CN115710089B - Yellow semitransparent fluorescent microcrystalline glass and preparation method thereof - Google Patents
Yellow semitransparent fluorescent microcrystalline glass and preparation method thereof Download PDFInfo
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- CN115710089B CN115710089B CN202211663360.0A CN202211663360A CN115710089B CN 115710089 B CN115710089 B CN 115710089B CN 202211663360 A CN202211663360 A CN 202211663360A CN 115710089 B CN115710089 B CN 115710089B
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- 239000011521 glass Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000010431 corundum Substances 0.000 claims description 5
- 239000000156 glass melt Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000009740 moulding (composite fabrication) Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 229910005224 Ga2O Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 21
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 229910018072 Al 2 O 3 Inorganic materials 0.000 abstract description 5
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 abstract description 5
- 229910005793 GeO 2 Inorganic materials 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract 1
- 239000002131 composite material Substances 0.000 description 7
- 239000000919 ceramic Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 239000013081 microcrystal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 230000004907 flux Effects 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000011224 oxide ceramic Substances 0.000 description 1
- 239000000075 oxide glass Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Abstract
The invention relates to yellow semitransparent fluorescent microcrystalline glass and a preparation method thereof, wherein the formula of the microcrystalline glass comprises the following components in percentage by weight: k (K) 2 O 3～9%，MgO 3～6%，Al 2 O 3 13～16%，Y 2 O 3 10～16%，Ga 2 O 3 3～12%，CeO 2 1～3%，ZrO 2 2～5%，GeO 2 3～6%，SiO 2 41-49%. Firstly, the microcrystalline glass raw materials are weighed according to the weight percentage, uniformly mixed, melted, molded and heat treated to obtain the yellow semitransparent fluorescent microcrystalline glass. The main crystal phase prepared by the invention is Y 3 Al 2.1 Ga 2.9 O 12 The fluorescent glass ceramics not only retain the excellent luminous performance of fluorescent materials, but also endow the fluorescent materials with good thermophysical performance, and ensure that the fluorescent conversion materials have stable conversion luminous capability under long-term high-power laser irradiation, thereby having wide application prospect.
Description
Technical Field
The invention relates to the technical field of new inorganic materials and semiconductor illumination, in particular to yellow semitransparent fluorescent microcrystalline glass and a preparation method thereof.
Background
White light LEDs are a new generation of illumination sources, and have the advantages of no pollution, high efficiency, long service life, high response speed and the like. However, the LED has a phenomenon of decreasing efficiency with increasing injection current, so that a single LED chip can only generate a small amount of luminous flux, and therefore, a plurality of LED chips need to be packaged in a concentrated array to increase the luminous flux. LD white light is considered as the most ideal solution for next-generation high-power high-brightness light sources, and has a core advantage in that high-power light emission of a single chip can be achieved. Practice proves that under the irradiation of high-power blue-off laser, heat can easily gather in the fluorescent conversion material, thereby leadingThe local temperature is too high, so that the traditional organic fluorescent conversion material cannot be suitable for a high-power laser light source, and the development of the fluorescent conversion material with high thermal stability based on inorganic oxide glass and ceramic is a necessary trend. Current processes for preparing fluorescent glass and fluorescent ceramics generally include the step of adding Ce to the glass 3+ Doped YAG phosphor (Ce: Y) 3 Al 5 O 12 ) Adding into glass powder or ceramic raw material, firing at high temperature to obtain block material, and cutting into required size. However Ce 3+ The doped YAG fluorescent powder has poor stability at high temperature, and is easy to decompose in the high-temperature sintering process of fluorescent glass or fluorescent ceramic to lose the capability of converting blue light, so that the current inorganic fluorescent conversion materials can be sintered at lower temperature generally, and the thermal physical properties of the fluorescent glass or fluorescent ceramic sintered at low temperature are not ideal, and the risks of thermal stress cracking and the like still exist although the aging phenomenon similar to that of the organic fluorescent material does not occur.
Disclosure of Invention
The invention aims to solve the technical problem of providing a semitransparent yellow fluorescent microcrystalline glass with semitransparent, zero air holes, high thermal conductivity and high luminous efficiency and a preparation method thereof.
In order to solve the technical problems, the technical scheme of the invention is as follows: the yellow semitransparent fluorescent microcrystalline glass is characterized by comprising the following components in percentage by weight: k (K) 2 O 3～9%，MgO 3～6%，Al 2 O 3 13～16%，Y 2 O 3 10～16%，Ga 2 O 3 3～12%，CeO 2 1～3%，ZrO 2 2～5%，GeO 2 3～6%，SiO 2 41～49%。
The preparation method of the yellow semitransparent fluorescent microcrystalline glass is characterized by comprising the following steps of: and weighing and uniformly mixing the glass ceramic raw materials according to the weight percentage, and obtaining the yellow semitransparent fluorescent glass ceramic through melting, forming and heat treatment.
