CN104003619B - A kind of white light LEDs cerium activated yttrium aluminium garnet devitrified glass and preparation method thereof - Google Patents
A kind of white light LEDs cerium activated yttrium aluminium garnet devitrified glass and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of white light LEDs cerium activated yttrium aluminium garnet devitrified glass, described devitrified glass is doped with YAG at low softening point glass material: Ce3+Fluorescent material；Wherein, described YAG: Ce3+Fluorescent material doping mass ratio in described devitrified glass is 1 ~ 80%, and described low softening point glass material is softening point at the glass material of 300 ~ 800 DEG C.The present invention discloses the preparation method of described devitrified glass, comprise the following steps: weigh glass matrix raw material and softening point regulator, uniformly mix, add heat fusing；Then by YAG: Ce3+Fluorescent material joins in the glass of described molten state, uniformly mixes, and then cooling solidify to form glass；Gained glass is annealed 6 ~ 48 hours, prepares white light LEDs cerium activated yttrium aluminium garnet devitrified glass.
Description
Technical field
The present invention relates to white light LEDs devitrified glass, specifically a kind of white light LEDs cerium activated yttrium aluminium garnet devitrified glass and preparation method thereof.
Background technology
Since the sixties in last century is born, LED illumination technology improves 30 times, speed development as " the sea hereby law " of prices 10 times with brightness in every 10 years, and its theoretical light efficiency is up to 260
lm/W.It is reported, the laboratory data of white light LEDs light efficiency is more than 100
Lm/W, and the large power white light LED entering commercial field also reaches 40
lm/W.Along with the breakthrough of key technology, the light efficiency of following great power LED still has a biggest rising space, the highest likely reaches 150～200 lm/W.
Compared with white light LEDs, the electric filament lamp of general lighting and halogen tungsten lamp, its light efficiency is 12～24 lm/W；The light efficiency of fluorescent lamp and HID lamp (xenon lamp) is 50～120 lm/W.For white light LEDs, in 1998, the light efficiency of white light LEDs only had 5 lm/W, had reached 15 lm/W by 1999, and this index is close with general domestic electric filament lamp, and when 2000, the light efficiency of white light LEDs reached 25 lumens/watt, and this index is close with halogen tungsten lamp.2012, the light efficiency of white light LEDs reached 120 lm/W, and white light LEDs starts to popularize as home lighting light source.When expecting the year two thousand twenty, the light efficiency of LED is expected to reach 200 lm/W.Simultaneously, though the electric filament lamp of general lighting and halogen tungsten lamp low price, but light efficiency low (power consumption in vain of the heat effect of lamp), life-span is short, maintenance workload is big, if but illuminate with white light LEDs, not only light efficiency is high, and life-span length (stream time more than 10000 hours), almost Maintenance free.It is contemplated that in the near future, white light LEDs surely can enter family and replace existing illuminating lamp.
The mode mainly monocrystalline blue-ray LED of white light LEDs luminescence combines with yellow fluorescent powder, white light emitting diode is not that semi-conducting material itself directly sends white light, but exciting coating gold-tinted YAG fluorescent powder above it by blue light-emitting diode, the gold-tinted that fluorescent material produces after being excited is with to be formerly used for the blue light that excites complementary and produce white light.
Traditional fluorescent material coating method is a powder pattern, directly in chip surface spot printing phosphor gel, phosphor powder will mix by a certain percentage with colloid (such as silica gel or epoxy resin etc.), make slurry, stir, be then coated on chip surface with fine needle class instrument.Along with LED chip develops rapidly, power is more and more higher, this transmitting power being conducive to improving LED luminescent powder, improves the emissive porwer of total transmitting (white light).But too high excitation density can cause the rotten of colloid, causes the disengaging of whole powder body.For solving this problem, He Haiping reports the devitrified glass about white-light LED encapsulation in " the white-light LED encapsulation research of Ce:YAG fluorescent glass-ceramics " (electronic component and material, in May, 2010, volume 29 the 5th phase) literary composition, and it is with CaO-Al2O3-SiO2-Y2O3Based on glass, glass (adding trace Ce), by 1050 DEG C of sintering, methods of 1150 DEG C of overall crystallizes, has prepared the white-light LED fluorescence devitrified glass with Ce:YAG as principal crystalline phase.Although the devitrified glass prepared by adopting in this way has is suitable for blue light activated emission spectrum, may be used for white-light LED encapsulation.But owing to the method treatment temperature is too high, therefore can have a negative impact for the composition of fluorescent material and luminescent properties thereof, prepared devitrified glass is still with the presence of a small amount of dephasign peak, and the luminous intensity of glass and transparency the most wayward, the luminescent properties of obtained devitrified glass is also affected because fluorescent material changes.
