CN114086238A - Gamma-Ga2O3Or Cu doped gamma-Ga2O3Nanocrystalline and preparation method and application thereof - Google Patents

Gamma-Ga2O3Or Cu doped gamma-Ga2O3Nanocrystalline and preparation method and application thereof Download PDF

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CN114086238A
CN114086238A CN202111296672.8A CN202111296672A CN114086238A CN 114086238 A CN114086238 A CN 114086238A CN 202111296672 A CN202111296672 A CN 202111296672A CN 114086238 A CN114086238 A CN 114086238A
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CN114086238B (en
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刘喜哲
张洁静
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Jilin University
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Abstract

A gamma-Ga compound of the present invention2O3Or Cu doped gamma-Ga2O3A nanocrystalline and a preparation method and application thereof belong to the technical field of nanomaterial synthesis and photovoltaic devices. The preparation method comprises the steps of mixing a gallium source, a copper source and a surfactant, adding deionized water, stirring to form a uniform mixed solution, adding ethylene glycol, adding a precipitator, carrying out hydrothermal reaction, cleaning, centrifuging and the like; preparation ofThe nano-crystal is used as a hole transport layer to prepare the perovskite solar cell. The invention prepares the gamma-Ga by using a low-temperature hydrothermal method for the first time2O3And Cu doped gamma-Ga2O3The nanocrystalline is used in a hole transport layer of a perovskite solar cell for the first time, and is expected to promote an ultra-wide band gap semiconductor material Ga2O3Development in the field of photovoltaic devices.

Description

Gamma-Ga2O3Or Cu doped gamma-Ga2O3Nanocrystalline and preparation method and application thereof
Technical Field
The present invention belongs to the field of nano material synthesis and photovoltaic technologyThe technical field of devices, in particular to gamma-Ga2O3And Cu doped gamma-Ga2O3A preparation method of a nanocrystal and a preparation method of a perovskite solar cell using the nanocrystal as a hole transport material.
Background
The solar photovoltaic technology is an effective scheme for solving the current fossil energy crisis and serious environmental pollution. The photoelectric conversion efficiency of the perovskite solar cell rapidly rises from 3.8% in 2009 to 25.5% reported at present, and the perovskite solar cell has a wide development prospect. The perovskite solar cell is generally composed of a transparent electrode, an electron transport layer, a perovskite light absorption layer, a hole transport layer and a metal back electrode. The hole transport layer plays a role in collecting and transporting holes, can block photo-generated electrons, and has one of the key factors influencing the photoelectric conversion efficiency of the perovskite solar cell. In the structural design of perovskite solar cells, the Highest Occupied Molecular Orbital (HOMO) or valence band maximum of the hole transport material is typically required to be slightly higher than the valence band maximum of the perovskite material to facilitate hole transport.
The most commonly used hole transport material in forward structure perovskite solar cells is currently the organic compound spiro-OMeTAD. Although the perovskite solar cell based on the spiro-OMeTAD obtains higher photoelectric conversion efficiency, the conjugated parts of the materials containing the triphenylamine are not coplanar and are difficult to orderly stack in space, so that the hole mobility of the materials is poor, and therefore, additives such as Li-TFSI and 4-tert-butylpyridine need to be introduced to improve the performance. However, such additives not only increase the manufacturing cost of the device, but also, since these additives are sensitive to humidity and temperature, damage to the adjacent perovskite layer under high humidity or high temperature conditions, further degrading the performance of the accelerator device. The most commonly used hole transport materials in inverted structure perovskite solar cells are the organic materials PTAA and PEDOT: PSS. PTAA, however, is not only expensive, low in hole mobility, but also hydrophobic on the surface, and perovskite films prepared thereon are generally poorly covered, requiring additional subsequent processing, making device reproducibility challenging. PSS, a relatively inexpensive PEDOT that is both acidic and hydrophilic, and due to its valence band position and calciumA certain hole transfer barrier exists between titanium ore materials, which also leads to poor device performance and poor stability. In view of the above disadvantages of organic hole transport materials, a variety of inorganic oxide hole transport materials have been currently explored and studied. Compared with organic materials, the inorganic oxide material has low cost and good stability, and is a promising hole transport material in the perovskite solar cell. In the perovskite solar cell based on the inorganic oxide hole transport material reported at present, NiO is based onxThe device achieves the highest photoelectric conversion efficiency of 23.07%. However, the NiOx film has low conductivity and poor interaction with the perovskite interface, resulting in poor crystalline quality of perovskite, and the energy level arrangement between the NiOx film and the perovskite film is yet to be optimized. Some binary metal oxides also have valence band sites suitable as hole transport materials. It is reported that hydrothermally synthesized ABO having delafossite structure2The type oxide can be used as a hole transport layer of a perovskite solar cell and is CuCrO2The inverted device as a hole transport layer achieved an optimum photoelectric conversion efficiency of 19.0%. In addition to being a dense hole transport layer, these delafossite oxides can also serve as mesoporous hole transport layers to increase NiOxProperties of the hole transport layer. However, these delafossite materials also have certain disadvantages, for example the hydrothermal synthesis of CuCrO2The reaction time is usually as long as 60 hours, and the grain size is hardly smaller than 10nm, while CuGaO2The synthesis of small size particles is difficult and the experimental reproducibility is not high.
