CN102092951A - Transparent glass ceramic material for ultraviolet excited white LED and preparation technique thereof - Google Patents
Transparent glass ceramic material for ultraviolet excited white LED and preparation technique thereof Download PDFInfo
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- CN102092951A CN102092951A CN2009101129451A CN200910112945A CN102092951A CN 102092951 A CN102092951 A CN 102092951A CN 2009101129451 A CN2009101129451 A CN 2009101129451A CN 200910112945 A CN200910112945 A CN 200910112945A CN 102092951 A CN102092951 A CN 102092951A
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Abstract
The invention discloses a transparent glass ceramic material for an ultraviolet excited white light emitting diode (LED) and a preparation technique thereof. The glass ceramic comprises the following components: 40 to 60mol% of SiO2, 10 to 30mol% of Al2O3, 5 to 25mol% of CeF3, 0 to 15mol% of NaF, 0 to 15mol% of LiF, 0.01 to 5mol% of ReF3, less than 0.5% of MSO4 and less than 0.02% of Fe. Re represents rare-earth ions (such as Eu, Tb, Dy or the like); M represents Mg or Ca or Ba or Sr; and the content of the NaF and the content of the LiF are not 0 at the same time. The preparation technique for the glass ceramic comprises two steps of melt quenching preparation of precursor glass and subsequent crystallization treatment of the precursor glass. By changing rare-earth doping, the glass ceramic can generate intense multi-color (comprising white color) tunable light emission under the excitation of ultraviolet, and is expected to be developed and applied to a novel white LED device excited by an ultraviolet chip.
Description
Technical field
The present invention relates to the solid luminescent material field, especially relate to and a kind ofly can under the ultraviolet excitation condition, realize polychrome (comprising white light) tunable luminous rare earth doping transparent glass-ceramic and technology of preparing thereof.
Technical background
In recent years, white light emitting diode (LED) head light with unique advantage such as energy-conservation, durable causes people's very big concern.At present, substitute traditional incandescent light and luminescent lamp with white light LEDs and become a kind of trend gradually.Common commercial white light LEDs is by blue light GaN chip and mixes Ce at present
3+Yttrium aluminum garnet (YAG) fluorescent material be packaged together and make, fluorescent material is mixed in the Resins, epoxy and is coated on the chip.The blue light part that the GaN led chip sends is absorbed by fluorescent material, make it be excited to send gold-tinted, and the yellow light mix that unabsorbed blue light and fluorescent material send just obtains white light.Because the luminescent lifetime of blue chip and YAG fluorescent material is different, after use for some time, the luminous of LED can produce aberration.In order to address this problem, can make white light LEDs by the mode that adopts the UV-light chip to apply special fluorescent material.At this moment, what chip sent can not UV-light seen by the naked eye be absorbed by fluorescent material fully, makes fluorescent material stimulated emission blue light and gold-tinted (or red, green, blue three coloured light), obtains white light after the mixing.Adopt this technology can avoid producing aberration substantially, but, will be shortened the work-ing life of white light LED part because wearing out can appear under the UV-light long-term irradiation in Resins, epoxy.The novel solid luminescent material of intense white light and ultraviolet resistance irradiation (structure, stable performance) is launched in research and development under ultraviolet excitation, be up-to-date direction [Y.Zheng, A.G.Clare, the Phys.Chem.Glasses. that develops the white light LEDs technology in the world, 46,467 (2005)].
Rear-earth-doped transparent oxyfluoride glass ceramic takes place partially-crystallized by unorganic glass attitude material and gets, and its constitutional features is that specific fluoride nano crystal evenly is embedded in the glass basis.As a class novel solid luminescent material, it combines the advantage of crystal of fluoride and glass material, can have close with crystal even better optical property, and have be similar to that the glass material technology of preparing is simple, thermostability and the high advantage of chemical stability.The transparent glass ceramics of launching intense white light under ultraviolet excitation can be processed into tabular and directly overlay on the chip, therefore, is expected to be used for substituting conventional fluorescent material and makes up novel white-light LED device.Compare with conventional LED device, this new device will have the remarkable advantage of photochromic stable, long service life.
