CN103319092A - Precious-metal-enhanced Ce-YAG microcrystalline-glass and preparation method thereof - Google Patents
Precious-metal-enhanced Ce-YAG microcrystalline-glass and preparation method thereof Download PDFInfo
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- CN103319092A CN103319092A CN2013102249955A CN201310224995A CN103319092A CN 103319092 A CN103319092 A CN 103319092A CN 2013102249955 A CN2013102249955 A CN 2013102249955A CN 201310224995 A CN201310224995 A CN 201310224995A CN 103319092 A CN103319092 A CN 103319092A
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Abstract
The invention discloses precious-metal-enhanced Ce-YAG microcrystalline-glass and a preparation method thereof. The method is composed of the following components: 45-50mol% of SiO2, 5-15mol% of Y2O3, 10-30mol% of Al2O3, 5-10mol% of Li2O, 0-5mol% of ZrO2, 0-5mol% of TiO2, and 0.1-5mol% of CeO2. The method provided by the invention has the advantages that: through regulation the components of the glass, for one thing, alkali metal oxide content is improved to above 5mol%, such that ion exchange is benefited; and for another, YAG crystal phase precipitation in glass is realized, and Ce<3+> enters precipitated YAG through occupying the lattices of Y<3+>. Ag nano-particles are precipitated from the surface of microcrystalline-glass. Through plasma resonance enhancing, yellow light emission of Ce<3+>:YAG microcrystalline-glass is enhanced.
Description
Technical field
The present invention relates to a kind of devitrified glass and preparation method thereof, more specifically, it relates to Ce-YAG devitrified glass of a kind of precious metal enhancing and preparation method thereof.
Background technology
In realizing the scheme of white light LEDs, InGaN (InGaN) led chip that utilizes the coloured light that turns blue and jaundice coloured light mix cerium ion (Ce
3+) (Cerium-doped Yttrium Aluminum Garnet is called for short Ce for the yttrium aluminum garnet that activates
3+: YAG) phosphor combination realizes the white light emission dominate.At present, domestic main employing is to apply fluorescent material and organic resin or silica gel mixture at chip surface.CN101696085 is described as patent, and the white light LEDs that adopts this mode to assemble impairs colour temperature, light efficiency of great power LED etc., and Ce:YAG will be dispersed in a kind of good terms of settlement of can yet be regarded as in the unorganic glass.The people such as Japanese scientist Masayuki Nishi were first at CaO-Y in 2004
2O
3-Al
2O
3-SiO
2-Er
2O
3Separate out the YAG crystal in the glass, its grain size is about 10 μ m.Patent CN1326790 discloses the CaO-Y of a kind of YAG of separating out
2O
3-Al
2O
3-SiO
2Glass system.The people such as Shunsuke Fujita were at 42.5mol%SiO in 2010
2-20mol%Y
2O
3-34mol%Al
2O
3-3mol%Li
2O-0.5mol%CeO
2Separated out the Ce:YAG crystallite in the glass, excited the lower gold-tinted that can send high brightness at blue light, but the Ce:YAG fluorescent material that its emissive porwer and high-temperature calcination obtain still has certain gap.
Surface plasma body resonant vibration strengthens and can be produced by internal electron collaborative vibration under the light action of its characteristic frequency of noble metal nano particles.Surface plasma body resonant vibration can greatly strengthen the electromagnetic field of its ambient particles, reduces the activation energy of particle, improves launching efficiency or the attenuation speed of particle, and corresponding luminous intensity is strengthened greatly.Patent CN102515548A has told the rear-earth-doped fluorine oxygen devitrified glass that a kind of precious metals ag strengthens, the people such as Wen-Hsuan Chao are at paper Journal of The Electrochemical Society, 156(12) J370-J374(2009) in narrated precious metals ag to Ce
3+The effect that the plasma resonance of doping YAG film strengthens, blue-light excited lower at 460nm, its emissive porwer has improved an order of magnitude.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, a kind of luminous efficiency Ce-YAG devitrified glass that precious metal high, that realize strong yellow emission strengthens and preparation method thereof is provided.
