CN108666428B - Perovskite single crystal thin film solar cell preparation method and device - Google Patents
Perovskite single crystal thin film solar cell preparation method and device Download PDFInfo
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Abstract
The invention is suitable for the technical field of solar cells, and provides a preparation method and a device of a perovskite single crystal thin film solar cell, wherein the method comprises the following steps: reacting an organometallic halide ABX3Fully mixing the single crystal particles and the organic halide AX solid powder, and grinding the mixture into a precursor perovskite mixture; distributing a precursor perovskite mixture over the first carrier transport layer, liquefying the precursor perovskite mixture and carrying out chemical reaction to form a liquid-phase perovskite thin film; pressurizing and annealing the liquid phase perovskite thin film to obtain a perovskite single crystal thin film; and sequentially preparing a second carrier transmission layer and a metal electrode on the upper surface of the perovskite single crystal film to prepare the solar cell. According to the invention, the perovskite single crystal thin film is obtained by liquefying the single crystal perovskite particles and processing the liquid phase perovskite, so that the preparation period of the perovskite single crystal thin film is effectively shortened, the preparation process is simplified, the preparation time of the perovskite single crystal thin film solar cell is shortened, the recycling of the perovskite mixture is realized, and the cost is saved.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a preparation method and a device of a perovskite single crystal thin film solar cell.
Background
Because the traditional fossil energy such as coal, petroleum and the like is non-renewable and increasingly lacks, the energy problem increasingly becomes a bottleneck restricting the development of international socioeconomic development, the solar energy with wide application, no pollution and reproducibility is valued by various countries, and the solar cell is developed rapidly. In 2009, japan scientist Miyasaka first used a perovskite-based semiconductor in a liquid-state sensitized solar cell, achieving a photoelectric conversion efficiency of 3.8%, but the cell efficiency decayed rapidly due to corrosion of the electrolyte (j.am.chem.soc.,2009,131,6050.). With the continuous and intensive research, the efficiency of the perovskite solar cell is further improved.
Various preparation methods such as a one-step or two-step solution coating method, a vacuum evaporation method, a liquid-gas mixing process and the like are developed for preparing the perovskite material of the polycrystalline perovskite type solar cell, and the preparation method is mainly designed on the basis of improving the solar light absorption performance of the material and improving the macroscopic performance of a cell device. However, due to grain boundaries and inevitable defects associated with grain boundaries and poor stability of polycrystalline perovskites, the rate of increase of the Photoelectric Conversion Efficiency (PCE) of Perovskite Solar Cells (PSCs) has been greatly slowed. In order to further improve the photoelectric conversion efficiency and stability of perovskite solar cells, PSCs have turned to the development of single crystal perovskite materials.
The perovskite single crystal film has small defect density, low carrier recombination probability and wide spectrum absorption rangeAnd the conversion efficiency of the perovskite solar cell is improved. Rao et al (chem. Commun.,2017,53,5163-5166.) use single crystal CH3NH3PbBr3The film grows by space-limited inverse temperature crystallization, and the highest photoelectric conversion efficiency in the reported single-crystal PSCs is 7.11%. Liu et al (Sci China Chem.,2016,59(1): 1-2.) cut single crystal blocks into single crystal wafers to prepare single crystal perovskite solar cell devices with cell efficiency of about 4%. Zhao et al (sci. Bull.,2017,62(17),1173-2Self-assembly growth of single crystal perovskite CH on substrate3NH3PbI3The photoelectric conversion efficiency was 8.78%. Huang et al (nat. Commun.,2017,8(1):1890.) utilize the bandgap absorption of perovskite single crystals to narrow the effective optical bandgap of the single crystals without changing their composition, and limit lateral crystal growth by hydrophobic interfaces, with a photoelectric conversion efficiency of 17.8%. Chen et al (J.Am.chem.Soc.,2016,138,16196-1619) prepared CH by a two-dimensional domain-restricted induction method using a mild solution method3NH3PbX3The single crystal perovskite thin film reported at present has long growth period and complex preparation process, and restricts the mass production.
Disclosure of Invention
In view of this, the embodiment of the invention provides a perovskite single crystal thin film solar cell preparation method and a device, so as to solve the problems that in the prior art, the perovskite single crystal thin film has a long growth period and a complex preparation process, so that the perovskite single crystal thin film solar cell has a long preparation period.
