CN108493341A - The preparation of perovskite solar cell using tantalum pentoxide as electron transfer layer - Google Patents
The preparation of perovskite solar cell using tantalum pentoxide as electron transfer layer Download PDFInfo
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- CN108493341A CN108493341A CN201810279046.XA CN201810279046A CN108493341A CN 108493341 A CN108493341 A CN 108493341A CN 201810279046 A CN201810279046 A CN 201810279046A CN 108493341 A CN108493341 A CN 108493341A
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- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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- H—ELECTRICITY
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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The preparation method for the perovskite solar cell that the present invention relates to a kind of using tantalum pentoxide as electron transfer layer：Tantalic chloride is dissolved in alcohol, the precursor solution of a concentration of 0.01mol/L 0.06mol/L is prepared；Precursor solution is coated in electrically conducting transparent substrate, is then annealed at 500 600 DEG C, to form the five oxidation two tantalum film that a layer thickness is 5nm 60nm on the surface of conductive substrates；Perovskite precursor solution is coated in the surface of five oxidation two tantalum film, is then annealed at 100 110 DEG C, to form the perovskite light-absorption layer that thickness is 400nm 500nm on the surface of five oxidation two tantalum film；Hole transmission layer and metal electrode are modified successively on the surface of perovskite light-absorption layer, obtain perovskite solar cell.The method and process of the present invention is simple, at low cost, using five oxidation two tantalum film as electron transfer layer, can accelerate the transfer ability of electronics and improve the utilization rate of light.
Description
Technical field
The present invention relates to solar cell preparing technical fields, more particularly to one kind is using tantalum pentoxide as electron-transport
The preparation of the perovskite solar cell of layer.
Background technology
With the rapid development of human society, demand of the mankind to the energy continues to increase, environmental pollution getting worse.Mesh
Before, increasingly severe energy crisis forces people to find new regenerative resource.In many new energy, solar energy is to be distributed
Extensively, the advantages of large storage capacity, clean and safe, receives significant attention.Solar cell can directly convert solar energy into electric energy, thus
There is very vast potential for future development.The high conversion efficiency of the highest silica-based solar cell of existing market share, technology maturation,
But its cost high disadvantage high with production energy consumption constrains its and widely develops.
A kind of solar cell based on organic inorganic hybridization perovskite material occurred in recent years causes people greatly to be closed
Note.Reported that so far, the transfer efficiency of perovskite solar cell energy is increased to rapidly from 3.8% for the first time from 2009
22.1%, and its simple process and low cost, it is presented in the vast potential for future development in area of solar cell.
Organic inorganic hybridization perovskite material crystal structure is perovskite crystal form, basic chemical structure ABX3(A is first
Amine groups (CH3NH3) etc. organic radicals, the inorganic metals such as B Pb, Cd, the halogens such as X I, Cl, Br).The perovskite sun
Battery is mainly by electro-conductive glass (FTO, ITO), electron transfer layer, perovskite light-absorption layer, hole transmission layer and to electrode (Au, Ag)
It constitutes.But the transfer efficiency of current perovskite solar cell energy and it still needs further improvement to the utilization rate of light.
Invention content
In order to solve the above technical problems, the object of the present invention is to provide a kind of using tantalum pentoxide as electron transfer layer
The preparation of perovskite solar cell, method and process of the invention is simple, at low cost, using five oxidation two tantalum film as electronics
Transport layer can accelerate the transfer ability of electronics and improve the utilization rate of light.
The preparation side for the perovskite solar cell that the present invention provides a kind of using tantalum pentoxide as electron transfer layer
Method includes the following steps：
(1) tantalic chloride is dissolved in alcohol, prepares the precursor solution of a concentration of 0.01mol/L-0.06mol/L；
(2) precursor solution is coated in electrically conducting transparent substrate, then anneal at 500-600 DEG C 1-5h, to lead
The surface of electric substrate forms the five oxidation two tantalum film that a layer thickness is 5nm-60nm；
(3) perovskite precursor solution is coated in the surface of five oxidation two tantalum film, is then annealed at 100-110 DEG C
30min-60min, to form thickness on the surface of five oxidation two tantalum film as the perovskite light-absorption layer of 400nm-500nm；
(4) hole transmission layer and metal electrode are modified successively on the surface of perovskite light-absorption layer, obtain perovskite solar energy
Battery.
