CN103921505A - Up-conversion photoluminescence glass and preparation method thereof - Google Patents
Up-conversion photoluminescence glass and preparation method thereof Download PDFInfo
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- CN103921505A CN103921505A CN201410118077.9A CN201410118077A CN103921505A CN 103921505 A CN103921505 A CN 103921505A CN 201410118077 A CN201410118077 A CN 201410118077A CN 103921505 A CN103921505 A CN 103921505A
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Abstract
The invention relates to the technical field of optical functional glass, in particular to an up-conversion photoluminescence glass. The up-conversion photoluminescence glass comprises a glass base plate and an up-conversion photoluminescence transparent film arranged on at least one surface of the glass base plate; the up-conversion photoluminescence glass is characterized in that the up-conversion photoluminescence transparent film is composed of partially or completely cured product of silicon dioxide sol and up-conversion photoluminescence crystallized grains, wherein the up-conversion photoluminescence crystallized grains are uniformly dispersed in the partially or completely cured product of silicon dioxide sol. The up-conversion photoluminescence glass has the advantages of simple structure, high visible light transmittance and low production cost, and is suitable for mass production. The invention also provides a high-efficiency low-cost preparation method of the up-conversion photoluminescence glass.
Description
Technical field:
The present invention relates to optical functional glass technical field, particularly a kind of upper converting photoluminescent glass and preparation method thereof.
Background technology:
Upper converting photoluminescent glass has extensive use at aspects such as solar energy utilization, false proof and optical detections.Upper converting photoluminescent glass and solar photovoltaic device are compound, part near infrared light in solar spectrum can be converted to visible ray and then improve utilization rate and the conversion efficiency of photovoltaic device to sunray.Along with photoelectric technology and the diversified development of display device, photoluminescent transparent display device causes people's research interest day by day, is one of effective way of preparing photoluminescent transparent display device by converting photoluminescent functionalization on glass.
At present, the method for glass light photoluminescence functionalization mainly contains following three kinds:
1) one of component using active ions or fluorescent material as glass joins in frit, prepares fluorescent glass through operations such as grinding, high-temperature calcinations, and this fluorescent glass heat endurance is high.
As Chinese patent CN103265172A discloses a kind of preparation method of fluorescent glass.Inventor is by the YAG:Sm of 0.8g
3+, Bi
3+the BaCO of fluorescent material and 1g
3, the NaCO of 0.4g
3, the H of 0.9g
3pO
4, the SiO of 0.3g
2, the Al of 0.56g
2o
3after ground and mixed is even, packs corundum crucible into and at 1400 DEG C of temperature lower calcinations, be incubated after 4 hours and take out the cooling fluorescent glass that obtains of nature, gained fluorescent glass has feature PLE and the emission spectra of samarium ion.
But it is unpractical that the raw material components using fluorescent material as float glass is produced in batches.
2) this external component of fluorescent material is directly penetrated into the glass plate of softening or partial melting from glass surface under high temperature action, finally form fluorescent powder/glass complex, this scheme technique is simple.
As US Patent No., 20130004699A1 discloses a kind of fluorescent glass and preparation method thereof.This fluorescent glass comprises two parts: glass matrix and fluorescence-glass composite, wherein fluorescence-glass composite is the vitreum that has wherein disperseed fluorescent material.The preparation method of this fluorescent glass is: cerium ion-doped terbium aluminium garnet fluorescent material is placed in to a glass plate upper surface, then heats this glass plate and make it to occur softening.In heating process, fluorescent material automatically infiltrates layer region on glass and disperses wherein, treat cooling solidify after this glass plate just become and be dispersed with the recombination region of fluorescent material and the glass basis region without fluorescent material, the former is fluorescence-glass composite.In this technical scheme, inventor is immersed cerium ion-doped terbium aluminium garnet fluorescent material in softening glass below glass melting temperature, can effectively avoid reacting between fluorescent material and glass, and then ensure the stability of inside glass fluorescent material physical and chemical performance and the reliability of spectrum property.
But this scheme is disadvantageous for conventionally all having certain radian profile and mechanical performance is required to strict vehicle glass, because glass not only can deform in high-temperature heating process, also can there is remarkable change in the mechanical performances such as its intensity of while, fragility.
