CN109308982A - A kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method - Google Patents
A kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method Download PDFInfo
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Abstract
The invention discloses a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation methods, comprising the following steps: (1) uses and enrich cheap bismuth source, copper source, in alkaline condition hydrothermal synthesis CuBi2O4Nanometer rods；(2) ion alternation physisorphtion is used, silver ion is supported on CuBi2O4In nanometer rods；(3) using FTO electro-conductive glass as substrate, CuBi is formed using drop-coating2O4/ Ag film, CVD method annealing；(4) material removing is transferred to by second block of FTO glass using particle transfer technology, be ultrasonically treated.Then physical absorption nitrogen-doped carbon quantum dot prepares nitrogen-doped carbon quantum dot and the co-modified CuBi of silver2O4Nanometer rods photocathode.The photocathode being prepared by the method for the invention under visible light illumination, shows good photoelectric catalytically active and visible light-responded characteristic, and stability gets a promotion, and can be efficiently applied to photoelectrocatalysis water decomposition and produce hydrogen field.
Description
Technical field
The present invention relates to optoelectronic materials technologies, and in particular to a kind of nitrogen-doped carbon quantum dot and silver-colored co-modified CuBi2O4
Nanometer rods photocathode preparation method.
Background technique
Environmental pollution and energy crisis have become the necessarily threat of human development, and there is an urgent need to find green and can hold at present
Continuous alternative energy source.Titanium dioxide (TiO is found from Hondas in 1972 and Teng Dao2) optoelectronic pole is in photoelectrochemical cell (PEC)
Since producing hydrogen, water becomes the sustainable focus material of energy by the purposes that decomposition can be used as hydrogen generation source, especially
Light PEC water decomposition can effectively convert solar energy into sustainable green energy resource-hydrogen, be acknowledged as solving environment dirt
The effective way of dye and crisis.Nevertheless, TiO2Wide energy gap (3.2eV) make its be only capable of absorb ultraviolet light, account for about about
1.4% solar energy causes light utilization efficiency low.Therefore, exploitation has the narrow bandgap semiconductor material of effective visible light activity extremely
It closes important.
Element metal oxide p-type semiconductor CuBi abundant2O4Since its unique property is considered a kind of effective
Water decomposition application material, such as sufficiently narrow direct band gap (1.8eV), very positive take-off potential and low cost.Assuming that all
Energy is absorbed and utilized by 100% efficiency, and the theoretical maximum density of photocurrent under AM1.5 irradiation can reach 19.7-29.0mA/cm2。
Regrettably, CuBi2O4Charge carrier transport and kinetics it is bad caused by photoelectric conversion efficiency it is poor and its with electricity
Corroding when electrolyte solution contacts from photoelectricity is unstable, limits its application and competitiveness in PEC water decomposition.
Improve CuBi2O4Optoelectronic pole makes it have optimal solar energy-chemical energy transfer efficiency, can pass through nanostructure
Design, selective element doping are realized, these implementations of strategies with certain semiconductors formation hetero-junctions or load cocatalyst
Facilitate light induced electron quick separating and be transported to surface to carry out proton reduction, therefore can improve in electrolyte solution
CuBi2O4Light conversion efficiency.But these results can not be compared with its theoretical value.Such as how simple and cheap mode
Obtain the CuBi with more high-photoelectric transformation efficiency and optical stability2O4Photocathode is still a challenge.
Summary of the invention
In view of the deficiencies of the prior art, the present invention is intended to provide a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation side
Method, nitrogen-doped carbon quantum dot and nano silver codope can effectively inhibit electrons and holes surface recombination and improve reaction power
It learns, with naked CuBi2O4Optoelectronic pole is compared, and PEC performance is greatly improved.
