CN116002748A - Inverted perovskite solar cell with quantum dots as hole transport layer and preparation method thereof - Google Patents
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Abstract
An inversion perovskite solar cell with quantum dots as hole transport layers and a preparation method thereof relate to the technical field of perovskite solar cells. CdSe or CdS quantum dots are prepared through a gas-heat-liquid reaction method and are applied to hole transport materials of perovskite solar cells. In the quantum dot preparation system, a gas reactant participates in and directly contacts with a liquid reactant, so that the quantum dot preparation system has better gas-liquid mass transfer. The generated sphalerite quantum dot has stronger light absorption capacity, so as to realize the preparation of the high-performance perovskite solar cell. The nano-scale quantum dots are used as a hole transport layer of the perovskite solar cell, so that the photoelectric conversion efficiency of the perovskite solar cell is improved, and the device performance is improved. The high-quality low-cost quantum dot is expected to effectively enhance light capture, form better contact with the perovskite film, can rapidly extract and transmit photo-generated holes, inhibit non-radiative recombination, and is beneficial to improving the performance of the perovskite solar cell.
Description
Technical Field
The invention relates to the technical field of perovskite solar cells, in particular to an inversion perovskite solar cell with quantum dots as hole transport layers and a preparation method thereof.
Background
Perovskite solar cells have attracted attention from numerous researchers due to their high absorption coefficient, adjustable band gap, simple structure, low manufacturing cost, excellent photovoltaic performance, and other advantages. In recent years, due to the contribution of researchers in the directions of perovskite morphology control, battery structure, device physics, interface engineering, energy bands and the like, perovskite solar cells are rapidly developed, and the photoelectric conversion efficiency of the perovskite solar cells is rapidly improved from 3.8% to more than 25%, but a certain gap exists from the limiting efficiency. Research surface, hole transport material is the key factor that restricts perovskite solar cell cost and performance, and hole transport ability weak can cause inside perovskite film to produce serious charge recombination, causes photovoltaic device performance to drop.
In order to solve the technical problem, the invention tries to prepare CdSe or CdS quantum dots, and takes the quantum dots as a hole transport material of the perovskite solar cell, thereby being expected to further improve the efficiency and the stability of the perovskite solar cell.
Disclosure of Invention
In order to solve the technical problems, the invention provides an inversion perovskite solar cell with quantum dots as hole transport layers and a preparation method thereof, wherein high-quality CdSe or CdS quantum dots are prepared by a gas-heat-liquid reaction method and are applied to hole transport materials of the perovskite solar cell, so that the performance of the perovskite solar cell is improved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
first, the invention provides a CdSe or CdS amountPreparation method of sub-point semiconductor material, under the protection of nitrogen flow, heating a mixture composed of 100-500 mg of cadmium oxide (CdO) powder, 50-150 mg of tri-n-octyl phosphine oxide (TOPO), 1-2 mL of Oleic Acid (OA) and 5-15 mL of Octadecene (ODE), and continuously introducing H below the liquid level 2 Se or H 2 S gas, wherein the reaction time is 25-50 min, and the reaction temperature is 190-210 ℃; and after the reaction is finished, centrifuging, washing and ligand exchanging the mixed solution to obtain the CdSe or CdS quantum dot semiconductor material.
As a preferable technical scheme of the preparation method of the quantum dot semiconductor material, the H is as follows 2 The Se gas is prepared from sodium borohydride (NaBH) 4 ) Continuously reacting selenium powder (Se) with deionized water mixture to obtain NaBH 4 The molar ratio between Se is 2-4:1; the H is 2 The S gas is formed by dilute sulfuric acid (H) 2 SO 4 ) And ferrous sulfide (FeS) mixture, H 2 SO 4 The molar ratio of FeS is 2-4:1.
Secondly, the invention also provides an inversion perovskite solar cell, and the structure of the inversion perovskite solar cell is that the hole transport layer is provided with a coating of the CdSe or CdS quantum dot semiconductor material.
