CN114284444A - Preparation method of CsPbBr3 perovskite solar cell - Google Patents
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Abstract
The application provides a preparation method of a cesium-lead-bromine perovskite solar cell, which comprises the following steps: preparing an FTO substrate at a high temperature in situ; spraying a tin source or a nickel source on the substrate, and converting the residual heat in the in-situ FTO preparation process into a tin oxide layer/nickel oxide layer to be a heat source; spraying CsBr and PbBr on the tin oxide layer2Mixed solution, forming CsPbBr by using the heat source3A film layer; in the CsPbBr3Preparing a hole transport layer/an electron transport layer and a metal electrode on the film layer in sequence to obtain CsPbBr3Perovskite solar cell. Besides the substrate, the invention does not need to additionally provide an external heat source in the preparation process, thereby saving energy consumption. And, CsPbBr3The film is formed in one step, and the preparation efficiency is further improved. In the present invention, CsPbBr is formed by spray coating3The perovskite layer can improve the stability of the battery and is beneficial to application.
Description
Technical Field
The application belongs to the technical field of perovskite solar cells, and particularly relates to a preparation method of a cesium-lead-bromine CsPbBr3 perovskite solar cell.
Background
Currently, perovskite solar cells are one of the solar cells that are receiving much attention. Generally, a perovskite solar cell mainly consists of FTO conductive glass, an electron transport layer, a perovskite material absorption layer, a hole transport layer and a metal electrode. The working principle of the photoelectric effect solar cell is as follows: when irradiated by sunlight, the perovskite layer firstly absorbs photons to generate electron-hole pairs, then, the electrons and holes which are not recombined are respectively collected by the electron transport layer and the hole transport layer, and finally, the photoelectric current is generated through a circuit which is connected with the FTO and the metal electrode.
Wherein, cesium lead bromine perovskite material (CsPbBr) is used3Perovskite) is an absorption layer, and has become a recent research hotspot due to relatively good performance such as open circuit voltage. Conventional CsPbBr3In the perovskite solar cell, the material of the electron transport layer is C60 or SnO2、TiO2And the like, wherein the hole transport layer is mainly made of PTAA and Spiro, and the metal electrode comprises Cu,The preparation of the perovskite layer of Al, Au, Ag and the like is mainly carried out by spraying or spin-coating perovskite precursor liquid.
However, there have been prepared transport layers and CsPbBr3In the process of the perovskite layer, high-temperature heating is mostly needed to be carried out independently, the energy consumption is high, the energy waste is caused, and the energy recovery period of the whole assembly is longer. At the same time, CsPbBr3The layers are usually prepared in two steps to multiple steps, and the preparation method is complicated and not beneficial to industrial large-scale production.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a cesium-lead-bromine perovskite solar cell, which saves energy consumption in the preparation process, has good cell stability and high preparation efficiency, and is beneficial to industrial production.
The application provides a preparation method of a cesium-lead-bromine perovskite solar cell, which comprises the following steps:
preparing an FTO substrate at a high temperature in situ;
spraying a tin source on the substrate, and converting the residual heat in the in-situ FTO preparation process into a tin oxide layer and serving as a heat source;
spraying CsBr and PbBr on the tin oxide layer2Mixing the solution, and forming CsPbBr by using heat source for preparing tin oxide layer3A film layer;
in the CsPbBr3Preparing a hole transport layer and a metal electrode on the film layer in sequence to obtain CsPbBr3Perovskite solar cell.
In a preferred embodiment of the present application, the hole transport layer has a thickness of 20 to 100 nm; the composition of the hole transport layer is PTAA or Sprio.
In the preferred embodiment of the present application, the spray CsBr and PbBr are2The thickness of the mixed solution is 200nm-1 μm.
In a preferred embodiment of the present application, the metal electrode is selected from one or more of Cu, Al, Au and Ag.
The application further provides a preparation method of the cesium-lead-bromine perovskite solar cell, which comprises the following steps:
preparing an FTO substrate at a high temperature in situ;
spraying a nickel source on the substrate, and converting the nickel source into a nickel oxide layer and serving as a heat source by using residual heat in the in-situ FTO preparation process;
CsBr and PbBr are sprayed on the nickel oxide layer2Mixing the solution, and forming CsPbBr by using the heat source for preparing nickel oxide layer3A film layer;
in the CsPbBr3Preparing an electron transport layer and a metal electrode on the film layer in sequence to obtain CsPbBr3Perovskite solar cell.
