CN109448999A - Efficient light anode and preparation method thereof based on II type core-shell quanta dots - Google Patents
Efficient light anode and preparation method thereof based on II type core-shell quanta dots Download PDFInfo
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- CN109448999A CN109448999A CN201811286502.XA CN201811286502A CN109448999A CN 109448999 A CN109448999 A CN 109448999A CN 201811286502 A CN201811286502 A CN 201811286502A CN 109448999 A CN109448999 A CN 109448999A
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/204—Light-sensitive devices comprising an oxide semiconductor electrode comprising zinc oxides, e.g. ZnO
-
- 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
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/542—Dye sensitized solar cells
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Luminescent Compositions (AREA)
Abstract
Efficient light anode and preparation method thereof based on II type core-shell quanta dots, belongs to light anode field.Light anode includes conductive substrate, the n-type semiconductor film for being adsorbed in conductive substrate, the sulfydryl alkanoic acid for being connected to n-type semiconductor film and the II type core-shell quanta dots for being connected to sulfydryl alkanoic acid.The conduction level of quantum dot shell is lower than the conduction level of quantum dot stratum nucleare, and the valence-band level of quantum dot shell is lower than the valence-band level of quantum dot stratum nucleare, and the conduction level of n-type semiconductor film is located between the conduction level and valence-band level of quantum dot shell.Extinction is high-efficient, interface charge separative efficiency is high, interface charge compound action is weak, incident photon-to-electron conversion efficiency is high.Preparation method includes impregnating the n-type semiconductor film for being deposited on conductive substrate in the sensitizer solution containing II type core-shell quanta dots after the alcohol solution for soaking containing sulfydryl alkanoic acid.Controllability is good, at low cost, applied widely, and light anode incident photon-to-electron conversion efficiency obtained is high.
Description
Technical field
The present invention relates to light anode fields, in particular to a kind of efficient light anode based on II type core-shell quanta dots
And preparation method thereof.
Background technique
Energy crisis is increasingly serious, and sensitization solar battery becomes new with the serial advantage such as its simple process, low in cost
The research hotspot of energy field.However, the interface of the limited spectral response of light anode and complexity electricity in sensitization solar battery
Lotus transfer and recombination process, make the extinction efficiency of battery and charge collection efficiency be restricted, leverage the photoelectricity of battery
Transformation efficiency.Therefore, the extinction efficiency of effectively enhancing light anode improves the interfacial charge transfer process of light anode with regulation, for
It improves the incident photon-to-electron conversion efficiency of battery and promotes significant for its practicalization.
However, the prior art has the following problems: the electronic structure of quanta point material usually used at present is without special
Design, electron population is irregular, this is resulted in: one side electronics is transferred to the limited speed in n-type semiconductor film from quantum dot,
It is difficult to realize efficient separation of charge and electron injection；On the other hand, state electronics answering from n-type semiconductor film to quantum dot is separated
Conjunction process is unable to get effective control, and the presence of the recombination process seriously affects the charge collection efficiency in light anode.It is above-mentioned normal
Rule quantum dot is transmitted with n-type semiconductor membrane interface charge causes the photoelectric properties of light anode to be limited with the defect of recombination process
System.
In view of this, special propose the application.
Summary of the invention
The purpose of the present invention is to provide a kind of efficient light anodes based on II type core-shell quanta dots, have extinction efficiency
High, the advantages that interface charge separative efficiency is high, interface charge compound action is weak, incident photon-to-electron conversion efficiency is high.
Another object of the present invention is to provide a kind of preparation method of efficient light anode based on II type core-shell quanta dots,
Its controllability is good, at low cost, applied widely, and the incident photon-to-electron conversion efficiency of light anode obtained is high.
The embodiment of the present invention is achieved in that
A kind of efficient light anode based on II type core-shell quanta dots including conductive substrate, is adsorbed in the N-shaped of conductive substrate partly
Electrically conductive film, the sulfydryl alkanoic acid for being connected to n-type semiconductor film and the II type core-shell quanta dots for being connected to sulfydryl alkanoic acid, II type nucleocapsid
Quantum dot includes quantum dot stratum nucleare and quantum dot shell, and the conduction level of quantum dot shell is lower than the conduction band energy of quantum dot stratum nucleare
Grade, the valence-band level of quantum dot shell are lower than the valence-band level of quantum dot stratum nucleare, and the conduction level of n-type semiconductor film is located at quantum
Between the conduction level and valence-band level of point shell.
