CN113193127B - Ytterbium and erbium co-doped perovskite film and application thereof in photoelectric detector - Google Patents

Ytterbium and erbium co-doped perovskite film and application thereof in photoelectric detector Download PDF

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CN113193127B
CN113193127B CN202110495278.0A CN202110495278A CN113193127B CN 113193127 B CN113193127 B CN 113193127B CN 202110495278 A CN202110495278 A CN 202110495278A CN 113193127 B CN113193127 B CN 113193127B
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张华芳
侯素敏
毛艳丽
杨溢
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Henan University
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Abstract

The invention discloses an ytterbium and erbium co-doped perovskite film and application thereof in a photoelectric detector, wherein the perovskite film is prepared by the following steps: (1) mixing BAI, FAI and PbI2Dissolving in DMF, stirring at room temperature, and standing to obtain solution A; (2) yb of2O3Dissolving the powder in water, heating to 90-110 deg.C, adding concentrated HCl until the solution becomes clear and evaporated to dryness to obtain YbCl3Powdering, mixing YbCl3Dissolving the powder in water to obtain YbCl3The aqueous solution B of (1); (3) er according to the method of step (2)2O3Preparation of ErCl powder3Powder of ErCl3Dissolving the powder in water to obtain ErCl3The aqueous solution C of (1); (4) adding the solution B and the solution C with the same volume into the solution A and stirring to obtain a solution D; (5) preheating the silicon wafer, dripping the solution D on the silicon wafer, spin-coating and drying to obtain the ytterbium and erbium co-doped film.

Description

Ytterbium and erbium co-doped perovskite film and application thereof in photoelectric detector
Technical Field
The invention belongs to the field of photoelectric detectors, and particularly relates to an ytterbium and erbium co-doped perovskite thin film and application thereof in a photoelectric detector.
Background
In recent years, three-dimensional organic-inorganic hybrid metal halide perovskites have attracted researchers' interest in the photovoltaic and optoelectronic fields (e.g., solar cells, light emitting diodes, and photodetectors) due to large absorption coefficients, high carrier mobilities, small exciton binding energies, and long charge carrier diffusion lengths. However, the most significant disadvantage of these three-dimensional perovskite materials is poor stability, especially in humid and high temperature environments. Compared with three-dimensional perovskite, the quasi-two-dimensional perovskite has better stability and better compatibility with other functional layers for assembling photovoltaic or photoelectric devices, and is a new material in the photovoltaic field. However, the lifetime of the photoluminescence composite is far shorter than that of a single crystal perovskite crystal due to crystal lattice defects caused by the perovskite in the preparation process (such as a substrate, the stoichiometry of a precursor, annealing time and temperature), particularly grain boundaries and intragranular defects. The presence of defects during application can significantly reduce the efficiency of the device. Therefore, the method for reducing the defects of the two-dimensional perovskite thin film is of great significance for expanding the application field of the two-dimensional perovskite material.
Disclosure of Invention
In view of the above, the present invention is directed to provide an ytterbium and erbium co-doped perovskite thin film and its application in a photodetector. Yb of the invention3+And Er3+Co-doped perovskite thin film effectively reduces two-dimensional perovskite material BA2FAPb2I7A method of defect luminescence. BA to be optimized2FAPb2I7The film is used as a light absorption material to prepare a photoelectric detector, and obtains excellent photoelectric properties.
In order to achieve the above object, the present invention provides the following technical solutions:
an ytterbium and erbium co-doped perovskite thin film, which is obtained by the following process:
(1) preparation of solution A
Mixing BAI, FAI and PbI2Dissolving the materials into DMF according to a molar ratio of 2:1:2, stirring for 5-7 h at room temperature, and standing for at least 2h to obtain a solution A;
(2) preparation of solution B
Yb of2O3Dissolving the powder in water, heating to 90-110 ℃, adding a concentrated HCl solution until the solution becomes clear, and evaporating to dryness at 145-155 ℃ to obtain YbCl3Powdering, mixing YbCl3Dissolving the powder in water to obtain YbCl3The aqueous solution B of (1);
(3) preparation of solution C
Adding Er2O3Dissolving the powder in water, heating to 90-110 ℃, and adding the concentrateThe HCl solution becomes clear until the solution becomes clear, and the ErCl is obtained by evaporating to dryness at 145-155 DEG C3Powder of ErCl3Dissolving the powder in water to obtain ErCl3The aqueous solution C of (1);
(4) preparation of solution D
Adding the solution B and the solution C with equal volumes into the solution A, and stirring for 3-5 hours to obtain a solution D;
(5) crystallization of
Preheating a silicon wafer with a single surface oxidized at 117-123 ℃ for 15-25 min, dripping the solution D on the silicon wafer, spin-coating, placing the spin-coated film at 117-123 ℃ and drying for 15-25 min to obtain the ytterbium and erbium co-doped BA2FAPb2I7A film.
