CN115084391A - Perovskite solar cell with hole interface gradient structure, perovskite precursor solution, perovskite composite thin film layer and preparation method - Google Patents

Perovskite solar cell with hole interface gradient structure, perovskite precursor solution, perovskite composite thin film layer and preparation method Download PDF

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CN115084391A
CN115084391A CN202210889273.0A CN202210889273A CN115084391A CN 115084391 A CN115084391 A CN 115084391A CN 202210889273 A CN202210889273 A CN 202210889273A CN 115084391 A CN115084391 A CN 115084391A
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perovskite
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王有生
刘立明
马亚婕
麦耀华
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Jinan University
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Abstract

The invention discloses a perovskite solar cell with a hole interface gradient structure, which sequentially comprises a transparent conductive film FTO, a hole transport layer with an interface gradient structure, and Al 2 O 3 A thin film layer and a perovskite composite thin film layer; the hole transport layer sequentially comprises a lithium-doped nickel oxide thin film layer, a nickel oxide thin film layer and poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine]A thin film layer; the perovskite film is F4-TCNQ- (OAm) 2 PbI 4 ‑FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 . The invention also discloses a perovskite precursor solution, a perovskite composite thin film layer and a preparation method thereof. The invention effectively solves the problem of trans-plane structure of calcium and titaniumThe problem that holes generated by light induction in the mine solar cell are transmitted to the transparent conductive film FTO, the barrier is high, and the energy level between interfaces is not matched is solved.

Description

Perovskite solar cell with hole interface gradient structure, perovskite precursor solution, perovskite composite thin film layer and preparation method
Technical Field
The invention relates to the field of solar cells, in particular to a perovskite solar cell with a hole interface gradient structure, a perovskite precursor solution, a perovskite composite thin film layer and a preparation method thereof.
Background
Based on inorganic nickel oxide (NiO) x ) The trans-perovskite solar cell has great potential in the aspects of preparing high-stability and low-cost large-area photovoltaic modules, laminated cells and the like. However, the large open-circuit voltage and fill factor loss have become constraints to further promote NiO x The main factors of the performance of the trans-perovskite solar cell.
In NiO x In the trans-perovskite solar cell, NiO is optimized through an interface engineering strategy x The surface or the effective hole transmission gradient structure is constructed, so that the non-radiative recombination loss of the device is reduced, and the efficiency of the device is improved.
In the patent (CN106531888B) of high et al, porphyrin derivatives are used for interface modification of hole transport layer/perovskite layer in an inverted perovskite solar cell, although the morphology of the perovskite layer is adjusted and the defect density is reduced, the problems of mismatch of hole interface energy levels and stability are still not solved.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a perovskite solar cell with a hole interface gradient structure, which effectively solves the problems that holes generated by light induction in a perovskite solar cell with a trans-planar structure are transmitted to a transparent conductive film FTO (fluorine doped oxide) to have higher potential barrier and the energy levels between interfaces are not matched.
The invention also aims to provide a perovskite precursor solution, and the defect density of the prepared perovskite thin film is low.
Still another object of the present invention is to provide a perovskite composite thin film layer and a method for preparing the same.
The purpose of the invention is realized by the following technical scheme:
the perovskite solar cell with the hole interface gradient structure sequentially comprises a transparent conductive film FTO, a hole transport layer with the interface gradient structure and Al 2 O 3 Film layerAnd a perovskite composite thin film layer;
the hole transport layer sequentially comprises a lithium-doped nickel oxide thin film layer, a nickel oxide thin film layer and a poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ] thin film layer;
the perovskite composite thin film layer is prepared from a perovskite precursor solution; the perovskite precursor solution comprises the following components dissolved in a solvent in parts by weight:
Figure BDA0003766915280000021
preferably, PEA is further arranged on the perovskite composite thin film layer 2 PbI 4 Two-dimensional perovskite thin film layer.
Preferably, the perovskite composite thin film layer contains a two-dimensional perovskite (OAm) 2 PbI 4 And three-dimensional perovskite FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 。
Preferably, the solvent comprises DMF and DMSO, wherein the volume ratio of DMF to DMSO is (0.8-0.86): (0.2-0.25).
