CN111777778A - Gold nanorod-single layer up-conversion nanoparticle composite film for modulating solar spectrum and preparation method thereof - Google Patents
Gold nanorod-single layer up-conversion nanoparticle composite film for modulating solar spectrum and preparation method thereof Download PDFInfo
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- 239000002356 single layer Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 8
- 238000001228 spectrum Methods 0.000 title claims description 20
- 238000006243 chemical reaction Methods 0.000 title abstract description 27
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title abstract description 7
- 239000010931 gold Substances 0.000 title abstract description 6
- 229910052737 gold Inorganic materials 0.000 title abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 103
- 239000002114 nanocomposite Substances 0.000 claims abstract description 28
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 238000004528 spin coating Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 4
- 239000010703 silicon Substances 0.000 claims abstract description 4
- 238000007664 blowing Methods 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 69
- 238000003756 stirring Methods 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 12
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 9
- 239000012300 argon atmosphere Substances 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910009523 YCl3 Inorganic materials 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000839 emulsion Substances 0.000 claims description 3
- SDQQBPKWLSANJO-UHFFFAOYSA-N methyl 2-methylprop-2-enoate;toluene Chemical compound COC(=O)C(C)=C.CC1=CC=CC=C1 SDQQBPKWLSANJO-UHFFFAOYSA-N 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 2
- 239000010410 layer Substances 0.000 abstract description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 abstract description 4
- 239000004926 polymethyl methacrylate Substances 0.000 abstract description 4
- 230000008033 biological extinction Effects 0.000 description 9
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 238000002189 fluorescence spectrum Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000000861 blow drying Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 rare earth ion Chemical class 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000002537 optical extinction spectroscopy Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
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- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
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Abstract
The invention discloses gold nanorod-monolayer up-conversion nanoparticles for modulating solar spectrumCAu composite film and preparation method thereof&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film. The method is to prepare NaYF firstly4:Er3+,Yb3+@NaYF4Adding toluene solution of toluene and PMMA, dripping the mixed solution on a silicon wafer to obtain a single-layer film by using a spin coating method, dripping CAu on the film after drying, and blowing and drying to obtain CAu&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film. The nano composite film is made into a light conversion layer and is placed on the solar cell, so that low-energy photons with poor response of the solar cell can be converted into high-energy photons with the frequency matched with the frequency of the solar cell, and the photoelectric conversion efficiency of the solar cell is improved.
Description
Technical Field
The invention relates to the technical field of composite nano materials, in particular to a gold nanorod-single layer up-conversion nano particle composite film for modulating solar spectrum and a preparation method thereof.
Background
Upconversion refers to the phenomenon of converting two or more low energy photons into one high energy photon. The single-layer nanoparticle film made of the up-conversion material is placed on the solar cell, so that the high transmittance of photons with other wavelengths can be ensured, the film can be efficiently utilized by the solar cell, and the film can not be absorbed by the film, and the photoelectric conversion efficiency of the solar cell is effectively improved. However, the conventional up-conversion materials have weak emission intensity as a light conversion layer.
Disclosure of Invention
The invention aims to solve the problem that the traditional up-conversion material is used as a light conversion layer and has weak luminous intensity, and provides a gold nanorod-single layer up-conversion nanoparticle composite film for modulating solar spectrum and a preparation method thereof, wherein the nano composite film is CAu&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film.
