CN111430480A - Homojunction perovskite photoelectric detector and preparation method and application thereof - Google Patents

Homojunction perovskite photoelectric detector and preparation method and application thereof Download PDF

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CN111430480A
CN111430480A CN202010304320.1A CN202010304320A CN111430480A CN 111430480 A CN111430480 A CN 111430480A CN 202010304320 A CN202010304320 A CN 202010304320A CN 111430480 A CN111430480 A CN 111430480A
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thin film
type perovskite
layer
perovskite thin
transport layer
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吴丹
王恺
刘皓宸
李文辉
昂科科觉
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Southwest University of Science and Technology
Southern University of Science and Technology
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Abstract

The invention relates to a homojunction perovskite photoelectric detector and a preparation method and application thereof, wherein the homojunction perovskite photoelectric detector comprises an N-type perovskite thin film and a P-type perovskite thin film which are adjacently arranged, an electron transmission layer and a transparent conductive substrate which are sequentially arranged on one side of the N-type perovskite thin film back to the P-type perovskite thin film, and a hole transmission layer and a metal electrode which are sequentially arranged on one side of the P-type perovskite thin film back to the N-type perovskite thin film.

Description

Homojunction perovskite photoelectric detector and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photoelectric detectors, and relates to a homojunction perovskite photoelectric detector, and a preparation method and application thereof.
Background
Photoelectric detectors are important optoelectronic components in the photoelectric information industry at present, and are often used in the fields of sensing, detection, imaging and the like. The existing traditional photoelectric detector materials such as Si, Ge, InGaAs and the like have the defects of complex preparation process, high cost, inflexibility and the like.
In recent years, perovskite materials have been widely used in the field of optoelectronic devices due to their high absorption coefficient, wide band coverage from ultraviolet to near infrared, high carrier mobility, and micron-scale diffusion length. However, how to further design the device structure and fully exert the excellent photoelectric characteristics of the perovskite material to meet the requirements of various detections is a great importance in the research and development of preparing the perovskite material-based photoelectric detector. The requirements of today's society for high performance photodetectors include: the method has the advantages of narrow-band response to the detected spectrum, continuously adjustable peak wavelength of each response spectrum, high external quantum efficiency, high response speed, capability of simultaneously integrating the response of a plurality of wave bands on one chip, flexibility, simple preparation process, low cost and the like. However, perovskite materials are simply introduced into a traditional device structure, and the prepared narrow-band multi-spectrum photoelectric detector has the difficulties of low External Quantum Efficiency (EQE), low response speed, narrow bandwidth and the like at present, and cannot exert excellent performance of the materials.
CN209785975U discloses a perovskite photodetector, which comprises a substrate, a bottom electrode, a light absorption layer, a top electrode and an optical modulation layer, wherein the substrate, the bottom electrode, the light absorption layer, the top electrode and the optical modulation layer are sequentially formed from bottom to top, the optical modulation layer comprises a lower dielectric layer and an upper light reflection film layer, and the dielectric layer is selected from Si, ZnO, ZnS and Si3N4、Al2O3、SiO2And TiO2The light reflective film layer is selected from one of Au, Ag, Al, Cu, Ni, Pt, Ti, TiN, and ZrN; CN109841703A discloses an all-inorganic perovskite photoelectric detector and a preparation method thereof, wherein the all-inorganic perovskite photoelectric detector comprises a transparent conductive positive electrode, an ultrathin alumina layer, an all-inorganic perovskite light absorption layer, an electron transmission layer and a metal negative electrode, and the photoelectric detectors in the scheme have the problems of insufficient response speed and external quantum efficiency.
Therefore, it is still of great significance to develop a perovskite photodetector with higher response speed and external quantum efficiency.
Disclosure of Invention
The invention aims to provide a homojunction perovskite photoelectric detector and a preparation method and application thereof, wherein the homojunction perovskite photoelectric detector comprises an N-type perovskite thin film and a P-type perovskite thin film which are adjacently arranged, an electron transmission layer and a transparent conductive substrate which are sequentially arranged on one side of the N-type perovskite thin film, which is back to the P-type perovskite thin film, and a hole transmission layer and a metal electrode which are sequentially arranged on one side of the P-type perovskite thin film, which is back to the N-type perovskite thin film.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a homojunction perovskite photoelectric detector, which comprises an N-type perovskite thin film and a P-type perovskite thin film which are adjacently arranged, wherein an electron transmission layer is arranged on one side of the N-type perovskite thin film, which is back to the P-type perovskite thin film, and a transparent conductive substrate is arranged on one side of the electron transmission layer, which is back to the N-type perovskite thin film; and a hole transport layer is arranged on one side of the P-type perovskite film back to the N-type perovskite film, and a metal electrode is arranged on one side of the hole transport layer back to the P-type perovskite film.
The homojunction perovskite photoelectric detector comprises a homojunction formed by an N-type perovskite film and a P-type perovskite film which are adjacently arranged, and can form a built-in electric field in a device, so that the problems of low response speed and low external quantum efficiency of the device caused by the fact that the traditional photoelectric detector can only use an external electric field to separate photo-generated electron-hole pairs are solved. The depletion layer in the perovskite homojunction in the homojunction perovskite photoelectric detector can form a built-in electric field, and the direction of the electric field is the same as that of an external electric field, so that the depletion layer can be acted together with the external electric field to strengthen the separation of photon-generated electron hole pairs and accelerate the transportation of current carriers, and further the EQE and the response speed of the device are effectively improved.
