CN115044362B - Preparation method of colloid quantum dot film and photoelectric detector - Google Patents

Preparation method of colloid quantum dot film and photoelectric detector Download PDF

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CN115044362B
CN115044362B CN202210566692.0A CN202210566692A CN115044362B CN 115044362 B CN115044362 B CN 115044362B CN 202210566692 A CN202210566692 A CN 202210566692A CN 115044362 B CN115044362 B CN 115044362B
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CN115044362A (en
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高亮
杨骏睿
鲁帅成
唐江
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Huazhong University of Science and Technology
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Abstract

The application provides a preparation method of a colloid quantum dot film and a photoelectric detector, comprising the following steps: determining the mixing proportion of iodide ions and bromide ions according to the size of the colloidal quantum dots; preparing mixed powder of iodide ions and bromide ions according to the mixing proportion, and preparing halogen ligand solution according to the mixed powder; mixing a halogen ligand solution and an initial quantum dot solution for liquid ligand exchange to obtain a ligand exchange solution; processing the ligand exchange solution to obtain a target quantum dot solution; and spin-coating the target quantum dot solution on a target object to form a colloid quantum dot film. According to the application, the mixing proportion of iodide ions and bromide ions can be determined according to the size of the colloidal quantum dots, and crystal faces are passivated by the bromide ions with higher concentration, so that dark current is reduced, shot noise is reduced, and the detection performance of the whole detection device is improved.

