CN104766901A - Photonic crystal structure for enhancing and adjusting up-conversion substance light emitting function and preparation method of photonic crystal structure - Google Patents
Photonic crystal structure for enhancing and adjusting up-conversion substance light emitting function and preparation method of photonic crystal structure Download PDFInfo
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- 239000004038 photonic crystal Substances 0.000 title claims abstract description 71
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 69
- 239000000126 substance Substances 0.000 title claims abstract description 25
- 230000002708 enhancing effect Effects 0.000 title abstract description 6
- 238000002360 preparation method Methods 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000001338 self-assembly Methods 0.000 claims abstract description 39
- 239000000843 powder Substances 0.000 claims abstract description 27
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 22
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims description 45
- 239000002131 composite material Substances 0.000 claims description 26
- 239000013078 crystal Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 21
- 238000010276 construction Methods 0.000 claims description 18
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000004005 microsphere Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- 238000005728 strengthening Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052775 Thulium Inorganic materials 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 229910052691 Erbium Inorganic materials 0.000 claims description 4
- 229910052693 Europium Inorganic materials 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 4
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims description 4
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000008188 pellet Substances 0.000 abstract 2
- 238000013329 compounding Methods 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 238000002189 fluorescence spectrum Methods 0.000 description 8
- 238000004020 luminiscence type Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 7
- 238000010408 sweeping Methods 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000004062 sedimentation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000000975 co-precipitation Methods 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- YNPNZTXNASCQKK-UHFFFAOYSA-N Phenanthrene Natural products C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 230000018199 S phase Effects 0.000 description 2
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000011514 reflex Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 2
- 229910052769 Ytterbium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000002560 therapeutic procedure Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- 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
- Y02E10/52—PV systems with concentrators
-
- 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 invention discloses a photonic crystal structure for enhancing and adjusting the up-conversion substance light emitting function. The photonic crystal structure is formed by compounding a photonic crystal layer, an up-conversion function substance layer and a photonic crystal layer. Each photonic crystal layer is formed by assembling silicon dioxide pellets on the nanoscale layer by layer. The up-conversion function substance layer is formed by flatly laying inorganic powder or organic fluorescent powder with the near infrared up-conversion function on the nanoscale. The silicon dioxide pellets are scattered to prepare a self-assembly solution, the self-assembly solution is added to a self-assembly region to be naturally dried, and then a first photonic crystal film is formed; the fluorescent powder with the up-conversion function is scattered in the solution, ultrasonically scattered and smeared to the surface of the first photonic crystal film and naturally dried, the self-assembly solution is added to the surface of the up-conversion function substance layer finally and naturally dried, and the photonic crystal structure is acquired after thermal treatment. By the adoption of the photonic crystal structure, up-conversion substance energy conversion efficiency is improved and visible near ultraviolet light emitting intensity is enhanced.
Description
Technical field
The present invention relates to field of optical functional material, particularly relate to and a kind of there is photon crystal structure strengthening and regulate upper transformational substance lighting function and preparation method thereof.
Background technology
Solar energy is the mankind's the abundantest utilizable clean energy resourcies, and the overwhelming majority of necessary for human energy is all direct or indirect from the sun.Society, development along with economy cause environmental pollution and non-renewable energy resources problem more and more serious, and in the process of exploitation non-renewable energy resources, the mankind destroy environment again, cause ecosystem disequilibrium, the non-renewable energy energy is fewer and feweri.But our daily life be unable to do without the energy, therefore greatly develop the clean environment firendly energy, improving the utilance of solar energy is that we solve the effective means of environmental problem and energy problem.In recent years, developing rapidly of catalysis material and solar cell, curbs environmental pollution to us and builds harmonious friendly society and bring fine vision.But up to the present, the major part of human use or sun visible ray and ultraviolet portion energy, the infrared light accounting for sunlight major part (48.3%) is not fully utilized.And in catalysis material and solar cell application, what mainly need is also high-octane Uv and visible light.Therefore, in order to improve the utilance of sunlight, the functional mass application with upper conversion is come in, infrared lights a large amount of in solar spectrum is converted to more high-octane visible ray and ultraviolet light, thus by catalysis material, electrode of solar battery utilized, this can put forward high-octane utilization ratio greatly, promote the development of new forms of energy, thus to build a fine harmonious environment friendly social for the mankind.