Disclosure of Invention
The invention aims to provide gamma-Ga2O3Or Cu doped gamma-Ga2O3The preparation method has the characteristics of low temperature and adjustable grain size.
The second purpose of the invention is to provide a method for doping gamma-Ga with Cu2O3The hole transport layer is applied to the preparation of perovskite solar cells.
The technical scheme of the invention is as follows:
Gamma-Ga2O3Or Cu doped gamma-Ga2O3Preparation method of nanocrystallineThe method comprises the following steps:
(1) placing reactants in a beaker, adding deionized water into the beaker, and stirring to form a uniform mixed solution, wherein the reactants comprise a gallium source, a copper source and a surfactant; wherein the gallium source and the copper source are in the form of Ga3+And Cu2+In a molar ratio of 1:0 to 0.12, per 3mmol of Ga3+0.4 grams of surfactant was used;
(2) adding ethylene glycol into the solution obtained in the step (1) under the condition of stirring, and stirring to form a uniform mixed solution, wherein each 3mmol of Ga3+7mL of ethylene glycol was used;
(3) slowly adding a precipitator into the mixed solution in the stirring in the step (2), and stirring again until the mixed solution is uniform;
(4) after stirring is finished, transferring the mixed solution obtained in the step (3) to a reaction kettle for carrying out;
(5) after the hydrothermal reaction is finished and the reaction kettle is cooled, cleaning the product, centrifuging and removing the supernatant to obtain the gamma-Ga2O3Or Cu doped gamma-Ga2O3And (4) a nanocrystalline product.
Further, the gallium source in step (1) is preferably gallium nitrate or other Ga-containing gallium3+The copper source comprises copper nitrate or other Cu-containing compounds2+The surfactant is preferably P123Polyethylene glycol or other high molecular polymers.
Further, the precipitant in step (3) includes potassium hydroxide, sodium hydroxide, ammonia water or other alkaline solutions such as ethylenediamine.
Further, the hydrothermal reaction in the step (4) is preferably carried out at 210 ℃ for 70 minutes.
Further, the cleaning method of the product in the step (5) comprises the following steps: the reaction product was washed 3 times with dilute ammonia, deionized water and isopropanol respectively and centrifuged to remove the supernatant.
Gamma-Ga2O3Or Cu doped gamma-Ga2O3Use of nanocrystals characterized by the presence of gamma-Ga2O3Or Cu doped gamma-Ga2O3Nanocrystal as voidThe hole transmission layer is used for preparing the perovskite solar cell and comprises the following steps:
1) etching FTO, and etching a trace with the width of 4mm on the FTO surface with the width of 1.5cm multiplied by 1.5cm by using a laser marking machine, wherein the FTO is SnO doped with fluorine2Transparent conductive glass;
2) cleaning the FTO, sequentially placing the etched FTO in a cleaning agent, deionized water and absolute ethyl alcohol for ultrasonic treatment for 15 minutes, then blowing the FTO by using air flow, and then carrying out ultraviolet ozone treatment for 15 minutes;
3) preparing a hole transport layer from gamma-Ga2O3Or Cu doped gamma-Ga2O3Dispersing the nanocrystalline in a mixed solvent of dimethyl sulfoxide and isopropanol with the volume ratio of 1:1 according to the concentration of 5mg/mL for later use; dripping 50 mu L of the dispersion liquid on the FTO treated in the step 2), spin-coating and drying to obtain a hole transport layer;
4) preparing a perovskite layer, taking dimethylformamide and dimethyl sulfoxide with a volume ratio of 4:1 as a mixed solvent, preparing a mixed solution by using 66mg of cesium iodide, 187mg of iodoformamidine, 12mg of bromomethylamine, 568mg of lead iodide and 80mg of lead bromide in each 1mL of solvent, adding hydroxyethyl acrylate with the volume ratio of 1% of the total solution to obtain a perovskite precursor solution, dropwise adding 50 mu L of the perovskite precursor solution onto the hole transport layer prepared in the step 3), spin-coating for 5s at the number of revolutions of 500r, spin-coating for 45s at the number of revolutions of 5000r, dropwise adding 100 mu L of chlorobenzene as an anti-solvent when 5000r spins for 15s, immediately putting the perovskite layer on a heating plate at 100 ℃ after spin-coating, and heating for 10 minutes to obtain the perovskite layer;
