CN104022185A - Perovskite membrane and preparation and application method thereof - Google Patents

Perovskite membrane and preparation and application method thereof Download PDF

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CN104022185A
CN104022185A CN201410268812.4A CN201410268812A CN104022185A CN 104022185 A CN104022185 A CN 104022185A CN 201410268812 A CN201410268812 A CN 201410268812A CN 104022185 A CN104022185 A CN 104022185A
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perovskite
perovskite film
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halide
pbi
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CN104022185B (en
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谭占鳌
李聪
侯旭亮
于露
屈江江
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North China Electric Power University
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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
    • H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • 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
    • H10K30/20—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising organic-organic junctions, e.g. donor-acceptor junctions
    • 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
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

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  • Chemical & Material Sciences (AREA)
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Abstract

The invention belongs to the technical field of solar cells and particularly relates to a perovskite membrane and a preparation and application method of the perovskite membrane. The perovskite membrane is generated through a two-step method, a PbI2 membrane is prepared through a solution processing method, and thus the technology is simple and efficient. Besides, due to the two-step method, the flatness of the surface of the perovskite membrane is effectively improved, recombination of carriers on the active layer interface is greatly reduced, the anti-solvent performance of the material is effectively improved, and the performance of a device is obviously improved. The perovskite membrane further has the advantages of being simple in preparation technology, low in cost, good in experimental repeatability, suitable for large-scale industrial production and the like.

Description

A kind of perovskite film and preparation and application method thereof
Technical field
The invention belongs to technical field of solar cells, particularly a kind of perovskite film and preparation and application method thereof.
Background technology
The Ca-Ti ore type solar cell of rising in recent years has that efficiency is high, cost is low, quality is light, and manufacture craft is simple, can be prepared into the outstanding advantages such as large area flexible device and receive much concern.Since two thousand nine, the development of perovskite battery is very rapid, has only used the time less than 4 years by the efficiency that develops into 16% less than 5% efficiency.Therefore the solar cell of the type has become the study hotspot in photovoltaic field.2013, the selected world of the research year ten large Progress & New Products of perovskite solar cell.
Perovskite solar cell refers to specifically with having ABO 3the perovskite material of configuration is as CH 3nH 3pbX 3(X is Cl, Br, I halogen atom) etc. is as the solar cell of light absorbing zone.Directly restrict the performance quality of perovskite solar cell as the quality of the perovskite thin film of light-absorption layer.And have two kinds about the preparation method of perovskite film: one-step method and two-step method.One-step method refers to lead halide as PbI 2with alkyl halide amine as CH 3nH 3i directly reacts synthesis of organometallic halide perovskite as CH 3nH 3pbI 3solution.When but one-step method is synthetic, need strict control experiment condition, water proof oxygen barrier, 60 DEG C are heated 12 hours.Experiment condition is wayward, easily makes perovskite oxidation or decomposes, and then can have influence on the purity of perovskite solution.Two-step method refers to and shows lead halide as PbI 2precursor solution is spin-coated on anode, and then with alkyl halide amine as CH 3nH 3i reaction, in substrate, original position generates organic metal halide perovskite thin film.Existing two-step method is by PbI 2be immersed in CH 3nH 3in the aqueous isopropanol of I, make it reaction and produce perovskite.Adopt the method often to cause PbI 2reaction not exclusively, causes calcium titanium ore bed to have impurity PbI 2existence.Impurity PbI 2be the complex centre in electronics and hole, directly affect device performance.In addition, the speed of the method battery surface reaction in course of reaction is not identical, often causes the variable thickness of film, causes the evenness of gained perovskite thin film poor.The present invention adopts two-step method vacuum synthesis perovskite, first by lead halide as PbI 2precursor solution is spin-coated on anode, spreads a little CH around battery 3nH 3i powder, covers culture dish lid, and under the condition of vacuum, 150 DEG C can produce the very fine and close smooth perovskite thin film of one deck after heat treatment 1-4 hour.The present invention preparation method used efficiently solves experiment condition loaded down with trivial details in one-step method, and reacts incomplete and the irregular problem of film in two-step method.The perovskite thin film of preparing by the method for the invention shows excellent photovoltaic performance.
