CN109119536A - Utilize extension TiO2The method that nano crystal array constructs efficient perovskite solar battery - Google Patents
Utilize extension TiO2The method that nano crystal array constructs efficient perovskite solar battery Download PDFInfo
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- CN109119536A CN109119536A CN201710494917.5A CN201710494917A CN109119536A CN 109119536 A CN109119536 A CN 109119536A CN 201710494917 A CN201710494917 A CN 201710494917A CN 109119536 A CN109119536 A CN 109119536A
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- H—ELECTRICITY
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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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- 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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Abstract
The invention belongs to area of solar cell, are a kind of utilization extension TiO2The method that nano crystal array constructs efficient perovskite solar battery.Using fluorine-doped tin oxide electro-conductive glass substrate as substrate, SnO is utilized2With rutile TiO2With high lattice match, the growth in situ rutile TiO on FTO matrix2Nano crystal array further improves FTO and rutile TiO by high-temperature heat treatment2The intergranular interface binding power of nano crystal.The present invention utilizes epitaxial growth rutile TiO2Nano crystal array compacted zone assembles perovskite solar battery as electron transfer layer, the compacted zone has the unique textures such as high-crystallinity (few body phase defect), mono-crystalline structures (no crystal boundary), coherent boundary (no boundary defect), reduce energy loss of the light induced electron in transfer and transmission process to the full extent, is a kind of efficient perovskite desired electronic transport layer used for solar batteries.
Description
Technical field
The invention belongs to area of solar cell, are a kind of utilization extension TiO2Nano crystal array constructs efficient perovskite
The method of solar battery.
Background technique
Perovskite solar battery is studied extensively due to having many advantages, such as high efficiency, low cost, preparing easy.
TiO2Compacted zone as electron transfer layer and hole blocking layer, played a crucial role in perovskite solar battery and
Directly affect the transformation efficiency of battery.Compacted zone is mostly to pass through the spin coating combination subsequent heat treatment of colloidal solution containing titanium precursors at present
Convert obtained Anatase TiO2, and the compacted zone that spin coating obtains will appear non-uniform phenomenon often, while sharp in compacted zone
Titanium ore TiO2There are a large amount of crystal boundaries between nano particle, and the SnO with Fluorin doped2Transparent conducting glass matrix (FTO) is without symbiosis and epibiosis
And there are a large amount of phase interfaces, electronics leads to energy loss there are a large amount of crystal boundaries and phase boundary defect scattering in transmission process, causes
Battery open circuit voltage and transformation efficiency reduce.Rutile Type TiO2Join with crystal structure identical with FTO and similar lattice
Number, the epitaxial growth rutile TiO in situ on FTO2Crystal array can significantly eliminate crystal boundary, phase bound pair photoproduction as compacted zone
The scattering process of electronics is a kind of effective means for improving the open-circuit voltage and transformation efficiency of battery.
Summary of the invention
The purpose of the present invention is to provide one kind on FTO conducting base growth in situ monocrystalline rutile TiO2Compacted zone
Method, so that TiO2Without boundary defect between FTO matrix, and TiO2Internal flaw reduces, and electronics and hole-recombination probability drop
Low, electron-transport efficiency improves, and perovskite solar battery is assembled using this dense film as electron transfer layer, can be effectively improved
The open-circuit voltage and transformation efficiency of battery.
The technical scheme is that
It is a kind of to utilize extension TiO2The method that nano crystal array constructs efficient perovskite solar battery, it is transparent with FTO
Electro-conductive glass is substrate, above it coherent growth densification rutile TiO in situ2Crystal array film, by increasing after heat treatment
Strong interface binding power；Perovskite solar battery is assembled using this film as electron transfer layer, utilizes its high-crystallinity, monocrystalline knot
The unique texture of structure, coherent boundary obtains the efficient perovskite solar battery of high open circuit voltage.
The coherent growth densification rutile TiO2Method include various chemistry, electrochemistry or physical method.
The coherent growth densification rutile TiO2Method be hydro-thermal method, electrochemical deposition method or sputter coating method.
The film heat-treatment temperature range is 100~800 DEG C, and the processing time is 10 minutes to 10 days, is heat-treated gas
Atmosphere is oxygen-enriched environment, and partial pressure of oxygen is 100Pa to 10MPa.
The oxygen-enriched environment is air or oxygen.
