CN113314673A - Perovskite photoelectric detector based on Mg ion doped hole transport layer and preparation method thereof - Google Patents
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Abstract
The invention relates to the technical field of photoelectric detectors, in particular to a perovskite photoelectric detector based on an Mg ion doped hole transport layer and a preparation method thereof. A perovskite photoelectric detector based on a Mg ion doped hole transport layer mainly comprises a substrate, a conductive anode, a hole transport layer, a perovskite photoactive layer, an electron transport layer, a modification layer and a metal cathode which are sequentially arranged, wherein the chemical formula of the material of the hole transport layer is NixMg1–xO, wherein x is more than 0 and less than 1. The invention uses a solution treatment mode, Mg ions are doped into the nickel oxide solution, and the Mg ions replace part of Ni ions to form NixMg1–xAnd O crystal lattice. The preparation process is simple, and the device cost is greatly reduced. And the doped device improves the carrier extraction of the hole transport layerThe quantum efficiency, the detectivity and the responsivity in the visible light range are improved.
Description
Technical Field
The invention relates to the technical field of photoelectric detectors, in particular to a perovskite photoelectric detector based on an Mg ion doped hole transport layer and a preparation method thereof.
Background
The photoelectric detector is a photoelectric device capable of converting optical signals into electric signals, and has wide application in the fields of video imaging, space optical communication, chemical/biological sensing, environment monitoring, space exploration, safety, night vision, motion detection and the like. Currently, commercial photodetector materials are predominantly inorganic semiconductors, including Si, GaN, InGaAs, and ZnO. These devices have a broad spectral response and high detectivity due to their excellent optical and electrical properties. However, the device manufacturing process is complicated and expensive, and requires metal organic chemical vapor deposition or the like. In recent years, researches show that the organic metal trihalide perovskite material has excellent photoelectric properties, can adjust band gap by exchanging atomic compositions, has the advantages of strong broadband absorption, high carrier mobility, long carrier diffusion length and the like, and is expected to become a next-generation solar cell due to the simple structure and manufacturing process of the perovskite solar cell and the rapid development in recent years. The conversion efficiency of the method achieves breakthrough increase from the initial 3.8% to the latest 25.5%. These advantages also make the emerging perovskite materials promising as replacements for conventional semiconductor materials used in detectors. In short, organic-inorganic hybrid perovskites are expected to be useful for rapid light detection. However, the contact property, the charge accumulation, the extraction and the transmission capability of the interface of the hole transmission layer and the perovskite layer at present are a great problem influencing the development of the perovskite detector, and the dark current of the device is still higher, so that the overall detection efficiency of the device is lower.
Disclosure of Invention
To solve the above problems, it is an object of the present invention to provide a perovskite photodetector based on a Mg ion-doped hole transport layer, which employs a simple solution process of Mg ion-doped nickel oxide as a hole transport layer.
The purpose of the invention is realized by the following technical scheme:
a perovskite photoelectric detector based on a Mg ion doped hole transport layer mainly comprises a substrate, a conductive anode, a hole transport layer, a perovskite photoactive layer, an electron transport layer, a modification layer and a metal cathode which are sequentially arranged, wherein the chemical formula of the material of the hole transport layer is NixMg1–xO, wherein x is more than 0 and less than 1.
Preferably, the chemical formula NixMg1–xThe value of x in O is more than 0.96 and less than 1.
Preferably, the thickness of the hole transport layer material is 20-40 nm.
Preferably, the substrate is a glass substrate or a PET plastic substrate; the conductive anode material is ITO or FTO.
Preferably, the material of the perovskite photoactive layer is MAPbI3The thickness is 400-550 nm;
the electron transport layer material is C60、C60Any one of the derivatives, the double fullerene or the double fullerene derivative, wherein the thickness is 20-40 nm;
the material of the decorative layer is BCP, and the thickness is 8-10 nm;
the metal cathode is one or more of Al, Ag or Cu, and the thickness of the metal cathode is 80-100 nm.