A kind of preparation method of the above-mentioned efficient light anode based on II type core-shell quanta dots comprising: it is led being deposited on
The n-type semiconductor film of electric substrate obtains surface and is connected with the N-shaped of sulfydryl alkanoic acid and partly lead in the alcohol solution for soaking containing sulfydryl alkanoic acid
Body film；The n-type semiconductor film that surface is connected with sulfydryl alkanoic acid is impregnated in the sensitizer solution containing II type core-shell quanta dots,
Obtain the efficient light anode based on II type core-shell quanta dots.
The beneficial effect of the embodiment of the present invention is:
Efficient light anode provided by the invention based on II type core-shell quanta dots, using the quantum of II type nucleocapsid electronic structure
Point, the conduction band and valence band of shell are respectively lower than the conduction band and valence-band level of stratum nucleare: on the one hand, the electron delocalization of core-shell quanta dots
Into shell, this is transferred to the electronics on core-shell quanta dots swimmingly on n-type semiconductor film by shell, to realize
Efficient separation of charge and electron injection between quantum dot and n-type semiconductor film；On the other hand, the hole confinement of quantum dot is in core
Layer is internal and shell substantially without hole, this, which can be effectively inhibited, separates state electronics on core-shell quanta dots on n-type semiconductor film
The recombination process in hole significantly increases the charge collection efficiency of light anode.Above structure characteristic makes based on II type core-shell quanta dots
Light anode show excellent photoelectric properties.
Sulfydryl alkanoic acid is used as the function bridge chain molecule of connection n-type semiconductor film and II type core-shell quanta dots, molecule one end
Carboxyl it is strong close in n-type semiconductor film surface, and the sulfydryl of the other end is strong closes on II type core-shell quanta dots surface, and N-shaped is partly led
Body film and II type core-shell quanta dots are closely linked by chemical bond, and light anode stability obtained is good, interface electronics is infused
Enter smooth, charge collection efficiency and incident photon-to-electron conversion efficiency is high.
The preparation method of efficient light anode provided by the invention based on II type core-shell quanta dots, successively by dip operation
Connect sulfydryl alkanoic acid and II type core-shell quanta dots on the n-type semiconductor film for be deposited on conductive substrate, controllability is good, cost
It is low, applied widely.Light anode obtained pointedly enhances the electronics transfer from quantum dot to n-type semiconductor film, cuts simultaneously
The weak electronics from n-type semiconductor film to quantum dot is compound, significantly improves the photoelectric properties of light anode.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the structural schematic diagram of the efficient light anode provided in an embodiment of the present invention based on II type core-shell quanta dots；
Fig. 2 is the interface charge process energy of the efficient light anode provided in an embodiment of the present invention based on II type core-shell quanta dots
Grade figure；
Fig. 3 is the TEM figure based on II type CdSe@CdS core shell quantum dot that the embodiment of the present invention 1 provides；
Fig. 4 is the interface for the efficient light anode based on II type CdSe CdS core shell quantum dot that the embodiment of the present invention 1 provides
Charge transmission and recombination kinetcs process spectrogram；
Fig. 5 is the sun for the efficient light anode based on II type CdSe CdS core shell quantum dot that the embodiment of the present invention 1 provides
The J-V curve graph of energy battery.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Have below to the efficient light anode and preparation method thereof based on II type core-shell quanta dots of the embodiment of the present invention
Body explanation.
Referring to Fig. 1, the present invention provides a kind of efficient light anode based on II type core-shell quanta dots, comprising: conductive substrate,
It is adsorbed in the n-type semiconductor film of conductive substrate, be connected to the sulfydryl alkanoic acid of n-type semiconductor film and is connected to the II of sulfydryl alkanoic acid
Type core-shell quanta dots.II type core-shell quanta dots include quantum dot stratum nucleare and quantum dot shell.The conduction level of quantum dot shell is low
In the conduction level of quantum dot stratum nucleare, the valence-band level of quantum dot shell is lower than the valence-band level of quantum dot stratum nucleare.N-type semiconductor
The conduction level of film is located between the conduction level and valence-band level of quantum dot shell.
Referring to Fig. 2, II type core-shell quanta dots, the conduction band and valence band of shell are respectively lower than the conduction band and valence band energy of stratum nucleare
Grade: on the one hand, for the electron delocalization of core-shell quanta dots into shell, this allows the electronics on core-shell quanta dots suitable by shell
It freely is transferred on n-type semiconductor film, to realize efficient separation of charge and electronics note between quantum dot and n-type semiconductor film
Enter；On the other hand, the hole confinement of quantum dot inside stratum nucleare and shell substantially without hole, this can effectively inhibit N-shaped half
The recombination process that state electronics hole on core-shell quanta dots is separated on electrically conductive film, significantly increases the charge collection efficiency of light anode.
