CN109037457A - The preparation method and applications of sull as electron transfer layer - Google Patents
The preparation method and applications of sull as electron transfer layer Download PDFInfo
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- CN109037457A CN109037457A CN201810660498.2A CN201810660498A CN109037457A CN 109037457 A CN109037457 A CN 109037457A CN 201810660498 A CN201810660498 A CN 201810660498A CN 109037457 A CN109037457 A CN 109037457A
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/30—Coordination compounds
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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
- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
- H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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- 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
- Y02E10/549—Organic PV cells
Abstract
The present invention discloses a kind of preparation method and applications of sull as electron transfer layer, and the preparation method of the sull includes the following steps: 1) to configure oxide precursor liquid solution, stirs evenly stand-by；2) oxide precursor liquid solution is added dropwise in substrate surface and starts spin coating, substrate is transferred in the sealing container containing inducing solvent ultrapure water after spin coating；3) sealing container heated, make its internal formation thermal and hydric environment, substrate surface occurs hydro-thermal reaction, forms sull.The present invention by adding inducing solvent in a sealed container, under high temperature and pressure, inducing solvent is atomization in sealing container, promote the oxide precursor liquid solution of substrate surface that hydro-thermal reaction occurs, so as to prepare under the conditions of lower temperature, crystal form is controllable and the lesser sull of roughness, when being used in solar cell device as electron transfer layer, the photovoltaic performance of device can be effectively improved.
Description
Technical field
The present invention relates to solar cell devices, in particular to the preparation side of the sull as electron transfer layer
Method, perovskite solar battery comprising the sull electron transfer layer and preparation method thereof, belong to perovskite semiconductor
Battery device field.
Background technique
The burning of the energy, this not only results in energy shortages, also creates serious greenhouse effects, acid rain, global pollution
Etc. serious environmental problems.Due to the fast development of modern industrialization, it is contemplated that the year two thousand fifty, the energy total amount of whole world consumption is than existing
About 1,500,000,000 watts of increase of energy-output ratio of today, the progress and development of future society deeply depend on cleaning, cheap and abundant
The acquisition of the energy.
The perovskite solar battery development very fast due to its photoelectric conversion efficiency, it is considered to be photovoltaic art is most in recent years
One of promising invention.PSCs photoelectric conversion efficiency experienced important breakthrough several times since 3.8% in 2009, and 2014
Year, its work function improves by doing modification to tin indium oxide (ITO) glass in the team of U.S. scientist foreign citizen of Chinese origin Yang Yang
And to the TiO as electron transfer layer2It is doped to improve the extraction of electronics and transmission, obtains 19.3% efficiency；?
In newest report, the photoelectric conversion efficiency of perovskite solar battery has broken through 23%, and is expected to be further developed.
Nano-titanium oxide material using very extensive, frequently as battery raw material, when being applied in lithium ion battery,
Because it is with fabulous high rate capability, cyclical stability, fast charging and discharging performance and higher capacity, not only efficiently solve
The safety issue of ion cathode material lithium also adds the stability of lithium battery, improves its chemical property, application prospect
It is wide；When it is applied in chemical energy solar battery, as electron transport layer materials, nano-titanium oxide is not only shown
Its superior stability, and its (its cost of manufacture is the 1/5~1/10 of silica-based solar cell) low in cost, also substantially
Degree improves the energy conversion efficiency of solar battery.
Conventional perovskite solar battery, main structure body includes cathode, electron transfer layer, perovskite active layer, sky
Cave transport layer, anode.Wherein other in addition to electron transfer layer layer can be prepared under the conditions of relatively low temperature,
By taking thin film of titanium oxide electron transfer layer as an example, existing common titanium dioxide preparation process needs carry out at 500~600 DEG C；
Therefore, temperature maximum of condition needed for electron transfer layer preparation must affect the industrialized production of perovskite solar battery.
Summary of the invention
Goal of the invention: aiming at the problem that needing higher temperature conditions when the preparation of electron transfer layer in the prior art, the present invention is mentioned
For a kind of preparation method of sull as electron transfer layer, it is controllable crystal form can be prepared under the conditions of lower temperature
And the lesser Oxide Electron of roughness transmits layer material；In addition, the present invention also provides a kind of oxidations comprising this method preparation
The perovskite solar battery of object thin film electronic transport layer and the preparation method of the perovskite solar battery.
