CN103395980B - A kind of bismuth-containing White light-emitting glass and preparation method thereof - Google Patents
A kind of bismuth-containing White light-emitting glass and preparation method thereof Download PDFInfo
- Publication number
- CN103395980B CN103395980B CN201310300781.1A CN201310300781A CN103395980B CN 103395980 B CN103395980 B CN 103395980B CN 201310300781 A CN201310300781 A CN 201310300781A CN 103395980 B CN103395980 B CN 103395980B
- Authority
- CN
- China
- Prior art keywords
- white light
- glass
- bismuth
- containing white
- emitting glass
- 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.)
- Expired - Fee Related
Links
- 239000011521 glass Substances 0.000 title claims abstract description 113
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 85
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 38
- 229910052751 metal Inorganic materials 0.000 claims abstract description 24
- 239000002184 metal Substances 0.000 claims abstract description 24
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000000137 annealing Methods 0.000 claims abstract description 13
- -1 terbium peroxide Chemical class 0.000 claims description 23
- 239000006004 Quartz sand Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 11
- 239000004327 boric acid Substances 0.000 claims description 11
- 238000007493 shaping process Methods 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 1
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 19
- 238000002844 melting Methods 0.000 abstract description 13
- 230000008018 melting Effects 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 10
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000005284 excitation Effects 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 25
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- 239000000843 powder Substances 0.000 description 7
- 239000000146 host glass Substances 0.000 description 6
- 150000002910 rare earth metals Chemical class 0.000 description 6
- 230000032683 aging Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229920000647 polyepoxide Polymers 0.000 description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 150000003016 phosphoric acids Chemical class 0.000 description 2
- 239000002096 quantum dot Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000002241 glass-ceramic Substances 0.000 description 1
- 125000001475 halogen functional group Chemical group 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
Landscapes
- Glass Compositions (AREA)
Abstract
A kind of bismuth-containing White light-emitting glass and preparation method thereof, its by molar fraction by 1 ~ 10% SiO
2, 23 ~ 78.99% B
2o
3, 20 ~ 60% Bi
2o
3, 0 ~ 2% Sb
2o
3with 0.01 ~ 5% Tb
2o
3composition.Above-mentioned raw materials is mixed to get admixtion; Admixtion is added melting in crucible and obtain glass metal, pour glass metal into die forming, be then placed in annealing furnace and be incubated, then be down to room temperature, obtain bismuth-containing White light-emitting glass.Only containing a kind of rare earth ion in this glass, can effectively by ultraviolet excitation, the gold-tinted that the blue light sent by bismuth and terbium send is composited white light, can be used in manufacturing novel white-light LED component.The present invention carries out under air conditions, glass melting temperature is low, simple for process, cost is low, can produce the bismuth-containing White light-emitting glass of large volume, be suitable for suitability for industrialized production, and have considerable economic and social benefit, application prospect is very wide.
Description
Technical field
The invention belongs to Material Field, relate to a kind of bismuth-containing White light-emitting glass and preparation method thereof.
Background technology
Illumination links together with social civilization and progress always.The mankind experienced by incandescent light, subatmospheric gas lamp discharge lamp, HID high-intensity gas discharge lamp three generations illumination, LED is because its life-span is long, energy consumption is little, the features such as environmental sound are thrown light on by as forth generation, its development will have influence on energy strategy and the Environmental Protection Strategy of countries and regions, Chinese Government also greatly develops LED illumination industry, and starts " 12 " state plan semiconductor lighting plan of science and technology.Illumination be unable to do without luminescent material, and a lot of materials of occurring in nature all have luminescent properties.For solid material, it can be divided into inorganic and luminous organic material by composition.Compared to luminous organic material, phosphor has higher stability and ageing-resistant radioresistance.The Study and appliance of current phosphor is very deep, comprise rare-earth garnet, alkaline earth sulfide, alkali earth metal aluminate, phosphoric acid salt, borate, silicate, rare-earth oxide sulfate, rare earth oxide, oxynitride etc., wherein rare earth luminescent material is in consequence.Rare earth element is not filled due to 4f layer, and by 5s
25p
6screening of nucleus, therefore has abundant electronic level, and energy level transition passage reaches more than 20 ten thousand, can produce diversified radiation absorption and transmitting, forms luminescent material widely.In addition its photoluminescent band is narrow, and light absorpting ability is strong, and process based prediction model is stablized, high temperature resistant, can bear the effect of great-power electronic bundle, high-energy radiation and strong UV-light.