The melting procedure is to put the glass ceramics raw material into a corundum crucible, put into a high-temperature electric furnace, heat up to 1550-1650 ℃ and keep the temperature for 2-3 hours to obtain uniform melt.
The molding process is to pour the glass melt which is melted uniformly into a mold preheated to 500-650 ℃ to form a glass block.
The heat treatment process is to transfer the formed and solidified glass block to an electric furnace at 500-650 ℃ to heat up to 1200-1350 ℃ at a rate of 5-10/min, and to preserve heat for 1-3 h.
In the heating process, in order to prevent the glass from softening and deforming, alumina powder is used for covering and compacting the glass block.
The main crystal phase of the yellow semitransparent fluorescent microcrystalline glass is Ce-Y 3 Al 2.1 Ga 2.9 O 12 。
The flexural strength of the yellow semitransparent fluorescent microcrystalline glass is 152-178 MPa.
Under the condition of excitation power of 5W, the luminous efficiency of the yellow semitransparent fluorescent microcrystalline glass is 133.61-161.39 lm/W, the color temperature is 4631-5279K, and the CIE color coordinates are (0.33 ).
The invention has the following beneficial effects:
(1) Compared with the traditional process of adding YAG fluorescent powder into glass powder and sintering at high temperature, the Ce-Y-based sintering process has the advantages that 3 Al 2.1 Ga 2.9 O 12 The fluorescent microcrystal is precipitated in situ in the glass, so that the decomposition failure of the fluorescent body at high temperature is avoided, the uniform distribution of the fluorescent body in the glass matrix is realized, and the size of the fluorescent crystal can be realized by adjusting the heat treatment parameters, so that the glass ceramic composite fluorescent material with high fluorescent crystal content can be obtained by the scheme.
(2) The prepared composite fluorescent material is formed by crystallization and transformation of solid glass material, so the composite fluorescent material has the characteristics of high density, zero air holes and the like glass, and the precipitated crystal can form a pinning effect to inhibit the expansion of microcracks, thereby improving the mechanical property of the composite fluorescent material and realizing the flexural strength of 152-178 MPa.
(3) By controllable heat treatment of the solid glass, ce and Y are directly separated from the glass 3 Al 2.1 Ga 2.9 O 12 Microcrystals, due to Ce: Y 3 Al 2.1 Ga 2.9 O 12 YAG-like structure and luminescence property of the microcrystal, so that the obtained glass ceramic also has excellent fluorescence conversion luminescence capability, and can realize stable conversion of blue laser into positive white light for output. Under the condition of excitation power of 5W, the luminous efficiency of the fluorescent material is 133.61-161.39 lm/W, the color temperature is 4631-5279K, and the CIE color coordinates are all near (0.33 ), so that the fluorescent material can be widely used for the positive white light conversion luminescence of blue laser.
Detailed Description
In order to further illustrate the technical means and effects adopted by the invention to achieve the preset aim, the following is a detailed description of specific implementation, method, steps, characteristics and effects of the yellow semitransparent fluorescent microcrystalline glass and the preparation method thereof according to the invention by combining with the preferred embodiment, wherein the detailed description is as follows:
embodiment one:
the embodiment is yellow semitransparent fluorescent microcrystalline glass and a preparation method thereof, and the preparation method comprises the following steps:
taking 3 parts of K 2 O (in K) 2 CO 3 Introduced as raw material), 6 parts of MgO, 13 parts of Al 2 O 3 12 parts of Y 2 O 3 9 parts of Ga 2 O 3 1 part CeO 2 3 parts of ZrO 2 5 parts of GeO 2 48 parts of SiO 2 After being uniformly mixed, the mixture is put into a corundum crucible, and is placed into a high-temperature electric furnace to be heated to 1650 ℃ and is kept for 2 hours, thus obtaining uniform melt. Pouring the glass melt which is melted uniformly into a mould preheated to 650 ℃ for molding, transferring the glass to an electric furnace at 650 ℃ after solidification of the glass, heating to 1330 ℃ at the speed of 10/min ℃ and preserving heat for 2h to obtain Ce: Y 3 Al 2.1 Ga 2.9 O 12 Yellow semitransparent fluorescent microcrystalline glass with main crystalline phase. The obtained composite fluorescent material has the flexural strength of 173 MPa, the luminous efficiency of 141.6 lm/W, the color temperature of 4631K and the CIE color coordinates of (0.33 ) when the excitation power is 5W.
