CN113270553A - Organic photoelectric detector preparation method and prepared organic photoelectric detector - Google Patents

Organic photoelectric detector preparation method and prepared organic photoelectric detector Download PDF

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CN113270553A
CN113270553A CN202110575986.5A CN202110575986A CN113270553A CN 113270553 A CN113270553 A CN 113270553A CN 202110575986 A CN202110575986 A CN 202110575986A CN 113270553 A CN113270553 A CN 113270553A
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active layer
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electrode
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王洋
刘青霞
蒋亚东
太惠玲
袁柳
肖建花
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University of Electronic Science and Technology of China
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Abstract

The invention discloses a preparation method of an organic photoelectric detector and the prepared organic photoelectric detector, wherein the preparation method comprises the steps of preparing a transparent conductive electrode, preparing a first electrode modification layer, preparing an active layer by adopting an active layer solution containing an organic material with temperature-dependent aggregation behavior, preparing a distributed synergistic heat treatment method of heating, spin coating and thermal annealing treatment in the preparation process of the active layer, preparing a second electrode modification layer, evaporating a metal electrode and packaging to obtain the photoelectric detector, and the organic photoelectric detector comprises a substrate, the transparent conductive electrode, the first electrode modification layer, the active layer, the second electrode modification layer and the metal electrode which are arranged from bottom to top; the invention can regulate and control the phase separation scale of the active layer and optimize the internal configuration of the active layer, keep the low dark current density of the thick-film device, and improve the optical response rate and external quantum efficiency EQE of the device, thereby improving the specific detection rate D of the device.

Description

Organic photoelectric detector preparation method and prepared organic photoelectric detector
Technical Field
The invention belongs to the technical field of organic semiconductors, and particularly relates to a preparation method of an organic photoelectric detector and the prepared organic photoelectric detector.
Background
The photoelectric detector is a device capable of converting optical signals into electric signals, and is widely applied to various fields such as military affairs, aerospace, biomedical treatment, optical communication, image sensing and the like. The traditional inorganic photoelectric detector has poor mechanical flexibility, complex preparation process and high price, and limits the development of the photoelectric detector in the directions of large area, flexibility, high sensitivity and low cost, and the organic photoelectric detector greatly makes up the defects of the inorganic photoelectric material due to the characteristics of rich organic photoelectric material types, excellent mechanical flexibility, solution processability, adjustable spectrum absorption characteristic and the like, so that the inorganic photoelectric detector has great research space and market value.
Dark current density (Jd) is one of the important performance parameters of the photodetector, and a high dark current density can reduce the sensitivity of the device to low-intensity optical signals and increase the minimum detectable light intensity of the device, thereby reducing the performance of the device, such as on-off ratio, Linear Dynamic Range (LDR), specific detectivity (D), and the like. Chinese patent publication No. CN111952454A discloses an organic photodetector based on a hybrid electron transport layer and a method for manufacturing the same, which describes a method for suppressing dark current by modifying and optimizing a carrier blocking layer, and chinese patent publication No. CN111933798A discloses an organic photodetector and a method for manufacturing the same, which describes a method for suppressing dark current by modifying and optimizing doping of an active layer, but both of the above-mentioned methods greatly increase the complexity of the manufacturing process of the device.
For organic photodetectors, increasing the thickness of the active layer is an effective way to suppress dark current. The principle is as follows: the increase of the thickness of the active layer can reduce the structural defects of the active layer and reduce the leakage current; in addition, the image charge effect (image charge effect) can be reduced after the thickness of the active layer is increased, the effective potential barrier of external circuit charge injection is increased, and the dark current density of the device is reduced. However, when the thickness of the active layer is too large, generally about 500nm, the optical response of the device is sharply reduced, and photo-generated carriers cannot be effectively extracted, so that the optical response rate and EQE of the device are reduced, and the specific detection rate D of the device is further reduced. Therefore, how to balance the dark current and the optical response is a compromise, and the optical response of the device is improved under the condition of keeping the low dark current density of the device, so as to achieve the effect of improving the overall performance of the device.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of an organic photoelectric detector and the prepared organic photoelectric detector.
The technical scheme adopted by the invention is as follows:
a method for preparing an organic photoelectric detector comprises
Cleaning and drying the substrate, and preparing a transparent conductive electrode on the surface of the substrate to obtain a substrate;
preparing a first electrode modification layer on the surface of the transparent conductive electrode by adopting a solution processing process;
preparing an active layer on the surface of the first electrode modification layer by adopting a distributed synergistic heat treatment method of firstly heating, spin coating and then thermal annealing, wherein the preparation material of the active layer comprises an organic material with temperature-dependent aggregation behavior;
preparing a second electrode modification layer on the surface of the active layer;
and evaporating a metal electrode on the second electrode modification layer and packaging to obtain the photoelectric detector.