3) utilize sol-gal process at glass surface deposition one deck Photoluminescence thin film, this film and glass basis form a multiple device.
As Chinese patent CN103205255A provides a kind of rare earth ion doped LiYF for preparing on glass basis
4the method of up-conversion luminescence film: first, a certain amount of trifluoroacetic acid is done to reactant by lithium acetate, acetic acid yttrium, acetic acid erbium is dissolved in and in methyl alcohol, forms trifluoroacetic acid solution, then by dip-coating method or spin coating method, above-mentioned solution is coated in to glass or above quartz substrate, it is heat-treated at a certain temperature and gets final product whitely and LiYF that luminescent properties is good after to be dried
4rete.
Utilizing sol-gel technique is to realize the comparatively feasible approach of glass devices luminescence generated by light functionalization at glass surface deposition one deck fluorescence membrane.Sol-gel technique belongs to wet chemistry method, the adverse effect that adopts suitable technique just can effectively avoid high-temperature process to cause glass basis.Gel rete and glass basis after heat treatment combine, and gel-type vehicle is illuminator: crystalline state LiYF
4: Er
3+, Yb
3+.Utilizing sol-gal process to prepare in the process of light-emitting film, the hydroxyl in solution can with active ions bonding.Due to vibration phonon energy and the Er of hydroxyl
3+the infrared transistion energy equivalence of ion, this bonding can the violent radiationless transition probability that increases active ions.Therefore in order to improve LiYF
4: Er
3+, Yb
3+the luminous efficiency of film, must carry out high-temperature heat treatment to it, and to get rid of with the hydroxyl of active ions bonding and to make film crystallization, but now film becomes white, no longer transparent.
Summary of the invention:
Technical problem to be solved by this invention is the above-mentioned technical problem existing for existing upper converting photoluminescent glass, a kind of simple in structure, upper converting photoluminescent glass that visible light transmissivity is high is provided, a kind of high efficiency is also provided simultaneously, goes up the preparation method of converting photoluminescent glass cheaply.
The present invention solves the technical scheme that its technical problem takes: converting photoluminescent glass in one, comprise glass substrate and at least one the lip-deep upper converting photoluminescent transparent membrane that is arranged on glass substrate, it is characterized in that: described upper converting photoluminescent transparent membrane is mainly made up of partly or completely cured product and the upper converting photoluminescent crystalline particles of silicon dioxide gel, and described upper converting photoluminescent crystalline particles is dispersed in the partly or completely cured product of described silicon dioxide gel.
Further, the density that described upper converting photoluminescent crystalline particles is disperseed on the face of upper converting photoluminescent transparent membrane is 0.05～2g/m
2.
Further; the thickness of described upper converting photoluminescent transparent membrane is not more than 10 μ m, and described upper converting photoluminescent crystalline particles is that cross-sectional diameter is that cylindrical particle, cross-sectional diameter that 0.05～10 μ m and length are not more than 20 μ m are that rod-shpaed particle or the particle diameter that 0.05～10 μ m and length are not more than 20 μ m is the spherical particle of 0.05～10 μ m.Preferably; the thickness of described upper converting photoluminescent transparent membrane is not more than 5 μ m, and described upper converting photoluminescent crystalline particles is that cross-sectional diameter is that cylindrical particle, cross-sectional diameter that 0.05～5 μ m and length are not more than 20 μ m are that rod-shpaed particle or the particle diameter that 0.05～5 μ m and length are not more than 20 μ m is the spherical particle of 0.05～5 μ m.
Further, described upper converting photoluminescent crystalline particles is Er
3+-Yb
3+mix altogether fluoride, Tm
3+-Yb
3+mix altogether fluoride or Tm
3+-Er
3+-Yb
3+mix altogether fluoride, described fluoride is ReF
3, AReF
4or RF
2, wherein, Re is rare earth element, and A is alkali metal, and R is alkali earth metal.Described fluoride is preferably NaYF
4, LiYF
4, NaGdF
4, NaLaF
4, GdF
3, LaF
3, YF
3, CaF
2, SrF
2or BaF
2.