Above structure characteristic makes the light anode based on II type core-shell quanta dots show excellent photoelectric properties.
Sulfydryl alkanoic acid is used as the function bridge chain molecule of connection n-type semiconductor film and II type core-shell quanta dots, molecule one end
Carboxyl it is strong close in n-type semiconductor film surface, and the sulfydryl of the other end is strong closes on II type core-shell quanta dots surface, and N-shaped is partly led
Body film and II type core-shell quanta dots are closely linked by chemical bond, and light anode stability obtained is good, interface electronics is infused
Enter smooth, charge collection efficiency and incident photon-to-electron conversion efficiency is high.
In some optional embodiments of the present invention, n-type semiconductor film is selected from TiO2Semiconductor film, ZnO semiconductor film
Or SnO2One of semiconductor film.
The semiconductor film for selecting mentioned kind makes the level structure and quantum dot stratum nucleare and quantum dot shell of n-type semiconductor film
There is preferable matching relationship between the level structure of layer, is conducive to enhance quantum dot to the electronics transfer of n-type semiconductor film, weakens
Electronics from n-type semiconductor film to Quantum Well is compound, so as to improve the photoelectric properties of light anode.
Sulfydryl alkanoic acid is selected from least one of 3- mercaptopropionic acid, 5- mercaptopentanoic acid or 11- mercaptoundecylic acid.Such as sulfydryl alkane
Acid can be a kind of 3- mercaptopropionic acid, 5- mercaptopentanoic acid one kind, 11- mercaptoundecylic acid one kind or 3- mercaptopropionic acid, 5- sulfydryl
Two or three of combination in valeric acid and 11- mercaptoundecylic acid.
The sulfydryl alkanoic acid of mentioned kind is selected, when preparation is easy to operate.Sulfydryl alkanoic acid both ends and n-type semiconductor film and II type
The bonding of core-shell quanta dots is stablized, and the light anode stability made is good, interface electron injection is smooth.
The present invention provides a kind of preparation method of above-mentioned efficient light anode based on II type core-shell quanta dots, comprising: will
The n-type semiconductor film of conductive substrate is deposited in the alcohol solution for soaking containing sulfydryl alkanoic acid, surface is obtained and is connected with sulfydryl alkanoic acid
N-type semiconductor film；The n-type semiconductor film that surface is connected with sulfydryl alkanoic acid is molten in the sensitizer containing II type core-shell quanta dots
It is impregnated in liquid, obtains the efficient light anode based on II type core-shell quanta dots.
Sulfydryl alkanoic acid and II type nucleocapsid are successively connected on the n-type semiconductor film for be deposited on conductive substrate by dip operation
Quantum dot, controllability are good, at low cost, applied widely.Light anode obtained pointedly enhances partly to be led from quantum dot to N-shaped
The electronics transfer of body film, while the electronics weakened from n-type semiconductor film to quantum dot is compound, significantly improves the photo electric of light anode
Energy.
In some optional embodiments of the present invention, the n-type semiconductor film for being deposited on conductive substrate is containing sulfydryl alkane
The time of the alcohol solution for soaking of acid is 5-10h, such as can be in 5h, 6h, 7h, 8h, 9h, 10h any one or it is any
Range between the two.It is bonded sulfydryl alkanoic acid steadily with n-type semiconductor film.
Optionally, the n-type semiconductor film for being deposited on conductive substrate is selected from TiO2Semiconductor film, ZnO semiconductor film or SnO2Half
One of electrically conductive film.
Further, in the alcoholic solution containing sulfydryl alkanoic acid, solvent is optionally methanol, ethyl alcohol etc..Sulfydryl alkanoic acid is selected from
At least one of 3- mercaptopropionic acid, 5- mercaptopentanoic acid or 11- mercaptoundecylic acid, the percent by volume in alcoholic solution is optional
Ground is any one or any range between the two in 3-8%, such as 3%, 4%, 5%, 6%, 7%, 8%.
In some optional embodiments of the present invention, surface is connected with the n-type semiconductor film of sulfydryl alkanoic acid in sensitizer
The time impregnated in solution be 5-20h, such as can be 5h, 6h, 7h, 8h, 9h, 10h, 11h, 12h, 13h, 14h, 15h, 16h,
Any one in 17h, 18h, 19h, 20h etc. or any range between the two.Make II type core-shell quanta dots and sulfydryl alkanoic acid
It is steadily bonded, the light anode stability made is good, interface electron injection is smooth.
Further, the solvent of sensitizer solution is selected from least one of n-hexane, heptane, toluene or chloroform.
