CN112079576A - Carbon nitride material, in-situ preparation method thereof and application of carbon nitride material in perovskite solar cell - Google Patents
Carbon nitride material, in-situ preparation method thereof and application of carbon nitride material in perovskite solar cell Download PDFInfo
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Abstract
The invention belongs to the technical field of solar cell materials, and particularly relates to a carbon nitride material, an in-situ preparation method thereof and application thereof in a perovskite solar cell. According to the invention, the titanium dioxide electron transport layer modified by carbon nitride is rapidly synthesized in situ on the titanium dioxide electron transport layer by using the FTO glass assisted calcination method, and the perovskite solar cell is assembled.
Description
Technical Field
The invention belongs to the technical field of solar cell materials, and particularly relates to a carbon nitride material, an in-situ preparation method thereof and application thereof in a perovskite solar cell.
Background
Perovskite Solar Cells (PSCs) have attracted continuous attention in the world for their unique attractions of excellent photovoltaic performance, low cost, ease of assembly, etc. during the last decade. Through the development of ten years, the photoelectric conversion efficiency of the photoelectric conversion device has increased from 3.8% in 2009 to more than 25%. At present, titanium dioxide, tin dioxide, zinc oxide, zinc stannate, barium stannate and other metal semiconductor oxides are all used as electron transport materials of perovskite solar cells. Among them, titanium dioxide is the most common, and most efficient electron transport layer material in typical n-i-p structured perovskite solar cells. However, the low electron mobility inherent in titanium oxide limits further enhancement of the photoelectric conversion efficiency to some extent. In addition, the strong photocatalytic property of titanium dioxide decomposes perovskite crystals under ultraviolet light, so that the stability of the battery is sharply reduced. Researchers have proposed incorporating two-dimensional materials into the titanium dioxide electron transport layer to enhance its electron mobility. Meanwhile, the hydrophobicity, the thermal conductivity and the like of the two-dimensional material also contribute to the improvement of the long-term stability of the battery.
The graphite phase carbon nitride material is a two-dimensional hot spot material with unique energy band structure, high surface area, high electron mobility, high physical and chemical stability, no toxicity and rich land, and has been successfully applied to the fields of sensing, energy conversion, environmental remediation and the like. Graphite phase carbon nitride is generally synthesized by bulk reaction or polycondensation from nitrogen-rich precursors such as urea, melamine, thiourea, etc. through a long-term (about 4 hours) pyrolysis reaction. At present, no relevant patent report that the carbon nitride material is prepared in situ by a glass auxiliary annealing method and applied to the perovskite solar cell exists.
Disclosure of Invention
The invention aims to provide a carbon nitride material, an in-situ preparation method thereof and application of the carbon nitride material in a perovskite solar cell. According to the invention, graphite phase carbon nitride is rapidly synthesized in situ on the titanium dioxide electron transport layer by using an FTO glass assisted calcination method, and the perovskite solar cell is assembled.
In order to achieve the purpose, the invention adopts the following technical scheme:
an in-situ preparation method of a carbon nitride material comprises the following steps:
step S1 preparation of the titanium dioxide dense layer:
preparing 0.15 mol/L of diisopropyl di (acetylacetonate) titanate n-butyl alcohol solution, and spin-coating the solution on the surface of the FTO conductive glass which is etched and cleaned in advance at the speed of 2000 revolutions per second.
Step S2 preparation of the graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. 5-15 mg of urea or melamine solid is weighed and dispersed in the titanium dioxide dispersion liquid A, fully stirred for 30 min and subjected to ultrasonic treatment for 30 min to completely dissolve the solid, so that dispersion liquid B is obtained. The dispersion liquid B was spin-coated on the titania dense layer obtained in step S1 at a rate of 2000 revolutions per second.
Step S3 FTO glass assisted firing method: and placing the FTO glass subjected to spin coating on a heating table, covering the FTO glass with the same size on the upper layer, and ensuring that the conductive surfaces of the upper glass and the lower glass are tightly attached with each other with the conductive surfaces facing downwards. And then, heating to 550 ℃ at the speed of 2 ℃/min, and keeping the temperature for 0.5 h to obtain the graphite-phase carbon nitride modified titanium dioxide electron transport layer. And finally, assembling the solar cell into a perovskite solar cell, and performing subsequent photoelectric property characterization.
The invention has the following remarkable advantages:
titanium dioxide materials are widely used in electron transport layers of perovskite solar cells due to their excellent photoelectric properties. The invention prepares the titanium dioxide electron transmission layer modified by carbon nitride by FTO glass auxiliary calcination method for the first time, assembles the perovskite solar cell,at 100 mW/cm2Under the conditions of light intensity and AM1.5, the photoelectric conversion efficiency of 17.98 percent is obtained, and is relatively improved by 12.0 percent compared with the battery efficiency of 16.05 percent based on a pure titanium dioxide electron transport layer. The method is simple and easy to implement, has high reproducibility, effectively improves the photoelectric property of the perovskite solar cell, and provides a new thought for high-performance and industrialized research of the perovskite solar cell.