In the homojunction perovskite photoelectric detector, the active layer is homojunction perovskite. Holes of high doping concentration are present in the P-type perovskite region, while electrons of high doping concentration are present in the N-type perovskite region. At the interface between the P-type perovskite thin film and the N-type perovskite thin film, holes diffuse from the P-type perovskite region to the N-type perovskite region due to the gradient change of the concentrations of the holes and the electrons, and electrons diffuse from the N-type perovskite region to the P-type perovskite region, so that the holes and the electrons meet and are recombined, and a depletion layer is formed at a PN junction region near the interface. After reaching the thermal equilibrium steady state, the depletion layer on the side close to the P-type perovskite region is negatively charged due to hole recombination; meanwhile, the depletion layer on the side close to the N-type perovskite region is positively charged due to electron recombination. The positive and negative ions generate a built-in electric field in the depletion layer, the direction of the built-in electric field is the same as that of the external electric field, the built-in electric field and the external electric field act together to strengthen the separation of electrons and holes, reduce the recombination probability of electron-hole pairs and improve the EQE value, and meanwhile, the existence of the built-in electric field promotes the accelerated motion of carriers, so that the carriers quickly reach the electrodes and the response speed of the device is improved.
The molecular formula of the perovskite thin film is CH3NH3PbX3Wherein X is any one or a combination of at least two of Cl, Br, or I, which illustratively includes a combination of Cl and Br, a combination of I and Cl, or a combination of Br and I, and the like. Wherein, in the preparation process of the N-type perovskite film, a precursor PbX is adopted2Molar mass of not less than CH3NH3Molar amount of X, preferably PbX2And CH3NH3The molar ratio of X is (1-1.15): 1. In the preparation process of the P-type perovskite film, a precursor PbX is used2Is less than CH3NH3Molar amount of X, preferably PbX2And CH3NH3The molar ratio of X is 0.89-0.93.
Preferably, the thickness of the N-type perovskite thin film is 400-500nm, such as 410nm, 420nm, 430nm, 440nm, 450nm, 460nm, 470nm, 480nm or 490nm and the like.
Preferably, the thickness of the P-type perovskite thin film is 50-100nm, such as 60nm, 70nm, 80nm or 90nm and the like.
Preferably, the ratio of the thickness of the N-type perovskite thin film to the thickness of the P-type perovskite thin film is 4-10, such as 5, 6, 7, 8 or 9.
Preferably, the electron transport layer comprises a dense layer and a mesoporous layer which are adjacently arranged, and the mesoporous layer is adjacent to the N-type perovskite thin film.
The mesoporous layer here serves to support and transport electrons and the dense layer serves to transport electrons and block holes.
Preferably, the material of the compact layer is TiO2、SnO2Or ZnO.
Preferably, the mesoporous layer is made of TiO2And/or Al2O3。
Preferably, the electron transport layer is prepared by solution and/or atomic layer deposition techniques.
Preferably, the thickness of the dense layer is 30-60nm, such as 35nm, 40nm, 45nm, 50nm, or 55nm, and the like.
Preferably, the thickness of the mesoporous layer is 150-200nm, such as 160nm, 170nm, 180nm or 190 nm.
Preferably, the N-type perovskite thin film is prepared by a solution method and/or an evaporation method.
Preferably, the hole transport layer includes at least one of spiro-OMeTAD, PTAA, CuSCN, or CuPc therein.
Preferably, the hole transport layer has a thickness of 200-300nm, such as 210nm, 220nm, 230nm, 240nm, 250nm, 260nm, 270nm, 280nm or 290 nm.
The size of the hole transport layer is controlled within the range, so that the hole transport layer is beneficial to extracting holes and transferring the holes to the electrode layer, and further, the response efficiency and the EQE value of the device are improved.
Preferably, the hole transport layer further comprises a lithium salt and/or a cobalt salt.
Preferably, the lithium salt comprises L i-TFSI.
Preferably, the cobalt salt comprises tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III) tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) (FK 209).
Preferably, the transparent conductive substrate is ITO or FTO transparent conductive glass.
Preferably, the transparent conductive substrate has a square resistance of 10 to 25 Ω, for example, 11 Ω, 13 Ω, 15 Ω, 17 Ω, 19 Ω, 20 Ω, 22 Ω, 24 Ω, or the like.
Preferably, the transparent conductive substrate has a transmittance of 80-95%, such as 82%, 84%, 86%, 88%, 90%, 92%, 94%, or the like. The transmittance here refers to the light transmittance.
The square resistance and the transmittance of the transparent conductive substrate in the homojunction photoelectric detector are controlled in the range, so that the response efficiency and the EQE value of the device are improved.
Preferably, the metal electrode includes any one of Al, Ag or Au or a combination of at least two thereof, which illustratively includes a combination of Al and Ag, a combination of Au and Al, or a combination of Ag and Au, and the like.
