CN109166971A - Enhance the perovskite solar cell preparation method of moisture resistance stability and photoelectric properties - Google Patents
Enhance the perovskite solar cell preparation method of moisture resistance stability and photoelectric properties Download PDFInfo
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- CN109166971A CN109166971A CN201810993533.2A CN201810993533A CN109166971A CN 109166971 A CN109166971 A CN 109166971A CN 201810993533 A CN201810993533 A CN 201810993533A CN 109166971 A CN109166971 A CN 109166971A
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Abstract
The invention discloses a kind of enhancing moisture resistance stability and the perovskite solar cell preparation methods of photoelectric properties.The first spin coating PEDOT:PSS solution in etched ITO electro-conductive glass substrate;Prepare PbI24- tert .-butylpyridine is added to PbI by solution2The sufficiently obtained PbI of heating stirring mixing in solution2- tBP precursor solution, is spun in substrate of glass, and porous and hydrophobic PbI is made2- tBP film;Spin coating CH again3NH3I and PbI2- tBP reacts to obtain CH3NH3PbI3- tBP functional layer;It is then spin coated onto one layer of PC61BM prepares electron transfer layer;One layer of Ag films are finally deposited on it, solar cell device is made.Present invention process is simply repeatable, and raw material is easy to get, cost is controllable, and the moisture resistance stability and photoelectric properties of made device are significantly improved, and very well satisfies perovskite solar cell in the practical application request of photovoltaic art.
Description
Technical field
The present invention relates to the preparation methods of the perovskite solar cell device in photovoltaic art, more particularly to a kind of enhancing
The perovskite solar cell preparation method of moisture resistance stability and photoelectric properties.
Background technique
It is increasingly increased in global energy consumption, today that environmental pollution is on the rise, solar energy resources are huge latent due to its
Power and spatter property and be concerned, be inexhaustible, nexhaustible green energy resource.Perovskite solar cell is a kind of novel
Photovoltaic device can be prepared compared with traditional silicon solar cell by solwution method, avoid high temperature and high vacuum process, production
Technique is more easy, and performance and cost have more advantage, and can be made into flexible device, its progress is very swift and violent in recent years, light
Electrotransformation efficiency hits new peak repeatly, has attracted the extensive concern of global numerous researchers and industrial circle, has become the forward position of photovoltaic art
Hot spot.
However, stability, which becomes, hinders the big problem of perovskite solar cell commercialized one, there are still not for current device
Moisture resistance and lead to CH3NH3I meets steam and is easy the disadvantages of decomposing, and limits its practical application.In consideration of it, the present invention innovatively will
TBP (4- tert .-butylpyridine) additive is introduced into the preparation process of perovskite battery.TBP is added to PbI2In, the PbI of spin coating2
Film is conducive to improve perovskite CH by pore-creating3NH3PbI3Crystallization and pattern, to improve the photoelectric efficiency of device;And by
Tert-butyl in tBP molecule has hydrophobic property, and appropriate remaining tBP can also play preferable hydrophobic effect, can effectively hinder
Every destruction of the steam in air to perovskite crystal structure, the humidity-proof ability and stability of device are increased.Pass through this side
Method, synchronizing realizes the beneficial effect for promoting perovskite solar cell moisture resistance stability and photoelectric properties, improves using valence
Value.
Summary of the invention
In order to solve the problems, such as background technique, the object of the present invention is to provide a kind of enhancing moisture resistance stability and
The perovskite solar cell preparation method of photoelectric properties.With PbI2It is dissolved in DMF for raw material, then adds tBP and PbI is made2- tBP forerunner
Liquid solution is prepared for PbI using spin coating2- tBP film, and by PbI2- tBP film and CH3NH3I reaction, it is good to have obtained pattern
CH3NH3PbI3- tBP film, to improve device stability and photoelectric properties.