In order to achieve the purpose, the technical scheme of the invention is as follows:
CAu for modulating the solar spectrum&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film comprises the following steps:
a: preparation of NaYF4:Er3+,Yb3+Nanoparticles
A-1: weighing RECl with the total amount of 2mmol according to the molar ratio3•6H2O, RE = Y/Er/Yb, 12 mL of oleic acid and 30 mL of 1-octadecene are added, the mixed solution is vacuumized and heated to 125-135 ℃, and the mixed solution is naturally cooled to room temperature after being kept for 40-45 min, so as to obtain a solution A;
a-2: 0.2000 g of NaOH and 0.2963 g of NH were weighed out4F, dissolving in methanol, dropwise adding the mixed methanol solution into the solution A, stirring at room temperature for 30-40min, heating to 62-63 ℃ under the argon atmosphere to distill out the methanol, then heating to 300-320 ℃, maintaining for 1-1.2 hours, and then cooling to room temperature to obtain a solution B;
a-3: centrifuging the solution B, and ultrasonically cleaning particles obtained after centrifugation to obtain NaYF4:Er3+,Yb3+Nanoparticles, finally dispersed in cyclohexane;
b: preparation of NaYF4:Er3+,Yb3+@NaYF4Nanoparticles
B-1: weighing 2mmol YCl3•6H2O, adding 12 mL of oleic acid and 30 mL of 1-octadecene, vacuumizing the mixed solution, heating to 125-135 ℃, keeping the temperature for 40-45 min, and naturally cooling to room temperature to obtain a solution C;
b-2: the NaYF obtained in the step A-34:Er3+,Yb3+Dropwise adding the nanoparticles into the solution C, stirring at room temperature for 30-40min, heating to 62-63 ℃ under the argon atmosphere to distill out methanol, then heating to 300-320 ℃, maintaining for 40-50 min, and cooling to room temperature to obtain a solution D;
b-3: 0.2000 g of NaOH and 0.2963 g of NH were weighed out4F, dissolving the mixed methanol solution in a methanol solution, dropwise adding the mixed methanol solution into the solution D to obtain an emulsion, stirring at room temperature for 30-40min, heating to 62-63 ℃ under an argon atmosphere to distill off methanol, then heating to 300-320 ℃, maintaining for 1-1.2 hours, and then cooling to room temperature to obtain a solution E;
b-4: centrifuging the solution E, and ultrasonically cleaning particles obtained after centrifugation to obtain NaYF4:Er3+,Yb3+@NaYF4Dispersing the nano particles in cyclohexane to obtain NaYF4:Er3+,Yb3+@NaYF4A solution;
c: preparation CAu
C-1: preparing a growth solution:
weighing 7 g of CTAB (cetyl trimethyl ammonium bromide) and 1.234 g of NaOL (sodium oleate) and pouring into a conical flask, adding 250 mL of deionized water, stirring for 20-30min, standing the mixed solution in a drying oven at 28-32 ℃ for 15-20 min;
② Erlenmeyer flask was charged with 24 mL of AgNO3Standing the mixed solution in a drying oven at 28-32 deg.C for 15-20 min;
③ into the Erlenmeyer flask was added 250 mL of HAuCl4Solution, stirring the obtained solution at the rotating speed of 700-800 rpm for 90-110 min to obtain growth liquid;
c-2: preparing seeds:
① mix 5 mL of HAuCl4Mixing the solution and 5 mL CTAB solution into a 15 mL centrifuge tube;
② Add 600. mu.L of NaBH to the 15 mL centrifuge tube4Rapidly shaking the centrifugal tube with an ice water solution covered, observing that the solution turns to light brown from yellow, and placing the solution into a drying box at 28-32 ℃ for 30-40min to obtain a seed solution;
c-3: adding the reagent dropwise to prepare CAu
Adding 3.6 mL of 37 wt% HCl into the growth solution, and uniformly stirring for one time;
adding 1.25 mL of AA (ascorbic acid) solution into the conical flask, and uniformly stirring for the second time;
③ adding 0.4 mL of prepared seed liquid into the conical flask, stirring evenly for three times, and then placing the conical flask into a drying oven at 28-32 ℃ for 12-14 h to obtain CAu;
D. the preparation of the nano-composite system is carried out,
2mmol of NaYF is taken4:Er3+,Yb3+@NaYF4500 μ L of the solution was centrifuged, and after removing the supernatant, the solution was addedAdding 1.8 mL of toluene and 0.2mL of PMMA (polymethyl methacrylate) toluene solution, performing ultrasonic dispersion uniformly, dropwise adding the mixed solution on a cleaned silicon wafer, preparing a single-layer film by using a spin-coating method, naturally drying, dropwise adding CAu on the film, and blow-drying to obtain CAu&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film.
In the step A-3 and the step B-4, the centrifugation is carried out for 15-20min at the rotating speed of 9000-10000rpm, and the cleaning takes absolute ethyl alcohol as a cleaning solution.
In step C-1, the AgNO3The molar concentration of the solution is 4 mM, and the HAuCl is4The molarity of the solution was 1 mM.
In step C-2, the HAuCl4The molarity of the solution was 0.5 mM, the molarity of the CTAB solution was 0.2M, and the NaBH was added4The molar concentration of the ice-water solution was 0.01M.