The perovskite material includes organic-inorganic hybrid structure or pure inorganic mechanism, organic-inorganic hybrid structure R-
NH3MAxB3-x: R-NH3Organic ammonium ion is represented, M represents metal Pb, Sn, Bi or Cu, and A and B are halogen, x=0~3；
Pure inorganic mechanism is MAMAxB3-x: MARepresenting alkali metal, M represents metal Pb, Sn, Bi or Cu, and A and B are halogen, x=0~
3.Wherein, organic ammonium ion is CH3NH3, halogen F, Cl, Br or I, alkali metal Cs.
The assembling process of the perovskite solar battery includes:
(1) FTO electrically conducting transparent matrix is cleaned；
(2) the epitaxial growth Rutile Type TiO on the FTO electrically conducting transparent matrix cleaned up2Nano crystal array is fine and close
Layer, and interface binding power is improved by heat treatment；
(3) in Rutile Type TiO2Perovskite thin film is deposited on nano crystal array compacted zone；
(4) the deposition of hole transport layer on perovskite thin film；
(5) deposit metal electrodes on the hole transport layer.
In the assembling process of the perovskite solar battery, perovskite thin film deposition process includes that various perovskites are thin
Membrane preparation method.
The perovskite thin film preparation method is solution spin-coating method, solution spraying method, gas-solid reaction method or thermal evaporation deposition.
Advantages of the present invention and beneficial effect are:
The present invention provides the rutile TiO using the epitaxial growth on FTO matrix2Nano crystal array dense film is made
For the electron transfer layer of perovskite solar battery, high-crystallinity (few body phase defect, carrier concentration 1016~1018), it is single
The unique textures such as crystal structure (no crystal boundary), coherent boundary (no boundary defect), reduce light induced electron to the full extent and are shifting
With the energy loss in transmission process, important references are provided to construct the perovskite solar battery of efficient, high open circuit voltage, into
And obtain the perovskite solar battery of high open circuit voltage.
Detailed description of the invention
Fig. 1: the battery structure schematic diagram in the specific embodiment of the invention.In figure, 1, conducting base；2, rutile TiO2
Nano crystal array compacted zone；3, perovskite thin film；4, hole transmission layer；5, metal electrode.
Fig. 2: the rutile TiO obtained in the embodiment of the present invention 12The scanning electron microscopy of nano crystal array dense film
Mirror photo (SEM).
Fig. 3: the plane perovskite solar cell I-V curve assembled in the embodiment of the present invention 1.Wherein: X-axis Voltage
It is density of photocurrent (mAcm for voltage (V), Y-axis J-2)。
Fig. 4: the rutile TiO obtained in the embodiment of the present invention 22The scanning electron microscopy of nano crystal array dense film
Mirror photo (SEM).
Fig. 5: the plane perovskite solar cell I-V curve assembled in the embodiment of the present invention 2.Wherein: X-axis Voltage
It is density of photocurrent (mAcm for voltage (V), Y-axis J-2)。
Specific embodiment
In the specific implementation process, the present invention utilizes epitaxial growth rutile TiO2Nano crystal array compacted zone is as electricity
The method that sub- transport layer constructs high open circuit voltage perovskite solar battery, using FTO transparent conducting glass as substrate, above it
Coherent growth densification rutile TiO in situ2Crystal array film, by enhancing interface binding power after high-temperature heat treatment；It is thin with this
Film assembles perovskite solar battery as electron transfer layer, obtains the perovskite solar battery of high open circuit voltage.Wherein, thin
Film heat-treatment temperature range is 100~800 DEG C, and the processing time is 10 minutes to 10 days, and heat-treating atmosphere is oxygen-enriched environment, oxygen
Pressure is 100Pa to 10MPa.Preferably, film heat-treatment temperature range is 400~600 DEG C, and the processing time is 0.5~2h, it is hot at
Qi-regulating atmosphere is oxygen-enriched environment, partial pressure of oxygen 104~105。
Carry out the present invention described in more detail below with reference to examples and drawings.
As shown in Figure 1, the perovskite solar battery structure of the present embodiment, from bottom to top successively are as follows: conducting base 1
(FTO), rutile TiO2Nano crystal array compacted zone 2,3 (CH of perovskite thin film3NH3PbI3), 4 (spiro- of hole transmission layer
OMeTAD), metal electrode 5 (Au).
Embodiment 1
In the present embodiment, FTO conducting base is cleaned, ultrasound 30min is distinguished in water, ethyl alcohol, acetone, isopropanol solvent,
Then with being dried with nitrogen, using O210~20min of corona treatment.It is total in situ on FTO conducting base using hydrothermal method
Lattice growing rutile TiO2Nano crystal array compacted zone: TiCl is prepared first4Hydrochloric acid solution (wherein Ti molar concentration is
0.015M, hydrochloric acid molar concentration are 3.5M, take above-mentioned solution 40ml to be put into reaction kettle liner, and the NaF of 20mg is added；Then
Cleaned sheet glass is put into solution, hydrothermal growth temperature is 245 DEG C, time 2h；The gold that will be obtained after hydrothermal growth
Red stone TiO2After nano crystal array film is cleaned up with a large amount of deionized waters, it is put into 500 DEG C of annealings in Muffle furnace
30min, obtained rutile TiO2Nano crystal array film is as shown in Fig. 2, based on nano crystal exposure (110) crystal face.
