CN105271735A - High-silica glass capable of emitting red light and preparation method thereof - Google Patents
High-silica glass capable of emitting red light and preparation method thereof Download PDFInfo
- Publication number
- CN105271735A CN105271735A CN201510723890.3A CN201510723890A CN105271735A CN 105271735 A CN105271735 A CN 105271735A CN 201510723890 A CN201510723890 A CN 201510723890A CN 105271735 A CN105271735 A CN 105271735A
- Authority
- CN
- China
- Prior art keywords
- yvo
- under
- ultrasonic vibration
- phosphor
- nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 62
- 239000000203 mixture Substances 0.000 claims abstract description 61
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 48
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 66
- 238000003756 stirring Methods 0.000 claims description 56
- 239000000463 material Substances 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 47
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 38
- 238000013019 agitation Methods 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000012153 distilled water Substances 0.000 claims description 25
- 239000000377 silicon dioxide Substances 0.000 claims description 24
- 239000002244 precipitate Substances 0.000 claims description 22
- 239000006185 dispersion Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 18
- 229960004756 ethanol Drugs 0.000 claims description 16
- 238000009413 insulation Methods 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 11
- 239000000725 suspension Substances 0.000 claims description 11
- 238000007669 thermal treatment Methods 0.000 claims description 11
- 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000005245 sintering Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 229910009372 YVO4 Inorganic materials 0.000 abstract 2
- 239000005373 porous glass Substances 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 238000001831 conversion spectrum Methods 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 230000005284 excitation Effects 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 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
- 230000004927 fusion Effects 0.000 description 1
- 238000001033 granulometry Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011056 performance test Methods 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
- 238000001778 solid-state sintering Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Landscapes
- Luminescent Compositions (AREA)
Abstract
The invention discloses high-silica glass capable of emitting red light. The high-silica glass consists of porous glass and red fluorescence composition, wherein the red fluorescence composition accounts for 0.01-1% of the total mass of the porous glass; the red fluorescence composition is YVO4:Eu<3+>, Sr<2+>@YVO4:Eu<3+>, Bi<3+>@SiO2. The invention also discloses a preparation method of the high-silica glass capable of emitting the red light. The glass capable of emitting the red light has the effects of high light conversion efficiency, wide light conversion spectrum and high luminous intensity; the red fluorescence composition is high in dispersibility in the glass; the uniform luminescence of the glass can be achieved.
Description
Technical field
The present invention relates to a kind of high silica red light emitting glass and manufacture method thereof.
Background technology
At present, in fluorescent glass, the luminous efficiency of its light emitting ionic is far below crystalline material, and mainly because high-temperature fusion is prepared in glass process, easy spontaneous formation is trooped and produced concentration delustring.In prior art, have by sintered glass is immersed in rare earth ion, then carry out solid state sintering to form the fluorescent glass of good dispersity, but its wave band absorbed is limited, and luminous efficiency need to improve, limit its application.
Summary 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 manufacture method thereof, this red light emitting glass have turn optical efficiency high, turn light spectral width, effect that luminous intensity is high, and ruddiness fluorescent composition is uniformly distributed and better dispersed in red light emitting glass.
Technical problem to be solved by this invention is achieved by the following technical programs:
A kind of high silica red light emitting glass, it is characterized in that, be made up of sintered glass and ruddiness fluorescent composition, wherein, this ruddiness fluorescent composition accounts for 0.01 ~ 1% of sintered glass total mass, and described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
A manufacture method for high silica red light emitting glass, comprises the following steps: after sintered glass being immersed in ruddiness fluorescent composition dispersion soln, and under oxygen atmosphere, carry out 1100 DEG C of sintering 30 ~ 60min, furnace cooling obtains high silica red light emitting glass; This ruddiness fluorescent composition accounts for 0.01 ~ 1% of sintered glass total mass, and described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
The present invention has following beneficial effect: this red light emitting glass have turn optical efficiency high, turn light spectral width, effect that luminous intensity is high, particularly use two light-conversion fluorescent powder, better can absorb the spectrum of different-waveband, improve further and turn light spectrum; Simultaneously ruddiness fluorescent composition is uniformly distributed and better dispersed in red light emitting glass, is conducive to improving luminous intensity, reduces the possibility that cluster causes delustring further.
