CN105271735B - A kind of high silica red light emitting glass and its manufacture method - Google Patents
A kind of high silica red light emitting glass and its manufacture method Download PDFInfo
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- CN105271735B CN105271735B CN201510723890.3A CN201510723890A CN105271735B CN 105271735 B CN105271735 B CN 105271735B CN 201510723890 A CN201510723890 A CN 201510723890A CN 105271735 B CN105271735 B CN 105271735B
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000011521 glass Substances 0.000 title claims abstract description 66
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 229910009372 YVO4 Inorganic materials 0.000 claims abstract description 75
- 239000000203 mixture Substances 0.000 claims abstract description 57
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 39
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 39
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 39
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 39
- 230000001413 cellular effect Effects 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims description 67
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 61
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 52
- 239000000463 material Substances 0.000 claims description 46
- 238000006243 chemical reaction Methods 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 239000012153 distilled water Substances 0.000 claims description 21
- 235000019441 ethanol Nutrition 0.000 claims description 20
- 239000002244 precipitate Substances 0.000 claims description 17
- 238000009413 insulation Methods 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 9
- 229910020700 Na3VO4 Inorganic materials 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 8
- GAGGCOKRLXYWIV-UHFFFAOYSA-N europium(III) nitrate Inorganic materials [Eu+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GAGGCOKRLXYWIV-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- DHEQXMRUPNDRPG-UHFFFAOYSA-N strontium nitrate Inorganic materials [Sr+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O DHEQXMRUPNDRPG-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Inorganic materials [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims 2
- 238000004140 cleaning Methods 0.000 claims 1
- 239000011258 core-shell material Substances 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 230000003595 spectral effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 238000009826 distribution Methods 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- 238000013019 agitation Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 229910002538 Eu(NO3)3·6H2O Inorganic materials 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 238000000295 emission spectrum Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000695 excitation spectrum Methods 0.000 description 1
- 238000001033 granulometry Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- -1 rare earth ion Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of high silica red light emitting glass, is made up of cellular glass and feux rouges fluorescent composition, wherein, the feux rouges fluorescent composition accounts for the 0.01 ~ 1% of cellular glass gross mass, and the feux rouges fluorescent composition is YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+@SiO2.The invention also discloses a kind of preparation method of high silica red light emitting glass.The red light emitting glass, which has, to be turned light efficiency height, turns the high effect of light spectral width, luminous intensity, and feux rouges fluorescent composition has preferably dispersiveness in the glass, and the uniformity that glass can be achieved lights.
Description
Technical field
The present invention relates to a kind of high silica red light emitting glass and its manufacture method.
Background technology
At present, in fluorescent glass, the luminous efficiency of its light emitting ionic is far below crystalline material, mainly due to high temperature melting
Melt and prepare in glass process, easily spontaneously form cluster and produce concentration delustring.In the prior art, have by the way that cellular glass is soaked
In rare earth ion, then solid-phase sintering is carried out to form the fluorescent glass of good dispersion, but its wave band absorbed is limited, and it is luminous
Efficiency need to be improved, and limits its application.
The content of the invention
In order to solve above-mentioned the deficiencies in the prior art, the invention provides a kind of high silica red light emitting glass and its manufacturer
Method, the red light emitting glass, which has, to be turned light efficiency height, turns the high effect of light spectral width, luminous intensity, and feux rouges fluorescent composition exists
It is uniformly distributed in red light emitting glass and dispersiveness is preferable.
The technical problems to be solved by the invention are achieved by the following technical programs：
A kind of high silica red light emitting glass, it is characterised in that it is made up of cellular glass and feux rouges fluorescent composition, wherein,
The feux rouges fluorescent composition accounts for the 0.01 ~ 1% of cellular glass gross mass, and the feux rouges fluorescent composition is YVO4: Eu3+,Sr2+@
YVO4: Eu3+,Bi3+@SiO2。
A kind of manufacture method of high silica red light emitting glass, comprises the following steps：Cellular glass is immersed in feux rouges fluorescence
After composition dispersion soln, 1100 DEG C of 30 ~ 60min of sintering are carried out under oxygen atmosphere, high silica red light emitting is made in furnace cooling
Glass；The feux rouges fluorescent composition accounts for the 0.01 ~ 1% of cellular glass gross mass, and the feux rouges fluorescent composition is YVO4: Eu3+,
Sr2+@YVO4: Eu3+,Bi3+@SiO2。
The present invention has the advantages that：This red light emitting glass, which has, to be turned light efficiency height, turns light spectral width, luminous intensity
High effect, especially with double light-conversion fluorescent powders, the spectrum of different-waveband can be more preferably absorbed, further improves and turns light light
Spectrum；Feux rouges fluorescent composition is uniformly distributed in red light emitting glass simultaneously and dispersiveness is preferable, is advantageous to improve luminous intensity, is entered
One step reduces the possibility that cluster causes delustring.