As solvent can be, hexane is a kind of, heptane is a kind of, toluene is a kind of, chloroform is a kind of or hexane, heptane, toluene and trichlorine
Two kinds, three kinds or four kinds of combination in methane.
Through inventor the study found that using above-mentioned solvent sensitizer solution so that II type core-shell quanta dots are in the solution
Dispersion performance it is good and be capable of being bonded for fast and stable with sulfydryl alkanoic acid.
In some specific embodiments of the present invention, II type core-shell quanta dots are made according to following methods:
Amount under the heating condition of inert protective gas protection, after quantum dot shell precursor solution to be added to thermal response
Son point stratum nucleare precursor solution.
Inert protective gas refers to inert gas, such as；Inert gas in the narrow sense such as helium, neon, argon gas
Deng, in another example inactive protection gas such as nitrogen of property etc., at least one of or combination both at least.
Above-mentioned preparation method first prepares quantum dot stratum nucleare by the way of hot solvent injection, then extension is raw outside stratum nucleare
Long quantum dot shell.The energy level of stratum nucleare and shell can be regulated and controled respectively by controlling the growth of stratum nucleare and shell quantum dot respectively
Structure, to accurately, effectively regulate and control the interface charge process between quantum dot and n-type semiconductor.Pass through core-shell quanta dots electricity
The control of minor structure pointedly enhances the electronics transfer from quantum dot to n-type semiconductor film, while weakening from n-type semiconductor
The electronics of film to quantum dot is compound, significantly improves the photoelectric properties of light anode.This method controllability is good, the at low cost, scope of application
Extensively, the extinction efficiency of light anode obtained and photoelectric efficiency are high.
Optionally, include: by the quantum dot stratum nucleare precursor solution after quantum dot shell precursor solution addition thermal response
Quantum dot stratum nucleare precursor solution is heated into 0.3-2h under the conditions of 210-250 DEG C, holding fluid temperature is 210-250 DEG C of condition
Under quantum dot shell precursor solution be added dropwise with the speed of 0.2-1mL/s react 0.1-10min again.
In some specific embodiments of the present invention, quantum dot stratum nucleare precursor solution is optionally CdSe core layer forerunner
One of liquid solution, CdS core layer precursor solution and CdTe stratum nucleare precursor solution.Specifically:
When quantum dot stratum nucleare precursor solution be CdSe core layer precursor solution when, be optionally cadmium containing tetradecanoic acid,
The 1- octadecene solution of selenium powder.Preferably, the concentration of selenium powder is 0.6-0.8mmol/L, the concentration of tetradecanoic acid cadmium in the solution
For 12-18mmol/L.
When quantum dot stratum nucleare precursor solution is CdS core layer precursor solution, it is optionally containing cadmium acetate, sulphur simple substance
And the 1- octadecene solution of tri-n-octyl phosphine.Preferably, the concentration of cadmium acetate is 0.1-0.2mol/L, sulphur simple substance in the solution
Concentration be 0.1-0.2mol/L, the concentration of tri-n-octyl phosphine is 10-4-10-3mol/L。
When quantum dot stratum nucleare precursor solution is CdTe stratum nucleare precursor solution, it is optionally containing octadecylphosphonic acid
The 1- octadecene solution of cadmium, tellurium powder.Preferably, the concentration of octadecylphosphonic acid cadmium is 0.03-0.04mol/L, tellurium in the solution
The concentration of powder is 0.03-0.04mol/L.
Quantum dot shell precursor solution be optionally CdS shell precursor solution, CdSe shell precursor solution and
One of CdTe shell precursor solution.Specifically:
When quantum dot shell precursor solution is CdS shell precursor solution, it is optionally containing cadmium oleate, sulphur simple substance
And the 1- octadecene solution of tri-n-octyl phosphine.Preferably, the concentration of cadmium oleate is 0.1-0.2mol/L, sulphur simple substance in the solution
Concentration be 0.1-0.2mol/L, the concentration of tri-n-octyl phosphine is 10-4-10-3mol/L。
When quantum dot shell precursor solution is CdSe shell precursor solution, it is optionally containing cadmium acetate, 18
The 1- octadecene solution of alkylamine, selenium powder and tributylphosphine.Preferably, the concentration of cadmium acetate is 10-20mmol/ in the solution
L, the concentration of octadecylamine are 0.5-2mmol/L, and the concentration of selenium powder is 0.5-1.5mmol/L, and the concentration of tributylphosphine is
0.3-0.8mmol/L。
When quantum dot shell precursor solution is CdTe shell precursor solution, it is optionally containing cadmium acetate, 18
The 1- octadecene solution of alkylamine, tellurium powder and tributylphosphine.Preferably, the concentration of cadmium acetate is 10-20mmol/ in the solution
L, the concentration of octadecylamine are 0.5-2mmol/L, and the concentration of tellurium powder is 0.5-1.5mmol/L, and the concentration of tributylphosphine is
0.3-0.8mmol/L。
The component of quantum dot shell and quantum dot stratum nucleare is preferably different, in some specific embodiments of the present invention,
The core-shell quanta dots being prepared are optionally CdSe@CdS core shell quantum dot, CdSe@CdTe core-shell quanta dots, CdTe@CdSe
One in core-shell quanta dots, CdTe@CdS core shell quantum dot, CdS@CdSe core shell quantum dot and CdS@CdTe core-shell quanta dots etc.