Accompanying drawing explanation
Fig. 1 represents the figure by the determination data of the size distribution of the different fluorescent material obtained, and wherein, 1-1 is the obtained YVO of step (three) of step one in embodiment 1
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+the particle size distribution data figure of nucleocapsid fluorescent material; 1-2 is the obtained YVO of step (four) of step one in embodiment 1
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2the particle size distribution data figure of ruddiness fluorescent composition; 1-3 is obtained NaYF
4: Yb
3+, Er
3+siO
2the particle size distribution data figure of nano-phosphor;
Fig. 2 represents the excitation spectrum of fluorescent glass 620nm supervisory wavelength that embodiment 1 to 6 and comparative example 1 to 3 obtain and the emmission spectrum of 365nm excitation wavelength; Wherein 2-1 to 2-9 represents the spectrogram corresponding to embodiment 1 to embodiment 6 and comparative example 1 to 3 respectively;
Fig. 3 represents obtained NaYF
4: Yb
3+, Er
3+siO
2nano-phosphor is at the emmission spectrum of 980nm excitation wavelength.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail.
Embodiment 1
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: the ruddiness fluorescent composition of 100 parts of sintered glasses and 0.25 part, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
A manufacture method for high silica red light emitting glass, specifically comprises the steps:
One, ruddiness fluorescent composition is prepared
(1) YVO is prepared
4: Eu
3+, Sr
2+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) by above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir), dropwise instillation contains the Y (NO of the certain proportioning of 1.5mmol below
3)
36H
2o, Eu (NO
3)
3, Sr (NO
3)
2(0.9:0.03:0.07) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200
oinsulation reaction 1h under C, is down to 150
oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y of median size 10 ~ 15nm
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor; (5) to Y
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h(and is rapidly heated, and heat-treats under preferably fluorescent material being in this annealing temperature when temperature reaches 500 DEG C again), the Y of median size 20 ~ 30nm after acquisition thermal treatment
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor.
(2) YVO is prepared
4: Eu
3+, Bi
3+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) limit is dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol
3)
36H
2o, Eu (NO
3)
3, Bi (NO
3)
3(0.87:0.03:0.1) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180
oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y that median size is about 10nm
0.87vO
4: Eu
3+ 0.03, Bi
3+ 0.1nano-phosphor.
(3) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 0.1g
4: Eu
3+, Sr
2+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained solution A; Take 0.008gYVO
4: Eu
3+, Bi
3+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (80KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 15min, obtained solution B; (2) limit ultrasonic agitation (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) solution A, limit dropwise instills solution B; Continue ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the YVO of median size 40 ~ 60nm
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material, its size distribution is as shown in the 1-1 in Fig. 1.
(4) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition
(1) nucleocapsid fluorescent material ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution C; Add a certain proportion of (4:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2nucleocapsid fluorescent material; (2) this is coated with SiO
2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain median size 70 ~ 100nm ruddiness fluorescent composition, its size distribution is as shown in the 1-2 in Fig. 1.
Two, in proportion ruddiness fluorescent composition is placed in ethanolic soln, ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained dispersion soln D; Sintered glass is immersed in 30min in above-mentioned dispersion soln A in proportion, continues ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 25min again; With washed with de-ionized water several, remove the excessive powder be not adsorbed on sintered glass; Under oxygen atmosphere, carry out 1100 DEG C of sintering 30 ~ 60min, furnace cooling obtains high silica red light emitting glass.
Embodiment 2
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: the ruddiness fluorescent composition of 100 parts of sintered glasses and 0.01 part, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.This red light emitting glass manufacture method is with embodiment 1.
Embodiment 3
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: the ruddiness fluorescent composition of 100 parts of sintered glasses and 1 part, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.This red light emitting glass manufacture method is with embodiment 1.
