CN109326672A - A kind of preparation method of the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot - Google Patents
A kind of preparation method of the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot Download PDFInfo
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- CN109326672A CN109326672A CN201810965934.7A CN201810965934A CN109326672A CN 109326672 A CN109326672 A CN 109326672A CN 201810965934 A CN201810965934 A CN 201810965934A CN 109326672 A CN109326672 A CN 109326672A
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- H—ELECTRICITY
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
- H01L31/054—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means
- H01L31/055—Optical elements directly associated or integrated with the PV cell, e.g. light-reflecting means or light-concentrating means where light is absorbed and re-emitted at a different wavelength by the optical element directly associated or integrated with the PV cell, e.g. by using luminescent material, fluorescent concentrators or up-conversion arrangements
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to a kind of preparation methods of solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot, belong to photo-electroluminescence technical field.The full-inorganic perovskite quantum dot of halogen doping is made the following steps are included: S1, be injected into caesium-oleic acid mixed solution before lead halide in body fluid by hot injection method in preparation method of the invention；S2, full-inorganic perovskite quantum dot and photoinitiator are dissolved in allyl monomer, and it is mixed with polythiol monomer, form mixed liquor, it is poured into mold after mixed liquor is ultrasonically treated 0.5-1.5min, it is dried 25-35min in vacuum environment, is then solidified using ultraviolet lamp irradiation, after solidification demoulding, using cutting, polishing process, the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot can be obtained.Solar energy fluorescence optical collector produced by the present invention is environmentally protective, good mechanical property；Spectral absorption range is wide, and adjustable, can be suitable for various different solar-energy photo-voltaic cells；Collection efficiency is high.
Description
Technical field
The invention belongs to photo-electroluminescence technical fields, are related to a kind of solar energy fluorescence based on full-inorganic perovskite quantum dot
The preparation method of optical collector.
Background technique
In past 150 years, as energy crisis and problem of environmental pollution become increasingly conspicuous, photovoltaic industry is by increasingly
Extensive concern.Over nearly 5 years, global photovoltaic technology is grown rapidly, and the yield and installation of photovoltaic module sharply rise.Currently,
In photovoltaic electrification component, battery material cost accounts for about 55%.Relative to component installation cost and other artificial costs, battery material
Expect that cost is high, this is the maximum technical problem faced in theCourse of PV Industry.In photovoltaic device incident photon-to-electron conversion efficiency one
In the case where fixed, more incident sunlights are obtained on unit area by optical collector, thus will be more substantially effectively using too
Sunlight provides a feasible technological approaches for the cost of photovoltaic device is greatly lowered.Traditional optical collector can pass through
Concave mirror and convex lens array are realized.In order to avoid mutually blocking between reflective mirror, building for traditional optical collector is needed
Occupy a large amount of place spaces.More serious problem is that angle of incidence of sunlight degree constantly changes, and concave mirror and convex lens need
To be rotated in real time according to sun angular, a set of pair day tracing system will greatly increase the use cost of traditional solar collector.
In order to reduce the use cost of traditional optical collector, further promote collection efficiency, the scientific research of the W.Weber of Ford of the U.S. is small
Group proposes the concept of solar energy fluorescence optical collector first.Fluorescence luminescent material is introduced into the transparent optical waveguides such as high refractive index polymer
In, while pasting solar battery panel in side, that is, constitute fluorescence solar collector.Fluorescent material in transparent medium is inhaled
Fluorescence is re-emitted after receiving sunlight, the fluorescence that the angle of departure is greater than critical angle will be finally installed after multiple total reflection
The solar battery panel of side is absorbed, and the sunlight for realizing large area is gathered small area solar battery by this technology
Purpose on panel.Compared with traditional optical collector, fluorescence solar collector has a clear superiority: 1. making full use of fluorescent material system
At optical waveguide realize sunlight aggregation and transmission, do not need that accurate focal point tracking system is installed；2. fuel factor is bright
It is aobvious to reduce；3. largely replacing expensive solar panel with media such as cheap polymer, photovoltaic industry cost is significant
It reduces；4. it is high with building compatibility, it is widely portable to the occasions such as roof, the glass curtain wall of building.