In order to achieve the above technical purposes, the present invention adopts the following technical scheme:
A kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method, includes the following steps:
Step S1, by 2.42g Bi (NO3)3·5H2O、0.6g Cu(NO3)3·5H2O and 0.87g NaOH is added sequentially to
In 40mL deionized water, stirs dissolution in 3 hours and obtain solution；
Step S2, solution obtained in step S1 is transferred in the autoclave of polytetrafluoroethyllining lining, 180 DEG C of items
It reacts under part for 24 hours, is cooled to room temperature after reaction to autoclave, the solid product being centrifugated out in solution, with nothing
Water-ethanol and high purity water alternately and repeatedly respectively wash dries in the drying box for be placed on afterwards three times 60 DEG C, obtains CuBi2O4Nanometer rods；
Step S3, CuBi obtained in 30mg step S2 is weighed2O4Nanometer rods are added in 10mL dehydrated alcohol, then plus
Enter the 0.05M AgNO of different volumes3Solution stirs 3h to adsorption equilibrium, dries, obtain powdered in 60 DEG C of drying box
Product；
Step S4, FTO glass is sequentially placed into acetone, dehydrated alcohol, is cleaned by ultrasonic in deionized water and takes out, then with anhydrous
Ethyl alcohol cleaning, N2Drying；
Step S5, it disperses the powdery product in 20mg step S3 in 0.1mL dehydrated alcohol and forms suspension, then
Drop coating is dried, then using CVD method in N on the FTO glass of the method processing through step S4 in 60 DEG C of drying box2Gas
The lower 450 DEG C of annealing 4h of atmosphere obtains the CuBi of Ag doping2O4Nanometer rods；
Step S6, the CuBi for being adulterated Ag made from step S5 as carbon paste band2O4Nanometer rods are removed from FTO glass to be turned
It moves on on the FTO glass of another piece of method processing through step S4, it is excessive to remove then to carry out ultrasonication in water
Ag/CuBi2O4Nano-bar material can obtain FTO/CuBi2O4/ Ag photocathode；
Step S7, by FTO/CuBi made from step S62O4/ Ag photocathode is placed in 10mL dehydrated alcohol, is added different
The nitrogen-doped carbon quantum dot solution of volume, 3h is to adsorption equilibrium for stirring, dries in 60 DEG C of drying boxes, and peripheral regions are used when drying
Epoxy resin covering can obtain nitrogen-doped carbon quantum dot and the co-modified CuBi of silver after drying2O4Nanometer rods photocathode.
Further, in step S2, the liner volume of the autoclave of the polytetrafluoroethyllining lining is 50mL.
Further, in step S3, the 0.05M AgNO3The addition volume of solution is 0.4mL.
Further, in step S5, by hanging drop be coated in the method through step S4 processing FTO glass on specific side
Method are as follows: pipette 0.05mL hanging drop on the FTO glass of the method processing through step S4 with liquid-transfering gun.
Further, in step S6, the ultrasonic power of the ultrasonication is 60W, ultrasonic time 15min.
Further, in step S7, the addition volume of the nitrogen-doped carbon quantum dot solution is 0.6mL.
The beneficial effects of the present invention are:
The method of the present invention, which is used, enriches cheap bismuth source, copper source, in alkaline condition hydrothermal synthesis CuBi2O4Nanometer rods, then
Using ion alternation physisorphtion, silver ion is supported on CuBi2O4In nanometer rods；Thereafter using FTO electro-conductive glass as substrate,
CuBi is formed using drop-coating2O4/ Ag film, CVD method annealing, and material removing is transferred to the using particle transfer technology
Two blocks of FTO glass, ultrasonic treatment.Last physical absorption nitrogen-doped carbon quantum dot prepares nitrogen-doped carbon quantum dot and silver is co-modified
CuBi2O4Nanometer rods photocathode.
Nitrogen-doped carbon quantum dot obtained and the co-modified CuBi of silver by the method for the invention2O4Nanometer rods photocathode (FTO/
CuBi2O4/ Ag/N-CQD) under visible light illumination, good photoelectric catalytically active and visible light-responded characteristic are shown, is stablized
Property get a promotion, can be efficiently applied to photoelectrocatalysis water decomposition produce hydrogen field.
Detailed description of the invention
Fig. 1 is the co-modified CuBi of nitrogen-doped carbon quantum dot and silver obtained in the embodiment of the present invention 12O4Nanometer rods photoelectricity yin
The SEM image of pole.
Fig. 2 is CuBi2O4The TEM image of/Ag/N-CQD composite material.
Fig. 3 is CuBi2O4Nanometer rods, CuBi2O4/ Ag material and CuBi2O4The XRD diffraction flower of/Ag/N-CQD composite material
Sample schematic diagram.
Fig. 4 is CuBi2O4Nanometer rods, CuBi2O4Nitrogen-doped carbon quantum dot obtained in/Ag material, the embodiment of the present invention 1
With the co-modified CuBi of silver2O4The solid diffusing reflectance spectra of nanometer rods photocathode.
Fig. 5 is CuBi2O4Nanometer rods, CuBi2O4/ Ag material, CuBi2O4The fluorescence Spectra of/Ag/N-CQD composite material.
