CN108191256A - Lower conversion anti-reflection film of one kind and preparation method and application - Google Patents
Lower conversion anti-reflection film of one kind and preparation method and application Download PDFInfo
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- CN108191256A CN108191256A CN201810082111.XA CN201810082111A CN108191256A CN 108191256 A CN108191256 A CN 108191256A CN 201810082111 A CN201810082111 A CN 201810082111A CN 108191256 A CN108191256 A CN 108191256A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 111
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 60
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 25
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 25
- 239000011521 glass Substances 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 40
- 239000011259 mixed solution Substances 0.000 claims description 31
- 238000010438 heat treatment Methods 0.000 claims description 29
- 235000019441 ethanol Nutrition 0.000 claims description 28
- 239000002202 Polyethylene glycol Substances 0.000 claims description 26
- 229920001223 polyethylene glycol Polymers 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 18
- BHXBZLPMVFUQBQ-UHFFFAOYSA-K samarium(iii) chloride Chemical compound Cl[Sm](Cl)Cl BHXBZLPMVFUQBQ-UHFFFAOYSA-K 0.000 claims description 15
- 239000003153 chemical reaction reagent Substances 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 5
- 229910001954 samarium oxide Inorganic materials 0.000 claims description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Natural products CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 claims description 2
- 230000029087 digestion Effects 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 229940075630 samarium oxide Drugs 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 6
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000005693 optoelectronics Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 105
- 229910052761 rare earth metal Inorganic materials 0.000 description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- 229910052681 coesite Inorganic materials 0.000 description 10
- 229910052906 cristobalite Inorganic materials 0.000 description 10
- 229910052682 stishovite Inorganic materials 0.000 description 10
- 229910052905 tridymite Inorganic materials 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 150000002910 rare earth metals Chemical class 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 238000010348 incorporation Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 230000007704 transition Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- -1 rare earth ion Chemical class 0.000 description 6
- 230000003595 spectral effect Effects 0.000 description 6
- 238000004020 luminiscence type Methods 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 239000003960 organic solvent Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000003980 solgel method Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 230000005283 ground state Effects 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical class CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 3
- 230000005281 excited state Effects 0.000 description 3
- 238000001755 magnetron sputter deposition Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000013543 active substance Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 238000002310 reflectometry Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 241000790917 Dioxys <bee> Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000010307 cell transformation Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
-
- 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
- H01L31/0248—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 characterised by their semiconductor bodies
- H01L31/0256—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 characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/028—Inorganic materials including, apart from doping material or other impurities, only elements of Group IV of the Periodic Table
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/213—SiO2
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes
-
- 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
- Y02E10/547—Monocrystalline silicon PV cells
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to anti-reflection film and preparation method and application is converted under one kind, belong to opto-electronic device field of material technology.The preparation method includes the following steps：With the silicon dioxide gel containing samarium in glass basic surface plated film, then it is heat-treated, cools down under conditions of 200 500 DEG C.This method is easy to operate, and equipment requirement is relatively low, time-consuming short, suitable for large-scale production.Thus obtained lower conversion anti-reflection film transmitance and relative luminous intensity are relatively strong, to visible ray also with certain anti-reflection function while with certain lower conversion performance.It uses it for preparing silica-based solar cell, the photoelectric conversion efficiency of silica-based solar cell can be improved.
Description
Technical field
The present invention relates to opto-electronic device field of material technology, and more particularly to a kind of lower conversion anti-reflection film and its preparation
Method and application.
Background technology
The maximum value of its photoelectric conversion efficiency of unijunction silica-based solar cell is 26.7% at present, and practical turn on the market
One of the main reason for change efficiency only 18%-22%, silica-based solar cell transfer efficiency is low：Silica-based solar cell cannot
Whole sunlights is converted into electric energy；Particularly in ultraviolet high frequency region, the characteristics of showing high reflection, low absorption.It is so logical
Cross spectral modulation make silica-based solar cell more fully, more reasonably using sunlight, improve the photoelectricity of silica-based solar cell
Transfer efficiency is the emphasis currently paid close attention to.
