CN114284443A - Preparation method of flexible photoelectric detector array - Google Patents

Preparation method of flexible photoelectric detector array Download PDF

Info

Publication number
CN114284443A
CN114284443A CN202111586089.0A CN202111586089A CN114284443A CN 114284443 A CN114284443 A CN 114284443A CN 202111586089 A CN202111586089 A CN 202111586089A CN 114284443 A CN114284443 A CN 114284443A
Authority
CN
China
Prior art keywords
perovskite quantum
inorganic perovskite
solution
quantum dot
molar concentration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202111586089.0A
Other languages
Chinese (zh)
Other versions
CN114284443B (en
Inventor
巫江
沈凯
任翱博
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Electronic Science and Technology of China
Original Assignee
University of Electronic Science and Technology of China
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Electronic Science and Technology of China filed Critical University of Electronic Science and Technology of China
Priority to CN202111586089.0A priority Critical patent/CN114284443B/en
Publication of CN114284443A publication Critical patent/CN114284443A/en
Application granted granted Critical
Publication of CN114284443B publication Critical patent/CN114284443B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00Energy generation through renewable energy sources
    • Y02E10/50Photovoltaic [PV] energy
    • Y02E10/549Organic PV cells

Landscapes

  • Light Receiving Elements (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention discloses a preparation method of a flexible photoelectric detector array, belongs to the technical field of photoelectric materials and devices, and aims to provide a preparation method of a flexible photoelectric detector array, which solves the problems that the air stability of materials is poor and the transport of current carriers is slow in the conventional perovskite detector device technology, a large number of clustering phenomena exist in colloidal quantum dots, and the conventional detector cannot be compatible with a flexible substrate. The invention is suitable for the preparation process of the high spectrum photoelectric detector.