The technical solution adopted by the present invention as shown in Figure 1, i.e. the step of preparation method are as follows:
1) tin indium oxide (ITO) electro-conductive glass is cleaned, is respectively cleaned with acetone, deionized water and dehydrated alcohol respectively, nitrogen
Drying, then it is handled in UV ozone atmosphere;
2) the poly- 3,4-rthylene dioxythiophene of spin coating (PEODT): kayexalate (PSS) solution takes clear in step 1)
Washed tin indium oxide (ITO) electro-conductive glass is fixed on spin coating instrument turntable, and on tin indium oxide (ITO) conductive glass surface, dynamic is revolved
PEODT:PSS solution is applied, preparation forms hole transmission layer;
3) PbI is prepared2- tBP precursor solution, by PbI2Powder is dissolved in n,N-Dimethylformamide (DMF) solution,
TBP (4- tert .-butylpyridine) solution is added, heating stirring is uniform;
4) spin coating PbI2The sample prepared in step 2) is added dropwise in the solution prepared in step 3) by-tBP precursor solution
On under specific rotation speeds carry out spin coating for a period of time, after spin coating take out in the heating plate of specific temperature heat a period of time,
Sample surfaces generate porous and hydrophobic PbI2- tBP film;
5) CH is prepared3NH3I solution, by CH3NH3I dissolution of crystals is in isopropanol, magnetic agitation under room temperature;
6)CH3NH3PbI3Sample prepared by step 4) is placed on spin coating instrument turntable, a dropping step 5 by-tBP film preparation)
The CH of middle preparation3NH3I solution just starts to rotate after static a period of time, carries out spin coating for a period of time under specific rotation speeds, spin coating
It takes out afterwards and heats a period of time in the heating plate of specific temperature, generate CH in sample surfaces3NH3PbI3- tBP film;
7) PC is prepared61BM solution, by PC61BM powder is dissolved in chlorobenzene, magnetic agitation under room temperature;
8) PC is prepared61BM layers, by step 6) prepare sample be placed on spin coating instrument turntable, a dropping step 7) in prepare it is molten
Liquid carries out spin coating for a period of time under specific rotation speeds, takes out after spin coating and heats a period of time in the heating plate of specific temperature,
Sample surfaces generate PC61BM film, as electron transfer layer;
9) silver metal electrodes are deposited, sample prepared by step 8) is placed in vacuum evaporation instrument, vapor deposition a layer thickness is 80
Perovskite solar cell device is made in~120 nanometers of silver electrode.
In the step 2), on tin indium oxide (ITO) conductive glass surface, dynamic spin coating PEODT:PSS solution specifically includes three
A stage: the first stage is 1800~2200 revs/min, is turned 8~12 seconds;Second stage is 4800~5200 revs/min and turns 20
~40 seconds;Phase III is 20~60 minutes in 115~125 degrees Celsius of lower heating times.First and second stage rotary courses
In PEODT:PSS solution spin coating is uninterruptedly added dropwise.
In the step 3), PbI2The concentration for being dissolved in DMF is 1~1.4 mole/milliliter, tBP:PbI2The volume ratio of solution is
1:50~1:10, heating stirring temperature are 65~75 degrees Celsius.
In the step 4), PbI2The spin speed of-tBP precursor solution is 4300~4700 revs/min, spin-coating time
It is 20~40 seconds, heating temperature is 65~75 degrees Celsius, and heating time is 10~20 minutes.
In the step 6), CH3NH3The quiescent time of I solution is 15~25 seconds, and spin speed is 3500~4500 revs/min
Clock, spin-coating time are 20~40 seconds, and heating temperature is 90~110 degrees Celsius, and heating time is 20~40 minutes.