YF is reported early in W.W.Piper in 1974 etc.3：Pr3+In lower transfer process, Pr3+:4f → 5d absorbs one
The photon of 185nm, and release a 407nm blue photons (1S0→1I6) and a 620nm red photons (3P0→3FJ,3HJ).Therefore surface introduces lower conversion luminescent layer on the solar cell, absorbs a poor ultraviolet shortwave of battery spectral response
Long photon, then launch the good two or more photons of spectral response, so that it may the spectral response of battery is improved, reduces current-carrying
Sub- thermalization loss increases the photoelectric conversion efficiency of silicon solar cell.Lower conversion is pure two-phonon process, by lower conversion layer application
In photovoltaic system, maximum advantage is not need to be changed existing solar cell.In theory, spectrum is utilized
Silicon solar cell photoelectric conversion efficiency may be increased to 39.63% by conversion, but realize so high conversion effect in practice
Rate is far away, thus needs more basic research.
Lower switching film luminescence mechanism is realized by the special level structure of rare earth ion, the photism of rare earth ion
Matter mainly depends on rare earth ion underfill and influenced by the 4f shell electron properties of outer shield, mainly includes between configuration
F-f transition in f-d transition and configuration, f-f transition relate generally to ion and include：Pr3+、Nd3+、Eu3+、Tb3+、Er3+And Yb3+
Deng.Wherein Pr3+、Er3+、Yb3+Though there is f electronics in ion, electron transition energy level is more, and between excitation state and ground state spectral cterm
Energy level spacing is smaller, and when being excited, transition of the f electronics between each spectral cterm will generate stronger Nonradiative decay so that
It shines relatively weak.And Eu3+And Tb3+Lowest excited state and ground state between energy level difference be respectively 12500cm-1With
14800cm-1, shine relatively above-mentioned ion it is stronger.
Lower switching film method is prepared at present mainly to include：Magnetron sputtering method and Sol-Gel methods.Wherein, magnetron sputtering method
The film quality of preparation is higher, uniformly, adhesive force it is good and more accurate to the control of film thickness.But it is higher to equipment requirement, be not easy
It is precisely controlled the incorporation of rare earth, is unsuitable for mass producing.Sol-Gel methods are compared to magnetron sputtering method, to rare earth incorporation
It is easy to control, and easy to operate, low to substrate requirements, convenient for preparing on a large scale, but silicon dioxide gel prepared by Sol-Gel methods
In contain great amount of hydroxy group, hydroxyl can weaken the luminescent properties of rare earth ion；And refractive index can increase after silica membrane heat treatment
Greatly so that the transmitance of film reduces.
Invention content
One of the objects of the present invention is to provide a kind of preparation methods of lower conversion anti-reflection film, and this method is easy to operate,
Equipment requirement is relatively low, time-consuming short, suitable for large-scale production.
The second object of the present invention is to provide a kind of lower conversion anti-reflection film being prepared by above-mentioned preparation method, be somebody's turn to do
Lower conversion anti-reflection film transmitance and relative luminous intensity are relatively strong, to visible ray while with certain lower conversion performance
Also there is certain anti-reflection function.
The third object of the present invention is to provide a kind of application of above-mentioned lower conversion anti-reflection film, such as can use it for
Silica-based solar cell is prepared, to improve the photoelectric conversion efficiency of silica-based solar cell.
The present invention is solved its technical problem and is realized using following technical scheme：
The present invention proposes a kind of preparation method of lower conversion anti-reflection film, includes the following steps：With the silica containing samarium
Then colloidal sol is heat-treated under conditions of 200-500 DEG C, cools down in glass basic surface plated film.
Preferably, plated film is carried out under the rejection film speed of 3000-4000r/min.
Preferably, before heat treatment, the film of gained after plated film is dried into 25-35min under conditions of 95-100 DEG C.
