CN109713128B - Broadband near-infrared photoelectric detector and preparation method thereof - Google Patents

Broadband near-infrared photoelectric detector and preparation method thereof Download PDF

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CN109713128B
CN109713128B CN201811607541.5A CN201811607541A CN109713128B CN 109713128 B CN109713128 B CN 109713128B CN 201811607541 A CN201811607541 A CN 201811607541A CN 109713128 B CN109713128 B CN 109713128B
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CN109713128A (en
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沈亮
李成龙
周敬然
郭文滨
沈平
赵岩
张歆东
刘彩霞
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Jilin University
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Abstract

A broadband near-infrared photoelectric detector and a preparation method thereof belong to the technical field of photoelectric detection. Comprises an ITO conductive glass substrate, a PTAA hole transport layer, perovskite CH3NH3PbI3An active layer, a PTB7-Th/F8IC organic heterojunction layer, C60The electron transport layer, the BCP cathode buffer layer and the Cu cathode. According to the invention, an organic donor material PTB7-Th and an organic acceptor material F8IC are blended to form a heterojunction, and the heterojunction is further mixed with organic-inorganic hybrid perovskite CH3NH3PbI3The detection is realized by combining the two components, so that the detector can detect ultra-wide wavelength of 300-1000 nm and has ultra-fast response below 1ns, and the problem that the self light absorption waveband of the organic-inorganic hybrid perovskite material is limited in the ultraviolet to visible light region and the application is limited in many aspects is solved.

Description

Broadband near-infrared photoelectric detector and preparation method thereof
Technical Field
The invention belongs to the technical field of photoelectric detection, and particularly relates to a broadband near-infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction and a preparation method thereof.
Background
The photoelectric detector belongs to a highly sensitive optical detection tool, has important application in military affairs and national economy, and the detection of the infrared band can particularly relate to military infrared remote sensing, missile guidance, thermal imaging and the like; the ultraviolet to visible light wave band has applications in the fields of UV detection, image sensing, ray detection, optical communication and the like. The organic-inorganic hybrid perovskite material has the advantages of high light absorption coefficient, high carrier mobility, long exciton diffusion length and the like, has made breakthrough progress in the field of solar cells, and is also an excellent material for manufacturing high-performance photoelectric detectors. The preparation method of the organic-inorganic hybrid perovskite photoelectric detector is simple, has low cost, and provides a prerequisite for large-scale manufacturing. However, the light absorption band of the organic-inorganic hybrid perovskite material is limited to the ultraviolet to visible light region, so that the application of the organic-inorganic hybrid perovskite material is limited in many aspects, researchers can widen the absorption range of the perovskite by technical means, and can only obtain low detectivity of the infrared band or sacrifice the rapid response of the device. It is a hot research issue how to manufacture perovskite detectors capable of detecting light in a wider wavelength band while maintaining high detectivity. On the other hand, for the photoelectric detector, the dark current of the photoelectric detector is a key factor influencing the performance of the photoelectric detector, the quality of the device is reflected, the detector with low dark current has fewer defects and impurity recombination, and the quick response of the device is ensured. The related research must produce a detector with an ultra-fast response with sufficiently low dark current.
Disclosure of Invention
Aiming at the problems stated in the background technology, the invention provides a broadband near-infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction and a preparation method thereof, so as to solve the problems of narrow detection wave band, not fast response speed and the like of the organic-inorganic hybrid perovskite detector.
