CN103865534B - A kind of preparation method of nitride fluorescent thin-film material - Google Patents
A kind of preparation method of nitride fluorescent thin-film material Download PDFInfo
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- CN103865534B CN103865534B CN201410120560.0A CN201410120560A CN103865534B CN 103865534 B CN103865534 B CN 103865534B CN 201410120560 A CN201410120560 A CN 201410120560A CN 103865534 B CN103865534 B CN 103865534B
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Abstract
The invention discloses a kind of preparation method of nitride fluorescent thin-film material.Be 2 × 10 by resistivity
-3~ 8 × 10
-3the heavily doped monocrystalline silicon piece of P type of Ω cm is cleaned and is placed in volume ratio HF:HNO
3: H
2corrode in the solution of O=1:3 ~ 5:5 ~ 10, volume percent 0.5% ~ 5% hydrofluoric acid rinse obtains spongy porous silicon film; Active metal ammino is dissolved and is formed ammino metal ion, and this ionic adsorption in porous silicon hole wall and surperficial forming reactions objects system, and loads nitrogenizing reaction stove, and normal pressure, 1000 DEG C ~ 1350 DEG C nitrogenizing reactions 5 ~ 24 hours, obtain nitride fluorescent thin-film material.The present invention guarantees the interatomic bond of metal and how empty silicon substrate, improve reactant mutual diffusion performance, accelerate solid phase synthesis speed, reduce synthesis temperature, obtain nitride fluorescent thin-film material, realize the best performance of material emission performance and the simple and feasible of finishing operations, reduce product cost and improve quality.
Description
Technical field
The present invention relates to the preparation method of fluorescence membrane material, especially relate to the preparation method of a kind of nitride fluorescent thin-film material of LED illumination light source.
Background technology
Nitride fluorescent material, because strong covalent crystal structure shows very high chemical stability and spectrum thermostability in performance, nitride fluorescent material efficiently can be excited, launch by blue light or near-ultraviolet light, warm white type spectrum is formed with blue light matched well, obtaining the colour temperature close with daylight, is the important raw and processed materials of white light LEDs.
The nitride fluorescent material applied at present is powder body material substantially, with Si (NH
2)
2, or Si
3n
4, the powders such as alkaline-earth metal or its nitride, rare earth metal and oxide compound thereof are raw material, adopt the technology such as carbothermic reduction, vapour phase reduction, multi-step reaction to prepare powder.Powder body material mixes with transparent resin adhesive usually, be coated on LED chip by gluing process, this paint-on technique not only production efficiency is low, also cause the irregular of phosphor powder layer concentration, uneven thickness even bisque shape, the ununiformity of the white light hot spot such as cause the white light of outgoing local partially yellow or partially blue, affects colourity and the brightness of LED, for improving the deficiency of gluing process, CN200710049460, CN200910030916, the patents such as CN201310079279 are by making powder and the sheet preparation method of transparent resin adhesive mixolimnion swaging in advance, fluorescent powder prefabricated film for white light LED is provided, but transparent resin is different with phosphor indices and resin thermostability is low etc., and problem cannot be avoided, have impact on optical throughput and the work-ing life of LED component, therefore along with the development of LED component is in the urgent need to high brightness, long lifetime, colour temperature, brightness uniformity is good, the novel fluorescence thin-film material of chemistry and good thermal stability.
Porous silicon is the type material in a kind of body with a large amount of pore space structure, the void density of different size and type can be obtained by controlling preparation technology parameter, voidage can change between 30% ~ 90%, specific surface area is very big, the area of hundreds of square metres can be reached in every cubic centimetre of silicon materials, it not only likely changes electron motion and causes luminescence, in the range scale of millimeter and nanometer, also likely change the mechanical property of material.High porosity porous silicon has very strong adsorptivity, is a kind of well solid support material, metal, non pinetallic nano quantum dot preparation in show potential application, porous silicon can also change the characteristics of luminescence of porous silicon by deposition of rare-earth ion.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nitride fluorescent thin-film material.