In a preferred embodiment of the present application, the thickness of the electron transport layer is 20 to 100 nm; the electron transport layer comprises C60 and SnO2Or TiO2。
In the preferred embodiment of the present application, the spray CsBr and PbBr are2The thickness of the mixed solution is 200nm-1 μm.
In a preferred embodiment of the present application, the metal electrode is selected from one or more of Cu, Al, Au and Ag.
The invention provides CsPbBr3The preparation method of the perovskite solar cell comprises the steps of preparing an FTO substrate by adopting the existing high-temperature in-situ preparation method of FTO, spraying a tin source or a nickel source, and converting residual heat in the in-situ preparation process of FTO into a tin oxide layer/nickel oxide layer to be used as a heat source; preparing CsPbBr on the tin oxide layer/nickel oxide layer by spraying method by using heat source for preparing tin oxide/nickel oxide in situ3(250 ℃), i.e. in the preparation of CsPbBr3And a heating link is not independently arranged in the process of the film, so that the perovskite solar cell is obtained. Besides the substrate, the invention does not need to additionally provide an external heat source in the preparation process, thereby saving energy consumption. And, CsPbBr3The film is formed in one step, and the preparation efficiency is further improved. In the present invention, CsPbBr is formed by spray coating3The perovskite layer can improve the stability of the cell, and the photoelectric conversion efficiency of the perovskite solar cell prepared by the method can reach 8%.
Detailed Description
The technical solutions in the embodiments of the present application are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The application provides a preparation method of a cesium-lead-bromine perovskite solar cell, which comprises the following steps:
preparing an FTO substrate at a high temperature in situ;
spraying a tin source or a nickel source on the substrate, and converting the residual heat in the in-situ FTO preparation process into a tin oxide layer or a nickel oxide layer serving as a heat source;
CsBr and PbBr are sprayed on the tin oxide layer or the nickel oxide layer2Mixing the solution, and forming CsPbBr by using heat source for preparing tin oxide layer or nickel oxide layer3A film layer;
in the CsPbBr3Sequentially preparing a hole transport layer/an electron transport layer and a metal electrode on the film layer to obtain CsPbBr3Perovskite solar cell.
The invention prepares CsPbBr3The perovskite solar cell method is low in energy consumption, simple and convenient to operate, high in efficiency and good in cell stability.
The method comprises the following steps of firstly preparing an FTO substrate by adopting the existing high-temperature in-situ mode; typically, FTO is prepared by spray coating or vapor phase processes at temperatures of about 670 ℃ to 700 ℃. The FTO substrate is SnO doped with fluorine2Transparent conductive glass (SnO)2F), abbreviated as FTO. The method for preparing the FTO film mainly comprises a vapor deposition method (CVD), sputtering, a thermal evaporation method and a sol-gel method; at present, the production mode of FTO coated glass mainly comprises the following steps: chemical Vapor Deposition (APCVD) and magnetron sputtering (PVD). The on-line chemical vapor deposition method is on-line high-temperature SnO deposition performed in the float production process2F is the main production mode of the existing photovoltaic FTO coating.
Specifically, the embodiment of the invention inserts the multi-channel film coating device into the narrow section of the tin bath of the float glass production lineWith monobutyl trichlorotin (C)4H9SnCl3MBTC) as a precursor, trifluoroacetic acid (CF)3COOH and TFA) as doping agent, and air and water as the oxidizing agent and catalyst for reaction; preferably, the carrier gas is MBTC with the mole fraction of 1.6%, TFA with the mole fraction of 0.88%, water with the mole fraction of 4.8% and nitrogen, and the carrier gas is gasified at 175 ℃ after entering an evaporator; after being gasified, the mixture enters a gas mixing chamber to be mixed and sprayed on the surface of glass with the temperature of 675 ℃ through a coating device, and the mixed gas reacts on a gas-solid phase interface to deposit and form a compact FTO solid film.
