CN109273604A - A kind of perovskite Cs used for solar batteries3BixIn2-xI9The preparation method of photoactive layer - Google Patents
A kind of perovskite Cs used for solar batteries3BixIn2-xI9The preparation method of photoactive layer Download PDFInfo
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Abstract
A kind of perovskite Cs used for solar batteries3BixIn2‑xI9The preparation method of photoactive layer, belongs to nano material and technical field of solar batteries.Cs3BixIn2‑xI9Photoactive layer preparation method: Cs3BixIn2‑xI9Photoactive layer is prepared by a step solution spin-coating method, by CsI, BiI3And InI3Powder, which is dispersed in DMF/DMSO mixed solution, forms precursor solution, and spin coating forms perovskite thin film on the glass substrate, by heating anneal；With Cs3BixIn2‑xI9Configured solution is spin-coated on Cs for the preparation of calcium titanium ore bed solar battery: configuration hole transmission layer solution (70 ㎎ spiro-MeoTAD, 17 μ l lithium salts, 28 μ l4- tert .-butylpyridines, 1ml chlorobenzene)3BixIn2‑xI9Perovskite surface after standing 12 hours, sample is placed in the silver-colored vacuum coater of steaming, the silver electrode of one layer of 60nm is deposited；After the completion of vapor deposition, being clashed light anode with butyrolactone can be obtained perovskite solar battery.Advantage: perovskite solar battery of the invention has extremely strong stability, and low in cost, preparation process is simple, environmental-friendly, can be carried out large-scale production.
Description
Technical field
The present invention relates to a kind of nano material and technical field of solar batteries, especially a kind of perovskite solar battery
Use Cs3BixIn2-xI9The preparation method of photoactive layer.
Background technique
Solar energy is the basic source of all energy (renewable energy and non-renewable energy resources) on the earth, inexhaustible use
It is inexhaustible, in new energy field be in leading position.Solar battery is exactly that luminous energy is directly converted to electricity using photovoltaic effect
The device of energy.Wherein, silicon solar cell is to develop maturation the most in the photovoltaic cells, but need in silicon raw material purification process big
Energy consumption is measured, so that the cost of silicon solar cell is high.
In recent years, novel perovskite solar battery was announced to the world splendidly, and battery efficiency also soars all the way, from 2009
3.8% rises to 22.1% in 2017.Perovskite battery is high with theoretical light photoelectric transformation efficiency, at low cost and preparation process is simple
The features such as single, causes the extensive concern of scientific circles, becomes one of the hot spot in current photoelectric conversion material field, is silica-based solar
One of ideal replacer of battery.
Perovskite solar battery has wide market application prospect, but not yet realizes industrialization at present, and there are many skills
Art problem need further solve and it is perfect.Perovskite solar battery is generally by conductive substrates (FTO), electron transfer layer, light
A few part compositions such as active layer and hole transmission layer and metal electrode.Photoactive layer is perovskite solar battery " heart ",
Common material is the organic-inorganic mixing halogenation lead compound ABX with perovskite structure3(A=CH3NH3 +,CH(NH2)2 +, B
=Pb2+,Sn2+, X=Cl, Br, I), such material is with high-efficient to visible absorption, carrier mobility is high, excitation electronics
The features such as service life length and long transmission distance.At the same time, the battery device performance prepared is unstable, constrains perovskite battery
Large-scale production and commercialization.In addition, the presence of Pb element can cause environmental pollution, cause damages to human health.It seeks
Seek the light active material substitution organic-inorganic mixing halogenation lead compound ABX of a kind of green non-pollution, efficient stable3Very must be
It wants.
Summary of the invention
The invention aims to provide a kind of perovskite Cs used for solar batteries3BixIn2-xI9The preparation side of photoactive layer
Method, it is intended to reduce the performance of the manufacturing cost of solar battery and the stability of optimization solar battery and photoelectric conversion efficiency.
