CN110707221B - Application of amino acid ionic liquid in preparation of perovskite layer in perovskite photoelectric device - Google Patents
Application of amino acid ionic liquid in preparation of perovskite layer in perovskite photoelectric device Download PDFInfo
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- H—ELECTRICITY
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Abstract
The invention discloses an application of amino acid ionic liquid in preparing perovskite layer in perovskite photoelectric device, wherein the amino acid ionic liquid is amino acid salt ionic liquid or amino acid ester ionic liquid, and the general formula of the amino acid salt ionic liquid is [ A ]] n+ [X ‑ ] n The general formula of the amino acid ester ionic liquid is [ HA ] 1 COOR] + X ‑ Wherein A is an amino acid, A 1 Is a part of the A molecule except carboxyl, n has a value ranging from 1 to 4, X ‑ And R represents an anion, and is an alkyl group having 1 to 3 carbon atoms. The research shows that the amino acid ion liquid can regulate the surface morphology of the perovskite layer, so that the performance of the formed perovskite photoelectric device is improved, and the perovskite photoelectric device has great application value in the field of perovskite photoelectric devices.
Description
Technical Field
The invention relates to an amino acid ionic liquid, in particular to application of the amino acid ionic liquid in preparing a perovskite layer in a perovskite photoelectric device.
Background
Solar technology is an effective means to solve the world energy crisis, while high efficiency, low cost solar cells are the basis of photovoltaic systems. As a third generation solar cell, since 2009, perovskite solar cells have been receiving attention from researchers because of their high light absorption coefficient, high carrier mobility, long carrier transport distance, low cost, solution processability, and the like. In a few years, the photoelectric conversion efficiency of the perovskite solar cell breaks through from 3.8% to 22.7%. For perovskite solar cells, how to improve the photoelectric conversion efficiency and stability of the perovskite solar cells is a main problem in research at present.
The growth of perovskite crystals is a complex phase change process, and different factors such as solution, temperature, solvent, additives and the like in a reaction system can cause the difference of the morphology and the structure of the final crystals. In a planar heterojunction perovskite solar cell, the structure of the solar cell is influenced by interface effect and surface tension during perovskite crystallization, so that the perovskite thin film can be too fast in crystallization speed and poor in film forming property, and pores of a perovskite layer are increased and surface roughness is increased. The hole transport layer or the electron transport layer deposited later can directly contact the compact layer through the holes, so that the leakage current of the battery is increased. However, perovskite crystals with lattice distortion have great influence on parameters such as band gap, carrier mobility, interface carrier injection and the like of the perovskite thin film. These factors can lead to a significant reduction in the performance of planar heterojunction perovskite solar cell devices, greatly limiting the development of perovskite solar cell technology. Therefore, preparing a perovskite crystal film with high quality and low defect state, and further improving the photoelectric conversion efficiency, stability and repeatability of the battery are one of key problems to be solved in the field. Currently, researchers have adopted various means to regulate the quality of perovskite layers, such as 2015, huang Jinsong et al, to control crystal growth and crystal morphology by inhibiting the rapid crystallization of lead iodide by adding a strongly coordinating solvent DMSO to a common DMF solvent. In 2012, snaith et al changed the degree of crystallization of lead methylamine iodide by introducing chlorine-containing compounds into the precursor solution, reduced the defects of the perovskite thin film, and increased the carrier diffusion length.
Ionic liquids are liquids that are composed entirely of ions, typically composed of a specific volume of relatively large structurally asymmetric organic cations and a smaller volume of anions. The ionic liquid is of various kinds, and theoretically any given organic cations and anions can be combined into the ionic liquid, so that different kinds of ionic liquids can be obtained by changing the kinds of the organic cations and anions. Amino acid ionic liquids are one of ionic liquids, and natural amino acids and their derivatives can serve as both anions and cations of the ionic liquid, such as glycine nitrate (GlyNO 3 ) 1-ethyl-3-methyl-imidazole glycinate (emigye), and the like. Amino acid ionic liquids are highly thermally stable, similar to conventional ionic liquids, and in addition have their unique propertiesThe material has a stronger hydrogen bond network structure, and can dissolve DNA and the like. At present, the performance research of the ionic liquid based on amino acid is mainly focused on chiral catalysis, and no research on the morphology regulation of a perovskite layer is discovered so far.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides application of the amino acid ionic liquid in preparing a perovskite layer in a perovskite photoelectric device, and researches show that the amino acid ionic liquid has the effect of regulating and controlling the morphology of the perovskite layer, and is beneficial to improving the performance of the perovskite photoelectric device.