The core of solar energy fluorescence optical collector is the light emission central material in optical waveguide matrix.In solar energy fluorescence optical collector
During photon transport, the photon that the centre of luminescence issues is possible to that optical collector can not be reached by adjacent centre of luminescence reabsorption
The solar battery panel of side.On the other hand, the photon of light emission central material transmitting is in light guide surface likely to be less than complete
Angle of reflection, so as to cause photonic surface escape.Therefore, the technical bottleneck that limitation fluorescence solar collector photon collection efficiency improves
It is how to reduce the surface escapement ratio of reabsorption probability and reduction photon during photon transmission.Good solar energy fluorescence
Optical collector light emission central material should have following spectroscopy feature: 1. wide spectrum absorbs；2. in entire absorption spectrum ranges,
Absorption efficiency is high；3. big Stokes shift；4. high luminous efficiency；5. the optimal spectrum of emission wavelength and solar battery
Response matches.There is full-inorganic perovskite quantum dot relatively wide spectral absorption and excellent monochromaticjty to shine, luminescent quantum
Yield is higher than 50%, and is easy to realize the regulation absorbed with launch wavelength by changing its chemical constituent.
Summary of the invention
The purpose of the present invention is high, the photon escape probabilities for reabsorption rate present in existing solar energy fluorescence optical collector
The high, technical problems such as collection efficiency is low, propose a kind of solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot
Preparation method, solar energy fluorescence optical collector obtained can effectively reduce during photon transport centre of luminescence reabsorption probability with
Photon escape probability has high collection efficiency, through preliminary test, the solar energy fluorescence collection based on full-inorganic perovskite quantum dot
The collection efficiency of light antetype device is greater than 5%.
Object of the invention can be realized by the following technical scheme:
A kind of preparation method of the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot, the preparation method packet
Include following steps,
The preparation of S1, full-inorganic perovskite quantum dot: caesium-oleic acid mixed solution is injected into lead halide by hot injection method
In preceding body fluid, the full-inorganic perovskite quantum dot of halogen doping is made；
The preparation of S2, solar energy fluorescence optical collector: full-inorganic perovskite quantum dot and photoinitiator are dissolved in allyl list
Body, and mixed with polythiol monomer, it is poured into mold after being ultrasonically treated 0.5-1.5min, 25- is dried in vacuum environment
35min, the heated at constant temperature 25-35min at a temperature of 65-75 DEG C are then solidified using ultraviolet lamp irradiation.Solidification demoulding
Afterwards, using cutting, polishing process, the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot can be obtained.
The present invention uses the photon transport basis material of mercaptan alkene copolymer (OSTE) as planar solar concentrator, with a variety of
Light emission central material of the full-inorganic perovskite quantum dot of halogen doping as planar solar concentrator, realizing has higher light harvesting
The preparation of the solar energy fluorescence light harvesting antetype device of efficiency.In terms of the reason of antetype device high collection efficiency, is following four:
First, compared to polymeric matrix materials such as traditional PMMA, PDMS, OSTE has higher theoretical refractive index (> 1.7), more
The photon escape rate in solar energy fluorescence light harvesting antetype device will be effectively reduced in the big angle of total reflection；Second, compared to existing
For the light emission central materials such as CdS, Si, CIGS, InP quantum dot, full-inorganic perovskite quantum dot of the invention has higher
Solar energy fluorescence will be effectively reduced in fluorescence quantum yield (> 50%), bigger Stokes shift, excellent spectroscopic properties
Photon reabsorption probability in light harvesting antetype device；Third, the present invention is quantum dot-doped by halogen and full-inorganic perovskite, realizes
The function of giving out light of full-inorganic perovskite quantum dot, and there is good stability of photoluminescence and monochromaticjty；4th, compared to existing
For the luminescent organic dyes molecule such as some Coumarin, Rhodamine, the full-inorganic perovskite amount of halogen doping in the present invention
Son point has better stability of photoluminescence and monochromaticjty.And full-inorganic perovskite quantum of the present invention makes compared with tradition
The noxious materials such as CdS quantum dot, it is more environmentally protective；The centres of luminescence such as the CIGS quantum dot used compared with tradition, cost
It is cheaper.
The present invention is added after the full-inorganic perovskite quantum dot of different halogen dopings using super in polymer monomer material
The process such as sonication, heated at constant temperature, vacuum drying, ultraviolet light solidification, demoulding, polishing fill full-inorganic perovskite quantum dot
Point dissolution and it is evenly dispersed into polymer monomer material.
