CN109166969B - Surface plasmon resonance enhanced perovskite thin film and preparation method thereof - Google Patents

Surface plasmon resonance enhanced perovskite thin film and preparation method thereof Download PDF

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CN109166969B
CN109166969B CN201810734581.XA CN201810734581A CN109166969B CN 109166969 B CN109166969 B CN 109166969B CN 201810734581 A CN201810734581 A CN 201810734581A CN 109166969 B CN109166969 B CN 109166969B
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徐清华
姜小芳
吴啸
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South China University of Technology SCUT
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Abstract

The invention belongs to the field of perovskite materials, and discloses a surface plasmon resonance enhanced perovskite thin film and a preparation method thereof. The perovskite thin film consists of a PTAA polymer layer and a MAPbI which are sequentially laminated3A perovskite layer, a PMMA polymer intermediate isolation layer and a PMMA-Au polymer-gold nanorod mixing layer. The invention utilizes the surface plasma resonance characteristic of gold nanoparticles and MAPbI3A PMMA protective layer is added on the perovskite film to regulate and control the gold nanorods and the MAPbI3Distance between perovskite thin films such that MAPbI3The laser property of the perovskite thin film is enhanced, namely the laser threshold is reduced, and the laser intensity is increased.

Description

Surface plasmon resonance enhanced perovskite thin film and preparation method thereof
Technical Field
The invention belongs to the field of perovskite materials, and particularly relates to a surface plasmon resonance enhanced perovskite thin film and a preparation method thereof.
Background
Since the development of the metal nanoparticle synthesis technology in the last century, the development and progress of the metal nanoparticle synthesis technology have been greatly advanced, and the target nanoparticles can be efficiently synthesized in a laboratory by using cheap raw materials and convenient technical means. And because the material with the physical size in the nanometer scale has the surface and interface effect, the small-size effect, the quantum size effect and the macroscopic quantum tunneling effect, the metal nano particles have a special attribute, namely surface plasmon resonance, and the fluorescence emission of the luminescent material can be enhanced by utilizing the special attribute. The gold nanorods are synthesized by sodium borohydride (NaBH)4) Mixing Au3+Reducing the Au into Au simple substance with extremely small particles, and further synthesizing into gold nanorods in a form of 'seed growth', wherein the method is stable and efficient, and can obtain the gold nanorods with higher purity.
Since 2009, perovskite materials have attracted considerable scientific attention for their excellent optoelectronic properties, such as very high extinction coefficient, tunable band gap, high quantum yield, balanced and very long exciton diffusion distance, low defect density, etc. Solar cells and light-emitting devices based on perovskite materials have been developed and advanced greatly in recent years, and due to the excellent photoelectric properties of the perovskite materials, the perovskite materials also have great application potential and prospect in the laser field.
Since the invention in 1960, lasers have been widely used in a wide variety of technical and research fields such as bio-imaging, manufacturing, spectroscopy, optical communication, and the like. However, in recent years, with the development and breakthrough of nanoscience and nanotechnology, attention has been drawn to a small solid-state laser capable of realizing one-dimensional or multi-dimensional physical dimensions equivalent to or even smaller than the optical diffraction limit, due to the demand for finer time resolution and spatial resolution by high-density data storage, optical integration, high-resolution bio-imaging, and other high-new technologies. Therefore, how to enhance the lasing property of the perovskite thin film and make the application of the perovskite material in the laser field further has important theoretical and practical significance for the skilled person in the field.
Disclosure of Invention
Based on the above prior art, the primary object of the present invention is to provide a surface plasmon resonance enhanced perovskite thin film. The invention utilizes the specific property of the nano metal particles, namely surface plasma resonance, and successfully introduces the gold nano particles into the perovskite material, thereby greatly enhancing the lasing property of the perovskite film and playing the roles of laying and throwing bricks to guide jade for subsequent scientific research and technical application.
Another object of the present invention is to provide a method for preparing the above surface plasmon resonance enhanced perovskite thin film.
The purpose of the invention is realized by the following technical scheme:
a perovskite thin film with enhanced surface plasmon resonance is prepared by sequentially laminating PTAA (poly [ bis (4-phenyl) (2,4, 6-trimethylphenyl) amine)]) Polymer layer, MAPbI3Perovskite layer, PMMA (polymethyl methacrylate) polymer intermediate barrier layerAnd a PMMA-Au polymer-gold nanorod mixed layer.