Brief description of the drawings
Fig. 1 represents the figure of the determination data of the particle diameter distribution of the different fluorescent material by obtaining, wherein, 1-1 is in embodiment 1
The step of step 1（Three）Obtained YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+The particle size distribution data figure of nucleocapsid fluorescent material；
The step of 1-2 is step 1 in embodiment 1（Four）Obtained YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+@ SiO2Feux rouges fluorescence group
The particle size distribution data figure of compound；1-3 is obtained NaYF4:Yb3+, Er3+@SiO2The particle size distribution data of nano-phosphor
Figure；
Fig. 2 represent the excitation spectrum of fluorescent glass 620nm supervisory wavelengths made from embodiment 1 to 6 and comparative example 1 to 3 and
The emission spectrum of 365nm excitation wavelengths；Wherein 2-1 to 2-9 represents that embodiment 1 is right to embodiment 6 and the institute of comparative example 1 to 3 respectively
The spectrogram answered；
NaYF obtained by Fig. 3 expressions4:Yb3+, Er3+@SiO2Emission spectrum of the nano-phosphor in 980nm excitation wavelengths.
Embodiment
The present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses and 0.25 part it is red
Light fluorescent composition, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@YVO4: Eu3+,Bi3+@SiO2。
A kind of manufacture method of high silica red light emitting glass, specifically comprises the following steps：
First, feux rouges fluorescent composition is prepared
（One）Prepare YVO4:Eu3+,Sr2+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5ml ethylene glycol and 2ml distilled water
In；（2）Above-mentioned solution side is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）Instill and contain dropwise below
There are the Y (NO that 1.5mmol is necessarily matched3)3·6H2O, Eu(NO3)3, Sr(NO3)2（0.9:0.03:0.07）8 ml ethylene glycol
In solution, then it is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）10min clarifies to solution, adds
20ml distilled water；（3）Reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 ml, in vacuum ring
Under border, 200oInsulation reaction 1h under C, is down to 150oInsulation reaction 1h under C, after reaction terminates, it is cooled to room temperature.Gained is suspended
Liquid is poured out, and is centrifuged and is cleaned 3 acquisition white precipitates with acetone；（4）This is deposited in 90o5h is dried under C, obtains average grain diameter
10 ~ 15nm Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor；（5）To Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor
Carry out 500 DEG C of vacuum heat 1h（It is rapidly heated, fluorescent material is preferably in the annealing temperature again when temperature reaches 500 DEG C
Under be heat-treated）, 20 ~ 30nm of average grain diameter Y after being heat-treated0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor.
（Two）Prepare YVO4:Eu3+,Bi3+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5ml ethylene glycol and 2ml distilled water
In；（2）Above-mentioned solution side is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）Side instill dropwise containing
Y (the NO that 1.5mmol is necessarily matched3)3·6H2O, Eu(NO3)3, Bi(NO3)3（0.87:0.03:0.1）8 ml ethylene glycol it is molten
In liquid, then it is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）10min clarifies to solution, adds 20ml
Distilled water；（3）Reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 ml, under vacuum conditions,
180oInsulation reaction 1.5h under C, after reaction terminates, it is cooled to room temperature.Gained suspension is poured out, centrifuges and cleans 3 with acetone
Secondary acquisition white precipitate；（4）This is deposited in 90o5h is dried under C, obtains average grain diameter about 10nm Y0.87VO4:Eu3+ 0.03,
Bi3+ 0.1Nano-phosphor.
（Three）Prepare YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+Nucleocapsid fluorescent material
（1）It is pre-dispersed：Weigh the YVO of 0.1g heat treatments4:Eu3+,Sr2+Nano-phosphor is placed in 10ml ethanol, and is carried out
Ultrasonic agitation（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）Scattered 30min, obtained solution A；Weigh
0.008gYVO4:Eu3+,Bi3+Nano-phosphor is placed in 10ml ethanol, and is stirred by ultrasonic（80KHz ultrasonic vibrations and
1000r/min centrifugal speeds stir）Scattered 15min, obtained solution B；（2）Side is stirred by ultrasonic（60KHz ultrasonic vibrations and 500r/
Min centrifugal speeds stir）Solution A, side instill solution B dropwise；Continue to be stirred by ultrasonic（50KHz ultrasonic vibrations and 100r/min from
Heart speed stirs）5min stands 5min again, centrifuges and cleans 3 acquisition white precipitates with acetone；（4）This is deposited in 90oUnder C
5h is dried, obtains 40 ~ 60nm of average grain diameter YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+Nucleocapsid fluorescent material, its particle diameter distribution is such as
Shown in 1-1 in Fig. 1.
（Four）Prepare YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+@SiO2Feux rouges fluorescent composition
（1）Nucleocapsid fluorescent material is stirred by ultrasonic（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）It is scattered in
In ethanol, obtained solution C；Add afterwards a certain proportion of（4:1）Water and ammoniacal liquor, are stirring evenly and then adding into tetraethyl orthosilicate and core
The mass ratio of shell fluorescent material is 1.5:1, regulation pH value is 9, and reaction temperature is 20 DEG C, is reacted 5 hours；Centrifuged and use third
Ketone cleans 3 acquisition white precipitates；This is deposited in 90o5h is dried under C, to obtain being coated with SiO2Nucleocapsid fluorescent material；（2）
This is coated with SiO2Nucleocapsid fluorescent material be placed under argon gas atmosphere carry out 800 DEG C heat treatment 1h, obtain average grain diameter 70 ~
100nm feux rouges fluorescent compositions, its particle diameter distribution is as shown in the 1-2 in Fig. 1.
