CN108735902A - Flexible all band photoelectric material, photoelectric device and its manufacturing method - Google Patents
Flexible all band photoelectric material, photoelectric device and its manufacturing method Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000002105 nanoparticle Substances 0.000 claims abstract description 56
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 53
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 49
- 239000004065 semiconductor Substances 0.000 claims abstract description 37
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 27
- HQHVZNOWXQGXIX-UHFFFAOYSA-J sodium;yttrium(3+);tetrafluoride Chemical compound [F-].[F-].[F-].[F-].[Na+].[Y+3] HQHVZNOWXQGXIX-UHFFFAOYSA-J 0.000 claims abstract description 26
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 20
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims abstract description 17
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920000301 poly(3-hexylthiophene-2,5-diyl) polymer Polymers 0.000 claims description 34
- 239000000243 solution Substances 0.000 claims description 19
- -1 rare earth trifluoroacetic acid salt Chemical class 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- MCEWYIDBDVPMES-UHFFFAOYSA-N [60]pcbm Chemical compound C123C(C4=C5C6=C7C8=C9C%10=C%11C%12=C%13C%14=C%15C%16=C%17C%18=C(C=%19C=%20C%18=C%18C%16=C%13C%13=C%11C9=C9C7=C(C=%20C9=C%13%18)C(C7=%19)=C96)C6=C%11C%17=C%15C%13=C%15C%14=C%12C%12=C%10C%10=C85)=C9C7=C6C2=C%11C%13=C2C%15=C%12C%10=C4C23C1(CCCC(=O)OC)C1=CC=CC=C1 MCEWYIDBDVPMES-UHFFFAOYSA-N 0.000 claims description 15
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 14
- 150000002500 ions Chemical class 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 12
- 239000011258 core-shell material Substances 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- UYCAUPASBSROMS-AWQJXPNKSA-M sodium;2,2,2-trifluoroacetate Chemical compound [Na+].[O-][13C](=O)[13C](F)(F)F UYCAUPASBSROMS-AWQJXPNKSA-M 0.000 claims description 10
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Divinylene sulfide Natural products C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 9
- 229920003227 poly(N-vinyl carbazole) Polymers 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 8
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 8
- 229930192474 thiophene Natural products 0.000 claims description 7
- 239000012298 atmosphere Substances 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 229920000123 polythiophene Polymers 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- OWMNIIXIMJDZDV-UHFFFAOYSA-N 2,2,2-trifluoroacetic acid;yttrium Chemical compound [Y].OC(=O)C(F)(F)F OWMNIIXIMJDZDV-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 4
- 229910052727 yttrium Inorganic materials 0.000 claims description 4
- 239000005964 Acibenzolar-S-methyl Substances 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 238000000137 annealing Methods 0.000 claims description 3
- 125000005605 benzo group Chemical group 0.000 claims description 3
- 150000001721 carbon Chemical class 0.000 claims description 3
- LQEJKDNALLXRCT-UHFFFAOYSA-N chloroform;toluene Chemical compound ClC(Cl)Cl.CC1=CC=CC=C1 LQEJKDNALLXRCT-UHFFFAOYSA-N 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- QEWYKACRFQMRMB-UHFFFAOYSA-N fluoroacetic acid Chemical compound OC(=O)CF QEWYKACRFQMRMB-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- KKFHAJHLJHVUDM-UHFFFAOYSA-N n-vinylcarbazole Chemical class C1=CC=C2N(C=C)C3=CC=CC=C3C2=C1 KKFHAJHLJHVUDM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 3
- 238000009938 salting Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000004528 spin coating Methods 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- TZIXKZZTELLTLA-UHFFFAOYSA-N 9-heptadecan-9-ylcarbazole Chemical compound C1=CC=C2N(C(CCCCCCCC)CCCCCCCC)C3=CC=CC=C3C2=C1 TZIXKZZTELLTLA-UHFFFAOYSA-N 0.000 claims 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical class ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 6
- 230000003287 optical effect Effects 0.000 abstract description 4
- 230000005693 optoelectronics Effects 0.000 abstract description 3
- 230000005284 excitation Effects 0.000 description 10
- 230000007704 transition Effects 0.000 description 10
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000011257 shell material Substances 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 4
- 230000002787 reinforcement Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 229920000139 polyethylene terephthalate Polymers 0.000 description 3
- 239000005020 polyethylene terephthalate Substances 0.000 description 3
- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical group ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 description 2
- 229910000661 Mercury cadmium telluride Inorganic materials 0.000 description 2
- 150000003851 azoles Chemical class 0.000 description 2
- 229940049706 benzodiazepine Drugs 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940117389 dichlorobenzene Drugs 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- DTQVDTLACAAQTR-UHFFFAOYSA-M Trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- MCMSPRNYOJJPIZ-UHFFFAOYSA-N cadmium;mercury;tellurium Chemical compound [Cd]=[Te]=[Hg] MCMSPRNYOJJPIZ-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- 239000003446 ligand Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920002120 photoresistant polymer Polymers 0.000 description 1