5) preparing electron transport layer, collecting 40 μ L PCB with concentration of 10mg/mL61M in chlorobenzene solution was added dropwise to the perovskite layer, spin-coated at 3000r for 30s, using C60Evaporating to form 30nm thick layer, evaporating to form 8nm thick layer with BCP as evaporating material to obtain electron transport layer, and making PCB61M is [6,6 ]]-phenyl C61 butyric acid methyl ester, said C60Is fullerene C60The BCP is bathocuproine;
6) plating electrodes, using silver as an evaporation material, and evaporating a layer of silver electrode with the thickness of 80nm on the surface of the electron transport layer by using an evaporation coating machine to obtain the gamma-Ga based on Cu doping2O3A hole transport layer.
Further, in preparing the hole transport layer in step 3), it is preferable to use Cu-doped γ -Ga2O3Nanocrystalline with doping amount of Cu2+:Ga3+3: 50; the spin coating and drying are carried out, preferably 60s at 4000r rotation speed each time, and 5 times in total, and the drying condition is preferably drying for 10 minutes at 100 ℃.
Has the advantages that:
the invention provides a nano-scale gamma-Ga2O3And Cu doped gamma-Ga2O3The preparation method of (1) is to prepare the gamma-Ga by using a low-temperature hydrothermal method for the first time2O3And Cu doped gamma-Ga2O3The nanocrystalline is used in a hole transport layer of a perovskite solar cell for the first time, and is expected to promote an ultra-wide band gap semiconductor material Ga2O3Development in the field of photovoltaic devices. Also has the following characteristics:
1. Gamma-Ga of the present invention2O3And Cu doped gamma-Ga2O3The preparation method has the advantages of simple process, easy control of doping amount, adjustable grain size and good experimental repeatability.
2. Gamma-Ga of the present invention2O3And Cu doped gamma-Ga2O3The preparation method of the invention uses cheap reaction raw materials and wide sources.
3. The method of the invention provides a new design scheme of the hole transport material;
4. the method of the invention is carried out by introducing gamma-Ga2O3In addition, Cu is doped, so that the content of gamma-Ga is improved2O3Performance of the device as a hole transport layer of a perovskite solar cell.
Drawings
FIG. 1 shows a gamma-Ga compound of the present invention2O3And Cu doped gamma-Ga2O3A flow chart of a low-temperature preparation method of the nanocrystalline;
FIG. 2 shows γ -Ga prepared in example 12O3The transmission electron microscope image of the nanocrystal, the average size of the nanocrystal is below 5 nm;
FIG. 3 is Cu doped γ -Ga prepared in example 32O3The transmission electron microscope image of the nanocrystal, the average size of the nanocrystal is below 5 nm;
FIG. 4 shows Cu doped γ -Ga prepared in example 32O3X-ray photoelectron spectroscopy of the hole transport material confirms the presence of Cu;
FIG. 5 shows Cu-doped γ -Ga prepared in example 92O3A scanning electron micrograph of the hole transport layer;
fig. 6 is a J-V curve of the perovskite solar cells prepared in examples 7, 8, 9 and 10.
Detailed Description
All features disclosed in this specification may be combined in any combination, except features and/or steps that are mutually exclusive.
The invention prepares the gamma-Ga by hydrothermal reaction2O3And Cu doped gamma-Ga2O3The chemical used by the nano-crystal mainly comprises gallium nitrate, copper nitrate, P123, ethylene glycol, deionized water, potassium hydroxide, ammonia water, dimethyl sulfoxide, isopropanol and the like. And reacting gamma-Ga2O3And Cu doped gamma-Ga2O3The method is applied to a hole transport layer of the perovskite solar cell.
The invention is described in detail below with reference to examples, which are intended to provide a better understanding of the invention, and are not intended to limit the scope of the invention.