Preferably, caesium-oleic acid mixed solution preparation process is in the step S1, by oleic acid (OA) and metatitanic acid caesium
(Cs2CO3) be added in octadecylene (ODE) and be stirred and heated to 190-210 DEG C, until white powder is completely dissolved, then true
0.8-1.2h is kept the temperature in Altitude at a temperature of 125-135 DEG C, that is, caesium-oleic acid mixed solution is made.
Preferably, in the step S1 in caesium-oleic acid mixed solution preparation process, described OA, Cs2CO3, ODE adds
Dosage is calculated according to following ratio: every 1g Cs2CO3Match 2.6-3.4mL OA, 45-55mL ODE.
Preferably, at a temperature of caesium-oleic acid mixed solution is stored in not less than 80 DEG C in the step S1, to avoid heavy
It forms sediment.
Preferably, in the step S1 before lead halide body fluid preparation process are as follows: by OA, oleyl amine (OLA), ODE and halogen
Change lead (PbX2) solid powder mixing, handle 25-35min at a temperature of 90-110 DEG C in vacuum environment to get lead halide is arrived
Preceding body fluid, described OA, OLA, ODE and PbX2The additive amount of solid powder is calculated according to following ratio: every 0.35-0.40mmol
PbX2Solid powder matches 1ml OA, 1ml OLA, 10ml ODE.
Preferably, PbX in the step S12For PbCl2、PbBr2、PbI2One of or a variety of (i.e. PbX2Middle X=
Cl、Br、I)。
Preferably, PbX in the step S12For PbCl2、PbBr2、PbI2In two or three.
Two samples of light emission central materials such as the full-inorganic perovskite quantum dot compared to single halogen doping, a variety of halogen dopings
Full-inorganic quantum dot have broader spectral absorption range (can reach 400nm to 700nm).The present invention is by using by two kinds
Or three kinds of lead halides compound the accurate adjusting, it can be achieved that inorganic perovskite quantum dot light emitting peak position, adjustable hair with special ratios
Photopeak position is easier to a variety of best response spectrums applied to the commercial photovoltaic devices based on different semiconductor materials, to make this hair
Bright optical collector can be applied to a variety of different solar-energy photo-voltaic cells；Meanwhile between different halogen dopings there is collaboration to make
With can further improve the collection efficiency of optical collector of the present invention.
Preferably, body fluid is stored in N before the lead halide2In environment.
Preferably, the detailed process of hot injection method is in the step S1, by body fluid before lead halide in vacuum environment
It is heated to 125-135 DEG C of heat preservation 25-35min, 155-165 DEG C is then heated to, is then rapidly injected caesium-oleic acid solutions,
4-6min is kept at 155-165 DEG C, then is quickly cooled down to get full-inorganic perovskite quantum dot is arrived.
Preferably, caesium-oleic acid solutions are injected into the ratio before lead halide in body fluid according to Cs and Pb in the step S1
Molar ratio be 1:(1-1.5) calculate.
Preferably, the full-inorganic perovskite quantum dot of halogen doping obtained is stored in vacuum drying in the step S1
In device or -10 DEG C of refrigerators.
Full-inorganic perovskite quantum dot obtained is very sensitive to humidity in the present invention, to avoid and the water in air environment
Molecule contacts occur to go bad, and need to be stored in drier or -10 DEG C of refrigerators.
Preferably, the concentration of full-inorganic perovskite quantum dot is 10 in the mixed liquor of the step S2-7-10-4mol/L。
Preferably, in the mixed liquor of the step S2, the content of photoinitiator, allyl monomer and polythiol monomer according to
Following ratio calculates, every 1g photoinitiator proportion 80-120mL allyl monomer and 80-120mL polythiol monomer.
Preferably, photoinitiator described in step S2 is 1- hydroxycyclohexylphenylketone, propyl monomer is triallyl-
1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketones, polythiol monomer are pentaerythrite four (3-thiopropionate).
Preferably, mold described in step S2 is Teflon mold.
Preferably, the preparation method further includes with mold pre-treatment step, specifically, preparing solar energy fluorescence
Mold is successively cleaned by ultrasonic before optical collector, dehydrated alcohol is handled, blotting paper is wiped to die surface drying.