The technical solution used in the present invention is:
Porous silicon matrix selected by the present invention is that chemical corrosion prepares, and porosity is 30%-90%.Active metal forms ammino metal ion in ammonia solvent, soaked in ammino metallic solution by porous silicon, and ammino molten metal is in the coating of porous silicon surface, make adsorption of metal ions in porous silicon hole and be distributed in porous silicon surface, the volatilization of ammonia solvent obtains solid state reaction objects system, under normal pressure nitrogen atmosphere, 1000 DEG C ~ 1350 DEG C, nitrogenize insulation prepares nitride fluorescent film in 5 ~ 24 hours, because preparation temperature is in below the fusing point of Pure Silicon Metal, to guarantee that the fluorescence membrane pattern of thing keeps porous silicon pattern and size.Active metal selected by the present invention is-Ш main group metal and rare earth metal, and main group metal is one in Li, K, Na, Mg, Ca, Sr, Ba, B, Al, Ga or two kinds, the one in preferred Ca, Ba, Sr or two kinds; Rare earth metal selected by the present invention is the one in Y, La, Ce, Sm, Eu, Yb, preferred Eu.The concrete steps of the method are as follows:
Step 1) porous silicon film is formed:
Resistivity is adopted to be 2 × 10
-3~ 8 × 10
-3the heavily doped monocrystalline silicon piece of P type of Ω cm, use acetone ultrasonic cleaning 10 ~ 20min at normal temperatures, remove its surperficial organic pollutant, use dehydrated alcohol ultrasonic cleaning 10 ~ 20min at normal temperatures, remove surface residual acetone, deionized water rinsing 2 ~ 10min, removing residual ethanol, is the hydrofluoric acid rinse 1 ~ 10min of 0.5% ~ 5% by volume percent, removes silicon chip surface zone of oxidation, deionized water rinsing 1 ~ 10min removes surface residual fluorion, and nitrogen dries up for subsequent use;
Clean silicon chip is placed in volume ratio HF:HNO
3: H
2in the solution of O=1:3 ~ 5:5 ~ 10, under normal temperature after oxide treatment 5-30min, take out silicon chip deionized water to soak, clean, be 0.5% ~ 5% hydrofluoric acid rinse 1 ~ 10min with volume percent, then use deionized water rinsing 1 ~ 10min to rinse, remove the liquid in duct, high pure nitrogen dries up, and obtains spongy porous silicon film, for subsequent use under being placed in ammonia atmosphere;
Step 2) dissolving of active metal ammino:
According to the mole ratio of each component of nitride fluorescent film, under normal temperature, in reducing atmosphere proterctive equipment, by active metal, i.e.-Ш main group metal and rare earth metal, is placed in clean container, injects dry liquefied ammonia solvent, stirring makes dissolving metal, forms ammino metallic solution, stand-by;
The acquisition of step 3) nitride fluorescent film reaction system:
Above-mentioned steps 1 is got by the component molar number ratio of nitride fluorescent film) porous silicon film, be placed in above-mentioned steps 2) ammino metallic solution soak, the ammino metal ion in solution is made to enter in spongy porous silica body, being combined with Siliciumatom dangling bonds is adsorbed in porous silicon hole, residue ammino metallic solution is successively coated on porous silicon surface, along with ammonia solvent volatilization, ammino metal is distributed in porous silicon hole and surface, obtains reactant system;
Step 4) is by above-mentioned steps 3) reactant system that obtains loads in the nitrogenizing reaction stove of nitrogen purging, and through-flow speed is the high-purity N of 20 ~ 200ml/min
2, keep stove internal gas pressure to be normal pressure, be warmed up to 1000 ~ 1350 DEG C, be incubated 5 ~ 24 hours, obtain nitride fluorescent film; Cut off subsequently and add thermoelectricity, continue to fill nitrogen and make to keep 0.1Mpa pressure in stove, furnace cooling, to normal temperature, stops filling nitrogen, takes out nitride fluorescent film.
Described nitrogenizing reaction stove is reductibility heating installation.
The nitrogen of described nitrogenizing reaction stove is the high-purity N of 99.99%
2; Described ammonia solvent is purity 99.99%, and through the drying treatment liquefied ammonia that dewaters, described active metal is analytical reagent.