Further, in the step (4), the doping amount of Yb is BA2FAPb2I75-15% of mole number, and the doping amount of Er is BA2FAPb2I70.5-1.5% of the mole number, and the molar ratio of Yb to Er is 10: 1.
Further, every 0.1mmol FAI in step (1) needs to be dissolved in 1mLDMF, and YbCl in the aqueous solution B in step (2)3ErCl in the aqueous solution C of step (3) at a concentration of 1mmol/ml3The concentration was 0.1 mmol/ml.
Further, in the step (4), the area of the silicon wafer is 2cm multiplied by 2cm, and the spin coating amount of the solution D is 60-100 mu L.
The perovskite film co-doped with ytterbium and erbium is put on a high-vacuum resistance evaporation coating machine for evaporation coating of interdigital electrodes, and the pressure intensity of a vacuum chamber is 5 multiplied by 10 when the coating machine works-5Pa, the thickness of the Au electrodes is 80nm, and the width between the Au electrodes is 100 μm.
The invention has the following advantages:
(1) the invention can greatly reduce the defects of materials and adjust the flatness of the film as shown in figures 1 and 2. The energy loss can be effectively reduced in the aspect of application devices.
(2) The preparation process is simple and is more beneficial to large-scale commercial production.
(3) Mixing BA2FAPb2I7Film as light absorbing layerThe perovskite solar photoelectric detector is applied to the perovskite solar photoelectric detector, and excellent photoresponse performance is obtained.
Drawings
FIG. 1 undoped BA2FAPb2I7Absorption and fluorescence spectra of the film, excitation wavelength 405 nm;
FIG. 2 undoped BA2FAPb2I7The change of the fluorescence spectrum of the film with the temperature is (a) 80-280K, (b)300-380K, and the excitation wavelength is 405 nm;
FIG. 3 shows the co-doping ratios of ytterbium and erbium (BA) in example 12FAPb2I7Respectively at a wavelength of 405 nm;
FIG. 4 (a), (b), (c) and (d) shows Yb/Er doping amounts of 0%/0%, 5%/0.5%, 10%/1% and 15%/1.5% (BA)2FAPb2I7SEM image of perovskite thin film, (e) Yb/Er (BA) doped 10%/1%2FAPb2I7Energy spectra of perovskite thin films.
In fig. 5: (a) schematic structural diagram of photoelectric detector, (b) pure BA2FAPb2I7Perovskite is at 0.3uW/cm2To 8mW/cm2Illumination I-V curves. The (c) photocurrent and light intensity relation of perovskite photoelectric detectors doped with different concentrations, (d) responsivity and irradiance dependence relation, and (e) detectivity changes with the variation of irradiance. The test bias was 2V.
FIG. 6 example 2 BA doping with different Yb levels2FAPb2I7Fluorescence spectrum of the film, excitation wavelength 405 nm;
FIG. 7 example 3 BA doped with different amounts of Er2FAPb2I7Fluorescence spectrum of the film, excitation wavelength 405 nm.
Detailed Description
The technical solutions of the present invention are further described in detail below with reference to the drawings and examples, but the scope of the present invention is not limited thereto.
The doping amounts in the following examples each refer to a doping molar amount.
Example 1
Yb (Yb)3+And Er3+Co-doped BA2FAPb2I7The perovskite film is prepared by the following steps:
(1) preparation of solution A
0.2mmol of BAI, 0.1mmol of FAI and 0.2mmol of PbI2Dissolving in 1ml of DMF, stirring for 6 hours at room temperature, and standing for 2 hours to obtain a solution A;
(2) preparation of solution B
Mixing 10mmol of Yb2O3The powder was dissolved in water and when the temperature was raised to 100 ℃, excess concentrated HCl solution (37 wt%, gumbo) was added until the solution became clear. Evaporating to dryness at 150 ℃ to obtain YbCl3Powder, YbCl prepared in 20ml of ultrapure water to a concentration of 1mmol/ml3The aqueous solution B of (1).