Up-conversion luminescent material has obtained development since 19th-century mid-term, and the luminescent material of nano-scale is owing to having small-size effect, high-ratio surface effect and quantum effect etc., thus becomes the focus in up-conversion luminescent material research.At present, many up-conversions of research mainly divide inorganic organic two classes, inorganic upconverting fluorescent material due to chemical stability good, luminous strong, powder size is little and by extensive concern; Organic fluorescence materials cost is low, can dissolve in organic solvent, easy and organic substance compound, more closing to reality application.In recent years, along with the development of science and technology, rear-earth-doped luminous material is in three-dimensional display, and photocatalysis, solar cell, the field such as bio-imaging and optical dynamic therapy demonstrates their irreplaceable application prospects.But often need the luminous intensity of up-conversion high in practical application, light-emitting zone is concentrated, colour purity is high, luminous efficiency is high, therefore, regulates the luminescent spectrum of up-conversion, luminescence is made to concentrate on a certain wave band, particularly UV, visible light optical band, for raising solar energy utilization ratio, promotes that the development such as catalysis material and solar cell has huge impetus.
In illumination field application, the light of adjustment or a certain wave band of enhancing luminescent substance is very helpful to practical application.Such as LED needs in luminescent spectrum set of regions, and colour purity is high, luminous strong.Catalysis material then needs the black light that receives abundant.Solar panel is maximum to visible absorption, needs abundant visible ray resource.Therefore, how to make upconverting fluorescent material send light required for us, namely how to regulate and strengthen fluorescent material specific band only have very much science and actual application value.But the emission spectrum of up-conversion self is fixing often, and the adjustment realizing spectrum often will by the special construction of outside such as photonic crystal.The maximum feature of photonic crystal is that it has very strong reflex to the light of a certain frequency, namely there is forbidden photon band.Its reflex to optional frequency light can be realized by controlling the unit periodic size of photonic crystal.When the bandgap center position of photonic crystal is coupled with a certain emission band of up-conversion, just can realizes the enhancing to a certain band of light of luminescent substance or compacting, thus reach spectrum regulating action.
Summary of the invention
The object of the invention is to provide a kind of photon crystal structure having enhancing and regulate upper transformational substance lighting function to improve the deficiencies in the prior art; Another object of the present invention is to provide the preparation method of above-mentioned photon crystal structure.
Technical scheme of the present invention is: the present invention utilizes the forbidden band effect of photonic crystal, the emission peak of up-conversion fluorescence powder correspondence position is suppressed, make it internal energy transfer, thus make the light of fluorescent material outgoing required for us, the spectrum realizing upconverting fluorescent material regulates.Meanwhile, because the ball spherical structure of photon crystal structure makes optical density increase, the luminescence of upconverting fluorescent material obtains overall enhancing.Therefore, the composite construction of layer of photonic crystals+upper conversion function material layer+layer of photonic crystals can realize the spectrum adjustment of upconverting fluorescent material and strengthen.
Concrete technical scheme of the present invention is: a kind of have the photon crystal structure strengthening and regulate upper transformational substance lighting function, it is characterized in that being composited by layer of photonic crystals+upper conversion function material layer+layer of photonic crystals; Wherein said layer of photonic crystals is made up of the silicon dioxide microsphere LBL self-assembly of 200-400nm; Described upper conversion function material layer is tiled by the inorganic nanometer powder or organic fluorescence powder with near-infrared upper conversion function to form.
The thickness of preferably above-mentioned layer of photonic crystals is between 2-3um; The thickness of preferably above-mentioned upper conversion function material layer is between 250nm-450nm.
