CN115224201A - Perovskite mesomorphic semiconductor material, preparation method and application in solar cell - Google Patents

Perovskite mesomorphic semiconductor material, preparation method and application in solar cell Download PDF

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CN115224201A
CN115224201A CN202210718186.9A CN202210718186A CN115224201A CN 115224201 A CN115224201 A CN 115224201A CN 202210718186 A CN202210718186 A CN 202210718186A CN 115224201 A CN115224201 A CN 115224201A
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perovskite
mesomorphic
ligand
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袁建宇
张旭良
黄贺贺
马万里
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Suzhou University
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    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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Abstract

The invention relates to a perovskite mesomorphic semiconductor material, a preparation method and application in a solar cell. The initiator which can react with oleic acid and oleylamine ligand on the surface of perovskite nanocrystal mildly is added to remove the surface ligand, and then the short-chain organic ligand is introduced to induce the material to self-assemble, so that the ordered nanoparticle superstructure with the mesoscopic scale of dozens of nanometers to several micrometers is obtained. The invention adopts the initiator and the organic ligand to regulate and control the chemical environment of the surface of the nanocrystal through solution phase ligand exchange, can effectively exchange insulating ligands on the surface of the nanocrystal and does not damage the crystal structure; the perovskite mesomorphic material with an ordered mesoscale structure is prepared by introducing a short-chain ligand to induce self-assembly of the nanocrystal; the highly dispersed and highly stable mesomorphic conductive ink is prepared by selecting the solvent, so that one-step spin coating or blade coating film forming can be realized without a complicated layer-by-layer deposition process and a complicated ligand exchange process, and the device preparation process is simplified; the prepared perovskite mesomorphic solar cell obtains the device efficiency of more than 14 percent.

Description

Perovskite mesomorphic semiconductor material, preparation method and application in solar cell
Technical Field
The invention relates to a perovskite mesomorphic semiconductor material, a preparation method and application in a solar cell, belonging to the technical field of photoelectric materials.
Background
The mesocrystal is a three-dimensional ordered assembly with a mesoscopic size (1-1000 nm) formed by bridging the nanocrystals through organic matters, partially connecting the nanocrystals through the organic matters or partially connecting the nanocrystals by themselves and completely connecting the nanocrystals by themselves, shows a property similar to a single crystal, and effectively reduces the recombination probability of a current carrier in the internal transmission process of the material. Oxide mesogenic semiconductor materials (e.g. ZnO, tiO) synthesized by hydrothermal or solvothermal methods 2 、Al 2 O 3 、SnO 2 Etc.) and lead-sulfur group mesomorphic semiconductor materials (such as CdS/CdSe, pbS, etc.) show great application potential in the fields of photocatalysis, solar cells and ion cells due to the unique photoelectric properties of the lead-sulfur group mesomorphic semiconductor materials.
Perovskite semiconductor is used as a new photoelectric star material, and is widely applied to the fields of solar cells, light emission, photo-detection, catalysis and the like due to the advantages of large defect tolerance, long carrier diffusion length, adjustable band gap and the like. However, the mesomorphic structure of the material is less researched, which is due to the poor structural stability of the perovskite material caused by the ionic property of the perovskite material. In 2015, the teaching of Kovalenko synthesized perovskite nanocrystals by hot injection method for the first time (see documents: l. Protesescu, s. Yakuin, m.i. Bodnarchuk, f. Krieg, r. Caputo, c.h. Hendon, r.x. Yang, a. Walsh, m.v. Kovalenko, nano lett. 2015, 15, 3692.), because of the size effect, the perovskite nanocrystals exhibited higher structural stability compared to bulk materials, which provides an important opportunity for preparing and studying perovskite mesomorphic semiconductors and superlattice materials.
At present, the surface of a perovskite nanocrystal prepared by a widely adopted thermal injection method is usually coated with long-chain insulated oleic acid and oleylamine ligands, so that a larger dielectric layer is arranged between the nanocrystal and the nanocrystal to block the transmission of current carriers, and the material is difficult to be directly applied to photoelectric devices; in the preparation process of the film, a layer-by-layer deposition process and complex solid-phase ligand exchange are required, so that the difficulty in regulating and controlling the surface ligand and the complexity of device preparation are greatly increased, and the perovskite nanocrystalline is difficult to popularize and apply on a large scale.