Embodiment two:
the embodiment is yellow semitransparent fluorescent microcrystalline glass and a preparation method thereof, and the preparation method comprises the following steps:
9 parts of K 2 O (in K) 2 CO 3 Introduced as raw material), 3 parts of MgO, 15 parts of Al 2 O 3 13 parts of Y 2 O 3 5 parts of Ga 2 O 3 3 parts of CeO 2 2 parts of ZrO 2 6 parts of GeO 2 44 parts of SiO 2 After being uniformly mixed, the mixture is put into a corundum crucible, and is placed into a high-temperature electric furnace to be heated to 1610 ℃ and is kept warm for 2 hours, so that uniform melt is obtained. Pouring the glass melt which is melted uniformly into a mould preheated to 560 ℃ for molding, transferring the glass to an electric furnace at 560 ℃ after solidification of the glass, heating to 1290 ℃ at a rate of 5/min ℃ and preserving heat for 2 hours to obtain Ce: Y 3 Al 2.1 Ga 2.9 O 12 Yellow semitransparent fluorescent microcrystalline glass with main crystalline phase. The obtained composite fluorescent material has the flexural strength of 167 MPa, the luminous efficiency of the fluorescent material is 137.3 lm/W, the color temperature of 5126K and the CIE color coordinates of (0.33 ) when the excitation power is 5W.
Embodiment III:
the embodiment is yellow semitransparent fluorescent microcrystalline glass and a preparation method thereof, and the preparation method comprises the following steps:
6 parts of K 2 O (in K) 2 CO 3 Introduced as raw material), 4 parts of MgO, 14 parts of Al 2 O 3 16 parts of Y 2 O 3 10 parts of Ga 2 O 3 2 parts of CeO 2 4 parts of ZrO 2 3 parts of GeO 2 41 parts of SiO 2 After being uniformly mixed, the mixture is put into a corundum crucible, and is placed into a high-temperature electric furnace to be heated to 1580 ℃ and is kept warm for 3 hours, so that uniform melt is obtained. Pouring the glass melt which is melted uniformly into a mould preheated to 500 ℃ for molding, transferring the glass to an electric furnace at 500 ℃ after solidification of the glass, heating to 1230 ℃ at the rate of 8/min ℃ and preserving the heat for 3 hours to obtain Ce: Y 3 Al 2.1 Ga 2.9 O 12 Yellow semitransparent fluorescent microcrystalline glass with main crystalline phase. The obtained composite fluorescent material has the flexural strength of 156 MPa, the luminous efficiency of the fluorescent material is 158.6 lm/W, the color temperature of 4983K and the CIE color coordinates of (0.33 ) when the excitation power is 5W.
Claims (4)
1. A yellow semitransparent fluorescent microcrystalline glass is characterized in that: the microcrystalline glass comprises the following components in percentage by weight: 3-9% of K2O, 3-6% of MgO, 13-16% of Al2O3, 10-16% of Y2O3, 3 3-12% of Ga2O, 2 1-3% of CeO, 2 2-5% of ZrO, 2 3-6% of GeO and 41-49% of SiO 2;
the preparation method of the yellow semitransparent fluorescent microcrystalline glass comprises the steps of weighing and uniformly mixing microcrystalline glass raw materials according to weight percentage, and obtaining the yellow semitransparent fluorescent microcrystalline glass through melting, forming and heat treatment;
the heat treatment process is to transfer the formed and solidified glass block into an electric furnace at 500-650 ℃ to be heated to 1200-1350 ℃ at a rate of 5-10/min ℃ and to keep the temperature for 1-3 h;
the main crystal phase of the yellow semitransparent fluorescent microcrystalline glass is Ce, Y3Al2.1Ga2.9O12;
the flexural strength of the yellow semitransparent fluorescent microcrystalline glass is 152-178 MPa;
under the condition of excitation power of 5W, the luminous efficiency of the yellow semitransparent fluorescent microcrystalline glass is 133.61-161.39 lm/W, the color temperature is 4631-5279K, and the CIE color coordinates are (0.33 ).
2. The yellow translucent fluorescent glass ceramic according to claim 1, wherein: the melting procedure is to put the glass ceramics raw material into a corundum crucible, put into a high-temperature electric furnace, heat up to 1550-1650 ℃ and keep the temperature for 2-3 hours to obtain uniform melt.
3. The yellow translucent fluorescent glass ceramic according to claim 1, wherein: the molding process is to pour the glass melt which is melted uniformly into a mold preheated to 500-650 ℃ to form a glass block.
4. The yellow translucent fluorescent glass ceramic according to claim 1, wherein: in the heating process, in order to prevent the glass from softening and deforming, alumina powder is used for covering and compacting the glass block.
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2022
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