CN106630604A - Low-melting-point tellurate glass ceramic, preparation method and application of low-melting-point tellurate glass ceramic - Google Patents
Low-melting-point tellurate glass ceramic, preparation method and application of low-melting-point tellurate glass ceramic Download PDFInfo
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- CN106630604A CN106630604A CN201611238050.9A CN201611238050A CN106630604A CN 106630604 A CN106630604 A CN 106630604A CN 201611238050 A CN201611238050 A CN 201611238050A CN 106630604 A CN106630604 A CN 106630604A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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Abstract
The invention discloses low-melting-point tellurate glass ceramic, a preparation method and the application of the low-melting-point tellurate glass ceramic. The low-melting-point tellurate glass ceramic consists of a glass raw material and a YAG fluorescent powder, wherein the glass raw material consists of the following components in percentage by mole: 50 to 70 percent of TeO2, 10 to 30 percent of Na2O and 5 to 25 percent of ZnO; the total mole percentage of all the components is 100 percent; the mass of the YAG fluorescent powder accounts for 6 to 10 percent of the total mass of the glass raw material. The preparation process of the glass ceramic has the advantages of simplicity in operation, low melting temperature, short production period, zero generation of toxic substances, easiness in large-scale production and the like. The prepared glass ceramic can be used on an LED device after being machined.
Description
Technical field
The present invention relates to technical field of inorganic nonmetallic materials, and in particular to a kind of low melting point tellurate glass ceramics, system
Preparation Method and its application.
Background technology
The advantages of white light LEDs are because with energy-conservation and pollution-free, high-color rendering and life-span length, fast response time, by people
Extensive concern.Its operation principle is combined by blue light for InGaN chip and yellow fluorescent powder, the blue light that InGaN chips send
Part is absorbed by fluorescent material so as to be excited to send gold-tinted, and unabsorbed blue light mixes with the gold-tinted that fluorescent material sends, just
To white light.At present the encapsulating material of LED is mainly mixed by a certain percentage by silica gel and resin with fluorescent material, this envelope
The white light that dress mode is obtained, due to encapsulating material chip pyrotoxin, the heat and shortwave radiation that chip is distributed can make encapsulating material
Accelerated ageing turns yellow causes transmitance to decline, and shortens white light LEDs service life.Accordingly it is desirable to pass through to prepare YAG:Ce is mono-
Brilliant, YAG:Ce glass ceramics, YAG:Ce ceramics are packaged substituting fluorescence resin, and then are solved that radiating is difficult, easily aging etc. asked
Topic.But the YAG of doping with rare-earth ions:It is long to there is the monocrystalline production cycle in Ce single crystal preparations, and ingredient requirement is strict, and technique is too multiple
Miscellaneous, production cost is too high, it is difficult to the problems such as forming large scale product.YAG:YAG is compared in the preparation of Ce ceramics:The preparation of Ce monocrystalline is more
Difficulty, starts to require high melt temperature and strict control atmosphere to eliminate pore until melting from powder.YAG:Ce glass is made pottery
Prepared by porcelain has glass melting temperature relatively low, with short production cycle, the advantages of low production cost, can overcome monocrystalline and transparent
Ceramics prepare on difficulty, in addition compared with powder, better heat stability, light decay is less, and the colour temperature amplitude of accommodation is wider, light compared with
Uniformly, it is expected to substitute powder.
Refractive index height (n=1.84) of YAG fluorescent powder particle, the refractive index low (n ≈ 1.5) of epoxy resin/silica gel, they
Mixing will cause light scattering loss serious and light extraction efficiency is low.Chinese scholars expert has been made that substantial amounts of work
Go to solve the problems, such as LED.In order to develop the fluorescent material of superior luminescence performance：They are carried out at the synthesis technique to fluorescent material
It is modified, using post-processing approach the stability of fluorescent material is improve, and phosphor surface is wrapped using chemical method
Film process makes the physical and chemical stability of fluorescent material more excellent；The matrix of fluorescent material is changed, glass, devitrified glass, pottery is such as used instead
Porcelain etc. is improved the coating processes of fluorescent material；Low-melting glass ceramics are compared with silica gel with resin, are had under light illumination
Excellent heat endurance, can effectively fill up the deficiency of LED encapsulation.