Meanwhile, the present invention also provides the preparation method of upper converting photoluminescent glass described in more than one, it is characterized in that: the method comprises the steps:
S10: prepare silicon oxide series masking liquid;
S20: ultrasonic upper converting photoluminescent crystalline particles being dispersed in described silicon oxide series masking liquid formed to luminescence generated by light masking liquid, and in described luminescence generated by light masking liquid, the concentration of upper converting photoluminescent crystalline particles is 1～15g/L;
S30: described luminescence generated by light masking liquid is coated at least one surface of glass substrate;
S40: by the described glass substrate that applies luminescence generated by light masking liquid, dry at 50～100 DEG C after 10～30 minutes, then dry 60～100 minutes at 150～200 DEG C of temperature, obtain converting photoluminescent glass after being finally cooled to room temperature.
Further, described silicon oxide series masking liquid is silicon dioxide gel, the preparation method of described silicon dioxide gel is: taking silicon oxide series matrix material as raw material, absolute ethyl alcohol, ethyl acetate, toluene, dimethylbenzene, isopropyl alcohol, propyl alcohol, n-butanol, ethylene glycol, or at least one in EGME is solvent, water is reactant, nitric acid, hydrochloric acid, acetic acid, lactic acid, maleic acid, one in malonic acid or oxalic acid is catalyst, and add wherein silane coupler, the mixture that at room temperature stirs above-mentioned raw materials makes, between raw material and solvent, hydrolysis occurs for 12～24 hours and obtains silicon dioxide gel.
Alternatively, described silicon oxide series matrix material is the water-disintegrable silicon compound of four functionalities, the molfraction of described silicon oxide series matrix material is 1 part, the molfraction of described water is 1～10 part, the molfraction of described silane coupler is 0.5～10 part, and amount of substance when the first proton dissociates completely in described catalyst is 0.01～5mol/L with respect to the concentration of the volume of described silicon oxide series matrix material.
Preferably, the time of the ultrasonic dispersion described in step S20 is more than 5 minutes.
Preferably, be applied to spin coating method, dip-coating method, spraying process, rolling method, meniscus rubbing method or the mould described in step S30 is coated with method.
Preferably, between step S10 and step S20, also comprise step S15: at least one in employing silica, polyvinylpyrrolidone or polyglutamic acid carried out finishing to described upper converting photoluminescent crystalline particles.
Preferably, between step S20 and step S30, also comprise step S25: glass baseplate surface is carried out to polishing.
The present invention is owing to having taked technique scheme, and it has following beneficial effect:
1) luminescence generated by light glass of the present invention is simple in structure, and visible light transmissivity is high, and low production cost is applicable to producing in enormous quantities.
2) the present invention is medium with silicon oxide series masking liquid, by sol-gel process, upper converting photoluminescent crystalline particles is attached to glass surface equably, and without luminescence generated by light particle being infiltrated to inside glass under melt temperature, avoided the adverse effect to glass machinery performance causing because glass surface being re-started to high-temperature heat treatment.
3) luminescence generated by light crystalline particles of the present invention is prior by solid phase method or the synthetic crystalline particles of liquid phase method, and active ions are fixed on intracell, do not participate in SiO
2the gelation reaction process of based sols, the hydroxyl in solution can not enter granule interior, also not can with lattice in active ions generation bonding, therefore without film is carried out to high-temperature heat treatment.
Brief description of the drawings:
Fig. 1 is the structural representation of upper converting photoluminescent glass of the present invention;
Fig. 2 is the SEM image of upper converting photoluminescent transparent membrane of the present invention;
Fig. 3 is the local enlarged diagram of Fig. 2;
Attached number in the figure explanation: 1 is upper converting photoluminescent transparent membrane, and 11 is upper converting photoluminescent crystalline particles, the 12 partly or completely cured products that are silicon dioxide gel, 2 is glass substrate.
Detailed description of the invention:
Below in conjunction with accompanying drawing, content of the present invention is described further.
As shown in Figures 1 to 3, converting photoluminescent glass in one of the present invention, comprise glass substrate 2 and at least one the lip-deep upper converting photoluminescent transparent membrane 1 that is arranged on glass substrate 2, it is characterized in that: described upper converting photoluminescent transparent membrane 1 is mainly made up of partly or completely cured product 12 and the upper converting photoluminescent crystalline particles 11 of silicon dioxide gel, and described upper converting photoluminescent crystalline particles 11 is dispersed in the partly or completely cured product 12 of described silicon dioxide gel.
