CN104218109B - A kind of high efficiency perovskite thin film solar cell and preparation method thereof - Google Patents
A kind of high efficiency perovskite thin film solar cell and preparation method thereof Download PDFInfo
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Abstract
A kind of high efficiency perovskite thin film solar cell, by glass substrate, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back electrode of layer, PVP modulation form and form pellicular cascade structure, and film thickness is respectively front electrode 350nm, compacted zone 30-50nm, porous TiO2Layer 300-600nm, perovskite thin film 300-600nm, hole transmission layer 50-200nm and back electrode 50-200nm. Advantage of the present invention: this perovskite thin film is by the size intensive internet that crystal grain forms relatively uniformly, presents the relatively smooth and continuous pattern in surface; With the perovskite thin film that does not add PVP as compared with the battery device of the same terms of absorbed layer, short circuit current, open press and fill factor, curve factor be all significantly increased, battery efficiency is improved significantly, for the development of low cost, efficient calcium titanium ore thin film solar cell provides a kind of new preparation method.
Description
Technical field
The present invention relates to technical field of solar cells, particularly relate to a kind of high efficiency perovskite thin film solar cell and preparation method thereof.
Background technology
The requirement that could meet real world applications must significantly be raised the efficiency, be reduced costs to photovoltaic, as a developing direction of future source of energy. Ca-Ti ore type thin film solar cell is simple in structure with it, preparation cost is cheap and the advantage such as easy production has attracted the very big interest of numerous researchers. The compound perovskite CH of organic-inorganic3NH3(X is halogen element I to PbX, Cl, Br or halogen compound) be direct band-gap semicondictor material, there is the advantages such as the absorption coefficient of light is large, carrier mobility is high, the life-span is long, in perovskite solar cell, show huge application prospect as light trapping material. Its cell photoelectric transformation efficiency brought up to rapidly 19.3% from 3.8% in nearly 5 years, but also had the larger space of further lifting, became a new direction of following theCourse of PV Industry.
The preparation method of Ca-Ti ore type thin film solar cell has two kinds conventionally: vacuum vapour deposition and solwution method. Compared with vapour deposition method, solwution method, due to without vacuum equipment, is the better approach of preparation low cost, efficient solar battery. Perovskite thin film is as the light absorbing zone of perovskite solar cell, and its pattern and performance are the key factors that affects battery. Concerning solution spin-coating method is prepared thin film solar cell, obtain perovskite thin film even, high coverage rate and remain the severe challenge that this low-cost technologies faces at present.
Polyvinylpyrrolidone (PVP) is a kind of nontoxic water-soluble high-molecular compound, has good stability and film forming characteristics. It not only can be used as surface agent, can also be used as chelating agent, controls crystal growth by modifying interfacial energy, or simultaneously as surface agent and chelating agent application. The present invention proposes in perovskite precursor solution, to add PVP to improve the film forming characteristics of perovskite, improves its coverage rate on porous layer, and then promotes the photoelectric characteristic of perovskite thin film solar cell.
Summary of the invention
The object of the invention is for above-mentioned existing problems, a kind of high efficiency perovskite thin film solar cell and preparation method thereof is provided, perovskite thin film prepared by the method is by the size intensive internet that crystal grain forms relatively uniformly, present the relatively smooth and continuous pattern in surface, adopt surface agent polyvinylpyrrolidone (PVP) to strengthen perovskite thin film surface coverage, and then improve perovskite efficiency of solar cell.
Technical scheme of the present invention:
A kind of high efficiency perovskite thin film solar cell, by glass substrate, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back electrode of layer, PVP modulation form and form pellicular cascade structure, and film thickness is respectively front electrode 350nm, compacted zone 30-50nm, porous TiO2Layer 300-600nm, perovskite thin film 300-600nm, hole transmission layer 50-200nm and back electrode 50-200nm.