- 238000005289 physical deposition Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
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- 239000000376 reactant Substances 0.000 description 1
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- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
- H10K30/35—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains comprising inorganic nanostructures, e.g. CdSe nanoparticles
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K2102/00—Constructional details relating to the organic devices covered by this subclass
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention provides a kind of flexible all band photoelectric material, photoelectric device and its manufacturing method, flexibility all band photoelectric material therein includes tetrafluoride yttrium sodium, ytterbium and the erbium of nano particle.Using organic semiconducting materials as flexible optoelectronic active layer, using rare earth doping nano particle as optical wavelength conversion material, by the way that the nonabsorbable infrared light of organic semiconductor is converted to the visible light that can be absorbed by organic semiconductor, to which the detection wavelength of photoelectric device is expanded to infrared region, detection of the flexible photoelectric device to all band photon is realized.The present invention has many advantages, such as that simple for process, manufacturing cost is low, all band photodetection can be achieved, photoresponse rate is high and high flexibility, has broad application prospects in multiple fields such as optical detection, wearable device, photon storage facilities.
Description
Technical field
The present invention relates to field of photoelectric technology, specifically a kind of flexible all band photoelectric material, photoelectric device and its
Manufacturing method.
Background technology
Currently, the critical material of photoelectric device mainly uses inorganic semiconductor material, such as silicon, germanium, III-V races partly to lead
Body and Group II-VI semiconductor material (GaAs, Gallium indium arsenide, cadmium telluride, cadmium mercury telluride).The spy of inorganic semiconductor photoelectric device
It surveys wavelength to be determined by band gap width, such as the band gap width of silicon materials is 1.12 eV, corresponding probing wave is a length of to be less than
1100nm.The advantages of inorganic semiconductor photoelectric device is can be by adjusting semi-conducting material constituent come the band of adjusting means
Gap width is to adjust the wave-length coverage (such as HgCdTe materials) of detected light.In order to which direct detection photon energy is lower red
Outer light, the band gap width of inorganic semiconductor photoelectric material needs to be adjusted to sufficiently small (photon energy of≤infrared light), smaller
Band gap width make inorganic semiconductor photoelectric material very sensitive to temperature, dark current at normal temperatures is larger, to reduce
Signal-to-noise ratio.In order to solve this problem, inorganic semiconductor infrared electro device usually requires cooling device, and cooling device is also significantly
Increase the cost of inorganic semiconductor infrared electro device.In addition, the manufacturing process of inorganic photoelectric device is complicated, need using more
The equipment, such as physical vapour deposition (PVD), molecular beam epitaxial growth etc. of kind physico-chemical process and costliness, therefore with higher
Manufacturing cost.Due to the mechanical equivalent of light fragility of inorganic material itself, inorganic semiconductor photoelectric device does not have flexibility, is unsuitable for the next generation
The manufacture of flexible device and wearable device.Compared with inorganic semiconductor material, organic semiconducting materials have it is at low cost, be easy to
The advantages that processing, be flexible.However, organic semiconducting materials usually have larger band gap width, photon energy can not be absorbed
Lower infrared light.For example, 3- hexyls substituting polythiophene (Poly (3-hexylthiophene-2,5-diyl), P3HT) conduct
A kind of common organic semiconducting materials, are widely used in organic solar batteries and photoelectric device.The band gap of P3HT is wide
Degree is 1.9eV, and corresponding absorbing wavelength is about 650nm, therefore, P3HT can not absorbing wavelength more than 650nm feux rouges and
Infrared light.A kind of effective scheme is using rare earth doped material as light conversion material, and converting infrared light to P3HT can be with
The visible light of absorption, it is seen that light, which is then absorbed by P3HT, generates photoexciton (i.e. electron-hole pair), under the action of extra electric field
Obtain photoelectric current.