In the step C-3, the molar concentration of the AA solution is 0.064M, the primary stirring is carried out for 15-20min at the rotating speed of 350-; the three times of stirring are evenly stirred for 30-35 s at the rotating speed of 1400-1600 rpm.
In the step D, the centrifugation is carried out for 15-20min at the rotating speed of 9000-11000 rpm, and the concentration of the PMMA toluene solution is 10 mg/mL.
In the step D, during spin coating, the spin coating is performed for 5 s at a rotation speed of 600rpm, and then the spin coating is performed for 30 s at a rotation speed of 2000 rpm.
The CAu is prepared for the first time by adopting the technical scheme&NaYF4:Er3+,Yb3+@NaYF4The nano composite film (CAu: gold nanorod with high length-diameter ratio) of the up-conversion nano particles effectively solves the problem that the traditional up-conversion material is weak in luminous intensity when used as a light conversion layer. Firstly, a nano-scale up-conversion luminescent material is selected, and the luminescence of the luminescent material can be obviously enhanced by utilizing the local surface plasmon polariton characteristic of noble metal nano-particles; secondly, the film only comprises a single layer of up-conversion nano particles with the thickness of nano level, and is placed on the surface of the solar cellThe high transmittance of visible light can be ensured, and the photoelectric conversion efficiency of the solar cell is improved. The effective excitation wavelength of the nano composite film is 980 nm, and the emission peaks are 520 nm (green light), 540 nm (green light) and 655 nm (red light). When the aspect ratio of CAu is 5.5 (length is 110 nm, width is 20 nm), the up-conversion red and green luminescence enhancement effect of the nano-composite system is most remarkable, and the maximum enhancement factors of red and green are 1.57 and 1.65 respectively.
The composite film of the invention has the advantages and the purposes that: the invention provides a gold nanoparticle-up-conversion material single-layer nano composite film for modulating solar spectrum for the first time, and the film has the advantages of low cost and high luminous efficiency. The nano composite film is made into a light conversion layer and is placed on the solar cell, so that low-energy photons with poor response of the solar cell can be converted into high-energy photons with the frequency matched with the frequency of the solar cell, and the photoelectric conversion efficiency of the solar cell is improved.
Drawings
FIG. 1 shows NaYF4:Er3+,Yb3+@NaYF4SEM image of monolayer film: (a) a surface map; (b) a cross-sectional view;
FIG. 2 is a related image of CAu, (a) SEM image of morphology and optical properties of CAu; (b) ultraviolet-visible-infrared extinction spectroscopy; (c) field intensity distribution at 970nm light emission; (d) FDTD simulation extinction, absorption and scattering spectrum;
CAu in FIG. 3&NaYF4:Er3+,Yb3+@NaYF4The micro-area up-conversion fluorescence spectrum: (a) converting fluorescence spectrum on the micro-area with or without CAu; the inset is an SEM image; (b) green and red spectral peak areas with or without CAu; the inset is a microscopic field of view.
Detailed Description
CAu for modulating the solar spectrum&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film comprises the following steps:
a: preparation of NaYF4:Er3+,Yb3+Nanoparticles
A-1: weighing RECl with the total amount of 2mmol according to the molar ratio3•6H2O, RE = Y/Er/Yb, 12 mL of oleic acid and 30 mL of 1-octadecene are added, the mixed solution is vacuumized and heated to 130 ℃, and the temperature is kept for 40min and then naturally cooled to room temperature to obtain a solution A;
a-2: 0.2000 g of NaOH and 0.2963 g of NH were weighed out4F, dissolving in 10 mL of methanol, dropwise adding the mixed methanol solution into the solution A, stirring at room temperature for 30min, heating to 62 ℃ under argon atmosphere to distill out methanol, then heating to 300 ℃, maintaining for 1 hour, and then cooling to room temperature to obtain a solution B;