Description

Preparation method of colloid quantum dot film and photoelectric detector
Technical Field
The application relates to the field of semiconductors, in particular to a preparation method of a colloid quantum dot film and a photoelectric detector.
Background
The quantum dot is a three-dimensional limited nano material, and quantum dots with different band gaps can be realized by adjusting the size of the quantum dot, so that the purposes of changing the first exciton absorption peak of the quantum dot and detecting spectra with different wave bands are realized.
The lead sulfide colloid quantum dot is a novel short wave infrared material, and the surface structure and the size of the lead sulfide colloid quantum dot are related. When the size of the lead sulfide quantum dot is smaller (the band gap is larger than 1.24 eV), the exposed crystal face (111) is taken as the main part of the surface of the lead sulfide quantum dot, and as the size of the lead sulfide quantum dot is gradually increased, the crystal face (100) gradually appears on the surface of the quantum dot, which is different from the structure that the crystal face (111) is all lead atoms, and the crystal face (100) is a structure that lead atoms and sulfur atoms are alternately arranged.
The defect passivation of the surface of the lead sulfide quantum dot is a hot spot in the current research, and the quantum dot film with excessive defects can reduce the service life of minority carriers, so that the prepared detection device has excessive dark current, increases shot noise and reduces the detection performance of the whole detection device. Therefore, passivation of the surface defects of the lead sulfide quantum dots is important for improving the detection performance.
The current method for passivating the lead sulfide colloid quantum dot adopts a mixed halogen ligand passivation scheme of high-concentration iodide ions and low-concentration bromide ions. Along with the increase of the size of the quantum dot, the proportion of the crystal face (100) in the body surface area is gradually increased, but iodine ions with high concentration in the solution are difficult to fully adsorb on the crystal face (100), so that the defect passivation of the crystal face (100) is poor, and a large number of defects exist in the finally prepared film, so that larger dark current is generated, and the detection performance of the device is influenced.
In view of this, overcoming the shortcomings of the prior art products is a problem to be solved in the art.
Disclosure of Invention
The application mainly solves the technical problems of providing a preparation method of a colloidal quantum dot film and a photoelectric detector, which can determine the mixing proportion of iodide ions and bromide ions according to the size of the colloidal quantum dot, passivate the (100) crystal face of the large-size quantum dot by using the bromide ions with higher concentration, reduce the defect state density, improve the service life of carriers, reduce dark current and reduce shot noise.
In order to solve the foregoing problems, the present embodiment provides a method for preparing a colloidal quantum dot film, including:
determining the mixing proportion of iodide ions and bromide ions according to the size of the colloidal quantum dots;
preparing mixed powder of iodide ions and bromide ions according to the mixing proportion, and preparing halogen ligand solution according to the mixed powder;
Mixing a halogen ligand solution and an initial quantum dot solution for liquid ligand exchange to obtain a ligand exchange solution;
processing the ligand exchange solution to obtain a target quantum dot solution;
And spin-coating the target quantum dot solution on a target object to form a colloid quantum dot film.
Further, the concentration of iodide ions was 0.266mmol/ml, and the concentration of bromide ions was 0.116mmol/ml.
Further, the preparing a mixed powder of iodide ions and bromide ions according to the mixing ratio, and the preparing a halogen ligand solution according to the mixed powder includes:
And dissolving mixed powder of iodide ions and bromide ions in a preset solvent to obtain a halogen ligand solution.
Further, the preset solvent is at least one of nitrogen-nitrogen dimethylformamide, methanol, ethanol, butanol and acetone.
Further, the initial quantum dot solution is a lead sulfide quantum dot solution.
Further, the lead sulfide quantum dot solution is prepared by lead sulfide quantum dots, the lead sulfide quantum dots comprise a plurality of PbS particles, and the average particle size of the PbS quantum dots is preferably 4-15 nm.
Further, the band gap of the PbS quantum dot is
Further, the initial quantum dot solution contains two colloidal quantum dots with different absorption peaks.
In order to solve the foregoing problems, the present embodiment provides another photodetector, where the photodetector includes an electron transport layer, a hole transport layer, and a colloidal quantum dot film, where the colloidal quantum dot film is located between the electron transport layer and the hole transport layer, and the colloidal quantum dot film is prepared according to the preparation method of the present application.
Further, the photoelectric detector is of a top incidence structure or of a bottom incidence structure.
The beneficial effects of the application are as follows: the application provides a preparation method of a colloid quantum dot film and a photoelectric detector, comprising the following steps: the bromide ion with higher concentration is adopted for the quantum dots with large size; preparing mixed powder of iodide ions and bromide ions according to the mixing proportion, and preparing halogen ligand solution according to the mixed powder; mixing a halogen ligand solution and an initial quantum dot solution for liquid ligand exchange to obtain a ligand exchange solution; processing the ligand exchange solution to obtain a target quantum dot solution; and spin-coating the target quantum dot solution on a target object to form a colloid quantum dot film. According to the application, the mixing proportion of iodide ions and bromide ions can be determined according to the size of the colloidal quantum dots, and for large-size quantum dots, crystal face (100) is passivated by using bromide ions with higher concentration, so that the defect state density is reduced, the service life of carriers is prolonged, thereby reducing dark current, reducing shot noise and improving the detection performance of the whole detection device.