The purpose of the present invention is solved by technical solution below.
Cs3BixIn2-xI9Photoactive layer preparation method: Cs3BixIn2-xI9Photoactive layer passes through a step solution spin coating legal system
It is standby, by CsI, BiI3And InI3Powder is dispersed in DMF/DMSO mixed solution and forms precursor solution, is spin-coated on substrate of glass
On, perovskite thin film is formed by heating anneal.
Concrete technology the following steps are included:
(1) one piece of electro-conductive glass (FTO) is taken, the sheet glass of the size of needs is cut into glass cutter；Successively by electro-conductive glass
It is put into deionized water, isopropanol, alcohol ultrasonic cleaning 30min, with being dried with nitrogen after alcohol washes；
(2) dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium are mixed to form compacted zone solution magnetic agitation 20~30
Minute；
(3) by compacted zone solution spraying on electro-conductive glass, 500 DEG C of annealing；
(4) by CsI, BiI of different ratio3And InI3It is dissolved in DMF/DMSO mixed solution, is placed in constant temperature blender with magnetic force
It heating stirring 50~60 minutes, is formed and is uniformly mixed perovskite precursor solution；
(5) the perovskite precursor solution of 60 μ l is coated on compacted zone, is placed on sol evenning machine and rotates, then 120 DEG C
Annealing can be obtained Cs in 15 minutes3BixIn2-xI9Perovskite thin film.
In step (2), the proportional volume ratio of dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium is 100:1.
In step (4), CsI, BiI of different ratio3And InI3Molal weight ratio is 3:X:2-X.
In step (5), 60 μ l perovskite precursor solutions are by the precursor solution that configures in step (4)；Sol evenning machine turns
Fast 5000r/min, time 30s.
With Cs3BixIn2-xI9For the preparation of calcium titanium ore bed solar battery:
Hole transmission layer solution is configured, 70 ㎎ spiro-MeoTAD are dissolved in 1ml chlorobenzene, and 17 μ l lithium salts, 28 μ are added
L4- tert .-butylpyridine is spin-coated on Cs as additive, by configured solution3BixIn2-xI9Perovskite surface stands 12 hours
Afterwards, sample is placed in the silver-colored vacuum coater of steaming, the silver electrode of one layer of 60nm is deposited；It is with butyrolactone that light is positive after the completion of vapor deposition
Pole, which clashes, can be obtained perovskite solar battery.
Beneficial effect, as the above scheme is adopted, this method can accurately control Cs3BixIn2-xI9The ruler of nano particle
Very little, pattern, and the photoactive film's thickness prepared is uniform, surface coverage is high, contacts with adjacent interfaces well.The active layer
Feature is mainly reflected in perovskite absorbent layer structure, and the layer is between electron transfer layer and hole transmission layer, by diameter range
It is closely packed together in 50~100nm nanometer sheet, the smooth imporosity of surface topography, fine and close Cs3BixIn2-xI9Photolytic activity
On the one hand layer is conducive to fully absorbing for sunlight；On the other hand the compound of electronics and hole is conducive to prevent, is avoided cell performance
The decaying of energy.The perovskite solar battery efficiency of assembling has reached 1.17%, with CH3NH3PbI3Perovskite solar energy is compared,
Stability test is improved significantly, and at 2000 hours, the photoelectric conversion efficiency of battery was maintained at 85% or more.This solar energy
Battery has manufacturing cost cheap, and preparation process is simple, advantages of environment protection, can be mass produced.
The full-inorganic halogen compound Cs of structure of double perovskite3BixIn2-xI9With preparing simple, environmentally protective (no Pb member
Element), the features such as object is mutually stable and photoelectric properties are excellent.The present invention is with Cs3BixIn2-xI9A system is provided for light active material
Standby low cost, the new way of high-performance and high stability perovskite solar battery.