Since Japanese Nichina company manufactures first white light LEDs in 1996, substantial contribution, human and material resources research and development white light LEDs inject in national governments, enterprise.1997 Nian Ya companies take the lead in adopting GaN chip and fluorescent material to obtain white light, after this White light LED technology obtains develop rapidly, and current white light LEDs mainly contains blue-light LED chip cooperation yellow fluorescent powder, ultraviolet LED excites red, green, blue three-color phosphor and red, green, blue three kinds of chip portfolios these three kinds.Blue-light LED chip coordinates yellow fluorescent powder, and the blue light components that LED chip sends is absorbed by fluorescent material, and excitated fluorescent powder produces gold-tinted, the yellow light mix that another part blue light and fluorescent material send and obtain white light.The light that this process chip sends all is not absorbed by fluorescent material, efficiency is lower, in addition the blue light that produces of LED chip and after fluorescent material is compounded to form white light, also can exist some more than blue light, the skew of white light tone can be caused, also likely penetration phosphor hole and formed blue light reveal, eyesight is caused damage.Ultraviolet LED is adopted to excite red, green, blue three-color phosphor, produce red, green and blue three primary colours, white light can be formed by the mixing ratio adjusting three kinds of fluorescent material, the packaged type of this white light LEDs is identical with the first scheme, main employing epoxy resin mixes with fluorescent material, because fluorescent material causes the skew of white light tone in coating procedure because the control of thickness is uneven, even produce halo effect.And traditional technique adopts epoxy encapsulation fluorescent material, but the thermally-stabilised difference of epoxy resin, life-time service can be aging, affects the luminescent properties of fluorescent material.Adopt red LED, green LED and blue LED die or luminotron to be composited white light, this white light LEDs needs controller to control assorted LED, easily adjust color, but cost is higher.In addition the light emitting diode with quantum dots (QLED) produced due to the excellent properties of quantum dot, but also there is the problem of life-span short, homogeneity and scale operation in its development.
For the conventional fluorescent powder used relative to white light LEDs, glass has network structure, and rare earth ion is in a low voice in subenvironment, thus has excellent fluorescence quantum efficiency, and active ions in glass doping can be relatively high.Because glass is inorganic materials, compared to epoxy resin, have the longer life-span, and can not be aging under ultraviolet lighting, the light that chip sends can hypersorption and luminous, and being luminescent material, is again packaged material, eliminates coating processes.White light emitting glass have luminescence center evenly, the advantage such as Heat stability is good, easy-formation and processing.Since Zhang equals the white light emitting glass report of 1991, became study hotspot in recent years.Glass or the devitrified glass such as silicate, borate, phosphoric acid salt having prepared rare earth ion list and mixed or mix altogether are reported at present.Fluorescent glass preparation method has two kinds on the whole, and the first founds host glass, is ground into glass powder after castable or shrend, then mixes light-emitting phosphor material, Homogeneous phase mixing, again founds or sinter to obtain fluorescent glass.The second becomes to add fluorescent material or rare earth luminescence material in frit, then founds and obtain fluorescent glass.Patent CN101643315A discloses low-melting-point fluorescent glass for white light LED and preparation method thereof, prepares low melting glass, then mixed with fluorescent material by low melting glass under 1300 DEG C of reducing atmospheres, after sintering, obtain low-melting-point fluorescent glass.Two-step approach is adopted to increase the complicacy of technique and need atmosphere protection.Patent CN102584015A discloses White light-emitting glass and preparation method thereof, adopts multiple rare earth ion doped borosilicate glass, 1550 ~ 1600 DEG C of high temperature meltings under reducing atmosphere condition.Its rare earth ion species used is many, and glass melting temperature is high.Patent CN102060442A discloses white light LEDs fluorescent glass-ceramics preparation method, obtains devitrified glass, found, anneal at 1000 DEG C reducing atmosphere 1700 ~ 1900 DEG C after adopting high temperature melting through thermal treatment.Not only complex process and glass melting temperature is high.In sum, the life-span that fluorescent glass can overcome current LED is short, easily aging and encapsulation problem, Simplified flowsheet.But current fluorescent glass also exists that preparation process cost is high, usually need to adopt reducing atmosphere in melting process, temperature of fusion is high, needs multiple rare earth ion, and host glass absorbs energy and non-luminous problem.
Summary of the invention
The object of the invention is to overcome prior art shortcoming, bismuth-containing White light-emitting glass that a kind of glass melting temperature is low, Rare Earth Elements Determination adds and can found under air conditions and preparation method thereof is provided.
For achieving the above object, the technical solution used in the present invention is:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 1 ~ 10% SiO
2, 23 ~ 78.99% B
2o
3, 20 ~ 60% Bi
2o
3, 0 ~ 2% Sb
2o
3with 0.01 ~ 5% Tb
2o
3composition.
A preparation method for bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 1 ~ 10%
2, 23 ~ 78.99% B
2o
3, 20 ~ 60% Bi
2o
3, 0 ~ 2% Sb
2o
3with 0.01 ~ 5% Tb
2o
3mix, obtain admixtion;
2) admixtion is joined in the crucible of 900 ~ 1000 DEG C, and add a cover; Then be warming up to 1000 ~ 1100 DEG C and be incubated, obtaining glass metal;
3) glass metal is poured in mould, be first placed in annealing furnace after shaping and be incubated, then cool to room temperature with the furnace, obtain bismuth-containing White light-emitting glass.
B in described step 1)
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide.
In described step 1), the uniformity coefficient of admixtion is greater than 98%.
Described step 2) in heat-up rate be 5 ~ 15 DEG C/min.
Described step 2) in soaking time be 1 ~ 2h.
In described step 3), the temperature of annealing furnace is 400 ~ 600 DEG C.
2 ~ 3h is incubated in the lehr in described step 3).
Relative to prior art, beneficial effect of the present invention is:
Bismuth-containing White light-emitting glass provided by the invention is only containing a kind of rare earth ion, i.e. terbium ion, and this bismuth-containing White light-emitting glass can effectively by ultraviolet excitation, and the gold-tinted that the blue light sent by the bismuth in host glass and rare earth ion terbium send is composited white light.Rare earth ion is easily fixed in bismuth-containing White light-emitting glass, is conducive to device, and can make light source and the novel white-light LED component of different shape, have considerable economic and social benefit, application prospect is very wide.
The preparation method of bismuth-containing White light-emitting glass provided by the invention, bismuth-containing White light-emitting glass has been prepared by scorification melt raw material under air conditions, rare earth ion is distributed in bismuth-containing White light-emitting glass more even than existing phosphor material powder, the method glass melting temperature is 1000 ~ 1100 DEG C, and glass melting temperature is low; Add a cover to crucible in preparation process, reduce the volatilization of raw material.In addition, preparation method of the present invention is simple for process, cost is low, can produce the bismuth-containing White light-emitting glass of large volume, be suitable for suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the emmission spectrum of bismuth-containing White light-emitting glass prepared by embodiment 1;
Fig. 2 is the emmission spectrum of bismuth-containing White light-emitting glass prepared by embodiment 4.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.
The uniformity coefficient of By Means of Electrical Conductivity admixtion is adopted in the present invention, its principle is: using the content difference of the water-soluble salt in sample as the index of uniformity coefficient judging admixtion, then according in admixtion everywhere the difference of specific conductivity just can judge the uniformity coefficient of this admixtion.
Uniformity coefficient=[1-(electric conductivity maximum value-electric conductivity minimum value)/electric conductivity mean value] × 100%.
Embodiment 1:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 5% SiO
2, 70% B
2o
3, 22% Bi
2o
3, 1% Sb
2o
3with 2% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 5%
2, the B of 70%
2o
3, the Bi of 22%
2o
3, the Sb of 1%
2o
3with 2% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is added in the crucible of 950 DEG C, and add a cover; Then rise to 1100 DEG C with the temperature rise rate of 10 DEG C/min and be incubated 2h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 500 DEG C after shaping is incubated 3 hours, then cools to room temperature with the furnace, obtains the White light-emitting glass of bismuth-containing.
By the photoluminescence spectra of Hitachi Hitachi F-4600 spectrophotofluorometer bismuth-containing White light-emitting glass in 374nm place testing example 1, as shown in Figure 1, in collection of illustrative plates, highest peak appears at 545nm place, wherein X-coordinate is wavelength of transmitted light, and ordinate zou is relative luminous intensity (unit a.u. represents arbitrary unit).
Embodiment 2:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 5% SiO
2, 60% B
2o
3, 32.5% Bi
2o
3, 1% Sb
2o
3with 1.5% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 5%
2, 60% B
2o
3, 32.5% Bi
2o
3, 1% Sb
2o
3with 1.5% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 950 DEG C, and add a cover; Then rise to 1080 DEG C with the temperature rise rate of 10 DEG C/min and be incubated 2h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 500 DEG C after shaping is incubated 3 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Embodiment 3:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 5% SiO
2, 50% B
2o
3, 43% Bi
2o
3, 1% Sb
2o
3with 1% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 5%
2, 50% B
2o
3, 43% Bi
2o
3, 1% Sb
2o
3with 1% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 950 DEG C, and add a cover; Then rise to 1050 DEG C with the temperature rise rate of 13 DEG C/min and be incubated 2h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 550 DEG C after shaping is incubated 3 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Embodiment 4:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 5% SiO
2, 40% B
2o
3, 53.5% Bi
2o
3, 1% Sb
2o
3with 0.5% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 5%
2, 40% B
2o
3, 53.5% Bi
2o
3, 1% Sb
2o
3with 0.5% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 950 DEG C, and add a cover; Then rise to 1050 DEG C with the temperature rise rate of 10 DEG C/min and be incubated 1.5h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 500 DEG C after shaping is incubated 3 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Bismuth-containing White light-emitting glass in embodiment 4 can effectively by ultraviolet excitation, the gold-tinted that the blue light sent by the bismuth in host glass and rare earth ion terbium send is composited white light, as shown in Figure 2, in collection of illustrative plates, highest peak appears at 550nm place to its transmitting collection of illustrative plates at 374nm place.
Embodiment 5:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 3% SiO
2, 64.5% B
2o
3, 28% Bi
2o
3, 0.5% Sb
2o
3with 4% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 3%
2, 64.5% B
2o
3, 28% Bi
2o
3, 0.5% Sb
2o
3with 4% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 920 DEG C, and add a cover; Then rise to 1010 DEG C with the temperature rise rate of 6 DEG C/min and be incubated 1.2h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 450 DEG C after shaping is incubated 2.2 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Embodiment 6:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 8% SiO
2, 30% B
2o
3, 57.5% Bi
2o
3, 1.5% Sb
2o
3with 3% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 8%
2, 30% B
2o
3, 57.5% Bi
2o
3, 1.5% Sb
2o
3with 3% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 960 DEG C, and add a cover; Then rise to 1060 DEG C with the temperature rise rate of 12 DEG C/min and be incubated 1.4h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 480 DEG C after shaping is incubated 2.4 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Embodiment 7:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 10% SiO
2, 23% B
2o
3, 60% Bi
2o
3, 2% Sb
2o
3with 5% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 10%
2, 23% B
2o
3, 60% Bi
2o
3, 2% Sb
2o
3with 5% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 900 DEG C, and add a cover; Then rise to 1000 DEG C with the temperature rise rate of 8 DEG C/min and be incubated 1h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 400 DEG C after shaping is incubated 2 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Embodiment 8:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 1% SiO
2, 78.99% B
2o
3, 20% Bi
2o
3with 0.01% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 1%
2, 78.99% B
2o
3, 20% Bi
2o
3with 0.01% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 1000 DEG C, and add a cover; Then rise to 1100 DEG C with the temperature rise rate of 5 DEG C/min and be incubated 1.8h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 600 DEG C after shaping is incubated 2.5 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
Embodiment 9:
A kind of bismuth-containing White light-emitting glass, by molar fraction by 6% SiO
2, 42.7% B
2o
3, 50% Bi
2o
3, 1.2% Sb
2o
3with 0.1% Tb
2o
3composition.
The preparation method of bismuth-containing White light-emitting glass, comprises the following steps:
1) by molar fraction, by the SiO of 6%
2, 42.7% B
2o
3, 50% Bi
2o
3, 1.2% Sb
2o
3with 0.1% Tb
2o
3be mixed into the admixtion that uniformity coefficient is greater than 98%; Wherein B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide;
2) admixtion is joined in the crucible of 980 DEG C, and add a cover; Then rise to 1030 DEG C with the temperature rise rate of 15 DEG C/min and be incubated 1.6h, obtaining glass metal;
3) pour in mould by glass metal, the annealing furnace being first placed in 520 DEG C after shaping is incubated 2.7 hours, then cools to room temperature with the furnace, obtains bismuth-containing White light-emitting glass.
The present invention is melted in atmosphere by scorification and has been prepared bismuth-containing White light-emitting glass.Bismuth-containing White light-emitting glass glass melting temperature prepared by this technique is low, rare earth kind is few and host glass can be luminous.The melting technology of bismuth-containing White light-emitting glass of the present invention simply, is easily prepared, and is suitable for suitability for industrialized production, and the bismuth-containing White light-emitting glass prepared has the advantage such as low cost, large volume.The blue light that prepared white light glass can be sent by host glass under UV-irradiation and the gold-tinted that rare earth ion sends are composited white light.
Rare earth ion distributes more even than phosphor material powder in bismuth-containing White light-emitting glass, and material is easily fixed, and is conducive to device, can make light source and the novel white-light LED component of different shape.Therefore, bismuth-containing White light-emitting glass prepared by the present invention has considerable economic and social benefit, and application prospect is very wide.
Claims (5)
1. a preparation method for bismuth-containing White light-emitting glass, is characterized in that, comprises the following steps:
1) by molar fraction, by the SiO of 1 ~ 10%
2, the B of 23 ~ 78.99%
2o
3, the Bi of 20 ~ 60%
2o
3, the Sb of 0 ~ 2%
2o
3with 0.01 ~ 5% Tb
2o
3mix, obtain admixtion;
2) admixtion is joined in the crucible of 900 ~ 1000 DEG C, and add a cover; Then be warming up to 1000 ~ 1100 DEG C and be incubated 1 ~ 2h, obtaining glass metal;
3) glass metal is poured in mould, be first placed in annealing furnace after shaping at 400 ~ 600 DEG C of insulation 2 ~ 3h, then cool to room temperature with the furnace, obtain the White light-emitting glass of bismuth-containing.
2. the preparation method of bismuth-containing White light-emitting glass according to claim 1, is characterized in that: described step 1) middle B
2o
3introduced by boric acid, SiO
2introduced by quartz sand, Tb
2o
3introduced by terbium peroxide.
3. the preparation method of bismuth-containing White light-emitting glass according to claim 1 and 2, is characterized in that: described step 1) in the uniformity coefficient of admixtion be greater than 98%.
4. the preparation method of bismuth-containing White light-emitting glass according to claim 1, is characterized in that: described step 2) in heat-up rate be 5 ~ 15 DEG C/min.
5., according to the bismuth-containing White light-emitting glass that the preparation method of the bismuth-containing White light-emitting glass in claim 1-4 described in any one obtains, it is characterized in that: by molar fraction by 1 ~ 10% SiO
2, 23 ~ 78.99% B
2o
3, 20 ~ 60% Bi
2o
3, 0 ~ 2% Sb
2o
3with 0.01 ~ 5% Tb
2o
3composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310300781.1A CN103395980B (en) | 2013-07-17 | 2013-07-17 | A kind of bismuth-containing White light-emitting glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310300781.1A CN103395980B (en) | 2013-07-17 | 2013-07-17 | A kind of bismuth-containing White light-emitting glass and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103395980A CN103395980A (en) | 2013-11-20 |
| CN103395980B true CN103395980B (en) | 2015-07-29 |
Family
ID=49559775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310300781.1A Expired - Fee Related CN103395980B (en) | 2013-07-17 | 2013-07-17 | A kind of bismuth-containing White light-emitting glass and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103395980B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103755138B (en) * | 2013-12-17 | 2015-09-30 | 陕西科技大学 | A kind of dual-functional glass and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004019802A1 (en) * | 2004-03-11 | 2005-11-17 | Schott Ag | Glass for use as part of a light emitting diode, gas discharge lamp or neon lamp contains oxide-based trivalent rare earth cation |
| CN101318773A (en) * | 2008-07-04 | 2008-12-10 | 华东理工大学 | Pr3+doped high-density scintillation glass and preparation method thereof |
| CN102452793A (en) * | 2010-10-19 | 2012-05-16 | 同济大学 | High-luminous-intensity terbium-activated silicate glass and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11317561A (en) * | 1998-03-03 | 1999-11-16 | Asahi Glass Co Ltd | Light amplifying glass |
-
2013
- 2013-07-17 CN CN201310300781.1A patent/CN103395980B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004019802A1 (en) * | 2004-03-11 | 2005-11-17 | Schott Ag | Glass for use as part of a light emitting diode, gas discharge lamp or neon lamp contains oxide-based trivalent rare earth cation |
| CN101318773A (en) * | 2008-07-04 | 2008-12-10 | 华东理工大学 | Pr3+doped high-density scintillation glass and preparation method thereof |
| CN102452793A (en) * | 2010-10-19 | 2012-05-16 | 同济大学 | High-luminous-intensity terbium-activated silicate glass and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| Bi2O3-B2O3-SiO2玻璃的热性质;赵彦钊等;《陶瓷》;20050430;第17-22页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103395980A (en) | 2013-11-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Lin et al. | Glass ceramic phosphors: towards long‐lifetime high‐power white light‐emitting‐diode applications–a review | |
| CN103803797B (en) | A kind of LED fluorescent glass and preparation method thereof | |
| Zhong et al. | Garnet-based Li 6 CaLa 2 Sb 2 O 12: Eu 3+ red phosphors: a potential color-converting material for warm white light-emitting diodes | |
| CN102730975B (en) | Glass-ceramic and preparation method thereof | |
| CN101314519A (en) | Rare earth doping luminescent glass for white radiation LED and producing thereof | |
| CN103395997B (en) | A kind of white light LEDs rare earth doping transparent glass-ceramic and preparation method thereof | |
| CN105198224B (en) | YAG microcrystalline glass and preparation method and application thereof | |
| CN103936281B (en) | A kind of rare earth doped luminescent glass and preparation method thereof | |
| CN105523715A (en) | Low-melting point transparent fluorescent glass and its preparation method and use in white light LED | |
| Cao et al. | A WLED based on LuAG: Ce3+ PiG coated red-emitting K2SiF6: Mn4+ phosphor by screen-printing | |
| WO2010133025A1 (en) | Rare earth ion doped silicate luminescence glass and preparation method thereof | |
| CN102121591A (en) | White LED light source and manufacturing method of phosphor thereof | |
| CN108545931A (en) | A kind of tellurate fluorescent glass material of rare earth doped Eu3+ and preparation method thereof | |
| CN103043908A (en) | Novel fluorescent glass and preparation method thereof | |
| CN105236750A (en) | Rare earth-doped white-light fluorescent phosphate glass ceramics material and preparation method thereof | |
| KR20140106332A (en) | Rare earth ion added glass-phosphor composite and light emitting diode comprising the same | |
| CN103468264A (en) | Manufacture method of polycrystalline Ce:YAG fluorophor | |
| US9580650B1 (en) | Method of manufacturing Ce:YAG polycrystalline phosphor | |
| CN102906043B (en) | White light emitting glass-ceramic and production method thereof | |
| CN107814484B (en) | Europium ion self-reduction-capability-containing luminescent transparent glass and preparation method thereof | |
| Caldiño et al. | Rare earth doped glasses for displays and light generation | |
| US20120138854A1 (en) | Green luminescent glass for ultraviolet led and preparation method thereof | |
| CN102584015A (en) | White light-emitting glass and preparation method thereof | |
| CN103395980B (en) | A kind of bismuth-containing White light-emitting glass and preparation method thereof | |
| CN105347677B (en) | A kind of photic white light glass and its preparation technology |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150729 |