Finally, the invention also provides a preparation method of the inversion perovskite solar cell, which comprises the following steps:
1) Cleaning of conductive substrates: sequentially carrying out ultrasonic cleaning on etched FTO or ITO conductive glass for 15-20 min by using detergent, deionized water, acetone, ethanol and isopropanol, and drying the glass by using a nitrogen gun after cleaning;
2) Preparing a hole transport layer: in glove box N 2 Under protection, the conductive glass and poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Uniformly spin-coating CdSe or CdS quantum dot solution on a substrate composed of (PTAA), wherein the spin-coating time is 20-30 s, the spin-coating speed is 3000-3500 rpm, and annealing is performed for 10-15 min at 60-80 ℃ after the spin-coating is finished;
3) Preparing a perovskite layer: spin coating is carried out at the rotation speed of 800-1200 rpm and 4200-4800 rpm respectively, and perovskite precursor solution with the concentration of 1-1.5 g/mL is fully coated on the hole transport layer; after spin coating, placing the substrate on a heating table at 90-110 ℃ for heating for 30-40 min to obtain a perovskite film;
4) And (3) preparing an electron transport layer: [6,6 ] with spin coating concentration of 20-30 mg/mL]-phenyl-C 61 Methyl butyrate (PC) 61 BM) -chlorobenzene solution, spin coating speed of 2500-3500 rpm, spin coating time of 20-40 s, annealing at 80-100 deg.c for 10-15 min after spin coating;
5) Preparing a buffer layer: dissolving 2, 9-dimethyl-4, 7-diphenyl phenanthroline (BCP) in methanol, taking saturated solution, spin-coating, wherein the spin-coating speed is 6000-7000 rpm, the spin-coating time is 20-40 s, and annealing for 10-15 min at 50-70 ℃ after the spin-coating is finished;
6) Preparation of metal electrode: and 5) placing the sample prepared in the step 5) in a thermal evaporation device to evaporate the metal electrode.
As a preferable technical scheme of the invention, in the perovskite solar cell preparation method, the perovskite precursor solution is CH 3 NH 3 PbI 3 The preparation method comprises the following steps: lead iodide (PbI) 2 ) And methyl ammonium iodide (CH) 3 NH 3 I) Mixed in N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, wherein PbI 2 、CH 3 NH 3 I. The molar ratio of DMSO is 1:1:1, the volume ratio of DMF to DMSO is 8:1, mixing and stirring for 40 min.
As another preferable embodiment of the invention, in the perovskite solar cell manufacturing method, the perovskite precursor solution is HC (NH 2 ) 2 PbI 3 The preparation method comprises the following steps: lead iodide (PbI) 2 ) And formamidine hydroiodidate (HC (NH) 2 ) 2 I) Mixed in N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, wherein PbI 2 、HC(NH 2 ) 2 I. The molar ratio of DMSO is 1:1:1, the volume ratio of DMF to DMSO is 8:1, mixing and stirring for 40 min.
Compared with the prior art, the invention has the beneficial effects that:
1) In the traditional technical field, the monodisperse quantum dots are generally synthesized by adopting a traditional heat injection method, and the heat injection method has complicated process and high requirement on synthesis conditions. In the quantum dot preparation system provided by the invention, the gas reactant participates in and directly contacts with the liquid reactant, so that the quantum dot preparation system has better gas-liquid mass transfer. Low temperature, easy control of synthesis route, good product dispersibility, low cost and large-scale synthesis potential. The generated sphalerite quantum dot has stronger light absorption capacity, and then the preparation of the high-performance perovskite solar cell is realized.
2) According to the invention, the nano-scale quantum dots are used as the hole transport layer of the perovskite solar cell, so that the photoelectric conversion efficiency of the perovskite solar cell is improved, and the device performance is improved. The high-quality low-cost quantum dot is expected to effectively enhance light capture, form better contact with the perovskite film, can rapidly extract and transmit photo-generated holes, inhibit non-radiative recombination, and contribute to improving the performance of the perovskite solar cell, and has important significance for developing the high-performance perovskite solar cell.
3) The preparation method has the advantages of simple preparation process, low cost, easy operation, safety and the like.
Drawings
FIG. 1 is a TEM image of CdSe quantum dots prepared according to the invention.
Fig. 2 is a SEM image of the surface of a perovskite thin film prepared according to the present invention.
Fig. 3 is a J-V graph of the perovskite solar cell (experiment No. 5) prepared in example 2 using CdSe quantum dots as hole transport layers, and the perovskite solar cell prepared in comparative example 1 without quantum dots added as hole transport layers.
Detailed Description
Example 1
The preparation method of the inverted perovskite solar cell comprises the following steps:
1) Preparation of CdSe quantum dot semiconductor material: a mixture consisting of cadmium oxide (CdO) powder, 100mg of tri-n-octylphosphinoxide (TOPO), 1.4mL of Oleic Acid (OA) and 8mL of Octadecene (ODE) was heated under nitrogen flow. The experiments are divided into three groups, wherein the weight of cadmium oxide (CdO) powder is 140mg, 280mg and 420mg respectively, and the weight corresponds to Cd: se molar ratio is 1:1, 2:1 and 3:1 respectively, and experiment numbers are 1,2 and 3 respectively.