The present invention relates to the fluorinated cerium (CeF of rare earth ion doping
3) nanocrystalline transparent glass ceramics and technology of preparing thereof.The present invention is containing CeF
3Mix rare earth ion as luminescence center in the nanocrystalline glass-ceramic, by control CeF
3Crystallization condition, make rare earth ion enter CeF
3In nanocrystalline.Select CeF
3Reason as the rare-earth luminescent center matrix is Ce
3+The 4f-5d transition that ion exists eelctric dipole to allow at ultraviolet region, thereby UV-light had very strong absorption cross.In addition, Ce
3+Thereby the UV-light transmission ofenergy that ion is easy to absorb produces VISIBLE LIGHT EMISSION efficiently for other rare earth ion.Test result shows, the Ce in the glass-ceramic of the present invention
3+Ion by ultraviolet excitation after, transmission ofenergy given be enriched in CeF
3Rare earth ion in nanocrystalline, polychrome (comprising white light) is tunable luminous efficiently thereby produce.
Summary of the invention
The present invention proposes a kind of rear-earth-doped CeF that contains
3The component of nano crystal transparent glass ceramic and preparation technology thereof, purpose are to prepare and are expected the solid luminescent material that is applied to novel white-light LED device, has the tunable characteristics of luminescence of polychrome.
The component and the molar content of transparent glass ceramics of the present invention are as follows:
SiO
2：40-60mol％；Al
2O
3：10-30mol％；CeF
3：5-25mol％；NaF：0-15mol％；LiF：0-15mol％；ReF
3：0.01-5mol％；MSO
4：＜0.5％；Fe：＜0.02％。Wherein, Re represents rare earth ion (as Eu, Tb, Dy etc.), and M represents Mg or Ca or Ba or Sr; NaF and LiF content are not 0 simultaneously.This glass-ceramic has following micro-structural feature: the CeF of uniform distribution hexagonal structure in glass basis
3Nanocrystalline, crystal particle scale is the 10-15 nanometer, and the Doped Rare Earth ion gathers partially in CeF
3In nanocrystalline.
Glass-ceramic of the present invention adopts melt supercooled method and subsequent heat treatment preparation.
The crystallization that melt supercooled method that the present invention adopts and subsequent heat treatment comprise forerunner's glass preparation and forerunner's glass is handled two steps.In the crystallization process of described forerunner's glass, thermal treatment temp is 600 ℃-720 ℃.
Rear-earth-doped by changing, glass-ceramic of the present invention can produce intensive polychrome (comprising white light) under ultraviolet excitation tunable luminous.
Glass-ceramic preparation technology of the present invention is simple, with low cost, and nontoxic pollution-free has good calorifics and chemical stability, is expected Application and Development in making up the novel white-light LED device that the ultraviolet chip excites.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of example 1 glass-ceramic;
Fig. 2 is the high resolution transmission electron microscopy bright field image of example 1 glass-ceramic;
Fig. 3 is the exciting light spectrogram of example 1 glass-ceramic corresponding to the emission of 407 nanometers;
Fig. 4 is the fluorescence spectrum figure of example 1 glass-ceramic under 335 nano wave lengths excite;
Fig. 5 is the exciting light spectrograms of example 2 glass-ceramic corresponding to the emission of 591 nanometers;
Fig. 6 is the fluorescence spectrum figures of example 2 glass-ceramic under 394 nano wave lengths excite;
Fig. 7 is the exciting light spectrograms of example 3 glass-ceramic corresponding to the emission of 543 nanometers;
Fig. 8 is the fluorescence spectrum figures of example 3 glass-ceramic under 335 nano wave lengths excite;
Fig. 9 is the exciting light spectrograms of example 4 glass-ceramic corresponding to the emission of 578 nanometers;
Figure 10 is the fluorescence spectrum figures of example 4 glass-ceramic under 335 nano wave lengths excite.
Embodiment
Various powder raw materials are compared weighing according to certain set of dispense, in agate mortar, mix and grind and be placed in the crucible, put into and be incubated 1～12 hour after resistance furnace is heated to 1300～1700 ℃ and make it fusion, then, glass melt is taken out and pouring into fast be shaped in the copper mold and obtain block forerunner's glass; The forerunner's glass that obtains is put into resistance furnace annealing to eliminate internal stress.Glass is carried out differential thermal analysis, record its glass transition temp and first crystallization temperature.Selected temperature is carried out 1～10 hour isothermal thermal treatment to above-mentioned glass between the glass transition temp and first crystallization temperature, makes it to take place partially-crystallized, obtains transparent glass ceramics.