Although preparing low melting point YAG:The document and patent of Ce fluorescent glass methods is disclosed report, but sums up general
Store-through is in two subject matters：One, the preparation technology of glass is more complicated, needs the technique that two steps are melted-cooled down to complete, and makes
Energy resource consumption is very big during standby；Two, Material composition design is unreasonable, and the refractive index of fluorescent powder grain and host glass is too
Greatly, the fluorescent glass transparency prepared is low, and optical property is poor.
Wuhan University of Technology application Chinese invention patent CN101643315B, " low-melting-point fluorescent glass for white light LED and
Disclose containing YAG in its preparation method ":The preparation method of the low-melting-point fluorescent glass of Ce phases, host glass consists of SiO2-
Al2O3-B2O3-CaO-ZnO-Na2O-MgO, fusion temperature is 900 DEG C -1300 DEG C.
In prior art, the preparation temperature of glass ceramics is general all more than 800 DEG C, and such as CN104445957A is " a kind of
In oxyfluoride tellurate glass ceramics ", glass smelting temperature is 1100 DEG C；Patent CN102390932B " fluoride nanometer
In brilliant transparent oxyfluoride tellurate glass ceramics ", glass smelting temperature is 850 DEG C -1100 DEG C, patent CN105198211A
In " a kind of glass powder with low melting point and preparation method thereof ", glass melting temperature is 1000 DEG C -1300 DEG C.
The content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of low melting point tellurate glass it is ceramic,
Preparation method and applications.Preparation process is simple of the present invention, glass melting temperature are low, and the consumption energy is few, with short production cycle.The glass for obtaining
The advantages of glass ceramics have low melting glass, high heat conductance and life-span length.
Technical solution of the present invention is specifically described as follows.
A kind of low melting point tellurate glass ceramics, it is made up of frit with YAG fluorescent powder two parts；Wherein：It is described
Frit is made up of the component of following mole percent, 50-70mol%TeO2, 10-30mol%Na2O, 5-25mol%ZnO,
Each component molar fraction sum is 100%；The quality of the fluorescent material is the 6-10% of frit gross mass.
In the present invention, effective material Na2The source of O is Na2CO3。
In the present invention, the YAG fluorescent powder is YAG:Ce fluorescent material.
In the present invention, TeO2Molar fraction be 53-65mol%, Na2The molar fraction of O is 13-26mol%, and ZnO's rubs
Your fraction is 9-22mol%.
In the present invention, TeO2Molar fraction be 55-64mol%, Na2The molar fraction of O is preferably 14-24mol%, ZnO
Molar fraction be preferably 10-22mol%.
In the present invention, the quality of fluorescent material is the 7-9% of frit gross mass.
The present invention also provides a kind of preparation method of above-mentioned low melting point tellurate glass ceramics, comprises the following steps that：First
By TeO2, Na2O, ZnO, YAG fluorescent powder is well mixed to be poured into crucible, and in the Muffle furnace of 500-700 DEG C of temperature 0.5h- is melted
2h；Then glass metal is poured on the mould that temperature is 180-220 DEG C and is made annealing treatment, temperature to be annealed is cooled to room temperature,
Obtain low melting point tellurate glass ceramics.
In the present invention, muffle furnace is 500-600 DEG C, and the melting time is 0.5-1h.
In the present invention, crucible is corundum crucible；Mould is pig mold.
Further, the present invention provides a kind of application of above-mentioned low melting point tellurate glass ceramics in white light LEDs field.This
The obtained glass ceramics of invention excites the strong white light of lower generation in 460nm blue light sources, can be applicable to white light LEDs.
Compared to the prior art, the beneficial effects of the present invention is：
(1) present invention is by introducing Na2O components make tellurate melt temperature be down to 500-700 DEG C, and glass melting temperature is low, drop
The low energy ezpenditure of preparation process, and production cost is reduced by using alumina crucible；
(2) preparation method is simple, with short production cycle, and direct frit is made pottery with the direct mixed melting of fluorescent material into glass
Porcelain, by adjusting the doping ratio of fluorescent material luminous strong and weak different glass ceramics is obtained, the luminous intensity of glass ceramics first with
The increase of fluorescent material ratio and strengthen, weaken with the increase of fluorescent material ratio within the specific limits afterwards；
Description of the drawings
Fig. 1 is the launching light spectrogram of the glass ceramics of embodiment 1.