At the same time, a solution consisting of 130mg sodium borohydride (NaBH) was continuously introduced below the liquid level 4 ) H formed by continuous reaction of 87mg selenium powder (Se) and deionized water mixture 2 Se gas, the reaction time is 50min, and the reaction temperature is 200 ℃. And after the reaction is finished, centrifuging, washing and ligand exchanging the mixed solution to obtain the CdSe quantum dot solution.
The ligand exchange process is as follows: dissolving washed CdSe quantum dots in toluene to obtain a solution A, dissolving 0.2g of mercaptopropionic acid in 10mL of methanol, regulating the pH value of the solution A to 12 by using a saturated solution of NaOH and methanol to obtain a solution B, mixing the solution A and the solution B according to the volume ratio of 1:1, stirring for 30min, centrifuging for 15min (the centrifugal speed is 15000 rpm), pouring out the supernatant, repeating the ligand exchange process for 2 times on the rest precipitate, and dissolving the last precipitate in water to form a CdSe quantum dot aqueous solution wrapped by mercaptopropionic acid, thereby facilitating the subsequent spin coating.
2) Cleaning of conductive substrates: sequentially using detergent, deionized water, acetone, ethanol and isopropanol to ultrasonically clean the etched ITO conductive glass for 20min, and drying the glass by using a nitrogen gun after cleaning.
3) Preparing a hole transport layer: in glove box N 2 Under the protection of ITO conductive glass and poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Uniformly spin-coating the CdSe quantum dot solution prepared in the step 1) on a substrate consisting of (PTAA), wherein the spin-coating time is 30s, the spin-coating speed is 3500rpm, and annealing is performed for 15min at 70 ℃ after the spin-coating is finished.
4) Preparing a perovskite layer: spin coating was performed at 1000rpm and 4500rpm, respectively, and a perovskite precursor solution having a concentration of 1.2g/mL was spin coated and spread over the hole transport layer. And (5) after spin coating, placing the substrate on a heating table at 100 ℃ and heating for 35min to obtain the perovskite film.
Wherein the perovskite precursor solution is CH 3 NH 3 PbI 3 The preparation method comprises the following steps: lead iodide (PbI) 2 ) And methyl ammonium iodide (CH) 3 NH 3 I) Mixed with N, N-Dimethylformamide (DMF) and dimethylformamideIn a sulfoxide base (DMSO) solvent, wherein PbI 2 、CH 3 NH 3 I. The molar ratio of DMSO is 1:1:1, the volume ratio of DMF to DMSO is 8:1, mixing and stirring for 40 min.
5) And (3) preparing an electron transport layer: [6,6 ] with spin-coating concentration of 25mg/mL]-phenyl-C 61 Methyl butyrate (PC) 61 BM) -chlorobenzene solution, spin coating speed of 3000rpm, spin coating time of 30s, annealing at 90 deg.C for 15min after spin coating.
6) Preparing a buffer layer: dissolving 2, 9-dimethyl-4, 7-diphenyl phenanthroline (BCP) in methanol, taking saturated solution, spin-coating, wherein the spin-coating speed is 6500rpm, the spin-coating time is 30s, and annealing for 15min at 60 ℃ after the spin-coating is finished.
7) Preparation of metal electrode: and (3) placing the sample prepared in the step (6) in a thermal evaporation device, and evaporating an 85nm metal electrode.
Table 1 different Cd: influence of CdSe quantum dots with Se concentration ratio on perovskite solar cell performance
As can be seen from table 1, different cds: the CdSe quantum dots prepared by Se concentration ratio have important influence on the efficiency of perovskite solar cells.
Example 2
The preparation method is the same as in example 1, except that the mass of cadmium oxide (CdO) powder is 280mg, corresponding to Cd: se molar ratio is 2:1, reaction time is adjusted to 25min, 40min and 50min, and experiment numbers are 4, 5 and 6 respectively.
TABLE 2 influence of CdSe Quantum dots generated at different reaction times on perovskite solar cell Performance
As can be seen from table 2, cdSe quantum dots prepared at different reaction times have a significant impact on perovskite solar cell efficiency.
FIG. 1 is a TEM image of CdSe quantum dots (experiment No. 5: cd: se molar ratio of 2:1, reaction time of 40 min) prepared in example 2. The crystal grains are uniformly distributed, the size is about 3nm, and the crystal grains belong to the size range of the quantum dots.