As a photoelectric detector material, the organic-inorganic hybrid perovskite material has the properties of low trap density, long carrier diffusion length, long carrier service life and the like, so that the prepared photoelectric detector can often obtain high detection rate, but the light absorption of the perovskite material is limited in the ultraviolet to visible light region, so that the prepared deviceThe application field is limited. The invention is prepared by mixing an organic donor material PTB7-Th (poly [4,8-bis (5- (2-ethylhexyl) thiophen-2-yl) benzol [1,2-b:4, 5-b']dithiophene -co-3-fluorothieno[3,4-b]thiophene-2-carboxylate]) Fused ring compounds synthesized with organic acceptor material F8IC (a 2- (5,6-difluoro-3-oxo-2, 3-dihydo-1H-inden-1-ylidine) -based malononitrile (2 FIC); synthetic methods reference is made to the reference1) Blending to form bulk heterojunction, and further mixing with organic-inorganic hybrid perovskite CH3NH3PbI3In combination, the perovskite material responds to optical signals in the ultraviolet to visible light region, and the heterojunction material responds to optical signals in the near infrared region; meanwhile, the perovskite and the PTB7-Th/F8IC heterojunction have high carrier mobility, and the whole device realizes ultra-wide wavelength detection and has low dark current and ultra-fast response.
The invention discloses a broadband near-infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction, which is characterized in that: the integral structure from the anode to the cathode sequentially comprises an ITO conductive glass substrate, a PTAA (poly (bis (4-phenyl) (2,4,6-trimethylphenyl) amine, a poly [ bis (4-phenyl) (2,4,6-trimethylphenyl) amine) hole transport layer, and an ultraviolet-visible light sensitive perovskite CH3NH3PbI3An active layer, a near-infrared photosensitive PTB7-Th/F8IC organic heterojunction layer, C60An electron transport layer, a BCP (2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline, 2,9-dimethyl-4, 7-biphenyl-1, 10-phenanthroline) cathode buffer layer and a Cu metal electrode. All of the above materials, except F8IC, are commercially available.
Perovskite CH of the invention3NH3PbI3The active layer is prepared by a common one-step method and is used as an ultraviolet-visible light absorption layer; the organic heterojunction layer prepared on the organic heterojunction layer consists of PTB7-Th and F8IC, wherein PTB7-Th is used as a donor material, F8IC is used as an acceptor material to form an organic bulk heterojunction, light in a near infrared region is absorbed, photo-generated electrons are transmitted to two electrodes of a detector after photoelectric conversion, and the perovskite CH sensitive to ultraviolet-visible light is connected with the detector3NH3PbI3Active layer bonding fromThe wide spectrum detection of ultraviolet-visible light region-near infrared band can be realized; in addition, the perovskite and the organic heterojunction have extremely high mobility, so that the obtained detector has ultrahigh response speed while maintaining high detection degree of each waveband.
The invention relates to a preparation method of a broadband near-infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction, which comprises the following steps:
the method comprises the following specific steps:
1) treatment of substrates
Ultrasonically cleaning ITO conductive glass for 10-30 minutes by using acetone, ultrasonically cleaning the ITO conductive glass for 10-30 minutes by using absolute ethyl alcohol, and ultrasonically cleaning the ITO conductive glass for 10-30 minutes by using deionized water; taking out the ITO conductive glass, and drying the ITO conductive glass by using nitrogen to serve as an anode of the device for later use;
2) preparation of hole transport layer and active layer
(1) Preparation of drug solution
Dissolving PTAA (poly [ bis (4-phenyl) (2,4,6-trimethylphenyl) amine ]) in toluene at the concentration of 1.0-3.0 mg/mL, and placing the solution on a magnetic stirrer to stir for 5-8 hours at room temperature;