Description

Preparation method of flexible photoelectric detector array
Technical Field
The invention belongs to the technical field of photoelectric materials and devices, and particularly relates to a preparation method of a flexible photoelectric detector array.
Background
With the rapid development of the internet of things and 5G, optoelectronic devices have been widely used in people's daily life, and people's demand for optoelectronic devicesAnd are increasing. As one of the most important components in photoelectric devices, a photoelectric detector can effectively convert optical signals into electrical signals based on the photoelectric effect, and is widely applied to the fields of optical communication, biological monitoring, environmental monitoring, imaging and the like. Currently, commercial photodetector technologies tend to mature and stabilize, for example: the silicon-based detector has the responsivity of 0.4A/W in the visible light range and the detectivity of 1010Jones. However, the thickness of the absorption layer is not less than 1 μm due to its low absorption coefficient. In addition, photodetectors made of other materials, such as indium gallium arsenic and tellurium cadmium mercury, have quite complicated processes and high prices, and are not suitable for the nano photoelectric integrated devices which are developed at a high speed at present. Compared to these traditional materials, organic-inorganic hybrid metal halide perovskites exhibit great potential in the field of optoelectronics. This is mainly due to its higher absorption coefficient, longer diffusion length, tunable bandwidth and faster carrier mobility. In addition, such perovskite materials can be prepared using a solution process, which has great advantages for realizing flexible photovoltaic devices.
Since solar cells based on hybrid perovskite materials were reported in 2009, photovoltaic devices based on perovskite materials were widely studied (Science,2012,338, 643-647). However, since the hybrid perovskite material is very sensitive to moisture and light and heat in air, the stability of the material and the device is poor. The invention provides an effective preparation method based on all-inorganic metal halogen all-inorganic perovskite quantum dots, and realizes high-quality and stable all-inorganic metal halogen all-inorganic perovskite quantum dots and a high-performance flexible photoelectric detector array based on the same by controlling the proportion of a precursor solution, a centrifugal process, an annealing process and accurately regulating and controlling mechanical scribing strength.
Disclosure of Invention
The invention aims to: the preparation method of the high-performance flexible photoelectric detector array is provided, and solves the problems that the air stability of materials is poor, the transport of current carriers is slow in the existing perovskite detector device technology, a large number of clustering phenomena exist in colloid quantum dots, and the existing traditional detector cannot be compatible with a flexible substrate.
The technical scheme adopted by the invention is as follows:
a method for preparing a flexible photodetector array comprises the following steps:
s1, dissolving lead bromide powder in a mixed solvent of isopropanol, propionic acid and n-butylamine, wherein the volume ratio of the isopropanol, the propionic acid and the n-butylamine is 1:1:1, and preparing a lead bromide precursor solution with the molar concentration of 0.5 mol/L;
s2, dissolving cesium carbonate powder in propionic acid to prepare a cesium carbonate precursor solution with the molar concentration of 1.8 mol/L;
s3, adding the lead bromide precursor solution and the cesium carbonate precursor solution prepared by S1 and S2 into a mixed solvent of isopropanol and n-hexane, wherein the volume ratio of the isopropanol to the n-hexane is 1:2, and preparing a homogeneous all-inorganic perovskite quantum dot precursor solution with the molar concentration of 0.006 mol/L;
s4, carrying out 2 times of centrifugal treatment after stirring the homogeneous phase all-inorganic perovskite quantum dot precursor solution, wherein the centrifugal speeds are 1500rpm and 2000rpm respectively, and the time of each centrifugal treatment is 2 minutes;
s5, re-dissolving the centrifuged all-inorganic perovskite quantum dot precursor solution in toluene, and performing ultrasonic treatment to prepare an all-inorganic perovskite quantum dot solution with the molar concentration of 0.0225 mol/L;
s6, using polyethylene glycol terephthalate as a flexible substrate, using indium tin oxide as a transparent electrode, wherein the thickness of the indium tin oxide is 100-150 nm, the surface resistance is 25-30 omega/sq, depositing titanium dioxide on the surface of the flexible substrate by an atomic layer deposition method to serve as an electron transmission layer, and the thickness of the titanium dioxide is 40-60 nm;