The Ce-YAG devitrified glass that this precious metal strengthens, by the mole percentage composition, composed of the following components: SiO
2: 45～50mol%; Y
2O
3: 5～15mol%; Al
2O
3: 10～30mol%; Li
2O:5～10mol%; ZrO
2: 0～5mol%; TiO
2: 0～5mol%; CeO
2: 0.1～5mol%.
The preparation method of the Ce-YAG devitrified glass that this precious metal strengthens, step is as follows:
The first step: take by weighing each component powders raw material by forming metering, the even mixing of raw material is placed in the crucible, this crucible is put in another large crucible of adding a cover, the bottom of large crucible is filled with carbon granule to guarantee in the electric stove hearth as reducing atmosphere, in 1600～1650 ℃ electric furnace, founded 1～5 hour, glass melt is cast in the stainless steel mould, then at the transition temperature T of glass
gNear annealing 2 hours cools to room temperature naturally, obtains parent glass;
Near second step: glass sample is carried out the differential thermal analysis test, the first crystallization peak position of glass, heat-treated 2～10 hours, obtain Ce
3+: the YAG devitrified glass, and cut and polish;
The 3rd step: preparation AgNO
3And NaNO
3Mixing salt, AgNO wherein
3Content is 0.5mol%～10mol%, and the two puts into crucible after fully mixing, and is fused into liquid state 300 ℃～350 ℃ temperature ranges, the Ce that second step is obtained
3+: the YAG devitrified glass places above-mentioned mixing salt liquation, so that the Na in the glass
+With the Ag in the fused salt
+Ion-exchange occurs in the two, and the time is 30～120 minutes;
The 4th step: devitrified glass remained on surface fused salt after the ion-exchange is spent ionic fluid clean, and to put into temperature be 300～500 ℃ electric furnace thermal treatment 5～360 minutes, nano-Ag particles is separated out on the devitrified glass surface, obtains the Ce-YAG devitrified glass that precious metal strengthens.
As preferably: the crucible in the first step is corundum crucible or platinum crucible.
The invention has the beneficial effects as follows: the present invention on the one hand, brings up to the content of alkalimetal oxide more than the 5mol% by adjusting glass ingredient, is conducive to ion-exchange, on the other hand, has realized YAG crystalline phase separating out in glass, simultaneously Ce
3+By occupying Y
3+Case enter among the YAG that separates out.The Ag nano particle that separate out on the devitrified glass surface strengthens by plasma resonance, has strengthened Ce
3+: the yellow emission of YAG devitrified glass.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) figure after embodiment 1 glass heat is processed.
Embodiment
Below in conjunction with drawings and Examples the present invention is described further.Although the present invention is described in connection with preferred embodiment, should know, do not represent to limit the invention among the described embodiment.On the contrary, the present invention will be contained alternative, modified version and the equivalent in the scope of the present invention that can be included in attached claims restriction.