② PbI with a molar ratio of 1: 12(lead iodide) and MAI (CH)3NH3I, iodomethylamine) was dissolved in DMF (N, N-dimethylformamide) and DMSO (dimethyl sulfoxide) at a volume ratio of 9: 1, the concentration range of the solute is 310-930 mg/mL, and the solute is fully dissolved by magnetic stirring for 10-12 hours at the temperature of 60-80 ℃ to obtain a perovskite precursor solution;
③ mixing the mixture with the molar ratio of 1: the PTB7-Th of 1 and F8IC are dissolved in DCB (1,2-dichlorobenzene, o-dichlorobenzene) together, the concentration of solute is 10-20 mg/mL, and the mixture is stirred at room temperature for 5-8 hours to be fully dissolved to obtain a PTB7-Th and F8IC blending solution;
(2) preparation of hole transport layer, perovskite active layer and organic heterojunction layer
Carrying out ultraviolet treatment on cleaned ITO conductive glass for 10-20 minutes, spin-coating a PTAA solution onto an ITO film of the ITO conductive glass at a speed of 3000-5000 rpm in a nitrogen atmosphere for 40-60 seconds, and then placing the ITO film on a heating table for annealing at a temperature of 80-100 ℃ for 20-40 minutes, so as to obtain a PTAA hole transport layer with a thickness of 1-5 nm on the ITO film;
② spin coating perovskite precursor solution onto the PTAA hole transport layer at 3500-4500 rpm for 40-60 s, dripping toluene, chlorobenzene or dichlorobenzene antisolvent 10-15 s before the end of spin coating, wherein the antisolvent dosage per unit area is 150-450 microliter/mm2Annealing at 80-100 ℃ for 20-40 minutes after the spin coating is finished to prepare an ultraviolet-visible light sensitive perovskite active layer with the thickness of 200-500 nm;
thirdly, spin-coating the PTB7-Th and F8IC blended solution on the perovskite active layer at the speed of 1000-3000 rpm, and annealing at the temperature of 60-80 ℃ for 20-40 minutes to obtain a near-infrared photosensitive organic heterojunction layer, wherein the thickness range is 50-100 nm;
3) preparation of electron transport layer, cathode buffer layer and metal electrode
① adjusting the temperature of the device obtained in step 2) to be lower than 5 × 10-4Growing a layer of C with the thickness of 20-40 nm on the organic heterojunction layer by a thermal evaporation method under the pressure of Pa60The evaporation rate of the material is 0.02-0.04 nm/s, and C is prepared60An electron transport layer;
② at C60Evaporating a layer of BCP material on the electron transport layer, wherein the thickness is 6-10 nm, and the evaporation rate is 0.01-0.03 nm/s, so as to prepare a cathode buffer layer;
evaporating a layer of metal electrode Cu on the cathode buffer layer, wherein the thickness of the metal electrode Cu is 80-100 nm, the evaporation rate is 0.05-0.08 nm/s, and preparing the metal electrode as a detector cathode, so that the broadband near-infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction is prepared.
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FIG. 1: the invention discloses a structural schematic diagram of a broadband near infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction; the names of all parts are as follows:
ITO conductive glass 1, PTAA hole transport layer 2, calcium titaniumMine CH3NH3PbI3Active layer 3, PTB7-Th/F8IC organic heterojunction layer 4, C60An electron transport layer 5, a BCP cathode buffer layer 6 and a Cu electrode 7.
FIG. 2: thin film absorption spectra of the perovskite active layer prepared in example 1, comparative example 2, the composite organic heterojunction layer, the organic heterojunction layer alone, and the perovskite layer alone. Wherein:
curve a represents the perovskite CH3NH3PbI3The light absorption profile of the active layer;
curve b represents the perovskite CH3NH3PbI3The light absorption curve of the active layer compounded PTB7-Th/F8IC organic heterojunction layer;
curve c represents the light absorption curve of the PTB7-Th/F8IC organic heterojunction layer alone;
as shown, perovskite CH3NH3PbI3The absorption range of the active layer is limited within 800nm, the PTB7-Th/F8IC organic heterojunction layer has stronger absorption in a near infrared region, and the combination of the two layers can have strong absorption extended to 1000nm, which fully proves that the combination of the two layers can effectively extend the absorption spectrum and is the optical basis of broadband detection in the invention.