Summary of the invention
For prior art deficiency, the invention provides a kind of perovskite film and preparation and application method thereof.
A preparation method for perovskite film, uses two step vacuum methodes, obtains the perovskite film of one deck densification.
A preparation method for perovskite film, its concrete grammar is as follows:
By lead halide PbX 2precursor solution is spin-coated on hole transmission layer, heating, drying, then lead halide film is moved in vacuum drying chamber, around lead halide film, sprinkle alkyl halide amine powder, cover culture dish lid, heating makes alkyl halide amine evaporate the organic metal halide calcium titanium ore bed that directly reacts the densification of generation one deck with lead halide.
Described X is Cl, Br or I.
Described lead halide is PbI 2, alkyl halide amine is CH 3nH 3i, organic metal halide calcium titanium ore bed is CH 3nH 3pbI 3.
Described lead halide PbX 2the solvent of precursor solution is one or both in DMF (DMF), gamma-butyrolacton.
A kind of perovskite film, described perovskite film is prepared by said method.
An application process for perovskite film, described perovskite film is for the preparation of perovskite solar cell.
In described perovskite solar cell, transparent conductive metal oxide skin(coating), hole transmission layer, perovskite film, electron transfer layer are connected in turn with metal electrode layer.
The material of described hole transmission layer is one or more in high work function metal oxide, p-type conjugated polymer and p-type electric-conducting polymer.
The material of described electron transfer layer is one or more in N-shaped metal oxide, fullerene and derivative thereof, N-shaped conjugated polymer and N-shaped conducting polymer.
Beneficial effect of the present invention is:
The present invention adopts two-step method to generate perovskite film, PbI 2film adopts the method preparation of solution processing, makes technique simple, efficient.Two-step method vacuum synthesis effectively raises the evenness on film surface in addition, has reduced greatly compound at active layer interface of charge carrier, effectively improves the solvent resistance energy of material, has improved significantly the performance of device.It is simple that the present invention also has preparation technology, with low cost, and experimental repeatability is good, be suitable for the features such as large-scale industrial production.
Brief description of the drawings
Fig. 1 is the synthetic perovskite film scanning electron microscopy shape appearance figure of one-step method;
Fig. 2 is two-step method vacuum synthesis perovskite film scanning electron microscopy shape appearance figure;
Fig. 3 is the current-voltage characteristic curve that the embodiment of the present invention 1 adopts the synthetic perovskite solar cell of one-step method, and obtained device structure is FTO/PEDOT:PSS/CH 3nH 3pbI 3/ PC 60bM/Al;
Fig. 4 is the current-voltage characteristic curve that the embodiment of the present invention 2 adopts the synthetic perovskite solar cell of two-step method vacuum 1h, and obtained device structure is FTO/PEDOT:PSS/CH 3nH 3pbI 3/ PC 60bM/Al;
Fig. 5 is the current-voltage characteristic curve that the present invention adopts the synthetic perovskite solar cell of two-step method vacuum 2h, and obtained device structure is FTO/PEDOT:PSS/CH 3nH 3pbI 3/ PC 60bM/Al;
Fig. 6 is the current-voltage characteristic curve that the present invention adopts the synthetic perovskite solar cell of two-step method vacuum 3h, and obtained device structure is FTO/PEDOT:PSS/CH 3nH 3pbI 3/ PC 60bM/Al;
Fig. 7 is the current-voltage characteristic curve that the present invention adopts the synthetic perovskite solar cell of two-step method vacuum 4h, and obtained device structure is FTO/PEDOT:PSS/CH 3nH 3pbI 3/ PC 60bM/Al.