s7, preparing the all-inorganic perovskite quantum dot film by using the all-inorganic perovskite quantum dot solution prepared by the S5 in a room-temperature environment through a one-step spin coating method, wherein the spin coating speed is 1000rpm, and the spin coating time is 60 seconds;
s8, immediately annealing the all-inorganic perovskite quantum dot film on a hot bench, wherein the annealing temperature is 120 ℃, the annealing time is 1 minute, repeating the operations of spin coating and annealing, increasing the thickness of the all-inorganic perovskite quantum dot film, the annealing temperature of the last layer of film is 120 ℃, and the annealing time is 5 minutes, so as to ensure the rapid crystallization of the film;
s9, spin-coating a 2,2 ', 7,7 ' -tetrabromo-9, 9 ' -spirodi-tri (4-iodobenzene) amine (Spiro-OMeTAD) solution on the top of the all-inorganic perovskite quantum dot film at the speed of 2500rpm for 25 seconds, and oxidizing for 12 hours in an oxygen-filled atmosphere;
s10, depositing nickel and gold by using a thermal evaporation method, wherein the thicknesses of the nickel and the gold are respectively 10-20 nm and 80-120 nm;
and S11, preparing an array by a mechanical scribing method, and arranging the independent electrodes in an array to form a flexible photoelectric detector array.
In the above scheme, in step S7, before the all-inorganic perovskite quantum dot thin film is prepared by using the one-step spin coating method in a room temperature environment, the all-inorganic perovskite quantum dot solution is placed in an ultrasonic machine for processing, the processing frequency is 40Hz, the processing temperature is 20-30 ℃, the all-inorganic perovskite quantum dots are kept in a vibration state at any time, clusters among the all-inorganic perovskite quantum dots are reduced, and the all-inorganic perovskite quantum dots are uniformly dispersed in the solvent.
In the above scheme, in step S9, the Spiro-OMeTAD solution is prepared by mixing Spiro-OMeTAD powder, 4-tert-butylpyridine and lithium bis (trifluoromethanesulfonylimide) solution in chlorobenzene to form a solution with a molar concentration of 0.056 mol/L. Wherein the volume ratio of the 4-tert-butylpyridine to the lithium bis (trifluoromethanesulfonylimide) solution to the chlorobenzene is 28.8:17.5: 1000.
In the scheme, the lithium bistrifluoromethanesulfonylimide solution is dissolved in acetonitrile, and the molar concentration is 1.8 mol/L.
In the above scheme, in step S11, the device to be processed is placed in the sample stage by using a mechanical scribing method, and the back side is vacuum-absorbed, so as to ensure that the sample does not move randomly during scribing.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the invention, the inorganic all-inorganic perovskite quantum dot material is adopted to replace the traditional silicon and III-V materials, and the excellent photoelectric characteristics and stability of the inorganic all-inorganic perovskite quantum dot are utilized to achieve the purposes of improving the response rate and the detection rate.
2. In the invention, the solvent with environment protection, low polarity and short chain ligand is used to replace the solvent with traditional high polarity and long chain ligand, and the solution method is used to prepare the all-inorganic perovskite quantum dot, thereby reducing the damage to the environment.
3. In the invention, the proportion of a precursor solvent is strictly controlled for the all-inorganic perovskite quantum dot film, so that crystals with stable crystal lattices are formed.
4. In the invention, a simple low-frequency (40Hz) and room-temperature (20-30 ℃) ultrasonic treatment method is used, and the all-inorganic perovskite quantum dot solution is placed in an ultrasonic machine for treatment, so that the all-inorganic perovskite quantum dots are kept in a continuous low-frequency vibration state, clusters among the all-inorganic perovskite quantum dots are reduced, the all-inorganic perovskite quantum dots are uniformly dispersed in a solvent, and a large-area, compact and smooth film is conveniently formed.
5. In the invention, the steps of spin coating and annealing are repeated by using a low-temperature annealing mode, so that the thickness of the absorption layer is increased, and the rapid crystallization of the thin film is ensured.
6. In the invention, a precise mechanical scribing method is adopted, so that the size of a single device can be designed according to requirements and the single device can be arranged neatly, and the imaging function is realized.
Drawings
FIG. 1 is a schematic structural diagram of a flexible photodetector array based on all-inorganic perovskite quantum dots according to the present invention;