In perovskite cell assembling processes, CH is used in this example3NH3I and PbCl2Molar ratio 3:1 is dissolved in dimethyl
In formamide (DMF) solution, using spin coating method by above-mentioned solution film forming in rutile TiO2Nano crystal array film surface
(wherein spin coating parameters are revolving speed 3000r/min retention time 60s), is inhaled by obtaining perovskite after 100 DEG C of annealing 90min
Photosphere (perovskite thin film)；The hole conductor that the present embodiment hole transmission layer uses is spiro-OMeTAD, the chlorine of hole conductor
Benzole soln is deposited on perovskite extinction layer surface (when wherein, spin coating parameters are that revolving speed 5000r/min is kept by the method for spin coating
Between 30s), after natural drying, aoxidize 12h under dry air；Evaporation metal electrode, this example use gold for apex electrode, benefit
It is 60nm with hot evaporation method evaporation thickness.The above-mentioned solar battery being prepared is tested under AM1.5 standard sources
Peak efficiency reaches 17.2% (Fig. 3).
Embodiment 2
In the present embodiment, FTO conducting base is cleaned, ultrasound 30min is distinguished in water, ethyl alcohol, acetone, isopropanol solvent,
Then with being dried with nitrogen, using O210~20min of corona treatment.It is total in situ on FTO conducting base using hydrothermal method
Lattice growing rutile TiO2Nano crystal array compacted zone: TiCl is prepared first4Hydrochloric acid solution (wherein Ti molar concentration is
0.015M, hydrochloric acid molar concentration are 3.5M, take above-mentioned solution 40ml to be put into reaction kettle liner, and the NaF of 50mg is added；Then
Cleaned sheet glass is put into solution, hydrothermal growth temperature is 245 DEG C, time 2h；The gold that will be obtained after hydrothermal growth
Red stone TiO2After nano crystal array film is cleaned up with a large amount of deionized waters, it is put into 500 DEG C of annealings in Muffle furnace
30min, obtained rutile TiO2Nano crystal array film is as shown in figure 4, based on nano crystal exposure (111) crystal face.
In perovskite cell assembling processes, CH is used in this example3NH3I and PbCl2Molar ratio 3:1 is dissolved in dimethyl
In formamide (DMF) solution, using spin coating method by above-mentioned solution film forming in rutile TiO2Nano crystal array film surface
(wherein spin coating parameters are revolving speed 3000r/min retention time 60s), is inhaled by obtaining perovskite after 100 DEG C of annealing 90min
Photosphere；For the hole conductor that the present embodiment hole transmission layer uses for spiro-OMeTAD, the chlorobenzene solution of hole conductor passes through rotation
The method of painting is deposited on perovskite extinction layer surface (wherein spin coating parameters are revolving speed 5000r/min retention time 30s), naturally dry
After dry, 12h is aoxidized under dry air；Evaporation metal electrode, this example use gold for apex electrode, are steamed using hot evaporation method
Plating is with a thickness of 60nm.The peak efficiency tested under AM1.5 standard sources the above-mentioned solar battery being prepared reaches
15.4% (Fig. 5).
Embodiment the result shows that, the present invention utilizes SnO using fluorine-doped tin oxide (FTO) electro-conductive glass substrate as substrate2
With rutile TiO2With high lattice match, the growth in situ rutile TiO on FTO matrix2Nano crystal array, into one
Step improves FTO and rutile TiO by high-temperature heat treatment2The intergranular interface binding power of nano crystal.Utilize rutile TiO2
Nano crystal array compacted zone assembles standard perovskite solar battery as electron transfer layer, and the open-circuit voltage of battery can reach
1.11V, peak efficiency have reached 17.2%.The present invention utilizes epitaxial growth rutile TiO2Nano crystal array compacted zone is made
Perovskite solar battery is assembled for electron transfer layer, which has high-crystallinity (few body phase defect), mono-crystalline structures (nothing
Crystal boundary), the unique textures such as coherent boundary (no boundary defect), reduce light induced electron to the full extent in transfer and transmission process
In energy loss, be a kind of efficient perovskite desired electronic transport layer used for solar batteries.