Preferably, the present invention is implemented in the following ways:
1) tin indium oxide (ITO) electro-conductive glass is cleaned, respectively cleans 15 points with acetone, deionized water and dehydrated alcohol respectively
Clock is dried with nitrogen, then it is handled 15 minutes in UV ozone atmosphere;
2) the poly- 3,4-rthylene dioxythiophene of spin coating (PEODT): kayexalate (PSS) solution takes clear in step 1)
Washed tin indium oxide (ITO) electro-conductive glass is fixed on spin coating instrument turntable, and on tin indium oxide (ITO) conductive glass surface, dynamic is revolved
Apply PEODT:PSS solution;
Dynamic spin coating process are as follows: spin coating instrument rotary speed is adjusted to 2000 revs/min and is first turned 10 seconds, then become 5000 turns/
Minute turn 30 seconds, uninterrupted simultaneously in two spin coating process that PEODT:PSS solution is added dropwise, being taken out after spin coating in temperature is 120 to take the photograph
It is heated 40 minutes in the heating plate of family name's degree;
3) PbI is prepared2- tBP precursor solution, by PbI2Powder is dissolved in n,N-Dimethylformamide (DMF) solution,
TBP (4- tert .-butylpyridine) solution is added, it is uniform in 70 degrees Celsius of lower heating stirrings;
4) spin coating PbI2The sample prepared in step 2) is added dropwise in the solution prepared in step 3) by-tBP precursor solution
On, spin speed is 4500 revs/min, and spin-coating time is 30 seconds, is taken out in the heating plate that temperature is 70 degrees Celsius after spin coating
Heating 15 minutes generates PbI in sample surfaces2- tBP film;
5) CH is prepared3NH3I solution, every 12 milligrams of CH3NH3I dissolution of crystals is in 1 milliliter of isopropanol, and magnetic force stirs under room temperature
It mixes 24 hours;
6)CH3NH3PbI3Sample prepared by step 4) is placed on spin coating instrument turntable, a dropping step 5 by-tBP film preparation)
The CH of middle preparation3NH3I solution starts to rotate after static 20 seconds, and spin coating 30 seconds, take out after spin coating under 4000 revs/min of revolving speeds
It is heated 30 minutes in the heating plate that temperature is 100 degrees Celsius, generates CH in sample surfaces3NH3PbI3- tBP film;
7) PC is prepared61BM solution, every 20 milligrams of PC61BM powder is dissolved in 1 milliliter of chlorobenzene, magnetic agitation 24 under room temperature
Hour;
8) PC is prepared61BM layers, by step 6) prepare sample be placed on spin coating instrument turntable, a dropping step 7) in prepare it is molten
Liquid, spin speed are 2000 revs/min, and spin-coating time is 30 seconds, are taken out in the heating plate that temperature is 80 degrees Celsius after spin coating
Heating 30 minutes generates PC in sample surfaces61BM film;
9) silver metal electrodes are deposited, sample prepared by step 8) is placed in vacuum evaporation instrument, vapor deposition a layer thickness is 80
Perovskite solar cell device is made in~120 nanometers of silver electrode.
The method of the present invention is unique, technology is novel, and simple process is repeatable, and raw material is easy to get, cost is controllable, passes through determining for tBP
Amount addition and the finely regulating to film morphology, make the moisture resistance stability of device and photoelectric properties be significantly improved, very well
Ground meets perovskite solar cell in the practical application request of photovoltaic art.
The invention has the advantages that:
1) perovskite solar cell that the present invention successfully prepares, raw material are easy to get, and simple process is repeatable, operability
By force;
2) perovskite solar cell that the present invention successfully prepares, moisture resistance stability are significantly improved.
3) perovskite solar cell that the present invention successfully prepares, photoelectric conversion efficiency are highly improved.
Detailed description of the invention
Fig. 1 is the flow diagram of perovskite solar cell device prepared by embodiment 1.
Fig. 2 is CH prepared by embodiment 13NH3PbI3Film and CH3NH3PbI3The X-ray diffraction (XRD) of-tBP film is composed
Figure.
Fig. 3 is CH prepared by embodiment 13NH3PbI3Film and CH3NH3PbI3The field emission scanning electron microscope of-tBP film
(FESEM) photo.
Fig. 4 is perovskite solar device VA characteristic curve figure prepared by embodiment 1 and does not add the device volt-ampere of tBP special
Linearity curve figure.