a-3: centrifuging the solution B at the rotating speed of 9200 rpm for 15 min, taking absolute ethyl alcohol as a cleaning solution, ultrasonically cleaning the particles obtained after centrifugation for 5 min, and repeatedly cleaning for three times to obtain NaYF4:Er3+,Yb3+Nanoparticles, finally dispersed in cyclohexane;
b: preparation of NaYF4:Er3+,Yb3+@NaYF4Nanoparticles
B-1: weighing 2mmol YCl3•6H2O, adding 12 mL of oleic acid and 30 mL of 1-octadecene, vacuumizing the mixed solution, heating to 130 ℃, keeping for 40min, and naturally cooling to room temperature to obtain a solution C;
b-2: the NaYF obtained in the step A-34:Er3+,Yb3+Dropwise adding the nanoparticles into the solution C, stirring at room temperature for 30min, heating to 62 ℃ under the argon atmosphere to distill out methanol, then heating to 300 ℃, maintaining for 40min, and then cooling to room temperature to obtain a solution D;
b-3: 0.2000 g of NaOH and 0.2963 g of NH were weighed out4F, dissolving the mixture in 10 mL of methanol solution, dropwise adding the mixed methanol solution into the solution D to obtain an emulsion, stirring at room temperature for 30min, heating to 62 ℃ under argon atmosphere to distill out methanol, heating to 300 ℃, maintaining for 1 hour, and cooling to room temperature to obtain a solution E;
b-4: centrifuging the solution E at the rotating speed of 9200 rpm for 15 min, taking absolute ethyl alcohol as a cleaning solution, ultrasonically cleaning the particles obtained after centrifugation for 5 min, and repeatedly cleaning for three times to obtain NaYF4:Er3+,Yb3+@NaYF4Dispersing the nano particles in cyclohexane to obtain NaYF4:Er3+,Yb3+@NaYF4A solution;
c: preparation CAu
C-1: preparing a growth solution:
weighing 7 g of CTAB and 1.234 g of NaOL, pouring into a conical flask, adding 250 mL of deionized water, stirring for 20-30min, standing the mixed solution in a drying oven at 28-32 ℃ for 15-20 min;
② Erlenmeyer flask was charged with 24 mL of AgNO3(4 mM) solution, standing the mixed solution in a drying oven at 28-32 ℃ for 15-20 min;
③ into the Erlenmeyer flask was added 250 mL of HAuCl4(1 mM) solution, stirring the obtained solution for 90-110 min at the rotating speed of 700-800 rpm to obtain a growth solution;
c-2: preparing seeds:
① mix 5 mL of HAuCl4(0.5 mM) solution and 5 mL CTAB (0.2M) solution were mixed into a 15 mL centrifuge tube;
② Add 600. mu.L of NaBH to the 15 mL centrifuge tube4(0.01M) adding an ice water solution, covering the ice water solution, rapidly shaking the centrifugal tube, observing that the solution is changed into light brown from yellow, and putting the solution into a drying box at the temperature of 28-32 ℃ for 30-40min to obtain a seed solution;
c-3: adding the reagent dropwise to prepare CAu
Adding 3.6 mL of HCl (37% wt) into the growth solution, and stirring at the rotation speed of 350-450rpm for 15-20 min;
adding 1.25 mL of AA (0.064M) into the conical flask, and stirring for 30-35 s at the rotating speed of 1400-1600 rpm;
thirdly, 0.4 mL of prepared seed liquid is added into the conical flask, stirred for 30-35 s at the rotating speed of 1400-32 rpm and then placed into a drying box at 28-32 ℃ for 12-14 h to obtain CAu;
D. the preparation of the nano-composite system is carried out,
2mmol of NaYF is taken4:Er3+,Yb3+@NaYF4500 mu L of the solution is centrifuged for 15-20min at the rotating speed of 9000-11000 rpm, and 1.8 mL of toluene and 0.2mL of the supernatant are addedCarrying out ultrasonic 5 min on a toluene solution (10 mg/mL) of mL PMMA to uniformly disperse, dropwise adding the mixed solution on a cleaned silicon wafer to prepare a single-layer film by using a spin coating method (pre-rotation is carried out for 600 rpm/5 s, and forward rotation is carried out for 2000 rpm/30 s), naturally drying, dropwise adding CAu on the film, and blow-drying to obtain CAu&NaYF4:Er3+,Yb3 +@NaYF4A single layer nanocomposite film.
FIG. 1 (a) shows NaYF4:Er3+,Yb3+@NaYF4SEM image of single layer film, it can be seen that the size of the particles is about 45nm, the uniformity of the particles is better, FIG. 1 (b) is NaYF4:Er3+,Yb3+@NaYF4SEM of the cross section of the single-layer film shows that the cross section thickness is about 45nm and is consistent with the particle size, which indicates that NaYF is successfully prepared4:Er3+,Yb3+@NaYF4A single layer film.