A preparation method for described high efficiency perovskite thin film solar cell, step is as follows:
1) adopt chemical bath method to prepare TiO on clean transparent conductive film FTO substrate2Compacted zone
Clean transparent conductive film FTO substrate is put into the TiCl that concentration is 0.04mol/L4In the aqueous solution, be then placed in baking box and heat 30min at 70 DEG C, take out substrate and rinse well, the 45min that anneals at 500 DEG C, obtains the TiO that thickness is 30-50nm2Compacted zone, as electronic barrier layer;
2) adopt spin-coating method to prepare porous TiO2Layer
By porous TiO2With absolute ethyl alcohol according to weight ratio 1:4 dilution, the porous TiO that spin coating has been diluted on compacted zone2Solution, 5000 revs/min are rotated 60 seconds, spin coating twice, then 500oC annealing 45min, obtains the porous TiO that thickness is 300-600nm2Layer, as insulating barrier;
3) adopt spin-coating method to prepare perovskite thin film
By methyl ammonium iodide (CH3NH3And lead chloride (PbCl I)2) be dissolved in DMF and obtain mixed liquor, in mixed liquor, the mol ratio of methyl ammonium iodide and lead chloride is 3:1, and magnetic agitation to solution is clarified, and in mixed liquor, adds PVP, and PVP addition is CH3NH3I and PbCl2The 0-5wt% of gross weight, continue to stir, the mixed liquor that contains PVP is dropped in to porous TiO2On layer, 5000 revs/min are rotated 60 seconds, and in baking box, air annealing 50min at 100-160 DEG C, obtains the perovskite thin film that thickness is 300-600nm;
4) spin coating Spiro-OMeTAD{2 on perovskite thin film, 2,7,7-tetra-[N, N-bis-(4-methoxyphenyl) amino]-9,9-spiral shell two fluorenes } hole transmission layer (HTM)
First two 520mg fluoroform sulfimide lithiums (Li-TFSI) are dissolved in 1mL acetonitrile solution, then the acetonitrile solution of 17.5 μ LLi-TFSI and 80mgspiro-OMeTAD, 28.5 μ L4-tert .-butylpyridine are dissolved in 1mL chlorobenzene altogether, obtain HTM solution, the HTM solution preparing is dropped on perovskite thin film, 5000 revs/min are rotated 60 seconds, spin coating twice, makes the hole transmission layer that thickness is 50-200nm;
5) adopt thermal evaporation to prepare back electrode
On hole transmission layer, thermal evaporation layer of Au, Ag or Al metallic film are as back electrode, and thickness is 50-200nm, make perovskite thin film solar cell.
Working mechanism of the present invention:
The method can strengthen perovskite thin film surface coverage, and then improves perovskite efficiency of solar cell. Utilize PVP stable performance, there is good film forming characteristics, joined in the precursor solution of perovskite thin film, improve the affinity between precursor solution and semiconductor porous layer or insulating barrier, strengthen perovskite thin film in its surperficial coverage rate. The lifting of perovskite thin film surface coverage, can reduce the light transmission not absorbed by perovskite thin film on the one hand and lose, and has strengthened light absorption; By reducing the cavity of surface of insulating layer, reduce the part that hole transmission layer directly contacts with insulating barrier on the other hand, reduce the recombination losses of carrier. Therefore make perovskite solar cell short-circuit current density, open and press and fill factor, curve factor all gets a promotion, and then battery efficiency is greatly improved
Advantage of the present invention and good effect are:
The perovskite thin film that adopts the present invention to prepare is by the size intensive internet that crystal grain forms relatively uniformly, presents the relatively smooth and continuous pattern in surface; By the adjusting of surface agent addition, can conveniently control the key parameter such as coverage rate, surface topography of film, thereby affect optical absorption intensity and photoelectric properties; With the perovskite thin film that does not add surface agent as compared with the battery device of the same terms of absorbed layer, short circuit current, open press and fill factor, curve factor be all significantly increased, battery efficiency has obtained significantly promoting, for the development of low cost, efficient calcium titanium ore thin film solar cell provides a kind of new preparation method.
Brief description of the drawings
Fig. 1 is AFM (AFM) shape appearance figure of the perovskite thin film of preparation.
Fig. 2 is the structure chart of this perovskite thin film solar cell.
Fig. 3 is the I-V performance diagram of this perovskite thin film solar cell.
Fig. 4 is the light absorption spectrogram of the perovskite thin film of preparation
The quantum efficiency curve map that Fig. 5 is the corresponding solar cell of perovskite thin film that is preparation with Fig. 4.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, technical solutions according to the invention are described in detail.