The present invention also proposes a kind of lower conversion anti-reflection film, is prepared by above-mentioned preparation method.
The present invention also proposes a kind of application of above-mentioned lower conversion anti-reflection film, such as uses it for preparing silica-based solar electricity
Pond.
The advantageous effect for the lower conversion anti-reflection film and preparation method and application that present pre-ferred embodiments provide is：
The lower conversion anti-reflection film of present pre-ferred embodiments is with rare-earth Sm3+As light-emitting element, lowest excited state and
Energy level difference between ground state is 7400cm-1, the Nonradiative decay probability of f-f transition is smaller, radiation wavelength in visible region, and
Sm3+Radiation wavelength is located at the visible ray of 500nm-700nm namely positioned at the highest optical wavelength of silica-based solar cell transformation efficiency
Range can effectively realize ultraviolet lower conversion, and Sm3+Price it is relatively cheap, convenient for large-scale production prepare.
The SiO prepared due to the embodiment of the present invention with sol-gel method2Film contains a large amount of organic solvent and water,
SiO2A large amount of hydroxyl is contained on the surface of particle, and hydroxyl can seriously weaken the luminescent properties of rare earth ion, also influence whether SiO2It is thin
The quality of forming film of film by heat treatment, can remove the organic solvent and water contained in film, improves and converts anti-reflection film under finished product
Photism.
The preparation method for the lower conversion anti-reflection film that present pre-ferred embodiments provide is easy to operate, and equipment requirement is relatively low,
It is time-consuming short, suitable for large-scale production.The lower conversion anti-reflection film transmitance and relative luminous be prepared by above-mentioned preparation method
Intensity is relatively strong, to visible ray also with certain anti-reflection function while with certain lower conversion performance.It uses it for
Silica-based solar cell is prepared, the photoelectric conversion efficiency of silica-based solar cell can be improved.
Description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, to embodiment or will show below
There is attached drawing needed in technology description to be briefly described.
Fig. 1 is lower switching film luminescent properties in test example 1 with Sm3+The change curve of incorporation；
Fig. 2 is emission spectrum contrast curve of the lower switching film at a temperature of different heat treatment in test example 2；
Fig. 3 is transmittance curve figure of the lower switching film at a temperature of different heat treatment in test example 3.
Specific embodiment
Purpose, technical scheme and advantage to make the embodiment of the present invention are clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Lower conversion anti-reflection film of the embodiment of the present invention and preparation method and application is specifically described below.
The preparation method of lower conversion anti-reflection film provided in the embodiment of the present invention for example may comprise steps of：To contain
Then the silicon dioxide gel of samarium is heat-treated under conditions of 200-500 DEG C, cools down in glass basic surface plated film.
Wherein, substrate uses silica glass compatible with existing solar battery process, environmental-friendly as substrate.
Optionally, the silicon dioxide gel containing samarium can by the first mixed solution, samarium trichloride and polyethylene glycol mix and
.Wherein, the first mixed solution is obtained by mixing by ethyl orthosilicate, organic alcohol and water, this step by disposably mixing addition,
Processing step, simplification of flowsheet can be saved.Preferably, above-mentioned Organic Alcohol is ethyl alcohol.What deserves to be explained is the embodiment of the present invention
In water used be deionized water, to avoid under the influence of the foreign ion in water convert anti-reflection film performance.
Further, above-mentioned samarium trichloride (SmCl3) can be by samarium oxide (Sm2O3) with water and mixed in hydrochloric acid and obtain.Preferably,
The concentration of above-mentioned samarium trichloride can be 0.05-2mol/L, more preferably, a concentration of 1mol/L of samarium trichloride.With rare-earth Sm3+As hair
Photoelement, the energy level difference between lowest excited state and ground state are 7400cm-1, the Nonradiative decay probability of f-f transition is smaller, spoke
Ejected wave is grown in visible region, and Sm3+Radiation wavelength is located at the visible ray of 500nm-700nm namely positioned at silica-based solar cell
The highest optical wavelength range of transformation efficiency can effectively realize ultraviolet lower conversion, and Sm3+Price it is relatively cheap, convenient for advising greatly
It is prepared by mould production.