Technical solution: the preparation method of the sull of the present invention as electron transfer layer, including following steps
It is rapid:
1) oxide precursor liquid solution is configured, is stirred evenly stand-by；
2) oxide precursor liquid solution is added dropwise in substrate surface and starts spin coating, substrate is transferred to containing luring after spin coating
In the sealing container for leading solvent ultrapure water；The preferred autoclave of sealing container, shell are stainless steel material, and liner is poly- four
Vinyl fluoride；
3) sealing container heated, make its internal formation thermal and hydric environment, the oxide precursor liquid solution of substrate surface occurs
Hydro-thermal reaction forms sull.
The effect of electron transfer layer is transmission electronics, and the sull as electron transfer layer of above-mentioned preparation can be oxygen
Change one of titanium, zinc oxide, tin oxide, zirconium oxide or many oxide film.
It can be suppression by solvent, diluted acid of alcohols in step (1) when Oxide Electron transmission layer film is thin film of titanium oxide
Preparation, tetraisopropyl titanate are persursor material, and configuration obtains titania precursor liquid solution.Wherein, diluted acid is preferably dilute hydrochloric acid
Or dust technology, alcohols are preferably ethyl alcohol or isopropanol.Further, in step 3), by sealing container at 120 DEG C~220 DEG C
At a temperature of heat 8~15h, substrate surface formed thin film of titanium oxide.
Above-mentioned steps 2) in, the volume of the inducing solvent of addition and the volume ratio of sealing container are 2~6:500, that is,
Say, by the volume of sealing container for 500ml in terms of, the volume of required inducing solvent is 2~6ml.
Perovskite solar battery of the present invention includes substrate, electron transfer layer, perovskite activity from bottom to top
Layer, hole transmission layer and cathode layer, substrate inside have anode material, wherein electron transfer layer is the oxygen of above method preparation
Compound film.
Wherein, glass, flexiplast etc. may be selected in substrate material.Anode material is located at substrate inner surface, can be indium
Tin-oxide (ITO, Indium Tin Oxide), fluorine tin-oxide (FTO, Fluorine doped Tin Oxide), fluorine doped
SnO2, aluminium zinc oxide (AZO, Aluminum doped Zinc Oxides) etc..What common industry had manufactured has anode
The substrate of material such as selects ITO electro-conductive glass or FTO electro-conductive glass.
Perovskite active layer uses perovskite material, and the effect in solar cell device is to absorb incident light, generates
Electron hole pair.It is made of using the perovskite active layer of solar battery of the invention fine and close perovskite crystal, thickness exists
500~600nm.Common active layer perovskite material mainly has ABX3(A=methylamino cation MA+, carbonamidine base cation FA+；B=Pb2+, Sn2+Deng；X=Cl-, Br-, I-Deng) the hybrid inorganic-organic perovskite of type crystal structure, energy band band gap is 1.0
~2.0eV.
The effect of hole transmission layer is mainly transporting holes, hole transport layer material be selected from Spiro-OMeTAD, PCDTBT,
One of PTAA, CuI (cupric iodide), CuSCN (cupric thiocyanate) etc. or a variety of.Spiro-OMeTAD refers to 2,2 ', 7,7 '-
Tetrakis [N, N-di (4-methoxyphenyl) amino] -9,9 '-spiro-bifluorene (2,2 ', 7,7 '-four [N,
N- bis- (4- methoxyphenyl) amino] two fluorenes of -9,9 '-spiral shell).PCDTBT refers to poly (N-9 '-heptadecanyl-2,7-
Carbazole-alt-5,5- (4 ', 7-di-2-thienyl-2 ', 1 ', 3 '-benzothiadiazole ([9- (1- octyl nonyl
Base) -9H- carbazole -2,7- diyl] -2,5- thiophene diyl -2,1,3- diazosulfide -4,7- diyl -2,5- thiophene diyl),
PTAA refers to poly- [bis- (4- phenyl) (2,4,6- trimethylphenyl) amine].
The material of cathode layer is generally using the conductive metallic material with higher work-functions, such as gold, silver.