In a second aspect, the present invention provides a method of fabricating a homojunction perovskite photodetector as described in the first aspect, the method comprising the steps of:
(1) preparing an electron transport layer on a transparent conductive substrate;
(2) preparing an N-type perovskite thin film on the surface of the electron transport layer obtained in the step (1);
(3) preparing a P-type perovskite film on the surface of the N-type perovskite film obtained in the step (2);
(4) preparing a hole transport layer on the surface of the P-type perovskite thin film obtained in the step (3);
(5) and (5) preparing a metal electrode on the surface of the hole transport layer obtained in the step (4) to obtain the homojunction perovskite photoelectric detector.
Preferably, the method for preparing the electron transport layer on the transparent conductive substrate in step (1) includes preparing a dense layer on the transparent conductive substrate, and then preparing a mesoporous layer on the surface of the obtained dense layer to obtain the electron transport layer.
Preferably, the material of the compact layer is TiO2And the preparation process of the compact layer comprises the steps of spin coating a titanium source solution on the transparent conductive substrate, and then annealing to obtain the compact layer.
Preferably, the titanium source is at least one of diisopropyl di (acetylacetonate) titanate, titanium tetrachloride or isopropyl titanate.
Preferably, the solvent of the titanium source solution is any one or a combination of at least two of 1-butanol, ethanol or isopropanol.
Preferably, the concentration of the titanium source solution is 0.1-0.2M, such as 0.12M, 0.14M, 0.15M, 0.16M, or 0.18M, and the like.
Preferably, the spin coating rate during the preparation of the dense layer is 1500-.
Preferably, in the preparation process of the dense layer, the annealing temperature is 450-.
Preferably, the temperature rise rate of annealing during the preparation of the dense layer is 4-6 deg.C/min, such as 4.5 deg.C/min, 5 deg.C/min, or 5.5 deg.C/min.
Preferably, the mesoporous layer is made of TiO2The preparation method of the mesoporous layer comprises the step of adding TiO2The slurry is spin-coated on the surface of the dense layer, and then annealed to obtain the mesoporous layer.
Preferably, the TiO is2The slurry is diluted with a solvent before spin coating.
Preferably, the solvent used for dilution comprises any one of ethanol, 1-butanol or isopropanol or a combination of at least two thereof.
Preferably, the TiO is2TiO in the slurry2The particle size is 18-30nm, such as 19nm, 20nm, 21nm, 22nm, 23nm, 24nm, 25nm, 26nm, 27nm, 28nm or 29 nm.
Preferably, the spin coating rate during the preparation of the mesoporous layer is 3500-4500rpm, such as 3600rpm, 3700rpm, 3800rpm, 3900rpm, 4000rpm, 4100rpm, 4200rpm, 4300rpm or 4400 rpm.
Preferably, the temperature of annealing in the preparation process of the mesoporous layer is 450-.
Preferably, the temperature rise rate of the annealing is 4-6 deg.C/min, such as 4.5 deg.C/min, 5 deg.C/min, or 5.5 deg.C/min, etc. during the preparation of the mesoporous layer.
Preferably, the method for preparing an N-type perovskite thin film in the step (2) comprises reacting CH3NH3X and PbX2The mixed solution is coated on the mesoporous layer in a spinning way and then is heated to obtain the N-type perovskite film, wherein PbX is contained in the N-type perovskite film2Molar mass of not less than CH3NH3Molar amount of X.
Preferably, in the preparation process of the N-type perovskite thin film, CH3NH3X and PbX2In the mixed solution of (2) PbX2And CH3NH3The molar ratio of X is (1-1.15):1, for example, 1.03:1, 1.05:1, 1.08:1, 1.1:1, 1.12:1, or 1.14: 1.
Preferably, the spin coating rate during the preparation of the N-type perovskite thin film is 3500-4500rpm, such as 3600rpm, 3800rpm, 4000rpm, 4200rpm or 4400 rpm.
Preferably, anisole is added on the surface of the spin coating in the process of the spin coating in the preparation process of the N-type perovskite thin film.
Preferably, the CH3NH3X and PbX2The solvent of the mixed solution of (1) is a mixed solution of dimethylformamide and dimethyl sulfoxide.
Preferably, the volume ratio of dimethylformamide to dimethyl sulfoxide in the mixed solution of dimethylformamide and dimethyl sulfoxide is (3-5):1, for example, 3.3:1, 3.5:1, 3.8:1, 4:1, 4.2:1, 4.4:1, 4.6:1 or 4.8:1, and preferably (3.5-4.5): 1.
Preferably, in the preparation process of the N-type perovskite thin film, the temperature of the heating treatment is 90-110 ℃, and the time of the heating treatment is 8-12min, such as 9min, 10min or 11 min.
Preferably, the method for preparing the P-type perovskite thin film in the step (3) comprises the step of carrying out vacuum vapor deposition PbX on the surface of the N-type perovskite thin film obtained in the step (2)2Then dipping it in CH3NH3Obtaining the P-type perovskite film in an X solution, wherein PbX is2Is less than CH3NH3Molar amount of X.
The preparation process of the P-type perovskite thin film adopts a method combining vacuum vapor deposition and impregnation, so that the influence on the structure of the N-type perovskite thin film in the preparation process of the P-type perovskite thin film can be avoided, and the preparation effect is improved.