FIG. 2 is a surface SEM image of a perovskite thin film produced in example 2 (experiment No. 5: cd: se molar ratio of 2:1, reaction time of 40 min). It can be seen that the perovskite crystal grains are about 240nm, and the crystal grains are uniformly distributed, so that no agglomeration phenomenon occurs.
Comparative example 1
The preparation method is the same as in example 1, except that the perovskite precursor solution is directly spin-coated on a substrate composed of ITO conductive glass and poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine ] (PTAA), and no CdSe quantum dot solution is prepared and spin-coated.
Fig. 3 is a J-V graph of the perovskite solar cell (experiment No. 5) prepared in example 2 using CdSe quantum dots as hole transport layer, and the perovskite solar cell prepared in comparative example 1 without quantum dots added as hole transport layer. It can be seen that the perovskite solar cell with the quantum dot as the hole layer has the efficiency of 17%, and the perovskite solar cell without the quantum dot as the hole transport layer has the efficiency of 14.9%, compared with the perovskite solar cell with the quantum dot as the hole transport layer, the performance of the perovskite solar cell is obviously improved.
Example 3
1) Preparation of CdS quantum dot semiconductor material: a mixture consisting of 400mg of cadmium oxide (CdO) powder, 120mg of tri-n-octylphosphinoxide (TOPO), 1.5mL of Oleic Acid (OA) and 10mL of Octadecene (ODE) was heated under nitrogen flow. Simultaneously, 2mL of 1.5mol/L dilute sulfuric acid (H) is continuously introduced below the liquid level 2 SO 4 ) 100mg of ferrous sulfide (FeS) mixture continuously reacts to form H 2 S gas, the reaction time is 35min, and the reaction temperature is 210 ℃. And after the reaction is finished, centrifuging, washing and ligand exchanging the mixed solution to obtain the CdS quantum dot solution.
The ligand exchange process is as follows: dissolving washed CdS quantum dots in toluene to obtain a solution A, dissolving 0.2g of mercaptopropionic acid in 10mL of methanol, regulating the pH value of the solution A to 12 by using a saturated solution of NaOH and methanol to obtain a solution B, mixing the solution A and the solution B according to the volume ratio of 1:1, stirring for 30min, centrifuging for 15min (the centrifugal speed is 15000 rpm), pouring out the supernatant, repeating the ligand exchange process for 2 times on the rest precipitate, and dissolving the last precipitate in water to form a CdS quantum dot aqueous solution wrapped by mercaptopropionic acid, thereby facilitating the subsequent spin coating.
2) Cleaning of conductive substrates: sequentially using detergent, deionized water, acetone, ethanol and isopropanol to ultrasonically clean the etched FTO conductive glass for 15min, and drying the glass by using a nitrogen gun after cleaning.
3) Preparing a hole transport layer: in glove box N 2 Under protection, the FTO conductive glass and poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Uniformly spin-coating the CdS quantum dot solution prepared in the step 1) on a substrate consisting of (PTAA), wherein the spin-coating time is 25s, the spin-coating speed is 3000rpm, and annealing is performed for 10min at 80 ℃ after the spin-coating is finished.
4) Preparing a perovskite layer: spin coating was performed at 800rpm and 4200rpm, respectively, and a perovskite precursor solution having a concentration of 1.5g/mL was spin coated and spread over the hole transport layer. And (5) after spin coating, heating the substrate on a heating table at 110 ℃ for 30min to obtain the perovskite film.
Wherein the perovskite precursor solution is HC (NH) 2 ) 2 PbI 3 The preparation method comprises the following steps: lead iodide (PbI) 2 ) And formamidine hydroiodidate (HC (NH) 2 ) 2 I) Mixed in N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, wherein PbI 2 、HC(NH 2 ) 2 I. The molar ratio of DMSO is 1:1:1, the volume ratio of DMF to DMSO is 8:1, mixing and stirring for 40 min.
5) And (3) preparing an electron transport layer: [6,6 ] with spin-coating concentration of 20mg/mL]-phenyl-C 61 Methyl butyrate (PC) 61 BM) -chlorobenzene solution, spin coating speed of 2500rpm, spin coating time of 40s, annealing at 100 deg.C for 10min after spin coating.
6) Preparing a buffer layer: dissolving 2, 9-dimethyl-4, 7-diphenyl phenanthroline (BCP) in methanol, taking saturated solution, spin-coating, wherein the spin-coating speed is 7000rpm, the spin-coating time is 20s, and annealing for 10min at 70 ℃ after the spin-coating is finished.
7) Preparation of metal electrode: and (3) placing the sample prepared in the step (6) in a thermal evaporation device, and evaporating an 85nm metal electrode.