The preparation method of perovskite solar battery of the present invention, includes the following steps:
1) preparation of substrate and anode material；The good glass substrate for being coated with required conductive layer of commercially available industrial production, it is real
It is cleaned up before testing；
2) preparation of electron transfer layer: configuration oxide precursor liquid solution stirs evenly stand-by；Oxygen is added dropwise in substrate surface
Compound precursor solution starts spin coating, and substrate is transferred in the sealing container containing inducing solvent after spin coating；To sealing
Container is heated, and forms sull in substrate surface；
3) preparation of perovskite active layer: the solution of configuration perovskite active layer material prepares calcium on the electron transport layer
Titanium ore activity layer film；Preferably, perovskite activity can be configured in the glove box of nitrogen environment or the laboratory of constant temperature and humidity
Layer solution simultaneously prepares perovskite activity layer film, and preparation method can be in the methods of solwution method, sedimentation, coevaporation method
It is a kind of；The material of perovskite active layer can choose MAPbI3、FAPbI3、MAPbBr3、MAPbI3-xClx、MAPbBr3-xClx、
(FAxMA1-x)PbI3Etc. one of or it is a variety of；；
4) preparation of hole transmission layer: configuring the solution of hole transport layer material, and spin coating obtains on perovskite active layer
Hole transmission layer；Preferably, can be configured in nitrogen glove box environment and spin coating hole transport layer material, material selection doped with
The Spiro-OMeTAD chlorobenzene solution of lithium salts and/or cobalt salt and four tertiary fourth pyridines；
5) preparation of cathode: conductive metal deposition material is as cathode on the hole transport layer；Vapor deposition apparatus can be used
Conductive metal deposition material, deposition thickness can be 80~120nm, and conductive metallic material can be gold or silver.
The utility model has the advantages that compared with the prior art, the advantages of the present invention are as follows: the present invention is lured by addition in a sealed container
Lead solvent ultrapure water, under high temperature and pressure, ultrapure water is atomization in sealing container, promotes the oxide precursor liquid solution of substrate surface
Hydro-thermal reaction occurs, crystal form is controllable and the lesser sull of roughness so as to preparing under the conditions of lower temperature,
When being used in solar cell device as electron transfer layer, the photovoltaic performance of device can be effectively improved；Moreover, the party
Method is simple to operation, and of less demanding to production equipment, is suitable for large-scale industrial application.
Detailed description of the invention
Fig. 1 is the process flow chart that thin film of titanium oxide is prepared using preparation method of the invention；
Fig. 2 (a)~2 (b) is that Oxide Electron made from embodiment 1 transmits scanning of the layer film under different enlargement ratios
Electron microscope；
Fig. 3 is the structural schematic diagram of the solar battery prepared by electron transfer layer of sull；
Fig. 4 is the scanning electron microscope (SEM) photograph of electron transfer layer made from embodiment 2；
Fig. 5 is the scanning electron microscope (SEM) photograph of electron transfer layer made from embodiment 3；
Fig. 6 is the scanning electron microscope (SEM) photograph of electron transfer layer made from embodiment 4；
Fig. 7 is the scanning electron microscope (SEM) photograph of electron transfer layer made from embodiment 5；
Fig. 8 is the solar cell device J-V characteristic curve prepared using sull as electron transfer layer.
Specific embodiment
Technical solution of the present invention is described further with reference to the accompanying drawing.
Perovskite thin film crystalline substance is with CH3NH3PbI3For, such as Fig. 1, the calcium titanium of high quality is prepared using method of the invention
Mine film, and make using the perovskite thin film as the solar cell device of active layer.
Embodiment 1
1) configuration of solution: TiO 2 precursor material of main part is selected from tetraisopropyl titanate, is dissolved in ethyl alcohol,
A small amount of hydrochloric acid is added as inhibitor within the scope of 1:10~1:20 in the volume ratio of solute and solvent.
2) cleaning of substrate: placing the substrate in dedicated substrate frame, successively uses cleaning agent, deionized water, acetone and second
Alcohol ultrasound twice, 20 minutes every time.After cleaning, it is put into baking oven and is dried for standby.By the electro-conductive glass of above-mentioned drying with ultraviolet
Line-ozone plasma handles 4min, to improve work content.