Preferably, the hole transport layer with the interface gradient structure has a gradual valence band structure, and the valence band structure is-4.98 eV, -5.1eV and-5.2 eV in sequence.
Preferably, the perovskite solar cell with the hole interface gradient structure has the following structure:
FTO/Li:NiO x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 PCBM/BCP/Ag; wherein Li is NiO x Is a lithium-doped nickel oxide film layer; NiO x Is a nickel oxide film layer; PTAA is poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine]A thin film layer; al (Al) 2 O 3 Is mesoporous alumina; F4-TCNQ- (OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 The perovskite composite thin film layer is characterized in that F4-TCNQ is p-type organic material 2,3,5, 6-tetrafluoro-7, 7',8,8' -tetracyanodimethyl p-benzoquinone; (OAm) 2 PbI 4 Is a two-dimensional perovskite; FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 Is a three-dimensional trihalide perovskite; PEA 2 PbI 4 Is a two-dimensional perovskite thin film layer; PCBM is an electron transport layer; BCP is a buffer layer; ag is the top electrode.
A perovskite precursor solution comprising, by weight, the following components dissolved in a solvent:
Figure BDA0003766915280000022
Figure BDA0003766915280000031
the preparation method of the perovskite composite thin film layer comprises the steps of carrying out spin coating on the perovskite precursor solution, carrying out anti-solvent treatment by utilizing ethyl acetate in the spin coating process, and carrying out heat treatment to obtain the gradient perovskite composite thin film layer.
Preferably, the heat treatment specifically comprises: heating for 18-22 minutes at 95-105 ℃.
The perovskite composite thin film layer is prepared by the preparation method of the perovskite composite thin film layer.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the perovskite solar cell with the hole interface gradient structure constructs a hole transport layer with the interface gradient structure: FTO/Li NiO x /NiO x (ii)/PTAA; wherein Li is NiO x The valence band (-4.98eV) is matched with the work function (-4.7eV) of the transparent conductive film FTO, so that the hole transport barrier is effectively reduced; in addition, the three hole transport layers further construct a gradually-changed valence band structure which is sequentially-4.98 eV, -5.1eV and-5.2 eV, and the structure is favorable for enhancing hole transport; at the same timeThe invention adopts a perovskite film F4-TCNQ- (OAm) with gradient 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 As a light absorbing layer; compared with an undoped perovskite film (the band gap is-1.58 eV, and the valence band is 5.80eV), F4-TCNQ and OAmI are simultaneously doped to effectively adjust the band gap of the perovskite film (the band gap is-1.56 eV, and the valence band is-5.3 eV), so that the valence band (-5.71eV) and the conduction band (-4.15eV) of the perovskite composite film are respectively matched with the hole transport layer and the electron transport layer, an effective hole and electron transport path is further constructed, and non-radiative recombination and interface defects are inhibited.
(2) The perovskite solar cell with the hole interface gradient structure has higher efficiency.
(3) The perovskite precursor solution of the invention forms a two-dimensional (2D) perovskite (OAm) by adding oleylamine iodide (OAmI) 2 PbI 4 The appearance of 2D perovskites suppresses three-dimensional (3D) perovskites FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 And the defect density of the prepared perovskite composite thin film layer is low. The 2D perovskite can effectively occupy the crystal boundary of the 3D perovskite thin film to form a 2D-3D-2D crystal structure, so that the defect state density at the crystal boundary is reduced, non-radiative recombination is inhibited, and finally charge transmission is promoted.
(4) The perovskite precursor solution effectively adjusts the band gap of the perovskite thin film by doping p-type organic molecules F4-TCNQ.
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FIG. 1 shows FTO/Li: NiO prepared by an example of the present invention x (a)、FTO/Li:NiO x /NiO x (b)、FTO/Li:NiO x /NiO x E of/PTAA (c) films F Fermi level test results.