FIG. 2 is a schematic diagram of a curved flexible photodetector array of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: reference numerals and letters designate similar items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention usually place when in use, and are simply used for simplifying the description of the present invention, but do not indicate or imply that the devices or elements indicated must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical" and the like do not imply that the components are required to be absolutely horizontal or pendant, but rather may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; mechanical connection or electrical connection can be realized; the two original pieces can be directly connected or indirectly connected through an intermediate medium, or the two original pieces can be communicated with each other. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
A method for preparing a flexible photodetector array comprises the following steps:
s1, dissolving lead bromide powder in a mixed solvent of isopropanol, propionic acid and n-butylamine, wherein the volume ratio of the isopropanol, the propionic acid and the n-butylamine is 1:1:1, and preparing a lead bromide precursor solution with the molar concentration of 0.5 mol/L;
s2, dissolving cesium carbonate powder in propionic acid to prepare a cesium carbonate precursor solution with the molar concentration of 1.8 mol/L;
s3, adding the lead bromide precursor solution and the cesium carbonate precursor solution prepared by S1 and S2 into a mixed solvent of isopropanol and n-hexane, wherein the volume ratio of the isopropanol to the n-hexane is 1:2, and preparing a homogeneous all-inorganic perovskite quantum dot precursor solution with the molar concentration of 0.006 mol/L;
s4, carrying out 2 times of centrifugal treatment after stirring the homogeneous phase all-inorganic perovskite quantum dot precursor solution, wherein the centrifugal speeds are 1500rpm and 2000rpm respectively, and the time of each centrifugal treatment is 2 minutes;
s5, re-dissolving the centrifuged all-inorganic perovskite quantum dot precursor solution in toluene, and performing ultrasonic treatment to prepare an all-inorganic perovskite quantum dot solution with the molar concentration of 0.0225 mol/L;
s6, using polyethylene glycol terephthalate as a flexible substrate, using indium tin oxide as a transparent electrode, wherein the thickness of the indium tin oxide is 100-150 nm, the surface resistance is 25-30 omega/sq, depositing titanium dioxide on the surface of the flexible substrate by an atomic layer deposition method to serve as an electron transmission layer, and the thickness of the titanium dioxide is 40-60 nm;
s7, preparing the all-inorganic perovskite quantum dot film by using the all-inorganic perovskite quantum dot solution prepared by the S5 in a room-temperature environment through a one-step spin coating method, wherein the spin coating speed is 1000rpm, and the spin coating time is 60 seconds;
s8, immediately annealing the all-inorganic perovskite quantum dot film on a hot bench, wherein the annealing temperature is 120 ℃, the annealing time is 1 minute, repeating the operations of spin coating and annealing, increasing the thickness of the all-inorganic perovskite quantum dot film, the annealing temperature of the last layer of film is 120 ℃, and the annealing time is 5 minutes, so as to ensure the rapid crystallization of the film;
s9, spin-coating a 2,2 ', 7,7 ' -tetrabromo-9, 9 ' -spirodi-tri (4-iodobenzene) amine (Spiro-OMeTAD) solution on the top of the all-inorganic perovskite quantum dot film at the speed of 2500rpm for 25 seconds, and oxidizing for 12 hours in an oxygen-filled atmosphere;
s10, depositing nickel and gold by using a thermal evaporation method, wherein the thicknesses of the nickel and the gold are respectively 10-20 nm and 80-120 nm;
and S11, preparing an array by a mechanical scribing method, and arranging the independent electrodes in an array to form a flexible photoelectric detector array.
Further, in step S7, before preparing the all-inorganic perovskite quantum dot thin film by using the one-step spin coating method in a room temperature environment, the all-inorganic perovskite quantum dot solution is placed in an ultrasonic machine for processing, the processing frequency is 40Hz, the processing temperature is 20-30 ℃, the all-inorganic perovskite quantum dots are kept in a vibration state at any time, clusters among the all-inorganic perovskite quantum dots are reduced, and the all-inorganic perovskite quantum dots are uniformly dispersed in the solvent.
Further, in step S9, the Spiro-OMeTAD solution is prepared by mixing Spiro-OMeTAD powder, 4-tert-butylpyridine and lithium bis (trifluoromethanesulfonylimide) solution in chlorobenzene to form a solution with a molar concentration of 0.056mol/L, wherein the volume ratio of the 4-tert-butylpyridine, lithium bis (trifluoromethanesulfonimide) solution to chlorobenzene is 28.8:17.5: 1000.