The preferably above-mentioned general formula with the inorganic nanometer powder of near-infrared upper conversion function is: NaYF
4: Yb
3+, R
3+, wherein R
3+for rare earth element, be preferably thulium (Tm
3+), erbium (Er
3+) or europium (Eu
3+) in one.
The preferably above-mentioned general formula with the organic fluorescence powder of near-infrared upper conversion function is: Yb
x, R
1-x(TTA)
3phen, wherein R is thulium (Tm
3+), erbium (Er
3+), or europium (Eu
3+) in one, x is any one real number between 0.1-0.9.
Present invention also offers the above-mentioned preparation method with the photon crystal structure strengthening and regulate above transformational substance lighting function, its concrete steps are as follows:
Prepared by A, layer of photonic crystals: be at room temperature distributed in solvent by the silicon dioxide microsphere of 200nm-400nm size, be made into self assembly liquid, the mass concentration of silicon dioxide dispersion soln is 0.5%-2%; Then by solution ultrasonic disperse; Finally by self assembly liquid join in self assembly region, form layer of photonic crystals after natural drying;
Prepared by B, upper conversion function material layer: be made into 10 for being dissolved in organic solvent by up-conversion phosphor
-5-10
-3the solution of mol/L concentration, ultrasonic disperse, uses the layer of photonic crystals surface that upper conversion solution spraying is prepared to steps A by spray gun; Obtained upper conversion function material layer;
C, prepare silicon dioxide photon self assembly liquid with steps A, then silicon dioxide self assembly liquid is joined on the obtained upper conversion function material layer of step B, then form one deck layer of photonic crystals; Natural drying (general 4-6 hour) obtains final composite construction;
D, sandwich obtained for step C is put in 200-300 degree Celsius of heat treatment 3-5 hour in Muffle furnace, obtains having the photon crystal structure strengthening and regulate upper transformational substance lighting function.
Solvent described in preferred steps A is ethanol or water; Organic solvent described in preferred steps B is cyclohexane, ethanol or dimethyl sulfoxide (DMSO).The parameter of the ultrasonic disperse described in preferred steps A and B is: power is 400-1200w, and the time is 0.5-1h.
In preferred steps A and C, the thickness of layer of photonic crystals is 2-3um; The thickness of general upper and lower two-layer layer of photonic crystals is identical; Generally the self assembly liquid of 0.2ml-0.5ml is joined 1-4cm
2can reach in the self assembly region of size; In preferred steps B, the thickness of upper conversion function material layer is between 250nm-450nm.
Described inorganic nano up-conversion fluorescence material is prepared by solvent-thermal method, and concrete grammar is article " the Uniform NaYF delivered with reference to this seminar
4: Yb, Tm hexagonal submicroplates:Controlledsynthesis and enhanced UV and blue upconversion luminescence ".
Described organic up-conversion fluorescence powder is prepared by coprecipitation, and concrete grammar is article " the Synthesis and luminescence properties of ternary complexes ofSm delivered with reference to this seminar
xtb
1-x(TTA)
3phen nanoparticles and their surface modification ".
This photonic crystal composite construction that the present invention obtains can suppress the outgoing (such as near infrared light transmitting) of the specific band of up-conversion fluorescence material, transformational substance energy conversion efficiency in raising, makes visible near ultraviolet luminous intensity strengthen about 2 times.
Beneficial effect:
Photonic crystal described in this patent and fluorescent material composite construction (layer of photonic crystals+upper conversion function material layer+layer of photonic crystals), utilize the close pile structure of ball ball of photonic crystal, structure internal optical density is increased, can effectively strengthen up-conversion fluorescence material luminescence, particularly visible and near ultraviolet luminescence, strengthens about 2 times.
Photonic crystal described in this patent and fluorescent material composite construction (layer of photonic crystals+upper conversion function material layer+layer of photonic crystals), by changing layer of photonic crystals construction unit Microsphere Size, form the forbidden band of specific band light, the a certain band of light (near infrared light) of upper conversion function material outgoing can be suppressed, material internal energy is shifted, strengthen ultraviolet light or VISIBLE LIGHT EMISSION, reach the effect improving up-conversion luminescence efficiency, turn optical efficiency and improve about 7%.