The first aspect of the embodiment of the invention provides a preparation method of a perovskite single crystal thin film solar cell, which comprises the following steps:
reacting an organometallic halide ABX3Fully mixing the single crystal particles and the organic halide AX solid powder, grinding the mixture into powder, and preparing a precursor perovskite mixture;
preparing a first carrier transport layer on the upper surface of a substrate with a transparent conductive layer;
placing a perovskite thin film mold on the upper surface of the first carrier transport layer, and uniformly distributing the precursor perovskite mixture in the perovskite thin film mold;
heating the precursor perovskite mixture to liquefy the precursor perovskite mixture and perform chemical reaction to prepare a liquid-phase perovskite thin film;
placing a high-temperature resistant film on the upper surface of the liquid-phase perovskite thin film, and pressurizing the high-temperature resistant film to obtain a perovskite single crystal thin film with the depth equal to that of the perovskite thin film mold;
annealing the perovskite single crystal film, naturally cooling to room temperature, and taking down the perovskite film mold;
and sequentially preparing a second carrier transmission layer and a metal electrode on the upper surface of the perovskite single crystal film to prepare the solar cell.
Optionally, the organometallic halide ABX3In the single crystal particles and the organic halide AX solid powder, A represents a methylamine cation CH3NH3 +Formamidine cation HC (NH)2)2 +Cesium ion Cs+Rb ion (Rb)+One or more mixed cations of (a); b represents germanium ion Ge2+Sn ion Sn2+Lead ion Pb2+Magnesium ion Mg2+Bismuth ion Bi3+One or more mixed metal ions; x represents iodide I-Bromine ion Br-Chloride ion Cl-One or more mixed halogen elements.
Optionally, the preparing the first carrier transport layer on the upper surface of the substrate with the transparent conductive layer includes:
anhydrous ethanol and hydrochloric acid are mixed according to a molar ratio of 500: 1-50: 1 mixing to prepare a first precursor solution;
anhydrous ethanol and tetraisopropyl titanate are mixed according to a molar ratio of 100: 1-20: 1 mixing to prepare a second precursor solution;
fully stirring and mixing the first precursor solution and the second precursor solution to prepare TiO2A precursor solution;
subjecting the TiO to a reaction2The precursor solution is spin-coated on the transparent conductive layer at a speed of 100-And preparing the first carrier transport layer.
Optionally, the perovskite thin film mold depth is 500nm-300 μm.
Optionally, the temperature of the heating treatment is 50-600 ℃, and the mass of the precursor perovskite mixture is 0.001-100 g.
Optionally, the pressure of the pressurization treatment is 0-10000N, and the time is 0.1s-10 h.
Optionally, the temperature of the annealing treatment is-50 ℃ to 550 ℃, and the time is 0.1s to 24 h.
Optionally, the transparent conductive layer is SnO doped with fluorine2A thin Film (FTO), an indium tin oxide thin film (ITO), or an aluminum-doped zinc oxide thin film (AZO).
Optionally, the first carrier transport layer is made of TiO2，SnO2，NiOn，Li/Na-NiOn，WOn，FeOnWherein n is more than or equal to 0 and less than or equal to 5; the material of the second carrier transport layer is 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino]-9,9' -spirobifluorene or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine.
A second aspect of the embodiments of the present invention provides a perovskite single crystal thin film solar cell, which includes a substrate, a transparent conductive layer, a first carrier transport layer, a perovskite single crystal thin film, a second carrier transport layer, and a metal electrode, which are connected in sequence; the substrate is made of glass, mica, metal sheets or polyethylene terephthalate; the metal electrode is made of Au, Cu or Ag.
Compared with the prior art, the embodiment of the invention has the following beneficial effects: according to the embodiment of the invention, the perovskite single crystal film is obtained by liquefying the single crystal perovskite particles and pressurizing and annealing the liquid phase perovskite, so that the preparation period of the perovskite single crystal film is effectively shortened, the preparation process is simplified, the preparation time of the perovskite single crystal film solar cell is shortened, the reutilization of the precursor perovskite mixture is realized, and the energy and the cost are saved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
FIG. 1 is a schematic flow chart of an implementation of a perovskite single crystal thin film solar cell manufacturing method provided by an embodiment of the invention;
FIG. 2 is a schematic diagram of a scanning electron microscope electron back scattering diffraction cuvette of a perovskite single crystal thin film provided by an embodiment of the invention;
FIG. 3 is a schematic structural diagram of a perovskite single crystal thin film solar cell provided by an embodiment of the invention;
FIG. 4 is a current density-voltage curve of a perovskite single crystal thin film solar cell provided by an embodiment of the invention;
FIG. 5 is a scanning electron micrograph of a perovskite polycrystalline thin film provided by an embodiment of the present invention.