The crucible that uses in the preparation process can be platinum crucible or corundum crucible.
Adopt above material component and preparation technology, can obtain in the oxide glass matrix, evenly to inlay CeF
3Nanocrystalline transparent glass ceramics.Electronic spectrum and spectroscopic analysis result show that the Doped Rare Earth ion enters in the nanometer crystalline phase.According to different rear-earth-doped situations, glass ceramic material produces the emission of intensive polychromatic light respectively under ultraviolet excitation.
Example 1: with analytically pure SiO
2, Al
2O
3, NaF and CeF
3Powder is pressed 50SiO
2: 25Al
2O
3: 15NaF: 10CeF
3The accurate weighing of the proportioning of (mol ratio) is placed in the agate mortar, make it uniform mixing more than grinding half an hour, then put into platinum crucible, in program control high temperature box type resistance furnace, be heated to 1400 ℃ after insulation 3 hours, then, glass melt is poured in the copper mold fast be shaped; The forerunner's glass that obtains is put into resistance furnace, 530 ℃ of annealing after 2 hours furnace cooling to eliminate internal stress.According to the differential thermal analysis result, the glass after the annealing 650 ℃ of insulations 2 hours, is obtained dun transparent glass ceramics.X-ray diffraction result (as shown in Figure 1) shows the CeF that separates out hexagonal structure in glass basis
3Crystalline phase; Transmission electron microscope observation (as shown in Figure 2) shows, is of a size of the CeF of 10-15 nanometer in this glass-ceramic in a large number
3Uniform crystal particles is distributed in the glass basis.
Sample is measured its room temperature with the FLS920 fluorescence spectrophotometer and is excited and emission spectrum through surface finish.At monitoring Ce
3+On the excitation spectrum of ion 407 nanometers emission, detect corresponding to Ce
3+: the excitation band (as shown in Figure 3) of the ultraviolet band of 4f → 5d transition (225-385 nanometer).On the emission spectrum that 335 nanometers excite, occur corresponding to Ce
3+: the strong blue emission of 5d → 4f transition (centre wavelength is 407nm) (as shown in Figure 4).
Example 2: with analytically pure SiO
2, Al
2O
3, LiF, CeF
3With purity be 99.99% EuF
3Powder is pressed 0.1EuF
3: 50SiO
2: 25Al
2O
3: 9.9LiF: 15CeF
3The accurate weighing of the proportioning of (mol ratio) is placed in the agate mortar, make it uniform mixing more than grinding half an hour, then put into platinum crucible, in program control high temperature box type resistance furnace, be heated to 1350 ℃ after insulation 6 hours, then, glass melt is poured in the copper mold fast be shaped; The forerunner's glass that obtains is put into resistance furnace, 500 ℃ of annealing after 2 hours furnace cooling to eliminate internal stress; According to the differential thermal analysis result, the glass after the annealing 600 ℃ of insulations 2 hours, is obtained dun transparent glass ceramics.The X-ray diffraction result shows the CeF that separates out hexagonal structure in glass basis
3Crystalline phase; Transmission electron microscope observation shows, is of a size of the CeF of 10-15 nanometer in this glass-ceramic in a large number
3Uniform crystal particles is distributed in the glass basis; Electronic spectrum and spectroscopic analysis show rare earth ion Eu
3+Gather in CeF partially
3In the nanocrystal.
Sample is measured its room temperature with the FLS920 fluorescence spectrophotometer and is excited and emission spectrum through surface finish.At monitoring Eu
3+On the excitation spectrum of ion 591 nanometers emission, detect corresponding to Eu
3+: the excitation band (as shown in Figure 5) of the ultraviolet-visible wave band of 4f → 4f transition (350-480 nanometer); On the emission spectrum that 394 nanometers excite, occur corresponding to Eu
3+: the emission peak (as shown in Figure 6) of 4f → 4f transition, visual inspection glass-ceramic sample sends bright ruddiness.
