CN105399325B - For the Ce of white light LEDs：YAG fluorescent glass and preparation method thereof - Google Patents
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- CN105399325B CN105399325B CN201510717960.4A CN201510717960A CN105399325B CN 105399325 B CN105399325 B CN 105399325B CN 201510717960 A CN201510717960 A CN 201510717960A CN 105399325 B CN105399325 B CN 105399325B
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Abstract
The present invention provides a kind of low softening point Ce for white light LEDs：YAG fluorescent glass and preparation method thereof is to uniformly disperse to have Ce in oxide glass matrix：YAG crystallites, the Ce：The additive amount of YAG crystallites is the 1~20% of oxide glass matrix weight.The preparation method of the fluorescent glass includes the following steps：By several oxide powders after mixing, it melts, obtains glass melt；The glass melt is quickly poured into cold water, obtains glass disintegrating slag；After the glass disintegrating slag is smashed to pieces and wears into uniform powder, sieving；By the glass powder Ce after sieving：YAG fluorescent microcrystallines after mixing, take out after heating, and molding obtains green body；The green body is annealed, obtains white light LEDs low softening point Ce：YAG fluorescent glass.Inventive formulation component is few, and cost of material is low, and glass softening point is low, and manufacture craft is simple, is suitble to mass production.Obtained fluorescent glass material transparent degree is high.
Description
Technical field
The present invention relates to a kind of white light LEDs low softening point Ce：YAG fluorescent glass and preparation method thereof belongs to luminous material
Material field.
Background technology
At present, white light emitting diodes (LED) headlamp has the various aspects such as energy-saving and environmental protection, long-life, strong designability
Advantage receives the very big concern of people, just gradually replaces traditional incandescent lamp, fluorescent lamp.The side that common white light LEDs are realized
The fluorescent powder of transmitting yellow light that formula can be stimulated by blue light for coating on blue-light LED chip, blue light and yellow light are mixed to form white light.But
Be coating fluorescent powder need before overcoating with the thermal conductivity of adhesives such as the mixing of the binding agents such as epoxy resin, epoxy resin and
Poor chemical stability, the easy aging of epoxy resin, the easy light decay of fluorescent material cause white LED lamp colour cast, failure.
For this problem, area research person has carried out various effort.It is viscous that organic material researcher studies epoxy resin etc.
Agent is tied, improves the thermal conductivity and chemical stability of binding agent, but this work at present need further to carry out or improve；Fluorescence
Powder researcher improves the stability of fluorescent powder by studying synthesizing formula, technique and the post processing of fluorescent powder.
In recent years, and there is a kind of fluorescent glass material, it is that answering for fluorescent grain is uniformly distributed in unorganic glass matrix
Condensation material.The thermal conductivity of glass is bigger than epoxy adhesive, and chemical stability is high, can make it with effective protection fluorescent grain
Photochromic stabilization, service life are long.Therefore, this mode of luminizing can be replaced, effectively solves the problems, such as white light LEDs light decay.
The certain patented technologies for white-light LED fluorescence glass material occurred at present are as follows：
The patent that the PCT Publication of Nippon Electric Glass Co., Ltd and Kyoto University's application is WO 2005/097938A1
" fluorescent material and LED " is disclosed a kind of containing Ce:The fluorescent glass of YAG fluorescence crystalline phases.Due to being mainly in glass matrix component
Sieve and silica-sesquioxide, material transparent is poor, the reasons such as crystallite lattice defect is more that high temperature crystallization is precipitated, cause its luminous efficiency compared with
It is low.
Wuhan University of Technology has applied for the patent of Chinese invention patent CN101643315B, and " white light LEDs low softening point is glimmering
Light glass and preparation method thereof " discloses a kind of containing Ce:The fluorescent glass of YAG fluorescence crystalline phases, glass matrix component are Na2O-
ZnO-B2O3-SiO2-Al2O3-CaO-MgO-K2O, glass ingredient substance is more, and the vitreum transparency is relatively low, leads to illumination effect
It is bad.
The patent of Chinese patent CN103183473A " is used for the Ce of white light LEDs:YAG devitrified glasses and preparation method thereof ",
It discloses a kind of containing Ce:The fluorescent glass of YAG fluorescence crystalline phases, glass matrix component are TeO2-GeO2-ZnO-K2O-SiO2-B2O3-
Sb2O3..., TeO in the raw material of glass ingredient2、GeO2Etc. expensive, the scale life of unsuitable civil LED fluorescent material
Production.
Invention content
The purpose of the present invention is to provide of low cost, the simple Ce of manufacture craft of one kind:YAG fluorescent glass and its preparation
Method.Material prescription component is few, and sintering temperature is low, and obtained fluorescent glass transparency is high, can be combined with blue-ray LED and realize white light
LED。
In a first aspect, the present invention provides a kind of low softening point Ce for white light LEDs：YAG fluorescent glass is in oxygen
Being uniformly dispersed in compound glass matrix has Ce：YAG crystallites, the Ce：The additive amount of YAG crystallites is oxide glass matrix weight
1~20%.