After FTO is prepared in situ, certain heat is remained, a tin source is sprayed immediately to form a tin oxide layer in situ, and the CsPbBr is prepared by further utilizing the heat source for preparing the tin oxide layer in situ through a spraying method3A film. Or, in the embodiment of the invention, a nickel source is sprayed on the FTO substrate immediately, the residual heat after the in-situ preparation of the FTO is utilized to convert the FTO into a nickel oxide layer and become a heat source, and CsPbBr is formed on the nickel oxide layer by spraying the heat source3A film.
In an embodiment of the present invention, CsPbBr is prepared by spray coating using residual heat (at least 250 ℃ C.)3The film is prepared by spraying cesium bromide (CsBr) and lead bromide (PbBr) as the slurry2) The mixed solution of (1). Wherein CsBr and PbBr2The concentration of the solution is between 0.5 and 1.5mol/L respectively, the spraying thickness can be between 200nm and 1 mu m, and CsPbBr is formed3A layer of material. Preferably, CsBr and PbBr2The concentrations of the components are 0.05mol/L and 1mol/L respectively, and the spraying thickness can be regarded as the thickness after the formation of the perovskite layer.
The method prepares CsPbBr by spraying3And a heating link is not independently arranged in the processes of films and the like, so that the energy consumption is reduced. CsPbBr in the invention3The film is formed in one step by spraying, so that the performance of the film layer is easily controlled, the performance of the battery is improved, and the preparation efficiency is also improved. Spin coating and the like are difficult to control well, and are not suitable for the preparation system of the application.
In some embodiments of the invention, if P-type NiO is prepared in situxNamely, the nickel oxide hole transport layer is prepared by utilizing waste heat,an electron transport layer and a metal electrode are further prepared on the formed perovskite material layer. The preparation methods of the electron transport layer and the metal electrode are conventional methods, such as a spraying method, a spin coating method and the like. Wherein the thickness of the electron transport layer can be 20nm-100nm, preferably 30-90nm, and more preferably 40-80 nm; the electron transport layer comprises C60 and stannic oxide (SnO)2) Titanium dioxide (TiO)2). The metal electrodes include, but are not limited to, copper (Cu), aluminum (Al), gold (Au), silver (Ag) electrodes; the present application is not particularly limited.
Illustratively, an electron transport layer is prepared on the perovskite light absorption layer by a thermal evaporation method, and the material is C60. The evaporation speed can be 0.1A/s to 0.5A/s, and is preferably 0.3A/s; the thickness is about 40-50 nm. And evaporating a metal counter electrode layer on the electron transport layer, wherein the material is high-purity copper (more than 99.99%). The evaporation speed can be 0.1A/s to 1.5A/s, and is preferably 0.3A/s; the thickness of the copper film was 100 nm.
In other embodiments of the invention, if prepared in situ, N-type SnO2Namely, SnO is prepared by utilizing waste heat2And an electron transport layer, and further preparing a hole transport layer and a metal electrode on the formed perovskite material layer. The preparation methods of the hole transport layer and the metal electrode are conventional methods; wherein the thickness of the hole transport layer may be 20 to 100nm, preferably 30 to 90nm, and more preferably 40 to 80 nm. The material of the hole transport layer is PTAA and Spiro, and the PTAA is poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine]The number average molecular weight can be 2-4 ten thousand; spiro is Spiro-OMeTAD, N2, N2, N2 ', N2', N7, N7, N7 ', N7' -octakis (4-methoxyphenyl) -9,9 '-spirobifluorene-2, 2',7,7 '-tetramine, 2,2',7,7 '-tetrakis (N, N-p-methoxyanilino) -9,9' -spirobifluorene. In addition, the metal electrode can be one or more of Cu, Al, Au and Ag.
In conclusion, the method is used for preparing CsPbBr3In the processes of perovskite layer and the like (substrate preparation removal), no external heat source is required to be additionally provided, the energy consumption is low, and the energy recovery period of the whole assembly is shortened. And, CsPbBr3The film is formed in one step, the preparation is simple and convenient, and the preparation efficiency is further improved. In the present invention, sprayingCsPbBr formed by coating method3The perovskite layer can improve the stability of the cell, and the perovskite solar cell prepared by the method has good photoelectric conversion efficiency and is beneficial to application.