It is carried out in the vacuum environment not higher than 133Pa preferably, being dried in the step S2.
Preferably, heated at constant temperature is heating water bath in the step S2.
Preferably, the power that ultraviolet lamp irradiates in the step S2 is not less than 50W, central wavelength 365nm, when irradiation
Between be 8-12s.
Compared with prior art, the invention has the following advantages: solar energy fluorescence optical collector produced by the present invention is green
Colour circle is protected, good mechanical property；Spectral absorption range is wide, and adjustable, can be suitable for various different solar-energy photo-voltaic cells；Collection
Light efficiency is high.
Detailed description of the invention
Fig. 1 is in the embodiment of the present invention 1 using the full-inorganic perovskite CsPbBr of hot injection method preparation3The transmission of quantum dot
Electron microscope picture (a), size distribution statistics figure (b), high resolution transmission electron microscopy (c).
Fig. 2 is different halogen full-inorganic perovskite quantum dots obtained in the embodiment of the present invention 1, embodiment 2 and embodiment 3
Fluorescence emission spectrum (a) and absorption spectra (b).
Fig. 3 is the fluorescence for the full-inorganic perovskite quantum dot that a variety of halogens obtained are composite mixed in the embodiment of the present invention 4
Emission spectra.
Fig. 4 is the weight of the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot made from the embodiment of the present invention 1
(c) and collection efficiency (d) is lost with the change of quantum dot doping concentration in absorption loss (a), again launch loss (b), photon escape
Change relationship.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
The preparation method of solar energy fluorescence optical collector in the present embodiment based on perovskite quantum dot includes the following steps,
(1) caesium-oleic acid mixed solution is prepared: by 0.6mL OA and 0.2g Cs2CO3It is added in 9.8mL ODE, stirring is simultaneously
200 DEG C are heated to, until white powder is completely dissolved, then 1.0h is kept the temperature at a temperature of 130 DEG C in vacuum environment, that is, is made
Caesium-oleic acid mixed solution, at a temperature of caesium obtained-oleic acid mixed solution is stored in not less than 80 DEG C, to avoid precipitating.
(2) body fluid before lead halide is prepared: by 1mL OA, 1mL OLA, 10mL ODE and 0.376mmol PbBr2Solid powder
End is added in the round-bottomed flask of 100mL, is placed in vacuum environment isothermal holding 30min at a temperature of 100 DEG C and is obtained lead halide
Preceding body fluid, wherein OLA solution and OA solution need to be rapidly injected in nitrogen atmosphere at 100 DEG C, by lead halide precursor obtained
Liquid is stored in N2In environment.
(3) it prepares full-inorganic perovskite quantum dot: body fluid before lead halide is heated to 130 DEG C of heat preservations in vacuum environment
30min, then heats to 160 DEG C, is then rapidly injected caesium-oleic acid solutions, makes the molar ratio of caesium-oleic acid solutions Cs and Pb
1:1 keeps 5min, then water-bath to be quickly cooled down to get CsPbBr is arrived at 160 DEG C3Quantum dot, full-inorganic perovskite amount obtained
Son point is stored in vacuum desiccator or -10 DEG C of refrigerators.
(4) preparation of solar energy fluorescence optical collector: Teflon mold is successively cleaned by ultrasonic, dehydrated alcohol processing,
Blotting paper wipes dry to die surface；By CsPbBr3Quantum dot and 0.02g photoinitiator (1- hydroxycyclohexylphenylketone,
Irgacure-184 it) is dissolved in 2mL allyl monomer (triallyl -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketones), and with
2mL polythiol monomer (pentaerythrite four (3-thiopropionate)) is mixed to form mixed liquor, makes CsPbBr3Quantum dot is in mixed liquor
Concentration be 2.1 × 10-5Mol/L is poured into Teflon mold after mixed liquor is ultrasonically treated 1min, in not higher than 133Pa's
30min is dried in vacuum environment, the water-bath heated at constant temperature 30min at 70 DEG C is then consolidated using ultraviolet light
Change, the power of ultraviolet lamp irradiation is that 100W, central wavelength 365nm, irradiation time 10s are thrown after final curing demoulding
Light technology to get arrive solar energy fluorescence optical collector.
Embodiment 2
PbX2For PbCl2, other are same as Example 1.