Optionally, in the first mixed solution, ethyl orthosilicate, second alcohol and water volume ratio such as can be 30-40：
30-40：5-6.Preferably, ethyl orthosilicate, second alcohol and water volume ratio be 35：36：5.5.
Optionally, in the first mixed solution, ethyl orthosilicate, second alcohol and water mass concentration ratio for example can be 1：
3-5：1-3, it is preferable that mass concentration ratio 1：3.5-4.5：1.5-2.5, more preferably, mass concentration ratio 1：4：2.
Optionally, the silicon dioxide gel containing samarium in the embodiment of the present invention can also by the first mixed solution, samarium trichloride and
Polyethylene glycol substep is obtained by mixing.Specifically, it can refer to following substep situation：The first mixed solution and samarium trichloride are first mixed, is obtained
Then second mixed solution remixes the second mixed solution and polyethylene glycol.
Second mixed solution is preferably stirred with polyethylene glycol under water-bath controlled temperature conditions.Wherein, bath temperature is controllable
System is at 50-60 DEG C, preferably 55 DEG C.It by water-bath temperature control, can not only promote the hydrolysis rate of ethyl orthosilicate, save the time,
And also can ensure that the second mixed solution and polyethylene glycol mix under relatively suitable temperature condition, it both improves mutual molten
Solution degree.Correspondingly, the time being stirred under above-mentioned temperature range can be for example controlled in 1h or so.
Why polyethylene glycol is added in the raw material of the silicon dioxide gel containing samarium, reason is：Polyethylene glycol exists
Modifying function is played in the embodiment of the present invention, hydroxyl in colloidal sol can be reduced by its cross-linking reaction between silicon dioxide gel ion
Influence of the base to rare earth luminescence performance.Also, the pore-creating effect of polyethylene glycol high polymerization degree macromolecular can also reduce dioxy
The refractive index of SiClx film.Optionally, the average molecular weight of above-mentioned polyethylene glycol can be 1000-2000.
Viscosity through the silicon dioxide gel containing samarium obtained by aforesaid operations is larger, substantially in 10-14Pas ranges.
Preferably, the pH value of above-mentioned second mixed solution is controllable to 2-3, then hydrochloric acid can be used to be adjusted beyond 2-3.It should
PH value range may advantageously facilitate teos hydrolysis and obtain silicon dioxide gel.
Further, it before plated film, will be aged as the silicon dioxide gel containing samarium obtained by the above method, as optional
Ground, digestion time for example can be 10-14h, preferably 12h, through the above-mentioned time be aged after the silicon dioxide gel containing samarium in
Each component is fully reacted, and quality is further improved.
Before the silicon dioxide gel for containing samarium is plated on glass basic surface, substrate of glass is cleaned.Optionally, it cleans for example
Ultrasonic cleaning can be used, by ul-trasonic irradiation, so as to which each position of substrate of glass fully be cleaned up.
Cleaning amounts to and can carry out four times in the embodiment of the present invention, is successively in water, the first reagent, the respectively by substrate of glass
It is cleaned by ultrasonic in two reagents and water.Wherein, the first reagent and the second reagent are respectively acetone and ethyl alcohol or the first reagent and second
Reagent is respectively sulfuric acid and hydrogen peroxide.
Above-mentioned first time is washed with water its purpose is that removing most of water-solubility impurity of substrate of glass.Acetone is used for the second time
Or the purpose of sulfuric acid cleaned is to remove lyophobic dust contained in substrate of glass, such as oil substances.Third time ethyl alcohol
Or the purpose of hydrogen peroxide cleaning is to remove the remaining acetone of institute or sulfuric acid after second of cleaning.The purpose washed with water for 4th time is
Remove the remaining ethyl alcohol of institute or hydrogen peroxide after third time is cleaned.
