CN110484880A - The preparation method of perovskite battery with single crystalline orientation hole transmission layer - Google Patents
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Abstract
The present invention relates to a kind of perovskite battery preparation methods with single crystalline orientation hole transmission layer, belong to perovskite area of solar cell.Technical solution of the present invention main points are as follows: the controllable hole transport layer film of crystalline orientation is grown in FTO Conducting Glass by the method for magnetron sputtering, then successively spin coating perovskite light-absorption layer, electron transfer layer on the hole transport layer, the perovskite battery based on single crystalline orientation hole transmission layer is made in last electrode evaporation.By regulating and controlling the crystal orientation of hole transport layer film, and then may be implemented to hole transmission layer film surface atom, band structure arrangement, coordination, the regulation of surface energy, fault of construction.The present invention is based on the hole transmission layer film preparations of single crystalline orientation into perovskite solar battery, not only increase the electric conductivity, carrier mobility and charge-extraction ability of hole transmission layer transport layer, and the pattern of perovskite thin film is improved, and then improve the photovoltaic performance of perovskite solar battery.
Description
Technical field
The present invention relates to a kind of preparation methods of perovskite battery with single crystalline orientation hole transmission layer, belong to calcium
Titanium ore area of solar cell.
Background technique
Crystal has anisotropy, by regulating and controlling the crystalline orientation of film, and then may be implemented to film surface atom, energy
Band structure arrangement, coordination, the regulation of surface energy, fault of construction.Xiaolin Zheng team demonstrates BiVO4[001] growth
Direction shows good inherent charge transmission and surface reaction ([1] HS Han, S Shin, DH Kim, et
al.Energy&Environmental Science,2018,11,1299-1306)；Wei Lin Leong proves height-oriented
The perovskite material of growth can be used for preparing solar battery ([2] T Ye, A Bruno, the G Han, Advanced of efficient stable
Functional Materials,2018,1801654)。
By regulating and controlling the crystalline orientation of hole transport layer film, and then may be implemented former to hole transmission layer film surface
Son, band structure arrangement, coordination, the regulation of surface energy, fault of construction.The present invention is based on the hole transmission layers of different crystallographic orientations
Perovskite solar battery made from film, not only increase the electric conductivity of hole transmission layer transport layer, carrier mobility and
Charge-extraction ability, and the pattern of perovskite thin film is improved, and then improve the photovoltaic performance of perovskite solar battery.
Summary of the invention
Technical solution of the present invention main points are as follows: growing crystal orientation on a transparent substrate by the method for magnetron sputtering can
The hole transport layer film of control, then successively spin coating perovskite light-absorption layer, electron transfer layer on hole transport layer film, finally
The perovskite solar battery based on the controllable hole transmission layer of crystalline orientation is made in electrode evaporation.
A kind of preparation method of the perovskite battery with single crystalline orientation hole transmission layer, it is characterised in that: use
The method of magnetron sputtering is led by adjusting the sputtering atmosphere in magnetron sputtering process, base reservoir temperature, annealing temperature parameter in FTO
The hole transport layer film of different crystallographic orientations is prepared in electric glass substrate, hole transport layer film crystalline orientation is controllable；So
Successively spin coating perovskite light-absorption layer, electron transfer layer, last electrode evaporation on NiO film afterwards are made and are taken based on single crystallization
To the perovskite battery of hole transmission layer.
Further, what the FTO Conducting Glass was selected is the FTO electro-conductive glass of light transmittance > 90%；Conductive glass
Glass is needed before the use by cleaning treatment and etching processing；Cleaning treatment is to be sequentially placed into FTO electro-conductive glass to wash
Agent, ionized water, ethyl alcohol, acetone, ultrasound 10-30min, twice of this process repetition in ultrasonic cleaning instrument in isopropanol equal solvent；
Ultrasound terminates FTO electro-conductive glass with being dried with nitrogen；Etching processing is that electro-conductive glass is placed in etching machine to etch 5-20min,
Obtain the good FTO electro-conductive glass of clean surface, wellability.
Further, the controllable hole transport layer film of crystalline orientation sputtering time in magnetron sputtering process is
30-90min；
The volume ratio of argon gas and oxygen is 1:10-1:100 in argon oxygen combination gas in magnetron sputtering process；Gas flow is
300-1000ml/min；Atmosphere pressure is 0-10pa；Sputtering power is 40-100W.