Embodiment 3
PbX2For PbI2, other are same as Example 1.
Embodiment 4
PbX2For PbCl2、PbBr2、PbI2In two or three of mixing, PbCl2、PbBr2、PbI2Molar ratio be
(0-1): (0-1): the mixture of (0-1), other are same as Example 1.
Embodiment 5
The preparation method of solar energy fluorescence optical collector in the present embodiment based on perovskite quantum dot includes the following steps,
(1) caesium-oleic acid mixed solution is prepared: by 0.5mL OA and 0.2g Cs2CO3It is added in 9.0mL ODE, stirring is simultaneously
190 DEG C are heated to, until white powder is completely dissolved, then 0.8h is kept the temperature at a temperature of 125 DEG C in vacuum environment, that is, is made
Caesium-oleic acid mixed solution, at a temperature of caesium obtained-oleic acid mixed solution is stored in not less than 80 DEG C, to avoid precipitating.
(2) body fluid before lead halide is prepared: by 1mL OA, 1mL OLA, 10mL ODE and 0.35mmol PbBr2Solid powder
It is added in the round-bottomed flask of 50mL, is placed in vacuum environment isothermal holding 30min at a temperature of 90 DEG C and obtains lead halide precursor
Liquid, wherein OLA solution and OA solution need to be rapidly injected in nitrogen atmosphere at 90 DEG C, and body fluid before lead halide obtained is stored
In N2In environment.
(3) it prepares full-inorganic perovskite quantum dot: body fluid before lead halide is heated to 125 DEG C of heat preservations in vacuum environment
25min, then heats to 155 DEG C, is then rapidly injected caesium-oleic acid solutions, makes the molar ratio of caesium-oleic acid solutions Cs and Pb
1:1 keeps 4min, then water-bath to be quickly cooled down to get CsPbBr is arrived at 155 DEG C3Quantum dot, full-inorganic perovskite amount obtained
Son point is stored in vacuum desiccator or -10 DEG C of refrigerators.
(4) preparation of solar energy fluorescence optical collector: Teflon mold is successively cleaned by ultrasonic, dehydrated alcohol processing,
Blotting paper wipes dry to die surface；By CsPbBr3Quantum dot and 0.02g photoinitiator (1- hydroxycyclohexylphenylketone,
Irgacure-184 it) is dissolved in 1.6mL allyl monomer (triallyl -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketones), and
It is mixed to form mixed liquor with 2.4mL polythiol monomer (pentaerythrite four (3-thiopropionate)), makes CsPbBr3Quantum dot is mixing
Concentration in liquid is 2.1 × 10-7Mol/L, will mixed liquor be ultrasonically treated 0.5min after pour into Teflon mold, in being not higher than
It is dried 30min in the vacuum environment of 133Pa, the water-bath heated at constant temperature 25min at 65 DEG C then uses ultraviolet light
Being solidified, the power of ultraviolet lamp irradiation is 130W, central wavelength 365nm, irradiation time 8s, after final curing demoulding,
Polishing process is carried out to get solar energy fluorescence optical collector is arrived.
Embodiment 6
The preparation method of solar energy fluorescence optical collector in the present embodiment based on perovskite quantum dot includes the following steps,
(1) caesium-oleic acid mixed solution is prepared: by 0.68mL OA and 0.2g Cs2CO3It is added in 11mL ODE, stirring is simultaneously
210 DEG C are heated to, until white powder is completely dissolved, then 1.2h is kept the temperature at a temperature of 135 DEG C in vacuum environment, that is, is made
Caesium-oleic acid mixed solution, at a temperature of caesium obtained-oleic acid mixed solution is stored in not less than 80 DEG C, to avoid precipitating.
(2) body fluid before lead halide is prepared: by 1mL OA, 1mL OLA, 10mL ODE and 0.40mmol PbBr2Solid powder
It is added in the round-bottomed flask of 50mL, is placed in vacuum environment isothermal holding 35min at a temperature of 110 DEG C and obtains lead halide precursor
Liquid, wherein OLA solution and OA solution need to be rapidly injected in nitrogen atmosphere at 110 DEG C, and body fluid before lead halide obtained is stored up
It is stored in N2In environment.