What deserves to be explained is reagent is compromise between security and reality used by above-mentioned second of cleaning and third time are cleaned
The preferred version selected is integrated with property.In addition, acetone also can be used toluene to replace, but toluene is larger to human body toxic；Ethyl alcohol
It can be replaced with isopropanol, but the practical degree of isopropanol is far below ethyl alcohol.
After cleaning, glass substrate is dried.Then plated film is carried out with the silicon dioxide gel containing samarium being aged.Plated film can
It is carried out on sol evenning machine, optionally, plated film can carry out, such as 3500r/min under the rejection film speed of 3000-4000r/min.
Further, the film of gained after plated film is dried into 25-35min under conditions of 95-100 DEG C.Then then at
Heat treatment 0.8-1.5h (such as 1h) under conditions of 200-500 DEG C (preferably 500 DEG C), cools down to get lower conversion anti-reflection film.
Why it is heat-treated, is the SiO prepared due to sol-gel method of the embodiment of the present invention2Film contains greatly
The organic solvent and water of amount, in SiO2A large amount of hydroxyl is contained on the surface of particle, and hydroxyl can seriously weaken shining for rare earth ion
Performance also influences whether SiO2The quality of forming film of film by heat treatment, can remove the organic solvent and water contained in film,
Improve the photism that anti-reflection film is converted under finished product.
In addition, the embodiment of the present invention additionally provides a kind of application of above-mentioned lower conversion anti-reflection film, such as can use it for
Silica-based solar cell is prepared, thus to improve the photoelectric conversion efficiency of silica-based solar cell.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
Using mass concentration ratio as 1:4:2 mix 35mL ethyl orthosilicates, 36mL ethyl alcohol and 5.5mL deionized waters, obtain the
One mixed solution.
Mix Sm2O3(purity 99.9%) and deionized water and hydrochloric acid, obtain the SmCl of 1mol/L3Solution.
Above-mentioned first mixed solution with the samarium trichloride of 2.3mL is mixed, obtains the second mixed solution.By the second mixed solution with
2g polyethylene glycol (average molecular weight 2000) is stirred 1h under the conditions of 55 DEG C of constant temperature water bath, obtains the silica containing samarium
Colloidal sol.The above-mentioned silicon dioxide gel containing samarium is aged 12h.
Substrate of glass piece is respectively cleaned by ultrasonic 20min in deionized water, acetone, ethyl alcohol and deionized water successively, is put into
It is dried in baking oven.
The silicon dioxide gel containing samarium being aged is subjected to plated film, rejection film on sol evenning machine to the glass substrate after cleaning
Speed is 3500r/min.Gained film after plated film is subjected to drying and processing 30min at 100 DEG C.
Then above-mentioned film print is put into annealing furnace at 500 DEG C again and is heat-treated 1h, taken with stove cooled to room temperature
Go out print, obtain lower conversion anti-reflection film.
Embodiment 2
Using mass concentration ratio as 1:3:1 mixes 30mL ethyl orthosilicates, 30mL ethyl alcohol and 5mL deionized waters, obtains first
Mixed solution.
Mix Sm2O3(purity 99.9%) and deionized water and hydrochloric acid, obtain the SmCl of 0.05mol/L3Solution.
Above-mentioned first mixed solution with the samarium trichloride of 2.0mL is mixed, adjusts pH value, it is molten to obtain the second mixing that pH value is 2
Liquid.Second mixed solution and 2g polyethylene glycol (average molecular weight 2000) are stirred under the conditions of 50 DEG C of constant temperature water bath
1.2h obtains the silicon dioxide gel containing samarium.The above-mentioned silicon dioxide gel containing samarium is aged 10h.
Substrate of glass piece is respectively cleaned by ultrasonic 15min in deionized water, sulfuric acid, hydrogen peroxide and deionized water successively, is put
Enter in baking oven and dry.