Kind.
In some specific embodiments of the present invention, such as:
When core-shell quanta dots are CdSe@CdS core shell quantum dot, the heating temperature of stratum nucleare precursor solution is preferably
230-240 DEG C, heating time is preferably 1-2h.The holding temperature of quantum dot stratum nucleare solution is preferably 230-240 DEG C.Shell
The rate of addition of precursor solution is preferably 0.2-0.5mL/s, and the time of isothermal reaction is optionally 0.1-10min, into
One step is optionally 0.4-2min.
When core-shell quanta dots are CdTe@CdS core shell quantum dot, the heating temperature of stratum nucleare precursor solution is preferably
230-250 DEG C, heating time is preferably 0.3-0.8h.The holding temperature of quantum dot stratum nucleare solution is preferably 230-250 DEG C.
The rate of addition of shell precursor solution is preferably 0.4-0.8mL/s, and the time of isothermal reaction is preferably 0.1-3min.
When core-shell quanta dots are CdTe@CdSe core shell quantum dot, the heating temperature of stratum nucleare precursor solution is preferably
230-250 DEG C, heating time is preferably 1.2-2h.The holding temperature of quantum dot stratum nucleare solution is preferably 230-250 DEG C.Shell
The rate of addition of layer precursor solution is preferably 0.2-0.7mL/s, and the time of isothermal reaction is preferably 2-8min.
When core-shell quanta dots are CdSe@CdTe core-shell quanta dots, the heating temperature of stratum nucleare precursor solution is preferably
230-250 DEG C, heating time is preferably 0.5-1.5h.The holding temperature of quantum dot stratum nucleare solution is preferably 230-250 DEG C.
The rate of addition of shell precursor solution is preferably 0.2-1mL/s, and the time of isothermal reaction is preferably 0.1-0.3min.
When core-shell quanta dots are CdS@CdSe core shell quantum dot, the heating temperature of stratum nucleare precursor solution is preferably
210-240 DEG C, heating time is preferably 0.5-1h.The holding temperature of quantum dot stratum nucleare solution is preferably 210-240 DEG C.Shell
The rate of addition of layer precursor solution is preferably 0.2-0.6mL/s, and the time of isothermal reaction is preferably 2-10min.
When core-shell quanta dots are CdS@CdTe core-shell quanta dots, the heating temperature of stratum nucleare precursor solution is preferably
210-240 DEG C, heating time is preferably 0.5-1h.The holding temperature of quantum dot stratum nucleare solution is preferably 210-240 DEG C.Shell
The rate of addition of layer precursor solution is preferably 0.2-1mL/s, and the time of isothermal reaction is preferably 0.1-0.6min.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
A kind of preparation method of the efficient light anode based on II type CdSe CdS core shell quantum dot, comprising:
6.3mL is contained the core of the 1- octadecene solution of 0.79mmol/L selenium powder and 15.8mmol/L tetradecanoic acid cadmium by S1
Layer precursor solution vacuumizes 30min, and 1mL is then then contained 0.05mol/L in 240 DEG C of heating 1h under protection of argon gas
The 18 weak solution fast speed of 1- of oleic acid instills, and obtains the solution containing CdSe quantum dot stratum nucleare.
S2, maintaining quantum dot stratum nucleare solution temperature is 230 DEG C, is instilled with the rate of addition of 0.3mL/s to it and contains 0.1mol/
L cadmium oleate, 0.1mol/L sulphur and 9 × 10-4The 1- 18 of mol/L tri octyl phosphine dilute quantum dot shell precursor solution, constant temperature
It is reacted after reacting 5min with ice bath termination.It uses ethyl alcohol as precipitating reagent, is centrifuged to obtain II type CdSe@CdS core shell quantum dot.
S3, disperse II type CdSe@CdS core shell quantum dot in heptane be made into concentration be 5 × 10-4The sensitizer of mol/L
Solution.It disperses 3- mercaptopropionic acid in and is made into the alcoholic solution that percent by volume is 5% in ethyl alcohol.