Fig. 5 is perovskite solar device normalization transfer efficiency statistical chart and the device for not adding tBP prepared by embodiment 1
Normalize transfer efficiency statistical chart.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
The embodiment of the present invention is as follows:
Embodiment 1:
Etched ITO electro-conductive glass is respectively cleaned 15 minutes with acetone, deionized water and dehydrated alcohol respectively, nitrogen is blown
It is dry, then it is handled 15 minutes in UV ozone atmosphere;Dynamic spin coating PEODT:PSS solution.All embodiments of the invention
PEODT:PSS solution derive from Xi'an Polymer Light Technology Co., Ltd..
Dynamic spin coating process are as follows: spin coating instrument revolving speed is adjusted to 2000 revs/min and first turns 10 seconds, is added dropwise simultaneously in this process
PEODT:PSS solution, then become 5000 revs/min and turn 30 seconds, it takes out and heats 40 points in the heating plate that temperature is 120 degrees Celsius
Clock;Spin coating PbI again2- tBP precursor solution, PbI2Solution concentration is 1.2 moles/milliliter, tBP:PbI2Liquor capacity ratio is 1:
25, spin speed is 4500 revs/min, and spin-coating time is 30 seconds, takes out and heats 15 in the heating plate that temperature is 70 degrees Celsius
Minute;It is then spin coated onto the CH of 12 mg/ml of concentration3NH3I aqueous isopropanol, solution stand rotate after 20 seconds, and spin coating parameters are
4000 revs/min 30 seconds, taking out in temperature is to heat 30 minutes in 100 degrees Celsius of heating plate;Then spin coating concentration is 20 again
The PC of mg/ml61BM chlorobenzene solution, spin speed are 2000 revs/min, and the time is 30 seconds, are 80 degrees Celsius in temperature
It is heated 30 minutes in heating plate;Perovskite solar cell device is made in the silver electrode that finally vapor deposition a layer thickness is 100 nanometers.
Fig. 2 is the CH prepared3NH3PbI3Film and CH3NH3PbI3X-ray diffraction (XRD) spectrogram of-tBP film, knot
CH in the position at brilliant peak and document3NH3PbI3Position be consistent, and add tBP after PbI2Than the PbI for not adding tBP2Due to more
Pore structure converts CH3NH3PbI3React more complete, without PbI2Residual.
Fig. 3 is the CH prepared3NH3PbI3Film and CH3NH3PbI3The field emission scanning electron microscope (FESEM) of-tBP film shines
Piece, it can be seen that the CH of the method for the present invention preparation3NH3PbI3Crystal structure is good, and crystal grain is big and smooth, is conducive to mentioning for efficiency
It rises.
Fig. 4 is addition tBP and the VA characteristic curve comparison diagram for being not added with tBP prepared by the method for the present invention, it is not difficult to find that
Device photoelectric performance prepared by the present invention is substantially better than the photoelectric properties for being not added with tBP.
Fig. 5 is the addition tBP of the method for the present invention preparation and the normalization transfer efficiency statistical chart for being not added with tBP, is not added
Add the statistical result of tBP obviously not as good as the statistical result of the method for the present invention.As it can be seen that being not added with the normalization conversion effect of tBP in figure
The curve of rate declines quickly compared with the slope of a curve of the normalization transfer efficiency of addition tBP, it is seen that and moisture resistance stability is very poor, and
The slope of curve of the normalization transfer efficiency of addition tBP of the invention is stablized, and it is fine to show moisture resistance stability.