3) in substrate, configured TiO 2 precursor solution, spin coating parameters the preparation of electron transfer layer: are added dropwise
For 2000rpm, time 40s.It after spin coating, places the substrates in closed reaction vessel autoclave, is added in autoclave
The ultrapure water of 4mL, then autoclave is placed in Muffle furnace.By heating to autoclave, the reaction of a high temperature, high pressure is createed
Environment, heating temperature are 180 DEG C, and heating time is 12 hours；The thickness of sull obtained is in 50nm or so；
4) preparation of perovskite active layer: MAI, PbI21:1:1 is dissolved in solvent DMF in molar ratio with DMSO, so that most
The concentration of whole solution is 1.5mmol/ml.Using more gradient spin coating proceedings, specific spin coating parameters are as follows: (1) 4000rpm, 10s
(2) 6000rpm, 20s.It is thin to perovskite that toluene is added dropwise perpendicular to substrate in appropriate time (when 7s to 8s) after spin coating starts
Film surface carries out shower.After spin coating, the hot temperature that setting thermal station adds is 100 DEG C, is annealed 10~20 minutes.Obtained calcium titanium
Mine active layer film thickness is within the scope of 400~600nm.
5) preparation of hole transmission layer: hole mobile material Spiro-OMeTAD is dissolved in chlorobenzene, concentration 72.3mg/
Ml, addition volume is the acetonitrile solution of the tBp solution of 28.8 μ L and the Li-TFSI of 17.5 μ L in the chlorobenzene solution of every 1mL
(520mg/mL, solvent acetonitrile) uses after being thoroughly mixed under room temperature.Spin coating parameters 3500rpm, time 30s, obtained sky
Cave transport layer thickness is within the scope of 150~190nm.It is placed on after the completion of spin coating in dry air (or drying cupboard) and stands oxidation
6 to 12 hours.
6) preparation of electrode: the substrate for being sequentially prepared above layers is transferred in vacuum chamber, in high vacuum condition
Under (4 × 10-4Pa) thermal evaporation deposition is with a thickness of 90nm silver electrode.
Structure such as Fig. 3 of perovskite solar cell device obtained, wherein 1 is FTO electro-conductive glass, and 2 be electron-transport
Layer；3 be perovskite light absorbing layer, and 4 be hole transmission layer, and 5 be metal electrode.
Embodiment 2
The perovskite solar battery referring to made from the method for embodiment 1, difference is, in step 3), prepares electronics biography
When defeated layer, the volume of ultrapure water is 2mL in autoclave.
Embodiment 3
The perovskite solar battery referring to made from the method for embodiment 1, difference is, in step 3), prepares electronics biography
When defeated layer, the volume of ultrapure water is 6mL in autoclave.
Embodiment 4
The perovskite solar battery referring to made from the method for embodiment 1, difference is, in step 3), prepares electronics biography
When defeated layer, the heating temperature to autoclave is 120 DEG C, heating time 15h.
Embodiment 5
The perovskite solar battery referring to made from the method for embodiment 1, difference is, in step 3), prepares electronics biography
When defeated layer, the heating temperature to autoclave is 220 DEG C, heating time 8h.
Scanning electron microscope (SEM) photograph such as Fig. 2 (a)~2 (b) of thin film of titanium oxide electron transfer layer made from Examples 1 to 3 step (3)
With Fig. 4~5.As can be seen that generating TiO in Examples 1 to 32Particle, wherein in thin film of titanium oxide made from embodiment 1
TiO2Material growth becomes little particle, is paved with imaging surface；It only grown the TiO of part in embodiment 22Particle, this is because luring
It is smaller to lead solvent volume, pressure is smaller in reaction kettle, fails to be catalyzed TiO completely2Growth；In embodiment 3, TiO2It is grown to serve as
Crystal grain, but hole defect on crystal grain cause pressure in reaction vessel excessive this is because inducing solvent content becomes larger,
Injury is caused to film surface.Illustrate that sull, and oxygen can be made at low temperature using preparation method of the invention
The pattern of compound film can be regulated and controled by the amount of inducing solvent.
The scanning electron microscope (SEM) photograph of thin film of titanium oxide electron transfer layer such as Fig. 6~7 made from embodiment 4~5, it can be seen that real
The pattern for applying titanium carbide films made from example 1 and embodiment 4~5 is close, TiO in thin film of titanium oxide2Material is grown to serve as small
Particle is paved with imaging surface, and it is controllable to illustrate that crystal form can be made in use method of the invention under 120~220 DEG C of cryogenic conditions
And the lesser sull of roughness；In addition, can see by Fig. 7, there is hole in partial oxidation titanium film surface, this be by
There are some destructions to film in temperature is too high, therefore, has preferable pattern to guarantee to be made thin film of titanium oxide, to sealing container
Heating temperature is preferably controlled in 120~220 DEG C.
The photoelectric properties of perovskite solar battery made from Examples 1 to 5 are tested, test result such as Fig. 6 and
The following table 1.
The solar cell device photoelectric characteristic test result that 1 Examples 1 to 5 of table is prepared
Complex chart 8 and 1 data of table can be seen that thin film of titanium oxide electron transfer layer application obtained by the method for the invention
Into solar cell device, every photovoltaic performance of device is all preferable；Moreover, compared with Example 1, embodiment 2~5 is made
Solar cell device photovoltaic performance it is slightly poor, wherein the electron transfer layer inferior quality that embodiment 2 obtains, it is final to be made
Device photovoltaic performance it is also worst；The volume for illustrating inducing solvent and hydrothermal temperature and time are to electron-transport layer film
Qualitative effects it is larger, and then directly affect solar cell device photovoltaic performance.
Claims (10)
1. a kind of preparation method of the sull as electron transfer layer, which is characterized in that include the following steps:
1) oxide precursor liquid solution is configured, is stirred evenly stand-by；
2) substrate surface be added dropwise oxide precursor liquid solution start spin coating, after spin coating by substrate be transferred to containing induction it is molten
In the sealing container of agent ultrapure water；
3) sealing container heated, make its internal formation thermal and hydric environment, it is thin that hydro-thermal reaction, formation oxide occur for substrate surface
Film.
2. the preparation method of the sull according to claim 1 as electron transfer layer, which is characterized in that described
Sull is thin film of titanium oxide, zinc-oxide film, SnO 2 thin film, zirconia film or titanium oxide, zinc oxide, oxidation
The composite oxide film that at least two oxides are formed in tin, zirconium oxide.
3. the preparation method of the sull according to claim 1 as electron transfer layer, which is characterized in that described
Sull is thin film of titanium oxide, and in step 1), using alcohols as solvent, diluted acid be inhibitor, tetraisopropyl titanate is forerunner
Body material configures titania precursor liquid solution.
4. the preparation method of the sull according to claim 3 as electron transfer layer, which is characterized in that step
3) in, by the sealing container 120 DEG C~220 DEG C at a temperature of heat 8~15h.
5. the preparation method of the sull according to claim 1 as electron transfer layer, which is characterized in that step
2) in, the volume of the inducing solvent and the volume ratio of sealing container are 2~6:500.
6. a kind of perovskite solar battery includes substrate, electron transfer layer, perovskite active layer, hole biography from bottom to top
Defeated layer and cathode layer, the substrate inside have anode material, which is characterized in that the electron transfer layer is claim 1 system
Standby sull.
7. perovskite solar battery according to claim 6, which is characterized in that the substrate material is glass or flexibility
Plastics, anode material be indium tin oxide, fluorine tin-oxide, fluorine doped SnO2Or aluminium zinc oxide.
8. perovskite solar battery according to claim 5, which is characterized in that the hole transport layer material is selected from 2,
2 ', 7,7 '-four [N, N- bis- (4- methoxyphenyl) amino] -9,9 '-spiral shell, two fluorenes, [9- (1- octyl nonyl) -9H- carbazole -2,7-
Diyl] -2,5- thiophene diyl -2,1,3- diazosulfide -4,7- diyl -2,5- thiophene diyl, it is poly- [bis- (4- phenyl) (2,4,
6- trimethylphenyl) amine], cupric iodide, one of cupric thiocyanate or a variety of.
9. perovskite solar battery according to claim 5, which is characterized in that the perovskite active layer material is
ABX3The hybrid inorganic-organic perovskite material of type crystal structure, wherein A is methylamino cation MA+Or carbonamidine base cation
FA+, B Pb2+Or Sn2+, X Cl-, Br-Or I-。
10. a kind of preparation method of perovskite solar battery as claimed in claim 6, which is characterized in that include the following steps:
1) preparing substrate and anode material；
2) preparation of electron transfer layer: configuration oxide precursor liquid solution stirs evenly stand-by；Oxide is added dropwise in substrate surface
Precursor solution starts spin coating, and substrate is transferred in the sealing container containing inducing solvent after spin coating；To sealing container
It is heated, forms sull in substrate surface；
3) preparation of perovskite active layer: the solution of configuration perovskite active layer material prepares perovskite on the electron transport layer
Active layer film；
4) preparation of hole transmission layer: configuring the solution of hole transport layer material, and spin coating obtains hole on perovskite active layer
Transport layer；
5) preparation of cathode: conductive metal deposition material is as cathode on the hole transport layer.
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