Further, the hole transport layer membrane materials include NiO, V2O5, CuO, CuSCN etc..
Further, it also to be followed the steps below before carrying out magnetron sputtering:
S1, target is mounted in magnetron sputtering coating system；
S2, cleaned substrate is put into magnetron sputtering vacuum chamber；
S3, vacuum pumping is carried out to vacuum chamber, and is filled with sputtering atmosphere.
Further, the perovskite light-absorption layer the preparation method comprises the following steps:
(1) preparation of perovskite precursor solution
PbI2 and MAI powder is weighed, is dissolved according to the ratio of 1.1:1 in the mixed solution of DMF and DMSO；
(2) one-step method prepares perovskite
On the hole transport layer by precursor solution drop coating, revolving speed 1000-6000rpm, time 10-60s；In 5-
Drop coating anti-solvent chlorobenzene 100-300ul when 25s, after heat 10-60min on hot plate, temperature is 100-200 DEG C.
Further, the preparation method of the electron transfer layer is: PCBM being dissolved in chlorobenzene and is prepared into presoma
Solution, by presoma drop coating on perovskite, revolving speed 1000-6000rpm, time 10-30s.
Further, the calcium titanium ore bed and electron transfer layer preparation are carried out in glove box.
Further, the preparation method of the electrode: it is deposited 50-500nm's on PCBM by the method for hot evaporation
Gold or silver are used as electrode.
The preparation method of perovskite battery with single crystalline orientation hole transmission layer as described above, specific preparation step
It is rapid as follows:
(1) FTO electro-conductive glass is successively immersed in dish washing liquid, deionized water, ethyl alcohol, acetone in aqueous isopropanol, is put into
It is cleaned by ultrasonic 10-30min in supersonic wave cleaning machine, later by glass immersion in aqueous isopropanol；Using it is preceding with nitrogen by glass
Glass drying, electro-conductive glass is placed in etching machine and etches 5-20min, obtains the good FTO electro-conductive glass of clean surface, wellability；
(2) in FTO conductive substrates, by adjusting sputtering atmosphere, sputtering power, atmosphere pressure in magnetron sputtering process
By force, the parameters such as gas flow, base reservoir temperature, annealing temperature prepare the hole transport layer film of different crystallographic orientations；
(3) suitable PbI is weighed2With MAI powder, proportionally it is dissolved in the mixed solution of DMF and DMSO and makes
The precursor solution of standby perovskite out.On the hole transport layer by precursor solution drop coating, revolving speed 1000-6000rpm, time
For 10-60s；The drop coating anti-solvent chlorobenzene 100-300ul in 5-25, after 10-60min is heated on hot plate, temperature is
100-200℃；
(4) PCBM is dissolved in chlorobenzene and is prepared into precursor solution, by presoma drop coating on perovskite, revolving speed
1000-6000rpm, time 10-30s；
(5) gold or silver for 50-500nm being deposited on PCBM by the method for hot evaporation are as electrode.
The present invention may be implemented by regulating and controlling the crystalline orientation of hole transport layer film to hole transport layer film table
Face atom, band structure arrangement, coordination, the regulation of surface energy, fault of construction.The present invention is based on the hole of different crystallographic orientations biographies
Perovskite solar battery made from defeated layer film not only increases electric conductivity, the carrier mobility of hole transmission layer transport layer
Rate and charge-extraction ability, and the pattern of perovskite thin film is improved, and then improve the photovoltaic of perovskite solar battery
Performance.
Detailed description of the invention
The X-ray diffractogram of the NiO of tri- kinds of single crystal orientations of Fig. 1.
The structure chart of Fig. 2 perovskite solar battery.
J-V curve of the NiO of Fig. 3<111>crystal orientation as the perovskite solar battery of hole transmission layer.
J-V curve of the NiO of Fig. 4<100>crystal orientation as the perovskite solar battery of hole transmission layer.
J-V curve of the NiO of Fig. 5<110>crystal orientation as the perovskite solar battery of hole transmission layer.
Specific embodiment
Technical solution of the present invention is described in detail below with reference to example, it is clear that described example is only this
Small part in invention, rather than whole examples.Those skilled in the art are changed under inspiration of the invention and are obtained
Every other example, shall fall within the protection scope of the present invention.