Example 3: with analytically pure SiO
2, Al
2O
3, NaF, CeF
3With purity be 99.99% TbF
3Powder is pressed 0.5TbF
3: 55SiO
2: 25Al
2O
3: 12.5NaF: 7CeF
3The accurate weighing of the proportioning of (mol ratio) is placed in the agate mortar, make it uniform mixing more than grinding half an hour, then put into platinum crucible, in program control high temperature box type resistance furnace, be heated to 1500 ℃ after insulation 6 hours, then, glass melt is poured in the copper mold fast be shaped; The forerunner's glass that obtains is put into resistance furnace, 550 ℃ of annealing after 2 hours furnace cooling to eliminate internal stress; According to the differential thermal analysis result, the glass after the annealing 670 ℃ of insulations 2 hours, is obtained dun transparent glass ceramics.The X-ray diffraction result shows the CeF that separates out hexagonal structure in glass basis
3Crystalline phase; Transmission electron microscope observation shows, is of a size of the CeF of 10-15 nanometer in this glass-ceramic in a large number
3Uniform crystal particles is distributed in the glass basis; Electronic spectrum and spectroscopic analysis show rare earth ion Tb
3+Gather in CeF partially
3In the nanocrystal.
Sample is measured its room temperature with the FLS920 fluorescence spectrophotometer and is excited and emission spectrum through surface finish.At monitoring Tb
3+On the excitation spectrum of ion 543 nanometers emission, detect corresponding to Ce
3+: 4f → 5d transition and Tb
3+: the excitation band (as shown in Figure 7) of the ultraviolet-visible wave band of 4f → 4f transition (225～500 nanometer) shows to have Ce in glass-ceramic
3+Ion is to Tb
3+The ionic useful energy transmits; On the emission spectrum that 335 nanometers excite, occur corresponding to Tb
3+: the emission peak (as shown in Figure 8) of 4f → 4f transition, visual inspection glass-ceramic sample sends bright green glow.
Can improve Ce by optimizing rear-earth-doped concentration
3+Ion is to Tb
3+Energy of ions transfer efficiency, thereby the green emission of reinforcing glass pottery.Experimental result shows, along with Tb
3+Doping content is increased to 2.0mol% from 0.1mol%, Ce
3+Ion is dull decline in the luminous intensity and the life-span of 407 nanometers, and Tb
3+Ionic green luminescence intensity is then dull to be increased, and shows Ce
3+To Tb
3+Energy transfer efficiency increase gradually.This system highest energy transfer efficiency can reach 80%.
Example 4: with analytically pure SiO
2, Al
2O
3, NaF, CeF
3With purity be 99.99% DyF
3Powder is pressed 1.0DyF
3: 44SiO
2: 28Al
2O
3: 16NaF: 11CeF
3The accurate weighing of the proportioning of (mol ratio) is placed in the agate mortar, make it uniform mixing more than grinding half an hour, then put into platinum crucible, in program control high temperature box type resistance furnace, be heated to 1400 ℃ after insulation 1 hour, then, glass melt is poured in the copper mold fast be shaped; The forerunner's glass that obtains is put into resistance furnace, 550 ℃ of annealing after 2 hours furnace cooling to eliminate internal stress; According to the differential thermal analysis result, the glass after the annealing 650 ℃ of insulations 4 hours, is obtained dun transparent glass ceramics.The X-ray diffraction result shows the CeF that separates out hexagonal structure in glass basis
3Crystalline phase; Transmission electron microscope observation shows, is of a size of the CeF of 10-15 nanometer in this glass-ceramic in a large number
3Uniform crystal particles is distributed in the glass basis; Electronic spectrum and spectroscopic analysis show rare earth ion Dy
3+Gather in CeF partially
3In the nanocrystal.