Example 1
Gamma-Ga2O3The low-temperature preparation method of the nanocrystalline comprises the following steps:
dissolving 0.2g P123 in 4mL of deionized water, stirring to obtain a uniform solution, adding 1.5mmol of gallium nitrate into the uniform solution, stirring uniformly, slowly adding 3.5mL of ethylene glycol into the uniform solution while stirring, slowly dropwise adding 0.5M potassium hydroxide solution into the solution while stirring, continuously stirring for more than 1 hour, transferring the uniformly stirred solution into a reaction kettle with the filling rate of 70%, sealing the reaction kettle, placing the reaction kettle in an oven preheated at 210 ℃, and reactingThe time is 70 minutes, after the reaction is finished and the reaction kettle is cooled to room temperature, the reaction kettle is opened to take out a reaction product, the product is sequentially washed by dilute ammonia water, deionized water and isopropanol for 3 times and then centrifuged to obtain gamma-Ga2O3The transmission electron micrograph of the nanocrystal is shown in FIG. 2.
Example 2
Cu-doped gamma-Ga2O3The low-temperature preparation method of the nanocrystalline comprises the following steps:
dissolving 0.2g P123 in 4mL of deionized water, stirring to obtain a uniform solution, adding 1.5mmol of gallium nitrate and 0.045mmol of copper nitrate into the uniform solution, stirring uniformly, slowly adding 3.5mL of ethylene glycol into the stirred uniform solution, slowly dropwise adding 0.5M potassium hydroxide solution into the solution under the stirring condition, continuously stirring for more than 1 hour, transferring the uniformly stirred solution into a reaction kettle with the filling rate of 70%, sealing the reaction kettle, placing the reaction kettle into a baking oven preheated at 210 ℃, reacting for 70 minutes, opening the reaction kettle after the reaction is finished and the reaction kettle is cooled to room temperature, taking out a reaction product, washing the product with dilute ammonia water, deionized water and isopropanol for 3 times in sequence, and centrifuging to obtain Cu-doped gamma-Ga2O3And (4) nanocrystals.
Example 3
Cu-doped gamma-Ga2O3The low-temperature preparation method of the nanocrystalline comprises the following steps:
dissolving 0.2g P123 in 4mL of deionized water, stirring to obtain a uniform solution, adding 1.5mmol of gallium nitrate and 0.09mmol of copper nitrate into the uniform solution, stirring uniformly, slowly adding 3.5mL of ethylene glycol into the uniform solution while stirring, slowly dropwise adding 0.5M potassium hydroxide solution into the solution while stirring, continuously stirring for more than 1 hour, transferring the uniformly stirred solution into a reaction kettle with the filling rate of 70%, sealing the reaction kettle, placing the reaction kettle into a baking oven preheated at 210 ℃, reacting for 70 minutes, opening the reaction kettle after the reaction is finished and the reaction kettle is cooled to room temperature, taking out a reaction product, washing the product with dilute ammonia water, deionized water and isopropanol for 3 times in sequence, and centrifuging to obtain Cu-doped gamma-Ga2O3NanocrystalFIG. 3 shows a transmission electron micrograph, and FIG. 4 shows an X-ray photoelectron spectrum.
Example 4
Cu-doped gamma-Ga2O3The low-temperature preparation method of the nanocrystalline comprises the following steps:
dissolving 0.2g P123 in 4mL of deionized water, stirring to obtain a uniform solution, adding 1.5mmol of gallium nitrate and 0.18mmol of copper nitrate into the uniform solution, stirring uniformly, slowly adding 3.5mL of ethylene glycol into the uniform solution while stirring, slowly dropwise adding 0.5M potassium hydroxide solution into the solution while stirring, continuously stirring for more than 1 hour, transferring the uniformly stirred solution into a reaction kettle with the filling rate of 70%, sealing the reaction kettle, placing the reaction kettle into a baking oven preheated at 210 ℃, reacting for 70 minutes, opening the reaction kettle after the reaction is finished and the reaction kettle is cooled to room temperature, taking out a reaction product, washing the product with dilute ammonia water, deionized water and isopropanol for 3 times in sequence, and centrifuging to obtain Cu-doped gamma-Ga2O3And (4) nanocrystals.