Preferably, the thickness of the PMMA polymer intermediate isolation layer is 8 +/-2 nm.
The preparation method of the surface plasmon resonance enhanced perovskite thin film comprises the following preparation steps:
(1) dispersing gold nanorods in an organic solvent, and then adding PMMA (polymethyl methacrylate) to dissolve uniformly to obtain a PMMA-Au polymer-gold nanorod mixed solution;
(2) spin-coating a PTAA polymer solution on a quartz plate, and carrying out annealing treatment to obtain a PTAA polymer layer;
(3) spin-coating ethanol on the PTAA polymer layer in the step (2) for wetting, and then spin-coating PbI2(lead iodide) solution, annealing, spin-coating MAI (methylamine iodide) solution, annealing, and forming MAPbI on the PTAA polymer layer3A perovskite thin film;
(4) MAPbI in step (3)3The perovskite film is spin-coated with PMMA polymer solution, and a PMMA polymer layer is obtained after drying;
(5) and (3) spin-coating the PMMA-Au polymer-gold nanorod mixed solution obtained in the step (1) on the PMMA polymer layer obtained in the step (4), and drying to obtain the surface plasmon resonance enhanced perovskite thin film.
Further, the method for dispersing the gold nanorods in the organic solvent in the step (1) comprises the following steps:
the gold nanorods are firstly subjected to surface modification by PEG-SH (polyethylene glycol-sulfydryl), and then are dispersed in an organic solvent. After the gold nanorods are dispersed in an organic solvent, LSPR (plasma resonance absorption) peaks of the gold nanorods are 522 +/-10 nm and 785 +/-10 nm.
Further, the solvent of the PTAA polymer solution in step (2) is toluene.
Further, the PbI in the step (3)2The solvent of the solution is N, N-dimethylformamide, and the solvent of the MAI solution is ethanol.
Further, the annealing treatment temperature in the step (2) is 100 ℃; spin coating PbI in step (3)2The post-annealing temperature of the solution is 80 ℃, and the post-annealing temperature of the spin-coated MAI solution is 100 ℃.
Further, the solvent of the PMMA polymer solution in the step (4) is chlorobenzene.
Further, the gold nanorods in the step (1) are prepared by the following method of 'reduction + seed growth':
(1) adding HAuCl4Mixing the solution, a surfactant and a reducing agent for reaction to obtain an Au seed solution;
(2) mixing surfactant and HAuCl4Solution, AgNO3And (2) mixing the solution, hydrochloric acid, an AA (ascorbic acid) solution and the Au seed solution in the step (1), standing for reaction, and growing gold nanorods (AuNRs) through seeds. The LSPR peaks of the resulting gold nanorods were 510 and 734 ± 100 nm.
In the above gold nanorods preparation method, the surfactant is preferably CTAB (cetyl trimethyl ammonium bromide), and the reducing agent is preferably NaBH4。
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the invention provides a technical means and a specific preparation method for enhancing the lasing property of a perovskite thin film by utilizing surface plasmon resonance. The gold nanorods with special properties (surface plasmon resonance enhanced fluorescence) are introduced to realize the enhancement of the laser property of the perovskite thin film and the enhancement of the MAPbI3A polymethyl methacrylate (PMMA) protective layer is added on the perovskite film to regulate and control the gold nanorods and the MAPbI3Distance between perovskite thin films such that MAPbI3The laser property of the perovskite thin film is enhanced, namely the laser threshold is reduced, and the laser intensity is increased.
(2) The invention obtains the gold nanorods and MAPbI3The optimal enhancement distance between perovskite thin films is 8nm, and MAPbI is subjected to the plasma resonance enhancement effect of gold nanorods and the protection effect of PMMA3The laser threshold of the perovskite thin film is from 22.11uJ/cm2Reduced to 13.07uJ/cm2The laser intensity is enhanced by 2.72 times.
Drawings
FIG. 1 shows the addition of various amounts of AgNO in example 13Absorption of the resulting AuNRsAnd (6) drawing.
