CN114628588A - PbS quantum dot sensitized organic photoelectric detector and preparation method thereof - Google Patents

PbS quantum dot sensitized organic photoelectric detector and preparation method thereof Download PDF

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CN114628588A
CN114628588A CN202210249108.9A CN202210249108A CN114628588A CN 114628588 A CN114628588 A CN 114628588A CN 202210249108 A CN202210249108 A CN 202210249108A CN 114628588 A CN114628588 A CN 114628588A
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王鹏展
顾德恩
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University of Electronic Science and Technology of China
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Abstract

The invention provides a PbS quantum dot sensitized organic photoelectric detector and a preparation method thereof.A device active layer mainly comprises lead sulfide PbS quantum dots and poly 3-hexylthiophene P3HT, wherein the PbS quantum dots and a P3HT organic active layer in the device active layer are combined in a plane heterojunction mode, and a PbS quantum dot ligand is 1, 2-ethanedithiol; the detection range of the organic photoelectric detector prepared by the method is 300-1500 nm, the maximum external quantum efficiency of a device in a visible light wave band is 69.4%, and the maximum specific detection rate is 1.74 multiplied by 1012Jones has a responsivity of 0.218A/W at most, a quantum efficiency of 3.97% at most outside the near infrared band, and a specific detectivity of 3.70 × 10 at most11Jones, responsivity was up to 0.046A/W.

Description

PbS quantum dot sensitized organic photoelectric detector and preparation method thereof
Technical Field
The invention belongs to the technical field of active layers of organic photoelectric detectors, and particularly relates to preparation based on an active layer structure of an organic photoelectric detector.
Background
At present, most of commercial Photodetectors are inorganic Photodetectors, but in recent years, with the rapid development of Organic semiconductor materials, Organic Photodetectors (OPDs) gradually appear in the ears of people, and compared with the high cost and complex preparation method of inorganic Photodetectors, OPDs have the advantages of small quality, strong flexibility, easy preparation, strong compatibility with flexible substrates, and the like. Based on the characteristics, OPDs can be attached to curved surfaces to be made into various curved surface screens, and can also be prepared into wearable detectors which are in contact with human skin, so as to detect physiological signals of people without influencing daily life. In addition, OPDs have great application potential in the fields of medical treatment, industry, military, smart phones, automobiles and the like. Therefore, the rapid development of OPDs has made it promising for next-generation commercial photodetectors. Although some OPDs have now outperformed inorganic photodetectors, there has been increased interest in organic and inorganic hybrid photodetectors due to the greater processability of organic semiconductors and the higher carrier mobility of inorganic semiconductor materials.
The nano material is used as a new material, and can regulate and control the photoelectric property according to the size of the material, so that the nano material is continuously applied to a photoelectric detector in recent years. Quantum Dots (QDs) have received attention from countless scholars as classical zero-dimensional inorganic materials. Zero-dimensional materials, as their name implies, refer to nanomaterials with extremely small three dimensions, with radii smaller than the bohr exciton radius, and in general, the radii of quantum dots vary from a few nanometers to tens of nanometers. And the Colloidal Quantum Dots (CQDs) which can be used for liquid phase treatment are widely applied to the photoelectric detector due to the obvious quantum confinement effect. And the most widely applied PbS quantum dots are used in many quantum dots.
The detection waveband of OPDs is mainly concentrated on the visible light waveband due to the limitation of materials, the near-infrared quantum dots can detect the near-infrared waveband due to the narrow band gap, the research on a pure quantum dot photoelectric detector is mature at home and abroad, and the development of the detection waveband by combining the infrared quantum dots and the OPDs still needs to be researched urgently. At present, the research at home and abroad mainly focuses on the combination of widely applied PbS quantum dots and OPDs active layers for spectrum broadening, and other quantum dots are used as charge traps of OPDs to enable the OPDs to have multiplication effects. The infrared band ratio detectivity is lower due to the fact that the quantum dots are used for broadening the infrared spectrum of OPDs, and therefore PbS quantum dots need to be effectively combined with an organic photoelectric detector, so that the device has good detectivity in the near infrared range.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the technical problems to be solved by the present invention are: the PbS quantum dot and the P3HT organic active layer are combined in a planar heterojunction mode, and the PbS quantum dot ligand is replaced by 1, 2-ethanedithiol from oleic acid to prepare the organic photoelectric detector with the performance exceeding that of a bulk heterojunction structure device.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an active layer of a PbS quantum dot sensitized organic photoelectric detector mainly comprises lead sulfide PbS quantum dots and poly 3-hexylthiophene P3HT, wherein the PbS quantum dots and a P3HT organic active layer in the active layer of the device are combined in a planar heterojunction mode, and a PbS quantum dot ligand is 1, 2-ethanedithiol.