Invention content
The present invention provides a kind of flexible all band photoelectric material, photoelectric device and its manufacturing method, by will it is organic partly
The nonabsorbable infrared light of conductor is converted to the visible light that can be absorbed by organic semiconductor, to the detection wavelength of photoelectric device
Infrared region is expanded to, realizes detection of the flexible photoelectric device to all band photon.
In order to achieve the above objectives, the present invention implements by the following technical programs：
Flexible all band photoelectric material includes the tetrafluoride yttrium sodium core shell nanoparticles of ytterbium and Er ions.
The ratio of the tetrafluoride yttrium sodium, ytterbium and erbium is according to mass fraction yttrium 50%-95%, preferred value 78%, ytterbium
5%-50%, preferred value 20%, erbium 0.5%-10%, preferred value 2%.
The manufacturing method of flexible all band photoelectric material, including：
Rare earth oxide is dissolved into trifluoroacetic acid and prepares trifluoroacetic acid salting liquid, rare earth three is obtained after solution is evaporated
Fluoroacetate powder；
Then rare earth trifluoroacetic acid salt powder and sodium trifluoroacetate powder are added to the molten of oleyl amine, oleic acid and octadecylene
In liquid, mixed solution is uniformly mixing to obtain under protective atmosphere；
The mixed solution is heated and continues to stir, the rare earth trifluoroacetate in mixed solution and sodium trifluoroacetate
It is thermally decomposed and reacts the tetrafluoride yttrium sodium nano particle for generating ytterbium and Er ions；
The oleic oil amine aqueous solution containing trifluoroacetic acid yttrium and sodium trifluoroacetate is added into mixed solution again, and continues to stir
Reaction is mixed, the tetrafluoride yttrium sodium shell of one layer of rare-earth free is formed in the tetrafluoride yttrium sodium nano grain surface of ytterbium and Er ions,
To obtain tetrafluoride yttrium sodium composite nanometer particle layer.
The temperature of the heating is 260-360 DEG C, preferably 300 DEG C.
The protective atmosphere is nitrogen or inert gas.
Preferably, it is maintained the temperature between 70-160 DEG C in course of dissolution, preferably 100 DEG C.
Flexible all band photoelectric device, including flexible substrate and the flexible all band photoelectric material, the flexibility all-wave
Section photoelectric material is coated on the flexible substrate.
The flexible substrate is laminated structure.
The manufacturing method of flexible all band photoelectric device, including by tetrafluoride yttrium sodium core shell nanoparticles (NaYF4:Yb,
Er@NaYF4) be distributed in solutions of organic semiconductors, above-mentioned solution is revolved with 1000-6000 rpms after ultrasonic disperse
5-60 seconds are applied to matrix, 100-150 DEG C of annealing is carried out later and obtains laminated film, tetrafluoride yttrium sodium core-shell nano in 1-5 minutes
Particle (NaYF4:Yb,Er@NaYF4) percent by volume of the nano particle in laminated film be 1-10vol%.