Example 1: perovskite solar battery of the NiO of<111>crystal orientation as hole transmission layer
Conductive substrates are cleaned up, are dried with nitrogen, etching processing.NiO film is prepared using the method for magnetron sputtering.It splashes
Penetrating the time is 30-90min, sputtering pressure 0-10pa, sputtering power 40-100W, argon gas flow 300-1000ml/
Min, base reservoir temperature are 25-550 DEG C.XRD test, as a result as shown in Figure 1.Spin coating calcium titanium ore bed, electron-transport on NiO film
Layer, the structure of last electrode evaporation, perovskite solar battery are as shown in Figure 2.Test the J-V of perovskite solar battery
Can, as shown in Figure 3.
Example 2: perovskite solar battery of the NiO of<100>crystal orientation as hole transmission layer
Conductive substrates are cleaned up, are dried with nitrogen, etching processing.NiO film is prepared using the method for magnetron sputtering.It splashes
Penetrating the time is 30-90min, sputtering pressure 0-10pa, sputtering power 40-100W, and argon gas, oxygen gas flow are 300-
1000ml/min, annealing temperature are 200-550 DEG C.XRD test, as a result as shown in Figure 1.On NiO film spin coating calcium titanium ore bed,
The structure of electron transfer layer, last electrode evaporation, perovskite solar battery is as shown in Figure 2.Test perovskite solar battery
J-V performance, as shown in Figure 4.
Example 3: perovskite solar battery of the NiO of<110>crystal orientation as hole transmission layer
Conductive substrates are cleaned up, are dried with nitrogen, etching processing.NiO film is prepared using the method for magnetron sputtering.It splashes
Penetrating the time is 30-90min, sputtering pressure 0-10pa, sputtering power 40-100W, argon gas flow 300-1000ml/
Min, annealing temperature are 200-550 DEG C.XRD test, as a result as shown in Figure 1.Spin coating calcium titanium ore bed, electronics pass on NiO film
Defeated layer, is finally deposited gold electrode, and the structure of perovskite solar battery is as shown in Figure 2.Test the J-V of perovskite solar battery
Performance, as shown in Figure 5.
Claims (10)
1. a kind of preparation method of the perovskite battery with single crystalline orientation hole transmission layer, it is characterised in that: use magnetic
The method for controlling sputtering, by adjusting the sputtering atmosphere in magnetron sputtering process, base reservoir temperature, annealing temperature parameter, in FTO conduction
The hole transport layer film of different crystallographic orientations is prepared in glass substrate, hole transport layer film crystalline orientation is controllable；Then
Successively spin coating perovskite light-absorption layer, electron transfer layer, last electrode evaporation on NiO film are made and are based on single crystalline orientation
The perovskite battery of hole transmission layer.
2. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
Be characterized in that the FTO Conducting Glass selection is the FTO electro-conductive glass of light transmittance > 90%；Electro-conductive glass is using
It is needed before by cleaning treatment and etching processing；Cleaning treatment is that FTO electro-conductive glass is sequentially placed into detergent, ion
Water, ethyl alcohol, acetone, ultrasound 10-30min, twice of this process repetition in ultrasonic cleaning instrument in isopropanol solvent；Ultrasound terminate by
FTO electro-conductive glass is with being dried with nitrogen；Etching processing is that electro-conductive glass is placed in etching machine to etch 5-20min, and it is clean to obtain surface
Only, the good FTO electro-conductive glass of wellability.
3. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
It is characterized in that the controllable hole transport layer film of crystalline orientation sputtering time in magnetron sputtering process is 30-90min；
The volume ratio of argon gas and oxygen is 1:10-1:100 in argon oxygen combination gas in magnetron sputtering process；Gas flow is 300-
1000ml/min；Atmosphere pressure is 0-10pa.
Sputtering power is 40-100W.
4. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
It is characterized in that the hole transport layer membrane materials include NiO, V2O5、CuO、CuSCN。
5. the preparation side of the perovskite battery with single crystalline orientation hole transmission layer according to claim 1
Method, it is characterised in that also to be followed the steps below before carrying out magnetron sputtering:
S1, target is mounted in magnetron sputtering coating system；
S2, cleaned substrate is put into magnetron sputtering vacuum chamber；
S3, vacuum pumping is carried out to vacuum chamber, and is filled with sputtering atmosphere.
6. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
Be characterized in that the perovskite light-absorption layer the preparation method comprises the following steps:
(1) preparation of perovskite precursor solution
PbI2 and MAI powder is weighed, is dissolved according to the ratio of 1.1:1 in the mixed solution of DMF and DMSO；
(2) one-step method prepares perovskite
On the hole transport layer by precursor solution drop coating, revolving speed 1000-6000rpm, time 10-60s；In 5-25s
When drop coating anti-solvent chlorobenzene 100-300ul, after heat 10-60min on hot plate, temperature is 100-200 DEG C.
7. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
Being characterized in that the preparation method of the electron transfer layer is: PCBM is dissolved in chlorobenzene and is prepared into precursor solution, will before
Body drop coating is driven on perovskite, revolving speed 1000-6000rpm, time 10-30s.
8. the preparation method of the perovskite battery according to claim 6 or 7 with single crystalline orientation hole transmission layer,
It is characterized in that the calcium titanium ore bed and electron transfer layer preparation are carried out in glove box.
9. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
It is characterized in that the preparation method of the electrode: the golden or silver-colored conduct of 50-500nm is deposited on PCBM by the method for hot evaporation
Electrode.
10. the preparation method of the perovskite battery according to claim 1 with single crystalline orientation hole transmission layer,
It is characterized in that specific preparation process is as follows:
(1) FTO electro-conductive glass is successively immersed in dish washing liquid, deionized water, ethyl alcohol, acetone in aqueous isopropanol, is put into ultrasound
It is cleaned by ultrasonic 10-30min in wave cleaning machine, later by glass immersion in aqueous isopropanol；Glass is blown with nitrogen using preceding
It is dry, electro-conductive glass is placed in etching machine and etches 5-20min, obtains the good FTO electro-conductive glass of clean surface, wellability；
(2) in FTO conductive substrates, by adjusting sputtering atmosphere, sputtering power, atmosphere pressure, gas in magnetron sputtering process
Body flow, base reservoir temperature, annealing temperature parameter prepare the hole transport layer film of different crystallographic orientations；
(3) suitable PbI is weighed2With MAI powder, proportionally it is dissolved in the mixed solution of DMF and DMSO and prepares calcium
The precursor solution of titanium ore；On the hole transport layer by precursor solution drop coating, revolving speed 1000-6000rpm, time 10-
60s；The drop coating anti-solvent chlorobenzene 100-300u l in 5-25s, after 10-60min, temperature 100- are heated on hot plate
200℃；
(4) PCBM is dissolved in chlorobenzene and is prepared into precursor solution, by presoma drop coating on perovskite, revolving speed 1000-
6000rpm, time 10-30s；
(5) gold or silver for 50-500nm being deposited on PCBM by the method for hot evaporation are as electrode.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113871539A (en) * | 2021-12-02 | 2021-12-31 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of perovskite solar cell |
| WO2023070338A1 (en) * | 2021-10-26 | 2023-05-04 | 宁德时代新能源科技股份有限公司 | Perovskite cell having multiple layers of hole transport layers and preparation method for perovskite cell |
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| CN108666429A (en) * | 2018-05-16 | 2018-10-16 | 上海交通大学 | A kind of preparation method of the perovskite thin film with high charge transport quality |
| CN109371376A (en) * | 2018-12-04 | 2019-02-22 | 北京科技大学 | A kind of controllable method for preparing of the NiO film of single crystal orientation |
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| CN106784341A (en) * | 2017-01-20 | 2017-05-31 | 电子科技大学中山学院 | Microwave annealing treatment method for perovskite solar cell photoactive layer |
| CN108666429A (en) * | 2018-05-16 | 2018-10-16 | 上海交通大学 | A kind of preparation method of the perovskite thin film with high charge transport quality |
| CN109371376A (en) * | 2018-12-04 | 2019-02-22 | 北京科技大学 | A kind of controllable method for preparing of the NiO film of single crystal orientation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023070338A1 (en) * | 2021-10-26 | 2023-05-04 | 宁德时代新能源科技股份有限公司 | Perovskite cell having multiple layers of hole transport layers and preparation method for perovskite cell |
| CN113871539A (en) * | 2021-12-02 | 2021-12-31 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method of perovskite solar cell |
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