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention. Wherein, the embodiment of the invention adopts the commercial raw materials.
Example 1
CsPbBr3The preparation method of the perovskite solar cell comprises the following specific steps:
inserting a multi-channel coating device into a narrow section of a tin bath of a float glass production line, and coating by using monobutyl tin trichloride with the purity of 95% (mass fraction, the same below) as a precursor, trifluoroacetic acid with the purity of 99% as a doping agent and using air and water as an oxidant and a catalyst for reaction; using a mole fraction of 1.6% MBTC, 0.88% TFA, 4.8% water and N2Is used as carrier gas, and is gasified at 175 ℃ after entering an evaporator; after being gasified, the mixture enters a gas mixing chamber to be mixed and is sprayed on the surface of glass with the temperature of 675 ℃ through a coating device, and a compact FTO solid film is formed through deposition.
Using 99% purity nickel nitrate in isopropanol (Ni (NO)3)2·6H2O) is a precursor solution, and film plating is carried out in an oxygen-rich environment: n with a purity of 99.9% is used2And 99% of O2According to the following steps: the flow ratio of 1 is carrier gas, the carrier gas enters an evaporator and is gasified at 175 ℃, the gasified carrier gas enters a gas mixing chamber and is mixed, the surface of FTO glass (the FTO glass with residual heat obtained in the preparation process) with the temperature of 450 ℃ is sprayed by a coating machine, and the mixed gas reacts at a gas-solid phase interface to deposit and form a compact nickel oxide solid film.
Converting the residual heat in the in-situ preparation process of the FTO into nickel oxide and forming a heat source, and preparing CsPbBr on the nickel oxide layer by using the heat source for in-situ preparation of the nickel oxide through a spraying method3(250 ℃), in particular, CsBr and PbBr are sprayed on the nickel oxide layer2Solution, in which the thickness of spray coating is 200nm, CsBr and PbBr2Dissolving in isopropanol and DMF respectively at a concentration0.05mol/L and 1mol/L respectively to form CsPbBr3A layer of material.
Prepared in situ from P-type NiOxAnd further preparing an electron transport layer and a metal electrode on the formed perovskite material layer, wherein the electron transport layer and the metal electrode are as follows:
and preparing an electron transport layer on the perovskite light absorption layer by a thermal evaporation method, wherein the material is C60. The evaporation speed is 0.3A/s; the thickness is about 40-50 nm.
And evaporating a metal counter electrode layer on the electron transport layer, wherein the material is high-purity copper. The evaporation speed is 0.3A/s; the thickness of the copper film was 100 nm.
The perovskite solar cell prepared by the method has the photoelectric conversion efficiency of 8%.
The method avoids CsPbBr in experiment3And NiOxTwo heating steps, according to Q ═ cmt, the required energy is proportional to the temperature, therefore, the method saves energy by about 40-50%; the time saving is about 20% per beat.
Example 2
CsPbBr3The preparation method of the perovskite solar cell comprises the following specific steps:
inserting a multi-channel coating device into a narrow section of a tin bath of a float glass production line, and coating by using monobutyl tin trichloride with the purity of 95% (mass fraction, the same below) as a precursor, trifluoroacetic acid with the purity of 99% as a doping agent and using air and water as an oxidant and a catalyst for reaction; using a mole fraction of 1.6% MBTC, 0.88% TFA, 4.8% water and N2Is used as carrier gas, and is gasified at 175 ℃ after entering an evaporator; after being gasified, the mixture enters a gas mixing chamber to be mixed and is sprayed on the surface of glass with the temperature of 675 ℃ through a coating device, and a compact FTO solid film is formed through deposition.
Taking an aqueous solution of tin oxide with the purity of 99% as a precursor solution, and plating a film in a polyoxygen environment: n with a purity of 99.9% is used2And 99% of O2According to the following steps: 1 flow ratio is carrier gas, the carrier gas is gasified at 175 ℃ after entering an evaporator, the gasified carrier gas enters a gas mixing chamber to be mixed, and the FTO glass (the FTO glass with residual heat obtained in the preparation process) with the temperature of 300 ℃ is sprayed by a coating machineThe mixed gas reacts at the gas-solid phase interface to deposit and form a compact tin oxide solid film.
