CN105038773A - High-luminescence-property silicon nanometer particle fluorescent powder and light-emitting film and preparing method thereof - Google Patents
High-luminescence-property silicon nanometer particle fluorescent powder and light-emitting film and preparing method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of solid-state light emitting and high molecular materials and particularly provides high-luminescence-property silicon nanometer particle fluorescent powder and a high-luminescence-property silicon nanometer particle light-emitting film and a preparing method thereof. Silicon nanometer particles and a water solution of silicate type water-borne bentonite are mixed so that the silicon nanometer particles can be attached to the surface of a lamellar structure of the bentonite and dispersed on the surface stably; after the silicon nanometer particles are dried, the fluorescent powder maintaining a high luminescence property of the original silicon nanometer particles is obtained; if a mixed solution of the silicon nanometer particles and the water-borne bentonite is mixed with a macro-molecular solution, the mixture is dried to obtain the light-emitting film of the silicon nanometer particles, and therefore the silicon nanometer particles have a wider actual application prospect in the field of solid-state light emitting. The preparing method is easy to operate, environmentally friendly, mild, efficient and low in cost, and saves energy; the prepared fluorescent powder and the light-emitting film have good light-emitting properties and high fluorescence stability, and have wider application prospects in the solid-state light emitting field of daily lighting sources, especially white light emitting diodes and the like.
Description
Technical field
The invention belongs to solid luminescent and technical field of polymer materials, be specifically related to a kind of silicon nano fluorescent material and luminescent film and preparation method thereof.
Background technology
Compared to other nanoparticles, silicon nano has unique advantage such as little in rich reserves, with low cost and toxicity, so in recent years, silicon nano all receives in multiple field and pays close attention to widely.In addition, silicon materials also have good biocompatibility, and can realize good combination with silicon semiconductor industry.These potential advantages, add the research that people are increasingly extensive to silicon nano, and all making it progressively substitute classical II-VI group heavy metal nanoparticle becomes possibility.And silicon nano is how to be stabilized in solid state substrate by silicon nano in the problem that the application aspect of solid state light emitters primarily solves.But, directly by the solvent evaporation in silicon nano colloidal solution to prepare the method for silicon nano fluorescent material and inadvisable, because in this drying process, silicon nano can occur assemble and produce aggregation inducing fluorescent quenching effect (AIQ, Aggregation-inducedquenchingeffect).Therefore, we need to find a kind of suitable solid substrate that silicon nano can be made wherein not assemble, thus silicon nano is prepared into fluorescent material or luminescent film, finally realize its solid luminescent.
Summary of the invention
The object of this invention is to provide a kind of the silicon nano fluorescent material and luminescent film and preparation method thereof with the excellent optical property such as the high and stable luminescent property of luminous efficiency.
The preparation method of silicon nano fluorescent material provided by the invention and luminescent film, concrete steps are as follows:
(1) hydrogen reduction of silicon tetrachloride prepares silicon nano: using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, glycol dimethyl ether is medium, with the organism (as carbazole etc.) containing the element such as nitrogen or oxygen for silicon nano coating materials or end-capping reagent, reaction 2-24h, through centrifugal, revolves steaming, add water redispersion, obtains the silicon nano colloidal solution that solid content is 0.5-15%;
(2) (be generally about 25 DEG C) under room temperature, add in deionized water by silicate-type water-based wilkinite lithium magnesium silicate, pre-mixing is mixed with the suspension that solid content is 0.1-20%, rapid stirring, makes its abundant swelling dispersion; As required, for different silicon nanoparticles, to this bentonite solution salt acid for adjusting pH to neutral or even acid;
(3) above-mentioned bentonite solution is mixed with the ratio of volume ratio 1:1000-1:100 with silicon nano colloidal solution, and fully stir;
(4) step (3) gained mixed solution is placed in 70-80 DEG C of dry more than the 24h of (preferably 75 DEG C) baking oven (being generally 24-48h), treats that moisture volatilizees completely, namely obtain the fluorescent material that luminescent properties is good;
Or, step (3) gained mixed solution fully mixed with film-forming properties macromolecular solution and water film, being placed in room temperature dehumidifier environment dry, namely obtaining the luminescent film that luminescent properties is good.