And/or the organic semiconducting materials include：3- hexyls substituting polythiophene (poly (3-
Hexylthiophene-2,5-diyl, P3HT), 60 derivative of carbon (phenyl-C61-butyric acid methyl
Ester, PCBM), poly- [[9- (1- octyls nonyl) -9H- carbazoles -2,7- diyl] -2,5- thiophene diyls -2,1,3- benzos thiophene two
Azoles -4,7- diyl -2,5- thiophene diyl] (poly [N-9-heptadecanyl-2,7-carbazole-alt-5,5- (4 ',
7 '-di-2-thienyl-2 ', 1 ', 3 '-benzothiadiazole)], PCDTBT), poly- (9- vinyl carbazoles) (poly (9-
Vinylcarbazole), PVK), poly ({ 4,8-bis [2-ethylhexyloxy] benzo [1,2-b:4,5-b′]
dithiophene-2,6-diyl}(PTB7), PTB7:PCBM mixtures, P3HT:PTB7:PCBM mixtures, P3HT:PVK is mixed
Close object, P3HT:PCBM mixtures, PCDTBT:Any one in PCBM mixtures；
And/or the solvent of the solutions of organic semiconductors includes chloroform, toluene, chloroform toluene mixture, adjacent dichloro
Benzene, any one in dichloromethane.
The present invention is using organic semiconducting materials as flexible optoelectronic active layer, using rare earth doping nano particle as light
Wavelength conversion material, by the nonabsorbable infrared light of organic semiconductor is converted to can be absorbed by organic semiconductor it is visible
Light realizes detection of the flexible photoelectric device to all band photon to which the detection wavelength of photoelectric device is expanded to infrared region.
The all band photoelectric device of the present invention has many advantages, such as at low cost, flexible high and high to the responsiveness of infrared light.?
In the present invention, for rare earth nanometer particle as light conversion material, the infrared light that needs can be detected is converted to visible light, and then quilt
Organic semiconductor active film, which absorbs, generates photoexciton (i.e. electron-hole pair), and photoelectric current is generated under the action of extra electric field.
Since rare earth nanometer particle is uniformly dispersed in organic semiconductor film, the photoelectric device that we prepare has good
Flexibility is suitable for the manufacture of flexible wearable device.In the present invention, a variety of materials component can use solwution method at low cost
It prepares, also, since the band gap width of used organic semiconducting materials is larger (corresponding absorbing wavelength is visible light), it can
To inhibit the dark current under room temperature well, therefore additional cooling device is not needed, thus greatly reduces photoelectric device
Cost.
Description of the drawings
Below according to drawings and examples, invention is further described in detail.
Fig. 1 rare earth doping nano particles NaYF4:The XRD diagram of Yb, Er；
Fig. 2 rare earth doping nano particles NaYF4:The TEM of Yb, Er scheme；
Fig. 3 rare earth doping nano particles NaYF4:The SEM figures (a) and size distribution plot (b) of Yb, Er；
Fig. 4 rare earth doping nano particles NaYF4:The EDX spectrograms of Yb, Er；
Fig. 5 rare earth doping nano particles NaYF4:The stabilized illumination spectrogram under 975nm laser excitations of Yb, Er；
Fig. 6 NaYF4:Stabilization of the core nano particle and Core-shell Structure Nanoparticles of Yb, Er under 975nm laser excitations
Shine spectrogram；
Fig. 7 NaYF4:Yb, Er nano particle time resolution fluorescence spectrum, exciting light：975nm laser；
Fig. 8 NaYF4:The steady generation spectrum of Yb, Er nano-particles reinforcement organic semiconductor P3HT films, exciting light：
975nm laser；
Fig. 9 NaYF4:Yb, Er nano particle and NaYF4:The green light feux rouges of Yb, Er nano particle P3HT laminated films integrates
Intensity rate, exciting light：975nm laser；
Figure 10 NaYF4:The AFM of Yb, Er nano-particles reinforcement organic semiconductor P3HT films schemes, 200 nm of scale；
Figure 11 NaYF4:The energy level transition schematic diagram under 975nm laser excitations of Yb, Er nano particle.
Specific implementation mode
Flexible all band photoelectric material includes the tetrafluoride yttrium sodium core shell nanoparticles of ytterbium and Er ions.