The beneficial effect that the present invention has is:
The present invention utilizes porous silicon film specific surface area large, porosity and thicknesses of layers controllability good, pore surface atom is with certain active easily adsorbing metal ions, and active metal forms the characteristic of ammino metal ion in liquefied ammonia, by liquid phase wet chemistry method adsorbing metal or ammino metal ion on porous silicon rete, guarantee the interatomic bond of metal and rete matrix, improve precursor species mutual diffusion performance, accelerate solid phase synthesis speed, reduce synthesis temperature, time, obtain nitride fluorescent thin-film material, realize the best performance of its luminescent properties and the simple and feasible of finishing operations, improve the quality of products while reducing product cost.
Accompanying drawing explanation
Fig. 1 is nitride fluorescent thin-film material XRD figure.
Fig. 2 is nitride fluorescent thin-film material PL spectrogram.
Embodiment
Embodiment 1
1) porous silicon film is formed:
Resistivity is adopted to be 2 × 10
-3the heavily doped silicon single crystal of Ω cm, φ 5 × 0.03cm P type.Use acetone ultrasonic cleaning 10min at normal temperatures, remove its surperficial organic pollutant, use dehydrated alcohol ultrasonic cleaning 10min at normal temperatures, remove surface residual acetone, deionized water rinsing 2min, removes residual ethanol, and 0.5% hydrofluoric acid rinse 1min removes silicon chip surface zone of oxidation, deionized water rinsing 10min removes surface residual fluorion, and nitrogen dries up for subsequent use;
Clean silicon chip is placed in HF:HNO
3: H
2in the solution of O=1:3:5 (volume ratio), under normal temperature after oxide treatment 30min, take out silicon chip deionized water to soak, cleaning, is 0.5% hydrofluoric acid rinse 1min with volume fraction, rinse with deionized water rinsing 10min again, remove the liquid in duct, high pure nitrogen dries up, and obtains spongy porous silicon film, weigh to obtain porous silicon 0.24g, for subsequent use under being placed in ammonia atmosphere;
2) active metal ammino is dissolved:
According to the mole ratio of each component of nitride fluorescent film, under normal temperature, in reducing atmosphere proterctive equipment, by 0.136 g calcium metal and 0.025 g rare-earth europium, be placed in clean container, inject the dry liquefied ammonia of 100ml, stirring makes dissolving metal, forms ammino metallic solution, stand-by;
3) acquisition of nitride fluorescent film reaction system:
The spongy porous silicon film obtained in step 1) is placed in above-mentioned steps 2) ammino metallic solution soak, the ammino metal ion in solution is made to enter in spongy porous silica body, being combined with Siliciumatom dangling bonds is adsorbed in porous silicon hole, remaining ammino metallic solution is successively coated on porous silicon surface, along with ammonia solvent volatilization, ammino metal is distributed in porous silicon hole and surface, obtains reactant system;
4) by above-mentioned steps 3) reactant system that obtains loads in the nitrogenizing reaction stove of nitrogen purging, and through-flow speed is the high-purity N of 100ml/min
2, keep stove internal gas pressure to be normal pressure, be warmed up to 1000 DEG C, insulation nitrogenizing reaction 5 hours, obtains nitride fluorescent film; Cut-out adds thermoelectricity, and continue to fill nitrogen and make to keep 0.1Mpa pressure in stove, furnace cooling, to normal temperature, stops filling nitrogen, takes out nitride fluorescent film, carries out crystal formation and luminescent properties mensuration, and as shown in Figure 1, luminescent properties measures as shown in Figure 2 crystal formation measurement result.