In the figure, 1, a substrate, 2, a transparent conducting layer, 3, a first carrier transmission layer, 4, a perovskite single crystal thin film, 5, a second carrier transmission layer, 6 and a metal electrode.
Detailed Description
In the following description, for purposes of explanation and not limitation, specific details are set forth, such as particular system structures, techniques, etc. in order to provide a thorough understanding of the embodiments of the invention. It will be apparent, however, to one skilled in the art that the present invention may be practiced in other embodiments that depart from these specific details. In other instances, detailed descriptions of well-known systems, devices, circuits, and methods are omitted so as not to obscure the description of the present invention with unnecessary detail.
In order to explain the technical means of the present invention, the following description will be given by way of specific examples.
Example one
Referring to fig. 1, a method for manufacturing a perovskite single crystal thin film solar cell includes:
step S101, will haveOrganic metal halide ABX3The single crystal particles and the organic halide AX solid powder are fully mixed and ground into powder to prepare a precursor perovskite mixture.
Step S102, a first carrier transmission layer is prepared on the upper surface of the substrate with the transparent conducting layer.
And S103, placing a perovskite thin film mold on the upper surface of the first carrier transport layer, and uniformly distributing the precursor perovskite mixture in the perovskite thin film mold.
And step S104, heating the precursor perovskite mixture to liquefy the precursor perovskite mixture and perform chemical reaction to prepare the liquid-phase perovskite thin film.
And S105, placing the high-temperature-resistant film on the upper surface of the liquid-phase perovskite film, and pressurizing the high-temperature-resistant film to obtain the perovskite single crystal film with the depth equal to that of the perovskite film mold.
And S106, annealing the perovskite single crystal film, naturally cooling to room temperature, and taking down the perovskite film die.
And S107, sequentially preparing a second carrier transmission layer and a metal electrode on the upper surface of the perovskite single crystal film to prepare the solar cell.
Specifically, in this example, the organometallic halide ABX3The mass ratio of the single crystal particles to the organic halide AX solid powder is 1: 0.01-1: 50, mixing well and grinding into powder. The second carrier transmission layer is prepared by adopting a spin coating process, and spin coating is carried out on the upper surface of the perovskite single crystal film for 1-60s at the speed of 500-6000 r/s.
In the embodiment, the perovskite single crystal thin film is obtained by liquefying the single crystal perovskite particles and pressurizing and annealing the liquid phase perovskite, so that the preparation period of the perovskite single crystal thin film is effectively shortened, the preparation process is simplified, the preparation time of the perovskite single crystal thin film solar cell is shortened, the perovskite mixture of the precursor is recycled, and the energy and the cost are saved.
Optionally, an organometallic halide ABX3In the single crystal particles and the organic halide AX solid powder, A represents methylamineCation CH3NH3 +Formamidine cation HC (NH)2)2 +Cesium ion Cs+Rb ion (Rb)+One or more mixed cations of (a); b represents germanium ion Ge2+Sn ion Sn2+Lead ion Pb2+Magnesium ion Mg2+Bismuth ion Bi3+One or more mixed metal ions; x represents iodide I-Bromine ion Br-Chloride ion Cl-One or more mixed halogen elements.
In the embodiment of the invention, CH can be selected3NH3PbI3Single crystal particles and organic halide CH3NH3And I, fully mixing the solid powder in a mass ratio of 1:2, grinding the solid powder into powder, and preparing a precursor perovskite mixture.
Optionally, the specific implementation method of step S102 is: anhydrous ethanol and hydrochloric acid are mixed according to a molar ratio of 500: 1-50: 1 mixing to prepare a first precursor solution; anhydrous ethanol and tetraisopropyl titanate are mixed according to a molar ratio of 100: 1-20: 1 mixing to prepare a second precursor solution; fully stirring and mixing the first precursor solution and the second precursor solution to prepare TiO2A precursor solution; adding TiO into the mixture2The precursor solution is spin-coated on the transparent conductive layer for 1-80s at the speed of 100-.
Optionally, the perovskite thin film mold depth is 500nm-300 μm. The depth of the perovskite thin film mould can be adjusted, and the thickness of the perovskite single crystal thin film is controlled by adjusting the depth of the perovskite thin film mould.
Optionally, the temperature of the heating treatment is 50-600 ℃, and the mass of the precursor perovskite mixture is 0.001-100 g. The liquefaction and chemical reaction of the precursor perovskite mixture are controlled by adjusting the temperature of the heating treatment.