Further, the density that described upper converting photoluminescent crystalline particles 11 is disperseed on the face of upper converting photoluminescent transparent membrane 1 is 0.05～2g/m
2.Select suitable point bulk density, both can ensure the illumination effect of luminescence generated by light glass, can also ensure the visible light transmissivity of luminescence generated by light glass.
Further; the thickness of described upper converting photoluminescent transparent membrane 1 is not more than 10 μ m, described upper converting photoluminescent crystalline particles 11 for cross-sectional diameter be that cylindrical particle, cross-sectional diameter that 0.05～10 μ m and length are not more than 20 μ m are that rod-shpaed particle or the particle diameter that 0.05～10 μ m and length are not more than 20 μ m is the spherical particle of 0.05～10 μ m.Preferably; the thickness of described upper converting photoluminescent transparent membrane 1 is not more than 5 μ m, described upper converting photoluminescent crystalline particles 11 for cross-sectional diameter be that cylindrical particle, cross-sectional diameter that 0.05～5 μ m and length are not more than 20 μ m are that rod-shpaed particle or the particle diameter that 0.05～5 μ m and length are not more than 20 μ m is the spherical particle of 0.05～5 μ m.
If upper converting photoluminescent crystalline particles 11 is oversize, on upper converting photoluminescent transparent membrane 1, there will be numb spot defect, even also can seriously reduce the visible light transmissivity of upper converting photoluminescent transparent membrane.Selecting the thickness of suitable upper converting photoluminescent transparent membrane, is in order to make upper converting photoluminescent transparent membrane be not easy to occur cracking on the one hand; That thickness in order to make described upper converting photoluminescent transparent membrane is consistent with cross-sectional diameter or the particle diameter of described upper converting photoluminescent crystalline particles on the other hand, or the thickness that makes described upper converting photoluminescent transparent membrane is a bit larger tham cross-sectional diameter or the particle diameter of described upper converting photoluminescent crystalline particles, can effectively upper converting photoluminescent crystalline particles be coated therein like this.
Preferably, described upper converting photoluminescent crystalline particles 11 is Er
3+-Yb
3+mix altogether fluoride, Tm
3+-Yb
3+mix altogether fluoride or Tm
3+-Er
3+-Yb
3+mix altogether fluoride, described fluoride is ReF
3, AReF
4or RF
2, wherein, Re is rare earth element, and A is alkali metal, and R is alkali earth metal.Described fluoride is preferably NaYF
4, LiYF
4, NaGdF
4, NaLaF
4, GdF
3, LaF
3, YF
3, CaF
2, SrF
2or BaF
2.Er
3+-Yb
3+, Tm
3+-Yb
3+, Tm
3+-Er
3+-Yb
3+these three kinds of ion populations are common up-conversion luminescence active ions combinations, have higher upper converting photoluminescent efficiency.For up-conversion luminescent material, its photoluminescence efficiency is affected by matrix phonon energy: matrix phonon energy is less, and upper converting photoluminescent efficiency is higher.And ReF of the present invention
3, AReF
4and RF
2these three serial fluorides all have less phonon energy, are applicable to being used as converting photoluminescent matrix of materials.
Described upper converting photoluminescent crystalline particles 11 can adopt solid phase method or liquid phase method to synthesize.Described liquid phase method is to adopt at least one in oleic acid, stearic acid, odium stearate, citric acid, natrium citricum, ethylenediamine tetra-acetic acid, polyethylene glycol, acrylic resin, polymine assist liquid phase to synthesize.The auxiliary synthetic object of liquid phase has two aspects: the crystalline particles pattern 1) being synthesized is controlled; 2) the crystalline particles surface being synthesized is coated by adjuvant, can improve the dispersiveness of crystalline particles in solvent, and for it is done and further does finishing processing and facilitate.
The present invention also provides a kind of preparation method of upper converting photoluminescent glass, it is characterized in that: the method comprises the steps:
S10: prepare silicon oxide series masking liquid, described silicon oxide series masking liquid is preferably silicon dioxide gel.
S20: ultrasonic upper converting photoluminescent crystalline particles being dispersed in described silicon oxide series masking liquid formed to luminescence generated by light masking liquid, and in described luminescence generated by light masking liquid, the concentration of upper converting photoluminescent crystalline particles is 1～15g/L; The time of described ultrasonic dispersion is preferably more than 5 minutes, and converting photoluminescent uniform particles is dispersed in described silicon oxide series masking liquid.