Another object of the present invention is to provide a method for preparing a perovskite photodetector based on a Mg ion doped hole transport layer, the method comprising the steps of:
1) cleaning, drying and ultraviolet ozone treatment are carried out on a substrate consisting of a substrate and a conductive anode;
2) gradient spin coating Ni on the substrate surfacexMg1–xCarrying out gradient annealing on the O solution to obtain a hole transport layer;
3) gradient spin coating MAPbI on the hole transport layer3Annealing the precursor solution to obtain a perovskite photoactive layer;
4) evaporating and plating an electron transport layer on the perovskite light active layer;
5) and sequentially evaporating a modification layer and a metal cathode on the electron transmission layer to obtain the required perovskite photoelectric detector.
Preferably, the cleaning in the step 1) is ultrasonic cleaning of the substrate by using a detergent, an acetone solution, isopropyl alcohol, alcohol and deionized water in sequence, wherein each ultrasonic cleaning is performed for 10-20 minutes.
Preferably, Ni is as defined in step 2)xMg1–xThe total molar concentration of the O solution is 1 mmol/mL;
the procedure of the gradient spin coating is as follows: spin-coating at 2000-3000 rpm for 10-20 s, and changing the rotation speed to 5000-6000 rpm for 45-60 s;
the gradient annealing comprises the following steps: annealing at 140-160 ℃ for 3-7 min and at 280-300 ℃ for 25-35 min.
Preferably, the MAPbI in step 3)3The total concentration of the precursor solution is 610-915mg/mL, and PbI2The molar ratio to MAI is 1: 1; the procedure of the gradient spin coating is as follows: spin-coating at 2000-3500 rpm for 10-15 s, changing the rotation speed to 4000-6000 rpm for 50-55 s, wherein the annealing temperature is 100 ℃ and the annealing time is 20 min.
Preferably, the vapor deposition in steps 4) and 5) is vacuum vapor deposition, and the air pressure in the vacuum vapor deposition machine is controlled to be less than 5 × 10-4Pa。
In summary, compared with the prior art, the invention has the following beneficial effects:
1. the device dark current is low. Book (I)According to the invention, the Mg ion doped nickel oxide is used as the hole transport layer, so that the carrier transport capability of the hole transport layer is improved, the leakage current in the device operation is reduced, and the dark current is greatly reduced. The device prepared by the method has low dark current density which can reach 2.2 multiplied by 10 under-0.1V bias-9A/cm2。
2. The external quantum efficiency is high. The technology of doping nickel oxide with Mg ions as a hole transport layer is favorable for promoting the growth of perovskite, increasing the grain size and improving the quality of a perovskite film, so that the absorption and conversion of light are enhanced, and the external quantum efficiency is up to 88.1% under the bias of 0V.
3. The device has high responsivity and detectivity. The technology of taking Mg ion doped nickel oxide as the hole transport layer is beneficial to improving and improving the contact and charge accumulation of the interface of the hole transport layer and the perovskite layer and the extraction and transmission capability of the hole transport layer, thereby improving the responsivity of the device, the responsivity and the detectivity of the prepared device are high, the responsivity can reach 0.41A/W under 0V bias voltage, and the detectivity can reach 0.56 multiplied by 1014Jones。
Drawings
Fig. 1 is a graph of dark current density of the perovskite photodetector based on Mg ion-doped nickel oxide as a hole transport layer obtained in example 1.
Fig. 2 is a graph of the external quantum efficiency at 0V bias for the perovskite photodetector based on Mg ion-doped nickel oxide as a hole transport layer obtained in example 1.
Fig. 3 is the spectral responsivity at 0V bias of the perovskite photodetector based on Mg ion doped nickel oxide as the hole transport layer obtained in example 1.
Fig. 4 shows the detectivity of the perovskite photodetector based on Mg ion-doped nickel oxide as a hole transport layer obtained in example 1 at a bias voltage of 0V.
Fig. 5 is a graph showing dark current density of the perovskite photodetector based on nickel oxide as a hole transport layer obtained in comparative example 1.
Fig. 6 is a graph of the external quantum efficiency at 0V bias for the perovskite photodetector based on nickel oxide as a hole transport layer obtained in comparative example 1.
Fig. 7 is a graph showing the spectral responsivity at 0V bias of the perovskite photodetector based on nickel oxide as a hole transport layer obtained in comparative example 1.
Fig. 8 shows the detectivity of the perovskite photodetector based on nickel oxide as a hole transport layer obtained in comparative example 1 at a bias of 0V.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. In addition, various modifications may occur to those skilled in the art upon reading the present disclosure, and such equivalent variations are within the scope of the present invention as defined in the appended claims.