In the present invention, the silicon nano of employing is luminophore.
In the present invention, as the organism containing nitrogen or oxygen element of silicon nano coating materials or end-capping reagent, select but be not limited to carbazole, 1,2,3,4-tetrahydro carbazole, pentanoic, n-Octanol etc.
In the present invention, silicate-type water-based wilkinite used is solid substrate, but is not limited to lithium magnesium silicate, as the wilkinites such as zeopan also can.
In the present invention, film-forming properties macromolecular material used can be, but not limited to polyvinyl alcohol (PVA), but also can be other arbitrary film-forming properties polymers.
In the present invention, silicate-type water-based wilkinite is used to stable silicon nanoparticle and prevents it from the key substance of fluorescent quenching occurring.
The present invention, by silicon nano and the bentonitic aqueous solution of silicate-type water-based, enables silicon nano attach to bentonitic laminated structure surface and stable dispersion thereon; After drying, the bentonitic laminated structure of silicate-type water-based has successfully intercepted the gathering of silicon nano in vertical structure on each lamella, thus can obtain the fluorescent material maintaining original silicon nano high luminescence energy.Silicon nano is positively charged by its surface exhibits after finishing, and in bentonite solution, clay layer needs to realize electric neutrality by absorption sodium ion, namely clay layer surface is electronegative, so can be combined by electrostatic interaction between silicon nano and clay layer structure.Preparation method of the present invention is simple to operate, green gentle, and efficient energy-saving is with low cost.In addition, if by silicon nano and the bentonitic mixing solutions of water-based blended with macromolecular solution again, the luminescent film of silicon nano can also be obtained after drying, make silicon nano be provided with more wide actual application prospect in solid luminescent field.
The present invention has following advantage:
(1) silicon nano that the present invention adopts has excellent luminous efficiency, and water-based wilkinite used is material common on the market, cheap; And the preparation method of this fluorescent material and film, simply efficiently, environmental protection, with low cost, may be used for scale operation.
(2) the silicon nano fluorescent material prepared of the present invention and luminescent film have the optical property close with liquid-state silicon nanoparticle, namely have excellent fluorescence property and optical stability, can be used for various Sony ericsson mobile comm ab.
Accompanying drawing explanation
Fig. 1 is obtained yellow silicon nano fluorescent material picture in the sunlight.
Fig. 2 is the obtained yellow silicon nano fluorescent material picture of (wavelength is 365nm) under ultra violet lamp.
Fig. 3 is obtained silicon nano-PVA light-emitting film picture in the sunlight.
Fig. 4 is the obtained silicon nano-PVA light-emitting film picture of (wavelength is 365nm) under ultra violet lamp.
Embodiment
Following examples for illustration of the present invention, but are not used in and limit the scope of the invention, every following instance is done according to technical spirit of the present invention any simple modification, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Raw material in following examples is commercial goods.
embodiment 1
1. using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, and glycol dimethyl ether is medium, and 1,2,3,4-tetrahydro carbazole is silicon nano coating materials, reaction 10h, to get supernatant liquor after the centrifugal 10min of 8000r/min rotating speed, 50 DEG C of rotary evaporations fall solvent, add water silicon nano redispersion, fully can obtain the silicon nano colloidal solution of the excellent in optical properties of stable dispersion in water after dispersion;
2. (about 25 DEG C) under room temperature, added in 2ml deionized water by 0.5g lithium magnesium silicate water-based wilkinite and carry out pre-mixing, rapid stirring makes its abundant swelling dispersion;
3. above-mentioned bentonite solution is mixed with 10ml silicon nano colloidal solution, and fully stir;
4. gained mixed solution is placed in 75 DEG C of dry 24h of baking oven, treats that moisture volatilizees completely, the green emitting phosphor that luminescent properties is good can be obtained.