2nd, feux rouges fluorescent composition is placed in ethanol solution in proportion, be stirred by ultrasonic（100KHz ultrasonic vibrations and
1000r/min centrifugal speeds stir）Scattered 30min, is made dispersion soln D；Cellular glass is immersed in proportion above-mentioned scattered
30min in solution A, continue to be stirred by ultrasonic（50KHz ultrasonic vibrations and the stirring of 100r/min centrifugal speeds）5min is stood again
25min；Cleaned for several times with deionized water, remove the unadsorbed excessive powder on cellular glass；Carried out under oxygen atmosphere
High silica red light emitting glass is made in 1100 DEG C of 30 ~ 60min of sintering, furnace cooling.
Embodiment 2
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses and 0.01 part it is red
Light fluorescent composition, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@YVO4: Eu3+,Bi3+@SiO2.The glass that glows
Glass manufacture method is the same as embodiment 1.
Embodiment 3
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses and 1 part of feux rouges
Fluorescent composition, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@YVO4: Eu3+,Bi3+@SiO2.The red light emitting glass
Manufacture method is the same as embodiment 1.
Embodiment 4
On the basis of embodiment 1, by the step in step 1（Three）YVO4: Eu3+,Sr2+With YVO4: Eu3+,
Bi3+Weight ratio be changed to 1：0.5, remaining is same as Example 1.
Embodiment 5
On the basis of embodiment 1, by the step in step 1（Three）YVO4: Eu3+,Sr2+With YVO4: Eu3+,
Bi3+Weight ratio be changed to 1：0.001, remaining is same as Example 1.
Embodiment 6
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses and 0.25 part it is red
Light fluorescent composition, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@YVO4: Eu3+,Bi3+@SiO2。
A kind of manufacture method of high silica red light emitting glass, specifically comprises the following steps：
First, feux rouges fluorescent composition is prepared
（One）Prepare YVO4:Eu3+,Sr2+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5ml ethylene glycol and 2ml distilled water
In；（2）Above-mentioned solution side is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）Instill and contain dropwise below
There are the Y (NO that 1.5mmol is necessarily matched3)3·6H2O, Eu(NO3)3, Sr(NO3)2（0.9:0.03:0.07）8 ml ethylene glycol
In solution, then it is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）10min clarifies to solution, adds
20ml distilled water；（3）Reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 ml, in vacuum ring
Under border, 200oInsulation reaction 1h under C, is down to 150oInsulation reaction 1h under C, after reaction terminates, it is cooled to room temperature.Gained is suspended
Liquid is poured out, and is centrifuged and is cleaned 3 acquisition white precipitates with acetone；（4）This is deposited in 90o5h is dried under C, obtains average grain diameter
10 ~ 15nm Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor；（5）To Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor
Carry out 500 DEG C of vacuum heat 1h（It is rapidly heated, fluorescent material is preferably in the annealing temperature again when temperature reaches 500 DEG C
Under be heat-treated）, 20 ~ 30nm of average grain diameter Y after being heat-treated0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor.
（Two）Prepare YVO4:Bi3+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5ml ethylene glycol and 2ml distilled water
In；（2）Above-mentioned solution side is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）Side instill dropwise containing
Y (the NO that 1.5mmol is necessarily matched3)3·6H2O, Bi(NO3)3（0.87:0.1）8 ml ethylene glycol solutions in, then be stirred by ultrasonic
（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）10min clarifies to solution, adds 20ml distilled water；（3）Will reaction
Solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 ml, under vacuum conditions, 180oInsulation reaction under C
1.5h, after reaction terminates, it is cooled to room temperature.Gained suspension is poured out, centrifuges and cleans 3 acquisition white precipitates with acetone；
（4）This is deposited in 90o5h is dried under C, obtains average grain diameter about 10nm Y0.87VO4:Bi3+ 0.1Nano-phosphor.
（Three）Prepare YVO4:Eu3+,Sr2+@YVO4:Bi3+Nucleocapsid fluorescent material
（1）It is pre-dispersed：Weigh the YVO of 0.1g heat treatments4:Eu3+,Sr2+Nano-phosphor is placed in 10ml ethanol, and is carried out
Ultrasonic agitation（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）Scattered 30min, obtained solution A；Weigh
0.008gYVO4:Bi3+Nano-phosphor is placed in 10ml ethanol, and is stirred by ultrasonic（80KHz ultrasonic vibrations and 1000r/
Min centrifugal speeds stir）Scattered 15min, obtained solution B1；（2）Side is stirred by ultrasonic（60KHz ultrasonic vibrations and 500r/min from
Heart speed stirs）Solution A, side instill solution B 1 dropwise；Continue to be stirred by ultrasonic（50KHz ultrasonic vibrations and 100r/min centrifugation speed
Degree stirring）5min stands 5min again, centrifuges and cleans 3 acquisition white precipitates with acetone；（4）This is deposited in 90oDried under C
5h, obtain 40 ~ 60nm of average grain diameter YVO4:Eu3+,Sr2+@YVO4:Bi3+Nucleocapsid fluorescent material.