The technical scheme adopted by the invention is as follows:
in a first aspect, the invention provides an application of an amino acid ionic liquid in preparing a perovskite layer in a perovskite photoelectric device, wherein the amino acid ionic liquid is an amino acid ionic liquid or an amino acid ester ionic liquid, and the general formula of the amino acid ionic liquid is [ A ]] n+ [X - ] n The general formula of the amino acid ester ionic liquid is [ HA ] 1 COOR] + X - Wherein A is an amino acid, A 1 Is a part of the A molecule except carboxyl, n has a value ranging from 1 to 4, X - And R represents an anion, and is an alkyl group having 1 to 3 carbon atoms.
According to some embodiments of the present invention, the amino acid is selected from glycine, D-methionine, L-methionine, DL-methionine, D-alanine, L-alanine, DL-alanine, D-valine, L-valine, DL-valine, D-leucine, L-leucine, DL-leucine, D-isoleucine, L-alanine, L-valine, L-leucine, L-valine, L-leucine, L leucine, L leucine DL-isoleucine, D-phenylalanine, L-phenylalanine, DL-phenylalanine, D-cysteine, L-cysteine, DL-cysteine, D-cystine, L-cystine, DL-cystine, D-threonine, L-threonine, DL-threonine, D-glutamic acid, L-cysteine, L-cystine L-glutamic acid, DL-glutamic acid, D-glutamine, L-glutamine, DL-glutamine, D-aspartic acid, L-aspartic acid, DL-aspartic acid, D-asparagine, L-asparagine, DL-asparagine, D-methionine, L-methionine, DL-methionine, D-serine, L-serine, DL-serine, D-proline, L-proline, DL-proline, D-tyrosine, L-tyrosine, DL-tyrosine, D-tryptophan, L-tryptophan, DL-tryptophan, D-lysine, L-lysine, DL-lysine, D-arginine, L-arginine, DL-arginine, D-histidine, L-histidine, DL-histidine, D-ornithine, L-ornithine, DL-ornithine, beta-alanine, 2-aminobutyric acid, 3-aminobutyric acid, 4-aminobutyric acid, 2-aminoisobutyric acid, 3-aminoisobutyric acid, 2-aminopentanoic acid, 2-aminocaproic acid, 6-aminocaproic acid, o-aminophenylpropionic acid, p-aminophenylpropionic acid, m-aminophenylpropionic acid.
According to some embodiments of the invention, X - Selected from Cl - (chloride ions), br - (Bromide ion), I - (iodide ion), NO 3 - (nitrate radical), clO 4 - (perchlorate radical), CF 3 CO 2 - (trifluoroacetate), CH 3 CO 2 - (acetate radical), NTf 2 - (bis-trifluoromethanesulfonyl) PF 6 - (hexafluorophosphate) BF 4 - (tetrafluoroborate) CF 3 SO 3 - (triflate).
According to some embodiments of the invention, the perovskite photovoltaic device is a perovskite solar cell.
In a second aspect of the invention there is provided an anti-solvent for the preparation of a perovskite layer comprising an amino acid ionic liquid as described in the application above.
According to some embodiments of the invention, benzene chloride is also included.
According to some embodiments of the invention, the mass fraction of the amino acid ionic liquid in the antisolvent is 0.01-2 wt%.
In a third aspect of the present invention, there is provided a method for producing a perovskite solar cell, comprising the step of producing a perovskite layer by an anti-solvent method, wherein the anti-solvent used is the anti-solvent for producing a perovskite layer as described above.
