CN105529403A - Method for modifying perovskite solar cell light-absorbing layer - Google Patents

Method for modifying perovskite solar cell light-absorbing layer Download PDF

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CN105529403A
CN105529403A CN201510902604.XA CN201510902604A CN105529403A CN 105529403 A CN105529403 A CN 105529403A CN 201510902604 A CN201510902604 A CN 201510902604A CN 105529403 A CN105529403 A CN 105529403A
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absorption layer
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CN105529403B (en
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贾春阳
韩飞
万中全
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University of Electronic Science and Technology of China
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    • 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
    • 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
    • H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E10/549—Organic PV cells

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Abstract

The invention discloses a method for modifying a perovskite solar cell light-absorbing layer, and belongs to the field of the solar cell. The method comprises the steps of 1) preparing a hole barrier layer on a substrate; and 2) adding a light-absorbing layer precursor liquid in a dropwise manner on the surface of the substrate with the hole barrier layer, performing spin coating, after the solvent of the light-absorbing layer precursor liquid is fully evaporated, adding modifying liquid in a dropwise manner and continuing to perform spin coating, wherein the modifying liquid is mixed liquid of organic solvent of a soluble light-absorbing layer material and organic solvent of an insoluble light-absorbing layer material; the volume ratio of the organic solvent of the insoluble light-absorbing layer material to the organic solvent of the soluble light-absorbing layer material is 16-21, and the volume ratio of the total volume of the modifying liquid to the volume of the light-absorbing layer precursor liquid is 1-1.5; and drying after completing spin coating. According to the light-absorbing layer preparation process, the light-absorbing layer is modified by the modifying liquid; namely, a perovskite layer is subjected to film formation firstly; then the modifying liquid is adopted to dissolve and modify the light-absorbing layer so as to enlarge the crystal grains of the light-absorbing layer and reduce the porosity of the light-absorbing layer; and consequently, the performance of the perovskite solar cell is effectively improved.

Description

A kind of method of modifying perovskite solar cell light-absorption layer
Technical field
The invention belongs to area of solar cell, be specifically related to a kind of method of modifying perovskite solar cell light-absorption layer.
Background technology
Perovskite solar cell (perovskitesolarcells) is that one has DSSC device architecture, to have ABX 3the organic-metallic halide of structure etc. are as the battery of core light absorption, opto-electronic conversion, photo-generated carrier conveying material.Perovskite solar cell preparation technology is simple, has excellent opto-electronic conversion performance, is thus expected to become the solar cell of new generation with advantages such as high efficiency, low cost, all solid state, flexible wearable.
Perovskite solar cell mainly adopts a step spin-coating method preparation, namely adopt spin coating, the method for annealing prepares titanium dioxide dense layer, mesoporous titanium dioxide layer, perovskite light-absorption layer, hole transmission layer respectively, then hot evaporation one deck gold or silver are as obtaining electrode.But the method technique is simple, in film deposition process, solvent evaporates is fast, and solution is rapidly concentrated, therefore CH 3nH 3i and PbI 2between reaction speed quickly, easily cause generate perovskite crystal size uneven, cause active layer to have more pin hole.The existence of these pin holes makes perovskite can not cover substrate completely, produces larger leakage current; And the less stable to water and oxygen, easily oxidized in encapsulation process, greatly affect the repeatability of its device performance, limit the performance of battery.
Summary of the invention
The present invention is directed to the defect that background technology exists, propose a kind of method of simple modification perovskite solar cell light-absorption layer.The present invention, by modifying light-absorption layer, increases light-absorption layer crystal grain, reduces light-absorption layer porosity, thus effectively improves the performance of perovskite solar cell.