(3) it prepares full-inorganic perovskite quantum dot: body fluid before lead halide is heated to 135 DEG C of heat preservations in vacuum environment
35min, then heats to 165 DEG C, is then rapidly injected caesium-oleic acid solutions, makes the molar ratio of caesium-oleic acid solutions Cs and Pb
1:1.5 keeps 6min, then water-bath to be quickly cooled down to get CsPbBr is arrived at 165 DEG C3Quantum dot, full-inorganic perovskite obtained
Quantum dot is stored in drier or -10 DEG C of refrigerators.
(4) preparation of solar energy fluorescence optical collector: Teflon mold is successively cleaned by ultrasonic, dehydrated alcohol processing,
Blotting paper wipes dry to die surface；By CsPbBr3Quantum dot and 0.02g photoinitiator (1- hydroxycyclohexylphenylketone,
Irgacure-184 it) is dissolved in 2.4mL allyl monomer (triallyl -1,3,5-triazines -2,4,6 (1H, 3H, 5H)-triketones), and
It is mixed to form mixed liquor with 1.6mL polythiol monomer (pentaerythrite four (3-thiopropionate)), makes CsPbBr3Quantum dot is mixing
Concentration in liquid is 10-4Mol/L is poured into Teflon mold after mixed liquor is ultrasonically treated 1.5min, in not higher than 133Pa's
35min is dried in vacuum environment, the water-bath heated at constant temperature 35min at 75 DEG C is then consolidated using ultraviolet light
Change, the power of ultraviolet lamp irradiation is that 150W, central wavelength 365nm, irradiation time 12s are thrown after final curing demoulding
Light technology to get arrive solar energy fluorescence optical collector.
Solar energy fluorescence optical collector obtained is solar energy fluorescence antetype device in the embodiment of the present invention, for convenient for detection,
The size of planar solar concentrator obtained is 6.0cm × 6.0cm × 0.3cm (length × width x thickness) in the above embodiment of the present invention.
The present invention carries out full-inorganic perovskite quantum dot obtained in above-described embodiment and solar energy fluorescence optical collector
A series of optic tests and characterization, test method and result are as follows:
The Technai F20 Flied emission of FEI Co. of the U.S. is used to the structural characterization that full-inorganic perovskite quantum dot carries out
High resolution transmission electron microscopy (HR-TEM) carries out；Steady-state fluorescence transmitting (PL) spectrum of full-inorganic perovskite quantum dot uses method
The Fluorolo-3 fluorometric investigation system of Jobin Yvon company of state production, excitation light source are the He-Cd optical collector (center of 30mW
Wavelength is 325nm)；It can be seen that R928 type photomultiplier tube (PMT) of the detector using Hamamatsu company of Japan；Full-inorganic calcium
The absorption spectra test of titanium ore quantum dot uses the UV3600 UV, visible light near infrared spectrometer of Shimadzu, Japan；Entirely
The outer quantum yield test of inorganic perovskite quantum dot is tested using the Quantaurus-QY Plus of Hamamatsu company of Japan
System.The fluorescence signal of all tests of the present invention is corrected according to instrument parameter, and has deducted ambient noise.
Fig. 1 is in the embodiment of the present invention 1 using the full-inorganic perovskite CsPbBr of hot injection method preparation3The transmission of quantum dot
Electron microscope picture (a), size distribution statistics figure (b), high resolution transmission electron microscopy (c).U.S. FEI is used in test
The Technai F20 Flied emission transmission electron microscope of company, acceleration voltage are maintained at 200kV.
Find out from Fig. 1 (a), CsPbBr3Quantum dot is evenly distributed, size is more uniform.As shown in Fig. 1 (b), according to figure
As processing software ImageJ statistical result, CsPbBr3The average-size of quantum dot is 8.4 ± 2.8nm.Fig. 1 (c) is high-resolution
Full-inorganic perovskite CsPbBr3The transmission electron microscope picture of quantum dot, by Fig. 1 (c) it is found that CsPbBr obtained3Quantum dot
Interplanar distance be 0.58nm, correspond to cubic structure CsPbBr3(001) crystal face of quantum dot.High-resolution TEM picture is further
Confirm the more uniform inorganic perovskite CsPbBr with Typical cubic structure of size3The synthesis of quantum dot.