Optionally, the pressure of the pressurization treatment is 0-10000N, and the time is 0.1s-10 h. The thickness and the surface appearance of the perovskite single crystal film are controlled by adjusting the pressure and the time of the pressurization treatment.
Optionally, the temperature of the annealing treatment is-50 ℃ to 550 ℃, and the time is 0.1s to 24 h.
Optionally, the transparent conductive layer is SnO doped with fluorine2A thin Film (FTO), an indium tin oxide thin film (ITO), or an aluminum-doped zinc oxide thin film (AZO).
In this embodiment, the transparent conductive layer may be an FTO thin film, an ITO thin film, or an AZO thin film.
Optionally, the first carrier transport layer is made of TiO2，SnO2，NiOn，Li/Na-NiOn，WOn，FeOnWherein n is in the range of 0-5. The material of the second carrier transport layer is 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino]-9,9' -spirobifluorene (Spiro-MEOTAD) or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine (PTAA).
Referring to fig. 2, fig. 2 is a scanning electron microscopy electron back scattering diffraction image of the perovskite single crystal thin film prepared by the above method. The Euler angles of the perovskite thin film are (57.2,55.4 and 51.4), and the corresponding crystal planes are (111) crystal planes, so that the perovskite thin film prepared by the method is further proved to be single crystal perovskite.
Referring to fig. 3, fig. 3 is a schematic structural diagram of a perovskite single crystal thin film solar cell prepared by the above method. The perovskite-type single crystal perovskite-type solar cell comprises a substrate 1, a transparent conducting layer 2, a first carrier transmission layer 3, a perovskite single crystal thin film 4, a second carrier transmission layer 5 and a metal electrode 6 which are sequentially connected. The material of the substrate 1 can be glass, mica, metal flake, polyethylene terephthalate or polyethylene naphthalate, and the material of the metal electrode 6 can be Au, Cu or Ag.
Embodiments of the present invention use CH3NH3PbI3The perovskite monocrystal film is used as a photosensitive layer, and has the advantages of low defect density, high stability, low carrier recombination probability and the like, so that the absorption range of a spectrum can be widened, and the conversion efficiency of the perovskite solar cell is improved.
Referring to fig. 4, fig. 4 shows the embodiment using CH3NH3PbI3The current density-voltage curve of the solar cell with the perovskite single crystal thin film as the photosensitive layer.CH3NH3PbI3The efficiency of the perovskite single crystal thin film assembled solar cell is 7.05%.
Example two
Referring to FIG. 5, FIG. 5 shows the use of CH3NH3PbI3Scanning electron microscope images of perovskite polycrystalline thin films prepared by clarifying solutions. As can be seen from the figure, CH is used3NH3PbI3The perovskite thin film prepared by the clear solution is different from CH3NH3PbI3Thin films prepared from perovskite single crystal particles. Using CH3NH3PbI3The perovskite thin film prepared by the clear solution has a polycrystalline structure.
In this example, CH is used3NH3PbI3The preparation method of the solar cell with the perovskite polycrystalline film as the photosensitive layer comprises the following steps:
firstly, mixing a molar ratio of 300: 7, mixing absolute ethyl alcohol and hydrochloric acid in a molar ratio of 30: 7 absolute ethyl alcohol and tetraisopropyl titanate are mixed, the two mixed solutions are fully stirred, and TiO is prepared2Precursor solution of TiO2The precursor solution is spin-coated on the transparent conductive layer for 60s at the speed of 2000r/s, and is annealed at 500 ℃ for 12 hours to form compact TiO2An electron transport layer. Secondly, mixing PbI2And CH3NH3I is added into gamma-butyrolactone, and stirred for 12h at 70 ℃ until the perovskite mixed solution is obtained after uniform clarification. Again, 15. mu.l of the perovskite mixed solution was dropped onto the TiO2Heating to 350 deg.C in perovskite film mould on the substrate of electron transmission layer. Then, covering a high-temperature resistant film on the perovskite mixed solution, applying a pressure 5N vertical to the substrate, annealing at the temperature of 120 ℃ for 3 minutes, naturally cooling to room temperature to form a perovskite polycrystalline film, and taking down the die. And finally, sequentially forming a carrier transmission layer and a metal electrode on the upper surface of the perovskite polycrystalline film to finish the preparation of the solar cell.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not substantially depart from the spirit and scope of the embodiments of the present invention, and are intended to be included within the scope of the present invention.