Preferably, the device comprises a substrate 1, a bottom electrode 2, an electron transport layer 3, an active layer 4, a hole transport layer 5 and a top electrode 6 in sequence from bottom to top.
Preferably, the particle size of the PbS quantum dots is 4.5 nm.
Preferably, the bottom electrode 2 is an ITO transparent electrode having a thickness of 135 nm.
Preferably, the electron transport layer 3 is a ZnO thin film.
Preferably, the hole transport layer 5 is MoO3The thickness of the film and/or the MoO3 film in the hole transport layer is 10 nm.
Preferably, the top electrode 6 is an Ag thin film; and/or the thickness of the top electrode 6Ag film is 100 nm.
The invention also provides a preparation method of the PbS quantum dot sensitized organic photoelectric detector, which comprises the following steps:
(1) preparing a bottom electrode on a substrate;
(2) the electron transport layer 3 was prepared by spin coating,
(3) preparing a PbS quantum dot film layer with a 1, 2-ethanedithiol ligand in the active layer 4 through multiple spin coating, wherein the annealing temperature is 100-120 ℃, and the annealing time is 3-10 min; preparing a P3HT film layer in the active layer by single spin coating, wherein the annealing temperature is 100-120 ℃, and the annealing time is 10-15 min;
(4) preparing the hole transport layer 5 by thermal evaporation;
(5) the top electrode 6 was prepared by thermal evaporation.
Preferably, the spin coating time for preparing the PbS quantum dot film layer in the step (3) is 4 times.
Preferably, the annealing temperature of the PbS quantum dot film layer in the step (3) is 110 ℃, and the annealing time is 5 min;
and/or the annealing temperature of the P3HT film layer in the step (3) is 110 ℃, and the annealing time is 10 min;
and/or the annealing temperature of the ZnO film of the electron transport layer in the step (2) is 200 ℃, and the annealing time is 30 min.
The invention has the beneficial effects that:
the detection range of the organic photoelectric detector prepared by the method is 300-1500 nm, the maximum external quantum efficiency of a device in a visible light wave band is 69.4%, and the maximum specific detection rate is 1.74 multiplied by 1012Jones has a responsivity of 0.218A/W at most, a quantum efficiency of 3.97% at most outside the near infrared band, and a specific detectivity of 3.70 × 10 at most11Jones, responsivity was up to 0.046A/W.
Drawings
FIG. 1 is a schematic diagram of an organic photodetector according to the present invention;
FIG. 2 is an EQE spectrum of external quantum efficiency of the PbS quantum dot sensitized organic photodetector prepared in example 2;
fig. 3 is a specific detectivity D spectrum of the PbS quantum dot sensitized organic photodetector prepared in example 2;
FIG. 4 is a responsivity R spectrum of the PbS quantum dot sensitized organic photodetector prepared in example 2;
FIG. 5 is a J-V characteristic curve of the PbS quantum dot sensitized organic photodetector prepared in example 2.
Description of the reference numerals: 1-substrate, 2-bottom electrode, 3-electron transport layer, 4-active layer, 5-hole transport layer, 6-top electrode.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
The embodiment provides a PbS quantum dot sensitized organic photoelectric detector, wherein an active layer of a device mainly comprises lead sulfide PbS quantum dots and poly-3-hexylthiophene P3HT, the PbS quantum dots and a P3HT organic active layer in the active layer of the device are combined in a plane heterojunction mode, and a ligand of the PbS quantum dots is 1, 2-ethanedithiol.