Embodiment
The invention provides a kind of perovskite film and preparation and application method thereof, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1 (comparative example)
Sputter is had to fluorine doping SnO 2(FTO) transparent conducting glass is used liquid detergent, running water, deionized water, acetone, isopropyl alcohol ultrasonic cleaning 2 times successively, nitrogen dries up, put into immediately UV ozone surface processing equipment (UVO) and process 15min, spin coating PEDOT:PSS solution under the rotating speed of 2000rpm, in air at 150 DEG C of temperature thermal annealing 15 minutes, obtain hole transmission layer, its thickness is 30nm left and right.Then by PbI 2with CH 3nH 3i is dissolved in DMF (N by the mass ratio of 1:1, dinethylformamide) in solution, heating 12h, prepare perovskite solution, under the rotating speed of the perovskite solution that is 30wt% by concentration with 3000rpm, be spun on above hole transmission layer, thermal annealing 2h afterwards, gained calcium titanium ore bed thickness is 300nm.Afterwards again by PC 60bM concentration is the PC of 20mg/mL 60dichloro-benzenes (ODCB) solution of BM is spun on above-mentioned calcium titanium ore bed under 1000rpm rotating speed, and gained film thickness is 5nm～15nm.Finally, 5 × 10 -4the aluminium that under handkerchief, vacuum evaporation 100nm is thick is as negative pole.Prepared device open circuit voltage under the simulated solar irradiation of every square centimeter of 100 milliwatt is 0.89 volt, and short circuit current is 11.29mA/cm 2, fill factor, curve factor is 57%, conversion efficiency is 5.44%.Fig. 3 has provided this device without irradiation and the current-voltage curve under the simulated solar irradiation of every square centimeter of 100 milliwatt.
Embodiment 2
Sputter is had to fluorine doping SnO 2(FTO) transparent conducting glass is used liquid detergent, running water, deionized water, acetone, isopropyl alcohol ultrasonic cleaning 2 times successively, nitrogen dries up, put into immediately UV ozone surface processing equipment (UVO) and process 15min, spin coating PEDOT:PSS solution under the rotating speed of 2000rpm, in air at 150 DEG C of temperature thermal annealing 15 minutes, obtain hole transmission layer, its thickness is 30nm left and right.Then by PbI 2concentration is the PbI of 300mg/mL 2precursor solution is directly spun on above-mentioned hole transmission layer under the rotating speed of 2000rpm, is then placed on hot platform, afterwards according to every 1cm 2gained PbI 2film approximately uses CH 3nH 3the usage ratio of I20mg, by CH 3nH 3i powder is evenly sprinkling upon gained PbI 2around film, cover with culture dish, at 150 DEG C of temperature, be incubated after 2 hours, clean and use dry nitrogen to dry up with isopropyl alcohol, obtain calcium titanium ore bed, its thickness is 300nm.Afterwards again by PC 60bM concentration is the PC of 20mg/mL 60dichloro-benzenes (ODCB) solution of BM is spun on above-mentioned calcium titanium ore bed under 1000rpm rotating speed, and gained film thickness is 5nm～15nm.Finally, 5 × 10 -4the aluminium that under handkerchief, vacuum evaporation 100nm is thick is as negative pole.Prepared device open circuit voltage under the simulated solar irradiation of every square centimeter of 100 milliwatt is 0.89 volt, and short circuit current is 12.51mA/cm 2, fill factor, curve factor is 49%, conversion efficiency is 5.47%.Fig. 4 has provided this device without irradiation and the current-voltage curve under the simulated solar irradiation of every square centimeter of 100 milliwatt.