Example 5
Cu-doped gamma-Ga2O3The low-temperature preparation method of the nanocrystalline comprises the following steps:
dissolving 0.2g P123 in 4mL of deionized water, stirring to obtain a uniform solution, adding 1.5mmol of gallium nitrate and 0.09mmol of copper sulfate into the uniform solution, stirring uniformly, slowly adding 3.5mL of ethylene glycol into the uniform solution while stirring, slowly dropwise adding 0.5M potassium hydroxide solution into the solution while stirring, continuously stirring for more than 1 hour, transferring the uniformly stirred solution into a reaction kettle with the filling rate of 70%, sealing the reaction kettle, placing the reaction kettle into a baking oven preheated at 210 ℃, reacting for 70 minutes, opening the reaction kettle after the reaction is finished and the reaction kettle is cooled to room temperature, taking out a reaction product, washing the product with dilute ammonia water, deionized water and isopropanol for 3 times in sequence, and centrifuging to obtain Cu-doped gamma-Ga2O3And (4) nanocrystals.
Example 6
Cu-doped gamma-Ga2O3The low-temperature preparation method of the nanocrystalline comprises the following steps:
dissolving 0.2g P123 in 4mL of deionized water, stirring to obtain a uniform solution, adding 1.5mmol of gallium nitrate and 0.09mmol of copper nitrate into the uniform solution, stirring uniformly, slowly adding 3.5mL of ethylene glycol into the uniform solution while stirring, slowly dropwise adding 0.5M of sodium hydroxide solution into the solution while stirring, continuously stirring for more than 1 hour, transferring the uniformly stirred solution into a reaction kettle with the filling rate of 70%, sealing the reaction kettle, placing the reaction kettle into a baking oven preheated at 210 ℃, reacting for 70 minutes, opening the reaction kettle after the reaction is finished and the reaction kettle is cooled to room temperature, taking out a reaction product, washing the product with dilute ammonia water, deionized water and isopropanol for 3 times in sequence, and centrifuging to obtain Cu-doped gamma-Ga2O3And (4) nanocrystals.
Example 7
Based on gamma-Ga2O3The preparation method of the perovskite solar cell of the hole transport layer comprises the following steps:
etching 1.5cm × 0.4cm traces on the surface of a 1.5cm × 1.5cm FTO substrate, sequentially placing the FTO in a cleaning agent, deionized water and absolute ethyl alcohol for 15 minutes by ultrasonic treatment, performing ultraviolet ozone treatment on the cleaned FTO for 15 minutes, and treating the gamma-Ga prepared in example 12O3Uniformly dispersing 5mg/mL of nanocrystalline in a mixed solution of isopropanol and dimethyl sulfoxide with the volume ratio of 1:1 to prepare a hole transport layer precursor solution, dropwise adding 50 mu L of the solution on FTO, spin-coating for 60s at the rotation speed of 4000r, repeating the step for 5 times, then placing the FTO on a heating plate, drying for 10 minutes at 100 ℃ to obtain gamma-Ga2O3A hole transport layer. Dissolving 66mg of cesium iodide, 187mg of iodoformamidine, 12mg of bromomethylamine, 568mg of lead iodide and 80mg of lead bromide in 1mL of mixed solution of dimethylformamide and dimethyl sulfoxide in a volume ratio of 4:1, adding hydroxyethyl acrylate in a total solution volume ratio of 1% to prepare perovskite precursor solution, dropwise adding 50 mu L of perovskite precursor solution onto a hole transport layer, spin-coating 5s at the speed of 500r, spin-coating 45s at the speed of 5000r, dropwise adding 100uL of chlorobenzene as an anti-solvent when 5000r is rotated for 15s, and immediately heating on a heating plate at 100 ℃ for 10 minutes after the spin-coating is finished. Prepare 10mg/mL PCB61M in chlorobenzene, prepared by spin-coating for 30s at 3000r, on a perovskite layer, with C60And BCP as an evaporation material, about 30nm and 8nm were evaporated, respectively. Finally, silver is used as an evaporation material, a silver electrode with the thickness of about 80nm is evaporated on the surface of the electron transport layer, and the gamma-Ga-based method is immediately completed2O3And preparing the hole transport layer perovskite solar cell.
The illumination intensity is 100mW cm-2The AM 1.5 of (1) tests the current density-voltage curve of the device under the irradiation of simulated sunlight, and the open-circuit voltage of the device is 0.98V and the short-circuit current density is 14.9mA cm-2The fill factor was 0.52 and the photoelectric conversion efficiency was 7.6%, and the J-V curve thereof is shown in FIG. 6.