According to some embodiments of the invention, the steps for preparing the perovskite layer using the antisolvent method are specifically: and (3) coating the perovskite precursor solution on a substrate, dripping the antisolvent in the coating process, and then annealing at 80-100 ℃ to obtain the perovskite layer.
In a fourth aspect of the present invention, there is provided a perovskite solar cell manufactured according to the above-described method of manufacturing a perovskite solar cell.
The embodiment of the invention has the beneficial effects that:
according to the embodiment of the invention, the amino acid ionic liquid is used for effectively reducing the crystallization rate of perovskite, so that a perovskite layer with larger crystallinity and lower roughness is formed, the defect of the perovskite layer is reduced, the band gap of the perovskite active layer is changed, and the leakage current phenomenon of a perovskite solar photoelectric device is effectively reduced.
Drawings
FIG. 1 is a surface topography of the perovskite layer produced in example 1 and the perovskite layer of comparative example 1;
fig. 2 is a graph showing performance curves of the solar cell manufactured in example 1 and the solar cell manufactured in comparative example 1.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Example 1
In the embodiment, the D-phenylalanine methyl ester hexafluorophosphate ionic liquid is selected as an object, and the influence of the D-phenylalanine methyl ester hexafluorophosphate ionic liquid on the morphology of a perovskite layer and the performance of a solar cell is researched, wherein the specific experimental process is as follows:
preparing D-phenylalanine methyl ester hexafluorophosphate ionic liquid:
taking 0.10mol of D-phenylalanine methyl ester hydrochloride and 0.12mol of potassium hexafluorophosphate, stirring in 20mL of acetonitrile for 50h, filtering to obtain filtrate, and removing the solvent from the filtrate by rotary evaporation to obtain the D-phenylalanine methyl ester hexafluorophosphate ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared D-phenylalanine methyl ester hexafluorophosphate ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the D-phenylalanine methyl ester hexafluorophosphate ionic liquid is 0.1wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 8s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 10min on a hot table at the temperature of 80 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 20mg/mL PC 61 And spin-coating the chlorobenzene solution of BM on the perovskite layer at 2000rpm for 30s to obtain the electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 150nm by a vacuum film plating machine.
Comparative example 1: comparative example 1 a solar cell was provided, which was identical to the solar cell structure and the production process in example 1, except that no D-phenylalanine methyl ester hexafluorophosphate ionic liquid was added to the antisolvent of step (5) for producing a perovskite layer.
The surface morphologies of the perovskite layer obtained in this example and the perovskite layer in comparative example 1 were subjected to SEM characterization, and the results are shown in fig. 1, in which fig. 1 (a) shows an SEM image of the perovskite layer in a perovskite solar cell to which a D-phenylalanine methyl ester hexafluorophosphate ionic liquid was added, and fig. 1 (b) shows an SEM image of the perovskite layer in a perovskite solar cell to which the ionic liquid was not added. As can be seen from the figure 1, the grain size of the perovskite layer prepared by using the antisolvent containing the D-phenylalanine methyl ester hexafluorophosphate ionic liquid is larger, the edge density is smaller, and the result shows that the D-phenylalanine methyl ester hexafluorophosphate ionic liquid has the effect of regulating the morphology of the perovskite layer.
The solar cells produced in this example and the solar cells produced in comparative example 1 were tested for performance, and the results are shown in FIG. 2, which shows that the results are 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) Short-circuit current (Jsc) = 22.81mA/cm of the solar cell in this embodiment 2 Open circuit voltage (Voc) =1.07V, fill Factor (FF) =0.76, photoelectric Conversion Efficiency (PCE) =18.5%, and short circuit current (Jsc) = 22.51mA/cm for the solar cell in comparative example 1 2 Open circuit voltage (Voc) =1.02V, fill Factor (FF) =0.73, photoelectric Conversion Efficiency (PCE) =16.7%. The results show that the use of D-phenylalanine methyl ester hexafluorophosphate ionic liquid can improve the performance of solar cells.