Embodiment 4
On basis based on embodiment 1, by the YVO of the step (three) in step one
4: Eu
3+, Sr
2+with YVO
4: Eu
3+, Bi
3+weight ratio change 1:0.5 into, all the other are identical with embodiment 1.
Embodiment 5
On basis based on embodiment 1, by the YVO of the step (three) in step one
4: Eu
3+, Sr
2+with YVO
4: Eu
3+, Bi
3+weight ratio change 1:0.001 into, all the other are identical with embodiment 1.
Embodiment 6
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: the ruddiness fluorescent composition of 100 parts of sintered glasses and 0.25 part, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
A manufacture method for high silica red light emitting glass, specifically comprises the steps:
One, ruddiness fluorescent composition is prepared
(1) YVO is prepared
4: Eu
3+, Sr
2+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) by above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir), dropwise instillation contains the Y (NO of the certain proportioning of 1.5mmol below
3)
36H
2o, Eu (NO
3)
3, Sr (NO
3)
2(0.9:0.03:0.07) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200
oinsulation reaction 1h under C, is down to 150
oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y of median size 10 ~ 15nm
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor; (5) to Y
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h(and is rapidly heated, and heat-treats under preferably fluorescent material being in this annealing temperature when temperature reaches 500 DEG C again), the Y of median size 20 ~ 30nm after acquisition thermal treatment
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor.
(2) YVO is prepared
4: Bi
3+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) limit is dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol
3)
36H
2o, Bi (NO
3)
3(0.87:0.1) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180
oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y that median size is about 10nm
0.87vO
4: Bi
3+ 0.1nano-phosphor.
(3) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Bi
3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 0.1g
4: Eu
3+, Sr
2+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained solution A; Take 0.008gYVO
4: Bi
3+nano-phosphor is placed in 10ml ethanol, and carries out ultrasonic agitation (80KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 15min, obtained solution B1; (2) limit ultrasonic agitation (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) solution A, limit dropwise instills solution B 1; Continue ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the YVO of median size 40 ~ 60nm
4: Eu
3+, Sr
2+yVO
4: Bi
3+nucleocapsid fluorescent material.
(4) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material
(1) by 0.05mmolEu (NO
3)
36H
2o ultrasonic disperse in 15ml ethanol solution, by YVO obtained for step 3
4: Eu
3+, Sr
2+yVO
4: Bi
3+nucleocapsid fluorescent material presoma is dispersed in above-mentioned solution; (2) (60KHz ultrasonic vibration and 500r/min centrifugal speed stir) after ultrasonic agitation 60min, reaction soln is left standstill 24h, ion exchange process is fully carried out.Wherein, Eu (NO
3)
36H
2the amount of O is according to chemical formula Y
(0.9-x)vO
4: Eu
3+ (x), Bi
3+ (0.1)determine, preferably excessive a little.After reaction terminates, centrifugal, and obtain white precipitate 3 times with dehydrated alcohol and distilled water wash.Finally, 90
ounder C, dry 5h, obtains YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material.
(5) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition
(1) nucleocapsid fluorescent material ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution C; Add a certain proportion of (4:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2nucleocapsid fluorescent material; (2) this is coated with SiO
2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain median size 70 ~ 100nm ruddiness fluorescent composition.
Two, in proportion ruddiness fluorescent composition is placed in ethanolic soln, ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained dispersion soln D; Sintered glass is immersed in 30min in above-mentioned dispersion soln D in proportion, continues ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 25min again; With washed with de-ionized water several, remove the excessive powder be not adsorbed on sintered glass; Under oxygen atmosphere, carry out 1100 DEG C of sintering 30 ~ 60min, furnace cooling obtains high silica red light emitting glass.