FIG. 2 shows FTO/Li: NiO prepared by the example of the present invention x (a)、FTO/Li:NiO x /NiO x (b)、FTO/Li:NiO x /NiO x E of/PTAA (c) films cut-off Binding energy test results.
FIG. 3 shows the results of testing the band gap of thin films prepared from perovskite precursor solutions without additive (a), with the addition of F4-TCNQ (b), with the addition of F4-TCNQ and OAmI (c).
FIG. 4 is a film E prepared from a perovskite precursor solution without additives (a), with addition of F4-TCNQ (b), with addition of F4-TCNQ and OAmI (c) cut-off Binding energy test results.
FIG. 5 is E of a film prepared from a perovskite precursor solution without additive (a), with addition of F4-TCNQ (b), with addition of F4-TCNQ and OAmI (c) F Fermi level test results.
FIG. 6 shows FTO/Li NiO prepared by an example of the present invention x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 Energy level diagram of battery with/PCBM/BCP/Ag structure.
Fig. 7 is a graph of GIWAXS bulk test results for additive-free perovskite composite thin films according to embodiments of the present invention.
FIG. 8 is a graph showing the results of a GIWAXS bulk test of a perovskite composite thin film to which F4-TCNQ was added according to an example of the present invention.
FIG. 9 is a graph of the results of a GIWAXS bulk test with the addition of F4-TCNQ and OAmI perovskite composite thin films according to an embodiment of the present invention.
FIG. 10 is a low resolution TEM image, a high resolution TEM image and a fast Fourier transform crystal phase image at the 3D/2D perovskite interface and perovskite phase of an embodiment of the invention.
Fig. 11 is a graph comparing the performance of the perovskite solar cell having the hole interface gradient structure according to the embodiment of the present invention and the control group.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Examples
In one embodiment of the invention, the preparation method of the perovskite solar cell with the hole interface gradient structure comprises the following steps:
(1) preparation of lithium-doped nickel oxide solution: dissolving 0.04g of lithium carbonate in 3mL of distilled water and 1mL of ethanol to fully dissolve the lithium carbonate, and marking the lithium carbonate as solution A; 0.25g of Ni (OCOCH) 3 ) 2 ·4H 2 Dissolving O in 10mL of absolute ethanol and 60 mu L of ethanol amine mixed solvent, and heating at 60 ℃ for 30 minutes to make the solution appear light blue, clear and transparent and marked as solution B; 1ml of the solution A is mixed with 4ml of the solution B to prepare the required lithium-doped nickel oxide solution, which is marked as solution C.
(2) Preparation of lithium-doped Nickel oxide thin film (FTO/Li: NiO) x ): spin coating (4000 rpm for 30s) the C solution on the cleaned FTO substrate, and heating at 200 deg.C for 5 min to obtain FTO/Li: NiO x A film.
(3)FTO/Li:NiO x /NiO x Preparing a film: spin coating (4000 rpm, 30s) the solution B on cleaned FTO/Li: NiO x Heating on the film for 30 minutes at 450 ℃ to obtain high-quality FTO/Li: NiO x /NiO x A film.
(4)FTO/Li:NiO x /NiO x Preparation of PTAA films: spin-coating a PTAA (concentration of 0.2mg/mL to 0.5mg/mL, rotation speed of 6000rpm, time of 30s) solution on cleaned FTO/Li: NiO x /NiO x On a film and heated at 120 ℃ for 10 minutes.
(5)FTO/Li:NiO x /NiO x /PTAA/Al 2 O 3 Preparing a film: spin-on Al 2 O 3 (the concentration is 0.2 wt% -0.6 wt%, the rotating speed is 3500rpm, the time is 30s) the solution is in FTO/Li: NiO x /NiO x The annealing temperature on the/PTAA film was 120 ℃ and the annealing time was 10 minutes.