FIG. 2 (a) is an SEM of CAu, from which it can be seen that: CAu has good dispersibility, uniform appearance and size, and particle diameter of about 110 nm and 20 nm. Fig. 2 (b) shows the uv-vis-ir extinction spectrum of CAu, from which: CAu has two extinction peaks, located at 517 nm and 970nm, wherein 517 nm is a transverse resonance extinction peak, 970nm is a longitudinal resonance extinction peak, at this time, CAu longitudinal resonance extinction peak can be matched with excitation light (980 nm), excitation efficiency can be enhanced, up-conversion rare earth ion luminescence is enhanced, and the distance between 517 nm peak position and 980 nm is far away, and the peak position is small, and influence on excitation efficiency can be ignored. Fig. 2 (c) shows the field intensity distribution of a single field CAu simulated by FDTD, which shows that: CAu the tip has a strong enhanced electric field, which in turn creates a hot spot. When the incident light acts on CAu, surface plasmon polaritons are generated around the incident light, the local field intensity effect is enhanced, and the emission efficiency of nearby up-conversion rare earth ions can be effectively enhanced. FIG. 2 (d) shows CAu simulated extinction spectra of FDTD, which shows that there are two plasmon resonance peaks at 517 nm and 970 nm. Compared with the CAu extinction spectrum measured by experiments, the extinction spectrum and the FDTD simulated plasma resonance peak are relatively consistent in peak position.
CAu in FIG. 3&NaYF4:Er3+,Yb3+@NaYF4The fluorescence spectrum is converted on the micro-area. We measured 5 micro-domain up-conversion fluorescence spectra with CAu regions and 5 without CAu regions, as shown in fig. 3 (a), and the peak areas of each spectrum are shown in fig. 3 (b). As can be seen from fig. 3 (a) and 3 (b), the red and green upconversion with CAu regions is enhanced with maximum enhancement factors of 1.57 and 1.65, respectively.
Claims (10)
1. CAu for modulating the solar spectrum&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: which comprises the following steps:
a: preparation of NaYF4:Er3+,Yb3+Nanoparticles
A-1: weighing RECl with the total amount of 2mmol according to the molar ratio3•6H2O, RE = Y/Er/Yb, 12 mL of oleic acid and 30 mL of 1-octadecene are added, the mixed solution is vacuumized and heated to 125-135 ℃, and the mixed solution is naturally cooled to room temperature after being kept for 40-45 min, so as to obtain a solution A;
a-2: 0.2000 g of NaOH and 0.2963 g of NH were weighed out4F, dissolving in methanol, dropwise adding the mixed methanol solution into the solution A, stirring at room temperature for 30-40min, heating to 62-63 ℃ under the argon atmosphere to distill out the methanol, then heating to 300-320 ℃, maintaining for 1-1.2 hours, and then cooling to room temperature to obtain a solution B;
a-3: centrifuging the solution B, and ultrasonically cleaning particles obtained after centrifugation to obtain NaYF4:Er3+,Yb3+Nanoparticles, finally dispersed in cyclohexane;
b: preparation of NaYF4:Er3+,Yb3+@NaYF4Nanoparticles
B-1: weighing 2mmol YCl3•6H2O, adding 12 mL of oleic acid and 30 mL of 1-octadecene, vacuumizing the mixed solution, heating to 125-135 ℃, keeping the temperature for 40-45 min, and naturally cooling to room temperature to obtain a solution C;
b-2: the NaYF obtained in the step A-34:Er3+,Yb3+Dropwise adding the nanoparticles into the solution C, stirring at room temperature for 30-40min, heating to 62-63 ℃ under the argon atmosphere to distill out methanol, then heating to 300-320 ℃, maintaining for 40-50 min, and cooling to room temperature to obtain a solution D;
b-3: 0.2000 g of NaOH and 0.2963 g of NH were weighed out4F, dissolving the mixed methanol solution in a methanol solution, dropwise adding the mixed methanol solution into the solution D to obtain an emulsion, stirring at room temperature for 30-40min, heating to 62-63 ℃ under an argon atmosphere to distill off methanol, then heating to 300-320 ℃, maintaining for 1-1.2 hours, and then cooling to room temperature to obtain a solution E;
b-4: centrifuging the solution E, and ultrasonically cleaning particles obtained after centrifugation to obtain NaYF4:Er3+,Yb3+@NaYF4Dispersing the nano particles in cyclohexane to obtain NaYF4:Er3+,Yb3+@NaYF4A solution;