Further, the heating spin coating process specifically comprises: the method comprises the steps of placing an active layer solution comprising an organic donor and an organic acceptor on a heating and stirring table for constant-temperature heating and stirring, then placing a substrate with a first electrode modification layer on a spin coater, and spin-coating the substrate by using the active layer solution, wherein the temperature difference between the substrate and the active layer solution in the spin coating process is not more than 10 ℃.
Further, the thickness of the active layer is 300nm to 1200 nm.
Furthermore, the mass ratio of the organic donor to the organic acceptor in the active layer solution is 0.5-2, and the content of the solvent additive is 0.1-3%.
Further, the organic donor material adopted in the active layer solution is PBDB-T, PM6 and/or PBDTS-TDZ, the organic acceptor material adopted is PC61BM, PC71BM, ITIC-Th, O-IDTBR, Y6 and/or IT-4F, the main solvent adopted is chlorobenzene, O-dichlorobenzene and/or chloroform, and the solvent additive is 1, 8-Diiodooctane (DIO), Chloronaphthalene (CN) and/or nitrobenzene.
Further, the annealing temperature of the thermal annealing treatment is 70-200 ℃, and the thermal annealing time is 10-60 min.
Further, the annealing temperature is 110 ℃.
An organic photoelectric detector prepared by the preparation method of the organic photoelectric detector adopts an inverse structure or a positive structure, when the inverse structure is adopted, the organic photoelectric detector comprises a substrate, a transparent conductive cathode, a cathode modification layer, an active layer, an anode modification layer and a metal anode which are arranged from bottom to top, when the positive structure is adopted, the organic photoelectric detector comprises a substrate, a transparent conductive anode, an anode modification layer, an active layer, a cathode modification layer and a metal cathode which are arranged from bottom to top, the active layer is prepared by adopting an active layer solution, the mass ratio of a donor to an acceptor in the active layer solution is 0.5-2, and the donor and/or the acceptor are/is made of organic materials with temperature-dependent aggregation behaviors.
Further, the thickness of the active layer is 300 nm-1200 nm.
Further, the transparent conductive cathode and the transparent conductive anode adopt ITO thin films or FTO thin films.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. by adopting a step-by-step cooperative heat treatment method of heating spin coating and thermal annealing treatment, the phase separation scale of an active layer is regulated and controlled, the internal configuration of the active layer is optimized, the photoresponse rate and the external quantum efficiency EQE of a thick-film device are improved on the basis of keeping the low dark current density of the thick-film device, the specific detectivity D of the device is further improved, the influence on the electrical property of the device when the dark current is inhibited by increasing the thickness of the active layer is effectively reduced, the dark current and the photoresponse of the device are balanced, the overall performance of the organic photoelectric detector is further improved, the preparation process is simple to operate and high in stability, and the quality stability and the reliability of the prepared product are effectively ensured;
2. an organic material with temperature-dependent aggregation behavior is selected as a material of a donor and/or an acceptor in the active layer, so that the phase separation scale of the active layer is effectively regulated and controlled, the dark current inhibition effect is further improved, and the overall performance of the organic photoelectric detector is improved;
3. the organic photoelectric detector prepared by adopting the step-by-step cooperative heat treatment method of heating spin coating and thermal annealing treatment can regulate and control the phase separation size of the active layer, optimize the internal configuration, improve the optical response of the device under the condition of keeping low dark current density, realize the balance of dark current and optical response performance and effectively improve the overall performance of the invention.
Drawings
FIG. 1 is a flow chart of a method for fabricating an organic photodetector according to the present invention.
Fig. 2 is a schematic structural diagram of an organic photodetector adopting an inversion structure in the first embodiment.
FIG. 3 is a graph of spectral-responsivity of the organic photodetector fabricated in the first example;
FIG. 4 is a graph of spectral-specific detectivity of an organic photodetector prepared in accordance with example one;
fig. 5 is a schematic structural diagram of an organic photodetector with a positive structure according to a second embodiment.
Detailed Description
A method for preparing an organic photodetector, as shown in FIG. 1, comprises
Cleaning and drying the substrate, and preparing a transparent conductive electrode on the surface of the substrate to obtain a substrate;
preparing a first electrode modification layer on the surface of the transparent conductive electrode by adopting a solution processing process;
preparing an active layer on the surface of the first electrode modification layer by adopting a distributed synergistic heat treatment method of firstly heating, spin coating and then thermal annealing, wherein the preparation material of the active layer comprises an organic material with temperature-dependent aggregation behavior;
preparing a second electrode modification layer on the surface of the active layer;
and evaporating a metal electrode on the second electrode modification layer and packaging to obtain the photoelectric detector.