The following embodiment provides a perovskite photoelectric detector based on Mg ion doped nickel oxide as a hole transport layer, which comprises a substrate, a conductive anode, a hole transport layer, a perovskite photoactive layer, an electron transport layer, a modification layer and a metal cathode which are sequentially arranged from bottom to top, wherein the chemical formula of the material of the hole transport layer is NixMg1–xO, the thickness of the film layer is 20-40 nm.
Example 1
A preparation method of a perovskite photoelectric detector based on Mg ion doped nickel oxide as a hole transport layer comprises the following steps:
(1) selecting glass as a substrate, using ITO as a conductive anode, and sequentially cleaning and pretreating a substrate consisting of the substrate and the conductive anode, wherein the cleaning and pretreating method comprises the following steps: sequentially putting a substrate into a detergent, an acetone solution, isopropyl alcohol, alcohol and deionized water for ultrasonic treatment for 15min, cleaning, blow-drying by using nitrogen, drying, and treating the surface of the substrate by using ultraviolet ozone for later use;
(2) 99 mol% of nickel nitrate hexahydrate and 1 mol% of MgCl2Dissolving in mixed solvent of ethylenediamine and ethylene glycol at a solvent volume ratio of 14:1 and a total solution molar concentration of 1mmol/mL at 70 deg.C for 2 hr to obtain Ni0.99Mg0.01And O, mixing the solution. The dissolved mixed solution was spin coated on a substrate using the following spin coating procedure: the spin speed was changed to 3000rpm for 12s spin, and then to 6000rpm for 50s spin. After the spin coating is finished, the substrate is subjected to gradient annealing, and the annealing conditions are as follows: annealing at 150 deg.C for 5min, and annealing at 280 deg.C for 30 min. And annealing to obtain the Mg ion doped hole transport layer.
(3) Transferring the substrate with the spin-coated hole transport layer into a glove box, weighing 1-1.5mmol of lead iodide and 1-1.5mmol of iodomethylamine solution (molar ratio is 1:1) in a mixed solvent of 1mLN, N-dimethylformamide and dimethyl sulfoxide (volume ratio is 9:1) to obtain perovskite MAPbI with the total solution concentration of 610-915mg/mL3Precursor solution, adding MAPbI3The precursor solution is spin-coated on the hole transport layer, and the spin-coating procedure is as follows: the spin speed was changed to 3000rpm for 10s, followed by 5000rpm for 50 s. Then annealing the substrate at 100 ℃ for 20min to prepare a perovskite photoactive layer;
(4) placing the substrate with anode, hole transport layer and perovskite layer into evaporation chamber of high vacuum evaporation plating machine, and evaporating electron transport layer C with thickness of 30nm on perovskite photoactive layer60；
(5) The pressure in the vacuum evaporator was 4.5X 10-4Under the Pa high vacuum environment, a modification layer BCP (copper bath) is evaporated on the electron transmission layer, the thickness of the film is controlled to be 8-10 nm, finally a copper electrode is evaporated, the thickness of the film is controlled to be 80-100 nm, and the structure of the substrate/ITO/Ni is finally obtained0.99Mg0.01O/CH3NH3PbI3/C60a/BCP/Cu perovskite photodetector. As shown in FIGS. 1 to 4, the dark current of the perovskite photodetector obtained in this example under a bias of-0.1V was 2.2X 10-9A/cm2The external quantum efficiency is up to 88.1%, the responsivity of the device at 640nm is 0.41A/W, and the highest detectivity is 0.56 multiplied by 1014Jones。
Example 2
Referring to example 1, only step (2) was changed to 98 mol% nickel nitrate hexahydrate with 2 mol% MgCl2Dissolving in mixed solvent of ethylenediamine and ethylene glycol, and obtaining the liner with the structure by the same process parameter conditions as example 1bottom/ITO/Ni0.98Mg0.02O/CH3NH3PbI3/C60a/BCP/Cu perovskite photodetector. The external quantum efficiency of the device under 0V bias reaches 83.4%, and the responsivity at 640nm is 0.38A/W.