The PbS quantum dot sensitized organic photoelectric detector sequentially comprises a substrate 1, a bottom electrode 2, an electron transport layer 3, an active layer 4, a hole transport layer 5 and a top electrode 6 from bottom to top.
Preferably, the particle size of the PbS quantum dots is 4.5 nm.
Preferably, the bottom electrode 2 is an ITO transparent electrode with a thickness of 135 nm.
Preferably, the electron transport layer 3 is a ZnO thin film.
Preferably, the hole transport layer 5 is MoO3The thickness of the film and/or the MoO3 film in the hole transport layer is 10 nm.
Preferably, the top electrode 6 is an Ag thin film; and/or the thickness of the top electrode 6Ag film is 100 nm.
The embodiment also provides a preparation method of the PbS quantum dot sensitized organic photoelectric detector, which comprises the following steps:
(1) preparing a bottom electrode on a substrate;
(2) the electron transport layer 3 was prepared by spin coating,
(3) preparing a PbS quantum dot film layer with a 1, 2-ethanedithiol ligand in the active layer 4 through multiple spin coating, wherein the annealing temperature is 100-120 ℃, and the annealing time is 3-10 min; preparing a P3HT film layer in the active layer by single spin coating, wherein the annealing temperature is 100-120 ℃, and the annealing time is 10-15 min;
(4) preparing a hole transport layer 5 by thermal evaporation;
(5) the top electrode 6 was prepared by thermal evaporation.
Preferably, the spin coating times for preparing the PbS quantum dot film layer in the step (3) are 4 times.
Preferably, the annealing temperature of the PbS quantum dot film layer in the step (3) is 110 ℃, and the annealing time is 5 min;
and/or the annealing temperature of the P3HT film layer in the step (3) is 110 ℃, and the annealing time is 10 min;
and/or the annealing temperature of the ZnO film of the electron transport layer in the step (2) is 200 ℃, and the annealing time is 30 min.
Example 2
As shown in FIG. 1, the invention provides a preparation method of a PbS quantum dot-based sensitized organic photoelectric detector, an active layer of a device mainly comprises lead sulfide PbS quantum dots and poly 3-hexylthiophene P3HT, the PbS quantum dots and a P3HT organic active layer in the active layer of the device are combined in a planar heterojunction mode, and a PbS quantum dot ligand is 1, 2-ethanedithiol.
The organic electroluminescent device sequentially comprises a substrate 1, a bottom electrode 2, an electron transport layer 3, an active layer 4, a hole transport layer 5 and a top electrode 6 from bottom to top.
In the specific embodiment, the substrate 1 is soda-lime glass, the bottom electrode 2 is an ITO transparent electrode, the electron transport layer 3 is a ZnO film, the active layer 4 is a P3HT/PbS-EDT plane heterojunction film, and the hole transport layer 5 is MoO3The film, the top electrode 6 is an Ag film.
As a preferable example, the thickness of the ITO transparent electrode in the bottom electrode 2 is 135nm, the annealing temperature of the ZnO film in the electron transport layer 3 is 200 ℃, the annealing time is 30min, the surface ligand of the PbS quantum dot in the active layer 4 is EDT, the particle diameter is 4.5nm, the number of spin-coated layers of the quantum dot film layer is 4, the annealing temperature is 110 ℃, the annealing time is 5min, the annealing temperature of P3HT is 110 ℃, the annealing time is 10min, and MoO in the hole transport layer 53The thickness of the film was 10nm, and the thickness of the Ag film in the top electrode 6 was 100 nm.