FIG. 2 is a graph of the absorption of AuNRs before and after surfactant turnover in example 1.
FIG. 3 shows the formation of MAPbI in steps (c) to (e) in step (3) of example 13A perovskite thin film (Q/M), a thin film (Q/M/P) for preparing a PMMA polymer layer and a thin film (Q/M/P8/P-Au) after preparing a PMMA-Au polymer-gold nanorod mixed layer.
FIG. 4 is a graph comparing the lasing thresholds of perovskite thin films of PMMA polymer intermediate spacers of different thicknesses in example 2.
FIG. 5 is a graph comparing the lasing intensity of perovskite thin films of PMMA polymer intermediate spacers of different thicknesses in example 2.
FIG. 6 is the absorption and MAPbI of gold nanorods for different LSPR peaks in example 33Fluorescence contrast map of perovskite thin film (PL).
FIG. 7 shows the gold nanorod couple to MAPbI for different LSPR peaks in example 33The lasing enhancement effect of the perovskite thin film is compared with that of the perovskite thin film.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
Example 1
(1) Preparing gold nanorods:
(a) adding HAuCl4(50mM, 50uL), CTAB (100mM, 10mL) were added sequentially to a 50mL Erlenmeyer flask and NaBH dissolved in ice water was injected rapidly4(10mM, 0.6mL), rapidly and violently shaking for 2 minutes, changing the color of the solution from yellow to tan, and standing for 5 hours for standby to obtain an Au seed solution;
(b) CTAB (100mM, 40mL), HAuCl4(50mM，400uL)，HCl(1M，800uL)，AgNO3(10mM), AA (100mM, 320uL) and the Au seed solution of step (a) are added to a 50mL test tube in sequence, the solution is gently shaken, turned from yellow to colorless, and is kept still overnight to obtain aqueous phase gold nanorods (AuNRs). By varying AgNO3The LSPR peak position of the gold nanorod can be changed. When AgNO3When the addition amount of the solution is 250uL, 300uL, 350uL and 400uL respectively, the obtained solutionThe absorption diagram of AuNRs is shown in FIG. 1.
(2) Gold nanorod surfactant conversion and preparation of PMMA-Au polymer-gold nanorod mixed solution:
the gold nanorods in the water phase cannot be dissolved in an organic solvent, so that the surfactant of the gold nanorods must be converted to be soluble in the organic solvent so as to be mutually soluble with PMMA. The specific operation is as follows:
(a) taking AgNO in step (1)3Centrifuging 5mL of the obtained water-phase gold nanorods when the addition amount of the solution is 300uL, wherein the rotating speed is 8000rmp, the time is 5min, removing supernatant after centrifugation, and re-dispersing in 5mL of deionized water for later use;
(b) preparing PEG-SH solution, wherein the solvent is deionized water and the concentration is 2mM for later use;
(c) adding 5mL of the solution (a) and 2mL of the solution (b) into a reagent bottle, and stirring by magnetic force overnight;
(d) centrifuging (8000rmp, 5min) the solution of (c), removing supernatant, dispersing again in tetrahydrofuran solution, centrifuging again (8000rmp, 5min), removing supernatant, and dispersing again in chlorobenzene solution.
Fig. 2 is an absorption diagram of AuNRs before and after surfactant conversion, and it can be seen that LSPR peaks of AuNRs are converted from 510nm and 734nm in the aqueous phase to 522nm and 785nm in the oil phase.
(e) And (d) adding PMMA into the chlorobenzene solution of the gold nanorods in the step (d) to be uniformly dissolved to obtain a PMMA-Au polymer-gold nanorod mixed solution for later use.
(3) Preparation of perovskite thin film-the whole process is operated in a nitrogen glove box.