The ratio of the tetrafluoride yttrium sodium, ytterbium and erbium is according to mass fraction yttrium 50%-95%, preferred value 78%, ytterbium
5%-50%, preferred value 20%, erbium 0.5%-10%, preferred value 2%.
The manufacturing method of flexible all band photoelectric material, including：
Rare earth oxide is dissolved into trifluoroacetic acid and prepares trifluoroacetic acid salting liquid, rare earth three is obtained after solution is evaporated
Fluoroacetate powder；
Then rare earth trifluoroacetic acid salt powder and sodium trifluoroacetate powder are added to the molten of oleyl amine, oleic acid and octadecylene
In liquid, mixed solution is uniformly mixing to obtain under protective atmosphere；
The mixed solution is heated and continues to stir, the rare earth trifluoroacetate in mixed solution and sodium trifluoroacetate
It is thermally decomposed and reacts the tetrafluoride yttrium sodium nano particle for generating ytterbium and Er ions；
The oleic oil amine aqueous solution containing trifluoroacetic acid yttrium and sodium trifluoroacetate is added into mixed solution again, and continues to stir
Reaction is mixed, the tetrafluoride yttrium sodium shell of one layer of rare-earth free is formed in the tetrafluoride yttrium sodium nano grain surface of ytterbium and Er ions,
To obtain tetrafluoride yttrium sodium composite nanometer particle layer.
The temperature of the heating is 260-360 DEG C, preferably 300 DEG C.
The protective atmosphere is nitrogen or inert gas.
Preferably, it is maintained the temperature between 70-160 DEG C in course of dissolution, preferably 100 DEG C.
Flexible all band photoelectric device, including flexible substrate and the flexible all band photoelectric material, the flexibility all-wave
Section photoelectric material is coated on the flexible substrate.
The flexible substrate is laminated structure.
The manufacturing method of flexible all band photoelectric device, including by tetrafluoride yttrium sodium core shell nanoparticles (NaYF4:Yb,
Er@NaYF4) be distributed in solutions of organic semiconductors, above-mentioned solution is revolved with 1000-6000 rpms after ultrasonic disperse
5-60 seconds are applied to matrix, 100-150 DEG C of annealing is carried out later and obtains laminated film, tetrafluoride yttrium sodium core-shell nano in 1-5 minutes
Particle (NaYF4:Yb,Er@NaYF4) percent by volume of the nano particle in laminated film be 1-10vol%.
And/or the organic semiconducting materials include：3- hexyls substituting polythiophene (poly (3-
Hexylthiophene-2,5-diyl, P3HT), 60 derivative of carbon (phenyl-C61-butyric acid methyl
Ester, PCBM), poly- [[9- (1- octyls nonyl) -9H- carbazoles -2,7- diyl] -2,5- thiophene diyls -2,1,3- benzos thiophene two
Azoles -4,7- diyl -2,5- thiophene diyl] (poly [N-9-heptadecanyl-2,7-carbazole-alt-5,5- (4 ',
7 '-di-2-thienyl-2 ', 1 ', 3 '-benzothiadiazole)], PCDTBT), poly- (9- vinyl carbazoles) (poly (9-
Vinylcarbazole), PVK), poly ({ 4,8-bis [2-ethylhexyloxy] benzo [1,2-b:4,5-b′]
dithiophene-2,6-diyl}(PTB7), PTB7:PCBM mixtures, P3HT:PTB7:PCBM mixtures, P3HT:PVK is mixed
Close object, P3HT:PCBM mixtures, PCDTBT:Any one in PCBM mixtures；
And/or the solvent of the solutions of organic semiconductors includes chloroform, toluene, chloroform toluene mixture, adjacent dichloro
Benzene, any one in dichloromethane.
Rare earth doping nano particle NaYF4:Yb, Er the tetrafluoride yttrium sodium of Er ions (ytterbium) are prepared using thermal decomposition method.Tool
Body method is as follows：
Rare earth oxide is dissolved at 80 DEG C in trifluoroacetic acid first and prepares trifluoroacetate.In a typical reaction
In, the rare earth trifluoroacetic acid salt powder and sodium trifluoroacetate that meet stoichiometric ratio are added to oleyl amine, oleic acid and octadecylene
In mixed solution, heats and stir 0.5 hour for 120 DEG C in a nitrogen atmosphere so that reactant is completely dissolved and removes in solution
Moisture and air.It is warming up to 330 DEG C later to heat and stir 1 hour, obtains NaYF4:Yb, Er nano particle.