Example 2
The embodiment provides a solar cell, wherein an amino acid ionic liquid in an antisolvent used in the process of preparing a perovskite layer is L-alanine hexafluorophosphate ionic liquid, and the specific experimental process is as follows:
preparing L-alanine hexafluorophosphate ionic liquid:
dissolving 0.10mol L-alanine and 0.10mol hexafluorophosphate in 10mL water, heating to 60 ℃, vacuum drying for 12h, and cooling to obtain the L-alanine hexafluorophosphate ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared L-alanine hexafluorophosphate ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the L-alanine hexafluorophosphate ionic liquid is 0.2wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 7s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 10min on a hot table at a temperature of 85 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 20mg/mL PC 61 And spin-coating the chlorobenzene solution of BM on the perovskite layer at 2000rpm for 30s to obtain the electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 150nm by a vacuum film plating machine.
The performance of the solar cell manufactured in this example was tested, and the result showed that it was 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) Short-circuit current (Jsc) =22.13 mA/cm of the solar cell in the present embodiment 2 The results of the open circuit voltage (Voc) =1.08V, the Fill Factor (FF) =0.74, and the Photoelectric Conversion Efficiency (PCE) =17.7 show that the solar cell obtained by treating with the D-phenylalanine methyl ester hexafluorophosphate ionic liquid has excellent photoelectric conversion performance.
Example 3
The embodiment provides a solar cell, wherein the amino acid ionic liquid in an antisolvent used in the process of preparing a perovskite layer is selected from D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid and DL-valine bis (trifluoromethanesulfonyl) imide ionic liquid, and the specific experimental process is as follows:
preparing D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid:
taking 0.10mol of D-leucine hydrochloride and 0.12mol of lithium bis (trifluoromethanesulfonyl) imide, dissolving in 1mL of water, reacting for 60 hours, taking the supernatant, vacuum drying for 12 hours, and cooling to obtain the D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid.
Preparing DL-valine bis (trifluoromethanesulfonyl) imide ionic liquid:
dissolving 0.10mol of DL-valine hydrochloride and 0.12mol of lithium bis (trifluoromethanesulfonyl) imide in 1mL of water, reacting for 60h, taking the supernatant, vacuum drying for 12h, and cooling to obtain the DL-valine bis (trifluoromethanesulfonyl) imide ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid and DL-valine bis (trifluoromethanesulfonyl) imide ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid is 0.1wt% and the mass fraction of the DL-valine bis (trifluoromethanesulfonyl) imide ionic liquid is 0.15wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 7s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 8min on a hot table at a temperature of 90 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 20mg/mL PC 61 And spin-coating the chlorobenzene solution of BM on the perovskite layer at 2000rpm for 30s to obtain the electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 150nm by a vacuum film plating machine.
The performance of the solar cell manufactured in this example was tested, and the result showed that it was 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) The present inventionShort-circuit current (Jsc) =23.17 mA/cm of solar cell in example 2 The results of the open circuit voltage (Voc) =1.08V, the Fill Factor (FF) =0.75 and the Photoelectric Conversion Efficiency (PCE) =18.8 show that the solar cell obtained by treating with the D-leucine bis (trifluoromethanesulfonyl) imide salt ionic liquid and the DL-valine bis (trifluoromethanesulfonyl) imide salt ionic liquid has excellent photoelectric conversion performance.
Example 4
The embodiment provides a solar cell, wherein the amino acid ionic liquid in the antisolvent used in the process of preparing a perovskite layer is selected from L-serine methyl ester hexafluorophosphate ionic liquid and L-serine ethyl ester hexafluorophosphate ionic liquid, and the specific experimental process is as follows:
preparing L-serine methyl ester hexafluorophosphate ionic liquid:
taking 0.10mol L-serine methyl ester hydrochloride and 0.12mol potassium hexafluorophosphate, stirring in 1mL of water for 60h, taking the lower layer of clear liquid, vacuum drying for 12h, and cooling to obtain the L-serine methyl ester hexafluorophosphate ionic liquid.