Reduce the manufacturing cost of solar battery and the stability and photoelectric conversion efficiency for optimizing solar battery
Performance has reached the purpose of the present invention.
Advantage: the present invention is first uniformly to mix three kinds of raw materials by magnetic agitation and obtain precursor solution, then pass through
One step spin-coating method prepares Cs3BixIn2-xI9Photoactive layer.It the advantage is that preparation process is simple and safe, respectively walked in preparation process
Suddenly poisonous and harmful substance is not generated.Perovskite solar battery of the invention has extremely strong stability, low in cost, preparation
Simple process, advantages of environment protection can be mass produced.
Detailed description of the invention
Fig. 1 is prepared by the present invention with Cs3BixIn2-xI9For the meso-hole structure perovskite solar battery knot of photoactive layer
Structure illustraton of model.
Fig. 2 is present invention preparation Cs3BixIn2-xI9The XRD spectrum of photoactive layer.
Fig. 3 is present invention preparation Cs3BixIn2-xI9The shape appearance figure that perovskite thin film is observed under scanning electron microscope.
Fig. 4 is present invention preparation Cs3BixIn2-xI9The uv-visible absorption spectroscopy figure of perovskite thin film.
Fig. 5 is the J-V curve graph that the present invention prepares solar battery.
In figure, 1. silver electrode；Two fluorenes of 2,2', 7,7'- tetra- 2. [N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell；③
Cs3BixIn2-xI9；4. poriferous titanium dioxide；5. compact titanium dioxide；6. electro-conductive glass.
Specific embodiment
Cs of the invention3BixIn2-xI9Photoactive layer preparation method: Cs3BixIn2-xI9Photoactive layer is revolved by a step solution
Coating preparation, by CsI (cesium iodide), BiI3(bismuth iodide) and InI3It is molten that (indium triiodide) powder is dispersed in DMF/DMSO mixing
Precursor solution is formed in liquid, spin coating forms perovskite thin film on the glass substrate, by heating anneal.
DMF (N,N-dimethylformamide)/DMSO (dimethyl sulfoxide) mixed solution: N,N-dimethylformamide and diformazan
Base sulfoxide is mixed with the ratio of 13:1.
Concrete technology the following steps are included:
(1) one piece of electro-conductive glass (FTO) is taken, the sheet glass of the size of needs is cut into glass cutter；Successively by electro-conductive glass
It is put into deionized water, isopropanol, alcohol ultrasonic cleaning 30min, with being dried with nitrogen after alcohol washes；
(2) dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium are mixed to form compacted zone solution magnetic agitation 20~30
Minute；
(3) by compacted zone solution spraying on electro-conductive glass, 500 DEG C of annealing；
(4) by CsI, BiI of different ratio3And InI3It is dissolved in DMF/DMSO mixed solution, is placed in constant temperature blender with magnetic force
It heating stirring 50~60 minutes, is formed and is uniformly mixed precursor solution；
(5) the perovskite precursor solution of 60 μ l is coated on compacted zone, is placed on sol evenning machine and rotates, then 120 DEG C
Annealing can be obtained Cs in 15 minutes3BixIn2-xI9Perovskite thin film.
In step (2), the proportional volume ratio of dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium is 100:1.
In step (4), CsI, BiI of different ratio3And InI3Molal weight ratio is 3:X:2-X.
In step (5), 60 μ l perovskite precursor solutions are by the precursor solution that configures in step (4)；Sol evenning machine turns
Fast 5000r/min, time 30s.
With Cs3BixIn2-xI9For the preparation of calcium titanium ore bed solar battery:
70 ㎎ spiro-MeoTAD are dissolved in 1ml chlorobenzene by configuration hole transmission layer solution, and 17 μ l lithium salts, 28 μ l4- are added
Tert .-butylpyridine is spin-coated on Cs as additive, by configured solution3BixIn2-xI9Perovskite surface, after standing 12 hours,
Sample is placed in the silver-colored vacuum coater of steaming, the silver electrode of one layer of 60nm is deposited；After the completion of vapor deposition, light anode is wiped with butyrolactone
It can be obtained perovskite solar battery out.