Summary of the invention
An object of the present invention is to provide a kind of white light LEDs cerium activated yttrium aluminium garnet devitrified glass, and to solve existing white-light LED encapsulation devitrified glass difficult quality and control, product stability is poor, luminous intensity and the problem such as transparency is wayward.
The two of the purpose of the present invention are to provide the preparation method of a kind of white light LEDs cerium activated yttrium aluminium garnet devitrified glass, to solve YAG: the Ce fluorescent glass-ceramics prepared of existing method, its phosphor constituents is susceptible to change, product luminescent properties easily fails, luminous intensity and the problem such as transparency is wayward.
First purpose of the present invention is to realize by following technical scheme:
White light LEDs cerium activated yttrium aluminium garnet devitrified glass provided by the present invention, in low softening point glass material doped with YAG: Ce3+Fluorescent material；Wherein, described YAG: Ce3+Fluorescent material doping mass ratio in described devitrified glass is 1 ~ 80%, and described low softening point glass material is softening point at the glass material of 300 ~ 800 DEG C.
White light LEDs cerium activated yttrium aluminium garnet devitrified glass of the present invention, described low softening point glass material is to form with blended melted the firing of glass matrix raw material and softening point regulator.
Concrete, described glass matrix raw material is SiO2、B2O3、H3BO3、P2O5、TeO2And GeO2In any one or any two or more mixture.
Concrete, described softening point regulator is alkali metal oxide, alkali carbonate, alkaline earth oxide, alkaline earth metal carbonate, Al2O3Or ZrO2In any one or any two or more mixture, further, described alkali metal oxide is lithium oxide, sodium oxide or potassium oxide, described alkali carbonate is lithium carbonate, sodium carbonate or potassium carbonate, described alkaline earth oxide is magnesium oxide, calcium oxide or Barium monoxide, and described alkaline earth metal carbonate is magnesium carbonate, calcium carbonate or brium carbonate.
Second object of the present invention is to realize by following technical scheme:
The preparation method of white light LEDs cerium activated yttrium aluminium garnet devitrified glass of the present invention, comprises the following steps:
(1) weigh glass matrix raw material, softening point regulator, uniformly mix, melt and be prepared as the molten glass that softening point is at 300 ~ 800 DEG C；
Wherein, described glass matrix raw material is selected from SiO2、B2O3、H3BO3、P2O5、TeO2And GeO2In any one or any two or more mixture；Described softening point regulator is selected from alkali metal oxide, alkali carbonate, alkaline earth oxide, alkaline earth metal carbonate, Al2O3Or ZrO2In any one or any two or more mixture, concrete, described alkali metal oxide is lithium oxide, sodium oxide or potassium oxide, described alkali carbonate is lithium carbonate, sodium carbonate or potassium carbonate, described alkaline earth oxide is magnesium oxide, calcium oxide or Barium monoxide, and described alkaline earth metal carbonate is magnesium carbonate, calcium carbonate or brium carbonate；
Adding the amount of softening point regulator in glass matrix raw material, after the two mixed melting, its softening point can control on the basis of 300 ~ 800 DEG C；
(2) by YAG: Ce3+Fluorescent material joins in described molten glass, uniformly mixes, and then cooling solidify to form glass；
(3) step (2) gained glass is annealed 6 ~ 48 hours, prepare white light LEDs cerium activated yttrium aluminium garnet devitrified glass；
Wherein, described in step (2) YAG: Ce3+The addition of fluorescent material, with in final gained devitrified glass YAG: Ce3+On the basis of the doping mass ratio of fluorescent material is 1-80%.