Embodiment 2
1) porous silicon film is formed:
Resistivity is adopted to be 5 × 10
-3the heavily doped monocrystalline silicon piece of Ω cm, φ 5 × 0.03cm P type.Use acetone ultrasonic cleaning 15min at normal temperatures, remove its surperficial organic pollutant, use dehydrated alcohol ultrasonic cleaning 15min at normal temperatures, remove surface residual acetone, deionized water rinsing 6min, removes residual ethanol, is that 2% hydrofluoric acid rinse 5min removes silicon chip surface zone of oxidation with volume fraction, deionized water rinsing 6min removes surface residual fluorion, and nitrogen dries up for subsequent use;
Clean silicon chip is placed in HF:HNO
3: H
2in the solution of O=1:4:8 (volume ratio), under normal temperature after oxide treatment 20min, take out silicon chip deionized water to soak, cleaning, is 2% hydrofluoric acid rinse 5min with volume fraction, rinse with deionized water rinsing 5min again, remove the liquid in duct, high pure nitrogen dries up, and obtains spongy porous silicon film, weigh to obtain porous silicon 0.92 g, for subsequent use under being placed in ammonia atmosphere;
2) active metal ammino is dissolved:
According to the mole ratio of each component of nitride fluorescent film, under normal temperature, in reducing atmosphere proterctive equipment, by 1.26g Preparation of Metallic Strontium and 0.20g rare-earth europium, be placed in clean container, inject the dry liquefied ammonia of 300ml, stirring makes dissolving metal, forms ammino metallic solution, stand-by;
3) acquisition of nitride fluorescent film reaction system:
The spongy porous silicon film obtained in step 1) is placed in above-mentioned steps 2) ammino metallic solution soak, the ammino metal ion in solution is made to enter in spongy porous silica body, being combined with Siliciumatom dangling bonds is adsorbed in porous silicon hole, remaining ammino metallic solution is successively coated on porous silicon surface, along with ammonia solvent volatilization, ammino metal is distributed in porous silicon hole and surface, obtains reactant system;
4) by above-mentioned steps 3) reactant system that obtains loads in the nitrogenizing reaction stove of nitrogen purging, and through-flow speed is the high-purity N of 100ml/min
2, keep stove internal gas pressure to be normal pressure, be warmed up to 1200 DEG C, insulation nitrogenizing reaction 15 hours, obtains nitride fluorescent film; Cut-out adds thermoelectricity, and continue to fill nitrogen and make to keep 0.1Mpa pressure in stove, furnace cooling, to normal temperature, stops filling nitrogen, takes out nitride fluorescent film.
Embodiment 3
1) porous silicon film is formed:
Resistivity is adopted to be 8 × 10
-3the heavily doped monocrystalline silicon piece of Ω cm, φ 5 × 0.03cm P type.Use acetone ultrasonic cleaning 20min at normal temperatures, remove its surperficial organic pollutant, use dehydrated alcohol ultrasonic cleaning 20min at normal temperatures, remove surface residual acetone, deionized water rinsing 10min, removes residual ethanol, is that 5% hydrofluoric acid rinse 10min removes silicon chip surface zone of oxidation with volume fraction, deionized water rinsing 1min removes surface residual fluorion, and nitrogen dries up for subsequent use;
Clean silicon chip is placed in HF:HNO
3: H
2in the solution of O=1:5:10 (volume ratio), under normal temperature after oxide treatment 5min, take out silicon chip deionized water to soak, cleaning, is 5% hydrofluoric acid rinse 10min with volume fraction, rinse with deionized water rinsing 1min again, remove the liquid in duct, high pure nitrogen dries up, and obtains spongy porous silicon film, weigh to obtain porous silicon 1.68 g, for subsequent use under being placed in ammonia atmosphere;
2) active metal ammino is dissolved:
According to the mole ratio of each component of nitride fluorescent film, under normal temperature, in reducing atmosphere proterctive equipment, by 3.44g barium metal and 0.69g Europium Metal, be placed in clean container, inject the dry liquefied ammonia of 500ml, stirring makes dissolving metal, forms ammino metallic solution, stand-by;
3) acquisition of nitride fluorescent film reaction system:
The spongy porous silicon film obtained in step 1) is placed in above-mentioned steps 2) ammino metallic solution soak, the ammino metal ion in solution is made to enter in spongy porous silica body, being combined with Siliciumatom dangling bonds is adsorbed in porous silicon hole, remaining ammino metallic solution is successively coated on porous silicon surface, along with ammonia solvent volatilization, ammino metal is distributed in porous silicon hole and surface, obtains reactant system;
4) by above-mentioned steps 3) reactant system that obtains loads in the nitrogenizing reaction stove of nitrogen purging, and through-flow speed is the high-purity N of 200ml/min
2, keep stove internal gas pressure to be normal pressure, be warmed up to 1350 DEG C, insulation nitrogenizing reaction 24 hours, obtains nitride fluorescent film; Cut-out adds thermoelectricity, and continue to fill nitrogen and make to keep 0.1Mpa pressure in stove, furnace cooling, to normal temperature, stops filling nitrogen, takes out nitride fluorescent film.