embodiment 2
1. using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, glycol dimethyl ether is medium, carbazole is silicon nano coating materials, reaction 2h, to get supernatant liquor after the centrifugal 10min of 8000r/min rotating speed, 50 DEG C of rotary evaporations fall solvent, add water silicon nano redispersion, the silicon nano colloidal solution of the excellent in optical properties of stable dispersion in water fully after dispersion, can be obtained;
2. (about 25 DEG C) under room temperature, added in 2ml deionized water by 0.5g silicate-type water-based wilkinite and carry out pre-mixing, rapid stirring makes its abundant swelling dispersion;
3. above-mentioned bentonite solution is mixed with 10ml silicon nano colloidal solution, and fully stir;
4. gained mixed solution is placed in 70 DEG C of dry 30h of baking oven, treats that moisture volatilizees completely, the blue colour fluorescent powder that luminescent properties is good can be obtained.
embodiment 3
1. using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, glycol dimethyl ether is medium, 4-methoxy diphenylamine is silicon nano coating materials, reaction 2h, to get supernatant liquor after the centrifugal 10min of 8000r/min rotating speed, 50 DEG C of rotary evaporations fall solvent, add water silicon nano redispersion, about its pH to 10 is regulated with sodium hydroxide solution after abundant dispersion, leave standstill and after some hours, have black precipitate generation, cross leaching filter residue and it is transferred in deionized water again, regulate its pH to middle slant acidity with hydrochloric acid, the silicon nano colloidal solution of the excellent in optical properties of stable dispersion in water can be obtained,
2. (about 25 DEG C) under room temperature, added in 2ml deionized water by 0.5g silicate-type water-based wilkinite and carry out pre-mixing, rapid stirring makes its abundant swelling dispersion;
3. above-mentioned bentonite solution is mixed with 10ml silicon nano colloidal solution, and fully stir;
4. gained mixed solution is placed in 75 DEG C of dry 28h of baking oven, treats that moisture volatilizees completely, the yellow fluorescent powder that luminescent properties is good can be obtained.
embodiment 4
1. using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, glycol dimethyl ether is medium, pentanoic is silicon nano coating materials, reaction 24h, to get supernatant liquor after the centrifugal 10min of 8000r/min rotating speed, 50 DEG C of rotary evaporations fall solvent, add water silicon nano redispersion, the silicon nano colloidal solution of the excellent in optical properties of stable dispersion in water fully after dispersion, can be obtained;
2. (about 25 DEG C) under room temperature, added in 2ml deionized water by 0.5g silicate-type water-based wilkinite and carry out pre-mixing, rapid stirring makes its abundant swelling dispersion;
3. above-mentioned bentonite solution is mixed with 10ml silicon nano colloidal solution, and fully stir;
4. gained mixed solution is placed in 75 DEG C of dry 30h of baking oven, treats that moisture volatilizees completely, the good green emitting phosphor of luminescent properties can be obtained.
embodiment 5
1. using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, and glycol dimethyl ether is medium, and 1,2,3,4-tetrahydro carbazole is silicon nano coating materials, reaction 20h, to get supernatant liquor after the centrifugal 10min of 8000r/min rotating speed, 50 DEG C of rotary evaporations fall solvent, add water silicon nano redispersion, fully can obtain the silicon nano colloidal solution of the excellent in optical properties of stable dispersion in water after dispersion;
2. (about 25 DEG C) under room temperature, added in 2ml deionized water by 0.5g aluminium magensium silicate water-based wilkinite and carry out pre-mixing, rapid stirring makes its abundant swelling dispersion;
3. above-mentioned bentonite solution is mixed with 10ml silicon nano colloidal solution, and fully stir;
4. gained mixed solution is placed in 80 DEG C of dry 24h of baking oven, treats that moisture volatilizees completely, the green emitting phosphor that luminescent properties is good can be obtained.
embodiment 6
1. using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, and glycol dimethyl ether is medium, and 1,2,3,4-tetrahydro carbazole is silicon nano coating materials, reaction 5h, to get supernatant liquor after the centrifugal 10min of 8000r/min rotating speed, 50 DEG C of rotary evaporations fall solvent, add water silicon nano redispersion, fully can obtain the silicon nano colloidal solution of the excellent in optical properties of stable dispersion in water after dispersion;
2. prepare the neusilin water-based bentonite solution that massfraction is 2%: take neusilin 0.2g in beaker, add 10ml deionized water and fully dissolve;
3. by above-mentioned for 0.3ml that bentonite solution mixes with 50ml silicon nano colloidal solution, and fully stir;
4. prepare polyvinyl alcohol (PVA) aqueous solution 100ml that massfraction is 4%, and mix with above-mentioned mixing solutions, fully stir;
5. gained mixed solution is carried out on the mould of 200mm × 275mm size watering film, be placed in temperature about 25 DEG C, air-dry more than 24h in the environment of humidity less than 40%;
6. treat that moisture evaporation is complete, can obtain homogeneous, the light-emitting film that luminescent properties is good and stable.