The silicon dioxide gel containing samarium being aged is subjected to plated film, rejection film on sol evenning machine to the glass substrate after cleaning
Speed is 3000r/min.Gained film after plated film is subjected to drying and processing 35min at 95 DEG C.
Then above-mentioned film print is put into annealing furnace at 200 DEG C again and is heat-treated 1.5h, with stove cooled to room temperature
Print is taken out, obtains lower conversion anti-reflection film.
Embodiment 3
Using mass concentration ratio as 1:5:3 mix 40mL ethyl orthosilicates, 40mL ethyl alcohol and 6mL deionized waters, obtain first
Mixed solution.
Mix Sm2O3(purity 99.9%) and deionized water and hydrochloric acid, obtain the SmCl of 2mol/L3Solution.
Above-mentioned first mixed solution with the samarium trichloride of 2.5mL is mixed, adjusts pH value, it is molten to obtain the second mixing that pH value is 3
Liquid.Second mixed solution and 2g polyethylene glycol (average molecular weight 2000) are stirred under the conditions of 60 DEG C of constant temperature water bath
0.8h obtains the silicon dioxide gel containing samarium.The above-mentioned silicon dioxide gel containing samarium is aged 14h.
Substrate of glass piece is respectively cleaned by ultrasonic 25min in deionized water, toluene, isopropanol and deionized water successively, is put
Enter in baking oven and dry.
The silicon dioxide gel containing samarium being aged is subjected to plated film, rejection film on sol evenning machine to the glass substrate after cleaning
Speed is 4000r/min.Gained film after plated film is subjected to drying and processing 25min at 98 DEG C.
Then above-mentioned film print is put into annealing furnace at 300 DEG C again and is heat-treated 0.8h, with stove cooled to room temperature
Print is taken out, obtains lower conversion anti-reflection film.
Embodiment 4
The present embodiment and embodiment 1 it is unique difference lies in：First mixed solution, samarium trichloride and polyethylene glycol mix simultaneously
It closes.
Embodiment 5
The present embodiment and embodiment 1 it is unique difference lies in：The mass concentration ratio of ethyl orthosilicate, ethyl alcohol and deionized water
It is 1:3.5:1.5.
Embodiment 6
The present embodiment and embodiment 1 it is unique difference lies in：The mass concentration ratio of ethyl orthosilicate, ethyl alcohol and deionized water
It is 1:4.5:2.5.
Embodiment 7
The present embodiment and embodiment 1 it is unique difference lies in：The temperature of heat treatment is 400 DEG C.
Embodiment 8
The present embodiment and embodiment 1 it is unique difference lies in：Organic Alcohol in first mixed solution is isopropanol.
Embodiment 9
The present embodiment and embodiment 1 it is unique difference lies in：Organic Alcohol in first mixed solution is methanol.
Embodiment 10
The present embodiment and embodiment 1 it is unique difference lies in：The average molecular weight of polyethylene glycol is 1000.
Embodiment 11
The present embodiment and embodiment 1 it is unique difference lies in：The average molecular weight of polyethylene glycol is 1500.
Embodiment 12
The present embodiment provides a kind of application of conversion anti-reflection film lower made from above-described embodiment 1-11 any embodiments, tools
Body is set to the surface of silica-based solar cell as conversion luminescent layer.
Test example 1
Using the lower anti-reflection film of converting obtained by the embodiment of the present invention into sample to be tested, Sm is measured3+The difference amount of participating under
The influence of anti-reflection film luminescent properties is converted, the results are shown in Figure 1.Fig. 1 is lower switching film luminescent properties with Sm3+Incorporation
Change curve, wherein (a) representative is not added with polyethylene glycol (PEG), (b) is represented added with polyethylene glycol.