Preferably, PbX is adopted in the preparation process of the P-type perovskite thin film2And CH3NH3The molar amount ratio of X is 0.89 to 0.93, for example 0.9, 0.91 or 0.92.
PreferablySaid CH3NH3The solvent of the X solution is isopropanol.
Preferably, in the preparation process of the P-type perovskite thin film, the method further comprises annealing treatment after the dipping is finished, wherein the annealing temperature is 95-105 ℃, such as 96 ℃, 97 ℃, 98 ℃, 99 ℃, 100 ℃, 101 ℃, 102 ℃, 103 ℃ or 104 ℃, and the annealing time is 5-20min, such as 8min, 10min, 12min, 15min or 18 min.
Preferably, the method for preparing the hole transport layer in the step (4) includes: and spin-coating a solution containing spiro-OMeTAD on the surface of the P-type perovskite thin film to obtain the hole transport layer.
Preferably, the solvent of the spiro-OMeTAD containing solution comprises chlorobenzene.
Preferably, the solution containing spiro-OMeTAD also comprises lithium salt and cobalt salt.
Preferably, the lithium salt comprises L i-TFSI.
Preferably, the cobalt salt comprises tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III) tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) (FK 209).
Preferably, the solution containing spiro-OMeTAD also contains 4-tert-butylpyridine.
Preferably, during the preparation of the hole transport layer, the spin coating speed is 3250 and 3750rpm, such as 3300rpm, 3400rpm, 3500rpm, 3600rpm or 3700 rpm.
Preferably, the metal electrode in the step (5) is prepared by a vacuum evaporation method.
Preferably, the pressure of the vacuum evaporation is less than 10-4Pa, e.g. 5 × 10-5Pa、10-5Pa、5×10-6Pa or 10-6Pa, and the like.
As a preferred technical scheme of the invention, the preparation method of the homojunction perovskite photoelectric detector comprises the following steps:
(1) preparing an electron transport layer on a transparent conductive substrate, wherein the preparation process comprises spin coating a titanium source solution on the transparent conductive substrate, and annealing to obtain TiO2Dense layer, then on the resulting TiO2Surface spin coating TiO of compact layer2Slurry and annealing to obtain TiO2A mesoporous layer, obtaining the electron transport layer;
(2) preparing an N-type perovskite thin film on the surface of the electron transport layer obtained in the step (1), wherein the N-type perovskite thin film comprises reacting CH3NH3X and PbX2Spin coating the TiO in step (1) with the mixed solution of2Heating at 90-110 deg.C for 8-12min to obtain the N-type perovskite thin film, wherein PbX is added2And CH3NH3The molar weight ratio of X is (1-1.15) to 1;
(3) preparing a P-type perovskite thin film on the surface of the N-type perovskite thin film obtained in the step (2), wherein PbX is subjected to vacuum vapor deposition on the surface of the N-type perovskite thin film obtained in the step (2)2Then dipping it in CH3NH3In X solution to obtain the P-type perovskite film, PbX2And CH3NH3The molar weight ratio of X is 0.89-0.93;
(4) preparing a hole transport layer on the surface of the P-type perovskite thin film obtained in the step (3), wherein the hole transport layer is obtained by spin-coating a solution containing spiro-OMeTAD, lithium salt, cobalt salt and 4-tert-butylpyridine on the surface of the P-type perovskite thin film;
(5) and (4) preparing a metal electrode on the surface of the hole transport layer obtained in the step (4) through vacuum evaporation to obtain the homojunction perovskite photoelectric detector.
In a third aspect, the present invention provides use of a homojunction perovskite photodetector as described in the first aspect for machine vision, biosensing and imaging or optical communication.
In a fourth aspect, the present invention provides a homojunction perovskite for use in a photodetector, wherein the homojunction perovskite has a structure comprising an N-type perovskite thin film and a P-type perovskite thin film which are adjacently disposed, and the structure of the photodetector obtained by applying the homojunction perovskite to the photodetector is as defined in the first aspect.
Compared with the prior art, the invention has the following beneficial effects:
the homojunction perovskite photoelectric detector is based on a homojunction optimized perovskite photoelectric detector, a built-in electric field is formed inside the photoelectric detector due to the existence of the homojunction perovskite inside the photoelectric detector, separation and transportation of photon-generated carriers can be enhanced, and the problems of low response speed and low external quantum efficiency of a device caused by the fact that the conventional photoelectric detector can only use an external electric field to separate photon-generated electron holes are solved.
Drawings
FIG. 1 is a schematic structural view of a homojunction perovskite photodetector according to the present invention;
the structure comprises a 1-transparent conductive substrate, a 2-electron transport layer, a 20-mesoporous layer, a 21-dense layer, a 3-N type perovskite thin film, a 4-P type perovskite thin film, a 5-hole transport layer and a 6-metal electrode.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
The structural schematic diagram of the homojunction perovskite photoelectric detector is shown in fig. 1, and as can be seen from fig. 1, the homojunction perovskite photoelectric detector sequentially comprises a transparent conductive substrate 1, an electron transmission layer 2, an N-type perovskite thin film 3, a P-type perovskite thin film 4, a hole transmission layer 5 and a metal electrode 6 from bottom to top, wherein the electron transmission layer 2 is composed of a mesoporous layer 20 and a dense layer 21, and the dense layer 21 is adjacent to the transparent conductive substrate 1.