S30: described luminescence generated by light masking liquid is coated at least one surface of glass substrate, glass baseplate surface is preferably through polishing, and optional painting method is: spin coating method, dip-coating method, spraying process, rolling method, meniscus rubbing method or mould are coated with method.
S40: by the described glass substrate that applies luminescence generated by light masking liquid, at 50～100 DEG C, dry after 10～30 minutes, make the solvent evaporates in described luminescence generated by light masking liquid, then at 150～200 DEG C, dry 60～100 minutes, converting photoluminescent transparent membrane 1 and glass substrate 2 are combined closely, obtain converting photoluminescent glass after being finally cooled to room temperature.
Further, described silicon dioxide gel preparation method is: taking silicon oxide series matrix material as raw material, at least one in absolute ethyl alcohol, ethyl acetate, toluene, dimethylbenzene, isopropyl alcohol, propyl alcohol, n-butanol, ethylene glycol or EGME is solvent, water is reactant, one in nitric acid, hydrochloric acid, acetic acid, lactic acid, maleic acid, malonic acid or oxalic acid is catalyst, and adds wherein silane coupler.Wherein, described silicon oxide series matrix material is preferably the water-disintegrable silicon compound of four functionalities, the molfraction of described silicon oxide series matrix material is 1 part, the molfraction of described water is 1～10 part, the molfraction of described silane coupler is 0.5～10 part, and amount of substance when the first proton dissociates completely in described catalyst is 0.01～5mol/L with respect to the concentration of the volume of described silicon oxide series matrix material.The mixture that at room temperature stirs above-mentioned raw materials makes, between raw material and solvent, hydrolysis occurs for 12～24 hours and obtains silicon dioxide gel.
Preferably, before ultrasonic dispersion, preferentially adopt at least one in silica, polyvinylpyrrolidone or polyglutamic acid to carry out finishing to described upper converting photoluminescent crystalline particles.Adopt these materials to carry out finishing processing to crystalline particles and can further improve the dispersed degree of crystalline particles in silicon oxide series masking liquid.
Below in conjunction with specific embodiment, the present invention is carried out to more detailed elaboration.
Embodiment 1
Taking ethyl orthosilicate as raw material, isopropyl alcohol, propylene glycol monomethyl ether and water are solvent, and nitric acid is catalyst, and add wherein silane coupler, and stirring makes, between raw material and solvent, hydrolysis occurs and prepares silicon dioxide gel; Get the NaYF that 2mg adopts the synthetic preparation of the auxiliary liquid phase of polyethylene glycol
4: Er
3+, Yb
3+fluorescent material, the ultrasonic luminescence generated by light masking liquid that is dispersed in described in 2ml in silicon dioxide gel to obtain.
Getting a thickness is 2.1mm, and the green glass that length and width are respectively 160mm × 100mm, does polishing by its surface; With glass bar by whole luminescence generated by light masking liquid blade coatings the green glass surface after polishing, and at 60 DEG C, dry after 30 minutes and at 160 DEG C, dry 70 minutes again, be cooled to room temperature and obtain converting photoluminescent glass.The fine and close evenly flawless of film making.This glass is can emitting bright green light under 980nm, the power laser beam irradiation that is 1.5W at wavelength.This glass is 80.88% in the transmitance of visible region.
Embodiment 2
Taking ethyl orthosilicate as raw material, isopropyl alcohol, propylene glycol monomethyl ether and water are solvent, and nitric acid is catalyst, and add wherein silane coupler, and stirring makes, between raw material and solvent, hydrolysis occurs and prepares silicon dioxide gel; Get the NaYF that 4mg adopts silicon dioxide modified mistake
4: Er
3+, Yb
3+fluorescent material, ultrasonic being dispersed in must luminescence generated by light masking liquid in the above-mentioned silicon dioxide gel of 2ml.