(6) Preparation of perovskite composite thin film layers (PCs): spin-coating perovskite composite precursor (70-73 mg FAI, 20-25 mg PbI) 2 ，10～15mg PbBr 2 4-5 mg MABr, 8-9 mg MACl, 0.7-0.8 mg F4-TCNQ and 0.5-0.8 mg oleylamine iodide (OAmI) dissolved in 0.8-0.86mL DMF and 0.2-0.25mL DMSO solvent) in a clean FTO/Li NiO x /NiO x /PTAA/Al 2 O 3 On the film, using ethyl acetate to carry out anti-solvent treatment in the spin coating process, finally heating for 20 minutes at 100 ℃ to form a 2D/3D perovskite-F4-TCNQ composite film layer, and constructing FTO/Li: NiO x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 Is a structured film.
Wherein the perovskite composite thin film layer contains two-dimensional perovskite (OAm) 2 PbI 4 And three-dimensional perovskite FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 。
(7) Constructing a 2D/3D/2D perovskite structure:
spin coating PEAI (0.5-2 mg/mL, preferably 1mg/mL, the spin speed is 1500 rpm-2500 rpm, preferably 2000rpm, the spin coating time is 30-50 s, preferably 40s) in FTO/Li: NiO solution x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 The annealing temperature on the film is 120 ℃, and the annealing time is 10 minutes.
(8) Preparing a complete device: sequentially spin-coating and thermal steaming to finally construct a device structure
FTO/Li:NiO x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 /PCBM/BCP/Ag。
And (3) testing:
for the FTO/Li NiO prepared by the embodiment of the invention x 、FTO/Li:NiO x /NiO x 、FTO/Li:NiO x /NiO x Ultraviolet electron spectroscopy (UPS) tests of the/PTAA films showed that the three films had different E's as shown in FIG. 1 F The fermi level.
For the FTO/Li NiO prepared by the embodiment of the invention x 、FTO/Li:NiO x /NiO x 、FTO/Li:NiO x /NiO x The UV-photoelectron spectroscopy (UPS) test of the/PTAA film showed that the three films had different E's as shown in FIG. 2 cut-off Binding energy.
The perovskite thin film is prepared by respectively using perovskite precursor solutions without additives, added with F4-TCNQ, added with F4-TCNQ and OAmI, solar cells with consistent structures are constructed, and band gap and ultraviolet light electron spectrum UPS tests are respectively carried out on the solar cells, and the results are respectively shown in figures 3-5.
FIG. 6 shows FTO/Li NiO prepared by an example of the present invention x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 The energy level diagram of the battery with the structure of/PCBM/BCP/Ag shows that the introduction of the additional interface layer and the additive can effectively adjust the energy level structure of the battery to form a hole transport structure with gradient.
The perovskite thin films without additives, added with F4-TCNQ, added with F4-TCNQ and OAmI are subjected to GIWAXS bulk phase test characterization, and the results are respectively shown in figures 7-9, so that after the surface of the 3D perovskite thin film is treated by PEAI, a 2D perovskite layer can be constructed on the surface of the perovskite thin film, but a part of PbI can still be observed 2 Residue (fig. 7); after introduction of OAmI, excess PbI 2 Is completely reacted to form 2D perovskite (OAm) 2 PbI 4 (FIG. 8); when F4-TCNQ was introduced, the crystallization of the perovskite thin film was not affected (FIG. 9).
In FIG. 10, (a), (b) and (c) are respectively a low resolution TEM image, a high resolution TEM image and a fast Fourier transform crystal phase image at the 3D/2D perovskite interface; (d) and (e) low resolution, high resolution TEM images and fast fourier transform crystal phase images of the perovskite phase, respectively, wherein the upper and lower two images in (f) are fast fourier transform crystal phase images of 2D and 3D perovskites, respectively. As can be seen from the figure, 3DPerovskite surface formation 2D (PEA) 2 PbI 4 Meanwhile, a 2D/3D perovskite heterojunction structure is formed in a bulk phase, and finally a 2D/3D/2D perovskite heterojunction film can be constructed.
Perovskite solar cell (experimental group) and comparison group (FTO/NiO device structure) with hole interface gradient structure prepared in the embodiment x /FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 /PCBM/BCP/Ag, i.e. no Li: NiO in the control group device x Layer, no OAmI and F4-TCNQ additive) properties are shown in fig. 11 and table 1.