Disclosure of Invention
The invention provides a perovskite mesomorphic semiconductor material, a preparation method and application in a solar cell, aiming at the defects of poor conductivity, poor stability, complicated device preparation and the like of the existing perovskite nanocrystalline material, and adopting a liquid phase ligand exchange process to prepare perovskite mesomorphic ink and form a film in one step.
The technical scheme for realizing the aim of the invention is to provide a preparation method of a perovskite mesomorphic semiconductor material, which comprises the following steps:
(1) Dispersing the perovskite nanocrystalline with the surface coated with oleic acid and oleylamine long-chain ligand in a solvent, and preparing a perovskite nanocrystalline solution with the concentration of 20-100 mg/ml; the solvent comprises one of n-hexane, n-octane, toluene and chloroform, or any combination thereof;
(2) Dropwise adding an initiator into the perovskite nanocrystalline solution prepared in the step (1) to perform liquid phase ligand exchange reaction, and then performing centrifugal treatment to obtain perovskite mesocrystals; the initiator comprises one of dipropylamine, dibutylamine and dipentylamine, or any combination thereof;
(3) Adding a short-chain ligand into a solvent to prepare a ligand solution with the concentration of 0.00001-1M, wherein the short-chain ligand comprises one of sulfocyanic acid Formamidine (FASCN), sulfocyanic acid Methylamine (MASCN), phenethylamine (PEA), amphetamine, triphenylphosphine (TPP), triphenylphosphine Oxide (TOP) and triphenyl phosphite (TPPI), or any combination of the two; the solvent comprises one of toluene, chlorobenzene and chloroform, or any combination thereof; and (3) adding the ligand solution into the perovskite mesogen prepared in the step (2), and fully mixing to obtain the perovskite mesogen ink.
The perovskite mesomorphic ink prepared according to the method is prepared into the perovskite mesomorphic film by adopting a one-step spin coating, spray coating or blade coating process.
The invention provides a preparation method of a perovskite mesomorphic semiconductor material, and the preferable process conditions are as follows: the liquid phase ligand exchange reaction time is 10 seconds to 10 minutes; the centrifugal treatment condition is 500-4000 r/min; the volume ratio of the initiator to the perovskite nanocrystal solution is 0.00001-1.
The concentration of the perovskite mesogen ink provided by the invention is 10-500 mg/ml.
The technical scheme of the invention also comprises the perovskite mesomorphic ink and the perovskite mesomorphic film which are obtained by the preparation method.
The invention provides application of perovskite mesomorphic ink in a light absorption layer of a solar cell, wherein the solar cell comprises a conductive glass substrate, an electron transmission layer, a perovskite mesomorphic light absorption layer, a hole transmission layer and a metal electrode, and is characterized by comprising the following steps:
(1) Preparing an electron transport layer on a conductive glass substrate;
(2) Preparing a hybrid perovskite thin film light absorption layer with the thickness of 50-800 nanometers on the electron transmission layer by adopting a one-step spin coating or blade coating process;
(3) Preparing a hole transport layer with the thickness of 30-80 nanometers on the light absorption layer by adopting a spin coating process;
(4) And depositing a metal electrode on the hole transport layer by adopting a vacuum coating process to obtain the perovskite mesomorphic solar cell.
The perovskite mesomorphic crystal semiconductor material provided by the invention has ordered nanoparticle superstructure with mesoscopic scale of dozens of nanometers to several micrometers, which is formed by self-assembling perovskite nanocrystals in a ligand-induced mode, and the crystal structure of the perovskite mesomorphic crystal semiconductor material is ABX 3 Wherein A is formamidine (CH (NH) 2 ) 2 + ) Or methylamine (CH) 3 NH 3 + ) An organic cation, B is Pb 2+ Or Sn 2+ X is I - 、Br - 、Cl - Or a mixture thereof; according to the invention, by adopting the technical scheme of adding the initiator and the short-chain ligand into the solution phase, the ligand exchange on the surface of the nano-crystal is adopted, and then the self-assembly is induced, so that the preparation of the ordered mesoscale structural perovskite mesomorphic material is realized.