S4, the TiO that conductive substrate will be deposited on2Semiconductor film obtains surface and is connected with sulfydryl alkane in alcohol solution for soaking 8h
The n-type semiconductor film of acid.The n-type semiconductor film that surface is connected with sulfydryl alkanoic acid is impregnated into 10h in sensitizer solution, must be based on
The efficient light anode of II type CdSe CdS core shell quantum dot.
Embodiment 2
A kind of preparation method of the efficient light anode based on II type CdTe CdS core shell quantum dot, the difference with embodiment 1
Place is:
In S1, quantum dot stratum nucleare precursor solution is the cadmium of octadecylphosphonic acid containing 0.035mol/L, 0.03mol/L tellurium powder
1- octadecene solution.Heating temperature is to 240 DEG C, heating time 0.5h.
In S2, quantum dot shell precursor solution drop rate into stratum nucleare solution is 0.8mL/s, and quantum dot shell is added
The isothermal reaction time is 1min after precursor solution.
It in S3, disperses core-shell quanta dots in toluene, sensitizer solution is containing 1 × 10-4The CdTe@CdS core shell of mol/L
The toluene solution of quantum dot；Sulfydryl alkanoic acid is 5- mercaptopentanoic acid；The percent by volume of sulfydryl alkanoic acid is 6% in ethanol solution.
In S4, it is 20h that surface, which is connected with soaking time of the n-type semiconductor film of sulfydryl alkanoic acid in sensitizer solution,.
Embodiment 3
A kind of preparation method of the efficient light anode based on II type CdTe CdSe core shell quantum dot, the difference with embodiment 1
Place is:
In S1, quantum dot stratum nucleare precursor solution is the cadmium of octadecylphosphonic acid containing 0.04mol/L, 0.04mol/L tellurium powder
1- octadecene solution.Heating temperature is to 240 DEG C, heating time 1.2h.
In S2, the temperature of quantum dot stratum nucleare solution maintains 240 DEG C.Quantum dot shell precursor solution is containing 15mmol/L
The 1- octadecene solution of cadmium acetate, 1mmol/L octadecylamine, 0.8mmol/L selenium powder and 0.5mmol/L tributylphosphine.Quantum
Point shell precursor solution drop rate into stratum nucleare solution is 0.2mL/s, and constant temperature after quantum dot shell precursor solution is added
Reaction time is 8min.
In S3, sensitizer solution is containing 3 × 10-4The chloroform soln of the CdTe@CdSe core shell quantum dot of mol/L.Mercapto
Base alkanoic acid is 11- mercaptoundecylic acid；The percent by volume of sulfydryl alkanoic acid is 8% in ethanol solution.
In S4, it is 16h that surface, which is connected with soaking time of the n-type semiconductor film of sulfydryl alkanoic acid in sensitizer solution,.
Embodiment 4
A kind of preparation method of the efficient light anode based on II type CdSe CdTe core-shell quanta dots, the difference with embodiment 1
Place is:
In S1, the heating time of stratum nucleare precursor solution is 0.6h.
In S2, the temperature of quantum dot stratum nucleare solution maintains 250 DEG C.Quantum dot shell precursor solution is containing 15mmol/L
The 1- octadecene solution of cadmium acetate, 1mmol/L octadecylamine, 0.8mmol/L tellurium powder and 0.5mmol/L tributylphosphine.Quantum
Point shell precursor solution drop rate into stratum nucleare solution is 1mL/s, and constant temperature is anti-after quantum dot shell precursor solution is added
It is 0.1min between seasonable.
In S3, sensitizer solution is containing 8 × 10-4The toluene solution of the CdSe@CdTe core-shell quanta dots of mol/L.Sulfydryl alkane
Acid is 5- mercaptopentanoic acid；The percent by volume of sulfydryl alkanoic acid is 4% in ethanol solution.
In S4, it is 9h that surface, which is connected with soaking time of the n-type semiconductor film of sulfydryl alkanoic acid in sensitizer solution,.
Embodiment 5
A kind of preparation method of the efficient light anode based on II type CdS CdSe core shell quantum dot, the difference with embodiment 1
Place is:
In S1, quantum dot stratum nucleare precursor solution is cadmium acetate containing 0.1mol/L, 0.15mol/L sulphur simple substance, 5 × 10- 4The 1- octadecene solution of mol/L tri-n-octyl phosphine.Heating temperature is to 210 DEG C, heating time 0.7h.