Accompanying drawing explanation
Fig. 1 is the UVPC mirror-reflection test result figure of the photonic crystal of the silicon dioxide self assembly of embodiment 1;
Fig. 2 is the surface sweeping Electronic Speculum figure of the layer of photonic crystals of the silicon dioxide self assembly of embodiment 1;
Fig. 3 is the inorganic upper conversion powder NaYF of embodiment 1
4: Yb
3+, Tm
3+surface sweeping Electronic Speculum figure;
Fig. 4 is the layer of photonic crystals+upper conversion function material layer+layer of photonic crystals composite construction sectional drawing of embodiment 1;
Fig. 5 is the NaYF of embodiment 1
4: Yb
3+, Tm
3+fluorescence spectrum figure in without photon crystal structure (a) and in photonic crystal composite construction (b);
Fig. 6 is the inorganic upper conversion powder NaYF of embodiment 2
4: Yb
3+, Er
3+surface sweeping Electronic Speculum figure;
Fig. 7 is the UVPC mirror-reflection test result figure of the photonic crystal of the silicon dioxide self assembly of embodiment 2;
Fig. 8 is the NaYF of embodiment 2
4: Yb
3+, Er
3+the fluorescence spectrum figure in without photon crystal composite structure (a) and in photonic crystal composite construction (b);
Fig. 9 is the Yb of embodiment 3
0.8, Er
0.2(TTA)
3the scanning electron microscope (SEM) photograph of Phen organic fluorescence powder;
Figure 10 is the Yb of embodiment 3
0.8, Er
0.2(TTA)
3phen without photon crystal composite structure (a) and the fluorescence spectrum figure in photonic crystal composite construction (b);
Figure 11 is the Yb of embodiment 4
0.25, Tm
0.75(TTA)
3the scanning electron microscope (SEM) photograph of Phen organic fluorescence powder;
Figure 12 is the Yb of embodiment 4
0.25, Tm
0.75(TTA)
3phen without photon crystal composite structure (a) and the fluorescence spectrum figure in photonic crystal composite construction (b).
Embodiment
Embodiment 1
First the silicon dioxide microsphere of 360nm is distributed in ethanolic solution, is made into the self assembly liquid that mass concentration is 1%, 1200w power ultrasonic dispersion 0.5h.Then gravity sedimentation 0.5ml self assembly liquid in the self assembly region of 1cm*1cm, the layer of photonic crystals obtained after natural drying, thickness is 2.5um.The test carrying out mirror anti-obtains Fig. 1, can find out that photonic crystal band is at 800nm place.Scanning electron microscope (SEM) photograph as shown in Figure 2, can find out that layer of photonic crystals self assembly is very regular.Solvent-thermal method is used to prepare NaYF
4: Yb
3+, Tm
3+nano-powder, inorganic up-conversion fluorescence material is six side's phases, and surface sweeping Electronic Speculum figure as shown in Figure 3.Inorganic upper conversion powder is scattered in cyclohexane and is made into 10
-3the solution of mol/L concentration, ultrasonic 0.5h under 600W power, then at room temperature sprays the inorganic up-conversion fluorescence substance solution of one deck in photonic crystal top layer.The 1% concentration silicon dioxide self assembly liquid of 0.5ml is deposited again on phosphor layer surface, natural drying in 4 hours after natural drying in 1 hour.Last 200 degrees Celsius of heat treatments obtained composite construction after 3 hours, and shown in profile scanning Electronic Speculum figure Fig. 4, can find out that we obtain layer of photonic crystals+upper this structure of transformational substance layer+layer of photonic crystals, general thickness is about 5.3um.Meanwhile, blank's sample sprays the inorganic up-conversion phosphor liquid solution of one deck of identical amount as a comparison.Figure 5 shows that NaYF
4: Yb
3+, Tm
3+fluorescence spectrum figure in without photon crystal composite structure (a) and in photonic crystal composite construction (b), can find out, relative to contrast sample, the visible light part of upper converted photons crystal composite material enhances about 2 times, near-infrared luminously relatively obtain compacting, upper conversion efficiency is improved.