Embodiment 2:
Etched ITO electro-conductive glass is respectively cleaned 15 minutes with acetone, deionized water and dehydrated alcohol respectively, nitrogen is blown
It is dry, then it is handled 15 minutes in UV ozone atmosphere;Dynamic spin coating PEODT:PSS solution.Dynamic spin coating process are as follows: rotation
Painting instrument revolving speed is adjusted to 1800 revs/min and first turns 8 seconds, PEODT:PSS solution is added dropwise simultaneously in this process, then become 4800
Rev/min turn 20 seconds, taking out in temperature is to heat 20 minutes in 115 degrees Celsius of heating plate;Spin coating PbI again2- tBP presoma
Solution, PbI2Solution concentration is 1 mole/milliliter, tBP:PbI2Liquor capacity ratio is 1:50, and spin speed is 4300 revs/min,
Spin-coating time is 20 seconds, takes out and heats 10 minutes in the heating plate that temperature is 65 degrees Celsius;It is then spin coated onto 12 milligrams of concentration/milli
The CH risen3NH3I aqueous isopropanol, solution stand rotate after 15 seconds, spin coating parameters be 3500 revs/min 20 seconds, take out in temperature
To be heated 20 minutes in 90 degrees Celsius of heating plates;Then again spin coating concentration be 20 mg/mls PC61BM chlorobenzene solution, rotation
Applying speed is 2000 revs/min, and the time is 30 seconds, is heated 30 minutes in the heating plate that temperature is 80 degrees Celsius;Finally it is deposited
A layer thickness is that perovskite solar cell device is made in 100 nanometers of silver electrode.
Flow chart, X-ray diffraction (XRD) spectrogram, field emission scanning electron microscope (FESEM) of sample prepared by the embodiment
Photo, VA characteristic curve figure and normalization Efficiency Statistics figure are close with embodiment 1.
Embodiment 3:
Etched ITO electro-conductive glass is respectively cleaned 15 minutes with acetone, deionized water and dehydrated alcohol respectively, nitrogen is blown
It is dry, then it is handled 15 minutes in UV ozone atmosphere;Dynamic spin coating PEODT:PSS solution.Dynamic spin coating process are as follows: rotation
Painting instrument revolving speed is adjusted to 2200 revs/min and first turns 12 seconds, PEODT:PSS solution is added dropwise simultaneously in this process, then become 5200
Rev/min turn 40 seconds, taking out in temperature is to heat 60 minutes in 125 degrees Celsius of heating plate;Spin coating PbI again2- tBP presoma
Solution, PbI2Solution concentration is 1.4 moles/milliliter, tBP:PbI2Liquor capacity ratio is 1:10, and spin speed is 4700 revs/min
Clock, spin-coating time are 40 seconds, take out and heat 20 minutes in the heating plate that temperature is 75 degrees Celsius;It is then spin coated onto 12 milli of concentration
The CH of grams per milliliter3NH3I aqueous isopropanol, solution stand rotate after 25 seconds, spin coating parameters be 4500 revs/min 40 seconds, take out exist
It is heated 40 minutes in the heating plate that temperature is 110 degrees Celsius;Then again spin coating concentration be 20 mg/mls PC61BM chlorobenzene is molten
Liquid, spin speed are 2000 revs/min, and the time is 30 seconds, are heated 30 minutes in the heating plate that temperature is 80 degrees Celsius;Finally
Perovskite solar cell device is made in the silver electrode that vapor deposition a layer thickness is 100 nanometers.Sample prepared by the embodiment
Flow chart, X-ray diffraction (XRD) spectrogram, field emission scanning electron microscope (FESEM) photo, VA characteristic curve figure and normalization effect
Rate statistical chart is close with embodiment 1.