Further, in step (1), alcohol is one or more of ethyl alcohol, isopropanol, normal propyl alcohol and n-butanol.
Further, in step (2), the material of electrically conducting transparent substrate is fluorine-doped tin oxide glass (FTO) or indium tin
Oxide conducting glass (ITO).
Further, it in step (2) and step (3), is coated using spin-coating method, spin speed 1000-3000
Rev/min.
Further, further include thin with tantalum pentoxide with ultraviolet light again after cooling down after annealing in step (2)
The step of conductive substrates of film (ultraviolet cleaning).Ultraviolet cleaning can improve the hydrophily of five oxidation two tantalum film, under being convenient for
The coating of one step perovskite precursor solution.
Further, in step (2), 500- is warming up to from room temperature (20-30 DEG C) according to the speed of 10-20 DEG C/min
600℃。
Further, in step (3), the mass concentration of perovskite precursor solution is 40-45%wt.
Further, in step (3), the preparation method of perovskite precursor solution includes the following steps：
By lead halide and iodine methylamine (CH3NH3I it) is dissolved in organic solvent, obtains perovskite precursor solution.
Further, lead halide is lead chloride (PbCl2).The molar ratio of lead halide and iodine methylamine is 1:3.
Further, lead halide is lead iodide (PbI2) and lead chloride (PbCl2)。PbI2、PbCl2With mole of iodine methylamine
Than being 1:1:3.
Further, organic solvent is dimethylformamide (DMF).Further, in step (4), hole transmission layer
Thickness be 200-300nm, the material of hole transmission layer is Spiro-OMeTAD or P3HT.
Further, in step (4), hole transmission layer is prepared using spin-coating method, spin speed be 1500-2500 turn/
Point.
Further, in step (4), the thickness of metal electrode is 50-200nm, and metal electrode is silver electrode or gold electricity
Pole.
Further, in step (4), using vapour deposition method in hole transport layer surface evaporation metal electrode, evaporation source is
Metal, evaporation rate 0.1-0.3nm/s, evaporation air pressure are 1 × 10-5Pa。
The present invention also provides a kind of perovskite solar cells using prepared by above-mentioned preparation method, including set successively
Electrically conducting transparent substrate, electron transfer layer (thickness 5-60nm), perovskite light-absorption layer (thickness 400-500nm), the hole transport set
Layer (thickness 200-300nm) and metal electrode (thickness 50-200nm), the material of electron transfer layer are five oxidation two tantalum film, five
The thickness for aoxidizing two tantalum films is 5nm-60nm.
Using five oxidation two tantalum film as electron transfer layer, the advantage ultra-thin using its, translucency is high is improving device
Light utilization efficiency and while electron transport ability, accelerate the separation of carrier, reduce the compound of charge, to improve
The performance of perovskite battery.For the plane perovskite electricity constituted with present invention five oxidation two tantalum film prepared by spin-coating method
Pond, peak efficiency can break through 10%.
According to the above aspect of the present invention, the present invention has at least the following advantages：
(1) five oxidation two tantalum film of the invention is prepared by the sintering that simply coats and anneal, method, technique letter
Single, at low cost, which can be also used for quantum dot cell, perovskite battery, the photoelectric fields such as photodetector.
(2) the five oxidation two tantalum film translucency prepared in the present invention is high, and thickness is thin, can both improve electron mobility,
The light utilization efficiency that device can also be improved, to improve the performance of perovskite battery.
(3) perovskite solar cell of the invention moves five oxidation two tantalum film as electron transfer layer, to the height of light
Permeability improves utilization of the battery to incident light；Using perovskite material as light absorbent (perovskite light-absorption layer), may be implemented
In total visible light range extinction.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, below with presently preferred embodiments of the present invention and after coordinating attached drawing to be described in detail such as.