Embodiment 2
Solvent-thermal method is used to prepare NaYF
4: Yb
3+, Er
3+nano-powder, inorganic up-conversion fluorescence material is six side's phases, and surface sweeping Electronic Speculum figure as shown in Figure 6.Inorganic upper conversion powder is scattered in cyclohexane and is made into 10
-4the solution of mol/L concentration, ultrasonic 0.5h under 800W power.The silicon dioxide microsphere of 250nm is distributed in the aqueous solution, is made into the self assembly liquid that mass concentration is 2%, 600w power ultrasonic dispersion 1h.Then gravity sedimentation self assembly liquid 0.3ml in the self assembly region of 2cm*2cm, after natural drying, ground floor photonic crystal thickness is 3um, and as shown in Figure 7, after can finding out the self assembly of 250nm microballoon, bandgap center position is 550nm to reflectance test.At room temperature spray the inorganic up-conversion fluorescence substance solution of one deck in photonic crystal top layer, thickness is 400nm.0.3ml silicon dioxide self assembly liquid is deposited again after 1 hour, after natural drying in 6 hours, in 300 degrees Celsius of Muffle furnaces, heat treatment obtained sandwich after 5 hours, meanwhile, blank's sample sprays the inorganic up-conversion fluorescence powder of one deck of identical amount as a comparison.Figure 8 shows that NaYF
4: Yb
3+, Er
3+the fluorescence spectrum figure in without photon crystal composite structure (a) and in photonic crystal composite construction (b), can find out, relative to contrast sample, the near ultraviolet 484nm light of photonic crystal compound up-conversion enhances about 7 times, near-infrared luminous 660nm is relative with visible ray green glow 550nm place obtains compacting, and upper conversion efficiency is improved.
Embodiment 3
Coprecipitation is used to prepare Yb
0.8, Er
0.2(TTA)
3phen organic fluorescence powder, surface sweeping Electronic Speculum figure as shown in Figure 9.A certain amount of organic fluorescence powder is dissolved in dimethyl sulfoxide (DMSO) and is made into 10
-5the solution of mol/L concentration, under 1000W power, ultrasonic 0.5h is for subsequent use.The silicon dioxide microsphere of 250nm is distributed in ethanolic solution, is made into the self assembly liquid that mass concentration is 0.5%, 1000w power ultrasonic dispersion 0.5h.Then gravity sedimentation silicon dioxide microsphere self assembly liquid 0.5ml in the self assembly region of 1.5cm*1.5cm, after natural drying, thickness is about 3um.At room temperature spray the organic up-conversion fluorescence substance solution of one deck in photonic crystal top layer, thickness is about 250nm.0.5ml silicon dioxide self assembly liquid is deposited again, natural drying after 5 hours after 0.5h.Last 200 degrees Celsius of heat treatments obtained composite structure after 3 hours, meanwhile, blank's sample sprayed one deck identical amount organic fluorescence powder as a comparison.Figure 10 shows that Yb
0.5, Er
0.5(TTA)
3phen without photon crystal composite structure (a) and the fluorescence spectrum figure in photonic crystal composite construction (b), can find out in this example, relative to contrast sample, the near ultraviolet 484nm light of photonic crystal compound up-conversion enhances about 7 times, visible red 660nm is relative with green glow 550nm place obtains compacting, and upper conversion efficiency is improved.