Example 3
Referring to example 1, only step (2) was changed to 97 mol% nickel nitrate hexahydrate with 3 mol% MgCl2Dissolving in mixed solvent of ethylenediamine and ethylene glycol, and obtaining substrate/ITO/Ni with the same conditions of other process parameters as those in example 10.97Mg0.03O/CH3NH3PbI3/C60a/BCP/Cu perovskite photodetector. The external quantum efficiency of the device under 0V bias reaches 83.1%, and the responsivity at 640nm is 0.39A/W.
Example 4
Referring to example 1, the anode material in step (1) was changed to FTO, and other process parameters and conditions were the same as those in example 1, to obtain a substrate/FTO/Ni structure0.99Mg0.01O/CH3NH3PbI3/C60a/BCP/Cu perovskite photodetector. The device has low dark current and high external quantum efficiency.
Example 5
Referring to example 1, only the electron transport layer C in step (4)60Modified to (6,6) -phenyl-C61-butyric acid methyl ester (PC)61BM) and other process parameter conditions are the same as those in example 1 to obtain ITO/Ni0.99Mg0.01O/CH3NH3PbI3/PC61BM/BCP/Cu perovskite photodetectors. The device has low dark current and high external quantum efficiency.
Comparative example 1
In order to verify the performance of the perovskite photoelectric detector based on Mg ion doped nickel oxide as a hole transport layer, a Mg ion material is not introduced into the hole transport layer of the comparative example, the hole transport layer is a single nickel oxide material, and the preparation steps are as follows:
(1) selecting glass as a substrate, using ITO as a conductive anode, and sequentially cleaning and pretreating a substrate consisting of the substrate and the conductive anode, wherein the cleaning and pretreating method comprises the following steps: sequentially putting a substrate into a detergent, an acetone solution, isopropyl alcohol, alcohol and deionized water for ultrasonic treatment for 15min, cleaning, blow-drying by using nitrogen, drying, and treating the surface of the substrate by using ultraviolet ozone for later use;
(2) dissolving nickel nitrate hexahydrate in a mixed solvent of ethylenediamine and ethylene glycol, wherein the volume ratio of the solvent is 14:1, the total concentration of the solution is 1mmol/mL, dissolving for 2 hours at 70 ℃ to obtain a nickel oxide precursor solution, and spin-coating the dissolved precursor solution on a substrate by using the following spin-coating procedures: the spin speed was changed to 3000rpm for 12s spin, and then to 6000rpm for 50s spin. After the spin coating is finished, the substrate is subjected to gradient annealing, and the annealing conditions are as follows: annealing at 150 deg.C for 5min, and annealing at 280 deg.C for 30 min. Annealing to obtain a hole transport layer;
(3) transferring the substrate with the spin-coated hole transport layer into a glove box, weighing 1-1.5mmol of lead iodide and 1-1.5mmol of iodomethylamine solution (molar ratio is 1:1) in a mixed solvent of 1mLN, N-dimethylformamide and dimethyl sulfoxide (volume ratio is 9:1) to obtain perovskite MAPbI with the total solution concentration of 610-915mg/mL3Precursor solution, adding MAPbI3The precursor solution is spin-coated on the hole transport layer, and the spin-coating procedure is as follows: the spin speed was changed to 3000rpm for 10s, followed by 5000rpm for 50 s. Then annealing the substrate at 100 ℃ for 20min to prepare a perovskite photoactive layer;
(4) placing the substrate with anode, hole transport layer and perovskite layer into evaporation chamber of high vacuum evaporation plating machine, and evaporating electron transport layer C with thickness of 30nm on perovskite photoactive layer60；
(5) The pressure in the vacuum evaporator was 4.5X 10-4Evaporating and plating a modification layer BCP on the electron transmission layer under a Pa high-vacuum environment, controlling the film thickness to be 8-10 nm, finally evaporating and plating a copper electrode, controlling the film thickness to be 80-100 nm, and finally obtaining the substrate/ITO/NiO/CH3NH3PbI3/C60a/BCP/Cu perovskite photodetector. As shown in FIGS. 5 to 8, the dark current density of the perovskite photodetector obtained in the comparative example was 5.7X 10 at a bias of-0.1V-9A/cm2External quantum efficiency80.0%, the responsivity of the device at 640nm is 0.37A/W, and the highest detectivity is 0.49 multiplied by 1014Jones。
And (4) conclusion: according to the test data of the embodiment and the comparative example, the Mg ions are doped in the hole transport layer of the perovskite photoelectric detector, so that the dark current can be reduced, the external quantum efficiency is improved, and the responsivity and the detection rate of the device are improved.