(3) Preparation of solution C
Adding 1mmol Er2O3The powder was dissolved in water and when the temperature was raised to 100 ℃, excess concentrated HCl solution (37 wt%, gumbo) was added until the solution became clear. Evaporating to dryness at 150 ℃ to obtain ErCl3Powder, ErCl prepared in 20ml ultrapure water to a concentration of 0.1mmol/ml3Aqueous solution C of (1).
(4) Preparation of solution D
Preparation of 0%/0%, 5%/0.5%, 10%/1%, and 15%/1.5% Yb/Er doping amount precursors:
preparing a solution with Yb/Er doping amount of 0%/0%: 1ml of A solution was stirred for 4 h.
Preparing a solution with Yb/Er doping amount of 5%/0.5%: add 5. mu. L B solution and 5. mu. L C solution to 1ml of solution A and stir for 4 h.
Preparing a solution with Yb/Er doping amount of 10%/1%: add 10. mu. L B solution and 10. mu. L C solution to 1ml of A solution and stir for 4 h.
Preparing a solution with Yb/Er doping amount of 15%/1.5%: add 15. mu. L B solution and 15. mu. L C solution to 1ml of solution A and stir for 4 h.
(5) Crystallization of
A silicon wafer with one oxidized surface (the area is 2cm multiplied by 2cm, single polishing is carried out, and the thickness is 300 nm SiO)2Layer, single-side oxidation, combined fertilizer and crystal material technology Co., Ltd.) was preheated for 20min on a heating plate at 120 deg.C, and 80 μ LYb/Er doped was taken outPrecursor solutions D with the impurity contents of 0%/0%, 5%/0.5%, 10%/1%, and 15%/1.5%, respectively, were dropped onto the silicon wafer at a rotation speed of 3000rpm for a period of 30 seconds. The spin-coated film is placed on a heating plate at 120 ℃ and heated for 20min to obtain BA with Yb/Er doping molar amounts of 0%/0%, 5%/0.5%, 10%/1% and 15%/1.5%2FAPb2I7A film. The whole process is completed in a glove box.
FIG. 1 is an undoped BA2FAPb2I7Absorption and fluorescence spectra of the thin film. The fluorescence peak having a wavelength of about 780nm has no absorption peak corresponding thereto. FIG. 2 is an undoped BA2FAPb2I7The fluorescence spectra of the film at different temperatures show that the fluorescence peak gradually decreases with increasing temperature, indicating that the peak is a defect luminescence peak. FIG. 3 is BA after co-doping with different Yb/Er contents2FAPb2I7As can be seen from the graph, the luminescence intensity of the defect near 780nm decreases and then increases with the increase of the doping content, and the intensity of the previous phonon peak increases and then decreases. When the doping amount of Yb/Er is 10%/1%, the defect luminescence completely disappears, indicating effective defect suppression. FIG. 4 is a diagram showing BA co-doped with Yb/Er of different contents2FAPb2I7According to the scanning electron microscope picture of the thin film, when the doping amount of Yb/Er is 10%/1%, the hollow holes of the thin film are the least, and the surface is the smoothest.
(6) Based on optimized two-dimensional perovskite BA2FAPb2I7Method for preparing photoelectric detector
BA with the doping amounts of the crystallized Yb/Er of 0%/0%, 5%/0.5%, 10%/1% and 15%/1.5% respectively2FAPb2I7The perovskite film is placed on a high vacuum resistance evaporation coating machine for evaporation coating of interdigital electrodes, and the pressure intensity of the vacuum chamber is 5 multiplied by 10 when the coating machine works-5Pa. The thickness of the Au electrodes is 80nm, and the width between the Au electrodes is 100 μm. The planar structure is Au-BA2FAPb2I7-Au. As shown in fig. 5 (a).
FIG. 5 (b) shows the optical power of a pure two-dimensional layered perovskite photodetector in the dark and at a wavelength of 450nmThe density is 0.3uW/cm2To 8mW/cm2I-V curve under laser irradiation. Under dark conditions, the current is linear with the bias voltage (I-V), which qualitatively shows that only a relatively small potential barrier exists between the perovskite and the electrode, which is beneficial for collecting the photo-generated carriers. At a voltage bias of 2v, the current of pure perovskites is as low as about 5X 10−11 A, and Yb doped at 5%/0.5% and 10%/1%3+ / Er3+Has a dark current of 1X 10−11 A (not shown in the figure). Dark current represents leakage current resulting from carrier recombination in the device, with lower dark current indicating more photocurrent will flow through the device, thereby reducing charge recombination.