Sample is measured its room temperature with the FLS920 fluorescence spectrophotometer and is excited and emission spectrum through surface finish.At monitoring Dy
3+On the excitation spectrum of ion 578 nanometers emission, detect corresponding to Ce
3+: 4f → 5d transition and Dy
3+: the excitation band (as shown in Figure 9) of the ultraviolet-visible wave band of 4f → 4f transition (225-500 nanometer) shows to have Ce in glass-ceramic
3+Ion is to Dy
3+The ionic useful energy transmits; On the emission spectrum that 335 nanometers excite, occur corresponding to Dy
3+: the emission peak (as shown in figure 10) of 4f → 4f transition, visual inspection glass-ceramic sample sends bright white light.The glow color of glass-ceramic sample is represented with 1931-CIE tristimulus coordinates figure calculation result shows that its chromaticity coordinate value is CIE-X=0.348, CIE-Y=0.366 is very approaching with the equal-energy white launch coordinate of standard.
Can improve Ce by optimizing rear-earth-doped concentration
3+Ion is to Dy
3+Energy of ions transfer efficiency, thereby the white light emission of reinforcing glass pottery.Experimental result shows, along with Dy
3+Doping content is increased to 2.0mol% from 0.1mol%, Ce
3+Ion is dull decline in the luminous intensity and the life-span of 407 nanometers, and Dy
3+Ionic white-light emitting intensity is then dull to be increased, and shows Ce
3+To Dy
3+Energy transfer efficiency increase gradually.This system highest energy transfer efficiency can reach 85%.
Claims (3)
1. a class can realize comprising the tunable luminous rare earth doping transparent glass-ceramic of polychrome of white light under the ultraviolet excitation condition, and its component is SiO
2: 40-60mol%, Al
2O
3: 10-30mol%, CeF
3: 5-25mol%, NaF:0-15mol%, LiF:0-15mol%, ReF
3: 0.01-5mol%, MSO
4:＜0.5%, Fe:＜0.02%; Wherein, Re represents rare earth ion Eu, Tb or Dy, and M represents Mg, Ca, Ba, Sr; NaF and LiF content are not 0 simultaneously; This glass-ceramic has following micro-structural feature: the CeF of uniform distribution hexagonal structure in glass basis
3Nanocrystalline, crystal particle scale is the 10-15 nanometer, and the Doped Rare Earth ion aggregation is in CeF
3In nanocrystalline.
2. the preparation method of transparent glass ceramics as claimed in claim 1 comprises the steps:
(1) forerunner's glass melt quench preparation;
(2) crystallization and thermal treatment of forerunner's glass.
3. the preparation method of transparent glass ceramics as claimed in claim 2, it is characterized in that: in the crystallization process of described forerunner's glass, thermal treatment temp is 600 ℃-720 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491642A (en) * | 2011-12-06 | 2012-06-13 | 中国科学院福建物质结构研究所 | Up-conversion white light emission glass ceramic and preparation method thereof |
| CN104163572A (en) * | 2014-07-15 | 2014-11-26 | 南昌大学 | Transparent glass ceramic having high efficiency white light emission and preparation method thereof |
| CN104703939A (en) * | 2012-06-29 | 2015-06-10 | 康宁股份有限公司 | Glass-ceramic substrates for semiconductor processing |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092282A (en) * | 2007-06-19 | 2007-12-26 | 浙江大学 | Glassceramic in applying to semiconductor illumination, and preparation method |
| CN101209900A (en) * | 2006-12-27 | 2008-07-02 | 中国科学院福建物质结构研究所 | Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof |
-
2009
- 2009-12-11 CN CN2009101129451A patent/CN102092951A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101209900A (en) * | 2006-12-27 | 2008-07-02 | 中国科学院福建物质结构研究所 | Neodymium-doped yttrium-fluoride nanocrystalline transparent glass ceramic with high stimulated emission cross section and preparation thereof |
| CN101092282A (en) * | 2007-06-19 | 2007-12-26 | 浙江大学 | Glassceramic in applying to semiconductor illumination, and preparation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491642A (en) * | 2011-12-06 | 2012-06-13 | 中国科学院福建物质结构研究所 | Up-conversion white light emission glass ceramic and preparation method thereof |
| CN104703939A (en) * | 2012-06-29 | 2015-06-10 | 康宁股份有限公司 | Glass-ceramic substrates for semiconductor processing |
| CN104163572A (en) * | 2014-07-15 | 2014-11-26 | 南昌大学 | Transparent glass ceramic having high efficiency white light emission and preparation method thereof |
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Application publication date: 20110615 |