Preparing L-serine ethyl ester hexafluorophosphate ionic liquid:
taking 0.10mol L-serine ethyl ester hydrochloride and 0.12mol potassium hexafluorophosphate, stirring in 1mL of water for 60h, taking the lower layer of clear liquid, vacuum drying for 12h, and cooling to obtain the L-serine ethyl ester hexafluorophosphate ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared L-serine methyl ester hexafluorophosphate ionic liquid and L-serine ethyl ester hexafluorophosphate ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the L-serine methyl ester hexafluorophosphate ionic liquid is 0.1wt% and the mass fraction of the L-serine ethyl ester hexafluorophosphate ionic liquid is 0.1wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 8s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 10min on a hot table at a temperature of 85 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 20mg/mL PC 61 And spin-coating the chlorobenzene solution of BM on the perovskite layer at 2000rpm for 30s to obtain the electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 150nm by a vacuum film plating machine.
The performance of the solar cell manufactured in this example was tested, and the result showed that it was 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) Short-circuit current (Jsc) =22.69 mA/cm of the solar cell in the present embodiment 2 The results of the open circuit voltage (Voc) =1.06V, the Fill Factor (FF) =0.76, and the Photoelectric Conversion Efficiency (PCE) =18.3 indicate that the solar cell obtained by treating with the L-serine methyl ester hexafluorophosphate ionic liquid and the L-serine ethyl ester hexafluorophosphate ionic liquid has excellent photoelectric conversion performance.
Example 5
The embodiment provides a solar cell, wherein the amino acid ionic liquid in the antisolvent used in the process of preparing a perovskite layer is selected from D-methionine methyl ester hexafluorophosphate ionic liquid and D-methionine methyl ester tetrafluoroborate ionic liquid, and the specific experimental process is as follows:
preparing D-methionine methyl ester hexafluorophosphate ionic liquid:
taking 0.10mol of D-methionine methyl ester hydrochloride and 0.12mol of potassium hexafluorophosphate, stirring in 1mL of water for 60 hours, taking the lower layer of clear liquid, vacuum drying for 12 hours, and cooling to obtain the D-methionine methyl ester hexafluorophosphate ionic liquid.
Preparing D-methionine methyl ester tetrafluoroborate ionic liquid:
taking 0.10mol of D-methionine methyl ester hydrochloride and 0.12mol of sodium tetrafluoroborate, stirring in 1mL of water for 60 hours, taking the lower layer of clear liquid, vacuum drying for 12 hours, and cooling to obtain the D-methionine methyl ester tetrafluoroborate ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared D-methionine methyl ester hexafluorophosphate ionic liquid and D-methionine methyl ester tetrafluoroborate ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the D-methionine methyl ester hexafluorophosphate ionic liquid is 0.2wt% and the mass fraction of the D-methionine methyl ester tetrafluoroborate ionic liquid is 0.3wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 8s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 8min on a hot table at a temperature of 100 ℃ to obtain a perovskite layer.
(6) Preparing an electron transport layer: and spin-coating 20mg/mL PC61BM in chlorobenzene solution at 2000rpm to form a film on the perovskite layer, wherein the spin-coating time is 30s to obtain the electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 150nm by a vacuum film plating machine.
The performance of the solar cell manufactured in this example was tested, and the result showed that it was 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) Short-circuit current (Jsc) =21.98 mA/cm of the solar cell in this example 2 The results of the open circuit voltage (Voc) =1.09V, the Fill Factor (FF) =0.75, and the Photoelectric Conversion Efficiency (PCE) =18.0 indicate that the solar cell obtained by treating with the D-methionine methyl ester hexafluorophosphate ionic liquid and the D-methionine methyl ester tetrafluoroborate ionic liquid has excellent photoelectric conversion performance.
Example 6
The embodiment provides a solar cell, wherein an amino acid ionic liquid in an antisolvent used in a process of preparing a perovskite layer is glycine methyl ester bis (trifluoromethanesulfonyl) imide ionic liquid, and the specific experimental process is as follows:
preparing glycine methyl ester bis (trifluoromethanesulfonyl) imide ionic liquid:
taking 0.10mol of glycine methyl ester hydrochloride and 0.12mol of bis (trifluoromethanesulfonyl) imine lithium, stirring in 1mL of water for 60h, taking the lower layer of clear liquid, vacuum drying for 12h, and cooling to obtain glycine methyl ester bis (trifluoromethanesulfonyl) imine ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared glycine methyl ester bis (trifluoromethanesulfonyl) imine ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the glycine methyl ester bis (trifluoromethanesulfonyl) imine ionic liquid is 0.1wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 8s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 10min on a hot table at the temperature of 80 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 30mg/mL of PC61BM in chlorobenzene is spin-coated to form a film on a perovskite layer at 2500rpm, and the spin-coating time is 30s to obtain an electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 200nm by a vacuum film plating machine.