Technical scheme of the present invention is as follows:
Modify a method for perovskite solar cell light-absorption layer, comprise the following steps:
Step 1: prepare hole blocking layer on substrate;
Step 2: in the substrate surface dropping light-absorption layer precursor liquid of the band hole blocking layer that step 1 obtains, start spin coating, after the solvent evaporates of light-absorption layer precursor liquid is complete, drip decorating liquid, continue spin coating; Described decorating liquid is the mixed liquor of the organic solvent of solubilized light-absorption layer material and the organic solvent of indissoluble solution light-absorption layer material, in described decorating liquid, the volume ratio of the organic solvent of indissoluble solution light-absorption layer material and the organic solvent of solubilized light-absorption layer material is: 16 ~ 21, and the cumulative volume of decorating liquid and the volume ratio of light-absorption layer precursor liquid are 1 ~ 1.5; After spin coating completes, dry, the light-absorption layer film of high coverage, large grain size, band mirror effect can be obtained.
Further, substrate described in step 1 is FTO glass, ito glass, flexible ITO, PEN (PEN) etc.
Further, hole barrier layer material described in step 1 is TiO 2, ZnO, Zn 2snO 4deng.
Further, in step 1, hole blocking layer also can prepare mesoporous layer; Mesoporous layer material is TiO 2, ZnO, SiTiO 3, ZrO 2, Zn 2snO 4deng.
Further, the organic solvent of described solubilized light-absorption layer material is DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO), gamma-butyrolacton (GBL), DMA (DMA) etc.; The organic solvent of described indissoluble solution light-absorption layer material is chlorobenzene, dichloro-benzenes, carrene, toluene etc.
Further, decorating liquid described in step 2 can be chlorobenzene and DMSO, chlorobenzene and DMF, chlorobenzene and GBL, chlorobenzene and DMA, carrene and GBL, carrene and DMF, carrene and DMA, carrene and DMSO, toluene and DMSO, toluene and DMA, toluene and DMF etc.
Adopt said method to modify a preparation method for the perovskite solar cell of light-absorption layer, comprise the following steps:
Step 1: prepare hole blocking layer on substrate;
Step 2: in the substrate surface dropping light-absorption layer precursor liquid of the band hole blocking layer that step 1 obtains, start spin coating, after the solvent evaporates of light-absorption layer precursor liquid is complete, drip decorating liquid, continue spin coating; Described decorating liquid is the mixed liquor of the organic solvent of solubilized light-absorption layer material and the organic solvent of indissoluble solution light-absorption layer material, in described decorating liquid, the volume ratio of the organic solvent of indissoluble solution light-absorption layer material and the organic solvent of solubilized light-absorption layer material is: 16 ~ 21, and the cumulative volume of decorating liquid and the volume ratio of light-absorption layer precursor liquid are 1 ~ 1.5; After spin coating completes, dry, the light-absorption layer film of high coverage, large grain size, band mirror effect can be obtained;
Step 3: the light-absorption layer after step 2 processes prepares hole transmission layer and successively to electrode.
Further, hole transport layer material described in step 3 is 2,2', 7,7'-tetra-[N, N-bis-(4-methoxyphenyl) is amino]-9, the organic hole transport material such as 9'-spiral shell two fluorenes (Spiro-OMeTAD), PTAA, and CuI, CuSCN, NiO, CuInS 2deng inorganic hole transporter; Described is gold, silver, carbon etc. to electrode.
Beneficial effect of the present invention is:
1, the present invention is preparing in light-absorption layer process, decorating liquid is adopted to modify light-absorption layer, namely calcium titanium ore bed film forming is first allowed, then adopt that decorating liquid dissolves, recrystallization again, both increased light-absorption layer crystal grain, and made original less particle growth and join together, effectively reduce again light-absorption layer porosity, avoid the generation of leakage current simultaneously, thus effectively improve the performance of perovskite solar cell, for preparation broad area device provides foundation.
2, the present invention prepares the method for perovskite solar cell simply, and efficiency is high, and cost is low, easily realizes industrialization large-scale production, and the performance of the solar cell obtained has a distinct increment.