Fig. 2 is the exciting light spectrogram of the glass ceramics of embodiment 1.
Fig. 3 is the launching light spectrogram of the glass ceramics of embodiment 2.
Fig. 4 is the exciting light spectrogram of the glass ceramics of embodiment 2.
Fig. 5 is the launching light spectrogram of the glass ceramics of embodiment 3.
Fig. 6 is the exciting light spectrogram of the glass ceramics of embodiment 3.
Fig. 7 is the luminous photo of sample after the glass ceramics of embodiment 1 is coupled with blue chip.
Specific embodiment
Below will present invention is described by specific embodiment.
Embodiment 1
By analytically pure TeO2, Na2O, ZnO, YAG fluorescent powder, according to 63mol%TeO2, 22mol%Na2O, 15mol%
ZnO, 7wt% fluorescent material is (with TeO2, Na2The ZnO gross mass meters of O) be precisely weighed after, in being placed in agate mortar, after grinding is uniform
In being placed in corundum crucible, it is put into 550 DEG C of Muffle furnace and melts 1 hour, glass melts are poured on 180 DEG C of pig mold afterwards
Made annealing treatment, treated that temperature is down to room temperature and takes out glass ceramics.
Using glass ceramics of the XRF (FLS8900, Edinburgh, Britain Instruments company) to above-mentioned gained
It is measured, spectrogram such as Fig. 1 of gained, shown in Fig. 2, in the case where 460nm wavelength is excited, its launch wavelength is located at 576nm, correspondence
In Ce3+5D1→2F7/2, using Hangzhou distant place STC4000 rapid spectrometers by the blue chip coupling of glass ceramics and 460nm
Close, send bright white light, as shown in Figure 7.
Embodiment 2
By analytically pure TeO2, Na2O, ZnO, YAG fluorescent powder, according to 63mol%TeO2, 22mol%Na2O, 15mol%
ZnO, 8wt% fluorescent material is (with TeO2, Na2The ZnO gross mass meters of O) be precisely weighed after, in being placed in agate mortar, after grinding is uniform
In being placed in corundum crucible, it is put into 600 DEG C of Muffle furnace and melts 1 hour, glass melts are poured on 200 DEG C of pig mold afterwards
Made annealing treatment, treated that temperature is down to room temperature and takes out glass ceramics.
Using glass ceramics of the XRF (FLS8900, Edinburgh, Britain Instruments company) to above-mentioned gained
It is measured, transmitting spectrogram such as Fig. 3 of gained, shown in Fig. 4, in the case where 460nm wavelength is excited, its launch wavelength is located at 576nm,
Corresponding to Ce3+5D1→2F7/2, using Hangzhou distant place STC4000 rapid spectrometers by the blue chip of glass ceramics and 460nm
Coupling, sends bright white light, and it is higher than embodiment 1 and embodiment 3 to measure light efficiency.
Embodiment 3
By analytically pure TeO2, Na2O, ZnO, YAG fluorescent powder, according to 60mol%TeO2, 22mol%Na2O, 18mol%
ZnO, 9wt% fluorescent material is (with TeO2, Na2The ZnO gross mass meters of O) be precisely weighed after, in being placed in agate mortar, after grinding is uniform
In being placed in corundum crucible, it is put into 700 DEG C of Muffle furnace and melts 1 hour, glass melts are poured on 220 DEG C of pig mold afterwards
Made annealing treatment, treated that temperature is down to room temperature and takes out glass ceramics.
Using glass ceramics of the XRF (FLS8900, Edinburgh, Britain Instruments company) to above-mentioned gained
It is measured, transmitting spectrogram such as Fig. 5 of gained, shown in Fig. 6, in the case where 460nm wavelength is excited, its launch wavelength is located at 576nm,
Corresponding to Ce3+5D1→2F7/2, using Hangzhou distant place STC4000 rapid spectrometers by the blue chip of glass ceramics and 460nm
Coupling, sends bright white light, measures that light efficiency is higher than embodiment 1, but lower than embodiment 2.