Above example is only preferable in the present invention as a result, being not intended to restrict the invention, all in principle basis of the present invention
On do on an equal basis replace or modify technical solution obtained, it is within the scope of the present invention.
Claims (10)
1. a kind of utilize extension TiO2The method that nano crystal array constructs efficient perovskite solar battery, it is characterised in that: with
FTO transparent conducting glass is substrate, above it coherent growth densification rutile TiO in situ2Crystal array film, at heat
Enhance interface binding power after reason；Using this film as electron transfer layer assemble perovskite solar battery, using its high-crystallinity,
The unique texture of mono-crystalline structures, coherent boundary obtains the efficient perovskite solar battery of high open circuit voltage.
2. described in accordance with the claim 1 utilize extension TiO2Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the coherent growth densification rutile TiO2Method include various chemistry, electrochemistry or physics side
Method.
3. utilizing extension TiO according to claim 22Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the coherent growth densification rutile TiO2Method be hydro-thermal method, electrochemical deposition method or sputtering plating
Embrane method.
4. described in accordance with the claim 1 utilize extension TiO2Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the film heat-treatment temperature range is 100~800 DEG C, and the processing time is 10 minutes to 10 days, heat
Processing atmosphere is oxygen-enriched environment, and partial pressure of oxygen is 100Pa to 10MPa.
5. described in accordance with the claim 3 utilize extension TiO2Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the oxygen-enriched environment is air or oxygen.
6. described in accordance with the claim 1 utilize extension TiO2Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the perovskite material includes organic-inorganic hybrid structure or pure inorganic mechanism, organic inorganic hybridization knot
Structure is R-NH3MAxB3-x: R-NH3Organic ammonium ion is represented, M represents metal Pb, Sn, Bi or Cu, and A and B are halogen, x=
0~3；Pure inorganic mechanism is MAMAxB3-x: MAAlkali metal is represented, M represents metal Pb, Sn, Bi or Cu, and A and B are halogen, x
=0~3.
7. utilizing extension TiO according to claim 62Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that organic ammonium ion is CH3NH3, halogen F, Cl, Br or I, alkali metal Cs.
8. described in accordance with the claim 1 utilize extension TiO2Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the assembling process of the perovskite solar battery includes:
(1) FTO electrically conducting transparent matrix is cleaned；
(2) the epitaxial growth Rutile Type TiO on the FTO electrically conducting transparent matrix cleaned up2Nano crystal array compacted zone, and
Interface binding power is improved by heat treatment；
(3) in Rutile Type TiO2Perovskite thin film is deposited on nano crystal array compacted zone；
(4) the deposition of hole transport layer on perovskite thin film；
(5) deposit metal electrodes on the hole transport layer.
9. utilizing extension TiO according to claim 82Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that in the assembling process of the perovskite solar battery, perovskite thin film deposition process includes various calcium
Titanium ore method for manufacturing thin film.
10. utilizing extension TiO according to claim 92Nano crystal array constructs the side of efficient perovskite solar battery
Method, which is characterized in that the perovskite thin film preparation method is solution spin-coating method, solution spraying method, gas-solid reaction method or heat
Vapour deposition method.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204885219U (en) * | 2015-09-06 | 2015-12-16 | 辽宁工业大学 | Catch formula nanoarray titanium dioxide perovskite type solar cell |
| CN205028929U (en) * | 2015-08-19 | 2016-02-10 | 辽宁工业大学 | Perovskite type solar cell |
| CN105552236A (en) * | 2015-12-08 | 2016-05-04 | 中国电子科技集团公司第十八研究所 | Perovskite solar cell and preparation method thereof |
-
2017
- 2017-06-26 CN CN201710494917.5A patent/CN109119536A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN205028929U (en) * | 2015-08-19 | 2016-02-10 | 辽宁工业大学 | Perovskite type solar cell |
| CN204885219U (en) * | 2015-09-06 | 2015-12-16 | 辽宁工业大学 | Catch formula nanoarray titanium dioxide perovskite type solar cell |
| CN105552236A (en) * | 2015-12-08 | 2016-05-04 | 中国电子科技集团公司第十八研究所 | Perovskite solar cell and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| HUA WANG等: ""Rutile TiO2 nano-branched arrays on FTO for dye-sensitized solar cells"", 《PHYS. CHEM. CHEM. PHYS》 * |
| HUI-SEON KIM等: ""High Efficiency Solid-State Sensitized Solar Cell-Based on Submicrometer Rutile TiO2 Nanorod and CH3NH3PbI3 Perovskite Sensitizer"", 《NANO LETTERS》 * |
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