Claims (4)
1. a preparation method for high luminescence energy silicon nano fluorescent material and luminescent film, is characterized in that concrete steps are:
(1) hydrogen reduction of silicon tetrachloride prepares silicon nano: using silicon tetrachloride as silicon source, naphthalene-sodium homogeneous phase solution is as reductive agent, glycol dimethyl ether is medium, with the organism containing nitrogen or oxygen element for silicon nano coating materials or end-capping reagent, reaction 2-24h, through centrifugal, revolves steaming, add water redispersion, obtains the silicon nano colloidal solution that solid content is 0.5-15%;
(2) under room temperature, silicate-type water-based wilkinite lithium magnesium silicate is added in deionized water, is hybridly prepared into the suspension that solid content is 0.1-20%, rapid stirring, make its abundant swelling dispersion; As required, for different silicon nanoparticles, extremely neutral with salt acid for adjusting pH to this bentonite solution, or to acid;
(3) above-mentioned bentonite solution is mixed with the ratio of volume ratio 1:1000-1:100 with silicon nano colloidal solution, and fully stir;
(4) step (3) gained mixed solution is placed in 75-85 DEG C of dry more than the 24h of baking oven, treats that moisture volatilizees completely, namely obtain the fluorescent material that luminescent properties is good; Or,
Step (3) gained mixed solution fully mixed with film-forming properties macromolecular solution and waters film, being placed in room temperature dehumidifier environment dry, namely obtaining the luminescent film that luminescent properties is good.
2. the preparation method of silicon nano fluorescent material according to claim 1 and luminescent film, it is characterized in that the organism containing nitrogen or oxygen element as silicon nano coating materials or end-capping reagent, select carbazole, 1,2,3,4-tetrahydro carbazole, pentanoic or n-Octanol.
3. the preparation method of silicon nano fluorescent material according to claim 1 and luminescent film, is characterized in that silicate-type water-based wilkinite used is as solid substrate, selects lithium magnesium silicate or zeopan.
4. the high luminescence energy silicon nano fluorescent material prepared by the described preparation method of one of claim 1-3 and luminescent film.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108841195A (en) * | 2018-06-11 | 2018-11-20 | 全椒祥瑞塑胶有限公司 | A kind of fluorescent material applied in luminescent plastic |
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| CN103923638A (en) * | 2014-04-21 | 2014-07-16 | 河北工业大学 | Water-soluble high-efficiency rare-earth luminescent material and preparation method thereof |
| CN104086927A (en) * | 2014-06-27 | 2014-10-08 | 河北工业大学 | Flexible rare-earth transparent light-emitting film and preparation method thereof |
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| CN1687305A (en) * | 2005-04-18 | 2005-10-26 | 南京师范大学 | Nano rare earth optical transfer agent in bionic state, Nano rare earth optical transfer agricultural film in bionic state, and preparation method thereof |
| CN103923638A (en) * | 2014-04-21 | 2014-07-16 | 河北工业大学 | Water-soluble high-efficiency rare-earth luminescent material and preparation method thereof |
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Non-Patent Citations (1)
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| QI LI ET AL.，: ""Surface-Modified Silicon Nanoparticles with Ultrabright Photoluminescence and Single-Exponential Decay for Nanoscale Fluorescence Lifetime Imaging of Temperature"及其Supporting information", 《J. AM. CHEM. SOC.》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108841195A (en) * | 2018-06-11 | 2018-11-20 | 全椒祥瑞塑胶有限公司 | A kind of fluorescent material applied in luminescent plastic |
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Application publication date: 20151111 |