Embodiment 1:
A kind of high efficiency perovskite thin film solar cell, by glass substrate, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back electrode of layer, PVP modulation form and form pellicular cascade structure, as shown in Figure 1, the preparation method of described high efficiency perovskite thin film solar cell, step is as follows:
1) adopt chemical bath method to prepare TiO on clean transparent conductive film FTO substrate2Compacted zone
The transparent conductive film FTO substrate that is 350nm by clean thickness is put into the TiCl that concentration is 0.04mol/L4In the aqueous solution, be then placed in baking box and heat 30min at 70 DEG C, take out substrate and rinse well, the 45min that anneals at 500 DEG C, obtains the TiO that thickness is about 30nm2Compacted zone, as electronic barrier layer;
2) adopt spin-coating method to prepare porous TiO2Layer
By porous TiO2With absolute ethyl alcohol according to weight ratio 1:4 dilution, the porous TiO that spin coating has been diluted on compacted zone2Solution, 5000 revs/min are rotated 60 seconds, spin coating twice, then 500oC annealing 45min, obtains the porous TiO that thickness is 400nm2Layer, as insulating barrier;
3) adopt spin-coating method to prepare perovskite thin film
By methyl ammonium iodide (CH3NH3And lead chloride (PbCl I)2) be dissolved in DMF and obtain mixed liquor, in mixed liquor, the mol ratio of methyl ammonium iodide and lead chloride is 3:1, magnetic agitation 12h clarifies to solution. Mixed liquor is dropped in to porous TiO2On layer, 5000 revs/min are rotated 60 seconds, and in baking box, air annealing 50min at 140 DEG C, obtains the perovskite thin film that thickness is about 400nm, and Fig. 1 is AFM (AFM) shape appearance figure of the perovskite thin film of preparation;
4) spin coating Spiro-OMeTAD{2 on perovskite thin film, 2,7,7-tetra-[N, N-bis-(4-methoxyphenyl) amino]-9,9-spiral shell two fluorenes } hole transmission layer (HTM)
First two 520mg fluoroform sulfimide lithiums (Li-TFSI) are dissolved in 1mL acetonitrile solution, then the acetonitrile solution of 17.5 μ LLi-TFSI and 80mgspiro-OMeTAD, 28.5 μ L4-tert .-butylpyridine are dissolved in 1mL chlorobenzene altogether, obtain HTM solution, the HTM solution preparing is dropped on perovskite thin film, 5000 revs/min are rotated 60 seconds, spin coating twice, makes the hole transmission layer that thickness is about 150nm;
5) adopt thermal evaporation to prepare back electrode
On hole transmission layer, thermal evaporation one deck Ag metallic film is as back electrode, and thickness is about 150nm, makes perovskite thin film solar cell.
Testing result is as in Figure 3-5: Jsc，VocBe respectively 13.12mA/cm with FF2, 0.787V, 43.7; Photoelectric transformation efficiency η is 4.51%.
Embodiment 2:
A kind of high efficiency perovskite thin film solar cell, by glass substrate, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back electrode of layer, PVP modulation forms and forms pellicular cascade structure, as shown in Figure 1, the preparation method of described high efficiency perovskite thin film solar cell, step 1), 2), 4) and 5) identical with embodiment 1, difference is that step 3) is:
3) by CH3NH3I and PbCl2Be dissolved in DMF and obtain mixed liquor, in mixed liquor, the mol ratio of methyl ammonium iodide and lead chloride is 3:1, and magnetic agitation 12h clarifies to solution, in mixed liquor, adds PVP, and PVP addition is CH3NH3I and PbCl2The 1.6wt% of gross weight, continue to stir, the mixed liquor that contains PVP is dropped in to porous TiO2On layer, 5000 revs/min are rotated 60 seconds, and in baking box, air annealing 50min at 140 DEG C, obtains the perovskite thin film that thickness is about 400nm.
Testing result is as in Figure 3-5: Jsc，VocBe respectively 14.96mA/cm with FF2, 0.823V, 48.5. Photoelectric transformation efficiency η is 5.97%.