Fig. 6 is FTO/CuBi2O4、FTO/CuBi2O4N doping carbon amounts obtained in/Ag optoelectronic pole and the embodiment of the present invention 1
Son point and the co-modified CuBi of silver2O4The impedance spectrum of nanometer rods photocathode.
Fig. 7 is FTO/CuBi2O4、FTO/CuBi2O4N doping carbon amounts obtained in/Ag optoelectronic pole and the embodiment of the present invention 1
Son point and the co-modified CuBi of silver2O4The MOtt-SchOttky curve of nanometer rods photocathode.
Fig. 8 is FTO/CuBi2O4、FTO/CuBi2O4N doping carbon amounts obtained in/Ag optoelectronic pole and the embodiment of the present invention 1
Son point and the co-modified CuBi of silver2O4The photoelectric properties figure of nanometer rods photocathode.
Fig. 9 is FTO/CuBi2O4、FTO/CuBi2O4N doping carbon amounts obtained in/Ag optoelectronic pole and the embodiment of the present invention 1
Son point and the co-modified CuBi of silver2O4The current versus time curve of nanometer rods photocathode.
Specific embodiment
Below with reference to attached drawing, the invention will be further described, it should be noted that the present embodiment is with this technology side
Premised on case, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to this reality
Apply example.
Embodiment 1
The present embodiment provides a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation methods, include the following steps:
Step S1, by 2.42g Bi (NO3)3·5H2O、0.6g Cu(NO3)3·5H2O and 0.87g NaOH is added sequentially to
In 40mL deionized water, stirs dissolution in 3 hours and obtain solution；
Step S2, solution obtained in step S1 is transferred in the autoclave of polytetrafluoroethyllining lining, 180 DEG C of items
It reacts under part for 24 hours, is cooled to room temperature after reaction to autoclave, the solid product being centrifugated out in solution, with nothing
Water-ethanol and high purity water alternately and repeatedly respectively wash dries in the drying box for be placed on afterwards three times 60 DEG C, obtains CuBi2O4Nanometer rods；
Step S3, CuBi obtained in 30mg step S2 is weighed2O4Nanometer rods are added in 10mL dehydrated alcohol, then plus
Enter the 0.05M AgNO of different volumes3Solution stirs 3h to adsorption equilibrium, dries, obtain powdered in 60 DEG C of drying box
Product；
Step S4, FTO glass is sequentially placed into acetone, dehydrated alcohol, is cleaned by ultrasonic in deionized water and takes out, then with anhydrous
Ethyl alcohol cleaning, N2Drying；
Step S5, the powdery product in 20mg step S3 is dissolved in 0.1mL dehydrated alcohol and forms suspension, then dripped
It is coated on the FTO glass of the method processing through step S4, is dried in 60 DEG C of drying box, then using CVD method in N2Atmosphere
Lower 450 DEG C of annealing 4h obtains the CuBi of Ag doping2O4Nanometer rods；
Step S6, the CuBi for being adulterated Ag made from step S5 as carbon paste band2O4Nanometer rods are removed from FTO glass to be turned
It moves on on the FTO glass of another piece of method processing through step S4, it is excessive to remove then to carry out ultrasonication in water
Ag/CuBi2O4Nano-bar material can obtain FTO/CuBi2O4/ Ag photocathode；
Step S7, by FTO/CuBi made from step S62O4/ Ag photocathode is placed in 10mL dehydrated alcohol, is added different
The nitrogen-doped carbon quantum dot solution of volume, 3h is to adsorption equilibrium for stirring, dries in 60 DEG C of drying boxes, and peripheral regions are used when drying
Epoxy resin covering can obtain nitrogen-doped carbon quantum dot and the co-modified CuBi of silver after drying2O4Nanometer rods photocathode.
Further, in step S2, the liner volume of the autoclave of the polytetrafluoroethyllining lining is 50mL.
Further, in step S3, the 0.05M AgNO3The optimal addition volume of solution is 0.4mL.
Further, in step S5, by hanging drop be coated in the method through step S4 processing FTO glass on specific side
Method are as follows: pipette 0.05mL hanging drop on the FTO glass of the method processing through step S4 with liquid-transfering gun.
Further, in step S6, the ultrasonic power of the ultrasonication is 60W, ultrasonic time 15min.
Further, in step S7, the optimal addition volume of the nitrogen-doped carbon quantum dot solution is 0.6mL.
Fig. 1 is nitrogen-doped carbon quantum dot made from the present embodiment method and the co-modified CuBi of silver2O4Nanometer rods photocathode
SEM image.Nitrogen-doped carbon quantum dot and the co-modified CuBi of silver as can be seen from Figure 12O4Nanometer rods photocathode is to be about 2 μm, wide
The nanometer rods of about 300nm.