Table 1 performance testing of perovskite solar cells of the invention and a control.
Figure BDA0003766915280000061
Figure BDA0003766915280000071
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (10)

1. The perovskite solar cell with the hole interface gradient structure is characterized by sequentially comprising a transparent conductive film FTO, a hole transport layer with the interface gradient structure and Al 2 O 3 A thin film layer and a perovskite composite thin film layer;
the hole transport layer sequentially comprises a lithium-doped nickel oxide thin film layer, a nickel oxide thin film layer and a poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine ] thin film layer;
the perovskite composite thin film layer is prepared from a perovskite precursor solution; the perovskite precursor solution comprises the following components dissolved in a solvent in parts by weight:
Figure FDA0003766915270000011
2. the perovskite solar cell of a hole interface gradient structure as claimed in claim 1, wherein PEA is further provided on the perovskite composite thin film layer 2 PbI 4 Two-dimensional perovskite thin film layer.
3. The perovskite solar cell of a hole interface gradient structure as claimed in claim 1, wherein the perovskite composite thin film layer contains a two-dimensional perovskite (OAm) 2 PbI 4 And three-dimensional perovskite FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 。
4. The hole interface gradient structured perovskite solar cell according to claim 1, wherein the solvent comprises DMF and DMSO, wherein the volume ratio of DMF and DMSO is (0.8-0.86): (0.2-0.25).
5. The perovskite solar cell of the hole interface gradient structure as claimed in claim 1, wherein the hole transport layer with the interface gradient structure has a graded valence band structure, and the valence band is-4.98 eV, -5.1eV and-5.2 eV in sequence.
6. The perovskite solar cell of the hole interface gradient structure as claimed in claim 1, characterized in that it has the structure:
FTO/Li:NiO x /NiO x /PTAA/Al 2 O 3 /F4-TCNQ-(OAm) 2 PbI 4 -FA 0.93 MA 0.07 Pb(I 0.79 Br 0.07 Cl 0.14 ) 3 /PEA 2 PbI 4 /PCBM/BCP/Ag。
7. a perovskite precursor solution characterized by comprising, by weight, the following components dissolved in a solvent:
Figure FDA0003766915270000021
8. the preparation method of the perovskite composite thin film layer is characterized in that the perovskite precursor solution of claim 7 is subjected to spin coating, ethyl acetate is used for anti-solvent treatment in the spin coating process, and the gradient perovskite composite thin film layer is obtained after heat treatment.
9. The method for producing a perovskite composite thin film layer according to claim 8, wherein the heat treatment is specifically: heating for 18-22 minutes at 95-105 ℃.
10. A perovskite composite thin film layer produced by the method for producing a perovskite composite thin film layer according to any one of claims 8 to 9.
CN202210889273.0A 2022-07-27 2022-07-27 Perovskite solar cell with hole interface gradient structure, perovskite precursor solution, perovskite composite thin film layer and preparation method Pending CN115084391A (en)

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CN115988945A (en) * 2022-12-15 2023-04-18 嘉庚创新实验室 Intermediate material, application thereof and preparation method of perovskite layer
CN116456790A (en) * 2023-06-19 2023-07-18 北京曜能科技有限公司 Perovskite film preparation method, perovskite solar cell and laminated cell
WO2024098655A1 (en) * 2022-11-10 2024-05-16 杭州纤纳光电科技有限公司 Multi-stage electron blocking thin film, perovskite solar cell, and preparation method

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WO2024098655A1 (en) * 2022-11-10 2024-05-16 杭州纤纳光电科技有限公司 Multi-stage electron blocking thin film, perovskite solar cell, and preparation method
CN115988945A (en) * 2022-12-15 2023-04-18 嘉庚创新实验室 Intermediate material, application thereof and preparation method of perovskite layer
CN115988945B (en) * 2022-12-15 2023-09-22 嘉庚创新实验室 Intermediate material, application thereof and preparation method of perovskite layer
CN116456790A (en) * 2023-06-19 2023-07-18 北京曜能科技有限公司 Perovskite film preparation method, perovskite solar cell and laminated cell
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