The embodiment also provides a preparation method of the PbS quantum dot sensitized organic photoelectric detector, which comprises the following steps:
(1) cleaning, preparing
Preparing an ITO bottom electrode on a glass substrate, rubbing and washing the ITO bottom electrode with detergent, washing the ITO bottom electrode with deionized water, placing the ITO bottom electrode on a substrate frame, placing the ITO bottom electrode in a beaker, carrying out ultrasonic treatment on the deionized water for 30min, acetone for 60min twice and isopropanol for 30min twice in sequence, replacing new acetone or isopropanol in the beaker after the ultrasonic treatment is finished each time, pouring the isopropanol in the beaker into a wastewater tank after the ultrasonic treatment is finished, and then pouring a proper amount of isopropanol again for preservation.
49.39mg of zinc acetate dihydrate and 13.74mg of ethanolamine are weighed on an electronic balance and put into a glass bottle, 500 mu L of 2-methoxyethanol is taken into the glass bottle by a liquid-transferring gun, and the glass bottle is sealed and stirred for 4 hours by a magnetic rotor on a stirring table to prepare the ZnO precursor solution. Weighing 5mgP3HT on an electronic balance in a glove box, filling into a glass bottle, weighing 5mgP3HT and 10mgPbS quantum dots, pouring into the same glass bottle, dripping 500 muL chlorobenzene into each glass bottle by using a liquid transfer gun, weighing 10mgPbS quantum dots, adding 500 muL n-octane into the glass bottle by using the liquid transfer gun, sealing, and heating and stirring on a stirring table at 50 ℃ for 12 h. A solution of 50. mu.L of EDT in acetonitrile and 5mL of acetonitrile was prepared by using a pipette to prepare a 1% EDT/acetonitrile solution, and then 200. mu.L of 1% EDT/acetonitrile solution was added with 10mL of acetonitrile to prepare a 0.02% EDT/acetonitrile solution.
2. Preparation of the Electron transport layer (3) by spin coating
Before preparing the device, the ITO substrate in isopropanol is taken out, dried by nitrogen and irradiated for 20min by an ultraviolet cleaner. After the ITO substrate is cooled to room temperature after ultraviolet irradiation, a spin coater is used for spin-coating ZnO precursor solution on the surface of the ITO substrate for 40s at the rotating speed of 4000rpm, the ITO substrate is placed on a heating table for annealing at 200 ℃ for 30min after the spin-coating is finished, and in the annealing process, the ZnO precursor solution film and oxygen undergo chemical reaction to generate a ZnO film which becomes an electron transport layer of OPDs.
3. Spin coating to prepare active layer
Both surface ligand replacement and spin-coating of the active layer were performed in a glove box and the procedure for preparing the P3HT/PbS-EDT active layer was as follows: spin-coating PbS-OA/n-octane dispersion liquid at the rotation speed of 2500rpm for 30s, then dropwise adding 0.02% EDT/acetonitrile solution on the surface of a device, ensuring that the solution can submerge the surface of the device, standing for 30s to ensure that oleic acid is fully replaced by EDT, then spin-coating at the rotation speed of 2500rpm for 30s, dropwise adding acetonitrile on the surface of the device for washing off redundant oleic acid molecules, then spin-coating at the rotation speed of 2500rpm for 30s, repeating the whole cleaning process for 2 times, and repeating the ligand replacement process for 4 times in total to ensure that the thickness of the PbS-EDT film is proper. Annealing at 110 deg.C for 5min on a heating table, spin-coating 40sP3 HT/chlorobenzene solution at 2500rpm, and annealing at 110 deg.C for 10min on a heating table.
4. Preparation of hole transport layer and Top electrode
The preparation of the hole transport layer MoO3 and the Ag electrode are carried out in a vacuum chamber of a vacuum coater, the device is placed in a designed mask plate, and the vacuum chamber is pumped to 7 x 10-4Pa or less, conducting MoO3Before coating, closing a baffle between an evaporation boat and a mask plate, regulating evaporation current to be 20A, preheating for 2 minutes, then regulating the evaporation current to be 40A, preheating for 2 minutes, opening the baffle, regulating the evaporation current, and controlling the film forming speed of MoO3 to be within the range
Figure BDA0003546066020000051
Finally forming MoO with the thickness of 10nm3A hole transport layer. Then the vacuum is pumped again until the vacuum degree of the vacuum chamber is 3 multiplied by 10-3Performing thermal evaporation coating of Ag electrode under Pa, and performing MOO3The evaporation method is similar, the evaporation of the Ag electrode needs to close the baffle plate, preheat for 2 minutes under the evaporation current of 40A and 60A, open the baffle plate, adjust the evaporation current, and control the film forming speed of Ag to be within
Figure BDA0003546066020000052
When the thickness of the Ag electrode film is 10nm, the evaporation current is adjusted, and the film forming speed of Ag is controlled to be
Figure BDA0003546066020000053
Finally forming an Ag electrode with the thickness of 100 nm.