In use of the homojunction perovskite photodetector shown in fig. 1, incident light enters the photodetector from one side of the transparent conductive substrate.
The photodetectors in the following embodiments all adopt the structure shown in fig. 1.
Example 1
In the embodiment, the transparent conductive substrate in the homojunction perovskite photoelectric detector is FTO transparent conductive glass, the square resistance of the transparent conductive substrate is 10 omega, and the transmittance of the transparent conductive substrate is 95%; the electron transport layer comprises TiO with a thickness of 30nm2Dense layer and thickness of 2TiO of 00nm2A mesoporous layer; n-type perovskite thin film (precursor PbX)2And CH3NH3X molar ratio of 1.05:1) was 480nm thick, and P-type perovskite thin film (PbX) was formed2And CH3NH3The molar ratio of X is 0.9) and the thickness is 60 nm; the thickness ratio of the N-type perovskite thin film to the P-type perovskite thin film is 8, the metal electrode is an Au electrode, and the thickness of the gold electrode is 80 nm.
The preparation method of the homojunction perovskite photodetector comprises the following steps:
(1) spin-coating a 1-butanol solution of diisopropyl di (acetylacetonate) titanate with the concentration of 0.15M on a transparent conductive substrate at the spin-coating speed of 2000rpm, and then annealing at 500 ℃ for 30min to obtain the TiO2Dense layer of TiO2The slurry (30NR-T, Dysol) was mixed and diluted with ethanol at a mass ratio of 6:1, and then spin-coated on the resulting TiO2Annealing the surface of the compact layer at 500 ℃ for 30min to obtain TiO2A mesoporous layer, obtaining the electron transport layer;
(2) will CH3NH3X and PbX2The TiO in the step (1) is spin-coated by using a mixed solution of dimethylformamide and dimethyl sulfoxide in a volume ratio of 4:1 as a solvent2Spin-coating on the mesoporous layer at 4000rpm, and heating at 100 deg.C for 10min to obtain the N-type perovskite thin film, wherein PbX2And CH3NH3The molar weight ratio of X is 1.05: 1;
(3) vacuum vapor deposition PbX on the surface of the N-type perovskite thin film obtained in the step (2)2Then dipping it in CH3NH3In X solution to obtain the P-type perovskite film, PbX2And CH3NH3The molar weight ratio of X is 0.9;
(4) and spin-coating a chlorobenzene solution containing spiro-OMeTAD, L i-TFSI, tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III), tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) and 4-tert-butylpyridine on the surface of the P-type perovskite thin film at a spin-coating rate of 3500rpm to obtain the hole transport layer, wherein the mass ratio of spiro-OMeTAD, L i-TFSI and tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III) tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) in the chlorobenzene solution is 7:1:0.25, and the volume ratio of the mass of spiro-OMeTAD to the 4-tert-butylpyridine is 2.41mg/m L.
(5) And (4) preparing an Au electrode on the surface of the hole transport layer obtained in the step (4) through vacuum evaporation to obtain the homojunction perovskite photoelectric detector.
Example 2
In the embodiment, the transparent conductive substrate in the homojunction perovskite photoelectric detector is FTO transparent conductive glass, the square resistance of the transparent conductive substrate is 25 omega, and the transmittance of the transparent conductive substrate is 80%; the electron transport layer comprises TiO 50nm thick2Compact layer and TiO with a thickness of 200nm2A mesoporous layer; n-type perovskite thin film (precursor PbX)2And CH3NH3X molar ratio of 1.15:1) was 500nm, and P-type perovskite thin film (precursor PbX)2And CH3NH3The molar weight ratio of X is 0.92), the thickness of the N-type perovskite thin film is 80nm, the thickness ratio of the N-type perovskite thin film to the P-type perovskite thin film is 6.25, the metal electrode is an Ag electrode, and the thickness of the Ag electrode is 100 nm.
The preparation method of the homojunction perovskite photodetector comprises the following steps:
(1) spin-coating a 1-butanol solution of diisopropyl di (acetylacetonate) titanate with the concentration of 0.2M on a transparent conductive substrate at the spin-coating speed of 2500rpm, and then annealing at 450 ℃ for 40min to obtain the TiO2Dense layer of TiO2The slurry (30NR-T, Dysol) was mixed and diluted with ethanol at a mass ratio of 5:1, and then spin-coated on the resulting TiO2Annealing the surface of the compact layer at 450 ℃ for 40min to obtain TiO2A mesoporous layer, obtaining the electron transport layer;
(2) will CH3NH3X and PbX2The TiO in the step (1) is spin-coated by using a mixed solution of dimethylformamide and dimethyl sulfoxide in a volume ratio of 4:1 as a solvent2Spin coating at 4000rpm on the mesoporous layer, and heating at 100 deg.C for 10min to obtain the NPerovskite thin film of the type wherein PbX2And CH3NH3The molar weight ratio of X is 1.15: 1;
(3) vacuum vapor deposition PbX on the surface of the N-type perovskite thin film obtained in the step (2)2Then dipping it in CH3NH3In X solution to obtain the P-type perovskite film, PbX2And CH3NH3The molar weight ratio of X is 0.92;
(4) and spin-coating a chlorobenzene solution containing spiro-OMeTAD, L i-TFSI, tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III), tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) and 4-tert-butylpyridine on the surface of the P-type perovskite thin film at a spin-coating rate of 3500rpm to obtain the hole transport layer, wherein the mass ratio of spiro-OMeTAD, L i-TFSI and tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III) tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) in the chlorobenzene solution is 6.5:1:0.3, and the volume ratio of the mass of spiro-OMeTAD to 4-tert-butylpyridine is 2.6mg/m L.