The performance of the solar cell manufactured in this example was tested,the results are shown at 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) Short-circuit current (Jsc) =20.89 mA/cm of the solar cell in this embodiment 2 The results of the open circuit voltage (Voc) =1.06V, the Fill Factor (FF) =0.63, and the Photoelectric Conversion Efficiency (PCE) =14.0 show that the solar cell obtained by treating with the glycine methyl ester bis (trifluoromethanesulfonyl) imide ionic liquid has excellent photoelectric conversion performance.
Example 7
The embodiment provides a solar cell, wherein the amino acid ionic liquid in an antisolvent used in the process of preparing a perovskite layer is selected from D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid and D-valine bis (trifluoromethanesulfonyl) imide ionic liquid, and the specific experimental process is as follows:
preparing D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid:
taking 0.10mol of D-leucine hydrochloride and 0.12mol of bis (trifluoromethanesulfonyl) imide lithium, stirring in 1mL of water for 60h, taking the lower layer of clear liquid, vacuum drying for 12h, and cooling to obtain the D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid.
Preparing D-valine bis (trifluoromethanesulfonyl) imide ionic liquid:
taking 0.10mol of D-valine and 0.12mol of lithium bis (trifluoromethanesulfonyl) imide, stirring in 1mL of water for 60h, taking the lower layer of clear liquid, vacuum drying for 12h, and cooling to obtain the D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid and D-valine bis (trifluoromethanesulfonyl) imide ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the D-leucine bis (trifluoromethanesulfonyl) imide ionic liquid is 0.1wt% and the mass fraction of the D-valine bis (trifluoromethanesulfonyl) imide ionic liquid is 0.15wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 8s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 10min on a hot table at the temperature of 80 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 30mg/mL of PC61BM in chlorobenzene is spin-coated to form a film on a perovskite layer at 2500rpm, and the spin-coating time is 30s to obtain an electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 200nm by a vacuum film plating machine.
The performance of the solar cell manufactured in this example was tested, and the result showed that it was 100mW/cm 2 Tested under illumination (effective area 0.06 cm) 2 ) Short-circuit current (Jsc) =21.04 mA/cm of the solar cell in this example 2 The results of the open circuit voltage (Voc) =1.07V, the Fill Factor (FF) =0.58 and the Photoelectric Conversion Efficiency (PCE) =13.1 show that the solar cell obtained by treating the D-leucine bis (trifluoromethanesulfonyl) imide salt ionic liquid and the D-valine bis (trifluoromethanesulfonyl) imide salt ionic liquid has excellent photoelectric conversion performance.
Example 8
The embodiment provides a solar cell, wherein an amino acid ionic liquid in an antisolvent used in a process of preparing a perovskite layer is glycine methyl ester bis (trifluoromethanesulfonyl) imide ionic liquid, and the specific experimental process is as follows:
preparing glycine methyl ester bis (trifluoromethanesulfonyl) imide ionic liquid:
taking 0.10mol of glycine methyl ester hydrochloride and 0.12mol of bis (trifluoromethanesulfonyl) imine lithium, stirring in 1mL of water for 60h, taking the lower layer of clear liquid, vacuum drying for 12h, and cooling to obtain glycine methyl ester bis (trifluoromethanesulfonyl) imine ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Preparing an antisolvent: dissolving the prepared glycine methyl ester bis (trifluoromethanesulfonyl) imine ionic liquid in chlorobenzene, and mixing to form an antisolvent, wherein the mass fraction of the glycine methyl ester bis (trifluoromethanesulfonyl) imine ionic liquid is 0.5wt%.