FIG. 3: external Quantum Efficiency (EQE) spectra corresponding to the perovskite active layer composite organic heterojunction layer detector, the organic heterojunction layer detector alone, and the perovskite layer detector alone prepared in example 1, comparative example 1, and comparative example 2, wherein:
curve a represents the perovskite CH3NH3PbI3EQE curve of active layer recombination PTB7-Th/F8IC organic heterojunction layer device;
curve b represents the perovskite CH alone3NH3PbI3EQE curve of active layer device;
curve c represents the EQE curve for the PTB7-Th/F8IC organic heterojunction device alone;
as can be seen from the EQE diagram, pure CH3NH3PbI3(curve b) has light absorption of 350-800 nm and no response after 800 nm; and PTB7-Th/F8IC organic heterojunctionThe device has weak response in a visible light region and strong near infrared response; perovskite CH3NH3PbI3After the PTB7-Th/F8IC organic heterojunction is compounded, the photoelectric detector can detect light in an ultra-wide range of 300-1000 nm. The detection range of the perovskite detector is successfully expanded to a near infrared region by the novel detector prepared by the invention, and the perovskite detector can be more widely applied in practice.
FIG. 4: current-voltage (I-V) characteristic curves in a dark state of the detectors prepared in example 1, comparative example 3, and comparative example 4; wherein:
curve A device C60Thickness 0, i.e. no C60；
Curve B device C60The thickness is 50 nm;
curve C device C60The thickness is 20 nm.
Dark current is caused by internal defects of a detector and the like and seriously affects device performance, and generally, the lower the dark current of a photodetector, the better. As shown in the figure, in the invention, when other conditions are preferably kept unchanged, 20nm is C corresponding to the lowest dark current of the detector60And (4) thickness.
FIG. 5: EQE curves corresponding to the detectors prepared in example 1, comparative example 3 and comparative example 4; wherein
Curve A device C60Thickness 0, i.e. no C60；
Curve B device C60The thickness is 20 nm;
curve C device C60The thickness is 50 nm.
As can be seen from the figure, the thickness of C is 20nm when other conditions are ensured to be preferably constant60The detector of the electron transport layer exhibits a near infrared EQE value much higher than the other comparative devices. With reference to FIG. 4 and FIG. 5, the method for preparing the broadband photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic heterojunction in the invention is characterized in that C is added in the preparation process60The optimal thickness is about 20nm, and the device shows the best performance.
FIG. 6: example 1 a response speed profile corresponding to the prepared detector.
The response speed is an important core performance for determining the quality of the photodetector, and a general method for measuring the response speed is a Transient Photocurrent (TPC) method. The photoelectric detector collects pulse light signals emitted by the pulse laser, and then photoelectric carriers are driven to reach respective electrodes by a built-in potential field or external voltage bias. At this time, the response speed may be defined as the photocurrent decay time from the peak to about 1/e after a single exponential fitting of the TPC curve
It can be seen from the figure that the response time of the broadband photoelectric detector based on the organic-inorganic hybrid perovskite combined with the organic heterojunction, which is manufactured by the invention, reaches 0.96ns, which is the fastest level that can be achieved in the same kind of photoelectric detectors so far, and the broadband photoelectric detector has a prominent effect in practical application.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, and the functional layers and the manufacturing methods in the embodiments can be replaced without contradiction.
Example 1:
a preparation method of a broadband near-infrared photoelectric detector based on the combination of organic-inorganic hybrid perovskite and organic polymer bulk heterojunction comprises the following steps:
1. preparing a solution required by an experiment:1dissolving the PTAA in toluene with the concentration of 2mg/mL, and stirring for 6 hours at room temperature; mixing a mixture of 1: 1 PbI of2(lead iodide) and MAI (CH)3NH3I, iodomethylamine) in DMF (N, N-dimethylformamide) and DMSO (dimethyl sulfoxide) at a volume ratio of 9: 1, the concentration is 465 mg/mL, and the solute is fully dissolved by magnetic stirring for 10 hours at 70 ℃ to prepare a precursor solution of the perovskite film by a one-step method; mixing a mixture of 1: PTB7-Th of 1 and F8IC were dissolved in DCB (1,2-dichlorobenzene, o-dichlorobenzene) at a concentration of 10mg/mL and thoroughly dissolved by stirring at room temperature for 6 hours;
2. carrying out ultrasonic cleaning on the ITO glass for 20 minutes by using acetone, absolute ethyl alcohol and deionized water in sequence, and carrying out ultraviolet ozone treatment for 10 minutes after drying for later use;
3. taking a proper amount of prepared PTAA solution, spin-coating the prepared PTAA solution on ITO glass at 4000rpm, and placing the ITO glass on a heating table to anneal for 30 minutes at 90 ℃; the PTAA hole transport layer was obtained with a thickness of about 15 nm.