Claims (10)
1. A preparation method of a perovskite single crystal thin film solar cell is characterized by comprising the following steps:
reacting an organometallic halide ABX3The mass ratio of the single crystal particles to the organic halide AX solid powder is 1: 0.01-1: 50, fully mixing, grinding into powder, and preparing into a precursor perovskite mixture;
preparing a first carrier transmission layer on the upper surface of a substrate with a transparent conductive layer;
placing a perovskite thin film mold on the upper surface of the first carrier transport layer, and uniformly distributing the precursor perovskite mixture in the perovskite thin film mold;
heating the precursor perovskite mixture to liquefy the precursor perovskite mixture and perform chemical reaction to prepare a liquid-phase perovskite thin film;
placing a high-temperature resistant film on the upper surface of the liquid-phase perovskite thin film, and pressurizing the high-temperature resistant film to obtain a perovskite single crystal thin film with the depth equal to that of the perovskite thin film mold;
annealing the perovskite single crystal film, naturally cooling to room temperature, and taking down the perovskite film mold;
and sequentially preparing a second carrier transmission layer and a metal electrode on the upper surface of the perovskite single crystal film to prepare the solar cell.
2. The method for preparing a perovskite single crystal thin film solar cell according to claim 1, wherein the organic metal halide ABX3In the single crystal particles and the organic halide AX solid powder, A represents a methylamine cation CH3NH3 +Formamidine cation HC (NH)2)2 +Cesium ion Cs+Rb ion (Rb)+One or more mixed cations of (a); b represents germanium ion Ge2+Sn ion Sn2 +Lead ion Pb2+Magnesium ion Mg2+Bismuth ion Bi3+One or more mixed metal ions; x represents iodide I-Bromine ion Br-Chloride ion Cl-One or more mixed halogen elements.
3. The method for preparing a perovskite single crystal thin film solar cell according to claim 1, wherein the first carrier transport layer is prepared on the upper surface of the substrate with the transparent conductive layer, and the method comprises the following steps:
anhydrous ethanol and hydrochloric acid are mixed according to a molar ratio of 500: 1-50: 1 mixing to prepare a first precursor solution;
anhydrous ethanol and tetraisopropyl titanate are mixed according to a molar ratio of 100: 1-20: 1 mixing to prepare a second precursor solution;
fully stirring and mixing the first precursor solution and the second precursor solution to prepare TiO2A precursor solution;
subjecting the TiO to a reaction2The precursor solution is spin-coated on the transparent conductive layer for 1-80s at the speed of 100-.
4. The method for preparing a perovskite single crystal thin film solar cell according to claim 1, wherein the depth of the perovskite thin film mold is 500nm to 300 μm.
5. The method for preparing a perovskite single crystal thin film solar cell according to claim 1, wherein the temperature of the heating treatment is 50-600 ℃, and the mass of the precursor perovskite mixture is 0.001-100 g.
6. The method for manufacturing a perovskite single crystal thin film solar cell according to claim 1, wherein the pressure of the pressurization treatment is 0 to 10000N and the time is 0.1s to 10 h.
7. The method for preparing the perovskite single crystal thin film solar cell according to claim 1, wherein the annealing treatment temperature is-50 ℃ to 550 ℃, and the time is 0.1s to 24 h.
8. The method for preparing the perovskite single crystal thin film solar cell according to claim 1, wherein the transparent conductive layer is SnO doped with fluorine2A thin Film (FTO), an indium tin oxide thin film (ITO), or an aluminum-doped zinc oxide thin film (AZO).
9. The method for preparing the perovskite single crystal thin film solar cell according to claim 1, wherein the material of the first carrier transport layer is TiO2，SnO2，NiOn，Li/Na-NiOn，WOn，FeOnWherein n is more than or equal to 0 and less than or equal to 5; the material of the second carrier transport layer is 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino]-9,9' -spirobifluorene or poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine.
10. The perovskite single crystal thin film solar cell prepared by the method of any one of claims 1 to 9, comprising a substrate, a transparent conductive layer, a first carrier transport layer, a perovskite single crystal thin film, a second carrier transport layer and a metal electrode which are connected in sequence; the substrate is made of glass, mica, metal sheets or polyethylene terephthalate; the metal electrode is made of Au, Cu or Ag.
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| CN113506853B (en) * | 2021-06-25 | 2024-04-12 | 南京邮电大学 | Preparation method and product of heterojunction tin-based perovskite film |
| CN113782685B (en) * | 2021-09-10 | 2022-10-21 | 华能新能源股份有限公司 | Preparation method of perovskite thin film |
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