Backward solution in be added shell material the precursor solution (oleic oil containing trifluoroacetic acid yttrium and sodium trifluoroacetate
Amine aqueous solution), continue to stir half an hour at 330 degree DEG C, obtains NaYF4:Yb, Er core shell nanoparticles.
The NaYF that table 1. is obtained by EDX results4:The atomic percent of each element in Yb, Er core shell nanoparticles
By XRD (X-ray diffraction) results it is found that prepared NaYF4:Yb, Er nano particle are the NaYF of hexagonal phase4
(JCPDS 16-0334), as shown in Figure 1.Wider peak width illustrates the crystallite dimension very little of nano particle.Pass through Scherrer formula meter
Calculation can obtain, and rear-earth-doped upper conversion nano grain size is about 25.6 ± 1.8nm.TEM (transmission electron microscope) photo
It shows (Fig. 2), the pattern of rare earth nanometer particle is nanometer rods, and nanometer is calculated by SEM (scanning electron microscope) photo
The Size Distribution of stick is 34.8 ± 11.4nm, and the draw ratio of nanometer rods is 1.89, such as Fig. 3.EDX composes (Energy dispersive x-ray light
Spectrum) result proves Y, Yb, the presence of Er elements, as shown in figure 4, the content for each element being calculated by EDX spectrums is shown in Table 1.It is dilute
The steady generation spectrum of native doped nanoparticle measures (Fig. 5) under 975nm laser excitations, wherein the emission peak at 525nm
Be due to2H11/2→4I15/2Energy level transition, the emission peak at 540nm be due to4S3/2→4I15/2Energy level transition, the hair at 654nm
Penetrate peak be due to4F9/2→4I15/2Energy level transition.Undoped NaYF4Shell material can effectively prevent due to nuclear particle surface
Fluorescent quenching caused by defect, impurity and surface ligand (such as OH and CH2 functional groups).Therefore, after coating one layer of shell,
NaYF4:The luminous intensity of Yb, Er nano particle substantially enhances, and the integrated intensity of green light increases 27 times, the integrated intensity of feux rouges
100 times are increased, as shown in Figure 6.NaYF4:The results are shown in Figure 7 for Yb, Er nano particle time resolution fluorescence spectrum, time solution
Analysing fluorescence spectrum is obtained to 540nm emission peak measurements under 975nm laser excitations.Time resolution fluorescence spectrum is singly referred to
Number formula I=I0Exp (- t/ τ) fittings can obtain (wherein I0It is the fluorescence intensity in t=0, τ is the fluorescence decay that fitting obtains
Time, that is, fluorescence lifetime), prepared NaYF4:Yb, Er nano particle4S3/2→4I15/2The fluorescence of (540nm) energy level transition
Die-away time is about 0.44ms.Fluorescence decay time characterizes radiation transistion and the nonradiative transition of particular excitation energy level.Fluorescence declines
Subtracting the time longer shows high fluorescence efficiency and low non-radiative loss.Fluorescence decay time numeric ratio document measured by us
Twice of the 0.20ms high of middle report1, show that our rare earth doping fluorescent nano particle has the spy of high fluorescent
Point.
NaYF4:Yb, Er nano-particles reinforcement organic semiconductor P3HT (3- hexyls substituting polythiophene) films by spin coating side
It is prepared by method.Specifically preparation method is：By NaYF4:Yb, Er nano particle are distributed in the chloroform and toluene mixed solution of P3HT
(1:1), after ultrasonic disperse by above-mentioned solution in 6000 rpms of spin coatings 60 seconds to matrix, to carry out 120 DEG C later and anneal 3 points
Clock obtains laminated film, NaYF4:Percent by volume of Yb, the Er nano particle in laminated film is 10vol%.
