CN109449291A - Can on perovskite thin film solwution method process SnO2The preparation method of film - Google Patents
Can on perovskite thin film solwution method process SnO2The preparation method of film Download PDFInfo
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- CN109449291A CN109449291A CN201811290837.9A CN201811290837A CN109449291A CN 109449291 A CN109449291 A CN 109449291A CN 201811290837 A CN201811290837 A CN 201811290837A CN 109449291 A CN109449291 A CN 109449291A
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- H—ELECTRICITY
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- 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
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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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
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- 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 invention discloses it is a kind of can solwution method is processed on perovskite thin film SnO2The preparation method of film, by SnO2Nanocrystalline ultrasonic disperse forms the tin oxide colloidal solution that concentration is 0.05-1.5mol/L in isopropanol；In the preparation process of perovskite solar cell, tin oxide colloidal solution is transferred on perovskite thin film using spin-coating method, annealing removal solvent isopropanol obtains the SnO as electron transfer layer2Layer.The present invention thoroughly solves traditional SnO2Slurry, and can not be the problem of forming a film because having destruction to perovskite thin film on perovskite thin film.By optimised devices preparation process, the efficiency of perovskite solar cell is improved, widens inorganic SnO2Application range in perovskite battery, moreover, the research based on ito transparent electrode battery can also lay the foundation for the exploitation of laminated device.
Description
Technical field
The present invention relates to a kind of solar battery SnO2The preparation method of film, and in particular to one kind can be in perovskite thin film
The SnO of upper solwution method processing2The preparation method of film.
Background technique
Currently, perovskite solar battery is respectively as follows: (a) mesoscopic structure, (b) mainly by attached three kinds of structures shown in FIG. 1
Planar structure is just set, planar structure (c) is inverted.
Wherein, mesoscopic structure battery (a) is the current mainstream structure for obtaining high-efficiency battery, but due to electron transport material
TiO2It needs not utilize practical application by high-temperature process, and complex steps.
In formal slab construction (b), TiO2, SnO2It is the most frequently used and efficient electron transport material can be obtained, especially
It is SnO2, recent studies indicate that, performance is better than traditional TiO2.But hole transport material in the device of formal slab construction
Material is usually all using organic material, such as Spiro-OMeTAD, PTAA, these materials have certain photo absorption performance, unfavorable
In being used in laminated device.Although inorganic NiO can be used as hole mobile material, its preparation process and perovskite are thin
Film is incompatible.
In trans- slab construction device (c), common electron transport material is PCBM, is similarly organic material, there is suction
The problems such as light and poor stability.The structure of efficient laminated device top battery is all transconfiguration at present, due to electron-transport material
The preparation process needs of material are compatible with the preparation process of perovskite material, i.e., must not destroy perovskite thin film, cause many excellent
And stable electron transport material, such as SnO2It is nanocrystalline, it cannot be applied in trans- device.About can be by SnO in existing document2
It is still very few to be applied to trans- perovskite device research, substantially needs first to prepare a protective layer such as C60, PCBM etc.,
Then, SnO is prepared using the method for ALD2Film, technique are extremely complex.
Summary of the invention
The purpose of the present invention is to provide a kind of electron transport material that can be applied in trans- perovskite device and its
Preparation method fills up inorganic electronic transmission material SnO2The blank of solwution method direct formation of film at surface on perovskite thin film can not be utilized,
It lays the foundation for efficient trans- perovskite battery and the development of perovskite/silion cell.
The present invention is implemented as follows:
It is a kind of can on perovskite thin film solwution method process SnO2The preparation method of film is by SnO2Nanocrystalline ultrasound
It is scattered in isopropanol, forms the tin oxide colloidal solution that concentration is 0.05-1.5mol/L；
In the preparation process of trans- perovskite solar battery, tin oxide colloidal solution is transferred to calcium using spin-coating method
On titanium ore film, annealing removal solvent isopropanol obtains the SnO as electron transfer layer2Layer.
Further scheme is:
The SnO2It is nanocrystalline to be prepared via a method which to obtain:
The source Sn is dissolved, the Sn solution that molar concentration is 0.1-3mol/L is obtained；
Glacial acetic acid and ammonium hydroxide are added into Sn solution, the pH value of solution is adjusted to 7-10；Make temperature of the solution at 60-190 DEG C
It is reacted 10-90 minutes in degree, generates colloidal solution；
Ethyl alcohol or isopropanol are added in obtained colloidal solution and is sufficiently mixed, then, with 2000-10000r/min's
Revolving speed is centrifuged 5-20 minutes, removes upper solution, retains lower sediment；It washs followed by ethyl alcohol or isopropanol and obtains three times repeatedly
To SnO2It is nanocrystalline.
Further scheme is:
In Sn solution, for ethylene glycol as solvent, the source Sn is SnCl4·5H2O、SnCl2·2H2O, tin acetate (II) and acetic acid
One of tin (IV).