The organic photoelectric detector is of an inverse structure or a positive structure, and when the inverse structure is adopted, the organic photoelectric detector comprises a substrate, a transparent conductive cathode, a cathode modification layer, an active layer, an anode modification layer and a metal anode which are arranged from bottom to top, and when the positive structure is adopted, the organic photoelectric detector comprises a substrate, a transparent conductive anode, an anode modification layer, an active layer, a cathode modification layer and a metal cathode which are arranged from bottom to top, the active layer is prepared from an active layer solution, the mass ratio of a donor to an acceptor in the active layer solution is 0.5-2, and the donor and/or the acceptor are/is made of an organic material with temperature-dependent aggregation behavior.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments.
The first embodiment is as follows:
a preparation method of an organic photoelectric detector adopts an inversion structure, and specifically comprises the following steps:
s01, the substrate is cleaned and, after cleaning, blown dry with nitrogen.
S02, preparing a transparent conductive cathode on the surface of the substrate by adopting a magnetron sputtering, thermal evaporation, electron beam evaporation, spin coating, screen printing, spray coating or blade coating method, and then cleaning with ultraviolet ozone.
The substrate is glass or a transparent flexible substrate, the transparent conductive cathode is an ITO thin film or an FTO thin film, the transparent conductive cathode ITO is taken as an example for explanation, and the substrate and the transparent conductive cathode together form ITO conductive glass.
S03, preparing a cathode modification layer on the surface of the transparent conductive cathode by adopting one solution processing technology of spin coating, screen printing, spraying and blade coating, wherein the cathode modification layer is made of ZnO, PEIE, TiO2, LiF or SeO 2.
In this embodiment, a ZnO mixed solution is preferably spin-coated on the surface of the transparent conductive cathode ITO, and a thermal annealing treatment is performed in an atmospheric environment to prepare an electron transport layer, i.e., a cathode modification layer. The spin-coating rotation speed and time were 4000rpm and 40s, respectively, and the temperature and time of the thermal annealing treatment were 200 ℃ and 30min, respectively.
S04, preparing an active layer on the surface of the cathode modification layer by adopting a heating spin coating process, and performing thermal annealing treatment after the spin coating is finished to obtain the active layer with the thickness of 300-1200 nm. The method specifically comprises the following steps:
401: and preparing an active layer solution.
The active layer is prepared from an active layer solution comprising an organic donor and an organic acceptor, wherein the mass ratio of the donor to the acceptor in the active layer solution is 1: (0.5-2), the active layer solution adopts an organic solvent as a main solvent and is added with a solvent additive with the content of 0.1% -3%. The main solvent is one or more of chlorobenzene, o-dichlorobenzene and chloroform, and the solvent additive is one or more of 1, 8-Diiodooctane (DIO), Chloronaphthalene (CN) and nitrobenzene; the organic donor material is one or more of PBDB-T, PM6 and PBDTS-TDZ; the organic acceptor material is one or more of PC61BM, PC71BM, ITIC-Th, O-IDTBR, Y6 and IT-4F.
In the present embodiment, the organic donor is preferably an organic material with temperature-dependent aggregation behavior, and the donor material PBDB-T and the organic acceptor material Y6 are dissolved in Chlorobenzene (CB) solvent according to the mass ratio of 1:1.2, and the total concentration of the solution is 50 mg/ml.
402: the distribution is coordinated with the heat treatment. The active layer solution was spin-coated on the substrate prepared with the ZnO layer under a nitrogen atmosphere, followed by thermal annealing at 110 ℃ for 10 min. The thickness of the obtained active layer was 500 nm.
The heating spin coating is realized by the following modes:
the solution of the active layer comprising the organic donor and the organic acceptor is placed on a heating and stirring table for constant-temperature heating and stirring before spin coating. And (3) placing the substrate with the cathode modification layer on a spin coater, and performing spin coating by using the heated and stirred active layer solution. In order to ensure the molecular activity and the electrical property of the active layer after spin coating, the temperature consistency of the substrate and the solution temperature of the active layer is ensured in the spin coating process, and the temperature difference between the substrate and the solution temperature of the active layer is not more than 10 ℃. In order to keep the temperature of the substrate consistent with that of the active layer solution, a spin coater with a heating function is adopted to heat the substrate at constant temperature, or the substrate is preheated and then quickly transferred to the spin coater to be subjected to spin coating, and the substrate is preheated by adopting a constant-temperature heating table, an oven, far infrared heating or hot air heating and the like.