Drawings
In order to more clearly illustrate the technical solution of the embodiments of the present application, the drawings that are required to be used in the embodiments of the present application will be briefly described below. It is evident that the drawings described below are only some embodiments of the present application and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a schematic flow chart of a method for preparing a colloidal quantum dot film according to an embodiment of the present application;
FIG. 2 is a dark current comparison of a device prepared by the preferred method provided by the example of the present application with a device prepared by the original method;
FIG. 3 is a comparison of defect state distribution of a film prepared by a preferred method provided by the examples of the present application and a film prepared by an original method;
FIG. 4 is a photo-induced fluorescence image comparison of a film prepared by the preferred method provided by the examples of the present application and a film prepared by the original method;
fig. 5 is a noise density spectrum of a device prepared by a preferred method provided by an embodiment of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to fall within the scope of the application.
In the description of the present application, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. indicate orientations or positional relationships based on the drawings are merely for convenience in describing the present application and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and thus should not be construed as limiting the present application. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more features. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present application, the term "exemplary" is used to mean "serving as an example, instance, or illustration. Any embodiment described as "exemplary" in this disclosure is not necessarily to be construed as preferred or advantageous over other embodiments. The following description is presented to enable any person skilled in the art to make and use the application. In the following description, details are set forth for purposes of explanation. It will be apparent to one of ordinary skill in the art that the present application may be practiced without these specific details. In other instances, well-known structures and processes have not been described in detail so as not to obscure the description of the application with unnecessary detail. Thus, the present application is not intended to be limited to the embodiments shown, but is to be accorded the widest scope consistent with the principles and features disclosed herein.
It should be noted that, because the method of the embodiment of the present application is executed in the electronic device, the processing objects of each electronic device exist in the form of data or information, for example, time, which is substantially time information, it can be understood that in the subsequent embodiment, if the size, the number, the position, etc. are all corresponding data, so that the electronic device can process the data, which is not described herein in detail.
Example 1:
For large-size quantum dots, the crystal face (100) occupies a larger proportion in the body surface area, but the crystal face (100) is difficult to be fully passivated by the high-iodine low-bromine mixed ligand commonly used in small-size quantum dots, so that the prepared quantum dot film has high-concentration defects, and the performance of a quantum dot device is degraded. In order to solve the foregoing problems, referring to fig. 1, the present embodiment provides a method for preparing a colloidal quantum dot film, which includes:
s1: determining the mixing proportion of iodide ions and bromide ions according to the size of the colloidal quantum dots;
Numerous studies by the inventors have found that bromide ions are more easily bound to the crystal plane (100) of lead sulfide quantum dots than iodide ions during ligand exchange. Therefore, the increase of the concentration of the bromide ions in the ligand solution is helpful for passivating the crystal face (100) of the lead sulfide quantum dot so as to achieve the purpose of reducing defects. Therefore, the mixing proportion of iodide ions and bromide ions can be determined according to the size of the colloidal quantum dots, crystal faces are passivated by the bromide ions with higher concentration, the defect state density is reduced, the dark current is reduced, the shot noise is reduced, and the detection performance of the whole detection device is improved.
In this example, a suitable solution is selected according to the mixing ratio of iodide ions and bromide ions, and in order to increase the ratio of bromide ions, a higher concentration of lead bromide may be used as the source of bromide ions.
Wherein, the concentration of iodine ions in the original scheme is 0.266mmol/ml, and the concentration of bromine ions is 0.029mmol/ml. In a preferred embodiment, the iodide ion concentration is 0.266mmol/ml and the bromide ion concentration is 0.116mmol/ml.
S2: preparing mixed powder of iodide ions and bromide ions according to the mixing proportion, and preparing halogen ligand solution according to the mixed powder;
In this example, mixed powder of iodide ions and bromide ions was dissolved in a predetermined solvent to obtain a halogen ligand solution. Wherein the preset solvent is at least one of nitrogen-nitrogen dimethylformamide, methanol, ethanol, butanol and acetone. In a preferred embodiment, the predetermined solvent is a solution of N-Dimethylformamide (DMF), wherein N-Dimethylformamide (DMF) is a colorless transparent liquid which is miscible with water and most organic solvents.
In this example, mixed powder of iodide ions and bromide ions was dissolved in 10ml to 15ml of a nitrogen-nitrogen dimethylformamide solution, shaken and mixed uniformly to obtain a halogen ligand solution.
S3: mixing a halogen ligand solution and an initial quantum dot solution for liquid ligand exchange to obtain a ligand exchange solution;
S4: processing the ligand exchange solution to obtain a target quantum dot solution;