Embodiment 7
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: 100 parts of sintered glasses, the ruddiness fluorescent composition of 0.25 part and 0.2 part of NaYF
4: Yb
3+, Er
3+fluorescent material, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
Embodiment 8
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: 100 parts of sintered glasses, the ruddiness fluorescent composition of 0.25 part and 0.01 part of NaYF
4: Yb
3+, Er
3+fluorescent material, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
Embodiment 9
A kind of high silica red light emitting glass, is made up of the raw material of following weight part: 100 parts of sintered glasses, the ruddiness fluorescent composition of 0.25 part and 1 part of NaYF
4: Yb
3+, Er
3+fluorescent material, described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
The manufacture method of the high silica red light emitting glass of embodiment 7 to 9, specifically comprises the steps:
One, as the preparation method of step one in embodiment 1 obtains ruddiness fluorescent composition;
Two, NaYF is prepared
4: Yb
3+, Er
3+siO
2the method of fluorescent material is as follows:
(1) 1.8mmolY (NO is taken
3)
36H
2o, 0.17mmolYb (NO
3)
35H
2o, 0.1mmolEr (NO
3)
35H
2o, with 2mmolNaNO
3mixing is also fully dissolved in 15ml ethylene glycol and forms solution E; By 8mmolNH
4f is fully dissolved in 15ml ethylene glycol and forms solution F; Ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) solution E, F30min respectively, at continuation ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 30min after two solution mixing; Mixing solutions is poured in polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180
oinsulation reaction 12h under C, is down to 150
oinsulation reaction 4h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with distilled water and dehydrated alcohol clean successively 3 times obtain fluorescent material; This is deposited in 80
odry 5h under C, obtains the NaYF of median size 30 ~ 60nm
4: Yb
3+, Er
3+nano-phosphor;
(2) by above-mentioned for 0.3g obtained nano NaY F
4: Yb
3+, Er
3+phosphor powder ultrasonic agitation 30min(100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) be scattered in 40ml dehydrated alcohol and 10ml distilled water; Be that the ammoniacal liquor of 28% and the tetraethoxy TEOS of 0.3ml add in above-mentioned dispersion soln by 2ml massfraction, at 20 DEG C, fully stir 4h, obtained NaYF
4: Yb
3+, Er
3+siO
2-powder; Carry out centrifugal and obtain white precipitate 3 times with distilled water and washes of absolute alcohol; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2naYF
4: Yb
3+, Er
3+nucleocapsid fluorescent material; By this NaYF
4: Yb
3+, Er
3+siO
2nucleocapsid fluorescent material carries out 800 DEG C of thermal treatment 60min under being placed in argon gas atmosphere, obtains the NaYF of median size 55 ~ 85nm
4: Yb
3+, Er
3+siO
2-nano-phosphor, its particle size determination 1-3 as shown in Figure 1, it launches corresponding characteristic peak under 980nm excitation wavelength, is particularly positioned at the highest peak of 655nm, as shown in Figure 3.
Three, in proportion ruddiness fluorescent composition is placed in ethanolic soln, ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained dispersion soln D; In proportion by NaYF
4: Yb
3+, Er
3+siO
2-nano-phosphor is placed in ethanolic soln, ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) dispersion 30min, obtained dispersion soln G; In proportion half and half sintered glass is immersed in 30min in above-mentioned dispersion soln D, G, continues ultrasonic agitation (50KHz ultrasonic vibration and 100r/min centrifugal speed stir) 5min and leave standstill 25min again; With washed with de-ionized water several, remove the excessive powder be not adsorbed on sintered glass; Mix two kinds of sintered glasses, under oxygen atmosphere, carry out 1100 DEG C of sintering 30 ~ 60min, furnace cooling obtains high silica red light emitting glass.