Accompanying drawing explanation
Fig. 1 is the basic structure schematic diagram of the perovskite solar cell of the embodiment of the present invention; Wherein: 1 is FTO glass, 2 is hole blocking layer, and 3 is mesoporous layer, and 4 is light-absorption layer, and 5 is hole transmission layer, and 6 is to electrode;
Fig. 2 is the key operation step schematic diagram of the modification perovskite solar cell light-absorption layer of the embodiment of the present invention; Wherein, a is spin coating light-absorption layer CH 3nH 3pbI 3the TiO of precursor liquid 2/ FTO glass, b is for adopting chlorobenzene and dmso treatment CH 3nH 3pbI 3light-absorption layer, c is the light-absorption layer after chlorobenzene and dmso treatment, and d is that the light-absorption layer after process is annealed on heating station;
Fig. 3 is the IV curve comparison figure of the perovskite solar cell that embodiment 1 and comparative example 1 obtain;
Fig. 4 is the IV curve comparison figure of the perovskite solar cell that embodiment 2 and comparative example 2 obtain.
Embodiment
Below in conjunction with drawings and Examples in detail, technical scheme of the present invention is described in detail.
Modify a method for perovskite solar cell light-absorption layer, comprise the following steps:
Step 1: prepare hole blocking layer on substrate;
Step 2: in the substrate surface dropping light-absorption layer precursor liquid of the band hole blocking layer that step 1 obtains, leave standstill 1 ~ 2min, then with the rotating speed spin coating 5 ~ 7s of 3000r/min, after light-absorption layer precursor liquid solvent evaporates is complete, drip decorating liquid, continue the rotating speed spin coating with 3000r/min, described decorating liquid is the mixed liquor of chlorobenzene and dimethyl sulfoxide (DMSO), the volume ratio of chlorobenzene and dimethyl sulfoxide (DMSO) is 16 ~ 21, and the cumulative volume of chlorobenzene and dimethyl sulfoxide (DMSO) and the volume ratio of light-absorption layer precursor liquid are 1 ~ 1.5; After spin coating completes, at 40 ~ 60 DEG C, toast 1 ~ 3min, then toast 10min at 100 DEG C, the light-absorption layer film of high coverage, large grain size, band mirror effect can be obtained.
Further, in step 1, hole blocking layer also can prepare mesoporous layer; Mesoporous layer material is TiO 2, ZnO, SiTiO 3, ZrO 2, Zn 2snO 4deng.
More specifically, a kind of method of modifying perovskite solar cell light-absorption layer, comprises the following steps:
Step 1: prepare titanium dioxide hole blocking layer and mesoporous titanium dioxide layer on FTO glass;
Step 2: the band titanium dioxide hole blocking layer obtained in step 1 and the FTO glass surface of mesoporous titanium dioxide layer drip the CH of 100 μ L1mM 3nH 3pbI 3precursor liquid, leaves standstill 1 ~ 2min, with the rotating speed spin coating 5 ~ 7s of 3000r/min; Then drip 100 μ L decorating liquids, described decorating liquid is the mixed liquor of chlorobenzene and dimethyl sulfoxide (DMSO), and the volume ratio of chlorobenzene and dimethyl sulfoxide (DMSO) is 19:1; After spin coating completes, at 40 ~ 60 DEG C, toast 1 ~ 3min, then toast 10min at 100 DEG C, the light-absorption layer film of high coverage, large grain size, band mirror effect can be obtained.
Further, titanium dioxide hole blocking layer described in step 1 adopts spin-coating method preparation, and spin coating liquid is: the butanol solution of 0.15M bis-(acetylacetone based) metatitanic acid diisopropyl ester, the ethanolic solution, titanium tetrachloride aqueous solution etc. of butyl titanate.
Further, CH described in step 2 3nH 3pbI 3precursor liquid is CH 3nH 3i (>99%, through four purifying) and PbI 2(99%) be dissolved in 1mLN with equimolar ratio, dinethylformamide (DMF), is made into the CH of 1mM 3nH 3pbI 3precursor liquid.
Further, the chlorobenzene described in step 2 and dimethyl sulfoxide (DMSO) purity are 99.8%.