4. Spin-coating a perovskite film precursor solution on a PTAA layer at the speed of 4000rpm for 50 seconds, dropwise adding toluene as an anti-solvent within 10 seconds before the end of spin-coating (the dropping amount of the anti-solvent on a hole transport layer in unit area is 300 microliter), and then placing the device on a heating table to anneal for 30 minutes at 90 ℃ to generate ultraviolet-visible light sensitive CH3NH3PbI3A perovskite active layer having a thickness of 200 nm.
5. The PTB7-Th and F8IC blended solution was spin coated on the perovskite active layer at 2000rpm and annealed at 80 ℃ for 30 minutes to obtain an organic heterojunction layer with a thickness of 80 nm.
6. Transferring the device into a multi-source organic vapor phase molecular deposition system, and controlling the gas pressure at 5 × 10-4Growing a layer of C on the surface of the organic heterojunction layer by a thermal evaporation method under Pa60An electron transport layer with a thickness of 20nm and an evaporation rate of 0.03 nm/s; at C60A BCP cathode buffer layer is evaporated on the electron transport layer, the thickness is 7nm, and the evaporation rate is 0.02 nm/s; and finally evaporating a layer of metal electrode Cu on the cathode buffer layer, wherein the thickness of the metal electrode Cu is 100nm, and the evaporation rate is 0.05 nm/s. The broadband near-infrared photoelectric detector based on the combination of the organic-inorganic hybrid perovskite and the organic polymer bulk heterojunction is prepared.
In order to further explore the performance factors affecting the broadband organic-inorganic hybrid perovskite photoelectric detector, the invention is provided with a comparative example
Comparative example 1
The organic-inorganic hybrid perovskite detector prepared in the comparative example 1 is the same as the organic-inorganic hybrid perovskite detector prepared in the example 1, and the preparation method is different from that of the organic-inorganic hybrid perovskite detector in that: the device has no PTB7-Th/F8IC organic heterojunction layer, and the specific structure is as follows: ITO/PTAA/CH3NH3PbI3/C60/BCP/Cu。
Comparative example 2
Comparative example 2 an organic photodetector based on a PTB7-Th/F8IC heterojunction layer was prepared in the same way as in example 1, except that: the device does not have a perovskite active layer, and the specific structure is as follows: ITO/PTAA/PTB7-Th:F8IC/C60/BCP/Cu。
comparative example 3
The preparation method of the broadband organic-inorganic hybrid perovskite photodetector of comparative example 3 is the same as that of example 1, except that C is not evaporated60An electron transport layer.
Comparative example 4:
the preparation method of the broadband organic-inorganic hybrid perovskite photodetector of comparative example 4 is the same as that of example 1, except that C60The thickness was 50 nm.