As seen from Figure 1, with Sm3+The increase of incorporation, the luminescent properties of lower conversion anti-reflection film also enhance therewith；
It is better than being not used the lower switching film of PEG modifications added with the luminescent properties of the PEG lower switching films being modified；Work as Sm3+Incorporation
When being 8%, the luminescent properties of material are best；Later again with Sm3+Incorporation continue to increase, the photism of lower switching film
It can be deteriorated, it follows that the Sm in lower switching film3+Quenching concentration 8% or so.Under normal conditions, the hair of luminescent material
Luminous intensity is as the doping concentration of optical active substance improves and is enhanced, but when optical active substance concentration reaches certain
After value, the luminous intensity of material can drastically decline or even no longer shine, and this phenomenon is referred to as concentration quenching.Due to SiO2It is molten
Hydroxyl in glue has rare earth luminescence a quenching effect, a large amount of oxygen atom and SiO in PEG2The a large amount of hydroxyls in sol particles surface
Base forms hydrogen bond, and PEG is made to be wrapped in SiO2Particle surface reduces quenching effect of the hydroxyl to rare earth luminescence, so as to reach
The effect of enhanced film luminescent properties.
Test example 2
Using the lower anti-reflection film of converting obtained by the embodiment of the present invention into sample to be tested, different heat treatment temperatures is measured under
The influence of anti-reflection film luminescent properties is converted, the results are shown in Figure 2.Fig. 2 is lower switching film at a temperature of different heat treatment
Emission spectrum contrast curve, wherein it is 200 DEG C that (a), which represents heat treatment temperature, it is 300 DEG C that (b), which represents heat treatment temperature,
(c) it is 400 DEG C to represent heat treatment temperature, and (d) represents heat treatment temperature as 500 DEG C.
As seen from Figure 2, to mixing Sm3+Lower conversion anti-reflection film carry out hot place and the film after heat treatment carried out glimmering
Light detection, the position of emission peak do not change, and emissive porwer changes greatly, with the raising of heat treatment temperature, the hair of film
Optical property is become better and better.The reason for this is that：To SiO2When film is heat-treated, with the raising of heat treatment temperature, lower conversion
Moisture and removing hydroxyl removal in film is more abundant, SiO2Reaction between particle is also strengthened, to caused by hydroxyl in material
The effect that rare earth luminescence is quenched is reduced so that SiO2Sm in film3+Luminescent properties become better and better；Since the present invention is implemented
The fusing point of substrate of glass is at 600 DEG C or so used by example, and 500 DEG C or more of heat treatment is not tested again, but theoretical
The luminescent properties of the upper film have substantially been stablized in 500 DEG C of heat treatments, and variation is little because organic solvent and water oneself wave completely
Hair, the number of hydroxyl is seldom, so in the heat treatment SiO of higher temperature2The luminous intensity variations of film can be less.
Test example 3
Using the lower anti-reflection film of converting obtained by the embodiment of the present invention into sample to be tested, different heat treatment temperatures is measured under
The influence of the transmitance of anti-reflection film is converted, the results are shown in Figure 3.Fig. 3 is lower switching film at a temperature of different heat treatment
Transmittance curve figure, wherein it is 300 DEG C that (a), which represents heat treatment temperature, it is 500 DEG C that (b), which represents heat treatment temperature, (c) represent
Blank glass.
As seen from Figure 3, lower switching film glass is after heat treatment, equal in the range of 380-800nm visible light wave ranges
There is higher transmitance, two cluster film sample of (a), (b) is high 7%-10% than blank glass transmitance in visible light wave range.
(b) 500 DEG C of heat treatments have dropped 1.5%- compared to (a) 300 DEG C of heat treatment film samples in the transmitance of entire visible waveband
2.4%.Influencing the factor of transmitance mainly has the thickness and refractive index of silica membrane, and the thickness of film is mainly by spin coating
The time of speed and silicon dioxide gel ageing determines that refractive index is matched by colloidal sol and the concentration of Doped ions determines.At heat
Comprehending makes organic matter in film largely decompose, and different heat treatment temperatures leads to roughness of film and SiO2Grain diameter
Difference shows as film refractive index and becomes larger so that film sample is declined in the transmitance of entirely test wave band.So using
PEG is modified the silicon dioxide gel of rare earth doped samarium, utilizes the pore-creating effect of PEG macromolecule link structures so that point
Gap increase between son, and reduce thin-film refractive index.[18] are pointed out in theoretical research, in the case of light vertical incidence, monofilm
Reflectivity：(n in formula1Refractive index for film layer；n0、nsRespectively film two
The refractive index of side medium).According to law of conservation of energy：R+ α+T=1, in the case where absorption α is identical, reflectivity R is smaller,
Transmissivity T is bigger, so as to increase the transmitance of film.