Further scheme is:
CH in the glacial acetic acid3NH in COOH and ammonium hydroxide3·H2The molar ratio of O is 1:1.5 to 1:5.
In order to absolutely prove technical solution of the present invention, below substantially by the preparation process of trans- perovskite solar battery
It is described as follows:
One layer of hole mobile material is prepared in FTO conductive substrates, NiOx, the CuGaO adulterated such as NiO, Cu2、CuFeO2、
CuInO2, one of CuO, CuSCN, CuI, PTAA, Spiro-TFB etc. or several.Then, perovskite thin film is prepared, such as
Methylamine based perovskite, carbonamidine based perovskite, can use one-step method or two-step method prepares perovskite thin film.It is then possible to sharp
With spin-coating method by the SnO of above-mentioned preparation2Nanocrystalline to be transferred on perovskite thin film, annealing removal solvent isopropanol passes through adjusting
Preparation process prepares the SnO of different-thickness2.Then, one layer of hole blocking layer of spin coating, such as BCP, acetylacetone,2,4-pentanedione zirconium (Zr
(acac)2), finally, electrode evaporation, such as Au, Ag, Cu or transparent electrode ITO, obtain trans- perovskite solar battery.
The present invention passes through the design and optimization of technique, is successfully prepared for based on SnO2Nanocrystalline electron transport material it is anti-
Formula perovskite device.The present invention is by optimization preparation process, obtained SnO2It is nanocrystalline that can be well dispersed in isopropanol molten
In agent.Since isopropanol there is no destructiveness to perovskite thin film, so that the SnO that we prepare2Dispersion liquid can be direct
It is spin-coated on perovskite thin film.Thoroughly solves traditional SnO2It can not be the problem of forming a film on perovskite thin film.Pass through optimizer
Part preparation process improves the efficiency of trans- perovskite solar cell, lays the foundation for the exploitation of laminated device.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of perovskite solar battery in the prior art；
Fig. 2 is the perovskite solar battery structure schematic diagram of preparation of the embodiment of the present invention.
Wherein, 1. electrode, 2. hole blocking layers, 3. electron transfer layers, 4. perovskite thin films, 5. hole transmission layers, 6.FTO
Conductive substrates
Specific embodiment
The present invention is further illustrated in the following with reference to the drawings and specific embodiments.
As shown in Fig. 2, one layer of hole transmission layer 5, the hole transport of hole transmission layer are prepared in FTO conductive substrates 6
Material, can be using NiOx, CuGaO such as NiO, Cu doping2、CuFeO2、CuInO2、CuO、CuSCN、CuI、PTAA、Spiro-
One of TFB etc. is several.Then, perovskite thin film 4 is prepared, such as methylamine based perovskite, carbonamidine based perovskite, Ke Yili
Film is prepared with one-step method or two-step method.It is then possible to using spin-coating method by the SnO of above-mentioned preparation2It is nanocrystalline to be transferred to calcium
On titanium ore film, annealing removal solvent isopropanol prepares the SnO of different-thickness by adjusting preparation process2, form electronics
Transmitting layer 3.Then, one layer of hole blocking layer 2 of spin coating, such as BCP, acetylacetone,2,4-pentanedione zirconium (Zr (acac)2), finally, electrode evaporation 1,
Such as Au, Ag, Cu or transparent electrode ITO obtain trans- perovskite solar battery.
The present invention is further detailed with specific several embodiments below.
1. using NiO as hole mobile material, using MA based perovskite as light absorbent, SnO2It is nanocrystalline to be passed as electronics
Defeated material, for BCP as hole blocking layer, Au is electrode.
2. using Cu-NiOx as hole mobile material, using MA based perovskite as light absorbent, SnO2It is nanocrystalline to be used as electricity
Sub- transmission material, for BCP as hole blocking layer, Au is electrode.
3. using Cu-NiOx as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be used as electricity
Sub- transmission material, for BCP as hole blocking layer, Au is electrode.
4. using CuGaO2 as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be used as electricity
Sub- transmission material, Zr (acac)2As hole blocking layer, Au is electrode.
5. using CuO as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be passed as electronics
Defeated material, Zr (acac)2, Au is electrode.
6. using CuI as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be passed as electronics
Defeated material, Zr (acac)2, Au is electrode.
7. using CuSCN as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be used as electronics
Transmission material, Zr (acac)2, Au is electrode.
8. using PTAA as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be used as electronics
Transmission material, Zr (acac)2, Ag is electrode.
9. using PTAA as hole mobile material, using FA based perovskite as light absorbent, SnO2It is nanocrystalline to be used as electronics
Transmission material, Zr (acac)2, ITO is electrode.Battery can two-sided receipts light at this time, it can is applied to the top electricity of laminated device
Pond.