Spiro-MeoTAD (Chinese: 2,2', 7,7'- tetra- [N, N- bis- (4- methoxyphenyl) amino] -9,9'- spiral shell
Two fluorenes).
Combined with specific embodiments below, technical solution of the present invention is described further.It should be understood that these embodiments are only
For illustrating the present invention rather than limiting the scope of the invention.In addition, it should also be understood that, without departing from spirit and scope of the invention to this
Invention carries out various changes and modifications will be apparent from for a person skilled in the art, and such equivalent forms are equally fallen within
The application says attached claims limited range.
Embodiment 1: meso-hole structure perovskite solar battery.
The meso-hole structure Cs of the present embodiment3BixIn2-xI9The specific steps of the preparation method of perovskite solar battery are such as
Under:
(1) prepared by compacted zone: taking one piece of electro-conductive glass (FTO), the sheet glass of the size of needs is cut into glass cutter.It will lead
Electric glass is sequentially placed into deionized water, 95% dehydrated alcohol, isopropanol, is cleaned by ultrasonic 30min in 99% dehydrated alcohol, and nitrogen is blown
It is dry.Dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium are mixed to form compacted zone solution magnetic agitation 20~30 minutes, led to
It crosses spray pyrolysis and sprays layer of titanium dioxide film in conducting surface, be put into 500 DEG C of annealing 1h of Muffle furnace later and form Anatase
Titanium dioxide.
(2) mesoporous layer preparation: by 18NRT and the mesoporous slurry of dehydrated alcohol (1:3.5) uniform mixed configuration, then using even
For glue machine by slurry for rotary coating on titanium dioxide dense layer, revolving speed 5000r/min, rotational time 30s are placed on thermal station later
Upper 100 DEG C of drying, the porous layer after drying is put into program furnace and is annealed, and 500 DEG C of annealing temperature, the time 1 hour.
In Fig. 2, with the increase of In content, the diffraction maximum of perovskite material increases, and improves calcium titanium to a certain extent
The crystallinity of mine.Particle diameter range is 200~300 nanometers, and rough degree is very big, the catalysis to electrode catalyst layer
Position will increase, and be conducive to the transmission of electronics.
(3) preparation of calcium titanium ore bed: by a certain amount of CsI, BiI3And InI3It is dissolved in DMF/DMSO mixed solution, is placed in perseverance
Heating stirring 50~60 minutes in warm magnetic stirring apparatus form and are uniformly mixed precursor solution, by a certain amount of perovskite forerunner
Liquid solution is spin-coated on porous layer, revolving speed 5000r/min, rotational time 30s；Then 120 DEG C of annealing can be obtained for 15 minutes
Cs3BixIn2-xI9Perovskite thin film.
In Fig. 3, comprising: Fig. 3 (a), Fig. 3 (b), Fig. 3 (c), Fig. 3 (d) and Fig. 3 (e)；In replaces perovskite after the Bi of part thin
Film becomes more uniform densification, to reduce the compound of hole and electronics.
In Fig. 4, Cs3BixIn2-xI9The corresponding absorption band edge of perovskite is about 580nm, while In content can excessively improve calcium
The band gap of titanium ore.
(4) vapor deposition of the preparation of hole transmission layer and silver electrode
By 70mg Spiro-MeoTAD, double fluoroform sulfanilamide (SN) imide li solution of 20 μ L and the 4-TBP of 28 μ L are molten
Liquid is mixed to form hole transmission layer solution；The solution prepared is spin-coated on perovskite surface, rotation speed 3500r/min, time
30s.12 hours are stood, known sample is placed in vacuum coating equipment, the silver electrode of one layer of 60nm is deposited.After the completion of vapor deposition, use
Butyrolactone, which clashes light anode, can be obtained Cs3BixIn2-xI9Perovskite solar battery.It is prepared cell performance in Fig. 5
Can: know that battery efficiency reaches 1.17% by I-V test.