Fig. 2 is different halogen full-inorganic perovskite quantum dots obtained in the embodiment of the present invention 1, embodiment 2 and embodiment 3
Fluorescence emission spectrum (a) and absorption spectra (b).Find out from Fig. 2 (a), different halogen full-inorganic perovskite quantum dots are shown
Good luminous monochromaticjty (shine halfwidth about 20nm), high fluorescence quantum yield (> 50%).Find out from Fig. 2 (b), no
Wide absorption spectrum ranges are shown with halogen full-inorganic perovskite quantum dot.
Fig. 3 is the fluorescence for the full-inorganic perovskite quantum dot that a variety of halogens obtained are composite mixed in the embodiment of the present invention 4
(wherein, the 1st, 4,8 peak is respectively the embodiment 1-3 full-inorganic perovskite amount obtained with single halogen doping to emission spectra
The fluorescence emission spectrum of son point, the 2nd, 3 peak are PbCl2、PbBr2The composite mixed full-inorganic perovskite quantum dot of two kinds of halogens
Fluorescence emission spectrum, the 5th, 6,7 peak are PbBr2、PbI2The fluorescence of the composite mixed full-inorganic perovskite quantum dot of two kinds of halogens is sent out
Penetrate spectrum, due to map sheet limit, the fluorescence emission spectrum of the full-inorganic perovskite quantum dot of a variety of halogen dopings only selected part in Fig. 3
Middle embodiment, other quantum dots in the fluorescence emission spectrum and Fig. 3 of the full-inorganic perovskite quantum dot of a variety of halogen dopings of other ratios
Fluorescent emission figure spectrogram shape it is close, spectral region is different).As seen from Figure 3, the composite mixed full-inorganic obtained of two kinds of halogens
Perovskite quantum dot is shown good luminous monochromaticjty (shine halfwidth about 20nm) as single halogen doping, high
Fluorescence quantum yield (> 50%)；The fluorescence spectrum of different proportion halogen doping full-inorganic perovskite quantum dot can be in 404nm-
It is adjustable in 640nm.Since the optimal spectrum response wave band of the photovoltaic device based on different semiconductor materials is different, the present invention
Doping ratio by controlling a variety of halide ions can be such that the perovskite quantum dot of preparation accurately matches, and there is special spectrum to ring
The photovoltaic device of wave band is answered, and then can be applied to the solar energy fluorescence optical collector in the present invention based on perovskite quantum dot respectively
Photovoltaic device of the kind based on different semiconductor materials.
Fig. 4 is the weight of the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot made from the embodiment of the present invention 1
(c) and collection efficiency (d) is lost with the change of quantum dot doping concentration in absorption loss (a), again launch loss (b), photon escape
Change relationship.It is 2.1 × 10 in the optimal quantum dot-doped concentration of full-inorganic perovskite-5When mol/L, about 73.9% incident light
Son is not absorbed, then launch loss is 13.1%, and photon escape probability is 2.1%, and mean wavelength collection efficiency is 5.4%.
Firstly, the non-absorption probability of photon gradually decreases in fluorescence solar collector as quantum dot-doped concentration gradually increases, this meaning
More incident photons absorbed by fluorescence solar collector, corresponding mean wavelength collection efficiency is gradually increased.Then, it measures
After son point doping concentration further increases, and photon number is absorbed in fluorescence solar collector and is increased, but photon is absorbed by quantum dot
Launch loss again rise, while photon escape probability is increased slightly, and fluorescence solar collector mean wavelength collection efficiency reaches
Peak value.Further increase quantum dot doping concentration, due to the increase of launch loss and photon escape probability again, mean wavelength collection
Light efficiency is gradually declined slightly instead.Therefore, the optimal amount of the fluorescence solar collector part based on full-inorganic perovskite quantum dot
Son point doping concentration is 2.1 × 10-5Mol/L, at this point, the collection efficiency of corresponding optimal solar energy fluorescence optical collector is 5.4%.
The collection efficiency of solar energy fluorescence optical collector obtained is respectively 5.3% and 5.2% in the embodiment of the present invention 2,3.
The collection efficiency of solar energy fluorescence optical collector obtained is between 5.8-6.2% in the embodiment of the present invention 4.
The collection efficiency of solar energy fluorescence optical collector obtained is respectively 5.3% and 5.4% in the embodiment of the present invention 5,6.