By testing EQE (shown in figure 2), D (shown in figure 3), R (shown in figure 4) and J-V (shown in figure 5) curves of the device, the detection range of the prepared organic photoelectric detector is 300-1500 nm, the external quantum efficiency of the device in a visible light waveband is 69.4% at most, and the specific detection rate is 1.74 multiplied by 10 at most12Jones has a maximum responsivity of 0.218A/W, a maximum quantum efficiency of 3.97% outside the near infrared band, and a maximum specific detectivity of 3.70 × 1011Jones, responsivity was up to 0.046A/W.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (10)

1. A PbS quantum dot sensitized organic photoelectric detector is characterized in that: an active layer of the device mainly comprises lead sulfide PbS quantum dots and poly-3-hexylthiophene P3HT, the PbS quantum dots and a P3HT organic active layer in the active layer of the device are combined in a planar heterojunction mode, and a PbS quantum dot ligand is 1, 2-ethanedithiol.
2. A PbS quantum dot sensitized organic photodetector according to claim 1, characterized in that: the organic electroluminescent device sequentially comprises a substrate (1), a bottom electrode (2), an electron transport layer (3), an active layer (4), a hole transport layer (5) and a top electrode (6) from bottom to top.
3. The PbS quantum dot sensitized organic photodetector of claim 1, wherein: the grain diameter of the PbS quantum dot is 4.5 nm.
4. The PbS quantum dot sensitized organic photodetector of claim 1, wherein: the bottom electrode (2) is an ITO transparent electrode, and the thickness is 135 nm.
5. The PbS quantum dot sensitized organic photodetector of claim 1, wherein: the electron transmission layer (3) is a ZnO film.
6. The PbS quantum dot sensitized organic photodetector of claim 1, wherein: the hole transport layer (5) is MoO3Thin film and/or MoO in the hole transport layer3The thickness of the film was 10 nm.
7. The PbS quantum dot sensitized organic photodetector of claim 1, wherein: the top electrode (6) is an Ag film; and/or the top electrode (6) Ag film has a thickness of 100 nm.
8. The method for preparing the PbS quantum dot sensitized organic photodetector as claimed in any one of claims 1 to 7, characterized by comprising the steps of:
(1) preparing a bottom electrode on a substrate;
(2) an electron transport layer (3) was prepared by spin coating,
(3) preparing a PbS quantum dot film layer with a 1, 2-ethanedithiol ligand in the active layer (4) through multiple spin coating, wherein the annealing temperature is 100-120 ℃, and the annealing time is 3-10 min; preparing a P3HT film layer in the active layer by single spin coating, wherein the annealing temperature is 100-120 ℃, and the annealing time is 10-15 min;
(4) preparing a hole transport layer (5) by thermal evaporation;
(5) the top electrode (6) was prepared by thermal evaporation.
9. The method for preparing a PbS quantum dot sensitized organic photodetector as claimed in claim 8, wherein: the spin coating times for preparing the PbS quantum dot film layer in the step (3) are 4 times.
10. The method for preparing a PbS quantum dot sensitized organic photodetector as claimed in claim 8, wherein: in the step (3), the annealing temperature of the PbS quantum dot film layer is 110 ℃, and the annealing time is 5 min;
and/or the annealing temperature of the P3HT film layer in the step (3) is 110 ℃, and the annealing time is 10 min;
and/or the annealing temperature of the ZnO film of the electron transport layer in the step (2) is 200 ℃, and the annealing time is 30 min.
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Application publication date: 20220614

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