Embodiment 1:
By the component molar content, glass consists of 45SiO
2-14.9Y
2O
3-26Al
2O
3-9Li
2O-5ZrO
2-0.1CeO
2, accurately take by weighing analytically pure SiO
2, Y
2O
3, Al
2O
3, Li
2CO
3, ZrO
2With specpure CeO
2, pour in the crucible after fully mixing, insulation is 2 hours in 1600 ℃ electric furnace, and the glass melt of melting is poured into rapidly in the mould, transfers in the annealing furnace rapidly behind the glass ware forming and anneals.The glass that makes is carried out differential thermal analysis, and the first crystallization peak temperature that records glass is 1050 ℃, and the glass sample after the annealing 1050 ℃ of thermal treatments 10 hours, is closed annealing furnace and naturally cooled to room temperature, obtains separating out the devitrified glass of Ce:YAG crystalline phase.By shown in Figure 1, through the test of X-ray powder diffraction and contrast PDF card, the crystalline phase of separating out is Y
3Al
5O
12(YAG).With the devitrified glass cutting and polishing, be used for the ion-exchange experiment.Preparation AgNO
3And NaNO
3Mixing salt, AgNO
3Content is 0.5mol%, and the two puts into crucible after fully mixing, and is incubated at 350 ℃, and the devitrified glass that makes is placed above-mentioned fused salt mixt liquation, so that the Na in the glass
+With the Ag in the fused salt
+Ion-exchange occurs in the two, and the time is 30 minutes.Devitrified glass remained on surface fused salt after the ion-exchange is spent ionic fluid to be cleaned, and to put into temperature be 400 ℃ electric furnace thermal treatment 120 minutes, nano-Ag particles is separated out on the devitrified glass surface, obtains the Ce:YAG devitrified glass that noble silver nano grain surface plasma body strengthens.By fluorescence spectrophotometer the devitrified glass before and after the ion-exchange is carried out the luminescent properties test, blue-light excited lower at 460nm, centre wavelength is that the yellow emission intensity of 530nm has improved 10 times.
Embodiment 2:
By the component molar content, glass consists of 48SiO
2-10Y
2O
3-30Al
2O
3-5Li
2O-2ZrO
2-3TiO
2-2CeO
2, accurately take by weighing analytically pure SiO
2, Y
2O
3, Al
2O
3, Li
2CO
3, ZrO
2, TiO
2With specpure CeO
2, pour in the crucible after fully mixing, insulation is 2 hours in 1620 ℃ electric furnace, and the glass melt of melting is poured into rapidly in the mould, transfers in the annealing furnace rapidly behind the glass ware forming and anneals.The glass that makes is carried out differential thermal analysis, and the first crystallization peak temperature that records glass is 1080 ℃, and the glass sample after the annealing 1080 ℃ of thermal treatments 5 hours, is closed annealing furnace and naturally cooled to room temperature, obtains separating out Ce
3+: the devitrified glass of YAG crystalline phase with the devitrified glass cutting and polishing, is used for the ion-exchange experiment.Preparation AgNO
3And NaNO
3Mixing salt, AgNO
3Content is 5mol%, and the two puts into crucible after fully mixing, and is incubated at 300 ℃, and the devitrified glass that makes is placed above-mentioned fused salt mixt liquation, so that the Na in the glass
+With the Ag in the fused salt
+Ion-exchange occurs in the two, and the time is 120 minutes.Devitrified glass remained on surface fused salt after the ion-exchange is spent ionic fluid clean, and to put into temperature be 500 ℃ electric furnace thermal treatment 30 minutes, nano-Ag particles is separated out on the devitrified glass surface, obtains the Ce that noble silver nano grain surface plasma body strengthens
3+: the YAG devitrified glass.By fluorescence spectrophotometer the devitrified glass before and after the ion-exchange is carried out the luminescent properties test, blue-light excited lower at 460nm, centre wavelength is that the yellow emission intensity of 530nm has improved 7 times.