The pure perovskite is biased at 2V and is 8mW/cm2Light-to-dark ratio under illumination conditions of 6X 102. The light/dark ratio of doped perovskite photodetectors is 8 x 103 (Yb 3+5% and Er3+0.5%) and 1 × 10%4 (Yb 3+10% and Er3+1.0%) (not shown in the figure).
In FIG. 5 (c), the photocurrent at different illumination intensities, it can be seen that the current continues to increase with increasing light intensity, wherein Yb is doped3+ 10%，Er 3+ At 1%, the current increase was greatest. This indicates that 10% Yb is doped3+And 1% Er3+The detector response to light is maximal. For photoconductive PDs, the optical responsivity and the detectivity are also important parameters determining the sensitivity of PDs. As can be seen from fig. 5 (d) and 5 (e), the photoresponsiveness and the detectivity decrease as the light intensity increases. Under the bias of 2V, the light responsivity is 181 mA/W (pure BA)2FAPb2I7) 333 mA/W (doped with 5% Yb)3+、0.5%Er3+) 555 mA/W (doped with 10% Yb)3+、1% Er3+) And 200 mA/W (15% Yb doped)3+、1.5% Er3+) (ii) a Under 2V bias, the detectivity is estimated to be 1.8 x 1012Jones (pure undoped BA)2FAPb2I7)，6.9×1012 Jones (doped with 5% Yb)3+, 0.5% Er3+)，1.6×1013Jones (doped with 10% Yb)3+, 1% Er3+) And 2.1X 1012Jones (doped with 5% Yb)3+, 0.5 % Er3+). It can be clearly seen that 10% Yb3+And 1% Er3+The doping effect of (2) is most outstanding.
Example 2
Yb (Yb)3+Singly doped BA2FAPb2I7The perovskite film is prepared by the following steps:
(1) preparation of solution A
Mixing 0.2mmol BAI, 0.1mmol FAI and 0.2mmol PbI2Dissolving in 1ml of DMF, stirring for 6 hours at room temperature, and standing for 2 hours to obtain a solution A;
(2) preparation of solution B
Mixing 10mmol of Yb2O3The powder was dissolved in water and when the temperature was raised to 100 ℃, excess concentrated HCl solution (37 wt%, gumbo) was added until the solution became clear. Evaporating to dryness at 150 ℃ to obtain YbCl3Powder, YbCl prepared in 20ml of ultrapure water to a concentration of 1mmol/ml3The aqueous solution B of (1).
(3) Preparation of solution C
And preparing a Yb solution with the doping amount of 5 percent. Add 5. mu. L B solution to 1ml of solution A and stir for 4 h.
And preparing a solution with the doping amount of 10% Yb. Add 10. mu. L B solution to 1ml of solution A and stir for 4 h.
And preparing a solution with the doping amount of 15 percent Yb. The 15. mu. L B solution was added to 1ml of A solution and stirred for 4 h.
(4) Crystallization of
A silicon wafer with one oxidized surface (the area is 2cm multiplied by 2cm, single polishing is carried out, and the thickness is 300 nm SiO)2Layer, single-side oxidation, combined fertilizer and crystal material technology limited) was preheated for 20min on a heating plate at 120 ℃, 80 μ L of solution precursor solution C with doping amounts of 5%, 10% and 15% Yb, respectively, was taken out and dropped on a silicon wafer at a rotation speed of 3000rpm for a duration of 30 s. Heating the spin-coated film on a heating plate at 120 deg.C for 20min to obtain BA with Yb doping amount of 5%, 10% and 15%2FAPb2I7A film. The whole process is completed in the glove box. FIG. 6 is BA after doping with Yb of 0%, 5%, 10% and 15%2FAPb2I7Thin films, as can be seen, the absence of material after Yb dopingThe trap luminescence is enhanced, which indicates that the defect can not be effectively inhibited by singly doping Yb.
Example 3
Er3+Singly doped BA2FAPb2I7The perovskite film is prepared by the following steps:
(1) preparation of solution A
Mixing 0.2mmol BAI, 0.1mmol FAI and 0.2mmol PbI2Dissolving in 1ml of DMF, stirring for 6 hours at room temperature, and standing for 2 hours to obtain a solution A;
(2) preparation of solution B
Adding 1mmol Er2O3The powder was dissolved in water and when the temperature was raised to 100 ℃, excess concentrated HCl solution (37 wt%, gumbo) was added until the solution became clear. Evaporating to dryness at 150 ℃ to obtain ErCl3Powder, ErCl prepared in 20ml ultrapure water to a concentration of 0.1mmol/ml3The aqueous solution C of (1).