The principle of the invention is as follows: adding polar organic molecular initiators which can react with the ligand on the surface of the nano-crystal, such as dipropylamine and the like, into the perovskite nano-crystal solution, removing the ligand on the surface of the nano-crystal without damaging the crystal structure of the material, after a liquid phase ligand exchange reaction is carried out for a period of time, removing a large amount of the ligand on the surface of the nano-crystal to induce aggregation and assembly, generating hybrid perovskite mesocrystals with the size of dozens of nanometers to several micrometers, and separating the obtained perovskite mesocrystals through centrifugal treatment; the obtained perovskite mesocrystal cannot be dispersed into solvents with smaller dielectric constants such as normal hexane, normal octane and the like because a large amount of surface ligands are removed and the assembly size is larger, and the perovskite mesocrystal is prepared by adding short-chain ligand short-chain organic amine or organic phosphine ligand into nonpolar solvents such as toluene and the like to prepare ligand solution and adding the ligand solution into the perovskite mesocrystal for full mixing; by controlling the concentration of the short-chain ligand and the volume of the solution, the perovskite mesomorphic ink with the concentration of 10-500 mg/ml, high dispersion stability (more than 2 months) and high electronic coupling can be obtained.
The invention adopts a proper surface chemical regulation and control means to realize the phase-ligand exchange of the perovskite nano-crystalline liquid phase, then introduces a new ligand to induce the self-assembly of the perovskite nano-crystalline to prepare the perovskite mesomorphic conductive ink, and can directly prepare the perovskite mesomorphic thin film with high electronic coupling by the perovskite mesomorphic ink prepared by the invention through one-step spin coating, spray coating, blade coating and other modes. The invention provides a novel film forming process, which is used for preparing a perovskite mesomorphic film of a photoelectric device, does not need to adopt a complex layer-by-layer deposition process and a complex solid-phase ligand exchange process, can be used for photosensitive layers of solar cells, photodetectors and light-emitting diodes, and has important practical significance for the commercial application of perovskite semiconductor materials in the photoelectric field.
Compared with the prior art, the technology of the invention has the following outstanding characteristics:
1. the invention provides a mild perovskite nanocrystal liquid phase ligand exchange process by selecting an initiator which can react mildly with a perovskite nanocrystal surface ligand; meanwhile, a new short-chain conductive ligand is introduced to passivate surface defects, nanocrystalline is induced to be self-assembled to form highly ordered mesocrystals, and the conductivity and stability of perovskite nanocrystalline are improved, so that the preparation of high-performance perovskite mesocrystal ink is realized.
2. The ink prepared by the invention provides a one-step film forming process compatible with technical means such as spin coating, spray coating, blade coating and the like, and solves the problems of complicated layer-by-layer deposition process and difficult-to-control solid phase ligand exchange in the preparation process of the traditional perovskite nanocrystalline device, thereby simplifying the preparation process of the device and being beneficial to the commercial popularization of the perovskite nanocrystalline.
3. The invention selects near infrared absorption perovskite nanocrystalline, prepares a high-efficiency perovskite mesomorphic solar cell, obtains the recording photoelectric conversion efficiency of the material in the application of the solar cell of 14.04% (the recording of the prior art is 13.2%, see the document J. Mater. Chem. A, 2020,8, 8104-8112), and proves the feasibility of the application of the material and the technical means in the photoelectric device.
Drawings
FIG. 1 is a Transmission Electron Microscope (TEM) comparison of perovskite mesocrystals prepared in example 1 of the present invention with standard perovskite nanocrystals;
FIG. 2 is a graph comparing the dynamic light scattering of perovskite mesocrystals prepared in example 2 of the present invention in different solvents;
fig. 3 is a schematic device structure diagram of a perovskite mesomorphic solar cell provided in embodiment 4 of the present invention;
FIG. 4 is a current density-voltage (J-V) plot of a perovskite mesogenic solar cell prepared in example 4 of the present invention;
in the figure, 1. A conductive glass substrate; 2. an electron transport layer; 3. a light absorbing layer; 4. a hole transport layer; 5. and a metal electrode.
Detailed Description
The technical scheme of the invention is further explained by combining the drawings and the embodiment.