Embodiment 3:
A kind of high efficiency perovskite thin film solar cell, by glass substrate, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back electrode of layer, PVP modulation forms and forms pellicular cascade structure, as shown in Figure 1, the preparation method of described high efficiency perovskite thin film solar cell, step 1), 2), 4) and 5) identical with embodiment 1, difference is that step 3) is:
3) by CH3NH3I and PbCl2Be dissolved in DMF and obtain mixed liquor, in mixed liquor, the mol ratio of methyl ammonium iodide and lead chloride is 3:1, and magnetic agitation 12h clarifies to solution, to the PVP that adds 3.3wt% in mixed liquor, continues to stir, and the mixed liquor that contains PVP is dropped in to porous TiO2On layer, 5000 revs/min are rotated 60 seconds, and in baking box, air annealing 50min at 140 DEG C, obtains the perovskite thin film that thickness is about 400nm.
Testing result is as in Figure 3-5: Jsc，VocBe respectively 17.54mA/cm with FF2, 0.848V, 58.8. Photoelectric transformation efficiency η is 8.74%.
Embodiment 4:
A kind of high efficiency perovskite thin film solar cell, by glass substrate, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back electrode of layer, PVP modulation forms and forms pellicular cascade structure, as shown in Figure 1, the preparation method of described high efficiency perovskite thin film solar cell, step 1), 2), 4) and 5) identical with embodiment 1, difference is that step 3) is:
3) by CH3NH3I and PbCl2Be dissolved in DMF and obtain mixed liquor, in mixed liquor, the mol ratio of methyl ammonium iodide and lead chloride is 3:1, and magnetic agitation 12h clarifies to solution, to the PVP that adds 5wt% in mixed liquor, continues to stir, and the mixed liquor that contains PVP is dropped in to porous TiO2On layer, 5000 revs/min are rotated 60 seconds, and in baking box, air annealing 50min at 140 DEG C, obtains the perovskite thin film that thickness is about 400nm.
Testing result is as in Figure 3-5: Jsc，VocBe respectively 16.56mA/cm with FF2, 0.837V, 36.8. Photoelectric transformation efficiency η is 5.10%.
The detailed performance parameter of solar cell prepared by embodiment of the present invention 1-4 is in table 1.
Table 1 adds and does not add the detailed performance parameter of PVP battery device
| Samples | Jsc (mA/cm2) | Voc (V) | FF | η(%) |
| 0% | 13.12 | 0.787 | 43.7 | 4.51 |
| 1.6% | 14.96 | 0.823 | 48.5 | 5.97 |
| 3.3% | 17.54 | 0.848 | 58.8 | 8.74 |
| 5% | 16.56 | 0.837 | 36.8 | 5.10 |
Because the present invention's emphasis is providing high coverage rate, the perovskite thin film of high photoelectric properties for efficient, low cost perovskite thin film solar cell. The device efficiency of battery can be promoted to 8.74% from 4.51%, means that the present invention can make the photoelectric properties of battery be improved significantly.
To sum up, the invention provides the preparation method who strengthens perovskite thin film surface coverage and then lifting efficiency of solar cell by surface agent, the method is simple, by the adjusting of surface agent addition, can conveniently control the key parameter such as coverage rate, surface topography of film, thereby affect its photoelectric properties, and then significantly promote the photoelectric transformation efficiency of solar cell. For the development of low cost, efficient calcium titanium ore thin film solar cell provides condition, make the practical possibility that becomes of this novel solar cell.