Embodiment 3
Sputter is had to fluorine doping SnO 2(FTO) transparent conducting glass is used liquid detergent, running water, deionized water, acetone, isopropyl alcohol ultrasonic cleaning 2 times successively, nitrogen dries up, put into immediately UV ozone surface processing equipment (UVO) and process 15min, spin coating PEDOT:PSS solution under the rotating speed of 2000rpm, in air at 150 DEG C of temperature thermal annealing 15 minutes, obtain hole transmission layer, its thickness is 30nm left and right.Then by PbI 2concentration is the PbI of 300mg/mL 2precursor solution is directly spun on above-mentioned hole transmission layer under the rotating speed of 2000rpm, is then placed on hot platform, afterwards according to every 1cm 2gained PbI 2film approximately uses CH 3nH 3the usage ratio of I20mg, by CH 3nH 3i powder is evenly sprinkling upon gained PbI 2around film, cover with culture dish, at 150 DEG C of temperature, be incubated after 4 hours, clean and use dry nitrogen to dry up with isopropyl alcohol, obtain calcium titanium ore bed, its thickness is 300nm.Afterwards again by PC 60bM concentration is the PC of 20mg/mL 60dichloro-benzenes (ODCB) solution of BM is spun on above-mentioned calcium titanium ore bed under 1000rpm rotating speed, and gained film thickness is 5nm～15nm.Finally, 5 × 10 -4the aluminium that under handkerchief, vacuum evaporation 100nm is thick is as negative pole.Prepared device open circuit voltage under the simulated solar irradiation of every square centimeter of 100 milliwatt is 0.85 volt, and short circuit current is 12.77mA/cm 2, fill factor, curve factor is 66%, conversion efficiency is 7.25%.Fig. 5 has provided this device without irradiation and the current-voltage curve under the simulated solar irradiation of every square centimeter of 100 milliwatt.
Embodiment 4
Sputter is had to fluorine doping SnO 2(FTO) transparent conducting glass is used liquid detergent, running water, deionized water, acetone, isopropyl alcohol ultrasonic cleaning 2 times successively, nitrogen dries up, put into immediately UV ozone surface processing equipment (UVO) and process 15min, spin coating PEDOT:PSS solution under the rotating speed of 2000rpm, in air at 150 DEG C of temperature thermal annealing 15 minutes, obtain hole transmission layer, its thickness is 30nm left and right.Then by PbI 2concentration is the PbI of 300mg/mL 2precursor solution is directly spun on above-mentioned hole transmission layer under the rotating speed of 2000rpm, is then placed on hot platform, afterwards according to every 1cm 2gained PbI 2film approximately uses CH 3nH 3the usage ratio of I20mg, by CH 3nH 3i powder is evenly sprinkling upon gained PbI 2around film, cover with culture dish, at 150 DEG C of temperature, be incubated after 3 hours, clean and use dry nitrogen to dry up with isopropyl alcohol, obtain calcium titanium ore bed, its thickness is 400nm.Afterwards again by PC 60bM concentration is the PC of 20mg/mL 60dichloro-benzenes (ODCB) solution of BM is spun on above-mentioned calcium titanium ore bed under 1000rpm rotating speed, and gained film thickness is 5nm～15nm.Finally, 5 × 10 -4the aluminium that under handkerchief, vacuum evaporation 100nm is thick is as negative pole.Prepared device open circuit voltage under the simulated solar irradiation of every square centimeter of 100 milliwatt is 0.92 volt, and short circuit current is 13.93mA/cm 2, fill factor, curve factor is 60%, conversion efficiency is 7.77%.Fig. 6 has provided this device without irradiation and the current-voltage curve under the simulated solar irradiation of every square centimeter of 100 milliwatt.