(a) Spin-coating a layer of 2mg/mL PTAA toluene solution on a quartz plate, rotating at 6000rmp for 40s, and annealing at 100 ℃ for 10 min;
(b) spin-coating ethanol on PTAA at 2800rmp for 30s, immediately followed by spin-coating PbI2The solution (solvent is N, N-dimethylformamide with concentration of 400mg/mL) is annealed at 80 deg.C for 10min at rotation speed of 3500rmp for 30 s;
(c) in PbI2Spin-coating MAI solution (solvent is ethanol, concentration is 35mg/mL), rotating speed is 3500rmp, time is 30s, annealing is carried out at 100 ℃ for 2h, MApB is generatedI3A perovskite thin film;
(d) in the generation of MAPbI3Spin-coating PMMA chlorobenzene solution with the concentration of 8mg/mL on the perovskite thin film, wherein the rotating speed is 3000rmp, the time is 30s, and drying is carried out to obtain a PMMA polymer layer which is 8nm in thickness and is used as an intermediate isolation layer;
(e) and (3) spin-coating the PMMA-Au polymer-gold nanorod mixed solution obtained in the step (2) on a PMMA polymer layer at the rotating speed of 3000rmp for 30s, standing overnight, and obtaining the surface plasmon resonance enhanced perovskite thin film after the solvent is completely volatilized.
MAPbI is formed in steps (c) to (e) of step (3) of this example3The fluorescence spectra of the perovskite thin film (Q/M), the thin film (Q/M/P) for preparing the PMMA polymer layer, and the thin film (Q/M/P8/P-Au) after preparing the PMMA-Au polymer-gold nanorod mixed layer are shown in FIG. 3.
Example 2
(1) Preparation of gold nanorods was the same as in example 1 (AgNO)3The amount of solution added was 300 uL).
(2) The same procedure as in example 1 was followed for the surfactant conversion of gold nanorods and the preparation of PMMA-Au polymer-gold nanorod mixture.
(3) Preparation of perovskite thin film-the whole process is operated in a nitrogen glove box.
(a) Spin-coating a layer of 2mg/mL PTAA toluene solution on a quartz plate, rotating at 6000rmp for 40s, and annealing at 100 ℃ for 10 min;
(b) spin-coating ethanol on PTAA at 2800rmp for 30s, immediately followed by spin-coating PbI2The solution (solvent is N, N-dimethylformamide with concentration of 400mg/mL) is annealed at 80 deg.C for 10min at rotation speed of 3500rmp for 30 s;
(c) in PbI2Spin-coating MAI solution (solvent is ethanol, concentration is 35mg/mL), rotating speed is 3500rmp, time is 30s, annealing is carried out at 100 ℃ for 2h, and MAPbI is generated3A perovskite thin film;
(d) in the generation of MAPbI3Spin-coating PMMA-chlorobenzene solution (blank, 4mg/mL, 8mg/mL, 12mg/mL, 16mg/mL, 20mg/mL) with different concentrations on the perovskite thin film, rotating at 3000rmp for 30s, and drying to obtain different thicknesses (0, 4 nm)8nm, 12nm, 16nm, 20nm) PMMA polymer intermediate spacer layer;
(e) and (3) spin-coating the PMMA-Au polymer-gold nanorod mixed solution obtained in the step (2) on a PMMA polymer layer at the rotating speed of 3000rmp for 30s, standing overnight, and obtaining the surface plasmon resonance enhanced perovskite thin film after the solvent is completely volatilized.
The results of comparing the lasing threshold and the lasing intensity of the perovskite thin film of the PMMA polymer intermediate isolation layer with different thickness obtained in this example are shown in fig. 4 and 5, respectively.
Example 3
(1) Preparing gold nanorods:
(a) adding HAuCl4(50mM, 50uL), CTAB (100mM, 10mL) were added sequentially to a 50mL Erlenmeyer flask and NaBH dissolved in ice water was injected rapidly4(10mM, 0.6mL), rapidly and violently shaking for 2 minutes, changing the color of the solution from yellow to tan, and standing for 5 hours for standby to obtain an Au seed solution;
(b) CTAB (100mM, 40mL), HAuCl4(50mM，400uL)，HCl(1M，800uL)，AgNO3(10mM), AA (100mM, 320uL) and the Au seed solution of step (a) are added to a 50mL test tube in sequence, the solution is gently shaken, turned from yellow to colorless, and is kept still overnight to obtain aqueous phase gold nanorods (AuNRs). By varying AgNO3The addition amount of (A) is 140uL and 300uL respectively, and the LSPR peak position of the gold nanorod can be changed. Resulting uptake and MAPbI of AuNRs3The fluorescence contrast of the perovskite thin film (PL) is shown in fig. 6. As can be seen from FIG. 6, AgNO3The addition amounts of (A) and (B) are respectively 140uL and 300uL, and the LSPR peak positions of the gold nanorods are respectively 690nm and 785 nm.