(3) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(4) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(5) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by the spin coating into a constant temperature glove box protected by nitrogen, dripping the perovskite precursor mixed solution onto a hole transmission layer, spin-coating for 8s at a rotation speed of 5000rpm, dripping an anti-solvent, closing a spin coater after dripping the anti-solvent for 3s, and annealing for 10min on a hot table at the temperature of 80 ℃ to obtain the perovskite layer.
(6) Preparing an electron transport layer: 30mg/mL of PC61BM in chlorobenzene is spin-coated to form a film on a perovskite layer at 2500rpm, and the spin-coating time is 30s to obtain an electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 200nm by a vacuum film plating machine.
The performance of the solar cell prepared in this example was tested, and the result shows that the solar cell obtained by treating with glycine methyl ester bis (trifluoromethanesulfonyl) imide ionic liquid has excellent photoelectric conversion performance.
Example 9
The embodiment provides a solar cell, wherein the amino acid ionic liquid in the antisolvent used in the process of preparing a perovskite layer is selected from p-aminobenzene propionic acid nitrate ionic liquid and 2-aminopentanoate acetate ionic liquid, and the specific experimental process is as follows:
preparing p-aminobenzene propionic acid nitrate ionic liquid:
dissolving 0.10mol of p-aminobenzene propionic acid and 0.10mol of 65% nitric acid in 10mL of water, reacting for 24 hours, distilling under reduced pressure at 60 ℃ to remove water, and drying in vacuum for 24 hours to obtain the p-aminobenzene propionic acid nitrate ionic liquid.
Preparing 2-aminopentanoate acetate ionic liquid:
dissolving 0.10mol of 2-aminopentanoic acid and 0.10mol of trifluoroacetic acid in 10mL of water, reacting for 24 hours, distilling under reduced pressure at 60 ℃ to remove water, and drying in vacuum for 24 hours to obtain the 2-aminopentanoic acid acetate ionic liquid.
Preparing a solar cell:
(1) In a constant temperature glove box protected by nitrogen, weighing iodomethylamine and lead iodide with a molar ratio of 1:1, dissolving in N, N-Dimethylformamide (DMF), and heating at a constant temperature of 60 ℃ for 24 hours after full dissolution. And cooling for 0.5h to room temperature to obtain the perovskite precursor mixed solution.
(2) Respectively ultrasonically cleaning the etched ITO conductive glass with an optical cleaner, distilled water, acetone and isopropanol for 20min, blow-drying with nitrogen, then ozone-cleaning with a PLASMA surface cleaner for 15min, blowing with nitrogen, and placing into a dust-free culture dish for standby.
(3) Preparing a hole transport layer: and spin-coating toluene solution of 2mg/mL PTAA on the cleaned ITO conductive glass, controlling the rotation speed to 6000rpm, spin-coating for 35s, and then annealing at 110 ℃ for 20min to form a hole transport layer.
(4) Preparing a perovskite layer: transferring the ITO conductive glass with the PTAA coated by spin into a constant temperature glove box protected by nitrogen, spin-coating the perovskite precursor mixed solution on a hole transport layer at a rotation speed of 5000rpm, and annealing for 10min on a heat table at the temperature of 80 ℃ to obtain a perovskite layer.
(5) Mixing p-aminobenzene propionic acid nitrate ionic liquid and 2-aminovaleric acid acetate ionic liquid to form mixed ionic liquid, soaking a perovskite layer in the mixed ionic liquid for 1h, taking out, flushing with chlorobenzene, and blow-drying with high-purity nitrogen.
(6) Preparing an electron transport layer: 30mg/mL of PC61BM in chlorobenzene is spin-coated to form a film on a perovskite layer at 2500rpm, and the spin-coating time is 30s to obtain an electron transport layer.
(7) Preparing an electron transport layer modification layer: and spin-coating a trifluoroethanol solution of 12mg/mL ZnO on the electron transport layer at 4000rpm for 60s to form an electron transport layer modification layer.
(8) Evaporating a counter electrode: and evaporating a metal aluminum electrode with the thickness of 200nm by a vacuum film plating machine.