c: preparation CAu
C-1: preparing a growth solution:
weighing 7 g of CTAB and 1.234 g of NaOL, pouring into a conical flask, adding 250 mL of deionized water, stirring for 20-30min, standing the mixed solution in a drying oven at 28-32 ℃ for 15-20 min;
② Erlenmeyer flask was charged with 24 mL of AgNO3Standing the mixed solution in a drying oven at 28-32 deg.C for 15-20 min;
③ into the Erlenmeyer flask was added 250 mL of HAuCl4Solution, stirring the obtained solution at the rotating speed of 700-800 rpm for 90-110 min to obtain growth liquid;
c-2: preparing seeds:
① mix 5 mL of HAuCl4Mixing the solution and 5 mL CTAB solution into a 15 mL centrifuge tube;
② Add 600. mu.L of NaBH to the 15 mL centrifuge tube4Uniformly shaking the ice water solution, and placing the ice water solution into a drying box at the temperature of 28-32 ℃ for 30-40min to obtain seed liquid;
c-3: adding the reagent dropwise to prepare CAu
Adding 37 wt% of HCl into the growth solution, and uniformly stirring for one time;
adding 1.25 mL of AA solution into the conical flask, and uniformly stirring for the second time;
③ adding 0.4 mL of prepared seed liquid into the conical flask, stirring evenly for three times, and then placing the conical flask into a drying oven at 28-32 ℃ for 12-14 h to obtain CAu;
D. the preparation of the nano-composite system is carried out,
2mmol of NaYF is taken4:Er3+,Yb3+@NaYF4500 mu L of solution is centrifuged, 1.8 mL of toluene and 0.2mL of PMMA toluene solution are added after supernatant is removed, ultrasonic dispersion is uniform, the mixed solution is dripped on a cleaned silicon wafer, a single-layer film is prepared by a spin coating method, CAu is dripped on the film after natural drying, and blowing and drying are carried out to obtain CAu&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film.
2. CAu for modulating the solar spectrum according to claim 1&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: in the step A-3 and the step B-4, the centrifugation is carried out for 15-20min at the rotating speed of 9000-10000rpm, and the cleaning takes absolute ethyl alcohol as a cleaning solution.
3. CAu for modulating the solar spectrum according to claim 1&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: in step C-1, the AgNO3The molar concentration of the solution is 4 mM, and the HAuCl is4The molarity of the solution was 1 mM.
4. CAu for modulating the solar spectrum according to claim 1&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: in step C-2, the HAuCl4The molarity of the solution was 0.5 mM, the molarity of the CTAB solution was 0.2M, and the NaBH was added4The molar concentration of the ice-water solution was 0.01M.
5. CAu for modulating the solar spectrum according to claim 1&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: in the step C-3, the molar concentration of the AA solution is 0.064M, the primary stirring is carried out for 15-20min at the rotating speed of 350-1600 rpm, and the secondary stirring is carried out for 30-35 s at the rotating speed of 1400-1600 rpm; the three times of stirring are evenly stirred for 30-35 s at the rotating speed of 1400-1600 rpm.
6. CAu for modulating the solar spectrum according to claim 1&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: in the step D, the centrifugation is carried out for 15-20min at the rotating speed of 9000-11000 rpm, and the concentration of the PMMA toluene solution is 10 mg/mL.
7. CAu for modulating the solar spectrum according to claim 1&NaYF4:Er3+,Yb3+@NaYF4The preparation method of the single-layer nano composite film is characterized by comprising the following steps: in the step D, during spin coating, the spin coating is performed for 5 s at a rotation speed of 600rpm, and then the spin coating is performed for 30 s at a rotation speed of 2000 rpm.
8. CAu obtained by the process according to any one of claims 1 to 7&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film.
9. CAu according to claim 8&NaYF4:Er3+,Yb3+@NaYF4A single layer nanocomposite film characterized by: the effective excitation wavelength of the composite film is 980 nm.
10. The CAu of claim 8&NaYF4:Er3+,Yb3+@NaYF4The application of the single-layer nano composite film in a solar cell.
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