(2) The same procedure as in example 1 was followed for the surfactant conversion of gold nanorods and the preparation of PMMA-Au polymer-gold nanorod mixture.
(3) The perovskite thin film was prepared as in example 1.
Gold nanorod couple MAPbI of different LSPR peaks of the example3The lasing enhancement effect of the perovskite thin film is shown in fig. 7. As can be seen from FIG. 7, when LSPR peak of gold nanorod is associated with MAPbI3When the fluorescence peaks of the perovskite thin film are not matched, the gold nanorods cannot play the surfacePlasmon resonance enhances the effect of fluorescence.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (7)

1. A surface plasmon resonance enhanced perovskite thin film characterized by: the perovskite thin film consists of a PTAA polymer layer and a MAPbI which are sequentially laminated3The perovskite layer, the PMMA polymer intermediate isolation layer and the PMMA-Au polymer-gold nanorod mixing layer;
the thickness of the PMMA polymer intermediate isolation layer is 8 +/-2 nm;
the surface plasmon resonance enhanced perovskite thin film is prepared by the following method:
(1) dispersing gold nanorods in an organic solvent, and then adding PMMA (polymethyl methacrylate) to dissolve uniformly to obtain a PMMA-Au polymer-gold nanorod mixed solution; after the gold nanorods are dispersed in an organic solvent, LSPR peaks of the gold nanorods are 522 +/-10 nm and 785 +/-10 nm;
(2) spin-coating a PTAA polymer solution on a quartz plate, and carrying out annealing treatment to obtain a PTAA polymer layer;
(3) spin-coating ethanol on the PTAA polymer layer in the step (2) for wetting, and then spin-coating PbI2Solution, annealing followed by spin coating of MAI solution, annealing to form MAPbI on the PTAA polymer layer3A perovskite thin film;
(4) MAPbI in step (3)3The perovskite film is spin-coated with PMMA polymer solution, and a PMMA polymer layer is obtained after drying;
(5) and (3) spin-coating the PMMA-Au polymer-gold nanorod mixed solution obtained in the step (1) on the PMMA polymer layer obtained in the step (4), and drying to obtain the surface plasmon resonance enhanced perovskite thin film.
2. The surface plasmon resonance enhanced perovskite thin film according to claim 1, wherein the method for dispersing gold nanorods in an organic solvent in the step (1) is: the gold nanorods are firstly subjected to surface modification by PEG-SH and then dispersed in an organic solvent.
3. A surface plasmon resonance enhanced perovskite thin film as defined in claim 1, wherein: the solvent of the PTAA polymer solution in step (2) is toluene; the PbI in the step (3)2The solvent of the solution is N, N-dimethylformamide, and the solvent of the MAI solution is ethanol; and (4) the solvent of the PMMA polymer solution in the step (4) is chlorobenzene.
4. A surface plasmon resonance enhanced perovskite thin film as defined in claim 1, wherein: the annealing temperature in the step (2) is 100 ℃; spin coating PbI in step (3)2The post-annealing temperature of the solution is 80 ℃, and the post-annealing temperature of the spin-coated MAI solution is 100 ℃.
5. The surface plasmon resonance enhanced perovskite thin film according to claim 1, wherein the gold nanorods in step (1) are prepared by the following method:
(1) adding HAuCl4Mixing the solution, a surfactant and a reducing agent for reaction to obtain an Au seed solution;
(2) mixing surfactant and HAuCl4Solution, AgNO3And (2) mixing the solution, hydrochloric acid, an AA solution and the Au seed solution in the step (1), standing for reaction, and growing the seeds to generate the gold nanorods.
6. A surface plasmon resonance enhanced perovskite thin film as claimed in claim 5, wherein: the LSPR peaks of the resulting gold nanorods were 510nm and 734. + -. 100 nm.
7. A surface plasmon resonance enhanced perovskite thin film as claimed in claim 5, wherein: the surfactant is CTAB, theThe reducing agent is NaBH4。
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