Further, the lithium bistrifluoromethanesulfonylimide solution was dissolved in acetonitrile at a molar concentration of 1.8 mol/L.
Furthermore, a mechanical scribing method is used, a device to be processed is placed in the sample table, and vacuum adsorption is carried out on the back surface of the device, so that the sample cannot move randomly during scribing.
In the implementation process, the preparation method of the high-quality all-inorganic metal halogen all-inorganic perovskite quantum dot comprises the following steps:
dissolving lead bromide powder in a mixed solvent of isopropanol, propionic acid and n-butylamine, and placing the mixed solvent on a hot table at 40 ℃ for fully stirring to form a lead bromide precursor solution with the molar concentration of 0.5 mol/L. Wherein the volume ratio of the isopropanol to the propionic acid to the n-butylamine is 1:1: 1. Meanwhile, cesium carbonate powder was dissolved in propionic acid and sufficiently stirred to form a cesium carbonate precursor solution having a molar concentration of 1.8 mol/L. And then respectively taking out appropriate lead bromide and cesium carbonate precursor solutions from the two precursor solutions, and adding the precursor solutions into a mixed solvent of isopropanol and n-hexane, wherein the volume ratio of the isopropanol to the n-hexane is 1:2, so as to form a homogeneous all-inorganic perovskite quantum dot precursor solution with the molar concentration of 0.006 mol/L. And then, stirring the homogeneous phase all-inorganic perovskite quantum dot precursor, and then centrifuging for 2 times, wherein the centrifuging speed is 1500rpm and 2000rpm respectively, and the centrifuging time is 2 minutes. Finally, the centrifuged all-inorganic perovskite quantum dots are re-dissolved in toluene and subjected to ultrasonic treatment, so that a solution of all-inorganic perovskite quantum dots with the molar concentration of 0.0225mol/L is formed, photoluminescence at about 525nm is realized, and the half-peak width is less than 26 nm.
Regarding the preparation of the high-performance flexible photodetector array:
for flexible photodetector arrays, we use polyethylene terephthalate (PET) as the flexible substrate and indium tin oxide as the transparent electrode. Wherein the thickness of the indium tin oxide is 100-150 nm, the surface resistance is 25-30 omega/sq, and the function of collecting electrons is achieved. And depositing titanium dioxide (an electron transport layer) on the surface of the substrate by an atomic layer deposition method, wherein the thickness of the titanium dioxide is 40-60 nm. The thickness of the transmission layer can be accurately controlled by using the method, and the surface of the material is smooth and flat. Thereafter, the all-inorganic perovskite quantum dot solution prepared in S5 was used to prepare an all-inorganic perovskite quantum dot thin film using a one-step spin coating method at a spin coating speed of 1000rpm for 60 seconds in a room temperature environment, and the thin film was immediately annealed on a hot stage at an annealing temperature of 120 degrees celsius for 1 minute. And repeating the steps of spin coating and annealing to increase the thickness of the absorption layer, wherein the annealing temperature of the last layer of film is 120 ℃, and the annealing time is 5 minutes. Thereafter, a 2,2 ', 7,7 ' -tetrabromo-9, 9 ' -spirodi, tris (4-iodobenzene) amine (Spiro-OMeTAD) solution was spin-coated over the all-inorganic perovskite quantum dot thin film at a spin-coating speed of 2000rpm for 30 seconds, and was oxidized in an oxygen-filled atmosphere for 12 hours. Wherein, the Spiro-OMeTAD solution is formed by mixing Spiro-OMeTAD powder, 4-tert-butylpyridine and lithium bistrifluoromethanesulfonylimide solution (Li-TFSI dissolved in acetonitrile and with the molar concentration of 1.8mol/L) in chlorobenzene, and the molar concentration of the solution is 0.056 mol/L. Wherein the volume ratio of the 4-tert-butylpyridine to the Li-TFSI to the chlorobenzene is 28.8:17.5: 1000. And finally, depositing nickel and gold by using a thermal evaporation method, wherein the thicknesses of the nickel and the gold are respectively 10-20 nm and 80-120 nm, preparing an array as required by using a mechanical scribing method, and arranging the independent electrodes in an array to form the flexible photoelectric detector array.
Example 1
A method for preparing a flexible photodetector array comprises the following steps:
s1, dissolving lead bromide powder in a mixed solvent of isopropanol, propionic acid and n-butylamine, wherein the volume ratio of the isopropanol, the propionic acid and the n-butylamine is 1:1:1, and preparing a lead bromide precursor solution with the molar concentration of 0.5 mol/L;