The performance of the solar cell prepared in the embodiment is tested, and the result shows that the solar cell obtained by soaking the p-aminobenzene propionic acid nitrate ionic liquid and the 2-aminovaleric acid acetate ionic liquid has excellent photoelectric conversion performance.
Claims (10)
1. An anti-solvent for preparing a perovskite layer is characterized by comprising an amino acid ionic liquid, wherein the amino acid ionic liquid is aminoAn acid salt ionic liquid or an amino acid ester ionic liquid, wherein the general formula of the amino acid salt ionic liquid is [ A ]] n+ [X - ] n The general formula of the amino acid ester ionic liquid is [ HA ] 1 COOR] + X - Wherein A is an amino acid, A 1 Is a part of the A molecule except carboxyl, n has a value ranging from 1 to 4, X - And R represents an anion, and is an alkyl group having 1 to 3 carbon atoms.
2. The antisolvent according to claim 1, characterized in that, the amino acid is selected from glycine, D-methionine, L-methionine, DL-methionine, D-alanine, L-alanine, DL-alanine, D-valine, L-valine, DL-valine, D-leucine, L-leucine, DL-leucine, D-isoleucine, L-alanine, L-valine, L-leucine, L-valine, L-leucine, L leucine L leucine L L-isoleucine, DL-isoleucine, D-phenylalanine, L-phenylalanine, DL-phenylalanine, D-cysteine, L-cysteine, DL-cysteine, D-cystine, L-cystine, DL-cystine, D-threonine, L-threonine, DL-threonine, L-cysteine, L cysteine L D-glutamic acid, L-glutamic acid, DL-glutamic acid, D-glutamine, L-glutamine, DL-glutamine, D-aspartic acid, L-aspartic acid, DL-aspartic acid, D-asparagine, L-asparagine, DL-asparagine, D-methionine, L-methionine, DL-methionine, D-serine, L-serine, DL-serine, D-proline, L-proline, DL-proline, D-tyrosine, L-tyrosine, DL-tyrosine, D-tryptophan, L-tryptophan, DL-tryptophan, D-lysine, L-lysine, DL-lysine, D-arginine, L-arginine, DL-arginine, D-histidine, L-histidine, DL-histidine, D-ornithine, L-ornithine, DL-ornithine, beta-alanine, 2-aminobutyric acid, 3-aminobutyric acid, 4-aminobutyric acid, 2-aminoisobutyric acid, 3-aminoisobutyric acid, 2-aminopentanoic acid, 2-aminocaproic acid, 6-aminocaproic acid, o-aminophenylpropionic acid, p-aminophenylpropionic acid, m-aminophenylpropionic acid.
3. The antisolvent according to claim 1, characterized in that X - Selected from Cl - 、Br - 、I - 、NO 3 - 、ClO 4 - 、CF 3 CO 2 - 、CH 3 CO 2 - 、NTf 2 - 、PF 6 - 、BF 4 - 、CF 3 SO 3 - Any one of them.
4. The antisolvent of claim 1, wherein the perovskite layer is a perovskite layer in a perovskite photovoltaic device.
5. The antisolvent of claim 4, wherein the perovskite photovoltaic device is a perovskite solar cell.
6. An anti-solvent for the preparation of perovskite layers according to any one of claims 1 to 5, further comprising benzene chloride.
7. The anti-solvent for preparing the perovskite layer according to claim 6, wherein the mass fraction of the amino acid ionic liquid in the anti-solvent is 0.01-2 wt%.
8. A method for producing a perovskite solar cell, comprising the step of producing a perovskite layer by an antisolvent method, wherein the antisolvent used is the antisolvent for producing a perovskite layer according to any one of claims 1 to 7.
9. The method for producing a perovskite solar cell according to claim 8, wherein the step of producing a perovskite layer by an antisolvent method specifically comprises: and (3) coating the perovskite precursor solution on a substrate, dripping the antisolvent in the coating process, and then annealing at 80-100 ℃ to obtain the perovskite layer.
10. A perovskite solar cell, characterized in that it is produced according to the method for producing a perovskite solar cell according to claim 8 or 9.
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