In S2, the temperature of quantum dot stratum nucleare solution maintains 240 DEG C.Quantum dot shell precursor solution is containing 15mmol/L
The 1- octadecene solution of cadmium acetate, 1mmol/L octadecylamine, 0.8mmol/L selenium powder and 0.5mmol/L tributylphosphine.Quantum
Point shell precursor solution drop rate into stratum nucleare solution is 0.5mL/s, and constant temperature after quantum dot shell precursor solution is added
Reaction time is 10min.
In S3, sensitizer solution is containing 6 × 10-4The hexane solution of the CdS@CdSe core shell quantum dot of mol/L.Ethyl alcohol is molten
The percent by volume of sulfydryl alkanoic acid is 5% in liquid.
In S4, it is 16h that surface, which is connected with soaking time of the n-type semiconductor film of sulfydryl alkanoic acid in sensitizer solution,.
Embodiment 6
A kind of preparation method of the efficient light anode based on II type CdS CdTe core-shell quanta dots, the difference with embodiment 1
Place is:
In S1, quantum dot stratum nucleare precursor solution is cadmium acetate containing 0.1mol/L, 0.15mol/L sulphur simple substance, 5 × 10- 4The 1- octadecene solution of mol/L tri-n-octyl phosphine.Heating temperature is to 210 DEG C, heating time 0.7h.
In S2, the temperature of quantum dot stratum nucleare solution maintains 230 DEG C.Quantum dot shell precursor solution is containing 15mmol/L
The 1- octadecene solution of cadmium acetate, 1mmol/L octadecylamine, 0.8mmol/L tellurium powder and 0.5mmol/L tributylphosphine.Quantum
Point shell precursor solution drop rate into stratum nucleare solution is 1mL/s, and constant temperature is anti-after quantum dot shell precursor solution is added
It is 0.1min between seasonable.
In S3, sensitizer solution is containing 1 × 10-3The chloroform soln of the CdS@CdTe core-shell quanta dots of mol/L.Sulfydryl
Alkanoic acid is 11- mercaptoundecylic acid；The percent by volume of sulfydryl alkanoic acid is 7% in ethanol solution.
In S4, it is 6h that surface, which is connected with soaking time of the n-type semiconductor film of sulfydryl alkanoic acid in sensitizer solution,.
Test example
To the interface charge transmission of the efficient light anode based on II type core-shell quanta dots made from embodiment 1-6 and compound speed
The incident photon-to-electron conversion efficiency of rate, interface charge separative efficiency and battery is tested, and the results are shown in Table 1.
1 performance test table of table
As shown in Table 1, the light anode provided in an embodiment of the present invention based on II type core-shell quanta dots, interface electron-transport
Rate is in zero point several to several nanoseconds, and interface electronics recombination rate is tens to several hundred a nanoseconds, ultrafast electron-transport and
Slower electronics recombination process results in interface charge separative efficiency (nearly 100%) of its superelevation.Meanwhile the interface charge of superelevation
Separative efficiency and weaker interface charge compound action make battery show higher incident photon-to-electron conversion efficiency.
Fig. 3 is the TEM figure based on II type CdSe/CdS core-shell quanta dots that the embodiment of the present invention 1 provides.It can according to Fig. 3
Know, the quantum dot of synthesis has core-shell structure, and CdSe core layer is wrapped in by CdS shell；According to size distribution statistics, CdSe/CdS
The size of core-shell quanta dots is about 4.2nm or so.
Fig. 4 is the interface for the efficient light anode based on II type CdSe CdS core shell quantum dot that the embodiment of the present invention 1 provides
Charge transmission and recombination kinetcs process spectrogram.As can be seen from FIG. 4, on the one hand, II type CdSe@CdS quantum dot and TiO2Half
Interface electron transfer rate between electrically conductive film shows fastly of about 0.315ns from CdSe@CdS quantum dot to TiO2Semiconductor film
Interface electronic transmission process it is very smooth.II type electronic structure designs the interface electronics so that from quantum dot to semiconductor film
Transmission rate and separation of charge efficiency are apparently higher than conventional quantum dot.
Fig. 5 is the sun for the efficient light anode based on II type CdSe CdS core shell quantum dot that the embodiment of the present invention 1 provides
The J-V curve graph of energy battery.As can be seen from FIG. 5, the open-circuit voltage of solar battery is 0.647V, short circuit current 13.6mA/
cm2, fill factor 67%, battery efficiency is up to 5.9%, and incident photon-to-electron conversion efficiency is apparently higher than under similarity condition based on conventional
The solar battery of quantum dot light anode.