10., using MA based perovskite as light absorbent, PCBM is as electron-transport material using NiO as hole mobile material
Material, for BCP as hole blocking layer, Ag is electrode.(comparison)
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that those skilled in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will fall in principle disclosed in the present application
Within scope and spirit.
Claims (4)
1. one kind can on perovskite thin film solwution method process SnO2The preparation method of film, it is characterised in that: by SnO2Nanometer
Brilliant ultrasonic disperse forms the tin oxide colloidal solution that concentration is 0.05-1.5mol/L in isopropanol；
In the preparation process of perovskite solar battery, tin oxide colloidal solution is transferred to perovskite thin film using spin-coating method
On, annealing removal solvent isopropanol obtains the SnO as electron transfer layer2Layer.
2. according to claim 1 can on perovskite thin film solwution method process SnO2The preparation method of film, feature exist
In:
The SnO2It is nanocrystalline to be prepared via a method which to obtain:
The source Sn is dissolved, the Sn solution that molar concentration is 0.1-3mol/L is obtained；
Glacial acetic acid and ammonium hydroxide are added into Sn solution, the pH value of solution is adjusted to 7-10；Make solution in 60-190 DEG C of temperature
Reaction 10-90 minutes generates colloidal solution；
Ethyl alcohol or isopropanol are added in obtained colloidal solution and is sufficiently mixed, then, with the revolving speed of 2000-10000r/min
Centrifugation 5-20 minutes removes upper solution, retains lower sediment；It washs followed by ethyl alcohol or isopropanol and obtains three times repeatedly
SnO2It is nanocrystalline.
3. according to claim 2 can on perovskite thin film solwution method process SnO2The preparation method of film, feature exist
In:
In Sn solution, for ethylene glycol as solvent, the source Sn is SnCl4·5H2O、SnCl2·2H2O, tin acetate (II) and tin acetate
One of (IV).
4. according to claim 2 can on perovskite thin film solwution method process SnO2The preparation method of film, feature exist
In:
CH in the glacial acetic acid3NH in COOH and ammonium hydroxide3·H2The molar ratio of O is 1:1.5 to 1:5.
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| CN201811290837.9A CN109449291A (en) | 2018-10-31 | 2018-10-31 | Can on perovskite thin film solwution method process SnO2The preparation method of film |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708302A (en) * | 2020-12-29 | 2021-04-27 | 无锡极电光能科技有限公司 | Electron transport layer coating ink and preparation method and application thereof |
| CN113745410A (en) * | 2021-08-24 | 2021-12-03 | 上海工程技术大学 | Based on P type CuNiO2Preparation method of thin film perovskite solar cell |
| CN116914031A (en) * | 2023-09-11 | 2023-10-20 | 西安电子科技大学 | Preparation method of semitransparent and trans-type all-inorganic perovskite solar cell |
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| CN104157788A (en) * | 2014-08-19 | 2014-11-19 | 武汉大学 | Perovskite film photovoltaic cell based on SnO2 and preparation method thereof |
| US20170133163A1 (en) * | 2015-11-06 | 2017-05-11 | The University Of Massachusetts | Perovskite-containing solar cells comprising fulleropyrrolidine interlayers |
| CN107742673A (en) * | 2017-09-22 | 2018-02-27 | 苏州协鑫纳米科技有限公司 | Electron transfer layer and preparation method thereof, perovskite battery and preparation method thereof |
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Patent Citations (3)
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| CN104157788A (en) * | 2014-08-19 | 2014-11-19 | 武汉大学 | Perovskite film photovoltaic cell based on SnO2 and preparation method thereof |
| US20170133163A1 (en) * | 2015-11-06 | 2017-05-11 | The University Of Massachusetts | Perovskite-containing solar cells comprising fulleropyrrolidine interlayers |
| CN107742673A (en) * | 2017-09-22 | 2018-02-27 | 苏州协鑫纳米科技有限公司 | Electron transfer layer and preparation method thereof, perovskite battery and preparation method thereof |
Non-Patent Citations (1)
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| 郑金凤等: "水热合成纳米 SnO2的制备与表征", 《粉末冶金材料科学与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112708302A (en) * | 2020-12-29 | 2021-04-27 | 无锡极电光能科技有限公司 | Electron transport layer coating ink and preparation method and application thereof |
| CN113745410A (en) * | 2021-08-24 | 2021-12-03 | 上海工程技术大学 | Based on P type CuNiO2Preparation method of thin film perovskite solar cell |
| CN113745410B (en) * | 2021-08-24 | 2023-09-29 | 上海工程技术大学 | Based on P type CuNiO 2 Preparation method of perovskite solar cell of thin film |
| CN116914031A (en) * | 2023-09-11 | 2023-10-20 | 西安电子科技大学 | Preparation method of semitransparent and trans-type all-inorganic perovskite solar cell |
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Application publication date: 20190308 |