The characterization result of laminated film is as follows：NaYF4:Yb, Er nano-particles reinforcement organic semiconductor P3HT films it is steady
State luminescent spectrum (Fig. 8) and individual NaYF4:The steady generation spectrum of Yb, Er nano particle compares display, the intensity of green light
Strength reduction relative to feux rouges.NaYF4:Yb, Er nano particle and NaYF4:Yb, Er nano particle P3HT laminated films
Green light feux rouges integrated intensity ratio as shown in figure 9, this ratio from NaYF4:The 0.56 of Yb, Er nano particle falls below THIN COMPOSITE
The 0.23 of film.This green light is caused by the selective absorbing due to P3HT to green light relative to the reduction of red light-emitting intensity.
NaYF4:The configuration of surface of Yb, Er nano particle P3HT laminated films is characterized by AFM (atomic force microscope), such as Figure 10 institutes
Show.Root mean square (RMS) surface roughness is about 7.79nm.It is smooth that lower RMS value shows that prepared laminated film has
Surface and the dispersion of uniform particle.NaYF4:The operation principle of Yb, Er nano particle P3HT laminated films is as follows：It is close in 975nm
Under Infrared irradiation, Yb ions pass through first2F7/2→2F5/2Energy level transition absorbs the energy of near-infrared excitation light.NaYF4:Yb,
The energy level transition under 975nm laser excitations of Er nano particles is as shown in figure 11.Then, Yb ions are from excitation state transition Hui Ji
State and the Er ions that energy is transferred to surrounding.Er ions receive multiple after the photon energy that Yb ions transmit, and reach one
High excitation state is such as4S3/2, and emitted by way of energy level transition and cross relaxation 540nm (4S3/2→4I15/2) and 654nm
(4F9/2→4I15/2) visible light.Since the band gap width of P3HT is 1.9 electron volts, correspond to absorbing wavelength less than 650nm's
Visible light, therefore, NaYF4:The visible light that Yb, Er nano particle are emitted is absorbed by the P3HT of surrounding, and is produced in P3HT films
Third contact of a total solar or lunar eclipse exciton (i.e. electron-hole pair).At this point, under the action of extra electric field, photoexciton row is at photoelectric current.The photoexciton of generation
More, then photo-signal is more apparent, the photoresponse efficiency of prepared laminated film is higher.NaYF4:Yb, Er nanometers
The luminous intensity of useful load and nano particle of the grain in P3HT determines the infrared light photoresponse rate of laminated film.Due to me
The NaYF that uses4:Yb, Er nano particle charging ratio high (10vol%) and prepared NaYF4:Yb, Er nanometers
Grain has high luminous intensity, therefore, it is expected to, and prepared laminated film has high infrared light photoresponse rate.
In order to verify the possibility for preparing flexible device using prepared laminated film, NaYF4:Yb, Er nano particle
P3HT laminated films are spun onto (polyethylene terephthalate, polyethylene on a kind of matrix flexible
terephthalate PET).After it have passed through and how long bend, does not find macroscopic slight crack, illustrate that laminated film exists
The adhesion having had on flexible substrate.This experimental result shows our NaYF4:Yb, Er nano particle P3HT are compound
Film is used for preparing flexible infrared electro device and protrudes potentiality.
Laminated film is spun to photoresist spinner above flexible substrate PET, then utilizes litho machine and optical cement in laminated film
Surface carries out the making of patterns of openings.Use physical deposition machine deposited metal as electrode later.Removed again using the method for separation
Optical cement and excess metal.Entire element manufacturing finishes, and can carry out the measurement of opto-electronic conversion.
Finally it should be noted that：The foregoing is merely the preferred embodiment of invention, it is not limited to invent, although
Invention is described in detail with reference to the foregoing embodiments, it for those skilled in the art, still can be to preceding
The technical solution recorded in each embodiment is stated to modify or equivalent replacement of some of the technical features.It is all to send out
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on, should be included in invention protection domain it
It is interior.