(5) And (4) preparing an Ag electrode on the surface of the hole transport layer obtained in the step (4) through vacuum evaporation to obtain the homojunction perovskite photoelectric detector.
Example 3
The present example is different from example 1 in that the thickness of the N-type perovskite thin film is 480nm, the thickness of the P-type perovskite thin film is 80nm, the ratio of the thickness of the N-type perovskite thin film to that of the P-type perovskite thin film is 6, and other conditions are exactly the same as those of example 1.
The preparation method of the homojunction perovskite photoelectric detector in the embodiment is different from that in the embodiment 1 only in that the use amount of raw materials in the preparation process of the N-type perovskite thin film and the P-type perovskite thin film is adjusted to enable the structure of the N-type perovskite thin film and the P-type perovskite thin film to meet the requirements, and other conditions are completely the same as those in the embodiment 1.
Example 4
This example is different from example 1 in that the thickness of the N-type perovskite thin film is 450nm, the thickness of the P-type perovskite thin film is 90nm, the ratio of the thickness of the N-type perovskite thin film to that of the P-type perovskite thin film is 5, and other conditions are exactly the same as those in example 1.
The preparation method of the homojunction perovskite photoelectric detector in the embodiment is different from that in the embodiment 1 only in that the use amount of raw materials in the preparation process of the N-type perovskite thin film and the P-type perovskite thin film is adjusted to enable the structure of the N-type perovskite thin film and the P-type perovskite thin film to meet the requirements, and other conditions are completely the same as those in the embodiment 1.
Example 5
This example differs from example 1 in that the precursor PbX was used in the preparation of the N-type perovskite thin film2And CH3NH3The molar weight ratio of X is 1:1, and a precursor PbX in the preparation process of the P-type perovskite thin film2And CH3NH3The molar weight ratio of X was 0.93:1, and other conditions were exactly the same as in example 1.
Example 6
This example differs from example 1 in that the precursor PbX was used in the preparation of the N-type perovskite thin film2And CH3NH3The molar weight ratio of X is 1.1:1, and the precursor PbX is adopted in the preparation process of the P-type perovskite film2And CH3NH3The molar weight ratio of X was 0.91:1, and other conditions were exactly the same as in example 1.
Example 7
The present example is different from example 1 in that the transparent conductive glass is replaced with ITO transparent conductive glass, and other conditions are completely the same as those in example 1.
Example 8
This example is different from example 1 in that the electron transport layer includes only the titania dense layer and does not include the mesoporous layer, and other conditions are completely the same as those in example 1.
Comparative example 1
This comparative example differs from example 1 in that the perovskite thin film contains only intrinsic perovskite (PbX)2And CH3NH3The molar ratio of X is 1:1), the thickness thereof is equal to the sum of the thicknesses of the N-type perovskite thin film and the P-type perovskite thin film in example 1, and other conditions are exactly the same as in example 1.
The preparation method of the perovskite thin film described in the present comparative example includes the steps of:
(a) spin-coating a 1-butanol solution of diisopropyl di (acetylacetonate) titanate with the concentration of 0.15M on a transparent conductive substrate at the spin-coating speed of 2000rpm, and then annealing at 500 ℃ for 30min to obtain the TiO2Dense layer of TiO2The slurry (30NR-T, Dysol) was mixed and diluted with ethanol at a mass ratio of 6:1, and then spin-coated on the resulting TiO2Annealing the surface of the compact layer at 500 ℃ for 30min to obtain TiO2A mesoporous layer, obtaining the electron transport layer;
(b) will CH3NH3X and PbX2The TiO in the step (a) is spin-coated with a mixed solution of dimethylformamide and dimethylsulfoxide in a volume ratio of 4:12Spin-coating on the mesoporous layer at 4000rpm, and heating at 100 deg.C for 10min to obtain the intrinsic perovskite thin film, wherein PbX2And CH3NH3The molar weight ratio of X is 1: 1;
(c) and (b) spin-coating a chlorobenzene solution containing spiro-OMeTAD, L i-TFSI, tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III), tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) and 4-tert-butylpyridine on the surface of the intrinsic perovskite thin film in the step (b) at a spin-coating rate of 3500rpm to obtain the hole transport layer, wherein the mass ratio of spiro-OMeTAD, L i-TFSI and tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III) tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt) in the chlorobenzene solution is 7:1:0.25, and the volume ratio of the mass of spiro-OMeTAD to the volume ratio of 4-tert-butylpyridine is 2.41mg/m L.
(d) And (c) preparing an Au electrode on the surface of the hole transport layer obtained in the step (c) through vacuum evaporation to obtain the homojunction perovskite photoelectric detector.
The comparative example does not contain a homojunction perovskite structure, and has a response speed of 1.1ms and an EQE value of 0.5 percent.