Comparative example 1
The difference of the present embodiment and embodiment 1 is: the preparation method of ruddiness fluorescent composition, and all the other are identical with embodiment 1.The preparation method of the ruddiness fluorescent composition of the present embodiment is as follows:
(1) YVO is prepared
4: Eu
3+, Sr
2+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) by above-mentioned solution limit ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir), dropwise instillation contains the Y (NO of the certain proportioning of 1.5mmol below
3)
36H
2o, Eu (NO
3)
3, Sr (NO
3)
2(0.9:0.03:0.07) in 8ml ethylene glycol solution, then ultrasonic agitation (80KHz ultrasonic vibration and 300r/min centrifugal speed stir) 10min clarifies to solution, adds 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200
oinsulation reaction 1h under C, is down to 150
oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y of median size 10 ~ 20nm
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor; (5) to Y
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h(and is rapidly heated, and heat-treats under preferably fluorescent material being in this annealing temperature when temperature reaches 500 DEG C again), the Y of median size 20 ~ 30nm after acquisition thermal treatment
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor.
(2) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material
By the Y obtained by the first step
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07fluorescent material (1.6mmol) is dispersed in 10ml ethylene glycol solution, and according to R value (nucleocapsid mol ratio, i.e. R=YVO
4: Eu
3+, Ba
2+/ YVO
4: Eu
3+, Bi
3+) calculate, by the Y (NO of certain molar weight
3)
36H
2o, Eu (NO
3)
3, Bi (NO
3)
35H
2o(mol ratio is 0.87:0.03:0.1) add in above-mentioned solution, and ultrasonic vibration 20min; (2) 1.2mmolNa
3vO
412H
2o adds in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water, dropwise instills in (1) gained solution while stirring, add 20ml distilled water after stirring 5min after dissolving completely; (3) gained reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml (compactedness 70%), 200
ounder C, isothermal holding 2h, after reaction terminates, cools to room temperature with the furnace.Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) finally this is deposited in 80
ounder C, dry 8h, obtains YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nano-phosphor.
(3) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition
(1) nucleocapsid fluorescent material ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution E; Add a certain proportion of (4:1) water and ammoniacal liquor afterwards, the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2nucleocapsid fluorescent material; (2) this is coated with SiO
2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain ruddiness fluorescent composition.
Comparative example 2
The difference of the present embodiment and embodiment 1 is: the preparation method of ruddiness fluorescent composition, and all the other are identical with embodiment 1.The preparation method of the ruddiness fluorescent composition of the present embodiment is as follows: on the basis based on embodiment 1, removes step (three), and in step (four), by heat treated for 1g YVO
4: Eu
3+, Sr
2+nano-phosphor and 0.05gYVO
4: Eu
3+, Bi
3+nano-phosphor mixing ultrasonic agitation (100KHz ultrasonic vibration and 1000r/min centrifugal speed stir) is scattered in ethanol, obtained solution E; Remaining preparation process is identical with embodiment 1.
Comparative example 3
The present embodiment difference from Example 1 is: the ruddiness fluorescent composition adopted is the YVO that ordinary method obtains
4: Eu
3+nano-phosphor; Remaining identical with embodiment 1.
Performance test analysis:
By YVO obtained for embodiment 1
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+carry out XRD diffraction, bragg peak positions all in diffractogram, relative intensity all with YVO
4standard card (JCPDS17-0341) is consistent, can be characterized by pure Tetragonal YVO
4crystalline structure, does not find other assorted peaks.
Average granulometry: the dispersion liquid obtained with ultrasonic homogenizer process, use laser diffraction formula particle size distribution device (Shimadzu Seisakusho Ltd.'s system " SALD-7000 ") to measure median size, result as shown in Figure 1.
Red light emitting glass obtained by embodiment 1 to 6 and comparative example 1 to 3 is carried out PL spectrum to measure, result as shown in Figure 2, as can be seen from Figure 2, comparative example 1 ruddiness fluorescent composition absorbs with certain broadening, the band edge of absorption band is to long wavelength's red shift, but it is not very strong in the absorption of the ultraviolet region of short wavelength; Comparative example 2 ruddiness fluorescent composition compares ratio the last 1 in the absorption in short UV light district; Comparative example 3 dominant absorption short UV light district, and its phototranstormation efficiency is not high; Embodiment 1 to 6 ruddiness fluorescent composition absorption band has certain broadening, not only the band edge of absorption band is to long wavelength's red shift, in short UV light district, also there is good absorption at it simultaneously, particularly embodiment 5, absorbing comparatively other embodiments at ultraviolet region absorbs the strongest, is also the strongest equally at the emission peak of 620nm wavelength.Using 365nm as excitation wavelength, the glass of embodiment 1,4,5,6 and comparative example 1,2 all can see that homogeneity sends ruddiness, and embodiment 2,3 due to add ruddiness fluorescent composition too much or very few, cause the problem of its non-uniform light.
The above embodiment only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (4)
1. a high silica red light emitting glass, is characterized in that, is made up of sintered glass and ruddiness fluorescent composition, and wherein, this ruddiness fluorescent composition accounts for 0.01 ~ 1% of sintered glass total mass, and described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
2. a manufacture method for high silica red light emitting glass, comprises the following steps: after sintered glass being immersed in ruddiness fluorescent composition dispersion soln, and under oxygen atmosphere, carry out 1100 DEG C of sintering 30 ~ 60min, furnace cooling obtains high silica red light emitting glass; This ruddiness fluorescent composition accounts for 0.01 ~ 1% of sintered glass total mass, and described ruddiness fluorescent composition is YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2.
3. the manufacture method of high silica red light emitting glass according to claim 2, is characterized in that, described YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition is obtained by following methods:
(1) YVO is prepared
4: Eu
3+, Sr
2+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed are stirred below the dropwise Y (NO of instillation containing the certain proportioning of 1.5mmol
3)
36H
2o, Eu (NO
3)
3, Sr (NO
3)
28ml ethylene glycol solution in, more simultaneously 80KHz ultrasonic vibration and 300r/min centrifugal speed stir 5 ~ 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200
oinsulation reaction 1h under C, is down to 150
oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
ounder C, dry 5h, obtains Y
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor; (5) to Y
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h, and after acquisition thermal treatment, median size is 20 ~ 30nmY
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor;
(2) YVO is prepared
4: Eu
3+, Bi
3+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stirring limit are dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol
3)
36H
2o, Eu (NO
3)
3, Bi (NO
3)
38ml ethylene glycol solution in, more simultaneously 80KHz ultrasonic vibration and 300r/min centrifugal speed stir 5 ~ 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180
oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtaining median size is 10nmY
0.87vO
4: Eu
3+ 0.03, Bi
3+ 0.1nano-phosphor;
(3) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 1g
4: Eu
3+, Sr
2+nano-phosphor is placed in 10ml ethanol, and disperses 30min, obtained solution A under carrying out 100KHz ultrasonic vibration and the stirring of 1000r/min centrifugal speed; Take 0.05gYVO
4: Eu
3+, Bi
3+nano-phosphor is placed in 10ml ethanol, and disperses 15min, obtained solution B under carrying out 80KHz ultrasonic vibration and the stirring of 1000r/min centrifugal speed; (2) limit 60KHz ultrasonic vibration and 500r/min centrifugal speed stirred solution A, limit dropwise instills solution B; Continue 50KHz ultrasonic vibration and 100r/min centrifugal speed to stir 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtaining median size is 40 ~ 60nmYVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material;
(4) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition
(1) nucleocapsid fluorescent material is scattered in ethanol under 100KHz ultrasonic vibration and 1000r/min centrifugal speed stir, obtained solution C; Additional proportion is water and the ammoniacal liquor of 4:1 afterwards, and the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2nucleocapsid fluorescent material; (2) this is coated with SiO
2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain ruddiness fluorescent composition.