(3) Preparation of solution C
And preparing a solution with the doping amount of 0.5 percent Er. Add 5. mu. L B solution to 1ml of A solution and stir for 4 h.
And preparing a solution with the doping amount of 1% Er. Add 10. mu. L B solution to 1ml of solution A and stir for 4 h.
And preparing a solution with the doping amount of 1.5 percent of Er. The 15. mu. L B solution was added to 1ml of A solution and stirred for 4 h.
(4) Crystallization of
A silicon wafer with one oxidized surface (the area is 2cm multiplied by 2cm, single polishing is carried out, and the thickness is 300 nm SiO)2Layer, single-side oxidation, combined fertilizer and crystal material technology limited) was preheated for 20min on a heating plate at 120C, 80 μ L of solution precursor solution C with doping amounts of 5%, 10% and 15% Er, respectively, was taken out and dropped on a silicon wafer at 3000rpm for 30 s. Heating the spin-coated film on a heating plate at 120 deg.C for 20min to obtain BA with Er doping amount of 0.5%, 1% and 1.5%2FAPb2I7A film. The whole process is completed in a glove box. FIG. 7 BA after 0%, 0.5%, 1% and 1.5% Er doping2FAPb2I7As can be seen from the figure, after Er is doped, the defect luminescence of the material is enhanced, which indicates that the defect cannot be effectively inhibited by singly doping Er.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims (5)

1. An ytterbium and erbium co-doped perovskite thin film, which is characterized by being obtained by the following process:
(1) preparation of solution A
Mixing BAI, FAI and PbI2Dissolving the materials into DMF according to a molar ratio of 2:1:2, stirring for 5-7 h at room temperature, and standing for at least 2h to obtain a solution A;
(2) preparation of solution B
Yb of2O3Dissolving the powder in water, heating to 90-110 ℃, adding a concentrated HCl solution until the solution becomes clear, and evaporating to dryness at 145-155 ℃ to obtain YbCl3Powdering, mixing YbCl3Dissolving the powder in water to obtain YbCl3The aqueous solution B of (1);
(3) preparation of solution C
Adding Er2O3Dissolving the powder in water, heating to 90-110 ℃, adding a concentrated HCl solution until the solution becomes clear, and evaporating to dryness at 145-155 ℃ to obtain ErCl3Powder of ErCl3Dissolving the powder in water to obtain ErCl3The aqueous solution C of (1);
(4) preparation of solution D
Adding the solution B and the solution C with the same volume into the solution A, and stirring for 3-5 hours to obtain a solution D;
(5) crystallization of
Preheating a silicon wafer with a single surface oxidized at 117-123 ℃ for 15-25 min, dripping the solution D on the silicon wafer, spin-coating, placing the spin-coated film at 117-123 ℃ and drying for 15-25 min to obtain the ytterbium and erbium co-doped BA2FAPb2I7A film.
2. The ytterbium and erbium-co-doped perovskite thin film as claimed in claim 1, wherein in the step (4), Yb is doped with BA in an amount of2FAPb2I75-15% of mole number, and the doping amount of Er is BA2FAPb2I70.5-1.5% of the mole number, and the molar ratio of Yb to Er is 10: 1.
3. The ytterbium and erbium co-doped perovskite thin film as claimed in claim 1, wherein step (1) requires dissolution in 1ml of ldmf for every 0.1mmol of fai, and step (2) requires YbCl in aqueous solution B3ErCl in the aqueous solution C of step (3) at a concentration of 1mmol/ml3The concentration was 0.1 mmol/ml.
4. Use of a ytterbium and erbium co-doped perovskite thin film according to any one of claims 1 to 3 in a photodetector.
5. The use according to claim 4, characterized in that the procedure is as follows: putting the ytterbium and erbium co-doped perovskite film on a high-vacuum resistance evaporation coating machine to evaporate and plate the interdigital electrode, wherein the pressure intensity of a vacuum chamber is 5 multiplied by 10 when the coating machine works-5Pa, the thickness of the Au electrodes is 80nm, and the width between the Au electrodes is 100 μm.
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