The initial quantum dot solution is lead sulfide quantum dot solution, and the volume of the lead sulfide quantum dot solution is 10 ml-15 ml. In other preferred embodiments, the initial quantum dot solution contains two colloidal quantum dots having different absorption peaks. For example, the absorption peak of one colloidal quantum dot is 1300nm, and the absorption peak of the other colloidal quantum dot is 1150nm, and the colloidal quantum dot film manufactured by the method can carry out flattening treatment on the active layer of the photoelectric detector to obtain a wide spectral response detector with lower dark current.
In this example, the ligand exchange solution was washed with n-octane; centrifuging the washed ligand exchange solution to obtain a precipitate; and mixing the precipitate with n-butylamine solution to obtain the target quantum dot solution.
In the practical application scene, the volume of the n-octane is 10 ml-15 ml. And (3) cleaning the ligand exchange solution at least twice by adopting n-octane, centrifuging the ligand exchange solution at a speed of 5000 rpm for 5 minutes after the cleaning is finished, uniformly dissolving the precipitate by using a mixed solution of nitrogen, azodicarbonamide and n-butylamine, and spin-coating the precipitate onto a substrate at a speed of 2500 rpm to finish the preparation of the quantum dot film.
S5: and spin-coating the target quantum dot solution on a target object to form a colloid quantum dot film.
The target is an ITO substrate, or the target can be an electron transport layer or a hole transport layer, and when the target quantum dot solution is spin-coated on the electron transport layer, a colloidal quantum dot film is formed on the electron transport layer to form a bottom incidence structure photodetector. When a target quantum dot solution is spin-coated on the hole transport layer, a colloidal quantum dot film is formed on the hole transport layer to form a photodetector of a top-injection structure.
The application aims to optimize the preparation process of the quantum dot film as much as possible under the condition of not influencing the transmission of the quantum dot film, thereby achieving the purposes of passivating the crystal face (100) and reducing defects. The mixed halogen ligand is combined, and other ligands capable of passivating the crystal face (100) of the lead sulfide colloid quantum dot are adopted, so that the defect concentration is reduced, and the effect of effectively passivating the large-size quantum dot can be achieved. After the technical scheme of the application is used, compared with the original scheme, the dark current is obviously reduced on the basis of not changing the external quantum efficiency.
In a preferred embodiment, the colloidal quantum dot film includes a first colloidal quantum dot and a second colloidal quantum dot, and absorption peaks of the first colloidal quantum dot and the second colloidal quantum dot are different to widen a detection range of the photodetector.
In this embodiment, the lead sulfide quantum dot solution is configured by the lead sulfide quantum dots, the PbS quantum dots are composed of PbS particles, the size range of the PbS particles is large (from several nm to several tens nm), and in the PbS quantum dots, when the average particle diameter of the PbS quantum dots is reduced to a size equal to or smaller than the pore diameter of the internal electrons, the band gap of the PbS quantum dots is changed. When the average particle diameter of PbS quantum dots is 15nm or less, the band gap can be controlled relatively easily by quantum size effect. Therefore, the average particle size of the PbS quantum dots is preferably 4nm to 15nm, wherein the average particle size of the PbS quantum dots means the average particle size of 10 to 20 PbS quantum dots.
In the present embodiment, the band gap of the PbS quantum dot is preferablyAccording to practical application, the upper limit of the band gap of the PbS quantum dot is preferably 1eV or less, and the lower limit of the band gap of the PbS quantum dot is preferably 0.8eV or more.
Example 2:
Based on the foregoing embodiment 1, the present embodiment provides a photodetector, where the photodetector includes an electron transport layer, a hole transport layer, and a colloidal quantum dot film, where the colloidal quantum dot film is located between the electron transport layer and the hole transport layer, and the colloidal quantum dot film is prepared according to the preparation method of the present application. Wherein the photoelectric detector is of a top incidence structure or of a bottom incidence structure.
The preferred method of making a device in fig. 2 compares the photo-dark current with the device made by the original method, wherein the preferred method of making a device dark current density at 0.1V reverse bias reduces the dark current density from 11.3 mua/cm 2 to 340nA/cm 2 compared to the device made by the original method.
Fig. 3 is a graph showing the defect state distribution obtained by temperature change admittance testing of the lead sulfide quantum dot layers prepared by the two methods, wherein the thin film prepared by the preferred method has lower defect state density (2.3×10 14cm-3) and shallower defect energy level (0.113 eV) than the thin film prepared by the original method. It is demonstrated that the reduction in dark current in fig. 2 results from more passivation of defects by bromide ions in the preferred method.
FIG. 4 is a photo-induced fluorescence image comparison of a film prepared by the preferred method provided by the examples of the present application with a film prepared by the original method. Wherein the film prepared by the preferred method has obviously reduced defect peak intensity compared with the original method, which represents that the preferred method effectively passivates defects and reduces defect state density.
Fig. 5 is a graph of the noise density spectrum of a device prepared by the preferred method found. The device prepared by the preferred method has lower noise, so that the normalized ratio detection rate of 5×10 12 can be obtained.
The foregoing description is only of embodiments of the present application, and is not intended to limit the scope of the application, and all equivalent structures or equivalent processes using the descriptions and the drawings of the present application or directly or indirectly applied to other related technical fields are included in the scope of the present application.