（Four）Prepare YVO4:Eu3+,Sr2+@YVO4: Eu3+,Bi3+Nucleocapsid fluorescent material
（1）By 0.05 mmol Eu (NO3)3·6H2O ultrasonic disperses are in 15 ml ethanol solutions, by step 3 system
The YVO obtained4:Eu3+,Sr2+@YVO4:Bi3+Nucleocapsid fluorescent material presoma is dispersed in above-mentioned solution；（2）After 60min is stirred by ultrasonic
（60KHz ultrasonic vibrations and the stirring of 500r/min centrifugal speeds）, reaction solution is stood into 24h so that ion exchange process is able to
Fully carry out.Wherein, Eu (NO3)3·6H2O amount can be according to chemical formula Y(0.9-x)VO4: Eu3+ (x), Bi3+ (0.1)Determine,
It is it is preferred that somewhat excessive.After reaction terminates, centrifugation, and with absolute ethyl alcohol and distill 3 acquisition white precipitates of water washing.Finally, exist
90o5h is dried under C, obtains YVO4:Eu3+,Sr2+@YVO4: Eu3+,Bi3+Nucleocapsid fluorescent material.
（Five）Prepare YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+@SiO2Feux rouges fluorescent composition
（1）Nucleocapsid fluorescent material is stirred by ultrasonic（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）It is scattered in
In ethanol, obtained solution C；Add afterwards a certain proportion of（4:1）Water and ammoniacal liquor, are stirring evenly and then adding into tetraethyl orthosilicate and core
The mass ratio of shell fluorescent material is 1.5:1, regulation pH value is 9, and reaction temperature is 20 DEG C, is reacted 5 hours；Centrifuged and use third
Ketone cleans 3 acquisition white precipitates；This is deposited in 90o5h is dried under C, to obtain being coated with SiO2Nucleocapsid fluorescent material；（2）
This is coated with SiO2Nucleocapsid fluorescent material be placed under argon gas atmosphere carry out 800 DEG C heat treatment 1h, obtain average grain diameter 70 ~
100nm feux rouges fluorescent compositions.
2nd, feux rouges fluorescent composition is placed in ethanol solution in proportion, be stirred by ultrasonic（100KHz ultrasonic vibrations and
1000r/min centrifugal speeds stir）Scattered 30min, is made dispersion soln D；Cellular glass is immersed in proportion above-mentioned scattered
30min in solution D, continue to be stirred by ultrasonic（50KHz ultrasonic vibrations and the stirring of 100r/min centrifugal speeds）5min is stood again
25min；Cleaned for several times with deionized water, remove the unadsorbed excessive powder on cellular glass；Carried out under oxygen atmosphere
High silica red light emitting glass is made in 1100 DEG C of 30 ~ 60min of sintering, furnace cooling.
Embodiment 7
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses, 0.25 part red
Light fluorescent composition and 0.2 part of NaYF4:Yb3+, Er3+Fluorescent material, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@
YVO4: Eu3+,Bi3+@SiO2。
Embodiment 8
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses, 0.25 part red
Light fluorescent composition and 0.01 part of NaYF4:Yb3+, Er3+Fluorescent material, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@
YVO4: Eu3+,Bi3+@SiO2。
Embodiment 9
A kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses, 0.25 part red
Light fluorescent composition and 1 part of NaYF4:Yb3+, Er3+Fluorescent material, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@YVO4:
Eu3+,Bi3+@SiO2。
The manufacture method of the high silica red light emitting glass of embodiment 7 to 9, specifically comprises the following steps：
First, feux rouges fluorescent composition is made in the preparation method of step 1 such as in embodiment 1；
2nd, NaYF is prepared4:Yb3+, Er3+@SiO2The method of fluorescent material is as follows：
（1）Weigh 1.8 mmol Y (NO3)3·6H2O、0.17 mmol Yb(NO3)3·5H2O、0.1 mmol Er
(NO3)3·5H2O, with 2 mmol NaNO3Mix and be completely dissolved in 15 ml ethylene glycol and form solution E；By 8mmolNH4F fills
Divide to be dissolved in 15 ml ethylene glycol and form solution F；It is stirred by ultrasonic respectively（80KHz ultrasonic vibrations and 300r/min centrifugal speeds are stirred
Mix）Solution E, F 30min, continuing to be stirred by ultrasonic after the mixing of two solution（80KHz ultrasonic vibrations and 300r/min centrifugal speeds are stirred
Mix）30min；Mixed solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions,
180oInsulation reaction 12h under C, is down to 150oInsulation reaction 4h under C, after reaction terminates, it is cooled to room temperature.Gained suspension is fallen
Go out, centrifuge and clean 3 acquisition fluorescent material successively with distilled water and absolute ethyl alcohol；This is deposited in 80o5h is dried under C, is obtained
30 ~ 60nm of average grain diameter NaYF4:Yb3+, Er3+Nano-phosphor；
（2）By 0.3g nano NaY F obtained above4:Yb3+, Er3+30min is stirred by ultrasonic in phosphor powder（100KHz surpasses
Acoustic vibration and the stirring of 1000r/min centrifugal speeds）It is scattered in 40ml absolute ethyl alcohols and 10ml distilled water；It is by 2 ml mass fractions
28 % ammoniacal liquor and 0.3 ml tetraethyl orthosilicate TEOS are added in above-mentioned dispersion soln, and 4 h are sufficiently stirred at 20 DEG C, are made
NaYF4:Yb3+, Er3+@SiO2Powder；Centrifuged and use distilled water and the acquisition white precipitates of washes of absolute alcohol 3 times；Should
It is deposited in 90o5h is dried under C, to obtain being coated with SiO2NaYF4:Yb3+, Er3+Nucleocapsid fluorescent material；By the NaYF4:Yb3+,
Er3+@SiO2Nucleocapsid fluorescent material, which is placed under argon gas atmosphere, carries out 800 DEG C of heat treatment 60min, obtains 55 ~ 85nm's of average grain diameter
NaYF4:Yb3+, Er3+@SiO2Nano-phosphor, its particle size determination 1-3 as shown in Figure 1, it is under 980nm excitation wavelengths, hair
Corresponding characteristic peak is penetrated, is particularly at 655nm highest peak, as shown in Figure 3.