Reference documents:
1.Dai S,Li T,Wang W,Xiao Y,Lau TK,Li Z,et al.Enhancing thePerformance of Polymer Solar Cells via Core Engineering of NIR-AbsorbingElectron Acceptors.Advanced materials 2018,30(15)。

Claims (2)

1. a preparation method of a broadband near-infrared photoelectric detector based on the combination of an organic-inorganic hybrid perovskite active layer and an organic polymer bulk heterojunction layer comprises the following steps:
1) treatment of substrates
Ultrasonically cleaning ITO conductive glass for 10-30 minutes by using acetone, ultrasonically cleaning the ITO conductive glass for 10-30 minutes by using absolute ethyl alcohol, and ultrasonically cleaning the ITO conductive glass for 10-30 minutes by using deionized water; taking out the ITO conductive glass, and drying the ITO conductive glass by using nitrogen to serve as an anode of the device for later use;
2) preparation of hole transport layer and active layer
(1) Preparation of drug solution
Dissolving the PTAA in toluene to obtain a solution with a concentration of 1.0-3.0 mg/mL, and stirring the solution on a magnetic stirrer at room temperature for 5-8 hours;
② PbI with a molar ratio of 1: 12And MAI dissolved in DMF and DMSO at a volume ratio of 9: 1, performing magnetic stirring for 10-12 hours at 60-80 ℃ to fully dissolve a solute to obtain a perovskite precursor solution, wherein the concentration of the mixed solvent is 310-930 mg/mL;
③ mixing the mixture with the molar ratio of 1: the PTB7-Th of 1 and the F8IC are dissolved in DCB together, the concentration of solute is 10-20 mg/mL, and the mixture is stirred for 5-8 hours at room temperature to be fully dissolved to obtain a PTB7-Th and F8IC blending solution;
(2) preparation of hole transport layer, perovskite active layer and organic polymer bulk heterojunction layer
Carrying out ultraviolet treatment on cleaned ITO conductive glass for 10-20 minutes, spin-coating a PTAA solution onto an ITO film of the ITO conductive glass at a speed of 3000-5000 rpm in a nitrogen atmosphere for 40-60 seconds, and then placing the ITO film on a heating table for annealing at a temperature of 80-100 ℃ for 20-40 minutes, so as to obtain a PTAA hole transport layer with a thickness of 1-5 nm on the ITO film;
② spin coating perovskite precursor solution onto the PTAA hole transport layer at 3500-4500 rpm for 40-60 s, dripping toluene, chlorobenzene or dichlorobenzene antisolvent 10-15 s before the end of spin coating, wherein the antisolvent dosage per unit area is 150-450 microliter/mm2Annealing at 80-100 ℃ for 20-40 minutes after the spin coating is finished to prepare an ultraviolet-visible light sensitive perovskite active layer with the thickness of 200-500 nm;
thirdly, spin-coating the PTB7-Th and F8IC blended solution on the perovskite active layer at the speed of 1000-3000 rpm, and annealing at the temperature of 60-80 ℃ for 20-40 minutes to obtain a near-infrared photosensitive organic polymer bulk heterojunction layer, wherein the thickness range is 50-100 nm;
3) preparation of electron transport layer, cathode buffer layer and metal electrode
① adjusting the temperature of the device obtained in step 2) to be lower than 5 × 10-4Growing a layer of C with the thickness of 20-40 nm on the organic polymer bulk heterojunction layer by a thermal evaporation method under the pressure Pa60The evaporation rate of the material is 0.02-0.04 nm/s, and C is prepared60An electron transport layer;
② at C60Evaporating a layer of BCP material on the electron transport layer, wherein the thickness is 6-10 nm, and the evaporation rate is 0.01-0.03 nm/s, so as to prepare a cathode buffer layer;
evaporating a layer of metal electrode Cu on the cathode buffer layer, wherein the thickness of the metal electrode Cu is 80-100 nm, the evaporation rate is 0.05-0.08 nm/s, and preparing the metal electrode as a detector cathode, so that the broadband near infrared photoelectric detector based on the combination of the organic and inorganic hybrid perovskite active layer and the organic polymer bulk heterojunction layer is prepared.
2. A broadband near-infrared photoelectric detector based on the combination of an organic-inorganic hybrid perovskite active layer and an organic polymer bulk heterojunction layer is characterized in that: is prepared by the method of claim 1.
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