Embodiment 4
Coprecipitation is used to prepare Yb
0.25, Tm
0.75(TTA)
3phen organic fluorescence powder, surface sweeping Electronic Speculum figure as shown in figure 11.Organic fluorescence powder is scattered in water and is made into 10
-5the solution of mol/L concentration, ultrasonic 1h under 1200W power.The silicon dioxide microsphere of 360nm is distributed in the aqueous solution, is made into the self assembly liquid that mass concentration is 2%, 1200w power ultrasonic dispersion 1h.Gravity sedimentation self assembly liquid 0.4ml in the self assembly region of 2cm*2cm, the organic up-conversion fluorescence substance solution of one deck is at room temperature sprayed in photonic crystal top layer after natural drying, 0.4ml silicon dioxide self assembly liquid is deposited again after 1 hour, 6 to be as a child placed in after 200 degrees Celsius of Muffle furnace heat treatments 5 hours, obtain composite structure, meanwhile, blank's sample sprays one deck identical amount organic fluorescence powder as a comparison.Figure 12 shows that Yb
0.25, Tm
0.75(TTA)
3phen without photon crystal composite structure (a) and the fluorescence spectrum figure in photonic crystal composite construction (b), can find out in this example, relative to contrast sample, the near ultraviolet reinforced partly about 7 times of converted photons crystalline material in compound, visible red 660nm is relative with green glow 550nm place obtains compacting, and upper conversion efficiency is improved.
Claims (9)
1. there is the photon crystal structure strengthening and regulate upper transformational substance lighting function, it is characterized in that being composited by layer of photonic crystals+upper conversion function material layer+layer of photonic crystals; Wherein said layer of photonic crystals is made up of the silicon dioxide microsphere LBL self-assembly of 200-400nm; Described upper conversion function material layer is tiled by the inorganic nanometer powder or organic fluorescence powder with near-infrared upper conversion function to form.
2. photon crystal structure according to claim 1, is characterized in that the thickness of described layer of photonic crystals is between 2-3um.
3. photon crystal structure according to claim 1; It is characterized in that the thickness of described upper conversion function material layer is between 250nm-450nm.
4. photon crystal structure according to claim 1, is characterized in that the general formula of described inorganic nanometer powder is: NaYF
4: Yb
3+, R
3+, wherein R
3+for the one in thulium, erbium or europium.
5. photon crystal structure according to claim 1, is characterized in that the general formula of described organic fluorescence powder is: Yb
x, R
1-x(TTA)
3phen, wherein R is the one in thulium, erbium or europium, and x is any one real number between 0.1-0.9.
6. prepare a method as claimed in claim 1 with the photon crystal structure strengthening and regulate upper transformational substance lighting function, its concrete steps are as follows:
Prepared by A, layer of photonic crystals: be distributed in solvent by the silicon dioxide microsphere of 200nm-400nm size, be made into self assembly liquid, the mass concentration of silicon dioxide dispersion soln is 0.5%-2%; Then by solution ultrasonic disperse; Finally by self assembly liquid join in self assembly region, form layer of photonic crystals after natural drying;
Prepared by B, upper conversion function material layer: be made into 10 for being dissolved in organic solvent by up-conversion phosphor
-5-10
-3the solution of mol/L concentration, ultrasonic disperse, uses the layer of photonic crystals surface that upper conversion solution spraying is prepared to steps A by spray gun; Obtained upper conversion function material layer;
C, prepare silicon dioxide photon self assembly liquid with steps A, then silicon dioxide self assembly liquid is joined on the obtained upper conversion function material layer of step B, then form one deck layer of photonic crystals; Natural drying obtains final composite construction;
D, sandwich obtained for step C is put in 200-300 degree Celsius of heat treatment 3-5 hour in Muffle furnace, obtains having the photon crystal structure strengthening and regulate upper transformational substance lighting function.
7. method according to claim 6, is characterized in that the solvent described in steps A is ethanol or water; Organic solvent described in step B is cyclohexane, ethanol or dimethyl sulfoxide (DMSO).
8. method according to claim 6, is characterized in that the parameter of the ultrasonic disperse described in steps A and B is: power is 400-1200w, and the time is 0.5-1h.
9. method according to claim 6, is characterized in that the thickness of layer of photonic crystals in steps A and C is 2-3um; In step B, the thickness of upper conversion function material layer is between 250nm-450nm.
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