CN110611032B - Method for improving crystallinity and coverage rate of cadmium-based perovskite light absorption layer - Google Patents
Method for improving crystallinity and coverage rate of cadmium-based perovskite light absorption layer Download PDFInfo
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- CN110611032B CN110611032B CN201810620391.5A CN201810620391A CN110611032B CN 110611032 B CN110611032 B CN 110611032B CN 201810620391 A CN201810620391 A CN 201810620391A CN 110611032 B CN110611032 B CN 110611032B
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Abstract
The invention provides a method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer, which comprises the following steps: transferring the cadmium-based perovskite precursor solution, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass by adopting a dripping method; and (3) carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the conductive glass at the temperature of 80-130 ℃. The cadmium-based perovskite light absorption layer provided by the invention has larger-sized grains and better film coverage rate, the larger-sized grains can enhance the transmission of electron and hole carriers in the grains and reduce the number of grain boundaries in the perovskite light absorption layer, the quenching and recombination of the electron and hole carriers at the grain boundaries can be reduced, and the transmission performance of the electron and hole carriers in the perovskite light absorption layer can be further improved; meanwhile, the good film coverage rate can effectively reduce the generation of dark current in the perovskite photoelectrochemical device, and finally, the photoelectric conversion efficiency of the perovskite photoelectrochemical device is effectively improved.
Description
Technical Field
The invention relates to a method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer, and belongs to the technical field of perovskite solar cells.
Background
With the development of the current world industry and the continued growth of the population, the global energy demand is also increasing, especially for non-renewable resources such as oil, coal, natural gas, etc. Due to the over-exploitation of fossil energy by humans, such energy reserves have approached the depletion margin. Meanwhile, with the continuous consumption of fossil energy, a large amount of pollutants are discharged into the nature, and the environmental problems caused by the emission are becoming more severe. Therefore, the related development and utilization of renewable clean energy is receiving more and more attention. In recent years, solar cells have been gaining acceptance as energy conversion devices for renewable clean energy sources.
Perovskite, as a novel photosensitive material, has been receiving more and more attention since 2009 due to a series of advantages of low cost, simple preparation, excellent light absorption performance, high electron mobility and the like. During the last years, with the introduction and application of new materials and new structures, the certified photocurrent conversion efficiency of perovskite solar cells is continuously improved, and the efficiency of the perovskite solar cells is preliminarily equivalent to that of commercial silicon solar cells. For perovskite cell devices, the crystallinity and coverage of the perovskite light absorption layer are key factors affecting the photoelectric conversion efficiency of the device. However, the conventional perovskite light absorption layer is mainly prepared by a one-step spin coating method, a two-step method, an evaporation method and an atmosphere treatment method, and means for controlling key parameters such as crystallinity and uniformity of the thin film are still insufficient, and the thin film with high crystallinity and coverage rate is difficult to obtain, so that the transport capacity of electron and hole carriers in the thin film cannot be further improved.
Therefore, providing a method for improving the crystallinity and the coverage rate of the cadmium-based perovskite light absorption layer has become an urgent technical problem to be solved in the field.
Disclosure of Invention
In order to solve the above disadvantages and shortcomings, an object of the present invention is to provide a method for improving crystallinity and coverage of a cadmium-based perovskite light absorption layer.
The invention also aims to provide the cadmium-based perovskite light absorption layer obtained by the method for improving the crystallinity and the coverage rate of the cadmium-based perovskite light absorption layer.
The invention also aims to provide a cadmium-based perovskite photoelectrochemical device which comprises the cadmium-based perovskite light absorption layer.
In order to achieve the above objects, in one aspect, the present invention provides a method for improving crystallinity and coverage of a cadmium-based perovskite light absorption layer, wherein the method comprises the steps of:
(1) Transferring the cadmium-based perovskite precursor solution, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass by adopting a dripping method;
(2) And (2) performing thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass in the step (1) at the temperature of 80-130 ℃ to obtain a cadmium-based perovskite thin film, namely the cadmium-based perovskite light absorption layer.
According to the method, in the step (2), the cadmium-based perovskite precursor solution dripped on the FTO conductive glass in the step (1) is subjected to thermal annealing treatment at the temperature of 80-130 ℃, wherein if the temperature is too low, the obtained film is not easy to dry; if the temperature is too high, the solvent is volatilized quickly, and the film forming property is not good;
preferably, step (2) is: firstly, carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass in the step (1) at the temperature of 80 ℃ for 1.0-1.5h; then the thermal annealing treatment is carried out for 0.5 to 1.0 hour at the temperature of 130 ℃.
According to the method of the present invention, preferably, the thickness of the cadmium-based perovskite thin film in the step (2) is 30 to 35 μm. In the embodiment of the present invention, a liquid-moving machine may be used to move the cadmium-based perovskite precursor liquid, and a dropping method (a conventional method in the art) is used to drop the cadmium-based perovskite precursor liquid onto the FTO conductive glass to prepare the cadmium-based perovskite thin film, the cadmium-based perovskite thin film with a target thickness may be obtained by the dropping method, and the thin film obtained by other methods in the art, such as a spin coating method, has insufficient thickness, which is not favorable for performing a photoelectrochemical test on the cadmium-based perovskite thin film.