The morphology of the CdS quantum dots prepared in example 3 is substantially similar to that of FIG. 1, and the efficiency of the prepared perovskite cell is 16.1%.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
Claims (7)
1. A process for preparing CdSe or CdS quantum dot semiconductor material features that under the protection of nitrogen stream, the mixture of cadmium oxide (CdO) powder (100-500 mg), tri-n-octylphosphine oxide (TOPO) (50-150 mg), oleic Acid (OA) (1-2 mL) and Octadecene (ODE) (5-15 mL) is heated, and H is continuously introduced under liquid surface 2 Se or H 2 S gas, wherein the reaction time is 25-50 min, and the reaction temperature is 190-210 ℃; and after the reaction is finished, centrifuging, washing and ligand exchanging the mixed solution to obtain the CdSe or CdS quantum dot semiconductor material.
2. The inverted perovskite solar cell of claim 1 wherein the CdO, H 2 Se or H 2 The molar ratio between S is 1-5:1.
3. The inverted perovskite solar cell of claim 1 or 2, wherein the H 2 The Se gas is prepared from sodium borohydride (NaBH) 4 ) Continuously reacting selenium powder (Se) with deionized water mixture to obtain NaBH 4 The molar ratio between Se is 2-4:1; the H is 2 The S gas is formed by dilute sulfuric acid (H) 2 SO 4 ) And ferrous sulfide (FeS) mixture, H 2 SO 4 The molar ratio of FeS is 2-4:1.
4. An inverted perovskite solar cell, characterized in that the hole transport layer thereof has a coating of CdSe or CdS quantum dot semiconductor material prepared by the method as claimed in claim 1,2 or 3.
5. A method of making an inverted perovskite solar cell as defined in claim 4 wherein the steps are as follows:
1) Cleaning of conductive substrates: sequentially carrying out ultrasonic cleaning on etched FTO or ITO conductive glass for 15-20 min by using detergent, deionized water, acetone, ethanol and isopropanol, and drying the glass by using a nitrogen gun after cleaning;
2) Preparing a hole transport layer: in glove box N 2 Under protection, the conductive glass and poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Uniformly spin-coating CdSe or CdS quantum dot solution on a substrate composed of (PTAA), wherein the spin-coating time is 20-30 s, the spin-coating speed is 3000-3500 rpm, and annealing is performed for 10-15 min at 60-80 ℃ after the spin-coating is finished;
3) Preparing a perovskite layer: spin coating is carried out at the rotation speed of 800-1200 rpm and 4200-4800 rpm respectively, and perovskite precursor solution with the concentration of 1-1.5 g/mL is fully coated on the hole transport layer; after spin coating, placing the substrate on a heating table at 90-110 ℃ for heating for 30-40 min to obtain a perovskite film;
4) And (3) preparing an electron transport layer: [6,6 ] with spin coating concentration of 20-30 mg/mL]-phenyl-C 61 Methyl butyrate (PC) 61 BM) -chlorobenzene solution, spin coating speed of 2500-3500 rpm, spin coating time of 20-40 s, annealing at 80-100 deg.c for 10-15 min after spin coating;
5) Preparing a buffer layer: dissolving 2, 9-dimethyl-4, 7-diphenyl phenanthroline (BCP) in methanol, taking saturated solution, spin-coating, wherein the spin-coating speed is 6000-7000 rpm, the spin-coating time is 20-40 s, and annealing for 10-15 min at 50-70 ℃ after the spin-coating is finished;
6) Preparation of metal electrode: and 5) placing the sample prepared in the step 5) in a thermal evaporation device to evaporate the metal electrode.
6. The method of claim 5, wherein the perovskite precursor solution is CH 3 NH 3 PbI 3 The preparation method comprises the following steps: lead iodide (PbI) 2 ) And methyl ammonium iodide (CH) 3 NH 3 I) Mixed in N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, wherein PbI 2 、CH 3 NH 3 I. The molar ratio of DMSO is 1:1:1, the volume ratio of DMF to DMSO is 8:1, mixing and stirring for 40 min.
7. The method of claim 5, wherein the perovskite precursor solution is HC (NH 2 ) 2 PbI 3 The preparation method comprises the following steps: lead iodide (PbI) 2 ) And formamidine hydroiodidate (HC (NH) 2 ) 2 I) Mixed in N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) solvent, wherein PbI 2 、HC(NH 2 ) 2 I. The molar ratio of DMSO is 1:1:1, the volume ratio of DMF to DMSO is 8:1, mixing and stirring for 40 min.
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