And (3) performance testing:
the response speed and EQE values of the photodetectors in the examples and comparative examples were tested, and the test results are shown in table 1;
TABLE 1
Speed of response, ns EQE，％
Example 1 225 14.5
Example 2 150 15.8
Example 3 158 15.4
Example 4 190 15.1
Example 5 155 15.2
Example 6 218 14.6
Example 7 248 14.3
Example 8 675 13.8
The above table shows that after the photoelectric detector is optimized based on the homojunction, the response speed and the EQE value of the photoelectric detector are obviously improved, the response speed can reach below 200ns, and the EQE value can reach above 15%; compared with the perovskite photodetector without the homojunction in the comparative example 1, the response speed and the EQE value are obviously improved.
Comparing examples 1 and 3 to 4 of the present invention, it can be seen that the response speed and EQE value of the obtained photodetector are both high by controlling the thickness ratio of the N-type perovskite thin film to the P-type perovskite thin film to be in the range of 4 to 10.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. A homojunction perovskite photoelectric detector is characterized by comprising an N-type perovskite thin film and a P-type perovskite thin film which are adjacently arranged, wherein one side of the N-type perovskite thin film, which is back to the P-type perovskite thin film, is provided with an electron transmission layer, and one side of the electron transmission layer, which is back to the N-type perovskite thin film, is provided with a transparent conductive substrate; and a hole transport layer is arranged on one side of the P-type perovskite film back to the N-type perovskite film, and a metal electrode is arranged on one side of the hole transport layer back to the P-type perovskite film.
2. A homojunction perovskite photodetector as claimed in claim 1 wherein the electron transport layer comprises a dense layer and a mesoporous layer disposed adjacently, the mesoporous layer being adjacent to the N-type perovskite thin film;
preferably, the material of the compact layer is TiO2、SnO2Or ZnO;
preferably, the mesoporous layer is made of TiO2And/or Al2O3；
Preferably, the electron transport layer is prepared by solution and/or atomic layer deposition techniques.
3. The homojunction perovskite photodetector of claim 1 or 2, wherein the thickness of the N-type perovskite thin film is 400-500 nm;
preferably, the thickness of the P-type perovskite thin film is 50-100 nm;
preferably, the thickness ratio of the N-type perovskite thin film to the P-type perovskite thin film is 4-10;
preferably, the N-type perovskite thin film is prepared by a solution method and/or an evaporation method.
4. A homojunction perovskite photodetector as claimed in any one of claims 1 to 3 wherein the hole transport layer comprises at least one of spiro-OMeTAD, ptaA, CuSCN or CuPc;
preferably, the hole transport layer further comprises a lithium salt and/or a cobalt salt.
5. A homojunction perovskite photodetector as claimed in any one of claims 1 to 4 wherein the transparent conductive substrate is ITO or FTO transparent conductive glass;
preferably, the square resistance of the transparent conductive substrate is 10-25 Ω;
preferably, the transmittance of the transparent conductive substrate is 80-95%;
preferably, the metal electrode includes any one or a combination of at least two of Al, Ag, or Au.
6. A method of fabricating a homojunction perovskite photodetector as claimed in any one of claims 1 to 5, wherein the method comprises the steps of:
(1) preparing an electron transport layer on a transparent conductive substrate;
(2) preparing an N-type perovskite thin film on the surface of the electron transport layer obtained in the step (1);
(3) preparing a P-type perovskite film on the surface of the N-type perovskite film obtained in the step (2);
(4) preparing a hole transport layer on the surface of the P-type perovskite thin film obtained in the step (3);
(5) and (5) preparing a metal electrode on the surface of the hole transport layer obtained in the step (4) to obtain the homojunction perovskite photoelectric detector.
7. The method according to claim 6, wherein the step (1) of preparing an electron transport layer on a transparent conductive substrate comprises preparing a dense layer on the transparent conductive substrate, and then preparing a mesoporous layer on the surface of the obtained dense layer to obtain the electron transport layer;
preferably, the material of the compact layer is TiO2The preparation process of the compact layer comprises the steps of spin coating a titanium source solution on a transparent conductive substrate, and then annealing to obtain the compact layer;
preferably, the titanium source is at least one of diisopropyl di (acetylacetonate) titanate, titanium tetrachloride or isopropyl titanate;
preferably, the solvent of the titanium source solution is any one or the combination of at least two of 1-butanol, ethanol or isopropanol;
preferably, the concentration of the titanium source solution is 0.1-0.2M;
preferably, in the preparation process of the compact layer, the speed of spin coating is 1500-;
preferably, in the preparation process of the dense layer, the annealing temperature is 450-550 ℃, and the annealing time is 20-40 min;
preferably, in the preparation process of the compact layer, the temperature rise rate of annealing is 4-6 ℃/min;
preferably, the mesoporous layer is made of TiO2The preparation method of the mesoporous layer comprises the step of adding TiO2The slurry is coated on the surface of the compact layer in a spinning mode, and then annealing is carried out, so that the mesoporous layer is obtained;
