among numerous environmentally protective and renewable energy source item, the semiconductor of natural daylight energy is utilized Photocatalysis technology has become one of most promising technology.1972, Japanese scholars Fujishima and Honda were reported for the first time In TiO2Research [the A. Fujishima and K. Honda. Photolysis- of electrode surface photoelectric decomposition water decomposition of water at the surface of an irradiated semiconductor. Nature, 1972,238,37-38.], this event for being considered to have milestone significance has greatly been pushed and has been urged based on photocatalysis/photoelectricity The research of the light energy switch technology of change technology.Unfortunately, the forbidden band of titanium dioxide is wider(3-3.2 eV), what can be utilized arrives Up to earth surface solar energy less than 5%(Ultraviolet light, λ<400 nm), it is made to can't be ideal catalysis material.Currently, Numerous studies are all concentrated in visible light wave range(400<λ<800 nm)It responds and the narrow band gap with highlight catalytic active is partly led [A. B. Murphy, P. R. F. Barnes, L. K. Randeniya, I. C. Plumb, I. E. on body material Grey, M. D. Horne and J. A. Glasscock. Efficiency of solar water splitting using semiconductor electrodes. Int. J. Hydrogen Energy, 2006, 31, 1999- 2017.], such as WO3、Fe2O3、BiVO4Equal oxides, CdS, Cu2ZnSnS4Sulfides, the nitrogen oxides such as TaON, ZnGaON, with And nonmetallic compound g-C3N4.
WO3It is a kind of N-shaped semiconductor material with wide forbidden band with good physical and chemical stability, by filling up the low of electronics It can valence band(Valence band, VB)With empty higher energy conduction band(Conduction band, CB)It constitutes.With other photochemical catalysts It compares, the energy gap of tungstic acid is relatively narrow, can have preferable absorption in visible-range, can be very good using in sunlight Visible light resource.But if using only tungstic acid semiconductor, existed easily unstable by photoetch, photo-catalysis capability The defects of, so this field expands a large amount of research around how improving tungstic acid photo-catalysis capability, it is proposed that many changes Property means reduce its energy gap with this, enhance the ability of light absorption, while also to promote its light induced electron and hole Separative efficiency reduces the combined efficiency of electronics and hole, promotes catalytic capability.Common method has WO3With other semiconductors Material(TiO2、ZnO、BiVO4)Carry out compound, but these methods cannot all reduce WO3Photoelectricity aoxidizes the overpotential of water.
Layered double-hydroxide LDH(Layered double hydroxide)It is a kind of co-catalysis of moisture parsing oxygen Agent can effectively reduce the overpotential of analysis oxygen, while can constitute hetero-junctions with other semi-conducting materials again to improve electronics The separating capacity in hole.Currently, utilizing WO3Combine to form WO with layered double-hydroxide LDH3The skill of-LDH laminated films Art, there is not been reported.
Invention content
In view of the above-mentioned problems, the present invention, which provides one kind, having efficient photoelectricity treater catalytic water capacity of decomposition WO3-LDH(Layered double hydroxide)The preparation method of laminated film, what this method was realized in:
(1)It is the ammonium tungstate solution of 0.017 g/ml to take mass concentration, adjusts pH=1, is placed in 40 DEG C of environment and stirs to shape At colourless transparent solution, it is then transferred in the polytetrafluoroethyllining lining of autoclave;
(2)By the FTO electro-conductive glass oblique cuttings pre-processed in inner liner of reaction kettle, solution did not had glass, and conduction is downwards;
(3)Reaction kettle is tamping to be put into baking oven and carries out solvent thermal reaction, is placed in 160 ~ 200 DEG C of environment and reacts at least 1h, cooled to room temperature;Taking-up FTO electro-conductive glass, 40 ~ 100 DEG C of dryings after being washed successively with deionized water, absolute ethyl alcohol, Obtain nattierblue film;
(4)By electro-conductive glass under air atmosphere protection, it is placed in 450 ~ 550 DEG C of environment and is heat-treated at least 1h, grown There is WO3FTO electro-conductive glass;
(5)Using three-electrode system, with WO3Film is working electrode, and the aqueous solution of nickel nitrate and ferric nitrate is electrolyte, In WO3Film surface galvanostatic deposition NiFe-LDH is passed through -0.10 mA/cm of constant current2, 50 ~ 400 s of electro-deposition obtains WO3- LDH laminated films.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated films, pretreatment Step is:Electro-conductive glass is cut into the small pieces of 3 cm x, 1.5 cm, uses acetone, deionized water, absolute ethyl alcohol ultrasound clear respectively It washes(The power of ultrasonic cleaning is 100 W)30 min, and cleaned electro-conductive glass is placed in absolute ethyl alcohol and is preserved, before use It is dried up with hair-dryer.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated films, step (5)The aqueous solution of the nickel nitrate and ferric nitrate obtains by the following method:By 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe(NO3)3·9H2O is added in 100mL water, that is, obtains the solution.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated films, step (1)Adjusting pH=1 refers to adjusting pH=1 with the HCl solution of a concentration of 6 mol/L.
Further, the WO of photoelectrocatalysis water decomposition of the present invention3In the preparation method of-LDH laminated films, step (5)The three-electrode system refers to, with WO3FTO electro-conductive glass be working electrode, Pt pieces be to electrode, saturation calomel Electrode is that reference electrode is formed by system.
The present invention is by WO3Combine to form WO with layered double-hydroxide LDH3- LDH laminated films, light induced electron and sky The separative efficiency in cave is high, and oxygen evolution potential is low, to make its catalytic capability be remarkably enhanced.The WO that the present invention obtains3- The photooxidation water decomposition current density of LDH laminated films is much larger than pure WO3, and take-off potential is lower show preferable application before Scape.
Description of the drawings
Fig. 1 is the WO prepared by the embodiment of the present invention 13The electron scanning micrograph of-LDH laminated films.
Fig. 2 is the WO prepared by the embodiment of the present invention 13The transmission electron microscope photo of-LDH laminated films.
Fig. 3 is the WO prepared by the embodiment of the present invention 13The distribution diagram of element of Film laminated film scanning Electronic Speculum.
Fig. 4 is the WO that the embodiment of the present invention 1 obtains3The WO that-LDH laminated films and embodiment 4 obtain3The XPS of film schemes Spectrum.
Fig. 5 is the photocurrent curve figure of the embodiment of the present invention 1 and 4.
Fig. 6 is the WO that embodiment 4 obtains3Film scanning electromicroscopic photograph.
Specific implementation mode
Embodiment is related to reagent and equipment source:
Ammonium tungstate analyzes pure AR, is purchased from Sinopharm Chemical Reagent Co., Ltd.;
Acetone, absolute ethyl alcohol, hydrochloric acid, six water nickel nitrates, nine water ferric nitrates and anhydrous sodium sulfate are the pure AR of analysis, are purchased from Nanjing Chemistry Reagent Co., Ltd.;
FTO electro-conductive glass:Pilkington products, thickness 2.2mm, 7 ohm of resistance, light transmittance 80%;
Autoclave:In triumphant Asia KH-50, enclosure material be 304 stainless steels, liner is polytetrafluoroethylene (PTFE);
Electrochemical workstation:Shanghai Chen Hua Instrument Ltd., CHI660A;
Scanning electron microscope:Japanese Hitachi companies S-4800, accelerating potential 10kV;
Transmission electron microscope:FEI company's Ts ecnai G2, accelerating potential 200kV;
X-ray photoelectron spectroscopy(XPS):5000 VersaProbe electron spectrometers of PHI.
Pretreated FTO electro-conductive glass described in embodiment is obtained by:FTO electro-conductive glass is cut out to 3 cm x The small pieces of 1.5 cm use acetone, deionized water and absolute ethyl alcohol to be cleaned by ultrasonic FTO electro-conductive glass 30min respectively(It is cleaned by ultrasonic Power is 100 W), the FTO electro-conductive glass after cleaning is placed in absolute ethyl alcohol and is preserved, hair dryer is used before use(About 60 ~ 80 ℃)Drying.
Embodiment 1
(1)The ammonium tungstate for weighing 0.5 g is dissolved in 30 ml water, pH value of solution=1 is adjusted with 6 mol/L HCl solutions, 40 Solution is transferred to the polytetrafluoroethyllining lining of 50 ml autoclaves by stirring later until forming colourless transparent solution at DEG C In;
(2)By pretreated FTO electro-conductive glass piece oblique cutting inside inner liner of reaction kettle, make conductive face-down;
(3)Reaction kettle sealing is tightly put into baking oven and carries out solvent thermal reaction, 180 DEG C of 5 h of thermal response are naturally cooled to Electro-conductive glass is washed by deionized water, absolute ethyl alcohol and after 40 DEG C dry, obtains nattierblue film by room temperature;
(4)By the electro-conductive glass with film under air atmosphere protection, 500 DEG C of 2 h of isothermal holding obtain yellow WO3Film.
(5)It is specific as follows using three-electrode system:With WO3FTO electro-conductive glass be working electrode, Pt pieces be to electricity Pole, saturated calomel electrode are reference electrode, and electrolyte contains 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe (NO3)3· 9H2O and 100 mL water, in WO3Film surface is with -0.10 mA/cm2Current density galvanostatic deposition NiFe-LDH, electricity is heavy The product time is that 200 s finally obtain WO3- LDH laminated films.
The WO that the present embodiment obtains3- LDH laminated film stereoscan photographs are shown in Fig. 1, it is seen that the WO of preparation3- LDH THIN COMPOSITEs Film is by rodlike WO3Particle and sheet LDH compositions.
The laminated film transmission electron microscope is shown in Fig. 2, and as shown in Figure 2, the product of synthesis is to crystallize good WO3Be covered in table The LDH materials in face form.
For the Elemental redistribution of the laminated film constituency scanning electron microscope as shown in figure 3, in Fig. 3, A is the shape for the embodiment 1 chosen Looks figure, B-E are respectively the distribution map of region W, O, Ni, Fe element, it is seen that element W, O, Fe, Ni are evenly distributed in film In.
Embodiment 2
(1)The ammonium tungstate for weighing 0.5 g is dissolved in 30 ml water, pH=1 of solution is adjusted with 6 mol/L HCl, at 40 DEG C Lower stirring is transferred to until forming colourless transparent solution in the polytetrafluoroethyllining lining of 50 ml autoclaves later;
(2)By pretreated FTO electro-conductive glass piece oblique cutting inside inner liner of reaction kettle, make conductive face-down;
(3)Reaction kettle sealing is tightly put into baking oven and carries out solvent thermal reaction, 160 DEG C of 1 h of reaction naturally cool to room Electro-conductive glass is obtained nattierblue film by temperature after deionized water, absolute ethyl alcohol washing and 60 DEG C of dryings successively;
(4)Under air atmosphere protection, 450 DEG C of heat treatments keep the temperature 1 h, obtain the electro-conductive glass with film of gained The WO of yellow3Film.
(5)Using three-electrode system, with WO3FTO electro-conductive glass be working electrode, Pt pieces be to electrode, saturation it is sweet Mercury electrode is reference electrode, and electrolyte contains 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe (NO3)3·9H2O and 100 ML water, in WO3Film surface is with -0.10 mA/cm2Current density galvanostatic deposition NiFe-LDH, electrodeposition time be 50 s, It is final to obtain WO3- LDH laminated films.
Embodiment 3
(1)The ammonium tungstate for weighing 0.5 g is dissolved in 30 ml water, and the pH to 1 of solution is adjusted with 6 mol/L HCl solutions, Stirring is transferred to until forming colourless transparent solution in the polytetrafluoroethyllining lining of 50 ml autoclaves later at 40 DEG C;
(2)By pretreated FTO electro-conductive glass piece oblique cutting inside inner liner of reaction kettle, make conductive face-down;
(3)Reaction kettle sealing is tightly put into baking oven and carries out solvent thermal reaction, 200 DEG C of 7 h of reaction naturally cool to room Temperature obtains nattierblue film by electro-conductive glass after deionized water, absolute ethyl alcohol washing and 100 DEG C of dryings;
(4)Under air atmosphere protection, 550 DEG C of heat treatments keep the temperature 2 h, obtain the electro-conductive glass with film of gained The WO of yellow3Film.
(5)Using three-electrode system, with WO3FTO electro-conductive glass be working electrode, Pt pieces be to electrode, saturation it is sweet Mercury electrode is reference electrode, and electrolyte contains 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe (NO3)3·9H2O and 100 ML water, in WO3Film surface is with -0.10 mA/cm2Current density galvanostatic deposition NiFe-LDH, electrodeposition time 400 S finally obtains WO3- LDH laminated films.
Embodiment 4
(1)The ammonium tungstate for weighing 0.5 g is dissolved in 30 ml water, and the pH to 1 of solution is adjusted with 6 mol/L HCl solutions, 40 oCLower stirring is transferred to until forming colourless transparent solution in the polytetrafluoroethyllining lining of 50 ml autoclaves later;
(2)By pretreated electro-conductive glass(FTO)Piece oblique cutting makes conductive face-down inside inner liner of reaction kettle;
(3)Reaction kettle sealing is tightly put into baking oven and carries out solvent thermal reaction, 180 DEG C of 5 h of reaction naturally cool to room Temperature obtains nattierblue film by electro-conductive glass after deionized water, absolute ethyl alcohol washing and 80 DEG C of dryings;
(4)For the electro-conductive glass with film of gained under air atmosphere protection, 500 DEG C of 2 h of isothermal holding obtain yellow WO3Film.
The WO that the present embodiment is obtained3Film(The pure WO of LDH is not deposited3Film)As a comparison sample, scanning electron microscope is shone Piece is as shown in fig. 6, the WO prepared as seen from Figure 63Film is by rodlike WO3Particle forms.
The WO that embodiment 1 obtains3The WO that-LDH laminated films and embodiment 4 obtain3The XPS collection of illustrative plates of film as shown in figure 4, From fig. 4, it can be seen that 1 product WO of embodiment3Surface is NiFe-LDH, and the valence state composition of 4 product of embodiment is strictly WO3
The photoelectric current of test product, test specific method are:Test equipment is CHI660A electrochemical workstations, three electrodes Test system is using Pt pieces as to electrode, saturated calomel electrode(SCE)As reference electrode device, with WO3And WO3- LDH's FTO glass is working electrode, and light passes through quartz glass electrolytic cell, and from the back sides FTO vertical irradiation, all test areas are fixed on 1cm2, the method for selecting linear scan, 0 ~ 1.5V of sweep interval(vs. SCE).Electrolyte uses the Na of 0.2 mol/L2SO4It is molten Liquid, pH value 6.6, logical nitrogen half an hour, dissolved oxygen is removed before testing.Light source uses the 200W xenon lamps of Newport companies, Additional filter plate(λ>420 nm).Fig. 5 is the photocurrent curve of embodiment 1 and 4, with pure WO3(Embodiment 4)It compares, WO3-LDH Laminated film(Embodiment 1)Photooxidation water decomposition current density be much larger than the latter, and take-off potential it is lower show it is preferable Application prospect.
It is described above to be only used as presently preferred embodiments of the present invention and application, the limitation of the present invention is should not be construed as, it is all The invention for being modification, replacement and the change in the other forms made of technological thought based on the present invention and realizing belongs to this hair Bright protection domain.Can several change can be cooked the present invention under the premise of not departing from the present invention for those skilled in the art Into and modification, these improvement and modification are also considered as protection scope of the present invention.

Claims (4)

1. a kind of WO of photoelectrocatalysis water decomposition3The preparation method of-LDH laminated films, which is characterized in that be as follows:
(1)It is the ammonium tungstate solution of 0.017g/ml to take mass concentration, adjusts pH=1, is placed in stirring in 40 DEG C of temperature and extremely forms nothing Color clear solution, is transferred in autoclave;
(2)In a kettle by pretreated FTO electro-conductive glass oblique cutting, it is immersed in step(1)In the solution of acquisition, conducting surface Downwards;
(3)Reaction kettle is placed in 160 ~ 200 DEG C of environment and reacts at least 1h, is cooled to room temperature;FTO electro-conductive glass is taken out, successively 20 ~ 100 DEG C of dryings after being washed with deionized water, absolute ethyl alcohol;
(4)Electro-conductive glass is placed in 450-550 DEG C of temperature and is heat-treated at least 1h, is obtained with WO3The FTO electro-conductive glass of film;
(5)Using three-electrode system, with WO3The FTO electro-conductive glass of film is working electrode, the water of nickel nitrate and ferric nitrate Solution is electrolyte, in WO3Film surface galvanostatic deposition NiFe-LDH is passed through -0.10 mA/cm of constant current2, electro-deposition 50- 400 s, that is, obtain WO3- LDH laminated films.
2. the WO of photoelectrocatalysis water decomposition according to claim 13The preparation method of-LDH laminated films, which is characterized in that Step(2)Described in pretreated FTO electro-conductive glass be obtained by:Acetone, deionized water and absolute ethyl alcohol are used respectively It is cleaned by ultrasonic FTO electro-conductive glass 30min, the FTO electro-conductive glass after cleaning is placed in absolute ethyl alcohol and is preserved, preceding drying is used.
3. the WO of photoelectrocatalysis water decomposition according to claim 23The preparation method of-LDH laminated films, which is characterized in that Step(5)What the aqueous solution of the nickel nitrate and ferric nitrate was obtained by:By 2.181 g Ni (NO3)2·6H2O and 1.784 g Fe(NO3)3·9H2O is added in 100mL water, that is, obtains the solution.
4. the WO of photoelectrocatalysis water decomposition according to claim 33The preparation method of-LDH laminated films, which is characterized in that Step(1)PH=1 that adjusts refers to adjusting pH value of solution=1 with the HCl of a concentration of 6 mol/L.
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