Claims (10)
1. The perovskite photoelectric detector based on the Mg ion doped hole transport layer is characterized by mainly comprising a substrate, a conductive anode, a hole transport layer, a perovskite light active layer, an electron transport layer, a modification layer and a metal cathode which are sequentially arranged, wherein the chemical formula of the material of the hole transport layer is NixMg1–xO, wherein x is more than 0 and less than 1.
2. The Mg ion doped hole transport layer based perovskite photodetector of claim 1, wherein the formula NixMg1–xThe value of x in O is more than 0.96 and less than 1.
3. The perovskite photodetector based on the Mg ion doped hole transport layer according to claim 1, wherein the thickness of the hole transport layer material is 20-40 nm.
4. A Mg ion doped hole transport layer based perovskite photodetector as claimed in any of claims 1 to 3 wherein said substrate is a glass substrate or a PET plastic substrate; the conductive anode material is ITO or FTO.
5. A Mg ion doped hole transport layer based perovskite photodetector as claimed in any of claims 1 to 3, characterized in that the material of the perovskite photoactive layer is MAPbI3The thickness is 400-550 nm;
the electron transport layer material is C60、C60Derivatives, bis-fullerenes or bisAny one of fullerene derivatives with the thickness of 20-40 nm;
the material of the decorative layer is BCP (bathocuproine), and the thickness is 8-10 nm;
the metal cathode is one or more of Al, Ag or Cu, and the thickness of the metal cathode is 80-100 nm.
6. The method for preparing a perovskite photodetector based on a Mg ion doped hole transport layer as claimed in claim 1, characterized in that the method comprises the following steps:
1) cleaning, drying and ultraviolet ozone treatment are carried out on a substrate consisting of a substrate and a conductive anode;
2) gradient spin coating Ni on the substrate surfacexMg1–xCarrying out gradient annealing on the O solution to obtain a hole transport layer;
3) gradient spin coating MAPbI on the hole transport layer3Annealing the precursor solution to obtain a perovskite photoactive layer;
4) evaporating and plating an electron transport layer on the perovskite light active layer;
5) and sequentially evaporating a modification layer and a metal cathode on the electron transmission layer to obtain the required perovskite photoelectric detector.
7. The preparation method of the perovskite photodetector based on the Mg ion doped hole transport layer according to claim 6, wherein the cleaning in the step 1) is ultrasonic cleaning of the substrate by using a detergent, an acetone solution, isopropyl alcohol, alcohol and deionized water in sequence, and each ultrasonic cleaning is carried out for 10-20 minutes.
8. The method for preparing perovskite photodetector based on Mg ion doping hole transport layer according to claim 6, Ni in step 2)xMg1–xThe total molar concentration of the O solution is 1 mmol/mL; the procedure of the gradient spin coating is as follows: spin-coating at 2000-3000 rpm for 10-20 s, and changing the rotation speed to 5000-6000 rpm for 45-60 s;
the gradient annealing comprises the following steps: annealing at 140-160 ℃ for 3-7 min and at 280-300 ℃ for 25-35 min.
9. The method of claim 6, wherein the MAPbI is applied in step 3)3The total concentration of the precursor solution is 610-915mg/mL, and PbI2The molar ratio to MAI is 1: 1;
the procedure of the gradient spin coating is as follows: spin-coating at 2000-3500 rpm for 10-15 s, and changing the rotation speed to 4000-6000 rpm for 50-55 s;
the annealing temperature is 100 ℃, and the annealing time is 20 min.
10. The method for preparing a perovskite photodetector based on a Mg ion doping hole transport layer according to claim 6, wherein the evaporation in the steps 4) and 5) is vacuum evaporation, and the air pressure in the vacuum evaporation machine is controlled to be less than 5 x 10-4Pa。
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| CN113790744A (en) * | 2021-09-10 | 2021-12-14 | 华能新能源股份有限公司 | Optical detection method and optical detector |
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