3rd, feux rouges fluorescent composition is placed in ethanol solution in proportion, be stirred by ultrasonic（100KHz ultrasonic vibrations and
1000r/min centrifugal speeds stir）Scattered 30min, is made dispersion soln D；In proportion by NaYF4:Yb3+, Er3+@SiO2Nanometer
Fluorescent material is placed in ethanol solution, ultrasonic agitation（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）It is scattered
30min, dispersion soln G is made；Half and half cellular glass is immersed in 30min in above-mentioned dispersion soln D, G in proportion, continues ultrasound
Stirring（50KHz ultrasonic vibrations and the stirring of 100r/min centrifugal speeds）5min stands 25min again；Cleaned for several times with deionized water,
Remove the unadsorbed excessive powder on cellular glass；Two kinds of cellular glasses are mixed, 1100 DEG C of sintering are carried out under oxygen atmosphere
High silica red light emitting glass is made in 30 ~ 60min, furnace cooling.
Comparative example 1
The present embodiment and the difference of embodiment 1 are：The preparation method of feux rouges fluorescent composition, remaining and embodiment
1 is identical.The preparation method of the feux rouges fluorescent composition of the present embodiment is as follows：
（One）Prepare YVO4: Eu3+,Sr2+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5ml ethylene glycol and 2ml distilled water
In；（2）Above-mentioned solution side is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）Instill and contain dropwise below
There are the Y (NO that 1.5mmol is necessarily matched3)3·6H2O, Eu(NO3)3, Sr(NO3)2（0.9: 0.03: 0.07）8 ml second two
In alcoholic solution, then it is stirred by ultrasonic（80KHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds）10min clarifies to solution, adds
20ml distilled water；（3）Reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 ml, in vacuum ring
Under border, 200oInsulation reaction 1h under C, is down to 150oInsulation reaction 1h under C, after reaction terminates, it is cooled to room temperature.Gained is suspended
Liquid is poured out, and is centrifuged and is cleaned 3 acquisition white precipitates with acetone；（4）This is deposited in 90o5h is dried under C, obtains average grain diameter
10 ~ 20nm Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor；（5）To Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor
Carry out 500 DEG C of vacuum heat 1h（It is rapidly heated, fluorescent material is preferably in the annealing temperature again when temperature reaches 500 DEG C
Under be heat-treated）, 20 ~ 30nm of average grain diameter Y after being heat-treated0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor.
（Two）Prepare YVO4: Eu3+, Sr2+ @YVO4: Eu3+, Bi3+Nucleocapsid fluorescent material
By the Y obtained by the first step0.9VO4: Eu3+ 0.03, Sr2+ 0.07Fluorescent material（1.6 mmol）It is dispersed in 10 ml second two
Alcoholic solution, and according to R values（Nucleocapsid mol ratio, i.e. R=YVO4: Eu3+, Ba2+ /YVO4: Eu3+, Bi3+）Calculate, will necessarily rub
Y (the NO of your amount3)3·6H2O, Eu(NO3)3, Bi(NO3)3·5H2O（Mol ratio is 0.87: 0.03: 0.1）Add above-mentioned molten
In liquid, and the min of ultrasonic vibration 20；（2）1.2 mmol Na3VO4·12H2O adds to be distilled containing 5 ml ethylene glycol and 2 ml
In the mixed solution of water, instilled dropwise while stirring after being completely dissolved（1）In resulting solution, 20ml steamings are added after stirring 5 min
Distilled water；（3）Gained reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 ml（Compactedness 70
%）, 200oUnder C, the h of isothermal holding 2, after reaction terminates, room temperature is cooled to the furnace.Gained suspension is poured out, centrifugation is used in combination
Acetone cleans 3 acquisition white precipitates；（4）This is finally deposited in 80o8 h are dried under C, obtain YVO4: Eu3+, Sr2+ @
YVO4: Eu3+, Bi3+Nano-phosphor.