Getting a thickness is 2.1mm, and the green glass that length and width are respectively 160mm × 100mm, does polishing by its surface; With glass bar by whole luminescence generated by light masking liquid blade coatings the green glass surface after polishing, at 60 DEG C, dry after 30 minutes and at 150 DEG C, dry 60 minutes again, be cooled to room temperature and obtain converting photoluminescent glass.The fine and close evenly flawless of film making.This glass is can emitting bright green light under 980nm, the power laser beam irradiation that is 1.5W at wavelength.This glass is 80.88% in the transmitance of visible region.
Embodiment 3
Taking ethyl orthosilicate as raw material, isopropyl alcohol, propylene glycol monomethyl ether and water are solvent, and nitric acid is catalyst, and add wherein silane coupler, and stirring makes, between raw material and solvent, hydrolysis occurs and prepares silicon dioxide gel; Get the LaF that 3mg adopts the auxiliary liquid phase synthesizing method of natrium citricum to prepare
3: Er
3+, Yb
3+fluorescent material, the ultrasonic luminescence generated by light masking liquid that is dispersed in described in 2ml in silicon dioxide gel to obtain.
Getting a thickness is 2.1mm, and the green glass that length and width are respectively 160mm × 100mm, does polishing by its surface; With glass bar by whole luminescence generated by light masking liquid blade coatings the green glass surface after polishing, at 60 DEG C, dry after 30 minutes and at 180 DEG C, dry 80 minutes again, be cooled to room temperature and obtain converting photoluminescent glass.The fine and close evenly flawless of film making.This glass is can emitting bright red light under 980nm, the power laser beam irradiation that is 1.5W at wavelength.This glass is 81.06% in the transmitance of visible region.
Above content specifically describes converting photoluminescent glass and preparation method thereof in one of the present invention; but the present invention is not subject to the limitation of detailed description of the invention content described above; so any improvement, equivalent modifications and replacement etc. that all foundations technical essential of the present invention is carried out, all belong to the scope of protection of the invention.
Claims (13)
1. a upper converting photoluminescent glass, comprise glass substrate and at least one the lip-deep upper converting photoluminescent transparent membrane that is arranged on glass substrate, it is characterized in that: described upper converting photoluminescent transparent membrane is mainly made up of partly or completely cured product and the upper converting photoluminescent crystalline particles of silicon dioxide gel, and described upper converting photoluminescent crystalline particles is dispersed in the partly or completely cured product of described silicon dioxide gel.
2. upper converting photoluminescent glass according to claim 1, is characterized in that: the density of disperseing on the face of described upper converting photoluminescent crystalline particles converting photoluminescent transparent membrane on described is 0.05～2g/m
2.
3. upper converting photoluminescent glass according to claim 1; it is characterized in that: the thickness of described upper converting photoluminescent transparent membrane is not more than 10 μ m, described upper converting photoluminescent crystalline particles is that cross-sectional diameter is that cylindrical particle, cross-sectional diameter that 0.05～10 μ m and length are not more than 20 μ m are that rod-shpaed particle or the particle diameter that 0.05～10 μ m and length are not more than 20 μ m is the spherical particle of 0.05～10 μ m.
4. upper converting photoluminescent glass according to claim 1; it is characterized in that: the thickness of described upper converting photoluminescent transparent membrane is not more than 5 μ m, described upper converting photoluminescent crystalline particles is that cross-sectional diameter is that cylindrical particle, cross-sectional diameter that 0.05～5 μ m and length are not more than 20 μ m are that rod-shpaed particle or the particle diameter that 0.05～5 μ m and length are not more than 20 μ m is the spherical particle of 0.05～5 μ m.
5. upper converting photoluminescent glass according to claim 1, is characterized in that: described upper converting photoluminescent crystalline particles is Er
3+-Yb
3+mix altogether fluoride, Tm
3+-Yb
3+mix altogether fluoride or Tm
3+-Er
3+-Yb
3+mix altogether fluoride, described fluoride is ReF
3, AReF
4or RF
2, wherein, Re is rare earth element, and A is alkali metal, and R is alkali earth metal.
6. upper converting photoluminescent glass according to claim 5, is characterized in that: described fluoride is NaYF
4, LiYF
4, NaGdF
4, NaLaF
4, GdF
3, LaF
3, YF
3, CaF
2, SrF
2or BaF
2.