Description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of the five oxidation two tantalum film prepared by the embodiment of the present invention 3；
Fig. 2 is the transmission plot of the five oxidation two tantalum film prepared by 1-3 of the embodiment of the present invention；
Fig. 3 is the photoluminescence spectra of the tantalum pentoxide comprising perovskite material prepared by 1-3 of the embodiment of the present invention
Figure；
Fig. 4 is perovskite solar cell of the tantalum pentoxide as electron transfer layer prepared by the embodiment of the present invention 4
C-V characteristic (J-V) curve graph.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
Embodiment 1
(1) tantalic chloride for weighing 17.90mg is dissolved in 5ml n-butanols, and heating stirring makes it completely dissolved, and is configured to
The precursor solution of 0.01M.It takes the precursor solution of 50 μ L to drop in clean FTO conductive glass surfaces with liquid-transfering gun, then leads to
The mode for crossing spin coating obtains uniformly penetrating film, and spin coating rotating speed is 1000 revs/min.
(2) the membrane electro-conductive glass prepared is put in annealing furnace, with the speed of 10 DEG C/min from room temperature liter
Temperature removes impurity to 500 DEG C of annealing 2h, and crystallization forms tantalum pentoxide (Ta2O5) film, thickness is about 30nm.Stove to be annealed
Cooled to room temperature, takes out the substrate with five oxidation two tantalum film, and ultraviolet cleaning 20min improves its hydrophily.
(3) 3 are pressed:1 molar ratio weighs iodine methylamine (CH respectively3NH3) and lead chloride (PbCl I2), it is dissolved in dimethyl formyl
In amine (DMF), uniform stirring 12h at a temperature of 60 DEG C configures the perovskite precursor solution of 40%wt clear homogeneous.Take 30
μ L perovskite precursor solutions are dripped on five oxidation two tantalum film, with 3000 revs/min of rate spin coating 40s, are then moved back for 100 DEG C
Fiery 40min, obtains the perovskite thin film of highly crystalline brownish red, and thickness is about 400nm.It is cooled to after room temperature with 2000
Rev/min rate spin coating on 30 μ L Spiro-OMeTAD solution, formed hole transmission layer, thickness 250nm.Then will
Substrate is placed in thermal evaporation instrument, and with the silver electrode of the upper 100nm thickness of evaporation rate vapor deposition of 0.1nm/s, evaporation source is silver, evaporation
Air pressure is 1 × 10-5Pa。
According to above-mentioned steps, perovskite solar cell is made, includes successively from bottom to top：Electrically conducting transparent substrate, electronics
The material of transport layer, perovskite light-absorption layer hole transmission layer and metal electrode, electron transfer layer is five oxidation two tantalum film, calcium titanium
Mine light-absorption layer material is CH3NH3PbI3-xClxFilm (0 ＜ x ＜ 0.5), hole transmission layer material are Spiro-OMeTAD.
Embodiment 2
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：Weigh the pentachloro- of 35.82mg
Change the precursor solution that tantalum is configured to 0.02M.
Embodiment 3
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：Weigh the pentachloro- of 71.64mg
Change the precursor solution that tantalum is configured to 0.04M.
SEM tests are carried out to the five oxidation two tantalum film prepared by embodiment 3, the results are shown in Figure 1, and Fig. 1 shows five oxygen
Change two tantalum films and completely cover FTO conductive glass surfaces, film surface is without hole, and thickness is uniform, and film maintains substantially
The surface topography of FTO electro-conductive glass does not cause larger pattern to change.
Light is carried out to the five oxidation two tantalum film prepared by above 3 embodiments using ultraviolet-visible-Infrared Spectroscopy
Transmission capacity tests (Fig. 2).For five oxidation two tantalum film prepared by the precursor solution of 0.02M, the transmissivity of light is very high, with
Pure electro-conductive glass FTO compares almost without light loss.In addition, using photic within the scope of fluorescence spectrometer scanning 700-850nm
Luminescent spectrum, test is in identical perovskite crystal preparation condition subtegulum for electron transfer capabilities, and the results are shown in Figure 3.It adopts
With the sample of five oxidation two tantalum film substrate prepared by the precursor solution of 0.02M, spectrum peak is minimum, illustrates the perovskite too
Positive energy battery has the separation and transmission of faster electronics in the interface of perovskite light-absorption layer and five oxidation two tantalum film.
Embodiment 4
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：Weigh the pentachloro- of 107.46mg
Change the precursor solution that tantalum is configured to 0.06M.
Volt-ampere curve test is made to perovskite solar cell manufactured in the present embodiment, as shown in figure 4, in 100mW/cm2
Simulated solar irradiation irradiation under, using tantalum pentoxide be used as the perovskite battery of the peak efficiency of electron transfer layer, open circuit light
Voltage is 0.95V, and short-circuit current density reaches 17.9mA/cm2, fill factor 59.6, photoelectric conversion efficiency 10.1%.