Drawings
FIG. 1 is a C1s spectrum of a carbon nitride modified titanium dioxide electron transport layer photoelectron spectrum;
FIG. 2 is a spectrum of N1s of a photoelectron spectrum of a titanium dioxide electron transport layer modified by carbon nitride;
FIG. 3 is a scanning electron micrograph of a carbon nitride-modified titanium dioxide electron transport layer;
FIG. 4 is a graph of the photovoltaic performance of a perovskite solar cell;
fig. 5, schematic representation of FTO glass assisted firing.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Preparing a titanium dioxide dense layer:
preparing 0.15 mol/L of diisopropyl di (acetylacetonate) titanate n-butyl alcohol solution, and spin-coating the solution on the surface of the FTO conductive glass which is etched and cleaned in advance at the speed of 2000 revolutions per second.
Preparing a graphite-phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. 5-15 mg of urea or melamine solid is weighed and dispersed in the titanium dioxide dispersion liquid A, fully stirred for 30 min and subjected to ultrasonic treatment for 30 min to completely dissolve the solid, so that dispersion liquid B is obtained. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
FTO glass assisted calcination method: and placing the FTO glass subjected to spin coating on a heating table, covering the FTO glass with the same size on the upper layer, and ensuring that the conductive surfaces of the upper glass and the lower glass are tightly attached with each other with the conductive surfaces facing downwards. And then, heating to 550 ℃ at the speed of 2 ℃/min, and keeping the temperature for 0.5 h to obtain two electron transport layers. The titanium dioxide electron transport layer obtained after spin coating of the dispersion liquid A and the titanium dioxide electron transport layer modified by graphite-phase carbon nitride obtained after spin coating of the dispersion liquid B. And finally, assembling the perovskite solar cell based on the two electron transport layers, and carrying out subsequent photoelectric property characterization.
The advantages of glass-assisted calcination are as follows: generally, the synthesis of graphite phase carbon nitride needs to be carried out in a muffle furnace by using a covered crucible for calcination, but most of reactants are decomposed due to more air in the crucible, and finally, only a small amount of products are left. When the glass auxiliary calcination method is adopted, the electron transmission layer is thin, so that a capillary effect is formed between the two pieces of glass, most of air is isolated, and graphite-phase carbon nitride can be rapidly generated.
Example 1, preparation of graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. Weighing 5 mg of urea solid, dispersing in 1 mL of titanium dioxide dispersion liquid A, fully stirring for 30 min, and performing ultrasonic treatment for 30 min to completely dissolve the solid to obtain dispersion liquid B. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
Example 2, preparation of graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. Weighing 10mg of urea solid, dispersing in 1 mL of titanium dioxide dispersion liquid A, fully stirring for 30 min, and performing ultrasonic treatment for 30 min to completely dissolve the solid to obtain dispersion liquid B. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
Example 3, preparation of graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. Weighing 15 mg of urea solid, dispersing in 1 mL of titanium dioxide dispersion liquid A, fully stirring for 30 min, and performing ultrasonic treatment for 30 min to completely dissolve the solid to obtain dispersion liquid B. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
Example 4 preparation of graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. Weighing 5 mg of melamine solid, dispersing in 1 mL of titanium dioxide dispersion liquid A, fully stirring for 30 min, and performing ultrasonic treatment for 30 min to completely dissolve the solid to obtain dispersion liquid B. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
Example 5 preparation of graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. Weighing 10mg of melamine solid, dispersing in 1 mL of titanium dioxide dispersion liquid A, fully stirring for 30 min, and performing ultrasonic treatment for 30 min to completely dissolve the solid to obtain dispersion liquid B. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
Example 6 preparation of graphite phase carbon nitride modified titanium dioxide electron transport layer: an appropriate amount of commercial titanium dioxide (Deysol 30NR-D) was diluted in absolute ethanol at a mass ratio of 1:9 to obtain a dispersion A. Weighing 15 mg of melamine solid, dispersing in 1 mL of titanium dioxide dispersion liquid A, fully stirring for 30 min, and performing ultrasonic treatment for 30 min to completely dissolve the solid to obtain dispersion liquid B. Dispersion A, B was separately spin coated onto the titania dense layer at 2000 revolutions per second.
Fig. 1 is a C1s spectrogram of a carbon nitride modified titanium dioxide electron transport layer photoelectron spectrum, which illustrates that the titanium dioxide electron transport layer contains carbon element.