Claims (9)
1. a kind of low melting point tellurate glass is ceramic, it is characterised in that it is made up of frit with YAG fluorescent powder two parts；
Wherein：The frit is made up of the component of following mole percent, 50-70mol%TeO2, 10-30mol%Na2O, 5-
25mol%ZnO, each component molar fraction sum is 100%；The quality of the fluorescent material is the 6- of frit gross mass
10%.
2. low melting point tellurate glass according to claim 1 ceramics, it is characterised in that the YAG fluorescent powder is
YAG:Ce fluorescent material.
3. low melting point tellurate glass according to claim 1 is ceramic, it is characterised in that TeO2Molar fraction be
53-65mol%, Na2The molar fraction of O is 13-26mol%, and the molar fraction of ZnO is 9-22mol%.
4. low melting point tellurate glass according to claim 1 is ceramic, it is characterised in that TeO2Molar fraction be
55-64mol%, Na2The molar fraction of O is preferably 14-24mol%, and the molar fraction of ZnO is preferably 10-22mol%.
5. low melting point tellurate glass according to claim 1 is ceramic, it is characterised in that the quality of fluorescent material is that glass is former
The 7-9% of material gross mass.
6. a kind of preparation method of low melting point tellurate glass according to claim 1 ceramics, it is characterised in that concrete step
It is rapid as follows：First by TeO2, Na2O, ZnO, YAG fluorescent powder is well mixed to be poured into crucible, in the Muffle furnace of 500-700 DEG C of temperature
Middle melting 0.5h-2h；Then glass metal is poured on the mould that temperature is 180-220 DEG C and is made annealing treatment, temperature to be annealed
Room temperature is cooled to, low melting point tellurate glass ceramics are obtained.
7. preparation method according to claim 6, it is characterised in that muffle furnace is 500-600 DEG C, the melting time is
0.5-1h。
8. preparation method according to claim 6, it is characterised in that crucible is corundum crucible；Mould is pig mold.
9. application of a kind of low melting point tellurate glass ceramics according to claim 1 in white light LEDs field.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611238050.9A CN106630604A (en) | 2016-12-28 | 2016-12-28 | Low-melting-point tellurate glass ceramic, preparation method and application of low-melting-point tellurate glass ceramic |
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| CN201611238050.9A CN106630604A (en) | 2016-12-28 | 2016-12-28 | Low-melting-point tellurate glass ceramic, preparation method and application of low-melting-point tellurate glass ceramic |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384533A (en) * | 2018-04-27 | 2018-08-10 | 上海应用技术大学 | A kind of thiazole fluorescent crystal material and preparation method thereof |
| CN113860744A (en) * | 2021-10-18 | 2021-12-31 | 昆明理工大学 | Novel microcrystalline glass sodium molybdate preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| 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 |
| CN105523715A (en) * | 2015-06-18 | 2016-04-27 | 温州大学 | Low-melting point transparent fluorescent glass and its preparation method and use in white light LED |
-
2016
- 2016-12-28 CN CN201611238050.9A patent/CN106630604A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101643315A (en) * | 2009-08-10 | 2010-02-10 | 武汉理工大学 | Low-melting-point fluorescent glass for white light LED and preparation method thereof |
| 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 |
| CN105523715A (en) * | 2015-06-18 | 2016-04-27 | 温州大学 | Low-melting point transparent fluorescent glass and its preparation method and use in white light LED |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108384533A (en) * | 2018-04-27 | 2018-08-10 | 上海应用技术大学 | A kind of thiazole fluorescent crystal material and preparation method thereof |
| CN113860744A (en) * | 2021-10-18 | 2021-12-31 | 昆明理工大学 | Novel microcrystalline glass sodium molybdate preparation method |
| CN113860744B (en) * | 2021-10-18 | 2024-01-26 | 昆明理工大学 | Preparation method of microcrystalline glass sodium molybdate |
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