Embodiment 5
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：In step (1), spin coating rotating speed
It it is 3000 revs/min, annealing temperature is 550 DEG C in step (2), and prepared five oxidation two tantalum film, thickness is about 5nm.
Embodiment 6
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：In step (1), spin coating rotating speed
It it is 2000 revs/min, annealing temperature is 600 DEG C in step (2), and prepared five oxidation two tantalum film, thickness is about 20nm.
Embodiment 7
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：In step (1), spin coating rotating speed
It it is 3000 revs/min, annealing temperature is 600 DEG C in step (2), and prepared five oxidation two tantalum film, thickness is about 10nm.
Embodiment 8
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：Perovskite precursor solution
Configuration method is as follows：
(1) 1 is pressed:1:3 molar ratio weighs lead iodide (PbI respectively2), lead chloride (PbCl2) and iodine methylamine (CH3NH3I)；
(2) above-mentioned load weighted drug is dissolved in the dimethylformamide (DMF) of 1ml by the mass fraction of 45wt%；
(3) above-mentioned suspension is placed on mixing platform, uniform stirring 12h at a temperature of 70 DEG C, clear homogeneous is made
Perovskite precursor solution, final gained perovskite light-absorption layer material is CH3NH3PbI3-xClxFilm (0 ＜ x ＜ 0.5).
Embodiment 9
Perovskite solar cell is prepared according to the method for embodiment 1, the difference is that：In step (3), gold evaporation
Electrode, thickness 100nm.
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of perovskite solar cell using tantalum pentoxide as electron transfer layer, which is characterized in that
Include the following steps：
(1) tantalic chloride is dissolved in alcohol, prepares the precursor solution of a concentration of 0.01-0.06mol/L；
(2) precursor solution is coated in conductive substrates, is then annealed at 500-600 DEG C, in conductive substrates
Surface forms the five oxidation two tantalum film that a layer thickness is 5-60nm；
(3) perovskite precursor solution is coated in the surface of the five oxidation two tantalum film, is then moved back at 100-110 DEG C
Fire, to form thickness on the surface of five oxidation two tantalum film as the perovskite light-absorption layer of 400-500nm；
(4) hole transmission layer and metal electrode are modified successively on the surface of the perovskite light-absorption layer, obtain the perovskite too
Positive energy battery.
2. preparation method according to claim 1, it is characterised in that：In step (1), the alcohol be ethyl alcohol, isopropanol,
One or more of normal propyl alcohol and n-butanol.
3. preparation method according to claim 1, it is characterised in that：In step (2), the material of the conductive substrates is
Fluorine-doped tin oxide glass or indium tin oxide electro-conductive glass.
4. preparation method according to claim 1, it is characterised in that：In step (2) and step (3), using spin-coating method
It is coated, spin speed is 1000-3000 revs/min.
5. preparation method according to claim 1, it is characterised in that：In step (2), further include after annealing it is cooling after again
The step of conductive substrates of five oxidation two tantalum film being carried with ultraviolet light.
6. preparation method according to claim 1, it is characterised in that：In step (3), the matter of perovskite precursor solution
Measure a concentration of 40-45%wt.
7. preparation method according to claim 1, which is characterized in that in step (3), the perovskite precursor solution
Preparation method include the following steps：
Lead halide and iodine methylamine are dissolved in organic solvent, the perovskite precursor solution is obtained.
8. preparation method according to claim 1, it is characterised in that：In step (4), the thickness of the hole transmission layer
Material for 200-300nm, the hole transmission layer is Spiro-OMeTAD or P3HT.
9. preparation method according to claim 1, it is characterised in that：In step (4), the thickness of the metal electrode is
50-200nm, the metal electrode are silver electrode or gold electrode.
10. the perovskite solar cell prepared by preparation method described in a kind of any one of claim 1-9, feature exist
In：Including conductive substrates, electron transfer layer, perovskite light-absorption layer, hole transmission layer and the metal electrode set gradually, the electricity
The material of sub- transport layer is five oxidation two tantalum film, and the thickness of the five oxidation two tantalum film is 5nm-60nm.
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