Example 8
Gamma-Ga based on Cu doping2O3The preparation method of the perovskite solar cell of the hole transport layer comprises the following steps:
etching 1.5cm × 0.4cm traces on the surface of a 1.5cm × 1.5cm FTO substrate, sequentially placing the FTO in a cleaning agent, deionized water and absolute ethyl alcohol for 15 minutes by ultrasonic treatment, performing ultraviolet ozone treatment on the cleaned FTO for 15 minutes, and doping the Cu prepared in the example 2 with gamma-Ga2O3Uniformly dispersing 5mg/mL of nanocrystalline in a mixed solution of isopropanol and dimethyl sulfoxide with the volume ratio of 1:1 to prepare a hole transport layer precursor solution, dropwise adding 50 mu L of the solution on FTO, spin-coating for 60s at the rotation speed of 4000r, repeating the step for 5 times, then placing the FTO on a heating plate, drying for 10 minutes at 100 ℃ to obtain Cu-doped gamma-Ga2O3FIG. 5 shows a scanning electron micrograph of the hole transport layer. Dissolving 66mg of cesium iodide, 187mg of iodoformamidine, 12mg of bromomethylamine, 568mg of lead iodide and 80mg of lead bromide in 1mL of mixed solution of dimethylformamide and dimethyl sulfoxide in a volume ratio of 4:1, adding hydroxyethyl acrylate in a total solution volume ratio of 1% to prepare perovskite precursor solution, dropwise adding 50 mu L of perovskite precursor solution onto a hole transport layer, spin-coating 5s at the speed of 500r, spin-coating 45s at the speed of 5000r, dropwise adding 100uL of chlorobenzene as an anti-solvent when 5000r is rotated for 15s, and immediately heating on a heating plate at 100 ℃ for 10 minutes after the spin-coating is finished. 10mg/mL ofPCB61M in chlorobenzene, prepared by spin-coating for 30s at 3000r, on a perovskite layer, with C60And BCP as an evaporation material, about 30nm and 8nm were evaporated, respectively. Finally, silver is used as an evaporation material, a silver electrode with the thickness of about 80nm is evaporated on the surface of the electron transport layer, and the gamma-Ga doping based on Cu is completed immediately2O3And preparing the hole transport layer perovskite solar cell.
The illumination intensity is 100mW cm-2The AM 1.5 of (1) is used for testing the current density-voltage curve of the device under the irradiation of simulated sunlight, and the open-circuit voltage of the device is 1.06V and the short-circuit current density is 21.8mA cm-2The fill factor was 0.69, the photoelectric conversion efficiency was 15.9%, and the J-V curve thereof is shown in FIG. 6.
Example 9
Gamma-Ga based on Cu doping2O3The preparation method of the perovskite solar cell of the hole transport layer comprises the following steps:
etching 1.5cm × 0.4cm traces on the surface of a 1.5cm × 1.5cm FTO substrate, sequentially placing the FTO in a cleaning agent, deionized water and absolute ethyl alcohol for 15 minutes by ultrasonic treatment, performing ultraviolet ozone treatment on the cleaned FTO for 15 minutes, and doping the Cu prepared in example 3 with gamma-Ga2O3Uniformly dispersing 5mg/mL of nanocrystalline in a mixed solution of isopropanol and dimethyl sulfoxide with the volume ratio of 1:1 to prepare a hole transport layer precursor solution, dropwise adding 50 mu L of the solution on FTO, spin-coating for 60s at the rotation speed of 4000r, repeating the step for 5 times, then placing the FTO on a heating plate, drying for 10 minutes at 100 ℃ to obtain Cu-doped gamma-Ga2O3A hole transport layer. Dissolving 66mg of cesium iodide, 187mg of iodoformamidine, 12mg of bromomethylamine, 568mg of lead iodide and 80mg of lead bromide in 1mL of mixed solution of dimethylformamide and dimethyl sulfoxide in a volume ratio of 4:1, adding hydroxyethyl acrylate in a total solution volume ratio of 1% to prepare perovskite precursor solution, dropwise adding 50 mu L of perovskite precursor solution onto a hole transport layer, spin-coating 5s at the speed of 500r, spin-coating 45s at the speed of 5000r, dropwise adding 100uL of chlorobenzene as an anti-solvent when 5000r is rotated for 15s, and immediately heating on a heating plate at 100 ℃ for 10 minutes after the spin-coating is finished. Prepare 10mg/mL PCB61M in chlorobenzene, prepared by spin-coating for 30s at 3000r, on a perovskite layer, with C60And BCP as an evaporation material, about 30nm and 8nm were evaporated, respectively. Finally, silver is used as an evaporation material, a silver electrode with the thickness of about 80nm is evaporated on the surface of the electron transport layer, and the gamma-Ga doping based on Cu is completed immediately2O3And preparing the hole transport layer perovskite solar cell.