Example 1
The embodiment provides a hybrid FAPBI 3 The preparation method of the perovskite mesomorphic ink comprises the following specific steps:
in the first step of the method,FAPBI coated with oleic acid and oleylamine and synthesized by hot injection method 3 Perovskite nanocrystals (the synthesis method is shown in the literature: nat. Commun. 2019, 10, 2842) are dispersed in n-hexane solution to prepare a nanocrystal solution with the concentration of 30 mg/ml for later use;
step two, taking dipropylamine as an initiator, dripping 30 microliters of dipropylamine into 20 milliliters of nanocrystal solution, standing for about 10 seconds, and gathering and assembling nanocrystals;
step three, centrifuging the product obtained in the step two for 2 minutes at the rotating speed of 1000 revolutions per minute, separating the settled mesogen, pouring out liquid after centrifugation, reserving the obtained solid, namely the hybrid perovskite mesogen, and weighing;
and step four, adding the hybrid perovskite mesogen obtained in the step three into a dispersant toluene, so that the hybrid perovskite mesogen has a good dispersion effect, and preparing the perovskite mesogen ink.
Referring to fig. 1, a Transmission Electron Microscope (TEM) comparison graph of the perovskite mesogen prepared in this example and a standard perovskite nanocrystal is shown; in the figure, (a) is a standard FAPBI without liquid phase ligand exchange 3 The morphology of the perovskite nanocrystal, and (b) the graph shows the morphology of the surface ligand-induced self-assembled hybrid perovskite mesogen provided in this example. Comparing the graph (a) with the graph (b) can prove that the aggregation assembly of the nanocrystals is induced after the reaction of the initiator and the ligands on the surfaces of the perovskite nanocrystals.
Example 2
This example provides a hybrid MAPbI 3 The preparation method of the perovskite mesomorphic ink comprises the following specific steps:
the method comprises the following steps: the MAPbI3 perovskite nano crystal coated with oleic acid and oleylamine (the synthesis method is shown in Chinese invention patent CN 114276800A) synthesized by a hot injection method is dispersed in a normal hexane solution to prepare a nano crystal solution with the concentration of 30 mg/ml for standby;
step two: dipropylamine is used as an initiator, 40 microliters of dipropylamine is dripped into 20 milliliters of nanocrystal solution, and the nanocrystal is stood for about 10 seconds and starts to be assembled in an aggregation way;
step three: separating the settled mesocrystals by a centrifugal machine, centrifuging for 3 minutes at the rotating speed of 1500 rpm, pouring out supernatant, and reserving and weighing the obtained solid;
step four: obtained hybrid MAPbI 3 The perovskite mesogen can not be dispersed in solvents with smaller dielectric constants such as normal hexane, normal octane and the like because a large amount of surface ligands are removed, the dispersion stability of the perovskite mesogen is tested by comparing nonpolar solvents with different dielectric constants such as normal hexane, chlorobenzene, chloroform, toluene and the like, and the perovskite mesogen ink with the best dispersion stability can be obtained by selecting the toluene as a dispersing agent.
Referring to fig. 2, a graph comparing the dynamic light scattering of the perovskite mesogen prepared in this example in different solvents is shown; in the figure, the non-polar solvent pairs with different dielectric constants such as n-hexane, chlorobenzene, chloroform, toluene and the like are respectively compared with MAPbI 3 The dispersity of the mesogen (the concentration is 20 mg/ml) is poor by using n-octane as shown in figure 2, the obtained perovskite mesogen can be dispersed by using other solvents, and the stability of the toluene-dispersed hybrid perovskite mesogen is better.
Example 3
The embodiment provides a hybrid FAPBI 3 The method for preparing the perovskite mesomorphic film by adopting the perovskite mesomorphic ink through the one-step spin coating process comprises the following specific steps:
the method comprises the following steps: FAPBI synthesized by hot injection method and coated with oleic acid and oleylamine 3 Dispersing the perovskite nano-crystal in a normal hexane solution to prepare 30 mg/ml for later use;
step two: adopting dibutylamine as an initiator, dropwise adding 30 microliters of dibutylamine into 20 milliliters of nanocrystal solution, standing for about 10 seconds, and allowing nanocrystals to start to be assembled in an aggregation manner;
step three: separating the settled mesocrystals by a centrifugal machine, centrifuging for 2 minutes at the rotating speed of 2000 r/min, pouring out supernatant, and reserving and weighing the obtained solid;
step four: TPP as a new ligand is dissolved in toluene with the concentration of 1.5 mg/ml, and then the solution is added into the obtained solid to prepare the required concentration, thus obtaining the hybridized FAPBI with high stability, high electron coupling and low surface defect state after ligand exchange 3 PerovskiteA mesogenic ink.
In this embodiment, toluene is selected as a solvent for dispersing the hybrid perovskite mesogen prepared in step three, perovskite mesogen inks with different concentrations are prepared according to the ink concentrations (mg/ml) provided in table 1, and high-quality perovskite thin films with different thicknesses are prepared by regulating the spin coating rate and adopting a one-step spin coating film forming process.
See table 1 for thickness parameters of films prepared with different concentrations of perovskite mesogenic ink and different spin speeds.
TABLE 1
Ink concentration (mg/ml) Spin speed (rpm) Film thickness (nanometer)
100 1000 150±20
200 1000 300±20
200 2000 200±20
300 1000 400±20
300 2000 350±20
The film provided by the embodiment can be used for photosensitive layers of photoelectric devices such as solar cells, photodetectors, light-emitting diodes, memristors or field effect transistors and the like, and has high application value.
At present, a layer-by-layer deposition process is an essential process for preparing perovskite nanocrystalline solar cells in the prior art (see documents: science 2016, 354, 92, sci. Adv. 2017, 3, eaao 4204); the preparation method of the perovskite mesomorphic ink thin film provided by the invention can obtain the thin film with the required thickness only by one-step operation, has simple process, and avoids the complex layer-by-layer deposition process and the complex solid phase ligand exchange process. The method provided by the invention can be expanded to blade coating and spraying processes and is compatible with large-area printing technology.
Example 4
The embodiment provides a hybrid FAPBI 3 The preparation method of the perovskite mesomorphic solar cell realizes the recording efficiency of the material solar cell, and the photoelectric conversion efficiency of the material solar cell is obviously improved. Referring to fig. 3, which is a schematic view of the device structure of the solar cell, as shown in fig. 3, an electron transport layer 2, a perovskite nanocrystal light absorption layer 3, a hole transport layer 4 and a metal electrode 5 are sequentially prepared on a conductive glass substrate 1. The preparation of the battery comprises the following steps:
sequentially carrying out ultrasonic washing treatment on fluorine-doped tin oxide (FTO) conductive glass by using liquid detergent, deionized water, isopropanol and acetone; preparation of dense TiO with thickness of about 40 nm on a cleaned conductive glass substrate 1 by chemical water bath deposition 2 Film-forming to obtain an electron transport layer 2, and annealing at 200 ℃ for 30 minutes;
step two, adopting a one-step spin coating film forming mode to prepare 200 mg/ml FAPBI prepared in the example 3 in a dry air atmosphere 3 The toluene solution is perovskite mesomorphic ink and is coated on FTO/TiO by spin coating 2 On a substrate at 1 per minuteSpin-coating at 000 rpm and 2000 rpm for 15 s and 20 s, respectively, and treating the film with FASCN solution of methyl acetate for 5 s to obtain light-absorbing layer 3 with thickness of 300 nm.
And step three, spin-coating a polymer PTAA on the light absorption layer 3 to prepare a hole transport layer 4. PTAA was dissolved in toluene to prepare a solution having a concentration of 15 mg/ml, and after spin-coating at 3000 rpm for 40 seconds, a hole transport layer having a thickness of about 70 nm was formed.
Step four, performing vacuum thermal evaporation on the metal electrode 5 on the hole transport layer 4 X The thickness of Ag is respectively 8 nanometers and 120 nanometers, and complete FAPbI is obtained 3 A perovskite mesomorphic solar cell.