s2, dissolving cesium carbonate powder in propionic acid to prepare a cesium carbonate precursor solution with the molar concentration of 1.8 mol/L;
s3, adding the lead bromide precursor solution and the cesium carbonate precursor solution prepared by S1 and S2 into a mixed solvent of isopropanol and n-hexane, wherein the volume ratio of the isopropanol to the n-hexane is 1:2, and preparing a homogeneous all-inorganic perovskite quantum dot precursor solution with the molar concentration of 0.006 mol/L;
s4, carrying out 2 times of centrifugal treatment after stirring the homogeneous phase all-inorganic perovskite quantum dot precursor solution, wherein the centrifugal speeds are 1500rpm and 2000rpm respectively, and the time of each centrifugal treatment is 2 minutes;
s5, re-dissolving the centrifuged all-inorganic perovskite quantum dot precursor solution in toluene, and performing ultrasonic treatment to prepare an all-inorganic perovskite quantum dot solution with the molar concentration of 0.0225 mol/L;
s6, using polyethylene glycol terephthalate as a flexible substrate, using indium tin oxide as a transparent electrode, wherein the thickness of the indium tin oxide is 100-150 nm, the surface resistance is 25-30 omega/sq, depositing titanium dioxide on the surface of the flexible substrate by an atomic layer deposition method to serve as an electron transmission layer, and the thickness of the titanium dioxide is 40-60 nm;
s7, preparing the all-inorganic perovskite quantum dot film by using the all-inorganic perovskite quantum dot solution prepared by the S5 in a room-temperature environment through a one-step spin coating method, wherein the spin coating speed is 1000rpm, and the spin coating time is 60 seconds;
s8, immediately annealing the all-inorganic perovskite quantum dot film on a hot bench, wherein the annealing temperature is 120 ℃, the annealing time is 1 minute, repeating the operations of spin coating and annealing, increasing the thickness of the all-inorganic perovskite quantum dot film, the annealing temperature of the last layer of film is 120 ℃, and the annealing time is 5 minutes, so as to ensure the rapid crystallization of the film;
s9, spin-coating a 2,2 ', 7,7 ' -tetrabromo-9, 9 ' -spirodi-tri (4-iodobenzene) amine (Spiro-OMeTAD) solution on the top of the all-inorganic perovskite quantum dot film at the speed of 2500rpm for 25 seconds, and oxidizing for 12 hours in an oxygen-filled atmosphere;
s10, depositing nickel and gold by using a thermal evaporation method, wherein the thicknesses of the nickel and the gold are respectively 10-20 nm and 80-120 nm;
and S11, preparing an array by a mechanical scribing method, and arranging the independent electrodes in an array to form a flexible photoelectric detector array.
Example 2
In addition to example 1, before the all-inorganic perovskite quantum dot thin film is prepared by the one-step spin coating method in the room temperature environment in step S7, the all-inorganic perovskite quantum dot solution is placed in an ultrasonic machine and processed, the processing frequency is 40Hz, the processing temperature is 20 to 30 ℃, the all-inorganic perovskite quantum dots are kept in a vibration state at any time, the clusters among the all-inorganic perovskite quantum dots are reduced, and the all-inorganic perovskite quantum dots are uniformly dispersed in the solvent.
Example 3
In step S9, the Spiro-OMeTAD solution is prepared by mixing Spiro-OMeTAD powder, 4-tert-butylpyridine and lithium bis (trifluoromethanesulfonylimide) solution in chlorobenzene to form a solution with a molar concentration of 0.056mol/L, wherein the volume ratio of the 4-tert-butylpyridine, lithium bis (trifluoromethanesulfonimide) solution to chlorobenzene is 28.8:17.5: 1000.
Example 4
On the basis of the above example, the lithium bistrifluoromethanesulfonylimide solution was dissolved in acetonitrile at a molar concentration of 1.8 mol/L.
Example 5
Based on example 1, in step S11, the device to be processed is placed in the sample stage by using a mechanical scribing method, and the back side is vacuum-absorbed, so as to ensure that the sample does not move freely during scribing.
The above description is an embodiment of the present invention. The foregoing is a preferred embodiment of the present invention, and the preferred embodiments in the preferred embodiments can be combined and used in any combination if not obviously contradictory or prerequisite to a certain preferred embodiment, and the specific parameters in the embodiments and examples are only for the purpose of clearly illustrating the invention verification process of the inventor and are not intended to limit the patent protection scope of the present invention, which is subject to the claims and the equivalent structural changes made by the content of the description and the drawings of the present invention are also included in the protection scope of the present invention.

