CN109865525A - A kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material - Google Patents
A kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of CoPi/Ag/ pucherite composite photoelectric anode material, are that CoPi/Ag is successfully loaded to BiVO by hydrothermal deposition4Surface forms stable photo cathode laminated film CoPi/Ag/BiVO4.The present invention utilizes the effect of plasma Ag nano particle and Co-Pi co-catalyst, expands pucherite to visible absorption range, allows to effectively capture light, reduce charge transfer resistance, accelerate the fast transferring of carrier, to inhibit the compound of electron-hole pair, and then improves BiVO4The PhotoelectrocatalytiPerformance Performance of complex light electrode.
Description
Technical field
The present invention relates to a kind of BiVO4 based composites, are related to a kind of CoPi/Ag/BiVO4The preparation side of optical anode material
Method is reacted mainly as photo cathode material for optical electro-chemistry water decomposition.
Background technique
Economic fast-developing bring energy shortage and environmental pollution is two hang-ups that the mankind face at present, therefore is sought
Looking for the new energy of clean and effective and curbing environmental pollution just is particularly important.Solar energy has inexhaustible, nothing
The advantages that polluting and is renewable, Hydrogen Energy has many advantages, such as that high fuel value and combustion product are pollution-free, therefore, utilizes solar energy photodissociation
Water prepares hydrogen as one of Future New Energy Source approach, is just increasingly subject to the great attention of people, photocatalysis technology is because in moisture
The fields such as hydrogen manufacturing and pollutant catalytic degradation of solution have outstanding advantages and as one of current research hotspots.Photocatalysis technology at present
Most distinct issues are: (1) Solar use is limited, and typical semiconductor light can only absorb the ultraviolet portion in sunlight according to agent
Point；(2) catalytic efficiency is relatively low.Scholars put forth effort on the spectral absorption range for expanding photocatalysis punishment in view of the above problems and searching can
Light-exposed catalyst, this will have an important influence on the utilization efficiency for improving solar energy.Too by optical electro-chemistry (PEC) system
The water decomposition that sun can drive is to generate clean fuel hydrogen (H using solar energy abundant2) effective ways.Solar energy photocatalytic
During hydrogen manufacturing, photocatalysis performance is mainly to be determined by the structure and performance of semiconductor material itself, therefore develop chemistry
Property is stable, the semiconductor material high to light utilization efficiency is the key that solve solar energy photocatalytic hydrogen producing technology.
In many semiconductor materials, pucherite (BiVO4) as visible light catalyst be ideal photochemical catalyzing
Hydrogen material is produced, while its is cheap, it is nontoxic.However, it but exists, photo-generated carrier is compound fastly, hole interfacial migration rate is slow
And the disadvantages of light corruption candle.The photocatalysis Decomposition aquatic products oxygen efficiency reported at present is all also far below its theoretical maximum, and people adopt
Such as noble metal decorated in many ways, element doping, surface modification improve its photocatalysis efficiency, but most of all compare
Complicated and noble metal is expensive.Therefore there is an urgent need to it is further proposed that reducing BiVO by people4Light induced electron and hole-recombination
Effective ways.In recent years, a large amount of research has solved BiVO4Electron-hole pair is in conjunction with low with solar conversion efficiency
The problem of.Currently, BiVO4Photoelectrochemical behaviour can obtain a degree of raising by various methods.Universal method
It include: ion doping, Morphological control, with WO3、ZnFeO4, graphene oxide, BiOI formed hetero-junctions, load produce oxygen co-catalyst
Co3O4, NiO, FeOOH, NiOOH etc., or in surface depositing noble metal nanoparticle Ag, Au etc..Due to noble metal nano grain
Sub- surface plasmon resonance effect, noble metal can be very good to improve photocatalysis performance and optical electro-chemistry in conjunction with semiconductor
Energy.Currently, being sensitized TiO using noble metal2、SrTiO3, ZnO etc. be widely used in photocatalysis degradation organic contaminant
The fields such as water are decomposed with three-electrode system optical electro-chemistry.However, we prefer to replace noble metal to reach with the metal of low cost
To better economic benefit.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of CoPi/Ag/ pucherite composite photoelectric anode, utilize plasma
The effect of body Ag nano particle and Co-Pi co-catalyst expands pucherite to visible absorption range, and then improves BiVO4
The PhotoelectrocatalytiPerformance Performance of complex light electrode.
One, CoPi/Ag/BiVO4The preparation of photo cathode
The method that the present invention prepares CoPi/Ag/ pucherite complex light electrode is using electrochemical deposition process that CoPi and Ag is same
When successfully loaded to porous BiVO4On film.Specific preparation method the following steps are included:
(1) preparation of Ag solution: sodium hydroxide solution is added in silver nitrate solution, after forming silver hydroxide brown precipitate, drop
Add ammonium hydroxide until solution becomes clarification, as Tollens solution；Tollens solution is added dropwise in glucose solution again, at 60 DEG C
It is vigorously stirred in ~ 70 DEG C of water-baths, the Ag solution of glassy yellow is made.Wherein, the molar ratio of sodium hydroxide and silver nitrate be 1:0.25 ~
1:0.3；The molar ratio of Tollens and glucose is 1:4 ~ 1:5.
(2) CoPi/BiVO4The preparation of photo cathode material: the 0.1 M potassium phosphate that cobalt nitrate solution is added to pH=7 is delayed
Wiring solution-forming in fliud flushing, and by BiVO4Light anode is put into the solution, in the case where Xenon light shining CV electro-deposition 200s ~
300s is clear, dry to get CoPi/BiVO4Optical anode material.Wherein, the molar ratio of cobalt nitrate and potassium phosphate is 1:0.2 ~ 1:
0.5。
(3) CoPi/Ag/BiVO4The preparation of photo cathode material: cobalt nitrate solution is added to 0.1 M phosphoric acid of pH=7
Wiring solution-forming in potassium buffer, the Ag solution that step (1) preparation is added into the solution stir evenly；And by BiVO4Light anode
Be put into the mixed solution, CV electro-deposition 200s ~ 300s in the case where Xenon light shining, cleaning, it is dry to get CoPi/Ag/
BiVO4Optical anode material.Wherein, the molar ratio of cobalt nitrate and potassium phosphate is 1:0.2 ~ 1:0.5；Ag in cobalt nitrate and Ag solution
Molar ratio is 1:0.01 ~ 1:0.03.
Two, CoPi/Ag/BiVO4The characterization of photo cathode material
Fig. 1 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4XRD diagram.As it can be seen that BiVO4All diffraction maximums show it
For monoclinic crystal, and occur without the diffraction maximum of other impurity peaks and other its crystal phases, shows the BiVO of monocline crystal phase4Succeed
Preparation.Other diffraction maximums are FTO(JCPDS. No. 41-1445) tetragonal phase SnO in substrate2Diffraction maximum.CoPi/BiVO4With
CoPi/Ag/BiVO4The intensity of diffraction maximum also enhances accordingly, and reason may be the crystallization with the extension composite material of time
Degree is more preferable.
Fig. 2 is pure BiVO4(a), CoPi/BiVO4(b) and CoPi/Ag/BiVO4(c) scanning electron microscope (SEM) photograph.As can be seen from Figure 2,
Relatively pure BiVO4Film, CoPi/BiVO4It can see that porous mass increased significantly on film.And in CoPi/Ag/BiVO4Film
On, it is clear that in pure BiVO4Uniform CoPi/Ag compound has been attached on film.So further proving
CoPi/Ag compound has successfully loaded to BiVO4On film.
Fig. 3 is CoPi/Ag/BiVO4Element mapping graph.Fig. 3 show to have in complex light anode material Bi, O, V, P,
Co, Ag element exist, and illustrate that material is successfully prepared.
Three, CoPi/Ag/BiVO4The photoelectrochemical behaviour of photo cathode material is tested
Fig. 4 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4The linear scan figure of electrode light reaction.BiVO4、CoPi/
BiVO4And CoPi/Ag/BiVO4For the photoelectrocatalysis water oxidation susceptibility of electrode in the analog light source of AM 1.5G, pH is 6.86
0.5MNa2SO4It is tested in solution.It was found that BiVO when no light4Film is almost without electric current, and in the voltage entirely tested
In range, the CoPi/Ag/BiVO of load C oPi/Ag compound4The electric current highest of electrode.In the normal potential 1.23 of water oxygen
When V vs.RHE, CoPi/Ag/BiVO4The photoelectric current of electrode is 3.31mA/cm2, it is BiVO4(1.32v) semiconductor is as sun
2.5 times of the theoretical photocurrent values that pole generates.Meanwhile with BiVO4Electrode is compared, CoPi/Ag/ BiVO4At the beginning of the water oxygen of electrode
Beginning current potential becomes 0.49V from 0.61 V, this shows that CoPi/Ag is a kind of excellent water oxidation promoters.
Fig. 5 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4The linear scan figure of electrode dark reaction.There is Fig. 5 can
Know, the BiVO for water oxygen4、CoPi/BiVO4And CoPi/Ag/BiVO4The take-off potential of light anode is respectively 2.26,2.20
With 2.19V(relative to RHE, j=0.1mA cm-2).The reduction of take-off potential shows that the CoPi of deposition and CoPi/Ag can be shown
Reduction BiVO4The take-off potential of water oxygen in the dark.
Fig. 6 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4The chopping the light current density linear scan figure of electrode.Institute
Having light anode all has outstanding photoelectric response characteristic, and fast response time.CoPi/Ag/BiVO4It is shown in entire voltage range
Show higher photoresponse value, this is consistent with the result in Fig. 4.
Fig. 7 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4Charge injection efficiency figure.The charge of electrode injects
Efficiency is the important parameter for the hole ratio that assessment participates in reaction.Within the system, charge injection efficiency can be by by electrode
The electric current of catalysis oxidation is divided by electrode catalyst Na2SO3The electric current of oxidation obtains.As shown, CoPi/Ag/BiVO4Electrode tool
There is highest charge injection efficiency, shows that the hole reactivity for reaching electrode surface after load C oPi/Ag compound is higher.
Fig. 8 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4IPCE figure.In order to better illustrate different wave length
Incident light irradiate the transmitting behavior of lower carrier, test in Na2SO4Photoelectric conversion effect when bias is 1.0V in electrolyte
Rate.Photoelectric conversion efficiency data are handled with following equation:
The Isc of IPCE=1240/(l Pin), wherein unit used in Isc, l and Pin is respectively μ A cm-2, nm and W m-2。
Calculated result shows between 350 ~ 500 nm, BiVO4Electrode photoelectric transfer efficiency is 3 ~ 11%, CoPi/Ag/BiVO4Electrode light
Photoelectric transformation efficiency is 20 ~ 38%.Fig. 8 shows BiVO4When more than 500 nm wavelength almost without photoelectric current, and bismuth metal is answered
Condensation material has photoelectric current between 500 ~ 550 nm wavelength.CoPi/Ag/BiVO4The photoelectric conversion efficiency ratio BiVO of electrode4Electrode
Much higher, this is also consistent with LSV figure.
Fig. 9 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4AC impedance figure of the electrode under illumination condition.For
Further exploration interfacial charge transfer process, has carried out the pure BiVO under illumination condition4With the electrochemical impedance of combination electrode
Compose (EIS) detection.Under light illumination, BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4The impedance electric arc of electrode becomes smaller, this meaning
Electric charge transfer between electrode and electrolyte it is very fast.CoPi/Ag/BiVO4It shows under irradiation and compares BiVO4And CoPi/
BiVO4Smaller impedance electric arc shows that the electric charge transfer after load C oPi/Ag is quicker.
In conclusion CoPi/Ag is successfully loaded to BiVO by hydrothermal deposition by the present invention4Surface forms stable light
Electric composite thin film anode CoPi/Ag/BiVO4。CoPi/Ag/BiVO4Density of photocurrent and light conversion efficiency be higher than pure BiVO4's
Photoelectric current.This outstanding performance is attributable to BiVO4The CoPi/Ag compound of outer layer load.It can effectively capture light,
Charge transfer resistance is reduced, accelerates the fast transferring of carrier, to inhibit the compound of electron-hole pair.In addition, CoPi/Ag/
BiVO4Electro-deposition also shows good stability, and the CoPi/Ag compound for showing that we prepare is a kind of light of good performance
Catalyst.New discovery will be the efficient of sustainable solar energy conversion, and stable photoelectrochemical system has paved road.
Detailed description of the invention
Fig. 1 is pure BiVO4、CoNi/BiVO4And CoPi/Ag/BiVO4XRD diagram.
Fig. 2 is (a) pure BiVO4、(b)CoPi/BiVO4(c) CoPi/Ag/BiVO4Scanning electron microscope (SEM) photograph.
Fig. 3 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4Element mapping graph.
Fig. 4 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4The linear scan figure of electrode light reaction.
Fig. 5 is pure BiVO4、CoPi/BiVO4And CoPi/Ag/BiVO4The linear scan figure of electrode dark reaction.
The pure BiVO of Fig. 64、CoPi/BiVO4And CoPi/Ag/BiVO4The chopping the light current density linear scan figure of electrode.
The pure BiVO of Fig. 74、CoPi/BiVO4And CoPi/Ag/BiVO4Charge injection efficiency figure.
The pure BiVO of Fig. 84、CoPi/BiVO4And CoPi/Ag/BiVO4Photoelectric conversion efficiency curve graph.
The pure BiVO of Fig. 94、CoPi/BiVO4And CoPi/Ag/BiVO4AC impedance figure of the electrode under illumination condition.
Specific embodiment
Below by specific embodiment to CoPi/Ag/BiVO of the present invention4Preparation and performance be described further.
(1) BiVO4The preparation of photo cathode
According to Kim and Choi seminar electro-deposition combination heat-treating methods, porous BiVO4Film is successfully prepared.Step: first
BiOI nanometer sheet is prepared by electrodeposition process with CHI 660D electrochemical workstation.With acetone/isopropanol/distilled water (volume ratio=
For FTO glass 1:1:1) being cleaned by ultrasonic as working electrode, Ag/AgCl (3.5 M KCl) electrode is reference electrode, Pt electricity
Extremely to electrode.Use 1MHNO350 mL0.4 M KI pH value of solution are adjusted to 1.5 ~ 1.7, add 0.970 g Bi (NO3)3·
5H2O is until dissolution, solution colour become orange red.Then 0.498 g 1,4- benzoquinones ethanol solution of 20ml is slowly added dropwise to stir
It mixes several minutes, solution becomes blood red again.Electro-deposition is scanned with cyclic voltammetry, voltage: -0.13-0 V, sweeps speed: 5 mV/ s.
BiOI film is obtained to be washed with distilled water.Then, by 0.1 mL, 0.2 M vanadyl acetylacetonate-dimethyl sulphoxide solution with micro
Syringe drips on the BiOI film prepared, rises to 450 DEG C of calcining 2h in Muffle furnace with 2 DEG C/min rate.Extra
V2O5It is impregnated and is eliminated with 1 M NaOH with bismuth oxide etc., leave the vanadic acid bismuth thin film of gilvous.The BiVO finally obtained4Electrode is used
Water washing is distilled to spontaneously dry.(this is that bibliography is done, not as protection content)
(2) preparation of Ag solution
The sodium hydroxide solution of 5mL0.8M is taken to be added in 10mL0.1M silver nitrate solution, after forming silver hydroxide brown precipitate, drop
Add ammonium hydroxide until solution becomes clarification, which is referred to as Tollens solution.0.25mLTollens solution is taken to be added dropwise to 100 mL
In 0.25M glucose solution, and it is vigorously stirred to obtain the Ag solution of glassy yellow in 70 DEG C of water-baths.
(3) CoPi/BiVO4The preparation of photo cathode
Wiring solution-forming in 0.1 M kaliumphosphate buffer (pH=7) is added in 0.5mM cobalt nitrate；By BiVO4It is molten that light anode is put into this
In liquid, CV electro-deposition 300s in the case where Xenon light shining is wash with distilled water, dry to get CoPi/BiVO4。
(4) CoPi/Ag/BiVO4The preparation of photo cathode
It takes 10 mL 0.5mM cobalt nitrates that the solution being made into 0.1 M kaliumphosphate buffer (pH=7) is added, is added into solution
0.1 mL Ag solution after mixing evenly, by BiVO4Light anode is put into the solution, CV electro-deposition in the case where Xenon light shining
300s, it is wash with distilled water, dry, obtain CoPi/Ag/BiVO4Optical anode material.
(5) CoPi/Ag/BiVO4Performance
With traditional three-electrode system connection CHI660D electrochemical workstation (Shanghai CHI) test, three electrodes are respectively Ag/
It AgCl(0.35MKCl) be reference electrode, platinum foil is to electrode and CoPi/Ag/BiVO4For working electrode.0.5 M of pH 6.86
Na2SO4 is electrolyte.The 300 W xenon lamps (CEL-HXF300) with optical filter are used as simulated solar irradiation, at room temperature from work
Electrode back side illuminaton, irradiated area 1cm2.Linear scan (LSV) test when sweeping speed and being 10 mV/s.Photoelectric conversion efficiency is used
The lower test of xenon lamp (PLS-SXE300C) irradiation with monochromator (71SWS, NewBide Science and Technology Ltd., Pekinese), it is additional
Voltage is 1.0 V Ag/AgCl (3.5 M).Under AM 1.5G irradiation, under direct current (DC) bias of 1.23 V and RHE, hand over
Galvanic electricity (AC) voltage amplitude is 5 mV, collects the result of AC impedance.
As a result, it has been found that: in the 1.23 V vs.RHE of normal potential of water oxygen, CoPi/Ag/BiVO4The photoelectric current of electrode
For 3.31mA/cm2；CoPi/Ag/BiVO4The charge injection efficiency of electrode reaches 53.3%；Under 0.1V bias, 350 ~
Between 500 nm, CoPi/Ag/BiVO4Electrode photoelectric transfer efficiency is 38%.
Claims (5)
1. a kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material, comprising the following steps:
(1) preparation of Ag solution: sodium hydroxide solution is added in silver nitrate solution, after forming silver hydroxide brown precipitate, drop
Add ammonium hydroxide until solution becomes clarification, as Tollens solution；Tollens solution is added dropwise in glucose solution again, at 60 DEG C
It is vigorously stirred in ~ 70 DEG C of water-baths, the Ag solution of glassy yellow is made；
(2) CoPi/BiVO4The preparation of optical anode material: cobalt nitrate solution is added in 0.1 M kaliumphosphate buffer of pH=7
Wiring solution-forming, and by BiVO4Light anode is put into the solution, CV electro-deposition 200s ~ 300s in the case where Xenon light shining, clearly
Clear, drying is to get CoPi/BiVO4Optical anode material；
(3) CoPi/Ag/BiVO4The preparation of optical anode material: cobalt nitrate solution is added to 0.1 M kaliumphosphate buffer of pH=7
Middle wiring solution-forming, the Ag solution that step (1) preparation is added into the solution stir evenly；And by BiVO4It is mixed that light anode is put into this
It closes in solution, CV electro-deposition 200s ~ 300s in the case where Xenon light shining, cleaning, drying are to get CoPi/Ag/BiVO4Light sun
Pole material.
2. a kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material as described in claim 1, it is characterised in that:
In step (1), the molar ratio of sodium hydroxide and silver nitrate is 1:0.25 ~ 1:0.30.
3. a kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material as described in claim 1, it is characterised in that:
In step (1), the molar ratio of Tollens and glucose is 1:4 ~ 1:5.
4. a kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode material as described in claim 1, it is characterised in that:
In step (2), (3), the molar ratio of cobalt nitrate and potassium phosphate is 1:0.2 ~ 1:0.5.
5. a kind of preparation method of CoPi/Ag/ pucherite composite photoelectric anode as described in claim 1, it is characterised in that: step
(3) in, the molar ratio of Ag is 1:0.01 ~ 1:0.03 in cobalt nitrate and Ag solution.
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Application publication date: 20190611 |