Claims (3)
1. a preparation method for nitride fluorescent thin-film material, is characterized in that, the concrete steps of the method are as follows:
Step 1) porous silicon film is formed:
Resistivity is adopted to be 2 × 10
-3~ 8 × 10
-3the heavily doped monocrystalline silicon piece of P type of Ω cm, use acetone ultrasonic cleaning 10 ~ 20min at normal temperatures, remove its surperficial organic pollutant, use dehydrated alcohol ultrasonic cleaning 10 ~ 20min at normal temperatures, remove surface residual acetone, deionized water rinsing 2 ~ 10min, removing residual ethanol, is the hydrofluoric acid rinse 1 ~ 10min of 0.5% ~ 5% by volume percent, removes silicon chip surface zone of oxidation, deionized water rinsing 1 ~ 10min removes surface residual fluorion, and nitrogen dries up for subsequent use;
Clean silicon chip is placed in volume ratio HF:HNO
3: H
2in the solution of O=1:3 ~ 5:5 ~ 10, under normal temperature after oxide treatment 5-30min, take out silicon chip deionized water to soak, clean, be 0.5% ~ 5% hydrofluoric acid rinse 1 ~ 10min with volume percent, then use deionized water rinsing 1 ~ 10min to rinse, remove the liquid in duct, high pure nitrogen dries up, and obtains spongy porous silicon film, for subsequent use under being placed in ammonia atmosphere;
Step 2) dissolving of active metal ammino:
According to the mole ratio of each component of nitride fluorescent film, under normal temperature, in reducing atmosphere proterctive equipment, by calcium metal and rare-earth europium, Preparation of Metallic Strontium and rare-earth europium or barium metal and rare-earth europium, be placed in clean container, inject dry liquefied ammonia solvent, stir and make dissolving metal, form ammino metallic solution, stand-by;
The acquisition of step 3) nitride fluorescent film reaction system:
Above-mentioned steps 1 is got by the component molar number ratio of nitride fluorescent film) porous silicon film, be placed in above-mentioned steps 2) ammino metallic solution soak, the ammino metal ion in solution is made to enter in spongy porous silica body, being combined with Siliciumatom dangling bonds is adsorbed in porous silicon hole, residue ammino metallic solution is successively coated on porous silicon surface, along with ammonia solvent volatilization, ammino metal is distributed in porous silicon hole and surface, obtains reactant system;
Step 4) is by above-mentioned steps 3) reactant system that obtains loads in the nitrogenizing reaction stove of nitrogen purging, and through-flow speed is the high-purity N of 20 ~ 200ml/min
2, keep stove internal gas pressure to be normal pressure, be warmed up to 1000 ~ 1350 DEG C, be incubated 5 ~ 24 hours, obtain nitride fluorescent film; Cut off subsequently and add thermoelectricity, continue to fill nitrogen and make to keep 0.1Mpa pressure in stove, furnace cooling, to normal temperature, stops filling nitrogen, takes out nitride fluorescent film.
2. the preparation method of a kind of nitride fluorescent thin-film material according to claim 1, is characterized in that: described nitrogenizing reaction stove is reductibility heating installation.
3. the preparation method of a kind of nitride fluorescent thin-film material according to claim 1, is characterized in that: the nitrogen of described nitrogenizing reaction stove is the high-purity N of 99.99%
2; Described ammonia solvent is purity 99.99%, and through the drying treatment liquefied ammonia that dewaters, described active metal is analytical reagent.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1805160A (en) * | 2005-11-23 | 2006-07-19 | 天津大学 | Electro-luminescent porous silica material and its preparation method |
| CN102259875A (en) * | 2010-05-25 | 2011-11-30 | 中国科学院微电子研究所 | Preparation method of light-emitting porous silicon |
| CN103173214A (en) * | 2013-03-06 | 2013-06-26 | 浙江理工大学 | Synthesizing method of spherical silicon-based nitrogen compound fluorescent material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1805160A (en) * | 2005-11-23 | 2006-07-19 | 天津大学 | Electro-luminescent porous silica material and its preparation method |
| CN102259875A (en) * | 2010-05-25 | 2011-11-30 | 中国科学院微电子研究所 | Preparation method of light-emitting porous silicon |
| CN103173214A (en) * | 2013-03-06 | 2013-06-26 | 浙江理工大学 | Synthesizing method of spherical silicon-based nitrogen compound fluorescent material |
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