Claims (5)

1. A method for preparing a flexible photoelectric detector array is characterized by comprising the following steps:
s1, dissolving lead bromide powder in a mixed solvent of isopropanol, propionic acid and n-butylamine, wherein the volume ratio of the isopropanol, the propionic acid and the n-butylamine is 1:1:1, and preparing a lead bromide precursor solution with the molar concentration of 0.5 mol/L;
s2, dissolving cesium carbonate powder in propionic acid to prepare a cesium carbonate precursor solution with the molar concentration of 1.8 mol/L;
s3, adding the lead bromide precursor solution and the cesium carbonate precursor solution prepared by S1 and S2 into a mixed solvent of isopropanol and n-hexane, wherein the volume ratio of the isopropanol to the n-hexane is 1:2, and preparing a homogeneous all-inorganic perovskite quantum dot precursor solution with the molar concentration of 0.006 mol/L;
s4, carrying out 2 times of centrifugal treatment after stirring the homogeneous phase all-inorganic perovskite quantum dot precursor solution, wherein the centrifugal speeds are 1500rpm and 2000rpm respectively, and the time of each centrifugal treatment is 2 minutes;
s5, re-dissolving the centrifuged all-inorganic perovskite quantum dot precursor solution in toluene, and performing ultrasonic treatment to prepare an all-inorganic perovskite quantum dot solution with the molar concentration of 0.0225 mol/L;
s6, using polyethylene glycol terephthalate as a flexible substrate, using indium tin oxide as a transparent electrode, wherein the thickness of the indium tin oxide is 100-150 nm, the surface resistance is 25-30 omega/sq, depositing titanium dioxide on the surface of the flexible substrate by an atomic layer deposition method to serve as an electron transmission layer, and the thickness of the titanium dioxide is 40-60 nm;
s7, preparing the all-inorganic perovskite quantum dot film by using the all-inorganic perovskite quantum dot solution prepared by the S5 in a room-temperature environment through a one-step spin coating method, wherein the spin coating speed is 1000rpm, and the spin coating time is 60 seconds;
s8, immediately annealing the all-inorganic perovskite quantum dot film on a hot bench, wherein the annealing temperature is 120 ℃, the annealing time is 1 minute, repeating the operations of spin coating and annealing, increasing the thickness of the all-inorganic perovskite quantum dot film, the annealing temperature of the last layer of film is 120 ℃, and the annealing time is 5 minutes, so as to ensure the rapid crystallization of the film;
s9, spin-coating a 2,2 ', 7,7 ' -tetrabromo-9, 9 ' -spirodi-tri (4-iodobenzene) amine (Spiro-OMeTAD) solution on the top of the all-inorganic perovskite quantum dot film at the speed of 2500rpm for 25 seconds, and oxidizing for 12 hours in an oxygen-filled atmosphere;
s10, depositing nickel and gold by using a thermal evaporation method, wherein the thicknesses of the nickel and the gold are respectively 10-20 nm and 80-120 nm;
and S11, preparing an array by a mechanical scribing method, and arranging the independent electrodes in an array to form a flexible photoelectric detector array.
2. The method of claim 1, wherein in step S7, before the all-inorganic perovskite quantum dot thin film is prepared by the one-step spin coating method in a room temperature environment, the solution of the all-inorganic perovskite quantum dots is placed in an ultrasonic machine for processing, wherein the processing frequency is 40Hz, the processing temperature is 20-30 ℃, the all-inorganic perovskite quantum dots are kept in a vibration state at all times, clusters among the all-inorganic perovskite quantum dots are reduced, and the all-inorganic perovskite quantum dots are uniformly dispersed in the solvent.
3. The method of claim 1, wherein in step S9, the Spiro-OMeTAD solution is prepared by mixing Spiro-OMeTAD powder, 4-tert-butylpyridine and lithium bis (trifluoromethanesulfonylimide) solution in chlorobenzene to form a solution with a molar concentration of 0.056mol/L, wherein the volume ratio of the lithium bis (trifluoromethanesulfonimide) solution to the 4-tert-butylpyridine is 28.8:17.5: 1000.
4. The method of claim 3, wherein the lithium bis (trifluoromethanesulfonylimide) solution is dissolved in acetonitrile at a molar concentration of 1.8 mol/L.
5. The method of claim 1, wherein in step S11, the device to be processed is placed in the sample stage by mechanical scribing, and vacuum suction is applied to the back side to ensure that the sample does not move freely during scribing.
CN202111586089.0A 2021-12-22 2021-12-22 Preparation method of flexible photoelectric detector array Active CN114284443B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111586089.0A CN114284443B (en) 2021-12-22 2021-12-22 Preparation method of flexible photoelectric detector array