To sum up, the efficient light anode provided in an embodiment of the present invention based on II type core-shell quanta dots, have extinction it is high-efficient,
The advantages that interface charge separative efficiency is high, interface charge compound action is weak, incident photon-to-electron conversion efficiency is high.Based on II type core-shell quanta dots
Efficient light anode preparation method, controllability is good, at low cost, applied widely, the photoelectric conversion of light anode obtained effect
Rate is high.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention
Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of efficient light anode based on II type core-shell quanta dots, which is characterized in that including conductive substrate, be adsorbed in described lead
The n-type semiconductor film of electric substrate, the sulfydryl alkanoic acid for being connected to the n-type semiconductor film and it is connected to the II of the sulfydryl alkanoic acid
Type core-shell quanta dots, the II type core-shell quanta dots include quantum dot stratum nucleare and quantum dot shell, and the quantum dot shell is led
It is lower than the conduction level of the quantum dot stratum nucleare with energy level, the valence-band level of the quantum dot shell is lower than the quantum dot stratum nucleare
Valence-band level, the conduction level of the n-type semiconductor film be located at the quantum dot shell conduction level and valence-band level it
Between.
2. efficient light anode according to claim 1, which is characterized in that the n-type semiconductor film is selected from TiO2Semiconductor
Film, ZnO semiconductor film or SnO2One of semiconductor film.
3. efficient light anode according to claim 1, which is characterized in that the sulfydryl alkanoic acid is selected from 3- mercaptopropionic acid, 5-
At least one of mercaptopentanoic acid or 11- mercaptoundecylic acid.
4. the preparation method of efficient light anode described in claim 1 characterized by comprising the conductive base will be deposited on
The n-type semiconductor film of piece obtains surface and is connected with the N-shaped of sulfydryl alkanoic acid and partly lead in the alcohol solution for soaking containing sulfydryl alkanoic acid
Body film；The n-type semiconductor film that the surface is connected with sulfydryl alkanoic acid is molten in the sensitizer containing the II type core-shell quanta dots
It is impregnated in liquid, obtains the efficient light anode based on II type core-shell quanta dots.
5. the preparation method according to claim 4, which is characterized in that the n-type semiconductor film is selected from TiO2Semiconductor film,
ZnO semiconductor film or SnO2One of semiconductor film；
And/or in the alcoholic solution, the percent by volume of the sulfydryl alkanoic acid is 3-8%；
And/or the sulfydryl alkanoic acid is selected from least one of 3- mercaptopropionic acid, 5- mercaptopentanoic acid or 11- mercaptoundecylic acid.
6. the preparation method according to claim 4, which is characterized in that the solvent of the sensitizer solution be selected from n-hexane,
At least one of heptane, toluene or chloroform；
And/or in the sensitizer solution, the concentration of the II type core-shell quanta dots is 10-4-10-3mol/L。
7. according to the described in any item preparation methods of claim 4-6, which is characterized in that the II type core-shell quanta dots according to
Lower section method is made:
Quantum dot under the heating condition of inert protective gas protection, after quantum dot shell precursor solution to be added to thermal response
Stratum nucleare precursor solution.
8. preparation method according to claim 7, which is characterized in that heat is added in the quantum dot shell precursor solution
The quantum dot stratum nucleare precursor solution after reaction includes: by the quantum dot stratum nucleare precursor solution in 210-250 DEG C of item
It heats 0.3-2h under part, the quantum dot shell is added dropwise with the speed of 0.2-1mL/s under the conditions of to keep fluid temperature be 210-250 DEG C
Layer precursor solution reacts 0.1-10min again.
9. preparation method according to claim 7, which is characterized in that the quantum dot stratum nucleare precursor solution is CdSe core
Layer precursor solution；It preferably, is cadmium containing tetradecanoic acid, the 1- octadecene solution of selenium powder；
And/or the quantum dot stratum nucleare precursor solution is CdS core layer precursor solution；Preferably, for containing cadmium acetate, sulphur list
The 1- octadecene solution of matter and tri-n-octyl phosphine；
And/or the quantum dot stratum nucleare precursor solution is CdTe stratum nucleare precursor solution；It preferably, is phosphine containing octadecyl
The 1- octadecene solution of sour cadmium, tellurium powder.
10. preparation method according to claim 7, which is characterized in that the quantum dot shell precursor solution is CdS shell
Layer precursor solution；It preferably, is the 1- octadecene solution containing cadmium oleate, sulphur simple substance and tri-n-octyl phosphine；
And/or the quantum dot shell precursor solution is CdSe shell precursor solution；Preferably, for containing cadmium acetate, 18
The 1- octadecene solution of alkylamine, selenium powder and tributylphosphine；
And/or the quantum dot shell precursor solution is CdTe shell precursor solution；Preferably, for containing cadmium acetate, 18
The 1- octadecene solution of alkylamine, tellurium powder and tributylphosphine.
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