4. the manufacture method of high silica red light emitting glass according to claim 2, is characterized in that, described YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition is obtained by following methods:
(1) YVO is prepared
4: Eu
3+, Sr
2+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min are dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol below
3)
36H
2o, Eu (NO
3)
3, Sr (NO
3)
28ml ethylene glycol solution in, then 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stir 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 200
oinsulation reaction 1h under C, is down to 150
oinsulation reaction 1h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y of median size 10 ~ 15nm
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor; (5) to Y
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor carries out 500 DEG C of vacuum heat treatment 1h, the Y of median size 20 ~ 30nm after acquisition thermal treatment
0.9vO
4: Eu
3+ 0.03, Sr
2+ 0.07nano-phosphor;
(2) YVO is prepared
4: Bi
3+nano-phosphor
(1) by 1.2mmolNa
3vO
412H
2o is dissolved in the mixing solutions containing 5ml ethylene glycol and 2ml distilled water; (2) above-mentioned solution limit 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stirring limit are dropwise instilled the Y (NO containing the certain proportioning of 1.5mmol
3)
36H
2o, Bi (NO
3)
38ml ethylene glycol solution in, then 80 ~ 100KHz ultrasonic vibration and 300r/min centrifugal speed stir 10min and clarify to solution, add 20ml distilled water; (3) reaction soln is poured in the polytetrafluoroethyllining lining autoclave that volume is 50ml, under vacuum conditions, 180
oinsulation reaction 1.5h under C, after reaction terminates, is cooled to room temperature; Gained suspension is poured out, centrifugal and with acetone clean 3 times obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the Y that median size is about 10nm
0.87vO
4: Bi
3+ 0.1nano-phosphor;
(3) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Bi
3+nucleocapsid fluorescent material
(1) pre-dispersed: to take the heat treated YVO of 0.1g
4: Eu
3+, Sr
2+nano-phosphor is placed in 10ml ethanol, and carries out 100KHz ultrasonic vibration and 1000r/min centrifugal speed dispersed with stirring 30min, obtained solution A; Take 0.008gYVO
4: Bi
3+nano-phosphor is placed in 10ml ethanol, and carries out 80KHz ultrasonic vibration and 1000r/min centrifugal speed dispersed with stirring 15min, obtained solution B1; (2) limit 60KHz ultrasonic vibration and 500r/min centrifugal speed stirred solution A, limit dropwise instills solution B 1; Continue ultrasonic agitation 50KHz ultrasonic vibration and 100r/min centrifugal speed to stir 5min and leave standstill 5min again, centrifugal and clean 3 times with acetone and obtain white precipitates; (4) this is deposited in 90
odry 5h under C, obtains the YVO of median size 40 ~ 60nm
4: Eu
3+, Sr
2+yVO
4: Bi
3+nucleocapsid fluorescent material;
(4) YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material
(1) by 0.05mmolEu (NO
3)
36H
2o ultrasonic disperse in 15ml ethanol solution, by YVO obtained for step 3
4: Eu
3+, Sr
2+yVO
4: Bi
3+nucleocapsid fluorescent material presoma is dispersed in above-mentioned solution; (2), after 60KHz ultrasonic vibration and 500r/min centrifugal speed stir 60min, reaction soln is left standstill 24h; After reaction terminates, centrifugal, and obtain white precipitate 3 times with dehydrated alcohol and distilled water wash; 90
ounder C, dry 5h, obtains YVO
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+nucleocapsid fluorescent material;
Five, YVO is prepared
4: Eu
3+, Sr
2+yVO
4: Eu
3+, Bi
3+siO
2ruddiness fluorescent composition
(1) by nucleocapsid fluorescent material 100KHz ultrasonic vibration and 1000r/min centrifugal speed dispersed with stirring in ethanol, obtained solution C; Additional proportion is water and the ammoniacal liquor of 4:1 afterwards, and the mass ratio adding tetraethoxy and nucleocapsid fluorescent material after stirring is 1.5:1, and adjust ph is 9, and temperature of reaction is 20 DEG C, reacts 5 hours; Carry out centrifugal and clean 3 acquisition white precipitates with acetone; This is deposited in 90
odry 5h under C, to obtain being coated with SiO
2nucleocapsid fluorescent material; (2) this is coated with SiO