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111586089.0A CN114284443B (en) 2021-12-22 2021-12-22 Preparation method of flexible photoelectric detector array

Publications (2)

Publication Number Publication Date
CN114284443A true CN114284443A (en) 2022-04-05
CN114284443B CN114284443B (en) 2023-04-07

Family

ID=80874143

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111586089.0A Active CN114284443B (en) 2021-12-22 2021-12-22 Preparation method of flexible photoelectric detector array

Country Status (1)

Country Link
CN (1) CN114284443B (en)

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014056962A (en) * 2012-09-13 2014-03-27 Peccell Technologies Inc Photoelectric conversion element using perovskite compound and method of manufacturing the same
JP2015056430A (en) * 2013-09-10 2015-03-23 大阪瓦斯株式会社 Photoelectric conversion device using perovskite-based material
CN107195789A (en) * 2017-06-01 2017-09-22 吉林大学 A kind of preparation method of inorganic mixed halogen perovskite thin film and its application in terms of solar cell is prepared
CN108155294A (en) * 2017-12-25 2018-06-12 上海集成电路研发中心有限公司 Photodetector and preparation method thereof, photodetector fabric
CN108807724A (en) * 2018-06-14 2018-11-13 香港中文大学(深圳) Preparation method, application and perovskite luminescent device of perovskite luminescent layer and preparation method thereof
CN110534655A (en) * 2018-05-24 2019-12-03 南京工业大学 Perovskite quantum dot film and preparation method and device thereof
US20200325391A1 (en) * 2019-04-12 2020-10-15 Daegu Gyeongbuk Institute Of Science And Technology Ligand exchange of perovskite quantum dots and solar cell devices manufactured using the same
US20210135135A1 (en) * 2019-04-11 2021-05-06 Zhejiang University Inverted thick 2d hybrid perovskite solar cell insensitive to film thickness and method for preparing the same
CN113130756A (en) * 2019-12-30 2021-07-16 Tcl集团股份有限公司 Composite material, preparation method thereof, thin film and photovoltaic device
CN113193123A (en) * 2021-04-09 2021-07-30 电子科技大学 Double-interface-layer-modified efficient perovskite solar cell and preparation method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2014056962A (en) * 2012-09-13 2014-03-27 Peccell Technologies Inc Photoelectric conversion element using perovskite compound and method of manufacturing the same
JP2015056430A (en) * 2013-09-10 2015-03-23 大阪瓦斯株式会社 Photoelectric conversion device using perovskite-based material
CN107195789A (en) * 2017-06-01 2017-09-22 吉林大学 A kind of preparation method of inorganic mixed halogen perovskite thin film and its application in terms of solar cell is prepared
CN108155294A (en) * 2017-12-25 2018-06-12 上海集成电路研发中心有限公司 Photodetector and preparation method thereof, photodetector fabric
CN110534655A (en) * 2018-05-24 2019-12-03 南京工业大学 Perovskite quantum dot film and preparation method and device thereof
CN108807724A (en) * 2018-06-14 2018-11-13 香港中文大学(深圳) Preparation method, application and perovskite luminescent device of perovskite luminescent layer and preparation method thereof
US20210135135A1 (en) * 2019-04-11 2021-05-06 Zhejiang University Inverted thick 2d hybrid perovskite solar cell insensitive to film thickness and method for preparing the same
US20200325391A1 (en) * 2019-04-12 2020-10-15 Daegu Gyeongbuk Institute Of Science And Technology Ligand exchange of perovskite quantum dots and solar cell devices manufactured using the same
CN113130756A (en) * 2019-12-30 2021-07-16 Tcl集团股份有限公司 Composite material, preparation method thereof, thin film and photovoltaic device
CN113193123A (en) * 2021-04-09 2021-07-30 电子科技大学 Double-interface-layer-modified efficient perovskite solar cell and preparation method thereof

Also Published As

Publication number Publication date
CN114284443B (en) 2023-04-07

Similar Documents

Publication Publication Date Title
Li et al. Photodetectors based on inorganic halide perovskites: Materials and devices
CN109817812B (en) Large-particle perovskite single crystal/polymer composite thick film, photoelectric detector and manufacturing method
JP2001156321A (en) Semiconductor device and its manufacturing method
CN108258117B (en) Stable high-performance perovskite photoelectric detector and preparation method thereof
CN106887482A (en) A kind of mechanical lamination solar cell and preparation method thereof
CN111525036B (en) Self-driven perovskite photoelectric detector and preparation method thereof
CN107768478A (en) A kind of organic/perovskite bulk-heterojunction nanowire photodiode detector and preparation method thereof
Zheng et al. Mesostructured perovskite solar cells based on Zn2SnO4 Single Crystal Mesoporous Layer with efficiency of 18.32%
CN111162173A (en) Organic photoelectric detector with doped electron transport layer and preparation method thereof
CN109354057B (en) Tin oxide nanocrystal and preparation method thereof and preparation method of solar cell
CN114284443B (en) Preparation method of flexible photoelectric detector array
CN109065720B (en) Perovskite solar cell with accurately doped crystal boundary and preparation method thereof
CN111834487B (en) All-inorganic perovskite nanowire self-powered-short wave photoelectric detector and preparation method thereof
CN109859950A (en) Biologic solar cell and preparation method thereof with three layers of chlorophyll structure
CN109904319A (en) The flat crystal of large scale perovskite, calcium titanium ore bed preparation method and solar battery
CN106449978A (en) Preparation method of visible blind ultraviolet detector based on CH3NH3PbCl3 film
CN108963011A (en) A kind of semiconductor film membrane module and the preparation method and application thereof
CN109449243A (en) II type hetero-junctions near infrared photodetector and preparation method thereof based on two-dimentional molybdenum disulfide nano film and cadmium-telluride crystal
CN108023018A (en) The preparation method of inversion perovskite solar cell based on the continuously adjustable control of band gap
CN104167453A (en) Perovskite solar battery based on CdSe nanocrystals and preparation method
CN111009613A (en) Perovskite quantum dot doped organic ultraviolet detector and preparation method thereof
CN111799380B (en) Organic-inorganic composite photoconductive detector, and preparation method and application thereof
CN210379115U (en) Perovskite solar cell with array structure electron transport layer
Lu et al. Noise characteristics of ZnO-nanowire photodetectors prepared on ZnO: Ga/glass templates
CN114242831A (en) CdTe/CsPbBr3Preparation method of quantum dot heterojunction light detection film

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant