CN102464450A - Green energy-saving fluorescent powder/glass composite luminescent material and preparation method thereof - Google Patents
Green energy-saving fluorescent powder/glass composite luminescent material and preparation method thereof Download PDFInfo
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- CN102464450A CN102464450A CN2011101829390A CN201110182939A CN102464450A CN 102464450 A CN102464450 A CN 102464450A CN 2011101829390 A CN2011101829390 A CN 2011101829390A CN 201110182939 A CN201110182939 A CN 201110182939A CN 102464450 A CN102464450 A CN 102464450A
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- 239000011521 glass Substances 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 57
- 239000000843 powder Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000004134 energy conservation Methods 0.000 claims abstract description 21
- 238000002844 melting Methods 0.000 claims abstract description 13
- 230000008018 melting Effects 0.000 claims abstract description 13
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 9
- 239000010452 phosphate Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000005365 phosphate glass Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 230000002688 persistence Effects 0.000 claims description 13
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 229910052749 magnesium Inorganic materials 0.000 claims description 2
- 229910052714 tellurium Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 229910000029 sodium carbonate Inorganic materials 0.000 claims 1
- 235000017550 sodium carbonate Nutrition 0.000 claims 1
- 239000011787 zinc oxide Substances 0.000 claims 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims 1
- 229960001763 zinc sulfate Drugs 0.000 claims 1
- 229910000368 zinc sulfate Inorganic materials 0.000 claims 1
- 238000000137 annealing Methods 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 229910003668 SrAl Inorganic materials 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000146 host glass Substances 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 150000002910 rare earth metals Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 150000004645 aluminates Chemical class 0.000 description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 2
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a green energy-saving fluorescent powder/glass composite luminescent material and a preparation method thereof. The long-afterglow luminescent glass synthesized by mixing and melting long-afterglow fluorescent powder and phosphate glass powder has the characteristics of no lead, no radioactivity, low melting point, energy conservation, weather resistance, low-temperature forming, stable luminescence, long afterglow and the like. The preparation method comprises the steps of preparing low-melting-point phosphate matrix glass, (b) grinding the matrix glass into powder, mixing the powder with a certain mass fraction of long-afterglow fluorescent powder, (c) briquetting the powder, and (d) melting, annealing and cooling the powder block at a certain temperature. The composite luminescent material emits light with certain color after being irradiated by visible light or ultraviolet light, and the luminescent performance of the long afterglow fluorescent powder is maintained. The fluorescent powder/glass composite luminescent material is used as a novel material and has wide application in the fields of building, energy conservation, aviation, emergency lighting, night display, artistic handicraft and the like.
Description
Technical field
The invention belongs to luminescent material, relate in particular to a kind of green energy conservation fluorescent material/glass composite luminescent material and preparation method thereof.
Background technology
Long after glow luminous material has long afterglow property, and it after can absorbing the energy of sunshine or light stores portion of energy, discharges the energy of storage with the form of visible light lentamente then.Utilize this characteristic to can be used as the lighting source at night and dark place, have important use to be worth in fields such as building, traffic and national defence.For example, as the sign at night of the vitals of exit emergency, hazardous location, fire escape and the factory of buildings, indicative illumination at night and cove lighting such as take aim at the simple and easy night of the panel board of fighter, firearms.In addition, make luminescent fibre and various luminous artistic articles, also have broad application prospects in fields such as industrial art.Utilize the characteristics of luminescence of long persistence luminescent powder and high thermal stability, chemicalstability, the transparency, the weathering resistance of glass, form composite luminescent material with high-performance thereby can combine them.
CN1305967A provides a kind of method of manufacture of rare earth yellow-green colour long-afterglow luminescent glass; This method selective oxidation strontium, aluminium sesquioxide, boron trioxide are glass matrix; Add solubility promoter and rare earth doped; After ground and mixed was even, constant temperature was treated to rare earth yellow-green colour long-afterglow luminescent glass, but only is confined to aluminate system glass.
One Chinese patent application CN1235935A provides a kind of high brightness luminous glass and method of manufacture thereof; Its fluorescent glass consists of (wt%): long afterglow luminescent powder of alkaline earth aluminate 10～30%; Glass powder 70～90%, its method of manufacture are after mixing, under 650～900 ℃ of temperature, to burn till high brightness luminous glass.It is complicated that this patent exists the host glass component, and the fluorescent material doping is high, and glass melting temperature is high, the problem of production cost height and complex process.
CN1397509A provides a kind of method of manufacture of long-afterglow luminescent glass; Its topmost characteristics are after in conventional silicate glass moulding process, mixing long after glow luminous material or glass powder with low melting point and long after glow luminous material thorough mixing, to become long-afterglow luminescent glass 700～1100 ℃ of heat-treated.The method of manufacture of this long-afterglow luminescent glass makes the commercialization of long-afterglow luminescent glass that very big development arranged, but still has certain limitation.
The present invention studies a kind of green energy conservation fluorescent material/glass composite luminescent material.This advanced luminescent material preparation technology is simple; Characteristics such as unleaded, "dead", weathering resistance, lower melting point, energy-conservation, low temperature moulding, luminous stable and steady persistence; To promoting the new energy development and the energy-conservation cause of China; Reduce and pollute, realize that the strategy of sustainable development of national economy has great importance.
Summary of the invention
It is high to the purpose of this invention is to provide a kind of luminous efficiency, stable performance, being easy to green energy conservation fluorescent material/glass composite luminescent material of moulding and preparation method thereof, the host glass of selecting for use is unleaded lower melting point phosphate glass.This green energy conservation fluorescent material/glass composite luminescent material has characteristics such as unleaded, "dead", weathering resistance, lower melting point, energy-conservation, low temperature moulding, luminous stable and steady persistence, under UV-light or radiation of visible light, launches long-after-glow light.
In order to carry out above-mentioned purpose; The technical scheme that the present invention adopts is: a kind of green energy conservation fluorescent material/glass composite luminescent material is characterized in that this composite luminescent material is prepared from the phosphate glass of massfraction 60～99.5% and 0.5～40% long persistence luminescent powder.The general formula of phosphate glass is (mol%): P
2O
5-ZnO-SO
3-Na
2O-SnO-M
xO
y
Wherein M is Mg, Ca, Sr, Ba, Ti, Te, one or more elements among Zr or the Sb.
Above-mentioned green energy conservation fluorescent material/glass composite luminescent material and preparation method thereof is characterized in that comprising following steps:
(1) phosphate matrix glass is prepared burden and batch mixing, found after mixing.200～400 ℃ of preheatings 1～5 hour, glass melting temperature was 500～900 ℃ before founding.
(2) glass grinding is become glass powder, and mix with certain mass fractional long persistence luminescent powder.With the powder compact that mixes.
(3) the powder block that suppresses is founded.Glass melting temperature is 400～800 ℃.The cooling of annealing at last promptly makes green energy conservation fluorescent material/glass composite luminescent material.
The glass transformation temperature Tg of resulting green energy conservation fluorescent material/glass composite luminescent material is 200～400 ℃.
The invention has the beneficial effects as follows: because the phosphate matrix glass of being selected for use has low glass transformation temperature Tg, and the not leaded heavy metal that waits, pollution-free so it is simple to have preparation technology, low temperature moulding, characteristics such as green energy conservation.Long persistence luminescent powder is mixed in the phosphate matrix glass powder; Through it is founded processing; Long-afterglow fluorescent pruinescence host glass is coated, thereby obtain the designability of high transparent, chemicalstability, thermostability, weathering resistance, uniqueness, the composite luminescent material of good performances such as workability with good long-persistence luminous performance of long persistence luminescent powder and phosphate matrix glass.Green energy conservation fluorescent material of the present invention/glass composite luminescent material can be launched long-after-glow light under the exciting of visible light or UV-light.Adopt this green energy conservation fluorescent material/glass composite luminescent material preparation method to promoting the new energy development and the energy-conservation cause of China, reduce and pollute, realize that the strategy of sustainable development of national economy has great importance.
Description of drawings
Fig. 1 is the phosphate matrix glass DSC curve of embodiment 1;
Fig. 2 is the SrAl of embodiment 1
2O
4: Eu
2+, Dy
3+The composite luminescent material emmission spectrum of long persistence luminescent powder and fluorescent material identical in quality such as being mixed with.
Embodiment
Embodiment 1
Glass host material is selected 29P for use
2O
5-42ZnO-9SO
3-18Na
2The phosphate glass of O-2SnO (mol%), this glass have to hang down founds characteristics such as temperature and softening temperature, and the DSC curve is as shown in Figure 1.Abrasive dust is to the 200-300 order behind the glass smelting.
Fluorescent material adopts commercially available SrAl
2O
4: Eu
2+, Dy
3+Long persistence luminescent powder.Fluorescent material and glass powder mass ratio 5: 95.
Above-mentioned materials is mixed the back depress to the powder block, found the back 320 ℃ of annealing, cool to room temperature afterwards with the furnace, promptly get embodiment 1 sample at 700 ℃ at hydropress pressure.Under the 365nm ultra violet lamp, matrix material is launched strong yellow green light, has long afterglow property, the long persistence luminescent powder luminous intensity basically identical of its luminous intensity and equal in quality.Fig. 2 is SrAl
2O
4: Eu
2+, Dy
3+Long persistence luminescent powder (solid line among Fig. 2) and the emmission spectrum of composite luminescent material (dotted line among Fig. 2) under the 365nm wavelength excites of fluorescent material identical in quality such as be mixed with, emmission spectrum shows that both luminescence spectrums are consistent
This preparation method has realized low temperature moulding property, stability of photoluminescence and the weathering resistance of this fluorescent material/glass composite luminescent material in addition.
Claims (7)
1. green energy conservation fluorescent material/glass composite luminescent material and preparation method thereof is characterized in that this composite luminescent material is prepared from the phosphate glass of massfraction 60～99.5% and 0.5～40% long persistence luminescent powder.The general formula of phosphate glass is (mo1%): P
2O
5-ZnO-SO
3-Na
2O-SnO-M
xO
y
Wherein: M is Mg, Ca, Sr, Ba, Ti, Te, one or more elements among Zr or the Sb.
2. the preparation method of green energy conservation fluorescent material according to claim 1/glass composite luminescent material is characterized in that may further comprise the steps:
(1) preparation lower melting point phosphate matrix glass;
(2) above-mentioned glass grinding is become glass powder, and with certain mass fractional long persistence luminescent powder uniform mixing after carry out powder compact;
(3) with the powder block that the suppresses cooling of founding and anneal.
3. green energy conservation fluorescent material according to claim 2/glass composite luminescent material is characterized in that the main raw material of phosphate matrix glass derives from ammonium di-hydrogen phosphate, zinc oxide, zinc sulfate, yellow soda ash.Auxiliary material derives from oxide compound and alkaline earth carbonate.
4. preparation process according to claim 2, the glass melting temperature that it is characterized in that phosphate matrix glass is 500～900 ℃.
5. preparation process according to claim 2 is characterized in that fluorescent material and particle size of glass powder are 1～100 μ m.
6. preparation process according to claim 2, the mixed powder that it is characterized in that glass powder and fluorescent material is at hydropress pressure lower lock block.
7. preparation process according to claim 2, the glass melting temperature that it is characterized in that composite luminescent material is 400～800 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101829390A CN102464450A (en) | 2011-07-01 | 2011-07-01 | Green energy-saving fluorescent powder/glass composite luminescent material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101829390A CN102464450A (en) | 2011-07-01 | 2011-07-01 | Green energy-saving fluorescent powder/glass composite luminescent material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102464450A true CN102464450A (en) | 2012-05-23 |
Family
ID=46068617
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|---|---|---|---|
| CN2011101829390A Pending CN102464450A (en) | 2011-07-01 | 2011-07-01 | Green energy-saving fluorescent powder/glass composite luminescent material and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104193346A (en) * | 2014-08-21 | 2014-12-10 | 厦门百嘉祥微晶材料科技股份有限公司 | Semitransparent fluorescent powder/glass composite luminescent ceramic wafer and preparation method thereof |
| CN105070816A (en) * | 2015-07-20 | 2015-11-18 | 佛山市南海区联合广东新光源产业创新中心 | LED fluorescent film powder slurry |
| KR20170106997A (en) * | 2015-08-28 | 2017-09-22 | 코아 가라스 가부시키가이샤 | Manufacturing method of glass-coated phosphorescent material and glass-coated phosphorescent material |
| CN107686243A (en) * | 2017-08-01 | 2018-02-13 | 北京科技大学 | A kind of preparation method of low-melting-point fluorescent glass |
| WO2018058935A1 (en) * | 2016-09-29 | 2018-04-05 | 华南农业大学 | Luminescent glass ceramic and preparation method therefor and use thereof in led illumination device |
| CN109574506A (en) * | 2018-12-20 | 2019-04-05 | 温州大学 | A kind of CsPb1-xTixBr3Quantum dot devitrified glass and preparation method thereof |
| CN109721250A (en) * | 2016-12-01 | 2019-05-07 | 天津理工大学 | The method for preparing luminescent glass ceramic with glass powder with low melting point |
| CN110005170A (en) * | 2019-04-16 | 2019-07-12 | 武汉永信美绿建新技术有限公司 | A kind of light emitting-type cement base grinding stone terrace system and its construction technology |
| CN110156326A (en) * | 2018-02-11 | 2019-08-23 | 天津理工大学 | Fluorescent glass ceramics based on glass powder with low melting point and preparation method thereof |
| CN110510871A (en) * | 2019-08-30 | 2019-11-29 | 华南农业大学 | The double emission glass ceramics of red blue light turn optical device and preparation method and Horticultural light lamp |
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| CN101696085A (en) * | 2009-09-27 | 2010-04-21 | 南通大学 | Yttrium aluminum garnet fluorescent glass, manufacturing method thereof and use thereof |
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| Title |
|---|
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| 王蕊等: "SrAl2O4:Eu2+，Dy3+长余辉发光玻璃的研制", 《沈阳化工学院学报》, vol. 22, no. 2, 30 June 2008 (2008-06-30), pages 137 - 140 * |
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| CN104193346A (en) * | 2014-08-21 | 2014-12-10 | 厦门百嘉祥微晶材料科技股份有限公司 | Semitransparent fluorescent powder/glass composite luminescent ceramic wafer and preparation method thereof |
| CN105070816A (en) * | 2015-07-20 | 2015-11-18 | 佛山市南海区联合广东新光源产业创新中心 | LED fluorescent film powder slurry |
| CN105070816B (en) * | 2015-07-20 | 2018-05-15 | 佛山市南海区联合广东新光源产业创新中心 | A kind of LED fluorescent powder film slurries |
| JPWO2017038687A1 (en) * | 2015-08-28 | 2018-06-14 | 興亜硝子株式会社 | Glass-coated phosphorescent material and method for producing glass-coated phosphorescent material |
| TWI610902B (en) * | 2015-08-28 | 2018-01-11 | 興亞玻璃股份有限公司 | Glass-covered photoluminescent material and method for producing glass-covered photoluminescent material |
| US20180037811A1 (en) * | 2015-08-28 | 2018-02-08 | Koa Glass Co., Ltd. | Glass-coated light-accumulating material and method for producing glass-coated light-accumulating material |
| KR102010313B1 (en) * | 2015-08-28 | 2019-08-13 | 코아 가라스 가부시키가이샤 | Method for producing glass-covered photoluminescent material and glass-covered photoluminescent material |
| CN107207326A (en) * | 2015-08-28 | 2017-09-26 | 兴亚硝子株式会社 | Glass is coated to light-storing material and glass is coated to the manufacture method of light-storing material |
| KR20170106997A (en) * | 2015-08-28 | 2017-09-22 | 코아 가라스 가부시키가이샤 | Manufacturing method of glass-coated phosphorescent material and glass-coated phosphorescent material |
| EP3284729A4 (en) * | 2015-08-28 | 2018-12-19 | Koa Glass Co. Ltd. | Glass-coated light-accumulating material and method for producing glass-coated light-accumulating material |
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| CN109721250A (en) * | 2016-12-01 | 2019-05-07 | 天津理工大学 | The method for preparing luminescent glass ceramic with glass powder with low melting point |
| CN109721250B (en) * | 2016-12-01 | 2021-11-26 | 天津理工大学 | Method for preparing luminescent glass ceramic by using low-melting-point glass powder |
| CN107686243A (en) * | 2017-08-01 | 2018-02-13 | 北京科技大学 | A kind of preparation method of low-melting-point fluorescent glass |
| CN107686243B (en) * | 2017-08-01 | 2020-04-10 | 北京科技大学 | Preparation method of low-melting-point fluorescent glass |
| CN110156326A (en) * | 2018-02-11 | 2019-08-23 | 天津理工大学 | Fluorescent glass ceramics based on glass powder with low melting point and preparation method thereof |
| CN110156326B (en) * | 2018-02-11 | 2021-11-26 | 天津理工大学 | Fluorescent glass ceramic based on low-melting-point glass powder and preparation method thereof |
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Application publication date: 20120523 |