Finally, it should be noted that since the conditional relationships such as collection efficiency and its size of solar energy fluorescence optical collector are huge
Greatly, and the present invention is convenient for detection, the solar energy fluorescence optical collector size prepared in above-described embodiment is smaller, if made
At larger size, collection efficiency will have and greatly improve, and can be at least up to 10% or more.
Collection efficiency in the present invention is to measure the module of fluorescence solar collector, is defined as receiving under each wavelength
Collect the ratio between number of photons and incident light subnumber, herein using mean wavelength collection efficiency as module, too according to AM1.5 standard
Number of photons under solar spectrum is weighted and averaged.Solar battery is defined as to collect number of photons and be incident on number of photons on optical collector
The ratio between.Collection efficiency in the present invention is tested under the conditions of AM1.5 standard solar spectrum.
Specific embodiment described herein is only an example for the spirit of the invention.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
Claims (10)
1. a kind of preparation method of the solar energy fluorescence optical collector based on full-inorganic perovskite quantum dot, which is characterized in that described
Preparation method includes the following steps,
The preparation of S1, full-inorganic perovskite quantum dot: caesium-oleic acid mixed solution is injected into lead halide precursor by hot injection method
In liquid, the full-inorganic perovskite quantum dot of halogen doping is made；
The preparation of S2, solar energy fluorescence optical collector: being dissolved in allyl monomer for full-inorganic perovskite quantum dot and photoinitiator, and
It is mixed with polythiol monomer, forms mixed liquor, poured into mold after mixed liquor is ultrasonically treated 0.5-1.5min, in vacuum environment
It is dried 25-35min, then the heated at constant temperature 25-35min at a temperature of 65-75 DEG C, is then carried out using ultraviolet lamp irradiation
After solidification demoulding, using cutting, polishing process, it is glimmering that the solar energy based on full-inorganic perovskite quantum dot can be obtained in solidification
Light optical collector.
2. preparation method according to claim 1, which is characterized in that caesium-oleic acid mixed solution system in the step S1
Standby process is, by oleic acid (OA) and metatitanic acid caesium (Cs2CO3) be added in octadecylene (ODE) and be stirred and heated to 190-210 DEG C, directly
It is completely dissolved to white powder, then keeps the temperature 0.8-1.2h at a temperature of 125-135 DEG C in vacuum environment, that is, caesium-oil is made
Sour mixed solution.
3. preparation method according to claim 2, which is characterized in that caesium-oleic acid mixed solution system in the step S1
During standby, described OA, Cs2CO3, ODE additive amount calculated according to following ratio: every 1g Cs2CO3Match 2.6-3.4mL
OA、45-55mL ODE。
4. preparation method according to claim 1, which is characterized in that in the step S1 before lead halide body fluid preparation
Journey are as follows: by OA, oleyl amine (OLA), ODE and lead halide (PbX2) solid powder mixing, in 90-110 DEG C of temperature in vacuum environment
Lower processing 25-35min is to get to body fluid before lead halide.
5. the preparation method according to claim 4, which is characterized in that described OA, OLA, ODE and PbX2Solid powder adds
Dosage is calculated according to following ratio: every 0.35-0.40mmol PbX2Solid powder matches 1ml OA, 1ml OLA, 10ml ODE.
6. the preparation method according to claim 4, which is characterized in that PbX in the step S12For PbCl2、PbBr2、PbI2
One of or it is a variety of.
7. the preparation method according to claim 4, which is characterized in that PbX in the step S12For PbCl2、PbBr2、PbI2
In two or three.
8. preparation method according to claim 5, which is characterized in that the detailed process of hot injection method in the step S1
For, body fluid before lead halide is heated to 125-135 DEG C of heat preservation 25-35min in vacuum environment, then heats to 155-165 DEG C,
Caesium-oleic acid solutions then are rapidly injected, 4-6min is kept at 155-165 DEG C, then are quickly cooled down to get full-inorganic perovskite is arrived
Quantum dot.
9. preparation method according to claim 1 or 5, which is characterized in that caesium-oleic acid solutions are injected into the step S1
Ratio before lead halide in body fluid is according to Cs and PbX2Molar ratio be 1:(1-1.5) calculate.
10. preparation method according to claim 1, which is characterized in that in the mixed liquor of the step S2, full-inorganic calcium titanium
The concentration of mine quantum dot is 10-7-10-4mol/L。
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