Claims (6)
1. a kind of perovskite Cs used for solar batteries3BixIn2-xI9The preparation method of photoactive layer, it is characterized in that: Cs3BixIn2- xI9Photoactive layer preparation method: Cs3BixIn2-xI9Photoactive layer is prepared by a step solution spin-coating method, by CsI, BiI3And InI3
Powder, which is dispersed in DMF/DMSO mixed solution, forms precursor solution, and spin coating on the glass substrate, is formed by heating anneal
Perovskite thin film.
2. a kind of perovskite Cs used for solar batteries according to claim 13BixIn2-xI9The preparation method of photoactive layer,
It is characterized in that: concrete technology the following steps are included:
(1) one piece of electro-conductive glass (FTO) is taken, the sheet glass of the size of needs is cut into glass cutter；Electro-conductive glass is sequentially placed into
Deionized water, isopropanol, alcohol are cleaned by ultrasonic 30min, with being dried with nitrogen after alcohol washes；
(2) dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium are mixed to form 20~30 points of compacted zone solution magnetic agitation
Clock；
(3) by compacted zone solution spraying on electro-conductive glass, 500 DEG C of annealing；
(4) by CsI, BiI of different ratio3And InI3It is dissolved in DMF/DMSO mixed solution, is placed in constant temperature blender with magnetic force and heats
Stirring 50~60 minutes forms and is uniformly mixed precursor solution；
(5) the perovskite precursor solution of 60 μ l is coated on compacted zone, is placed on sol evenning machine and rotates, then 120 DEG C of annealing
It can be obtained Cs within 15 minutes3BixIn2-xI9Perovskite thin film.
3. a kind of perovskite Cs used for solar batteries according to claim 23BixIn2-xI9The preparation method of photoactive layer,
It is characterized in that: the proportional volume ratio of dehydrated alcohol and diisopropoxy bis-acetylacetonate titanium is 100:1 in step (2).
4. a kind of perovskite Cs used for solar batteries according to claim 23BixIn2-xI9The preparation method of photoactive layer,
It is characterized in that: in step (4), CsI, BiI in solution3And InI3Molal weight ratio is 3:X:2-X.
5. a kind of perovskite Cs used for solar batteries according to claim 23BixIn2-xI9The preparation method of photoactive layer,
It is characterized in that: in step (5), 60 μ l perovskite precursor solutions are by the precursor solution that configures in step (4)；Sol evenning machine turns
Fast 5000r/min, time 30s.
6. being based on a kind of perovskite Cs used for solar batteries described in claim 13BixIn2-xI9Photoactive layer prepares solar energy
The method of battery, it is characterized in that: with Cs3BixIn2-xI9For the preparation of calcium titanium ore bed solar battery:
Hole transmission layer solution is configured, 70 ㎎ spiro-MeoTAD are dissolved in 1ml chlorobenzene, and 17 μ l lithium salts, 28 μ uncles l4- are added
Butyl-pyridinium is spin-coated on Cs as additive, by configured solution3BixIn2-xI9It perovskite surface will after standing 12 hours
Sample is placed in the silver-colored vacuum coater of steaming, and the silver electrode of one layer of 60nm is deposited；After the completion of vapor deposition, light anode is clashed with butyrolactone
It can be obtained perovskite solar battery.
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| CN111341916A (en) * | 2020-03-05 | 2020-06-26 | 苏州大学 | Indium compound doped perovskite film, preparation method and application thereof |
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| CN106082329A (en) * | 2016-06-12 | 2016-11-09 | 上海科技大学 | A kind of containing bismuth and the semi-conducting material of halogen and preparation thereof and the method for analysis |
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