preferably, the TiO is2Diluting the slurry by using a solvent before spin coating;
preferably, the solvent used for dilution comprises any one of ethanol, 1-butanol or isopropanol or a combination of at least two of the above;
preferably, in the preparation process of the mesoporous layer, the spin coating rate is 3500-4500 rpm;
preferably, the annealing temperature in the preparation process of the mesoporous layer is 450-;
preferably, in the preparation process of the mesoporous layer, the temperature rise rate of annealing is 4-6 ℃/min;
preferably, the method for preparing an N-type perovskite thin film in the step (2) comprises reacting CH3NH3X and PbX2The mixed solution is coated on the mesoporous layer in a spinning way and then is heated to obtain the N-type perovskite film, wherein PbX is contained in the N-type perovskite film2Molar mass of not less than CH3NH3The molar amount of X;
preferably, in the preparation process of the N-type perovskite thin film, CH3NH3X and PbX2In the mixed solution of (2) PbX2And CH3NH3The molar weight ratio of X is (1-1.15) to 1;
preferably, in the preparation process of the N-type perovskite thin film, the spin coating speed is 3500-4500 rpm;
preferably, in the preparation process of the N-type perovskite thin film, anisole is added on the surface of spin coating in the spin coating process;
preferably, the CH3NH3X and PbX2The solvent of the mixed solution is mixed solution of dimethyl formamide and dimethyl sulfoxide;
preferably, the volume ratio of the dimethyl formamide to the dimethyl sulfoxide in the mixed solution of the dimethyl formamide and the dimethyl sulfoxide is (3-5) to 1, preferably (3.5-4.5) to 1;
preferably, in the preparation process of the N-type perovskite thin film, the heating treatment temperature is 90-110 ℃, and the heating treatment time is 8-12 min;
preferably, the method for preparing the P-type perovskite thin film in the step (3) comprises the step of carrying out vacuum vapor deposition PbX on the surface of the N-type perovskite thin film obtained in the step (2)2Then dipping it in CH3NH3Obtaining the P-type perovskite film in an X solution, wherein PbX is2Is less than CH3NH3The molar amount of X;
preferably, PbX is adopted in the preparation process of the P-type perovskite thin film2And CH3NH3The molar weight ratio of X is 0.89-0.93;
preferably, the CH3NH3The solvent of the X solution is isopropanol;
preferably, the preparation method of the hole transport layer in the step (4) comprises spin-coating a solution containing spiro-OMeTAD on the surface of the P-type perovskite thin film to obtain the hole transport layer;
preferably, the solvent of the spiro-OMeTAD containing solution comprises chlorobenzene;
preferably, the solution containing spiro-OMeTAD also comprises lithium salt and cobalt salt;
preferably, the lithium salt comprises L i-TFSI;
preferably, the cobalt salt comprises tris [ 4-tert-butyl-2- (1H-pyrazol-1-yl) pyridine ] cobalt (III) tris (1,1, 1-trifluoro-N- [ (trifluoromethyl) sulfonyl ] methanesulfonamide salt);
preferably, the solution comprising spiro-OMeTAD further comprises 4-tert-butylpyridine;
preferably, in the preparation process of the hole transport layer, the rotation speed of spin coating is 3250 and 3750 rpm;
preferably, the metal electrode in the step (5) is prepared by a vacuum evaporation method;
preferably, the pressure of the vacuum evaporation is less than 10-4Pa。
8. The method of claim 6 or 7, comprising the steps of:
(1) preparing an electron transport layer on a transparent conductive substrate, wherein the preparation process comprises spin coating a titanium source solution on the transparent conductive substrate, and annealing to obtain TiO2Dense layer, then on the resulting TiO2Surface spin coating TiO of compact layer2Slurry and annealing to obtain TiO2A mesoporous layer, obtaining the electron transport layer;
(2) preparing an N-type perovskite thin film on the surface of the electron transport layer obtained in the step (1), wherein the N-type perovskite thin film comprises reacting CH3NH3X and PbX2Spin coating the TiO in step (1) with the mixed solution of2Heating at 90-110 deg.C for 8-12min to obtain the N-type perovskite thin film, wherein PbX is added2And CH3NH3The molar weight ratio of X is (1-1.15) to 1;
(3) preparing a P-type perovskite thin film on the surface of the N-type perovskite thin film obtained in the step (2), wherein PbX is subjected to vacuum vapor deposition on the surface of the N-type perovskite thin film obtained in the step (2)2Then dipping it in CH3NH3In X solution to obtain the P-type perovskite film, PbX2And CH3NH3The molar weight ratio of X is 0.89-0.93;
(4) preparing a hole transport layer on the surface of the P-type perovskite thin film obtained in the step (3), wherein the hole transport layer is obtained by spin-coating a solution containing spiro-OMeTAD, lithium salt, cobalt salt and 4-tert-butylpyridine on the surface of the P-type perovskite thin film;
(5) and (4) preparing a metal electrode on the surface of the hole transport layer obtained in the step (4) through vacuum evaporation to obtain the homojunction perovskite photoelectric detector.
9. Use of a homojunction perovskite photodetector as claimed in any one of claims 1 to 5 for machine vision, biosensing and imaging or optical communication.
10. Use of homojunction perovskites in photodetectors, characterized in that the structure of the homojunction perovskites consists of an N-type perovskite thin film and a P-type perovskite thin film disposed adjacently, and the structure of the photodetectors obtained by applying the homojunction perovskites in photodetectors is as claimed in any one of claims 1 to 5.
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Application publication date: 20200717