Embodiment 1
Take FTO as substrate, titanium dioxide is hole blocking layer, titanium dioxide is mesoporous layer, CH 3nH 3pbI 3for light-absorption layer, Spiro-OMeTAD be hole transmission layer, gold is the preparation method to the perovskite solar cell of electrode:
Step 1: size FTO glass being cut into 2cm × 2cm, adopt deionized water, acetone and washes of absolute alcohol surface successively, nitrogen dries up stand-by;
Step 2: add in 1000mg1-butanols by 103mg bis-(acetylacetone based) metatitanic acid diisopropyl ester, stirs 30min, makes it mix, obtain mixed liquor A;
Step 3: the FTO glass surface spin coating mixed liquor A after step 1 is cleaned, toast at 125 DEG C, then anneal 30min at 500 DEG C, obtains titanium dioxide hole blocking layer;
Step 4: added by 200mg titania slurry in 700mg absolute ethyl alcohol, stirs 30min, makes it mix, obtain mixed liquid B;
Step 5: in the FTO glass surface spin coating mixed liquid B of the band titanium dioxide hole blocking layer that step 3 obtains, toasts at 125 DEG C, and the 30min that anneals at 500 DEG C, obtain mesoporous titanium dioxide layer;
Step 6: by 461mgPbI 2and 159mgCH 3nH 3i is dissolved in 1mLDMF, at the uniform velocity stirs 12h, obtains the CH of 1mM 3nH 3pbI 3precursor liquid;
Step 7: the band titanium dioxide hole blocking layer obtained in step 5 and the FTO glass surface of mesoporous titanium dioxide layer drip the CH that 100 μ L steps 6 prepare the 1mM obtained 3nH 3pbI 3precursor liquid, after leaving standstill 2min, with the rotating speed spin coating 6s of 3000r/min, treat that light-absorption layer precursor liquid solvent DMF is evaporated completely, then drip 100 μ L decorating liquids, continue spin coating, described decorating liquid is the mixed liquor of chlorobenzene and dimethyl sulfoxide (DMSO), and the volume ratio of chlorobenzene and dimethyl sulfoxide (DMSO) is 19:1; After spin coating completes, at 60 DEG C, toast 3min to dry solvent, then toast 10min at 100 DEG C, the light-absorption layer film of high coverage, large grain size, band mirror effect can be obtained;
Step 8: the light-absorption layer film surface obtained in step 7 adopts spin-coating method to prepare Spiro-OMeTAD hole transmission layer; Spin coating solution is the acetonitrile solution (520mgml of 72.3mgSpiro-OMeTAD, 28.8 μ L4-tert .-butylpyridine and 17.5 μ L bis trifluoromethyl sulfimides -1) to add in 1mL chlorobenzene that preparation obtains; Described Spiro-OMeTAD purity is greater than 99%, 4-tert .-butylpyridine purity >99%, bis trifluoromethyl sulfimide purity 99%, chlorobenzene and acetonitrile purity 99.8%;
Step 9: the gold that the hole transmission layer surface evaporation 80nm obtained in step 8 is thick, as to electrode.
Comparative example 1
Take FTO as substrate, titanium dioxide is hole blocking layer, titanium dioxide is mesoporous layer, CH 3nH 3pbI 3for light-absorption layer, Spiro-OMeTAD be hole transmission layer, gold is the preparation method to the perovskite solar cell of electrode:
Step 1: size FTO glass being cut into 2cm × 2cm, adopt deionized water, acetone and washes of absolute alcohol surface successively, nitrogen dries up stand-by;
Step 2: add in 1000mg1-butanols by 103mg bis-(acetylacetone based) metatitanic acid diisopropyl ester, stirs 30min, makes it mix, obtain mixed liquor A;
Step 3: the FTO glass surface spin coating mixed liquor A after step 1 is cleaned, toast at 125 DEG C, then anneal 30min at 500 DEG C, obtains titanium dioxide hole blocking layer;
Step 4: added by 200mg titania slurry in 700mg absolute ethyl alcohol, stirs 30min, makes it mix, obtain mixed liquid B;
Step 5: in the FTO glass surface spin coating mixed liquid B of the band titanium dioxide hole blocking layer that step 3 obtains, toasts at 125 DEG C, and the 30min that anneals at 500 DEG C, obtain mesoporous titanium dioxide layer;