According to the method provided by the invention, preferably, the cadmium-based perovskite precursor solution is obtained by uniformly mixing methylamine hydrochloride and cadmium chloride in a molar ratio of 2:1 in an N, N-dimethylformamide solution.
On the other hand, the invention also provides the cadmium-based perovskite light absorption layer obtained by the method for improving the crystallinity and the coverage rate of the cadmium-based perovskite light absorption layer, wherein the crystallinity of the cadmium-based perovskite light absorption layer is 65-85%, and the coverage rate is 85-95%.
In still another aspect, the invention also provides a cadmium-based perovskite photoelectrochemical device which contains the cadmium-based perovskite light absorption layer.
In the invention, the structural formula of the cadmium-based perovskite is A 2 BX 4 Wherein A is CH 3 NH 3 + B is Cd 2+ X is Cl - 。
The cadmium-based perovskite light absorption layer provided by the invention has larger-sized grains and better film coverage rate, the larger-sized grains can enhance the transmission of electron and hole carriers in the grains and reduce the number of grain boundaries in the perovskite light absorption layer, and can also reduce the quenching and recombination of the electron and hole carriers at the grain boundaries, thereby further improving the transmission performance of the electron and hole carriers in the perovskite light absorption layer; meanwhile, the good film coverage rate can effectively reduce the generation of dark current in the perovskite photoelectrochemical device, and finally, the photoelectric conversion efficiency of the perovskite photoelectrochemical device is effectively improved.
Drawings
Fig. 1 is a process flow diagram of a method for improving crystallinity and coverage of a cadmium-based perovskite light absorption layer according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a photoelectrochemical cell device and an apparatus for performing a photoelectrochemical test thereon according to embodiment 5 of the present invention; wherein 101 is perovskite (CH) 3 NH 3 ) 2 CdCl 4 Working electrode, 102 silver/silver nitrate (Ag/AgNO) 3 ) A reference electrode, 103 a platinum (Pt) counter electrode, 104 a light source and 105 an electrochemical working cell;
FIG. 3 is a scanning electron micrograph of a cadmium-based perovskite light absorption layer prepared in example 1 of the present invention;
FIG. 4 is a scanning electron micrograph of a cadmium-based perovskite light absorption layer prepared in example 2 of the present invention;
FIG. 5 is a scanning electron micrograph of a cadmium-based perovskite light absorption layer prepared in example 3 of the invention;
FIG. 6 is a scanning electron micrograph of a cadmium-based perovskite light absorption layer prepared in example 4 of the present invention;
FIG. 7 is a scanning electron microscope image of a cross section of a cadmium-based perovskite light absorption layer prepared in example 1 of the present invention;
fig. 8 is a graph of photoelectrochemical response curves (current density-voltage curves) of cadmium-based perovskite light-absorbing layers prepared under different annealing conditions (examples 1 to 4).
Detailed Description
In order to clearly understand the technical features, objects and advantages of the present invention, the following detailed description of the technical solutions of the present invention will be made with reference to the following specific examples, which should not be construed as limiting the implementable scope of the present invention.
Example 1
The embodiment provides a method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer, a process flow chart of the method is shown in fig. 1, and as can be seen from fig. 1, the method comprises the following steps:
placing methylamine hydrochloride and cadmium chloride with the molar ratio of 2:1 in an N, N-dimethylformamide solution, and uniformly mixing to obtain a cadmium-based perovskite precursor solution;
transferring the cadmium-based perovskite precursor solution by using a liquid transfer device, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass;
carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass at 80 ℃ for 1h; and then continuously carrying out thermal annealing treatment for 1h at 130 ℃ to obtain the cadmium-based perovskite thin film (the thickness is 30-35 mu m), namely the cadmium-based perovskite light absorption layer.
Example 2
The embodiment provides a method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer, a process flow chart of the method is shown in fig. 1, and as can be seen from fig. 1, the method comprises the following steps:
placing methylamine hydrochloride and cadmium chloride with the molar ratio of 2:1 in an N, N-dimethylformamide solution, and uniformly mixing to obtain a cadmium-based perovskite precursor solution;
transferring the cadmium-based perovskite precursor solution by using a liquid transfer device, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass;
and then, carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass at the temperature of 80 ℃ for 1h to obtain a cadmium-based perovskite thin film (the thickness is 30-35 mu m), namely the cadmium-based perovskite light absorption layer.
Example 3
The embodiment provides a method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer, a process flow chart of the method is shown in fig. 1, and as can be seen from fig. 1, the method comprises the following steps:
placing methylamine hydrochloride and cadmium chloride with the molar ratio of 2:1 in an N, N-dimethylformamide solution, and uniformly mixing to obtain a cadmium-based perovskite precursor solution;
transferring the cadmium-based perovskite precursor solution by using a liquid transfer device, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass;
and then, carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass at 100 ℃ for 1h to obtain a cadmium-based perovskite thin film (with the thickness of 30-35 mu m), namely the cadmium-based perovskite light absorption layer.