Converting the residual heat in the process of preparing the FTO in situ into tin oxide and serving as a heat source, and preparing CsPbBr on the tin oxide layer by using the heat source for preparing the tin oxide in situ through a spraying method3(250 ℃ C.), specifically, CsBr and PbBr are sprayed on the formed tin oxide layer2Solution, in which the thickness of spray coating is 200nm, CsBr and PbBr2Respectively dissolved in isopropanol and DMF with the concentration of 0.05mol/L and 1mol/L respectively to form CsPbBr3A layer of material.
Prepared in situ from N-type SnO2And further preparing a hole transport layer and a metal electrode on the formed perovskite material layer, wherein the hole transport layer and the metal electrode are as follows: and preparing a hole transport layer on the perovskite light absorption layer by a spin coating method, wherein the material is PTAA. The PTAA solvent is chlorobenzene with the concentration of 0.5mol/L and the thickness of about 20-30 nm.
And evaporating a metal counter electrode layer on the electron transport layer, wherein the material is high-purity copper. The evaporation speed is 0.3A/s; the thickness of the copper film was 100 nm.
The perovskite solar cell prepared by the method has the photoelectric conversion efficiency of 6%.
According to the embodiments, the invention does not need to provide an external heat source except for the substrate in the preparation process, so that the energy consumption is saved. And, CsPbBr3The film is formed in one step, and the preparation efficiency is further improved. CsPbBr formed by spraying method of the invention3The perovskite layer can improve the stability of the cell, and the photoelectric conversion efficiency of the perovskite solar cell prepared by the method can reach 8%. The battery prepared by the invention has good stability and high preparation efficiency, and is beneficial to industrial production.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (6)
1. A preparation method of a cesium-lead-bromine perovskite solar cell is characterized by comprising the following steps:
preparing an FTO substrate at a high temperature in situ;
spraying a tin source on the substrate, and converting the residual heat in the in-situ FTO preparation process into a tin oxide layer and serving as a heat source;
spraying CsBr and PbBr on the tin oxide layer2Mixing the solution, and forming CsPbBr by using heat source for preparing tin oxide layer3A film layer;
in the CsPbBr3Preparing a hole transport layer and a metal electrode on the film layer in sequence to obtain CsPbBr3Perovskite solar cell.
2. The production method according to claim 1, wherein the hole transport layer has a thickness of 20 to 100 nm; the composition of the hole transport layer is PTAA or Sprio.
3. A preparation method of a cesium-lead-bromine perovskite solar cell is characterized by comprising the following steps:
preparing an FTO substrate at a high temperature in situ;
spraying a nickel source on the substrate, and converting the nickel source into a nickel oxide layer and serving as a heat source by using residual heat in the in-situ FTO preparation process;
CsBr and PbBr are sprayed on the nickel oxide layer2Mixing the solution, and forming CsPbBr by using the heat source for preparing nickel oxide layer3A film layer;
in the CsPbBr3Preparing an electron transport layer on the film layer in sequence andmetal electrode to obtain CsPbBr3Perovskite solar cell.
4. The production method according to claim 3, wherein the thickness of the electron transport layer is 20 to 100 nm; the electron transport layer comprises C60 and SnO2Or TiO2。
5. The method according to any one of claims 1 to 4, wherein the spray CsBr and PbBr are used2The thickness of the mixed solution is 200nm-1 μm.
6. The production method according to any one of claims 1 to 4, wherein the metal electrode is one or more selected from the group consisting of Cu, Al, Au and Ag.
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| PCT/CN2022/099757 WO2023115854A1 (en) | 2021-12-23 | 2022-06-20 | Preparation method for cspbbr3 perovskite solar cell |
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|---|---|---|---|---|
| WO2023115854A1 (en) * | 2021-12-23 | 2023-06-29 | 中国华能集团清洁能源技术研究院有限公司 | Preparation method for cspbbr3 perovskite solar cell |
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| WO2023115854A1 (en) | 2023-06-29 |
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