Preferably, the spin-coating heating temperature is not lower than room temperature and not higher than 140 ℃, and the thermal annealing temperature range and the thermal annealing time range are respectively 70-200 ℃ and 10-60 min.
And S05, preparing the anode modification layer on the surface of the active layer by adopting a vacuum evaporation or solution method. The anode modification layer is made of one or more of poly-TPD, PVK, MoO3, P3HT and PEDOT and PSS. Preferably, a hole transport layer MoO3, i.e. an anode modification layer, is evaporated on the surface of the active layer, and the pressure of the evaporated hole transport layer is 10-4Pa and the thickness is 10 nm.
And S06, evaporating a metal anode on the surface of the anode modification layer, and then packaging to obtain the organic photoelectric detector. The metal anode material is one or more of Ag, Al and Au. Preferably, the hole transport layer is evaporated with a metal anode Ag, the pressure of the evaporated metal anode is 10-4Pa and the thickness is 100 nm.
As shown in figure 2, the organic photoelectric detector prepared by the preparation method comprises a substrate, a transparent conductive cathode, a cathode modification layer, an active layer, an anode modification layer and a metal anode electrode which are arranged from bottom to top, wherein the mass ratio of an organic donor to an organic acceptor in the active layer is 0.5-2, the organic donor is made of an organic material with temperature-dependent aggregation behavior, and the preparation thickness of the active layer is 300-1200 nm.
Example two:
this example is different from the first example in that the organic photodetector is fabricated in a positive type structure. The preparation method of the organic photoelectric detector comprises the following steps:
s01, the substrate is cleaned and, after cleaning, blown dry with nitrogen.
S02, preparing a transparent conductive anode on the surface of the substrate by adopting a magnetron sputtering, thermal evaporation, electron beam evaporation, spin coating, screen printing, spray coating or blade coating method, and then cleaning with ultraviolet ozone.
The transparent conductive anode is an ITO film or an FTO film, and the substrate and the transparent conductive anode jointly form ITO conductive glass.
S03, preparing an anode modification layer on the surface of the transparent conductive anode by adopting one solution processing technology of spin coating, screen printing, spray coating and blade coating, wherein the anode modification layer is made of one or more of poly-TPD, PVK, MoO3, P3HT and PEDOT and PSS.
S04, preparing an active layer on the surface of the anode modification layer by adopting a heating spin coating process, and performing thermal annealing treatment after the spin coating is completed to obtain the active layer with the thickness of 300-1200 nm.
And S05, preparing a cathode modification layer on the surface of the active layer by adopting a vacuum evaporation or solution method. The cathode modification layer is made of ZnO, PEIE, TiO2, LiF or SeO 2.
And S06, evaporating a metal cathode on the surface of the cathode modified layer, and then packaging to obtain the organic photoelectric detector.
As shown in FIG. 5, the organic photoelectric detector prepared by the preparation method comprises a substrate, a transparent conductive anode, an anode modification layer, an active layer, a cathode modification layer and a metal cathode which are arranged from bottom to top, wherein the mass ratio of an organic donor to an organic acceptor in the active layer is 0.5-2, the organic donor is made of an organic material with temperature-dependent aggregation behavior, and the preparation thickness of the active layer is 300-1200 nm.
The active layer (the thickness is 300 nm-1200 nm) prepared by the method is thicker than that of a common organic photoelectric detector (50 nm-300 nm), so that the device has the characteristic of low dark current, meanwhile, one or more organic materials with Temperature Dependent Aggregation (TDA) behaviors are adopted in the active layer solution preparation materials, and a step-by-step synergistic heat treatment method is adopted, so that the aggregation of organic material components can be effectively inhibited, the balanced aggregation of a donor and an acceptor is realized, the microstructure regulation/phase separation scale regulation of the active layer is further realized, the light response rate and EQE of the device are improved while the low dark current of the device is maintained, the specific detection rate D of the device is improved, and the light response of the device is improved.
The technical effect of the invention is verified by specific test data as follows:
three organic photoelectric detector samples are selected to prepare the active layer in different preparation modes under the same test condition, and the samples adopt an inverse structure. At 0.307mW/cm2The data of the photoelectric properties under a bias of-0.5V measured by a Keithly4200 digital source table under a light source of 650nm are shown in Table 1:
Figure BDA0003083636870000061
as can be seen from table 1, under the condition that the thickness of the active layer is substantially the same, compared with a device prepared by directly spin-coating at room temperature, a device prepared by heating and spin-coating the active layer at 60 ℃ has substantially the same dark current, but the responsivity R of a sample subjected to heating and spin-coating is significantly improved, which proves that the photoelectric property of the organic photoelectric detector can be effectively improved by heating and spin-coating, and the comparison result of data obtained by thermal annealing treatment and no thermal annealing treatment proves that the photoelectric properties such as the responsivity of the device can be further improved after thermal annealing at 110 ℃.