（Three）Prepare YVO4: Eu3+,Sr2+@YVO4: Eu3+,Bi3+@SiO2Feux rouges fluorescent composition
（1）Nucleocapsid fluorescent material is stirred by ultrasonic（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）It is scattered in
In ethanol, obtained solution E；Add afterwards a certain proportion of（4:1）Water and ammoniacal liquor, are stirring evenly and then adding into tetraethyl orthosilicate and core
The mass ratio of shell fluorescent material is 1.5:1, regulation pH value is 9, and reaction temperature is 20 DEG C, is reacted 5 hours；Centrifuged and use third
Ketone cleans 3 acquisition white precipitates；This is deposited in 90o5h is dried under C, to obtain being coated with SiO2Nucleocapsid fluorescent material；（2）
This is coated with SiO2Nucleocapsid fluorescent material be placed under argon gas atmosphere carry out 800 DEG C heat treatment 1h, obtain feux rouges fluorescent composition.
Comparative example 2
The present embodiment and the difference of embodiment 1 are：The preparation method of feux rouges fluorescent composition, remaining and embodiment
1 is identical.The preparation method of the feux rouges fluorescent composition of the present embodiment is as follows：On the basis of embodiment 1, remove step
（Three）, and in step（Four）In, by the YVO of 1g heat treatments4: Eu3+,Sr2+Nano-phosphor and 0.05gYVO4: Eu3+,Bi3+
Nano-phosphor mixing ultrasonic agitation（100KHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds）It is scattered in ethanol, makes
Obtain solution E；Remaining preparation process is same as Example 1.
Comparative example 3
The present embodiment difference from Example 1 is：Used feux rouges fluorescent composition is made from conventional method
YVO4: Eu3+Nano-phosphor；It is remaining same as Example 1.
Performance test analysis：
By YVO made from embodiment 14: Eu3+,Sr2+@YVO4: Eu3+,Bi3+XRD diffractions are carried out, institute in diffraction pattern
Some bragg peak positions, relative intensity all with YVO4Standard card (JCPDS 17-0341) is consistent, may be characterized as pure four
Square phase YVO4Crystal structure, other miscellaneous peaks are not found.
Average granulometry：Obtained dispersion liquid is handled with ultrasonic homogenizer, is surveyed using laser diffraction formula size distribution
Determine device (Shimadzu Seisakusho Ltd.'s system " SALD-7000 ") measure average grain diameter, as a result as shown in Figure 1.
The obtained red light emitting glass of embodiment 1 to 6 and comparative example 1 to 3 is subjected to PL spectrum measure, as a result such as Fig. 2 institutes
Show, from figure 2 it can be seen that the feux rouges fluorescent composition of comparative example 1 is absorbed with certain widthization, the band edge of absorption band is to long wave
Long red shift, but it is not very strong in the absorption of the ultraviolet region of short wavelength；The feux rouges fluorescent composition of comparative example 2 is purple in short wavelength
Comparative example the last 1 is compared in the absorption in Wai Guang areas；Comparative example 3 mainly absorbs short UV light area, and its phototranstormation efficiency is not high；
The feux rouges fluorescent composition absorption band of embodiment 1 to 6 has certain widthization, and not only the band edge of absorption band is to long wavelength's red shift, together
Shi Qi also has in short UV light area preferably to be absorbed, particularly embodiment 5, is absorbed in ultraviolet region compared with other implementations
Example absorption is most strong, is also most strong equally in the emission peak of 620nm wavelength.Using 365nm as excitation wavelength, embodiment 1,4,5,6
And the glass of comparative example 1,2 can be seen uniformity and send feux rouges, and embodiment 2,3 is due to the feux rouges fluorescent composition mistake of addition
It is more or very few, the problem of causing its non-uniform light.
Embodiment described above only expresses embodiments of the present invention, and its description is more specific and detailed, but can not
Therefore the limitation to the scope of the claims of the present invention is interpreted as, as long as the skill obtained using the form of equivalent substitution or equivalent transformation
Art scheme, it all should fall within the scope and spirit of the invention.