Claims (5)
1. the perovskite solar cell preparation method of a kind of enhancing moisture resistance stability and photoelectric properties, it is characterised in that this method
The step of it is as follows:
1) tin indium oxide (ITO) electro-conductive glass is cleaned, is respectively cleaned, is dried with nitrogen with acetone, deionized water and dehydrated alcohol respectively,
It is handled in UV ozone atmosphere again;
2) the poly- 3,4-rthylene dioxythiophene of spin coating (PEODT): kayexalate (PSS) solution takes cleaned in step 1)
Tin indium oxide (ITO) electro-conductive glass be fixed on spin coating instrument turntable, in the conductive glass surface dynamic spin coating of tin indium oxide (ITO)
PEODT:PSS solution;
3) PbI is prepared2- tBP precursor solution, by PbI2Powder is dissolved in n,N-Dimethylformamide (DMF) solution, then plus
Enter tBP (4- tert .-butylpyridine) solution, heating stirring is uniform;
4) spin coating PbI2The solution prepared in step 3) is added dropwise on the sample prepared in step 2)-tBP precursor solution
Spin coating is carried out for a period of time under specific rotation speeds, is taken out after spin coating and is heated a period of time in the heating plate of specific temperature, in sample
The porous and hydrophobic PbI of Surface Creation2- tBP film;
5) CH is prepared3NH3I solution, by CH3NH3I dissolution of crystals is in isopropanol, magnetic agitation under room temperature;
6)CH3NH3PbI3- tBP film preparation, by step 4) prepare sample be placed on spin coating instrument turntable, a dropping step 5) in match
The CH of system3NH3I solution just starts to rotate after static a period of time, carries out spin coating for a period of time under specific rotation speeds, takes after spin coating
A period of time is heated in the heating plate of specific temperature out, generates CH in sample surfaces3NH3PbI3- tBP film;
7) PC is prepared61BM solution, by PC61BM powder is dissolved in chlorobenzene, magnetic agitation under room temperature;
8) PC is prepared61BM layers, by step 6) prepare sample be placed on spin coating instrument turntable, a dropping step 7) in prepare solution exist
Spin coating is carried out for a period of time under specific rotation speeds, is taken out after spin coating and is heated a period of time in the heating plate of specific temperature, in sample
Surface Creation PC61BM film;
9) silver metal electrodes are deposited, sample prepared by step 8) is placed in vacuum evaporation instrument, vapor deposition a layer thickness is 80~120
The silver electrode of nanometer, is made perovskite solar cell device.
2. the perovskite solar cell preparation side of a kind of enhancing moisture resistance stability according to claim 1 and photoelectric properties
Method, it is characterised in that: in the step 2), dynamic spin coating PEODT:PSS solution is specific on tin indium oxide (ITO) conductive glass surface
Including three phases: the first stage is 1800~2200 revs/min, is turned 8~12 seconds;Second stage is 4800~5200 revs/min
Clock turns 20~40 seconds;Phase III is 20~60 minutes in 115~125 degrees Celsius of lower heating times.
3. the perovskite solar cell preparation side of a kind of enhancing moisture resistance stability according to claim 1 and photoelectric properties
Method, it is characterised in that: in the step 3), PbI2The concentration for being dissolved in DMF is 1~1.4 mole/milliliter, tBP:PbI2The body of solution
For product than being 1:50~1:10, heating stirring temperature is 65~75 degrees Celsius.
4. the perovskite solar cell preparation side of a kind of enhancing moisture resistance stability according to claim 1 and photoelectric properties
Method, it is characterised in that: in the step 4), PbI2The spin speed of-tBP precursor solution is 4300~4700 revs/min, rotation
Applying the time is 20~40 seconds, and heating temperature is 65~75 degrees Celsius, and heating time is 10~20 minutes.
5. the perovskite solar cell preparation side of a kind of enhancing moisture resistance stability according to claim 1 and photoelectric properties
Method, it is characterised in that: in the step 6), CH3NH3The quiescent time of I solution be 15~25 seconds, spin speed be 3500~
4500 revs/min, spin-coating time is 20~40 seconds, and heating temperature is 90~110 degrees Celsius, and heating time is 20~40 minutes.
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Cited By (1)
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CN110311037A (en) * | 2019-06-24 | 2019-10-08 | 浙江理工大学 | A kind of flexibility perovskite hole transmission layer used for solar batteries and its preparation method and application |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110311037A (en) * | 2019-06-24 | 2019-10-08 | 浙江理工大学 | A kind of flexibility perovskite hole transmission layer used for solar batteries and its preparation method and application |
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Application publication date: 20190108 |