The illumination intensity is 100mW cm-2The AM 1.5 of (1) is used for testing the current density-voltage curve of the device under the irradiation of simulated sunlight, and the open-circuit voltage of the device is 1.12V and the short-circuit current density is 22.9mA cm-2The fill factor was 0.76 and the photoelectric conversion efficiency was 19.5%, and the J-V curve thereof is shown in FIG. 6.
Example 10
Gamma-Ga based on Cu doping2O3The preparation method of the perovskite solar cell of the hole transport layer comprises the following steps:
etching 1.5cm × 0.4cm traces on the surface of a 1.5cm × 1.5cm FTO substrate, sequentially placing the FTO in a cleaning agent, deionized water and absolute ethyl alcohol for 15 minutes by ultrasonic treatment, performing ultraviolet ozone treatment on the cleaned FTO for 15 minutes, and doping the Cu prepared in example 4 with gamma-Ga2O3Uniformly dispersing 5mg/mL of nanocrystalline in a mixed solution of isopropanol and dimethyl sulfoxide with the volume ratio of 1:1 to prepare a hole transport layer precursor solution, dropwise adding 50 mu L of the solution on FTO, spin-coating for 60s at the rotation speed of 4000r, repeating the step for 5 times, then placing the FTO on a heating plate, drying for 10 minutes at 100 ℃ to obtain Cu-doped gamma-Ga2O3A hole transport layer. Dissolving 66mg of cesium iodide, 187mg of iodoformamidine, 12mg of bromomethylamine, 568mg of lead iodide and 80mg of lead bromide in 1mL of mixed solution of dimethylformamide and dimethyl sulfoxide in a volume ratio of 4:1, adding hydroxyethyl acrylate in a total solution volume ratio of 1% to prepare perovskite precursor solution, dropwise adding 50 mu L of perovskite precursor solution onto a hole transport layer, spin-coating 5s at the speed of 500r, spin-coating 45s at the speed of 5000r, dropwise adding 100uL of chlorobenzene as an anti-solvent when 5000r is rotated for 15s, and immediately heating on a heating plate at 100 ℃ for 10 minutes after the spin-coating is finished. Prepare 10mg/mL PCB61M chlorobenzeneSolution prepared by spin-coating at 3000r for 30s on a perovskite layer using C60And BCP as an evaporation material, about 30nm and 8nm were evaporated, respectively. Finally, silver is used as an evaporation material, a silver electrode with the thickness of about 80nm is evaporated on the surface of the electron transport layer, and the gamma-Ga doping based on Cu is completed immediately2O3And preparing the hole transport layer perovskite solar cell.
The illumination intensity is 100mW cm-2The AM 1.5 of (1) tests the current density-voltage curve of the device under the irradiation of simulated sunlight, and the open-circuit voltage of the device is 0.99V and the short-circuit current density is 21.3mA cm-2The fill factor was 0.59 and the photoelectric conversion efficiency was 12.4%, and the J-V curve thereof is shown in FIG. 6.
TABLE 1 parameters of perovskite solar cells prepared in examples 7-10
Figure BDA0003335149390000081
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that are not conceived by the inventive step should be included within the scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope defined by the claims.

Claims (7)

1. Gamma-Ga2O3Or Cu doped gamma-Ga2O3The preparation method of the nanocrystalline comprises the following steps:
(1) placing reactants in a beaker, adding deionized water into the beaker, and stirring to form a uniform mixed solution, wherein the reactants comprise a gallium source, a copper source and a surfactant; wherein the gallium source and the copper source are in the form of Ga3+And Cu2+In a molar ratio of 1:0 to 0.12, per 3mmol of Ga3+0.4 grams of surfactant was used;
(2) adding ethylene glycol into the solution obtained in the step (1) under the condition of stirring, and stirring to form a uniform mixed solution, wherein each 3mmol of Ga3+7mL of ethylene glycol was used;
(3) slowly adding a precipitator into the mixed solution in the stirring in the step (2), and stirring again until the mixed solution is uniform;
(4) after stirring is finished, transferring the mixed solution obtained in the step (3) to a reaction kettle for carrying out;
(5) after the hydrothermal reaction is finished and the reaction kettle is cooled, cleaning the product, centrifuging and removing the supernatant to obtain the gamma-Ga2O3Or Cu doped gamma-Ga2O3And (4) a nanocrystalline product.