Claims (1)
1. a kind of high silica red light emitting glass, it is made up of the raw material of following parts by weight:100 parts of cellular glasses, 0.25 part of feux rouges
Fluorescent composition and 0.2 part of NaYF4:Yb3+, Er3+Fluorescent material, the feux rouges fluorescent composition are YVO4: Eu3+,Sr2+@YVO4:
Eu3+,Bi3+@SiO2；
A kind of manufacture method of high silica red light emitting glass, specifically comprises the following steps：
First, YVO is prepared4: Eu3+,Sr2+@YVO4: Eu3+,Bi3+@SiO2Feux rouges fluorescent composition
（One）Prepare YVO4:Eu3+,Sr2+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5mL ethylene glycol and 2 mL distilled water；
（2）By above-mentioned solution side be stirred by ultrasonic, 80kHz ultrasonic vibrations and 300r/min centrifugal speeds stirring, side instill dropwise containing
Y (the NO that 1.5mmol is necessarily matched3)3·6H2O, Eu(NO3)3, Sr(NO3)2, mol ratio 0.9:0.03:0.07,8 mL second
In glycol solution, then it is stirred by ultrasonic, 80kHz ultrasonic vibrations and 300r/min centrifugal speeds stir 10min and clarified to solution, add
20 mL distilled water；（3）Reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 mL, in vacuum ring
Under border, 200oInsulation reaction 1h under C, is down to 150oInsulation reaction 1h under C, after reaction terminates, room temperature is cooled to, gained is suspended
Liquid is poured out, and is centrifuged and is cleaned 3 acquisition white precipitates with acetone；（4）This is deposited in 90o5h is dried under C, obtains average grain diameter
10 ~ 15nm Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor；（5）To Y0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nano-phosphor
Carry out 500 DEG C of vacuum heat 1h, 20 ~ 30nm of average grain diameter Y after being heat-treated0.9VO4:Eu3+ 0.03, Sr2+ 0.07Nanometer
Fluorescent material；
（Two）Prepare YVO4:Eu3+,Bi3+Nano-phosphor
（1）By 1.2mmol Na3VO4·12H2O is dissolved in the mixed solution containing 5 mL ethylene glycol and 2 mL distilled water；
（2）By above-mentioned solution side be stirred by ultrasonic, 80kHz ultrasonic vibrations and 300r/min centrifugal speeds stirring, side instill dropwise containing
Y (the NO that 1.5mmol is necessarily matched3)3·6H2O, Eu(NO3)3, Bi(NO3)3, mol ratio 0.87:0.03:0.1,8 mL second
In glycol solution, then it is stirred by ultrasonic, 80kHz ultrasonic vibrations and 300r/min centrifugal speeds stir 10min and clarified to solution, add
20 mL distilled water；（3）Reaction solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 mL, in vacuum ring
Under border, 180oInsulation reaction 1.5h under C, after reaction terminates, room temperature is cooled to, gained suspension is poured out, centrifuges and uses acetone
3 acquisition white precipitates of cleaning；（4）This is deposited in 90o5h is dried under C, obtains average grain diameter 10nm Y0.87VO4:Eu3 + 0.03, Bi3+ 0.1Nano-phosphor；
（Three）Prepare YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+Nucleocapsid fluorescent material
（1）It is pre-dispersed：Weigh the YVO of 0.1g heat treatments4:Eu3+,Sr2+Nano-phosphor is placed in 10 mL ethanol, and is surpassed
Sound stirs, and 100kHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds, disperses 30min, obtained solution A；Weigh
0.008gYVO4:Eu3+,Bi3+Nano-phosphor is placed in 10 mL ethanol, and is stirred by ultrasonic, 80kHz ultrasonic vibrations and
1000r/min centrifugal speeds are dispersed with stirring 15min, obtained solution B；（2）Side is stirred by ultrasonic, 60kHz ultrasonic vibrations and 500r/
Min centrifugal speed agitating solution A, side instills solution B dropwise；Continue to be stirred by ultrasonic, 50kHz ultrasonic vibrations and 100r/min centrifugations
Speed stirring 5min stands 5min again, centrifuges and cleans 3 acquisition white precipitates with acetone；（4）This is deposited in 90oDone under C
Dry 5h, obtain 40 ~ 60nm of average grain diameter YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+Nucleocapsid fluorescent material, wherein YVO4: Eu3+,
Sr2+With YVO4: Eu3+,Bi3+Weight ratio be changed to 1：0.001；
（Four）Prepare YVO4:Eu3+,Sr2+@YVO4:Eu3+,Bi3+@SiO2Feux rouges fluorescent composition
（1）Nucleocapsid fluorescent material is stirred by ultrasonic, 100kHz ultrasonic vibrations and the stirring of 1000r/min centrifugal speeds, is scattered in ethanol
In, obtained solution C；4 are added afterwards:1 water and ammoniacal liquor, it is stirring evenly and then adding into the mass ratio of tetraethyl orthosilicate and nucleocapsid fluorescent material
For 1.5:1, regulation pH value is 9, and reaction temperature is 20 DEG C, is reacted 5 hours；Centrifuged and clean 3 times with acetone and obtain white
Precipitation；This is deposited in 90o5h is dried under C, to obtain being coated with SiO2Nucleocapsid fluorescent material；（2）This is coated with SiO2Core