Step 6: by 461mgPbI 2and 159mgCH 3nH 3i is dissolved in 1mLDMF, at the uniform velocity stirs 12h, obtains the CH of 1mM 3nH 3pbI 3precursor liquid;
Step 7: the band titanium dioxide hole blocking layer obtained in step 5 and the FTO glass surface of mesoporous titanium dioxide layer drip the CH that 100 μ L steps 6 prepare the 1mM obtained 3nH 3pbI 3precursor liquid, after leaving standstill 2min, with the rotating speed spin coating of 3000r/min; After spin coating completes, at 60 DEG C, toast 3min to dry solvent, then toast 10min at 100 DEG C, obtain light-absorption layer film;
Step 8: the light-absorption layer film surface obtained in step 7 adopts spin-coating method to prepare Spiro-OMeTAD hole transmission layer; Spin coating solution is the acetonitrile solution (520mgml of 72.3mgSpiro-OMeTAD, 28.8 μ L4-tert .-butylpyridine and 17.5 μ L bis trifluoromethyl sulfimides -1) to add in 1mL chlorobenzene that preparation obtains; Described Spiro-OMeTAD purity is greater than 99%, 4-tert .-butylpyridine purity >99%, bis trifluoromethyl sulfimide purity 99%, chlorobenzene and acetonitrile purity 99.8%;
Step 9: the gold that the hole transmission layer surface evaporation 80nm obtained in step 8 is thick, as to electrode.
Fig. 3 is the IV curve comparison figure of the perovskite solar cell that embodiment 1 and comparative example 1 obtain; The light-absorption layer of the perovskite solar cell that the light-absorption layer of perovskite solar cell embodiment 1 obtained respectively and comparative example 1 obtain, at AM1.5G, 100mW/cm 2xenon lamp irradiate the lower three-electrode method that adopts and carry out IV test, wherein scanning voltage is 0 ~ 1.2V, and sweep speed is 10mV/s.As shown in Figure 3, under same scan speed, the perovskite solar cell of embodiment 1 compares the electric current of the perovskite solar cell of ratio 1 and fill factor, curve factor obviously increases, and shows that the perovskite solar cell that embodiment 1 obtains has better performance.
Embodiment 2
Being distinguished as of the present embodiment and embodiment 1: decorating liquid described in step 7 is the mixed liquor of chlorobenzene and DMF, and the volume ratio of described chlorobenzene and DMF is 19:1.All the other steps are identical with embodiment 1.
Comparative example 2
Comparative example 2 is distinguished as with comparative example 1: the process of step 7 is: the band titanium dioxide hole blocking layer obtained in step 5 and the FTO glass surface of mesoporous titanium dioxide layer drip the CH that 100 μ L steps 6 prepare the 1mM obtained 3nH 3pbI 3precursor liquid, after leaving standstill 2min, with the rotating speed spin coating 6s of 3000r/min, treats that light-absorption layer precursor liquid solvent DMF is evaporated completely, then drip 100 μ L decorating liquids, continue spin coating, after spin coating completes, at 60 DEG C, toast 3min to dry solvent, then toast 10min at 100 DEG C, obtain light-absorption layer film.All the other steps are identical with comparative example 1.
Fig. 4 is the IV curve comparison figure of the perovskite solar cell that embodiment 2 and comparative example 2 obtain; The light-absorption layer of the perovskite solar cell that the light-absorption layer of perovskite solar cell embodiment 2 obtained respectively and comparative example 2 obtain, at AM1.5G, 100mW/cm 2xenon lamp irradiate the lower three-electrode method that adopts and carry out IV test, wherein scanning voltage is 0 ~ 1.2V, and sweep speed is 10mV/s.As shown in Figure 4, under same scan speed, the electric current that the perovskite solar cell of embodiment 2 compares the perovskite solar cell of ratio 2 obviously increases, and shows that the perovskite solar cell that embodiment 2 obtains has better performance.