Second object of the present invention also can be realized by following technical scheme:
The preparation method of white light LEDs cerium activated yttrium aluminium garnet devitrified glass of the present invention, comprises the following steps:
(1) weigh glass matrix raw material, softening point regulator, uniformly mix, melt and be prepared as the molten glass that softening point is at 300 ~ 800 DEG C；
Wherein, described glass matrix raw material is selected from SiO2、B2O3、H3BO3、P2O5、TeO2And GeO2In any one or any two or more mixture；Described softening point regulator is selected from alkali metal oxide, alkali carbonate, alkaline earth oxide, alkaline earth metal carbonate, Al2O3Or ZrO2In any one or any two or more mixture, concrete, described alkali metal oxide is lithium oxide, sodium oxide or potassium oxide, described alkali carbonate is lithium carbonate, sodium carbonate or potassium carbonate, described alkaline earth oxide is magnesium oxide, calcium oxide or Barium monoxide, and described alkaline earth metal carbonate is magnesium carbonate, calcium carbonate or brium carbonate；
Adding the amount of softening point regulator in glass matrix raw material, after the two mixed melting, its softening point can control on the basis of 300 ~ 800 DEG C；
(2) by after described molten glass natural cooling, powder is made, then by YAG: Ce3+Fluorescent material joins in described powder, uniformly mixes, and melting at 300 ~ 800 DEG C lowers the temperature after firing 0.5 ~ 2h again solidify to form glass；
(3) step (2) gained glass is annealed 6 ~ 48 hours, prepare white light LEDs cerium activated yttrium aluminium garnet devitrified glass；
Wherein, described in step (2) YAG: Ce3+The addition of fluorescent material, with in gained devitrified glass YAG: Ce3+On the basis of the doping mass ratio of fluorescent material is 1-80%.
In the present invention, the mensuration of glass softening point is carried out according to GB/T 28,195 2011 " glass softening point method of testing "；The method that glass annealing point provides according to GB/T 28,196 2011 " glass annealing point and strain point method of testing " is determined.
In the present invention, described softening point regulator doping mol ratio in described low softening point glass is preferably 10 ~ 40%.
The devitrified glass of the present invention, fluorescent material with the formal distribution of crystallite in glass, and the character of fluorescent material does not changes, thus the devitrified glass prepared by the present invention not only has the good characteristics of luminescence of crystal but also have the light transmission of glass, it is at 450-470nm(blue light) place has stronger light to absorb.Fluorescent material is fired in glass, owing to glass can bear higher temperature, thus can avoid the restriction of excitation density, simultaneously the fluorescent material in glass can well scattered light, make white light spatial distribution evenly, brightness is the most consistent.The blue light of LED emission can excite Ce in glass to activate YAG fluorescent powder, thus Yellow light-emitting low temperature, blue light can get up emit white light with yellow light combine by devitrified glass transmission again simultaneously.
Devitrified glass prepared by the present invention is mainly used in white light LEDs, has good heat stability and chemical stability, more can meet the demand of great power LED, meets green, environmental protection, the development trend of sustainable white light LEDs.
In the preparation method of the present invention, by YAG: Ce of higher melt3+Fluorescent material is mutually mixed with the formation substrate of low-melting glass, by YAG after making glass melt at a lower temperature: Ce3+Fluorescent material is coated with, then annealing forms devitrified glass, eliminate the problem that the performance of fluorescent material can be produced impact in traditional preparation methods processing procedure, being not only convenient for being controlled luminous intensity and the transparency of glass by the mass ratio of regulation fluorescent material with glass, prepared devitrified glass performance is more preferable.
Accompanying drawing explanation
Fig. 1 be the present invention devitrified glass in crystallite YAG: Ce3+Fluorescent material distribution schematic diagram in glass matrix.
Fig. 2 is YAG: the Ce prepared by embodiment 13+Fluorescent material doping content is respectively the devitrified glass sample of 5wt%, 10wt% and 15wt%.
Fig. 3 is YAG: Ce3+The X-ray diffractogram of fluorescent material and with standard card comparison diagram.
Fig. 4 be the sample 3 prepared by embodiment 1 X-ray diffractogram and with standard card comparison diagram.
Fig. 5 is the excitation spectrum of the sample 3 prepared by embodiment 1.
Fig. 6 is the emission spectra of the sample 3 prepared by embodiment 1,.
Fig. 7 is the transmission plot under blue light illumination of the sample 1 prepared by embodiment 1.
Detailed description of the invention
In the embodiment of the present invention used YAG: Ce3+Fluorescent material and glass matrix raw material, softening point regulator all can be by commercially available by way of being commercially available.
Embodiment 1
(1) glass matrix raw material TeO is measured at 6: 1: 2 in molar ratio2With softening point regulator ZnO, Na2CO3, uniformly mix, be then placed in high temperature furnace melted (founding 1 hour for 600 DEG C), make the glass of molten state.
(2) by the glass natural cooling of prepared molten state, it is then ground to glass powder, by the consumption in table 1, the YAG fluorescent powder (i.e. YAG: Ce of Ce will be mixed3+Fluorescent material) uniformly mix with glass powder, melted fire 1 hour for 500 DEG C in high temperature furnace, then natural cooling cooling solidify to form glass.
(3) step (2) gained glass is annealed 6 hours at 200 DEG C, prepare YAG: Ce3+Fluorescent material doping content is followed successively by 5wt%(sample 1), 10wt%(sample 2), 15wt%(sample 3) cerium activated yttrium aluminium garnet devitrified glass, finally to formed microcrystalline glass polishing both surfaces, as shown in Figure 2.
Table 1:
| Glass powder (g) | YAG∶Ce3+Fluorescent material (g) | |
| Sample 1 | 6.5 | 0.34210 |
| Sample 2 | 6.5 | 0.72222 |
| Sample 3 | 6.5 | 1.14705 |
Interpretation of result: as seen from Figure 2, YAG: Ce3+When fluorescent material doping content (wt%) in devitrified glass is 5%, the transparency (i.e. light transmittance) of made glass sample (i.e. sample 1) is preferable, thus can ensure there is preferable percent of pass (as shown in Figure 7) to blue light, works as YAG: Ce3+When fluorescent material doping content (wt%) in devitrified glass is 10% and 15%, made glass sample (i.e. sample 2, sample 3) light transmittance is poor.
It follows that with YAG: Ce3+The rising of fluorescent material doping content, the lower conversion efficiency of obtained cerium activated yttrium aluminium garnet devitrified glass raises the most accordingly, but the opacity of made glass raises (i.e. light transmittance variation) the most simultaneously, and it is the lowest to the transmitance of useful light (blue light) certainly.In actual application, should as required, by regulation YAG: Ce3+Fluorescent material doping content in glass matrix chooses the equilibrium point between light transmittance and lower conversion efficiency, to obtain best using effect.
To YAG: Ce3+Fluorescent material and sample 3 carry out X-ray diffraction analysis, and by analysis result respectively with YAG: Ce3+The X-ray diffraction standard card of fluorescent material contrasts, and result is as shown in Figure 3, Figure 4.Fig. 3 is YAG: Ce3+The X-ray diffractogram of fluorescent material and standard card comparison diagram, Fig. 4 is sample 3(YAG: Ce3+The devitrified glass of fluorescent material doping content 15wt%) X-ray diffractogram and standard card comparison diagram.Comparison diagram 3 and Fig. 4 can be seen that, the diffraction maximum occurred in Fig. 4 is consistent with the diffraction maximum in Fig. 3, therefore the diffraction maximum that sharp line is YAG in Fig. 4, additionally, in Fig. 4 in addition to the diffraction maximum of YAG, not having miscellaneous peak to occur, the fluorescent material being indicated above in the devitrified glass prepared by the present invention is to be present in glass with the microcrystalline form of pure phase, its structure does not changes, from being effectively guaranteed Ce3+It is to produce to launch in the crystal of YAG.Fig. 1 gives in devitrified glass of the present invention YAG: Ce of crystallite3+Fluorescent material distribution schematic diagram in glass matrix, the structure illustrating devitrified glass of the present invention of comparison image.
Can also be drawn by above result, fluorescent material exists and in glass with microcrystalline form, the advantage with the following aspects: the devitrified glass of (1) present invention not only has the good characteristics of luminescence of crystal but also have the light transmission of glass；(2) light can well be scattered by the fluorescent material of crystallite, so that white light being more evenly distributed, unanimously in space；(3) fluorescent material being present in glass with microcrystalline form, has good heat stability and chemical stability, so being suitable for the demand of following large power white light LED.
It addition, to the exciting of sample 3, emission spectra is monitored respectively, result is the most as shown in Figure 5, Figure 6.In Fig. 5, curve is the excitation spectrum of monitoring 534nm wavelength sample 3, and in Fig. 6, curve 1 is the emission spectrum that monitoring 340nm excites sample 3, and curve 2 is the emission spectrum that monitoring 460nm excites sample 3.From Fig. 5, Fig. 6 it can be seen that cerium activated yttrium aluminium garnet devitrified glass (Ce prepared by the present invention3+Activate YAG devitrified glass) at 450-470nm(blue light) there is wide band absorption at place, the peak value of its emission spectrum is positioned at 534nm at, presents yellow, and it presents white light with the blue light combination transmitted through devitrified glass.
Embodiment 2:
(1) glass matrix raw material H is measured at 2: 1: 2 in molar ratio3BO3、SiO2With softening point regulator Na2CO3, uniformly mix, be then placed in high temperature furnace melted (founding 1h for 750 DEG C), make the glass of molten state；
(2) consumption in table 2 is pressed, by YAG: Ce3+Fluorescent material joins in the glass of (1) step molten state and mix homogeneously, and then natural cooling cooling solidify to form glass.
(3) step (2) gained glass is annealed 30 hours at 400 DEG C, prepare YAG: Ce3+Fluorescent material doping content is followed successively by 2%(sample 4), 5%(sample 5), 10%(sample 6) cerium activated yttrium aluminium garnet devitrified glass, finally to formed sheet glass polishing both surfaces.
Table 2:
| Glass powder (g) | YAG∶Ce3+Fluorescent material (g) | |
| Sample 4 | 9.5 | 0.19387 |
| Sample 5 | 9.5 | 0.50000 |
| Sample 6 | 9.5 | 1.05555 |
Embodiment 3
(1) glass matrix raw material P is measured at 2: 1: 2 in molar ratio2O5With softening point regulator Al2O3、ZrO2, uniformly mix, be then placed in high temperature furnace melted (founding 1h for 800 DEG C), make the glass of molten state；
(2) consumption in table 3 is pressed, by YAG: Ce3+Fluorescent material joins in the glass of (1) step molten state and mix homogeneously, and then natural cooling cooling solidify to form glass.
(3) step (2) gained glass is annealed 30 hours at 400 DEG C, prepare YAG: Ce3+Fluorescent material doping content is followed successively by 30%(sample 7), 60%(sample 8), 80%(sample 9) cerium activated yttrium aluminium garnet devitrified glass, finally to formed sheet glass polishing both surfaces.
Table 3:
| Glass powder (g) | YAG∶Ce3+Fluorescent material (g) | |
| Sample 7 | 9.5 | 1.22143 |
| Sample 8 | 9.5 | 14.25 |
| Sample 9 | 9.5 | 39.2 |
Detecting the sample (sample 4 ~ 9) prepared by embodiment 2,3 according to the detection method in embodiment 1, result shows, the devitrified glass prepared by embodiment 2,3 has microstructure as shown in Figure 1 equally, i.e. YAG: Ce3+Fluorescent material is present in glass with microcrystalline form, and it is at 450-470nm(blue light) there is wide band absorption at place, and the peak value of emission spectrum is positioned at 534nm.Along with the rising of doping content, the opacity of made glass gradually rises.
Above example is intended to devitrified glass to the present invention and preparation method thereof and illustrates, and is not the restriction to present invention.
Claims (3)
1. a white light LEDs cerium activated yttrium aluminium garnet devitrified glass, is characterized in that, described devitrified glass is doped with YAG at low softening point glass material: Ce3+Fluorescent material；Wherein, described YAG: Ce3+Fluorescent material doping mass ratio in described devitrified glass is 1 ~ 80%, and described low softening point glass material is softening point at the glass material of 300 ~ 800 DEG C；
Wherein, described low softening point glass material is to form with blended melted the firing of glass matrix raw material and softening point regulator；
Described glass matrix raw material is SiO2、B2O5、H3BO3、P2O5In any one or any two or more mixture；Described softening point regulator is alkali metal oxide, alkali carbonate, alkaline earth oxide, alkaline earth metal carbonate, Al2O3Or ZrO2In any one or any two or more mixture；Described alkali metal oxide is lithium oxide, sodium oxide or potassium oxide, described alkali carbonate is lithium carbonate, sodium carbonate or potassium carbonate, described alkaline earth oxide is magnesium oxide, calcium oxide or Barium monoxide, and described alkaline earth metal carbonate is magnesium carbonate, calcium carbonate or brium carbonate；
Described softening point regulator doping mol ratio in described low softening point glass is 10 ~ 40%.
2. the preparation method of cerium activated yttrium aluminium garnet devitrified glass of white light LEDs described in claim 1, is characterized in that, comprise the following steps:
(1) weigh glass matrix raw material, softening point regulator, uniformly mix, melt and be prepared as the molten glass that softening point is at 300 ~ 800 DEG C；
(2) by YAG: Ce3+Fluorescent material joins in described molten glass, uniformly mixes, and then cooling solidify to form glass；
(3) step (2) gained glass is annealed 6 ~ 48 hours, prepare white light LEDs cerium activated yttrium aluminium garnet devitrified glass；
Wherein, described in step (2) YAG: Ce3+The addition of fluorescent material, with in gained devitrified glass YAG: Ce3+On the basis of the doping mass ratio of fluorescent material is 1-80%.
3. the preparation method of cerium activated yttrium aluminium garnet devitrified glass of white light LEDs described in claim 1, is characterized in that, comprise the following steps:
(1) weigh glass matrix raw material, softening point regulator, uniformly mix, melt and be prepared as the molten glass that softening point is at 300 ~ 800 DEG C；
(2) by after described molten glass natural cooling, powder is made, then by YAG: Ce3+Fluorescent material joins in described powder, uniformly mixes, and melting at 300 ~ 800 DEG C lowers the temperature after firing 0.5 ~ 2h again solidify to form glass；
(3) step (2) gained glass is annealed 6 ~ 48 hours, prepare white light LEDs cerium activated yttrium aluminium garnet devitrified glass；
Wherein, described in step (2) YAG: Ce3+The addition of fluorescent material, with in gained devitrified glass YAG: Ce3+On the basis of the doping mass ratio of fluorescent material is 1-80%.
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| CN104445955A (en) * | 2014-12-05 | 2015-03-25 | 南京奥依菲光电科技有限公司 | Tunable transparent glass ceramic light-emitting fluorophor for LED and preparation method of tunable transparent glass ceramic light-emitting fluorophor |
| CN107176791B (en) * | 2017-03-20 | 2019-01-11 | 中山大学 | A kind of high power illumination and display fluorescent glass ceramics and its preparation method and application |
| CN107162427B (en) * | 2017-03-24 | 2019-01-11 | 中山大学 | A kind of high power semiconductor light source activation glass ceramics and its preparation method and application |
| CN111153594B (en) * | 2020-01-09 | 2022-06-07 | 温州大学 | YAG-Ce glass ceramic and preparation method and application thereof |
| CN113620599A (en) * | 2021-06-15 | 2021-11-09 | 福建江夏学院 | Novel long-afterglow luminescent glass-ceramic and preparation method thereof |
| CN113860744B (en) * | 2021-10-18 | 2024-01-26 | 昆明理工大学 | Preparation method of microcrystalline glass sodium molybdate |
| CN116082029A (en) * | 2022-12-26 | 2023-05-09 | 江苏锡沂高新材料产业技术研究院有限公司 | Preparation method of fluorescent device for reflective laser illumination |
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| CN103183473A (en) * | 2013-04-10 | 2013-07-03 | 中国科学院福建物质结构研究所 | Ce:YAG microcrystalline glass used for white light LED and preparation method of Ce:YAG microcrystalline glass |
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| CN101601145A (en) * | 2007-02-07 | 2009-12-09 | 旭硝子株式会社 | The optical element lining reaches the light-emitting device that is covered by glass with glass |
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