FIG. 2 is a N1s spectrum of a photoelectron spectrum of a carbon nitride-modified titanium dioxide electron transport layer, illustrating that the titanium dioxide electron transport layer contains nitrogen element. The nitrogen content is low, probably because of partial reaction products, such as urea or melamine, and decomposition reaction occurs during the calcination process. While the peaks of the carbons in fig. 1 are strong and may contain two carbons: one is carbon in carbon nitride and the other is a small amount of carbon remaining after calcination in a small amount of organic binder such as cellulose in commercial titanium dioxide slurry. Combining the results of fig. 1 and 2, the presence of carbon nitride can be demonstrated.
FIG. 3 is a scanning electron microscope image of a carbon nitride-modified titanium dioxide electron transport layer, which shows that the morphology of the carbon nitride-modified titanium dioxide electron transport layer is not much different from that of an unmodified titanium dioxide electron transport layer, and the particle size of the titanium dioxide nanoparticles is about 20-30 nm. The morphology of the carbon nitride material was not observed, probably because the carbon nitride was also in the nanoparticle morphology and could not be distinguished from the titanium dioxide nanoparticles.
Fig. 4 is a graph of the photovoltaic performance of a perovskite solar cell. Short-circuit current J when unmodified carbon nitride titanium dioxide is used as an electron transport layerscIs 21.52 mA/cm2Open circuit voltage Voc At 1.04V, the corresponding photoelectric conversion efficiency was 16.05%. Short-circuit current J when using carbon nitride modified titanium dioxide as electron transport layerscAnd an open circuit voltage VocAre all improved and are respectively 23.08 mA/cm2And 1.06V, the corresponding photoelectric conversion efficiency is also improved to 17.98 percent.
Fig. 5 is a schematic representation of FTO glass assisted firing. And the FTO glass which is spin-coated with the electronic transmission layer is arranged on the heating table, the conductive surface faces upwards, a piece of FTO glass with the same size is added above the FTO glass, the conductive surface faces downwards, and the electronic transmission layer is positioned between the conductive surfaces of the two pieces of glass.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. An in-situ preparation method of a carbon nitride material is characterized by comprising the following steps: the method comprises the following steps:
step S1 preparation of the titanium dioxide dense layer:
preparing 0.15 mol/L of diisopropyl di (acetylacetonate) titanate n-butyl alcohol solution, and spin-coating the solution on the surface of FTO conductive glass which is etched and cleaned in advance at the speed of 2000 revolutions per second;
step S2 preparation of the graphite phase carbon nitride modified titanium dioxide electron transport layer: diluting commercial titanium dioxide in absolute ethyl alcohol to obtain a dispersion liquid A; weighing a carbon source, dispersing the carbon source in the titanium dioxide dispersion liquid A, and fully dispersing to completely dissolve solids to obtain a dispersion liquid B; spin-coating the dispersion liquid B on the titanium dioxide dense layer obtained in step S1;
step S3 FTO glass assisted firing method: placing the FTO glass which is well spun on a heating table, covering the FTO glass with the same size on the upper layer of the FTO glass, and ensuring that the conductive surfaces of the upper glass and the lower glass are tightly attached with each other with the conductive surfaces facing downwards; and then, heating and preserving the temperature for a period of time to obtain the graphite-phase carbon nitride modified titanium dioxide electron transport layer material.
2. The in-situ preparation method of a carbon nitride material according to claim 1, wherein: step S2 the mass ratio of commercial titanium dioxide Deysol 30NR-D to absolute ethanol was 1: 9.
3. The in-situ preparation method of a carbon nitride material according to claim 1, wherein: the carbon source in step S2 is specifically 5-15 mg of urea or melamine solid.
4. The in-situ preparation method of a carbon nitride material according to claim 1, wherein: the step S2 of fully dispersing is to stir for 30 min and perform ultrasonic treatment for 30 min.
5. The in-situ preparation method of a carbon nitride material according to claim 1, wherein: the spin coating in step S2 is specifically spin coating at a speed of 2000 revolutions per second.
6. The in-situ preparation method of a carbon nitride material according to claim 1, wherein: the temperature rise and the heat preservation are carried out for a period of time, specifically, the temperature is raised to 550 ℃ at the speed of 2 ℃/min, and the constant temperature is kept for 0.5 h.
7. A carbon nitride material obtained by the production method according to any one of claims 1 to 6.
8. Use of a carbon nitride material obtained by the production method according to any one of claims 1 to 6 in a perovskite solar cell, characterized in that: the titanium dioxide electron transport layer material modified by graphite phase carbon nitride is assembled in the perovskite solar cell.
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| CN113540360A (en) * | 2021-06-22 | 2021-10-22 | 湖北大学 | Method for preparing halogenated perovskite solar cell modified based on nanosheet material and product |
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