7. a preparation method for the arbitrary described upper converting photoluminescent glass of claim 1～6, is characterized in that: the method comprises the steps:
S10: prepare silicon oxide series masking liquid;
S20: ultrasonic upper converting photoluminescent crystalline particles being dispersed in described silicon oxide series masking liquid formed to luminescence generated by light masking liquid, and in described luminescence generated by light masking liquid, the concentration of upper converting photoluminescent crystalline particles is 1～15g/L;
S30: described luminescence generated by light masking liquid is coated at least one surface of glass substrate;
S40: by the described glass substrate that applies luminescence generated by light masking liquid, dry at 50～100 DEG C after 10～30 minutes, then dry at 150～200 DEG C 60～100 minutes, obtain converting photoluminescent glass after being finally cooled to room temperature.
8. the preparation method of upper converting photoluminescent glass according to claim 7, it is characterized in that: described silicon oxide series masking liquid is silicon dioxide gel, the preparation method of described silicon dioxide gel is: taking silicon oxide series matrix material as raw material, absolute ethyl alcohol, ethyl acetate, toluene, dimethylbenzene, isopropyl alcohol, propyl alcohol, n-butanol, ethylene glycol, or at least one in EGME is solvent, water is reactant, nitric acid, hydrochloric acid, acetic acid, lactic acid, maleic acid, one in malonic acid or oxalic acid is catalyst, and add wherein silane coupler, the mixture that at room temperature stirs above-mentioned raw materials makes, between raw material and solvent, hydrolysis occurs for 12～24 hours and obtains silicon dioxide gel.
9. the preparation method of upper converting photoluminescent glass according to claim 8, it is characterized in that: described silicon oxide series matrix material is the water-disintegrable silicon compound of four functionalities, the molfraction of described silicon oxide series matrix material is 1 part, the molfraction of described water is 1～10 part, the molfraction of described silane coupler is 0.5～10 part, and amount of substance when the first proton dissociates completely in described catalyst is 0.01～5mol/L with respect to the concentration of the volume of described silicon oxide series matrix material.
10. the preparation method of upper converting photoluminescent glass according to claim 7, is characterized in that: the time of the ultrasonic dispersion described in step S20 is more than 5 minutes.
The preparation method of 11. upper converting photoluminescent glass according to claim 7, is characterized in that: be applied to spin coating method, dip-coating method, spraying process, rolling method, meniscus rubbing method or mould described in step S30 are coated with method.
The preparation method of 12. upper converting photoluminescent glass according to claim 7, is characterized in that: between step S10 and step S20, also comprise step S15: at least one in employing silica, polyvinylpyrrolidone or polyglutamic acid carried out finishing to described upper converting photoluminescent crystalline particles.
The preparation method of 13. upper converting photoluminescent glass according to claim 7, is characterized in that: between step S20 and step S30, also comprise step S25: glass baseplate surface is carried out to polishing.
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| CN105883827A (en) * | 2016-04-20 | 2016-08-24 | 苏州吉人高新材料股份有限公司 | Silica sol having fluorescence properties and preparation method thereof |
| CN107418580A (en) * | 2017-07-31 | 2017-12-01 | 南京工业大学 | A kind of preparation method for improving up-conversion luminescence film |
| CN112652942A (en) * | 2020-12-21 | 2021-04-13 | 中国科学院上海光学精密机械研究所 | Laser amplifier based on wavelength-adjustable partition plate glass |
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| CN101003729A (en) * | 2007-01-04 | 2007-07-25 | 吉林大学 | Nano incandescnet particles of composite organic dyestuff of silicon dioxide with dual structures, and preparation method |
| CN101775290A (en) * | 2010-02-10 | 2010-07-14 | 西北大学 | Preparation method of visible light absorption type upper conversion luminescent material |
| CN102064209A (en) * | 2010-09-21 | 2011-05-18 | 南京工业大学 | Light conversion enhanced photocatalysis composite material and preparation method thereof |
| CN103183479A (en) * | 2013-04-16 | 2013-07-03 | 浙江大学 | Preparation method of anti-reflection thin film with photo-transformation function |
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| CN107418580A (en) * | 2017-07-31 | 2017-12-01 | 南京工业大学 | A kind of preparation method for improving up-conversion luminescence film |
| CN112652942A (en) * | 2020-12-21 | 2021-04-13 | 中国科学院上海光学精密机械研究所 | Laser amplifier based on wavelength-adjustable partition plate glass |
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