The spectral response of the organic photoelectric detector prepared by each sample is tested by adopting a DSR100 wide-spectrum photoelectric testing system, the testing wave band is 300-1000nm, the testing bias voltage is-0.5V, the spectrum-responsivity curve graph 3 of the sample shows that the spectrum-specific detectivity curve of the sample is shown in figure 4, and the results of the figure 3 and the figure 4 prove that the photoelectric performance of the device in the whole response wave band is effectively improved after heating, spin coating and thermal annealing.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. A preparation method of an organic photoelectric detector is characterized by comprising the following steps: comprises that
Cleaning and drying the substrate, and preparing a transparent conductive electrode on the surface of the substrate to obtain a substrate;
preparing a first electrode modification layer on the surface of the transparent conductive electrode by adopting a solution processing process;
preparing an active layer on the surface of the first electrode modification layer by adopting a distributed synergistic heat treatment method of firstly heating, spin coating and then thermal annealing, wherein the preparation material of the active layer comprises an organic material with temperature-dependent aggregation behavior;
preparing a second electrode modification layer on the surface of the active layer;
and evaporating a metal electrode on the second electrode modification layer and packaging to obtain the photoelectric detector.
2. The method for manufacturing an organic photodetector as claimed in claim 1, wherein: the heating spin coating process specifically comprises the following steps: the method comprises the steps of placing an active layer solution comprising an organic donor and an organic acceptor on a heating and stirring table for constant-temperature heating and stirring, then placing a substrate with a first electrode modification layer on a spin coater, and spin-coating the substrate by using the active layer solution, wherein the temperature difference between the substrate and the active layer solution in the spin coating process is not more than 10 ℃.
3. The method for manufacturing an organic photodetector as claimed in claim 2, wherein: the thickness of the active layer is 300 nm-1200 nm.
4. The method for producing an organic photodetector as claimed in any one of claims 1 to 3, wherein: the mass ratio of the organic donor to the organic acceptor in the active layer solution is 0.5-2, and the content of the solvent additive is 0.1-3%.
5. The method for manufacturing an organic photodetector as claimed in any one of claims 4, wherein: the organic donor material adopted in the active layer solution is PBDB-T, PM6 and/or PBDTS-TDZ, the organic acceptor material adopted is PC61BM, PC71BM, ITIC-Th, O-IDTBR, Y6 and/or IT-4F, the main solvent adopted is chlorobenzene, O-dichlorobenzene and/or chloroform, and the solvent additive is 1, 8-Diiodooctane (DIO), Chloronaphthalene (CN) and/or nitrobenzene.
6. The method for manufacturing an organic photodetector as claimed in claim 1, wherein: the annealing temperature of the thermal annealing treatment is 70-200 ℃, and the thermal annealing time is 10-60 min.
7. The method for manufacturing an organic photodetector as claimed in claim 6, wherein: the annealing temperature was 110 ℃.
8. An organic photodetector prepared by the method of claim 1, wherein the organic photodetector has an inverse structure or a positive structure, and when the inverse structure is adopted, the organic photodetector comprises a substrate, a transparent conductive cathode, a cathode modification layer, an active layer, an anode modification layer and a metal anode electrode arranged from bottom to top, and when the positive structure is adopted, the organic photodetector comprises a substrate, a transparent conductive anode, an anode modification layer, an active layer, a cathode modification layer and a metal cathode electrode arranged from bottom to top, and the method comprises the following steps: the active layer is prepared from an active layer solution, the mass ratio of a donor to an acceptor in the active layer solution is 0.5-2, and the donor and/or the acceptor are/is made of an organic material with a temperature-dependent aggregation behavior.
9. The organic photodetector manufactured by the method for manufacturing an organic photodetector according to claim 8, wherein: the thickness of the active layer is 300 nm-1200 nm.
10. The organic photodetector manufactured by the method for manufacturing an organic photodetector according to claim 8, wherein: the transparent conductive cathode and the transparent conductive anode adopt ITO films or FTO films.
CN202110575986.5A 2021-05-25 2021-05-25 Organic photoelectric detector preparation method and prepared organic photoelectric detector Pending CN113270553A (en)

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