Fig. 1 is the basic structure schematic diagram of the perovskite solar cell of embodiment; Fig. 2 is the key operation step schematic diagram of the modification perovskite solar cell light-absorption layer of embodiment.Perovskite solar cell of the present invention is only modified on perovskite light-absorption layer, effectively overcome the defects such as one-step method pin hole, light-absorption layer not exclusively cover, obtain the light-absorption layer film of high coverage, large grain size, band mirror effect, the fill factor, curve factor of solar cell and electric current are obviously increased, improves the performance of solar cell.
The present invention modifies perovskite light-absorption layer on the basis of conventional method, namely calcium titanium ore bed film forming is first allowed, then adopt decorating liquid dissolve again, recrystallization, both light-absorption layer crystal grain had been increased, make original less particle growth and join together, effectively reducing again light-absorption layer porosity, avoid the generation of leakage current simultaneously, thus effectively improve the performance of perovskite solar cell, for preparation broad area device provides foundation.The inventive method is simple to operate, and cost is low, easily realizes industrialization large-scale production.

Claims (6)

1. modify a method for perovskite solar cell light-absorption layer, comprise the following steps:
Step 1: prepare hole blocking layer on substrate;
Step 2: in the substrate surface dropping light-absorption layer precursor liquid of the band hole blocking layer that step 1 obtains, start spin coating, after the solvent evaporates of light-absorption layer precursor liquid is complete, drip decorating liquid, continue spin coating; Described decorating liquid is the mixed liquor of the organic solvent of solubilized light-absorption layer material and the organic solvent of indissoluble solution light-absorption layer material, in described decorating liquid, the volume ratio of the organic solvent of indissoluble solution light-absorption layer material and the organic solvent of solubilized light-absorption layer material is: 16 ~ 21, and the cumulative volume of decorating liquid and the volume ratio of light-absorption layer precursor liquid are 1 ~ 1.5; After spin coating completes, dry, light-absorption layer film can be obtained.
2. the method for modification perovskite solar cell light-absorption layer according to claim 1, it is characterized in that, described in step 2, the organic solvent of solubilized light-absorption layer material is DMF, dimethyl sulfoxide (DMSO), gamma-butyrolacton, DMA; The organic solvent of described indissoluble solution light-absorption layer material is chlorobenzene, dichloro-benzenes, carrene, toluene.
3. the method for modification perovskite solar cell light-absorption layer according to claim 1, is characterized in that, substrate described in step 1 is FTO glass, ito glass, flexible ITO, PEN; Described hole barrier layer material is TiO 2, ZnO, Zn 2snO 4.
4. the method for modification perovskite solar cell light-absorption layer according to claim 1, is characterized in that, in step 1, hole blocking layer also can prepare mesoporous layer; Mesoporous layer material is TiO 2, ZnO, SiTiO 3, ZrO 2, Zn 2snO 4.
5. a preparation method for perovskite solar cell, comprises the following steps:
Step 1: prepare hole blocking layer on substrate;
Step 2: in the substrate surface dropping light-absorption layer precursor liquid of the band hole blocking layer that step 1 obtains, start spin coating, after the solvent evaporates of light-absorption layer precursor liquid is complete, drip decorating liquid, continue spin coating; Described decorating liquid is the mixed liquor of the organic solvent of solubilized light-absorption layer material and the organic solvent of indissoluble solution light-absorption layer material, in described decorating liquid, the volume ratio of the organic solvent of indissoluble solution light-absorption layer material and the organic solvent of solubilized light-absorption layer material is: 16 ~ 21, and the cumulative volume of decorating liquid and the volume ratio of light-absorption layer precursor liquid are 1 ~ 1.5; After spin coating completes, dry, light-absorption layer film can be obtained;
Step 3: prepare hole transmission layer successively and to electrode on the light-absorption layer that step 2 obtains.
6. the preparation method of perovskite solar cell according to claim 5, is characterized in that, hole transport layer material described in step 3 is 2,2', 7,7'-tetra-[N, N-bis-(4-methoxyphenyl) is amino]-9,9'-spiral shell two fluorenes, PTAA, CuI, CuSCN, NiO, CuInS 2; Described is gold, silver, carbon to electrode.
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