Claims (6)

1. The preparation method of the colloid quantum dot film is characterized by comprising the following steps of:
determining the mixing proportion of iodide ions and bromide ions according to the size of the colloidal quantum dots;
preparing mixed powder of iodide ions and bromide ions according to the mixing proportion, and preparing halogen ligand solution according to the mixed powder;
Mixing a halogen ligand solution and an initial quantum dot solution for liquid ligand exchange to obtain a ligand exchange solution;
processing the ligand exchange solution to obtain a target quantum dot solution;
Spin-coating a target quantum dot solution on a target object to form a colloid quantum dot film;
wherein the concentration of the iodide ions is 0.266mmol/ml, and the concentration of the bromide ions is 0.116mmol/ml;
The initial quantum dot solution comprises two colloid quantum dots with different absorption peaks;
the initial quantum dot solution is lead sulfide quantum dot solution; preparing a lead sulfide quantum dot solution by using lead sulfide quantum dots, wherein the lead sulfide quantum dots comprise a plurality of PbS particles, and the average particle size of the PbS quantum dots is 4-15 nm;
the processing of the ligand exchange solution specifically includes: washing the ligand exchange solution by n-octane; centrifuging the washed ligand exchange solution to obtain a precipitate; the precipitate was mixed with n-butylamine solution.
2. The method of preparing as claimed in claim 1, wherein preparing a mixed powder of iodide ions and bromide ions in the mixing ratio, preparing a halogen ligand solution from the mixed powder comprises:
And dissolving mixed powder of iodide ions and bromide ions in a preset solvent to obtain a halogen ligand solution.
3. The method of claim 2, wherein the predetermined solvent is at least one of nitrogen-nitrogen dimethylformamide, methanol, ethanol, butanol, and acetone.
4. The method of claim 1, wherein the PbS quantum dots have a bandgap of
5. A photodetector comprising an electron transport layer, a hole transport layer, and a colloidal quantum dot film, wherein the colloidal quantum dot film is disposed between the electron transport layer and the hole transport layer, and wherein the colloidal quantum dot film is prepared according to the preparation method of any one of claims 1-4.
6. The photodetector of claim 5 wherein said photodetector is a top-incidence structure or said photodetector is a bottom-incidence structure.
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Citations (1)

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CN114220920A (en) * 2021-12-09 2022-03-22 华中科技大学 Quantum dot infrared detector and preparation method thereof

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WO2019218060A1 (en) * 2018-05-14 2019-11-21 The Governing Council Of The University Of Toronto Passivation of nanocrystals tailored to different facets, and its application to optoelectronic devices

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CN114220920A (en) * 2021-12-09 2022-03-22 华中科技大学 Quantum dot infrared detector and preparation method thereof

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Title
Cation-Exchange Synthesis of Highly Monodisperse PbS Quantum Dots from ZnS Nanorods for Efficient Infrared Solar Cells;Yong Xia等;Adv. Funct. Mater.;第30卷(第4期);1907379（3, 5, 10 of 11） *
Yong Xia等.Cation-Exchange Synthesis of Highly Monodisperse PbS Quantum Dots from ZnS Nanorods for Efficient Infrared Solar Cells.Adv. Funct. Mater..2019,第30卷(第4期),1907379（3,5,10 of 11）. *

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