Fig. 2 is CuBi2O4The TEM image of/Ag/N-CQD composite material.Nanorod surfaces load as can be seen from Figure 2 has nitrogen
The carbon quantum dot of doping.
It can be seen that co-modified product CuBi from X-ray diffraction style shown in Fig. 32O4/ Ag/N-CQD, only modification Ag
Product CuBi2O4/Ag、CuBi2O4X-ray diffraction style it is similar, have slight offset.
It can be seen that from uv drs shown in Fig. 4 and CuBi2O4It compares, co-modified product CuBi2O4/Ag/N-CQD
Only modify the product CuBi of Ag2O4The absorption of visible light is not remarkably reinforced in/Ag.
From fluorescence spectrum interpretation of result shown in fig. 5, with CuBi2O4It compares, only modifies the product CuBi of Ag2O4/ Ag's is glimmering
Luminous intensity weaken, show Ag doped be conducive to charge separation.And co-modified product CuBi2O4The fluorescence intensity of/Ag/N-CQD
It is most weak, show that nitrogen-doped carbon quantum dot can efficiently separate photo-generated carrier.
From impedance spectra interpretation of result shown in fig. 6, with FTO/CuBi2O4Optoelectronic pole and FTO/CuBi2O4/ Ag optoelectronic pole
It compares, co-modified product nitrogen-doped carbon quantum dot made from the present embodiment method and the co-modified CuBi of silver2O4Nanometer rods photocathode
(FTO/CuBi2O4/ Ag/N-CQD) impedance is minimum, shows co-modified to improve charge transfer effciency.
MOtt-SchOttky Dependence Results analysis shown in Fig. 7, with FTO/CuBi2O4Optoelectronic pole is compared, FTO/
CuBi2O4Co-modified product nitrogen-doped carbon quantum dot made from/Ag optoelectronic pole, the present embodiment method and the co-modified CuBi of silver2O4It receives
The corresponding slope of curve of rice stick photocathode all becomes larger, and shows co-modified to be conducive to improve carrier concentration.
Embodiment 2
The present embodiment is to nitrogen-doped carbon quantum dot made from embodiment 1 and the co-modified CuBi of silver2O4Nanometer rods photocathode into
The test of row PhotoelectrocatalytiPerformance Performance, test condition are as described below: using standard three electrode system, saturated calomel electrode and Pt electrodes
Respectively as reference electrode and to electrode.1.5 solar simulator (100mW/cm of AM2) it is used as light source.Take 85mL 0.5ML
For phosphate buffer solution in photovoltaic reaction pond, light source is 10cm at a distance from reaction system, has 0.5cm from front illuminated2
Electrolyte exposed area working electrode.Potential range is -0.6-0.5V, and scanning speed is 10mV ˙ s-1.Electrode potential uses
RHE standard, E(RHE)=E(SCE)+0.059*6.6+0.242。
From photoelectric properties figure interpretation of result shown in Fig. 8, with FTO/CuBi2O4Optoelectronic pole and FTO/CuBi2O4/ Ag photoelectricity
Pole is compared, nitrogen-doped carbon quantum dot made from embodiment 1 and the co-modified CuBi of silver2O4Nanometer rods photocathode shows higher
Photoelectric current, show it is co-modified increase charge transfer effciency and carrier separation efficiency, improve decompose aquatic products hydrogen ability.
From current versus time curve interpretation of result shown in Fig. 9, with FTO/CuBi2O4Optoelectronic pole and FTO/CuBi2O4/ Ag light
Electrode is compared, nitrogen-doped carbon quantum dot made from embodiment 1 and the co-modified CuBi of silver2O4Nanometer rods photocathode is shown well
Stability.
For those skilled in the art, it can be made various corresponding according to above technical solution and design
Change and modification, and all these change and modification should be construed as being included within the scope of protection of the claims of the present invention.
Claims (6)
1. a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method, which comprises the steps of:
Step S1, by 2.42g Bi (NO3)3·5H2O、0.6g Cu(NO3)3·5H2O and 0.87g NaOH is added sequentially to 40mL
In deionized water, stirs dissolution in 3 hours and obtain solution；
Step S2, solution obtained in step S1 is transferred in the autoclave of polytetrafluoroethyllining lining, under the conditions of 180 DEG C
Reaction for 24 hours, is cooled to room temperature to autoclave, the solid product being centrifugated out in solution, with anhydrous second after reaction
Pure and mild high purity water alternately and repeatedly respectively washs dries in the drying box for be placed on afterwards three times 60 DEG C, obtains CuBi2O4Nanometer rods；
Step S3, CuBi obtained in 30mg step S2 is weighed2O4Nanometer rods are added in 10mL dehydrated alcohol, are then added not
The 0.05M AgNO of same volume3Solution stirs 3h to adsorption equilibrium, dries in 60 DEG C of drying box, obtain powdery product；
Step S4, FTO glass is sequentially placed into acetone, dehydrated alcohol, is cleaned by ultrasonic in deionized water and takes out, then use dehydrated alcohol
Cleaning, N2Drying；
Step S5, it disperses the powdery product in 20mg step S3 in 0.1mL dehydrated alcohol and forms suspension, then drop coating
On the FTO glass of the method processing through step S4, dried in 60 DEG C of drying box, then using CVD method in N2Under atmosphere
450 DEG C of annealing 4h obtain the CuBi of Ag doping2O4Nanometer rods；
Step S6, the CuBi for being adulterated Ag made from step S5 as carbon paste band2O4Nanometer rods are removed from FTO glass and are transferred to
On the FTO glass of another piece of method processing through step S4, ultrasonication is carried out in water then to remove excessive Ag/
CuBi2O4Nano-bar material can obtain FTO/CuBi2O4/ Ag photocathode；
Step S7, by FTO/CuBi made from step S62O4/ Ag photocathode is placed in 10mL dehydrated alcohol, and different volumes are added
Nitrogen-doped carbon quantum dot solution, 3h is to adsorption equilibrium for stirring, dries in 60 DEG C of drying boxes, peripheral regions epoxy when drying
Resin covering can obtain nitrogen-doped carbon quantum dot and the co-modified CuBi of silver after drying2O4Nanometer rods photocathode.
2. a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method according to claim 1, which is characterized in that step
In rapid S2, the liner volume of the autoclave of the polytetrafluoroethyllining lining is 50mL.
3. a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method according to claim 1, which is characterized in that step
In rapid S3, the 0.05M AgNO3The addition volume of solution is 0.4mL.
4. a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method according to claim 1, which is characterized in that step
In rapid S5, hanging drop is coated on the FTO glass of the processing of the method through step S4 method particularly includes: pipetted with liquid-transfering gun
0.05mL hanging drop is on the FTO glass of the method processing through step S4.
5. a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method according to claim 1, which is characterized in that step
In rapid S6, the ultrasonic power of the ultrasonication is 60W, ultrasonic time 15min.
6. a kind of co-modified bismuthic acid copper nanometer rods photocathode preparation method according to claim 1, which is characterized in that step
In rapid S7, the addition volume of the nitrogen-doped carbon quantum dot solution is 0.6mL.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110201676A (en) * | 2019-06-21 | 2019-09-06 | 西北工业大学 | A kind of bismuthic acid Copper thin film that inlaying no ligand quantum dot, preparation method and application |
| CN110205638A (en) * | 2019-07-08 | 2019-09-06 | 辽宁大学 | A kind of Z-type CuBi2O4/SnO2Photocathode film and its preparation method and application |
| CN111482150A (en) * | 2020-04-22 | 2020-08-04 | 上海市普陀区人民医院(上海纺织第一医院) | Visible light response all-copper-based series photoelectric catalytic device and preparation method thereof |
| CN113308711A (en) * | 2021-05-26 | 2021-08-27 | 绍兴文理学院 | Preparation method and application of F-doped CBO nanorod array photocathode material |
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| CN110201676A (en) * | 2019-06-21 | 2019-09-06 | 西北工业大学 | A kind of bismuthic acid Copper thin film that inlaying no ligand quantum dot, preparation method and application |
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| CN110205638B (en) * | 2019-07-08 | 2021-01-08 | 辽宁大学 | Z-shaped CuBi2O4/SnO2Photoelectric cathode film and preparation method and application thereof |
| CN111482150A (en) * | 2020-04-22 | 2020-08-04 | 上海市普陀区人民医院(上海纺织第一医院) | Visible light response all-copper-based series photoelectric catalytic device and preparation method thereof |
| CN111482150B (en) * | 2020-04-22 | 2022-07-19 | 上海市普陀区人民医院(上海纺织第一医院) | Visible light response all-copper-based series photoelectric catalytic device and preparation method thereof |
| CN113308711A (en) * | 2021-05-26 | 2021-08-27 | 绍兴文理学院 | Preparation method and application of F-doped CBO nanorod array photocathode material |
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