2nucleocapsid fluorescent material be placed in argon gas atmosphere under carry out 800 DEG C of thermal treatment 1h, obtain ruddiness fluorescent composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510723890.3A CN105271735B (en) | 2015-10-29 | 2015-10-29 | A kind of high silica red light emitting glass and its manufacture method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510723890.3A CN105271735B (en) | 2015-10-29 | 2015-10-29 | A kind of high silica red light emitting glass and its manufacture method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105271735A true CN105271735A (en) | 2016-01-27 |
| CN105271735B CN105271735B (en) | 2017-12-26 |
Family
ID=55141660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510723890.3A Active CN105271735B (en) | 2015-10-29 | 2015-10-29 | A kind of high silica red light emitting glass and its manufacture method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105271735B (en) |
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 |
|---|
| 刘利娜等: "YVO4:Eu3+@SiO2核壳结构纳米复合材料的合成与表征", 《发光学报》 * |
| 詹钰成: "铕离子掺杂纳米钒酸钇的制备及发光性能研究", 《中国优秀硕士学位论文全文数据库 信息科技辑》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105271735B (en) | 2017-12-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9156733B2 (en) | Rare earth ions doped alkali metal silicate luminescent glass and the preparation method thereof | |
| JP7255940B2 (en) | Infrared selective nano-functional composition for radiative cooling and method of making same | |
| CN110229348A (en) | A kind of Er with blue up-conversion3+/Tm3+- MOFs fluorescent material and preparation method thereof | |
| CN106753371A (en) | A kind of holmium ytterbium codope bismuth tungstate fluorescent material and preparation method thereof | |
| CN104710982B (en) | A kind of aluminosilicate novel green light fluorescent powder of rare earth ion codope and preparation method thereof | |
| CN102191060A (en) | Vanadate phosphor and preparation method thereof | |
| Tao et al. | Effect of Al3+ on the photoluminescence and radioluminescence properties of Mn2+-Doped high silica glass | |
| CN101456570A (en) | Method for preparing cerium doped yttrium aluminum garnet | |
| CN105238284A (en) | A kind of EVA film | |
| CN101037797A (en) | Erbium ytterbium boracic acid gadolinium strontium doped laser crystal and preparation method and usage thereof | |
| Zhou et al. | Effect of surfactants on morphology and luminescent properties of Ca3 (VO4) 2: Bi, Eu3+ red phosphors | |
| Xia et al. | Sol-gel method for preparing a novel red-emitting phosphor YVO4: Sm3+, Eu3+ with ideal red color emission | |
| CN102604635B (en) | Zirconium-phosphate-based luminescent material, preparation method thereof, and application thereof | |
| CN102559175B (en) | Sr2SiO4:XEu<2+> fluorescent powder and preparation method thereof | |
| CN105271735A (en) | High-silica glass capable of emitting red light and preparation method thereof | |
| CN102869749B (en) | Borate based red light emitting material and preparation method thereof | |
| CN105271729A (en) | Red light emitting glass and manufacturing method for red light emitting glass | |
| CN1962811A (en) | Fluorescent powder for white light LED and method for production thereof | |
| CN102888218A (en) | A kind of preparation method of M3Si6O12N2:xRe system green phosphor | |
| CN102492420A (en) | Cesium aluminosilicate phosphor and preparation method thereof | |
| CN105368448A (en) | Alkaline earth metal silicate yellow-orange fluorescent powder and preparation method therefor and application thereof | |
| CN101898873B (en) | Preparation method of green fluorescent glass doped with rare earth ions | |
| CN107267148A (en) | A kind of terbium ion doping zirconic acid lanthanum fluorescent material and preparation method thereof | |
| CN105295918A (en) | Red fluorescent composition and EVA adhesive film | |
| CN105238302A (en) | EVA film used in solar cell packaging |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20231127 Address after: 528300, No.13C Industrial Avenue, Xintang Village, Lunjiao Street, Shunde District, Foshan City, Guangdong Province (Residence Declaration) Patentee after: Foshan Shunde District Senxuyang Intelligent Technology Co.,Ltd. Address before: 528518 No. 112 Mingcheng Second Road, Gaoming District, Foshan City, Guangdong Province Patentee before: Yan Meixia |