The above; only for preferably detailed description of the invention of the present invention, but protection scope of the present invention is not limited to this, is anyly familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention. Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (1)
1. a preparation method for perovskite thin film solar cell, described perovskite thin film solar cell is by glass linedThe end, front electrode, compacted zone, porous TiO2Perovskite thin film, hole transmission layer and the back of the body of layer, PVP modulationElectrode forms and forms pellicular cascade structure, film thickness be respectively front electrode 350nm, compacted zone 30-50nm,Porous TiO2Layer 300-600nm, perovskite thin film 300-600nm, hole transmission layer 50-200nm and back of the body electricityUtmost point 50-200nm, is characterized in that preparation process is as follows:
1) adopt chemical bath method to prepare TiO on clean transparent conductive film FTO substrate2Compacted zone
Clean transparent conductive film FTO substrate is put into the TiCl that concentration is 0.04mol/L4The aqueous solutionIn, be then placed in baking box and heat 30min at 70 DEG C, take out substrate and rinse well, at 500 DEG CAnnealing 45min, obtains the TiO that thickness is 30-50nm2Compacted zone, as electronic barrier layer;
2) adopt spin-coating method to prepare porous TiO2Layer
By porous TiO2With absolute ethyl alcohol, according to weight ratio 1:4 dilution, on compacted zone, spin coating has been dilutedPorous TiO2Solution, 5000 revs/min are rotated 60 seconds, spin coating twice, then 500 DEG C of annealing 45min,Obtain the porous TiO that thickness is 300-600nm2Layer, as insulating barrier;
3) adopt spin-coating method to prepare perovskite thin film
By methyl ammonium iodide (CH3NH3And lead chloride (PbCl I)2) be dissolved in and in DMF, obtain mixed liquor, mixedClosing the mol ratio of methyl ammonium iodide and lead chloride in liquid is 3:1, and magnetic agitation to solution is clarified, to mixingIn liquid, add PVP, PVP addition is CH3NH3I and PbCl2The 0-5wt% of gross weight, continueStir, the mixed liquor that contains PVP is dropped in to porous TiO2On layer, 5000 revs/min are rotated 60 seconds,Air annealing 50min at 100-160 DEG C in baking box, the perovskite that obtains thickness and be 300-600nm is thinFilm;
4) spin coating Spiro-OMeTAD{2 on perovskite thin film, 2,7,7-tetra-[N, N-bis-(4-methoxybenzeneBase) amino]-9,9-spiral shell two fluorenes } hole transmission layer (HTM)
First two 520mg fluoroform sulfimide lithiums (Li-TFSI) are dissolved in 1mL acetonitrile solution,Then by the acetonitrile solution of 17.5 μ LLi-TFSI and 80mgspiro-OMeTAD, the 28.5 μ L4-tert-butyl groupsPyridine is dissolved in 1mL chlorobenzene altogether, obtains HTM solution, and the HTM solution preparing is dropped in to calcium titaniumOn the film of ore deposit, 5000 revs/min are rotated 60 seconds, and spin coating twice, makes the hole that thickness is 50-200nmTransport layer;
5) adopt thermal evaporation to prepare back electrode
On hole transmission layer, thermal evaporation layer of Au, Ag or Al metallic film are as back electrode, and thickness is50-200nm, makes perovskite thin film solar cell.
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| CN106328813B (en) * | 2015-06-29 | 2018-08-28 | 清华大学 | A kind of high stability mixes caesium Ca-Ti ore type solar cell and preparation method thereof |
| CN105609645B (en) * | 2015-12-22 | 2017-12-01 | 嵊州北航投星空众创科技有限公司 | A kind of photovoltaic material of micropore perovskite structure and preparation method thereof |
| CN105870336A (en) * | 2016-06-01 | 2016-08-17 | 华东师范大学 | Mesoporous perovskite solar cell |
| KR20180007585A (en) * | 2016-07-13 | 2018-01-23 | 엘지전자 주식회사 | Tandem solar cell, tanden solar cell module comprising the same and method for manufacturing thereof |
| RU2645221C1 (en) * | 2016-09-30 | 2018-02-19 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Perovskite solar cell and method of its manufacture |
| CN110352507A (en) * | 2018-01-30 | 2019-10-18 | 南方科技大学 | Preparation method and application of perovskite thin film |
| US10573766B2 (en) * | 2018-02-01 | 2020-02-25 | Panasonic Corporation | Solar cell |
| CN109888103A (en) * | 2019-03-01 | 2019-06-14 | 北京理工大学 | A method of inhibit small molecule hole transport layer hole to generate |
| CN110176546A (en) * | 2019-04-28 | 2019-08-27 | 华南师范大学 | A kind of light emitting diode and preparation method thereof based on multiple addition calcium titanium material layer |
| CN111403607A (en) * | 2020-03-25 | 2020-07-10 | 华东理工大学 | Chelated perovskite material, film, device and preparation method and application thereof |
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