In conclusion the preparation method of lower conversion anti-reflection film provided in an embodiment of the present invention is easy to operate, equipment requirement
It is relatively low, it is time-consuming short, suitable for large-scale production.The lower conversion anti-reflection film transmitance that be prepared by above-mentioned preparation method and opposite
Luminous intensity is relatively strong, to visible ray also with certain anti-reflection function while with certain lower conversion performance.By its
Silica-based solar cell is used to prepare, the photoelectric conversion efficiency of silica-based solar cell can be improved.
Embodiments described above is part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of lower conversion anti-reflection film, which is characterized in that include the following steps：It is molten with the silica containing samarium
Then glue is heat-treated under conditions of 200-500 DEG C, cools down in glass basic surface plated film；
Preferably, plated film is carried out under the rejection film speed of 3000-4000r/min；
Preferably, before heat treatment, the film of gained after plated film is dried into 25-35min under conditions of 95-100 DEG C.
2. preparation method according to claim 1, which is characterized in that the silicon dioxide gel containing samarium is through following steps
It obtains：Mix the first mixed solution, samarium trichloride and polyethylene glycol；
First mixed solution is obtained by mixing by ethyl orthosilicate, organic alcohol and water；
Preferably, the Organic Alcohol is ethyl alcohol.
3. preparation method according to claim 2, which is characterized in that the samarium trichloride is by samarium oxide and water and mixed in hydrochloric acid
And it obtains；
Preferably, a concentration of 0.05-2mol/L of the samarium trichloride；
More preferably, a concentration of 1mol/L of the samarium trichloride.
4. preparation method according to claim 2, which is characterized in that the ethyl orthosilicate, the second alcohol and water body
Product is than being 30-40：30-40：5-6；
Preferably, the ethyl orthosilicate, the second alcohol and water volume ratio be 35：36：5.5.
5. preparation method according to claim 2, which is characterized in that the ethyl orthosilicate, the second alcohol and water matter
It is 1 to measure concentration ratio：3-5：1-3；
Preferably, the ethyl orthosilicate, the second alcohol and water mass concentration ratio be 1：3.5-4.5：1.5-2.5；
More preferably, the ethyl orthosilicate, the second alcohol and water mass concentration ratio be 1：4：2.
6. preparation method according to claim 2, which is characterized in that first mix first mixed solution and the chlorination
Samarium, obtains the second mixed solution, then remixes second mixed solution and the polyethylene glycol；
Preferably, the pH value of second mixed solution is 2-3；
Preferably, second mixed solution is stirred with the polyethylene glycol under conditions of 50-60 DEG C.
7. preparation method according to claim 1, which is characterized in that before plated film, by the silicon dioxide gel containing samarium
It is aged；
Preferably, digestion time 10-14h.
8. preparation method according to claim 1, which is characterized in that before plated film, clean the substrate of glass；
Preferably, cleaning is using ultrasonic cleaning；
Preferably, cleaning is to be cleaned by ultrasonic the substrate of glass in water, the first reagent, the second reagent and water successively；
First reagent and second reagent are respectively acetone and ethyl alcohol or first reagent and second reagent point
It Wei not sulfuric acid and hydrogen peroxide.
9. the lower conversion anti-reflection film of one kind, which is characterized in that the lower conversion anti-reflection film is by such as any one of claim 1-8 institutes
The preparation method stated is prepared.
10. application of the lower conversion anti-reflection film as claimed in claim 9 in silica-based solar cell is prepared.
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