Embodiment 3:
By the component molar content, glass consists of 50SiO
2-15Y
2O
3-18Al
2O
3-10Li
2O-5TiO
2-2CeO
2, accurately take by weighing analytically pure SiO
2, Y
2O
3, Al
2O
3, Li
2CO
3, ZrO
2, TiO
2With specpure CeO
2, pour in the crucible after fully mixing, insulation is 2 hours in 1650 ℃ electric furnace, and the glass melt of melting is poured into rapidly in the mould, transfers in the annealing furnace rapidly behind the glass ware forming and anneals.The glass that makes is carried out differential thermal analysis, and the first crystallization peak temperature that records glass is 1100 ℃, and the glass sample after the annealing 1100 ℃ of thermal treatments 2 hours, is closed annealing furnace and naturally cooled to room temperature, obtains separating out Ce
3+The devitrified glass of Ce:YAG crystalline phase with the devitrified glass cutting and polishing, is used for the ion-exchange experiment.Preparation AgNO
3And NaNO
3Mixing salt, AgNO
3Content is 2mol%, and the two puts into crucible after fully mixing, and is incubated at 320 ℃, and the devitrified glass that makes is placed above-mentioned fused salt mixt liquation, so that the Na in the glass
+With the Ag in the fused salt
+Ion-exchange occurs in the two, and the time is 360 minutes.Devitrified glass remained on surface fused salt after the ion-exchange is spent ionic fluid clean, and to put into temperature be 300 ℃ electric furnace thermal treatment 360 minutes, nano-Ag particles is separated out on the devitrified glass surface, obtains the Ce that noble silver nano grain surface plasma body strengthens
3+: the YAG devitrified glass.By fluorescence spectrophotometer the devitrified glass before and after the ion-exchange is carried out the luminescent properties test, blue-light excited lower at 460nm, centre wavelength is that the yellow emission intensity of 530nm has improved 5 times.
Embodiment 4:
By the component molar content, glass consists of 50SiO
2-12Y
2O
3-20Al
2O
3-8Li
2O-3ZrO
2-2TiO
2-5CeO
2, accurately take by weighing analytically pure SiO
2, Y
2O
3, Al
2O
3, Li
2CO
3, ZrO
2, TiO
2With specpure CeO
2, pour in the crucible after fully mixing, insulation is 5 hours in 1650 ℃ electric furnace, and the glass melt of melting is poured into rapidly in the mould, transfers in the annealing furnace rapidly behind the glass ware forming and anneals.The glass that makes is carried out differential thermal analysis, the the first crystallization peak temperature that records glass is 1150 ℃, with annealing after glass sample 1150 ℃ of thermal treatments 5 hours, close annealing furnace and naturally cool to room temperature, obtain separating out the devitrified glass of Ce:YAG crystalline phase, with the devitrified glass cutting and polishing, be used for the ion-exchange experiment.Preparation AgNO
3And NaNO
3Mixing salt, AgNO
3Content is 1mol%, and the two puts into crucible after fully mixing, and is incubated at 330 ℃, and the devitrified glass that makes is placed above-mentioned fused salt mixt liquation, so that the Na in the glass
+With the Ag in the fused salt
+Ion-exchange occurs in the two, and the time is 120 minutes.Devitrified glass remained on surface fused salt after the ion-exchange is spent ionic fluid clean, and to put into temperature be 400 ℃ electric furnace thermal treatment 60 minutes, nano-Ag particles is separated out on the devitrified glass surface, obtains the Ce that noble silver nano grain surface plasma body strengthens
3+: the YAG devitrified glass.By fluorescence spectrophotometer the devitrified glass before and after the ion-exchange is carried out the luminescent properties test, blue-light excited lower at 460nm, centre wavelength is that the yellow emission intensity of 530nm has improved 3 times.
Claims (7)
1. the Ce-YAG devitrified glass that precious metal strengthens is characterized in that: by the mole percentage composition, composed of the following components: SiO
2: 45～50mol%; Y
2O
3: 5～15mol%; Al
2O
3: 10～30mol%; Li
2O:5～10mol%; ZrO
2: 0～5mol%; TiO
2: 0～5mol%; CeO
2: 0.1～5mol%.
2. the Ce-YAG devitrified glass of precious metal enhancing according to claim 1 is characterized in that: by the mole percentage composition, composed of the following components: 45SiO
2-14.9Y
2O
3-26Al
2O
3-9Li
2O-5ZrO
2-0.1CeO
2
3. the Ce-YAG devitrified glass of precious metal enhancing according to claim 1 is characterized in that: by the mole percentage composition, composed of the following components: 48SiO
2-10Y
2O
3-30Al
2O
3-5Li
2O-2ZrO
2-3TiO
2-2CeO
2
4. the Ce-YAG devitrified glass of precious metal enhancing according to claim 1 is characterized in that: by the mole percentage composition, composed of the following components: 50SiO
2-15Y
2O
3-18Al
2O
3-10Li
2O-5TiO
2-2CeO
2
5. the Ce-YAG devitrified glass of precious metal enhancing according to claim 1 is characterized in that: by the mole percentage composition, composed of the following components: 50SiO
2-12Y
2O
3-20Al
2O
3-8Li
2O-3ZrO
2-2TiO
2-5CeO
2
6. one kind prepares the method that requires the Ce-YAG devitrified glass that 1 precious metal strengthens such as profit, and it is characterized in that: the method comprises
Following steps:
The first step: take by weighing each component powders raw material by forming metering, the even mixing of raw material is placed in the crucible, this crucible is put in another large crucible of adding a cover, the bottom of large crucible is filled with carbon granule to guarantee in the electric stove hearth as reducing atmosphere, in 1600～1650 ℃ electric furnace, founded 1～5 hour, glass melt is cast in the stainless steel mould, then at the transition temperature T of glass
gNear annealing 2 hours cools to room temperature naturally, obtains parent glass;
Near second step: glass sample is carried out the differential thermal analysis test, the first crystallization peak position of glass, heat-treated 2～10 hours, obtain Ce
3+: the YAG devitrified glass, and cut and polish;
The 3rd step: preparation AgNO
3And NaNO
3Mixing salt, AgNO wherein
3Content is 0.5mol%～10mol%, and the two puts into crucible after fully mixing, and is fused into liquid state 300 ℃～350 ℃ temperature ranges, the Ce that second step is obtained
3+: the YAG devitrified glass places above-mentioned mixing salt liquation, so that the Na in the glass
+With the Ag in the fused salt
+Ion-exchange occurs in the two, and the time is 30～120 minutes;
The 4th step: devitrified glass remained on surface fused salt after the ion-exchange is spent ionic fluid clean, and to put into temperature be 300～500 ℃ electric furnace thermal treatment 5～360 minutes, nano-Ag particles is separated out on the devitrified glass surface, obtains the Ce-YAG devitrified glass that precious metal strengthens.
7. the preparation method of the Ce-YAG devitrified glass that strengthens of precious metal according to claim 6, it is characterized in that: the crucible in the first step is corundum crucible or platinum crucible.
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Cited By (5)
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|---|---|---|---|---|
| CN103666475A (en) * | 2013-12-11 | 2014-03-26 | 昆明理工大学 | Rare earth doped glass frequency conversion luminous material and preparation method thereof |
| CN111410427A (en) * | 2020-03-26 | 2020-07-14 | 五邑大学 | Microcrystalline glass for high-power white light L ED, preparation method and L ED device |
| CN111847883A (en) * | 2020-08-31 | 2020-10-30 | 贵州赛义光电科技有限公司 | Fluorescent glass ceramic and preparation method thereof |
| US20210355021A1 (en) * | 2020-05-14 | 2021-11-18 | Corning Incorporated | Novel glass and glass-ceramic compositions |
| CN114538774A (en) * | 2022-03-08 | 2022-05-27 | 浙江大学 | High-concentration fluorescent powder-doped glass ceramic and preparation method and application thereof |
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|---|---|---|---|---|
| CN103666475A (en) * | 2013-12-11 | 2014-03-26 | 昆明理工大学 | Rare earth doped glass frequency conversion luminous material and preparation method thereof |
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| US11905208B2 (en) * | 2020-05-14 | 2024-02-20 | Corning Incorporated | Glass and glass-ceramic compositions |
| CN111847883A (en) * | 2020-08-31 | 2020-10-30 | 贵州赛义光电科技有限公司 | Fluorescent glass ceramic and preparation method thereof |
| CN114538774A (en) * | 2022-03-08 | 2022-05-27 | 浙江大学 | High-concentration fluorescent powder-doped glass ceramic and preparation method and application thereof |
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Application publication date: 20130925 |