Shell fluorescent material, which is placed under argon gas atmosphere, carries out 800 DEG C of heat treatment 1h, obtains average grain diameter 70 ~ 100nm feux rouges fluorescent compositions；
2nd, NaYF is prepared4:Yb3+, Er3+@SiO2The method of fluorescent material is as follows：
（1）Weigh 1.8 mmol Y (NO3)3·6H2O、0.17 mmol Yb(NO3)3·5H2O、0.1 mmol Er(NO3)3·
5H2O, with 2 mmol NaNO3Mix and be completely dissolved in 15 mL ethylene glycol and form solution E；By 8mmolNH4F fully dissolves
Solution F is formed in 15 mL ethylene glycol；It is stirred by ultrasonic respectively, 80kHz ultrasonic vibrations and 300r/min centrifugal speed agitating solutions
E, F 30min, continuing to be stirred by ultrasonic after the mixing of two solution, 80kHz ultrasonic vibrations and the stirring of 300r/min centrifugal speeds
30min；Mixed solution is poured into the polytetrafluoroethyllining lining autoclave that volume is 50 mL, under vacuum conditions,
180oInsulation reaction 12h under C, is down to 150oInsulation reaction 4h under C, after reaction terminates, it is cooled to room temperature；Gained suspension is fallen
Go out, centrifuge and clean 3 acquisition fluorescent material successively with distilled water and absolute ethyl alcohol；This is deposited in 80o5h is dried under C, is obtained
30 ~ 60nm of average grain diameter NaYF4:Yb3+, Er3+Nano-phosphor；
（2）By 0.3g nano NaY F obtained above4:Yb3+, Er3+30min, 100KHz ultrasound shakes is stirred by ultrasonic in phosphor powder
Dynamic and 1000r/min centrifugal speeds are dispersed with stirring in 40 mL absolute ethyl alcohols and 10 mL distilled water；It is 28 by 2 mL mass fractions
% ammoniacal liquor and 0.3 mL tetraethyl orthosilicate TEOS are added in above-mentioned dispersion soln, and 4 h are sufficiently stirred at 20 DEG C, are made
NaYF4:Yb3+, Er3+@SiO2Powder；Centrifuged and use distilled water and the acquisition white precipitates of washes of absolute alcohol 3 times；Should
It is deposited in 90o5h is dried under C, to obtain being coated with SiO2NaYF4:Yb3+, Er3+Nucleocapsid fluorescent material；By the NaYF4:Yb3+,
Er3+@SiO2Nucleocapsid fluorescent material, which is placed under argon gas atmosphere, carries out 800 DEG C of heat treatment 60min, obtains 55 ~ 85nm's of average grain diameter
NaYF4:Yb3+, Er3+@SiO2Nano-phosphor；
3rd, feux rouges fluorescent composition is placed in ethanol solution in proportion, be stirred by ultrasonic, 100kHz ultrasonic vibrations and 1000r/
Min centrifugal speeds are dispersed with stirring 30min, and dispersion soln D is made；In proportion by NaYF4:Yb3+, Er3+@SiO2Nano-phosphor
It is placed in ethanol solution, is stirred by ultrasonic, 100kHz ultrasonic vibrations and 1000r/min centrifugal speeds is dispersed with stirring 30min, are made and divide
Dissipate solution G；Half and half cellular glass is immersed in 30min in above-mentioned dispersion soln D, G in proportion, continues to be stirred by ultrasonic, 50kHz surpasses
Acoustic vibration and 100r/min centrifugal speeds stirring 5min stand 25min again；Cleaned for several times, removed unadsorbed more with deionized water
Excessive powder on the glass of hole；Two kinds of cellular glasses are mixed, 1100 DEG C are carried out under oxygen atmosphere and sinters 30 ~ 60min, it is cold with stove
But high silica red light emitting glass is made.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928111A (en) * | 2009-06-26 | 2010-12-29 | 海洋王照明科技股份有限公司 | Luminescent glass, making method and application thereof |
| CN102701590A (en) * | 2012-06-29 | 2012-10-03 | 中国科学院上海光学精密机械研究所 | Preparation method of near ultraviolet-excited high silica blue-light-emitting glass |
| CN103449717A (en) * | 2012-05-30 | 2013-12-18 | 广州锐得森特种陶瓷科技有限公司 | Eu<2+>/Al<3+> codoped high silica glass having adjustable Eu<2+> fluorescence characteristic |
| CN104017580A (en) * | 2014-06-18 | 2014-09-03 | 东南大学 | Preparation method of ultra-small NaYF4: Yb3+, Er3+ upconversion luminescent material |
-
2015
- 2015-10-29 CN CN201510723890.3A patent/CN105271735B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928111A (en) * | 2009-06-26 | 2010-12-29 | 海洋王照明科技股份有限公司 | Luminescent glass, making method and application thereof |
| CN103449717A (en) * | 2012-05-30 | 2013-12-18 | 广州锐得森特种陶瓷科技有限公司 | Eu<2+>/Al<3+> codoped high silica glass having adjustable Eu<2+> fluorescence characteristic |
| CN102701590A (en) * | 2012-06-29 | 2012-10-03 | 中国科学院上海光学精密机械研究所 | Preparation method of near ultraviolet-excited high silica blue-light-emitting glass |
| CN104017580A (en) * | 2014-06-18 | 2014-09-03 | 东南大学 | Preparation method of ultra-small NaYF4: Yb3+, Er3+ upconversion luminescent material |
Non-Patent Citations (2)
| Title |
|---|
| YVO4:Eu3+@SiO2核壳结构纳米复合材料的合成与表征;刘利娜等;《发光学报》;20150831;第36卷(第8期);第882-887页 * |
| 铕离子掺杂纳米钒酸钇的制备及发光性能研究;詹钰成;《中国优秀硕士学位论文全文数据库 信息科技辑》;20150215(第2期);摘要，第9，24-41页 * |
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