2. gamma-Ga according to claim 12O3Or Cu doped gamma-Ga2O3The preparation method of the nano-crystal is characterized in that the gallium source in the step (1) is gallium nitrate or other Ga-containing gallium3+The copper source is copper nitrate or other Cu-containing compounds2+The surfactant is P123Or polyethylene glycol.
3. gamma-Ga according to claim 12O3Or Cu doped gamma-Ga2O3The preparation method of the nanocrystal is characterized in that the precipitator in the step (3) is potassium hydroxide, sodium hydroxide, ammonia water or ethylenediamine.
4. gamma-Ga according to claim 12O3Or Cu doped gamma-Ga2O3The method for preparing the nanocrystal is characterized in that the hydrothermal reaction in the step (4) is carried out at 210 ℃ for 70 minutes.
5. gamma-Ga according to claim 12O3Or Cu doped gamma-Ga2O3The preparation method of the nanocrystalline is characterized in that the cleaning method of the product in the step (5) is as follows: the reaction product was washed 3 times with dilute ammonia, deionized water and isopropanol respectively and centrifuged to remove the supernatant.
6. gamma-Ga prepared according to claim 12O3Or Cu doped gamma-Ga2O3Use of nanocrystals characterized by the presence of gamma-Ga2O3Or Cu doped gamma-Ga2O3The preparation method of the perovskite solar cell by using the nanocrystalline as a hole transport layer comprises the following steps:
1) etching FTO, and etching a trace with the width of 4mm on the FTO surface with the width of 1.5cm multiplied by 1.5cm by using a laser marking machine, wherein the FTO is SnO doped with fluorine2Transparent conductive glass;
2) cleaning the FTO, sequentially placing the etched FTO in a cleaning agent, deionized water and absolute ethyl alcohol for ultrasonic treatment for 15 minutes, then blowing the FTO by using air flow, and then carrying out ultraviolet ozone treatment for 15 minutes;
3) preparing a hole transport layer from gamma-Ga2O3Or Cu doped gamma-Ga2O3Dispersing the nanocrystalline in a mixed solvent of dimethyl sulfoxide and isopropanol with the volume ratio of 1:1 according to the concentration of 5mg/mL for later use; dripping 50 mu L of the dispersion liquid on the FTO treated in the step 2), spin-coating and drying to obtain a hole transport layer;
4) preparing a perovskite layer, taking dimethylformamide and dimethyl sulfoxide with a volume ratio of 4:1 as a mixed solvent, preparing a mixed solution by using 66mg of cesium iodide, 187mg of iodoformamidine, 12mg of bromomethylamine, 568mg of lead iodide and 80mg of lead bromide in each 1mL of solvent, adding hydroxyethyl acrylate with the volume ratio of 1% of the total solution to obtain a perovskite precursor solution, dropwise adding 50 mu L of the perovskite precursor solution onto the hole transport layer prepared in the step 3), spin-coating for 5s at the number of revolutions of 500r, spin-coating for 45s at the number of revolutions of 5000r, dropwise adding 100 mu L of chlorobenzene as an anti-solvent when 5000r spins for 15s, immediately putting the perovskite layer on a heating plate at 100 ℃ after spin-coating, and heating for 10 minutes to obtain the perovskite layer;
5) preparing electron transport layer, collecting 40 μ L PCB with concentration of 10mg/mL61M in chlorobenzene solution was added dropwise to the perovskite layer, spin-coated at 3000r for 30s, using C60Evaporating to form 30nm thick layer, evaporating to form 8nm thick layer with BCP as evaporating material to obtain electron transport layer, and making PCB61M is [6,6 ]]-phenyl C61 butyric acid methyl ester, said C60Is fullerene C60The BCP is bathocuproine;
6) plating electrodes, using silver as an evaporation material, and evaporating a layer of silver electrode with the thickness of 80nm on the surface of the electron transport layer by using an evaporation coating machine to obtain the gamma-Ga based on Cu doping2O3A hole transport layer.
7. A γ -Ga according to claim 62O3Or Cu doped gamma-Ga2O3Use of nanocrystals, characterized in that in the preparation of a hole transport layer in step 3), Cu is used to dope γ -Ga2O3Nanocrystalline with the doping amount of Cu according to the molar ratio2+:Ga3+3: 50; the spin coating and drying are carried out, wherein the spin coating is carried out for 60s at the rotation speed of 4000r for 5 times in total, and the drying condition is that the drying is carried out for 10 minutes at the temperature of 100 ℃.
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