Example 4
The embodiment provides a method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer, a process flow chart of the method is shown in fig. 1, and as can be seen from fig. 1, the method comprises the following steps:
placing methylamine hydrochloride and cadmium chloride with the molar ratio of 2:1 in an N, N-dimethylformamide solution, and uniformly mixing to obtain a cadmium-based perovskite precursor solution;
transferring the cadmium-based perovskite precursor solution by using a liquid transfer device, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass;
and then, carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass at 130 ℃ for 1h to obtain a cadmium-based perovskite thin film (with the thickness of 30-35 mu m), namely the cadmium-based perovskite light absorption layer.
Scanning electron microscope analysis is respectively carried out on the cadmium-based perovskite light absorption layer prepared in the embodiments 1-4, the scanning electron microscope images are respectively shown in fig. 3-6, the cross-sectional scanning electron microscope image of the cadmium-based perovskite light absorption layer prepared in the embodiment 1 is shown in fig. 7, and as can be seen from fig. 3-6, the cadmium-based perovskite light absorption layer prepared in the embodiment 1 has higher crystallinity and coverage rate, the crystallinity can reach 65% -85%, and the coverage rate can reach 85% -95%; therefore, when the cadmium-based perovskite light absorption layer prepared by the method is used for a photoelectrochemical device, the generation of dark current in the perovskite photoelectrochemical device can be effectively reduced, and the photoelectric conversion efficiency of the perovskite photoelectrochemical device is finally and effectively improved.
As can be seen from fig. 7, the cadmium-based perovskite light absorption layer prepared in example 1 had a thickness of 30 to 35 μm.
Example 5
This example provides four cadmium-based perovskite photoelectrochemical devices comprising the cadmium-based perovskite light absorbing layers prepared in examples 1 to 4, respectively.
Wherein the device and the apparatus for performing photoelectrochemical testing thereof are schematically shown in FIG. 2. As can be seen from FIG. 2, the device comprises a perovskite (CH) 3 NH 3 ) 2 CdCl 4 Working electrode 101, silver/silver nitrate (Ag/AgNO) 3 ) A reference electrode 102, a platinum (Pt) counter electrode 103, a light source 104, and an electrochemical cell 105.
The graph of the photoelectrochemical response curve (current density-voltage curve) of the cadmium-based perovskite light absorption layer prepared under different annealing conditions (examples 1 to 4) obtained in the embodiment is shown in fig. 8, and as can be seen from fig. 8, the cadmium-based perovskite light absorption layer prepared by the preferred preparation method in example 1 of the present invention has relatively stronger photoelectrochemical response, that is, has stronger electron and hole transport capabilities.
In conclusion, the cadmium-based perovskite light absorption layer provided by the invention has larger-sized grains and better film coverage rate, the larger-sized grains can enhance the transmission of electron and hole carriers in the grains, reduce the number of grain boundaries in the perovskite layer, reduce the quenching and recombination of the electron and hole carriers at the grain boundaries, and further improve the transmission performance of the electron and hole carriers in the perovskite light absorption layer; meanwhile, the good film coverage rate can effectively reduce the generation of dark current in the perovskite photoelectrochemical device, and finally, the photoelectric conversion efficiency of the perovskite photoelectrochemical device is effectively improved.
Claims (4)
1. A method for improving the crystallinity and the coverage rate of a cadmium-based perovskite light absorption layer is characterized by comprising the following steps:
(1) Transferring the cadmium-based perovskite precursor solution, and dripping the cadmium-based perovskite precursor solution on FTO conductive glass by adopting a dripping method;
(2) Firstly, carrying out thermal annealing treatment on the cadmium-based perovskite precursor solution dropwise coated on the FTO conductive glass in the step (1) at 80 ℃ for 1.0-1.5h; and then continuously carrying out thermal annealing treatment for 0.5-1.0h at 130 ℃ to obtain the cadmium-based perovskite thin film, namely the cadmium-based perovskite light absorption layer, wherein the crystallinity of the cadmium-based perovskite light absorption layer is 65% -85%, the coverage rate is 85% -95%, and the thickness is 30-35 mu m.
2. The method according to claim 1, wherein the cadmium-based perovskite precursor solution is obtained by uniformly mixing methylamine hydrochloride and cadmium chloride in a molar ratio of 2:1 in a N, N-dimethylformamide solution.
3. The cadmium-based perovskite light absorption layer obtained by the method for improving the crystallinity and the coverage rate of the cadmium-based perovskite light absorption layer according to claim 1 or 2, wherein the crystallinity of the cadmium-based perovskite light absorption layer is 65% -85%, and the coverage rate is 85% -95%.
4. A cadmium-based perovskite photoelectrochemical device comprising the cadmium-based perovskite light absorbing layer according to claim 3.
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