Referring to fig. 4, this example provides selection of a hybrid FAPbI 3 The current density-voltage (J-V) curve graph of the perovskite solar cell prepared by taking the perovskite nanocrystalline as a light absorption layer, utilizing solution phase ligand exchange, using TPP (thermoplastic vulcanizate) for surface modification and adopting a one-step spin coating film forming process; at AM 1.5, 100 mV/cm 2 Under the standard test conditions, the short-circuit current density of the device was measured to be 17.28 mA/cm 2 The open circuit voltage is 1.156V, the fill factor is 0.703, and the photoelectric conversion efficiency is 14.04%, whereas the recording efficiency of the present material is 13.2% (see literature:J. Mater. Chem. A, 2020,8, 8104-8112）。

Claims (9)

1. a preparation method of a perovskite mesomorphic semiconductor material is characterized by comprising the following steps:
(1) Dispersing the perovskite nanocrystalline with the surface coated with oleic acid and oleylamine long-chain ligand in a solvent, and preparing a perovskite nanocrystalline solution with the concentration of 20-100 mg/ml; the solvent comprises one of n-hexane, n-octane, toluene and chloroform, or any combination thereof;
(2) Dropwise adding an initiator into the perovskite nanocrystalline solution prepared in the step (1) to perform liquid phase ligand exchange reaction, and then performing centrifugal treatment to obtain perovskite mesocrystals; the initiator comprises one of dipropylamine, dibutylamine and dipentylamine, or any combination thereof;
(3) Adding a short-chain ligand into a solvent to prepare a ligand solution with the concentration of 0.00001-1M, wherein the short-chain ligand comprises one of sulfocyanic acid Formamidine (FASCN), sulfocyanic acid Methylamine (MASCN), phenethylamine (PEA), amphetamine, triphenylphosphine (TPP), triphenylphosphine Oxide (TOP) and triphenyl phosphite (TPPI), or any combination of the two; the solvent comprises one of toluene, chlorobenzene and chloroform, or any combination thereof; and (3) adding the ligand solution into the perovskite mesogen prepared in the step (2), and fully mixing to obtain the perovskite mesogen ink.
2. The method for preparing a perovskite mesogenic semiconductor material according to claim 1, wherein: the liquid phase ligand exchange reaction time is 10 seconds to 10 minutes.
3. The method for preparing a perovskite mesogenic semiconductor material according to claim 1, wherein: the centrifugal treatment condition is 500-4000 r/min.
4. The method for preparing a perovskite mesogenic semiconductor material according to claim 1, characterized in that: the volume ratio of the initiator to the perovskite nanocrystalline solution is 0.00001-1.
5. The method for preparing a perovskite mesogenic semiconductor material according to claim 1, wherein: the concentration of the perovskite mesogen ink is 10-500 mg/ml.
6. A preparation method of a perovskite mesomorphic semiconductor material is characterized by comprising the following steps: the perovskite mesomorphic ink prepared according to the method in the claim 1 is prepared into the perovskite mesomorphic film by adopting a one-step spin coating, spray coating or blade coating process.
7. A perovskite mesogenic ink obtained by the preparation method according to claim 1.
8. A perovskite mesomorphic film obtained by the process of claim 6.
9. Use of the perovskite mesogenic ink as defined in claim 7 in a light absorbing layer of a solar cell comprising a conductive glass substrate, an electron transporting layer, a perovskite mesogenic light absorbing layer, a hole transporting layer and a metal electrode, characterized in that it comprises the steps of:
(1) Preparing an electron transport layer on a conductive glass substrate;
(2) Preparing a hybrid perovskite thin film light absorption layer with the thickness of 50-800 nanometers by adopting a one-step spin coating or blade coating process on the electron transmission layer;
(3) Preparing a hole transport layer with the thickness of 30-80 nanometers on the light absorption layer by adopting a spin coating process;
(4) And depositing a metal electrode on the hole transport layer by adopting a vacuum coating process to obtain the perovskite mesomorphic solar cell.
CN202210718186.9A 2022-06-23 2022-06-23 Perovskite mesomorphic semiconductor material, preparation method and application in solar cell Pending CN115224201A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115835659A (en) * 2023-02-22 2023-03-21 北京科技大学 Hybrid perovskite solar cell and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115835659A (en) * 2023-02-22 2023-03-21 北京科技大学 Hybrid perovskite solar cell and preparation method thereof

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