Claims (9)
1. flexible all band photoelectric material, includes tetrafluoride yttrium sodium, ytterbium and the erbium of nano particle.
2. photoelectric material according to claim 1, which is characterized in that the ratio of the tetrafluoride yttrium sodium, ytterbium and erbium be by
According to mass fraction yttrium 50%-95%, preferred value 78%, ytterbium 5%-50%, preferred value 20%, erbium 0.5%-10%, preferred value
2%.
3. the manufacturing method of flexible all band photoelectric material, including：
Rare earth oxide is dissolved into trifluoroacetic acid and prepares rare earth trifluoroacetic acid salting liquid, rare earth three is obtained after solution is evaporated
Fluoroacetate powder；
Then rare earth trifluoroacetic acid salt powder and sodium trifluoroacetate powder are added to the solution of oleyl amine, oleic acid and octadecylene
In, it is uniformly mixing to obtain mixed solution under protective atmosphere；
The mixed solution is heated and continues to stir, mixed solution middle rare earth trifluoroacetate and heated point of sodium trifluoroacetate
It solves and reacts the tetrafluoride yttrium sodium nano particle for generating ytterbium and Er ions；
The oleic oil amine aqueous solution containing trifluoroacetic acid yttrium and sodium trifluoroacetate is added into mixed solution again, and it is anti-to continue stirring
It answers, the tetrafluoride yttrium sodium shell of one layer of rare-earth free is formed in the tetrafluoride yttrium sodium nano grain surface of ytterbium and Er ions, to
Obtain tetrafluoride yttrium sodium composite nanometer particle layer.
4. manufacturing method according to claim 3, which is characterized in that the temperature of the heating is 260-360 DEG C, preferably
300℃。
5. manufacturing method according to claim 3, which is characterized in that the protective atmosphere is nitrogen or inert gas.
6. manufacturing method according to claim 3, which is characterized in that maintained the temperature in course of dissolution 70-160 DEG C it
Between, preferably 100 DEG C.
7. flexible all band photoelectric device, including flexible substrate and the flexible all band photoelectric material, the flexibility all band
Photoelectric material is coated on the flexible substrate.
8. photoelectric device according to claim 7, which is characterized in that the flexible substrate is laminated structure.
9. the manufacturing method of flexible all band photoelectric device, including by tetrafluoride yttrium sodium core shell nanoparticles (NaYF4:Yb,Er@
NaYF4) be distributed in solutions of organic semiconductors, by above-mentioned solution with 1000-6000 rpms of spin coating 5- after ultrasonic disperse
Laminated film, tetrafluoride yttrium sodium core shell nanoparticles are obtained within 1-5 minutes on matrix, carrying out 100-150 DEG C of annealing later within 60 seconds
(NaYF4:Yb,Er@NaYF4) percent by volume of the nano particle in laminated film be 1-10vol%；
And/or the organic semiconducting materials include：3- hexyls substituting polythiophene (poly (3-hexylthiophene-2,
5-diyl, P3HT), 60 derivative of carbon (phenyl-C61-butyric acid methyl ester, PCBM), poly- [[9- (1-
Octyl nonyl) -9H- carbazole -2,7- diyls] -2,5- thiophene diyl -2,1,3- diazosulfide -4,7- diyl -2,5- thiophene two
Base] (poly [N-9-heptadecanyl-2,7-carbazole-alt-5,5- (4 ', 7 '-di-2-thienyl-2 ', 1 ', 3 '-
Benzothiadiazole)], PCDTBT), poly- (9- vinyl carbazoles) (poly (9-vinylcarbazole), PVK), poly
({4,8-bis[2-ethylhexyloxy]benzo[1,2-b:4,5-b′]dithiophene-2,6-diyl}(PTB7)、
PTB7:PCBM mixtures, P3HT:PTB7:PCBM mixtures, P3HT:PVK mixtures, P3HT:PCBM mixtures, PCDTBT:
Any one in PCBM mixtures；
And/or the solvent of the solutions of organic semiconductors includes chloroform, toluene, chloroform toluene mixture, o-dichlorohenzene, two
Any one in chloromethanes.
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