Embodiment 5
Sputter is had to fluorine doping SnO 2(FTO) transparent conducting glass is used liquid detergent, running water, deionized water, acetone, isopropyl alcohol ultrasonic cleaning 2 times successively, nitrogen dries up, put into immediately UV ozone surface processing equipment (UVO) and process 15min, spin coating PEDOT:PSS solution under the rotating speed of 2000rpm, in air at 150 DEG C of temperature thermal annealing 15 minutes, obtain hole transmission layer, its thickness is 30nm left and right.Then by PbI 2concentration is the PbI of 300mg/mL 2precursor solution is directly spun on above-mentioned hole transmission layer under the rotating speed of 2000rpm, is then placed on hot platform, afterwards according to every 1cm 2gained PbI 2film approximately uses CH 3nH 3the usage ratio of I20mg, by CH 3nH 3i powder is evenly sprinkling upon gained PbI 2around film, cover with culture dish, at 150 DEG C of temperature, be incubated after 4 hours, clean and use dry nitrogen to dry up with isopropyl alcohol, obtain calcium titanium ore bed, its thickness is 400nm.Afterwards again by PC 60bM concentration is the PC of 20mg/mL 60dichloro-benzenes (ODCB) solution of BM is spun on above-mentioned calcium titanium ore bed under 1000rpm rotating speed, and gained film thickness is 5nm～15nm.Finally, 5 × 10 -4the aluminium that under handkerchief, vacuum evaporation 100nm is thick is as negative pole.Prepared device open circuit voltage under the simulated solar irradiation of every square centimeter of 100 milliwatt is 0.83 volt, and short circuit current is 16.1mA/cm 2, fill factor, curve factor is 57%, conversion efficiency is 7.72%.Fig. 7 has provided this device without irradiation and the current-voltage curve under the simulated solar irradiation of every square centimeter of 100 milliwatt.

Claims (10)

1. a preparation method for perovskite film, is characterized in that: use two step vacuum methodes, obtain the perovskite film of one deck densification.
2. the preparation method of a kind of perovskite film according to claim 1, is characterized in that, concrete grammar is as follows:
By lead halide PbX 2precursor solution is spin-coated on hole transmission layer, heating, drying, then lead halide film is moved in vacuum drying chamber, around lead halide film, sprinkle alkyl halide amine powder, cover culture dish lid, heating makes alkyl halide amine evaporate the organic metal halide calcium titanium ore bed that directly reacts the densification of generation one deck with lead halide.
3. the preparation method of a kind of perovskite film according to claim 2, is characterized in that: described X is Cl, Br or I.
4. the preparation method of a kind of perovskite film according to claim 2, is characterized in that: described lead halide is PbI 2, alkyl halide amine is CH 3nH 3i, organic metal halide calcium titanium ore bed is CH 3nH 3pbI 3.
5. the preparation method of a kind of perovskite film according to claim 2, is characterized in that: described lead halide PbX 2the solvent of precursor solution is one or both in DMF, gamma-butyrolacton.
6. a perovskite film, is characterized in that: described perovskite film is to be prepared by the method described in claim 1～5 any one claim.
7. the application process of a kind of perovskite film as claimed in claim 6, is characterized in that: described perovskite film is for the preparation of perovskite solar cell.
8. the application process of a kind of perovskite film according to claim 7, is characterized in that: in described perovskite solar cell, transparent conductive metal oxide skin(coating), hole transmission layer, perovskite film, electron transfer layer are connected in turn with metal electrode layer.
9. the application process of a kind of perovskite film according to claim 8, is characterized in that: the material of described hole transmission layer is one or more in high work function metal oxide, p-type conjugated polymer and p-type electric-conducting polymer.
10. the application process of a kind of perovskite film according to claim 8, is characterized in that: the material of described electron transfer layer is one or more in N-shaped metal oxide, fullerene and derivative thereof, N-shaped conjugated polymer and N-shaped conducting polymer.
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CN104250723A (en) * 2014-09-09 2014-12-31 许昌学院 Chemical method for in-situ large-area controlled synthesis of perovskite type CH3NH3PBI3 membrane material based on lead simple-substance membrane
CN104485423A (en) * 2014-11-28 2015-04-01 武汉工程大学 Planar structure perovskite photovoltaic cell with CrOx thin film prepared by solution method as anode interface layer and preparation method of planar structure perovskite photovoltaic cell
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CN104966763B (en) * 2015-07-20 2017-04-12 大连理工大学 Method of improving efficiency of perovskite solar cell
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