Preferably, the oxide glass matrix by the following component of mole percent by being formed：
PbO：0~60%；B2O3：20~60%；ZnO：0~30%, SiO2：0~10%.
Preferably, the Ce：The additive amount of YAG crystallites is the 2~8% of oxide glass matrix weight.
Second aspect, the present invention also provides a kind of low softening point Ce：The preparation method of YAG fluorescent glass, including such as
Lower step：
A) by PbO, B2O3, ZnO, SiO2 powder after mixing, melted at 500~1100 DEG C, obtain glass melt；
B) glass melt is quickly poured into cold water, obtains glass disintegrating slag, be poured into water to reach rapidly cold rapidly
But effect；
C) after the glass disintegrating slag is smashed to pieces and wear into uniform powder, 100~325 mesh sieve is crossed；
D) by the glass powder Ce after sieving：YAG fluorescent microcrystallines after mixing, at 500~700 DEG C keep the temperature 20~
It is taken out after 60min, is molded, obtains green body；
The green body at 200~400 DEG C is annealed, obtains white light LEDs low softening point Ce：YAG fluorescent glass.
The third aspect, the present invention also provides another low softening point Ce：The preparation method of YAG fluorescent glass, including
Following steps：
A) glass for softening temperature being less than 500~700 DEG C and being melted completely at this temperature is at 500~1100 DEG C
Lower fusing, obtains glass melt；
B) glass melt is quickly poured into cold water, obtains glass disintegrating slag；
C) after the glass disintegrating slag is smashed to pieces and wear into uniform powder, 100~325 mesh sieve is crossed；
D) by the glass powder Ce after sieving：YAG fluorescent microcrystallines after mixing, at 500~700 DEG C keep the temperature 20~
It is taken out after 60min, is molded, obtains green body；
E) green body at 200~400 DEG C is annealed, obtains white light LEDs low softening point Ce：YAG fluorescent glass.
Glass formula in this technology, will not be with Ce：YAG powder chemically reacts, and softening point is low, forms glass dust
Afterwards with Ce：YAG powder mixes, and need to handle molding under the lower temperature at 500~700 DEG C at this time.According to common glass, melt
Change the temperature range of (non-softening) higher than 700 DEG C, the Ce mixed：The fluorescence property of YAG powder will fail significantly.
The fluorescent glass internal structure is uniformly has inlayed Ce in oxide glass matrix：YAG crystallites are excited in blue light
Under the conditions of, it can be achieved that yellow emission, so as to combine generation white light.
Compared with prior art, the present invention proposes fluorescent glass and its preparation side of a kind of cheap, new component formula
Method, softening point is low, simple for process, and material prescription component is few, and cost of material is low, can guarantee white-light LED fluorescence material durability,
Stability.
Description of the drawings
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is the photo in kind of 1 fluorescent glass of embodiment；
Fig. 2 is the pictorial diagram after being encapsulated together with the fluorescent glass and blue chip prepared using embodiment 1；
Fig. 3 is blue chip light source light spectrogram；
Spectrogram after being encapsulated together with the fluorescent glass and blue chip that Fig. 4 is prepared using embodiment 1；
White light chromaticity diagram after being encapsulated together with the fluorescent glass and blue chip that Fig. 5 is prepared using embodiment 1.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
A kind of white light LEDs low softening point Ce：YAG fluorescent glass and preparation method thereof, it is carried out successively in the steps below：
By PbO, B2O3、ZnO、SiO2Powder material weighs according to a certain percentage, is uniformly mixed, spare；
By uniformly mixed powder uniform melt, 500~1100 DEG C of fusion temperature keeps the temperature 1~3 hour, obtains glass and melt
Body；Glass melt is quickly poured into cold water, obtains glass disintegrating slag；
Glass disintegrating slag is smashed to pieces and wears into uniform powder, and powder is crossed into 100~325 mesh sieve；
By glass powder and the Ce of certain mass：YAG fluorescence micro mists (Ce：The content of YAG fluorescence micro mists is glass matrix
1~20wt%) uniformly mixing, it is spare；
Uniformly mixed glass-fluorescent powder is directly placed into 500~700 DEG C of resistance furnaces of temperature, heat preservation 20~
60min；
It is taken out after heat preservation, pours into shape needed for die for molding rapidly, be placed in the resistance furnace of 200~400 DEG C of temperature
Annealing cooling, so as to obtain white light LEDs low softening point Ce：YAG fluorescent glass.
Embodiment 1
By 48%PbO：33%B2O3：14%ZnO：5%SiO2(mol ratios) weighs powder material, is melted after mixing, temperature
It is 800 DEG C to spend, and keeps the temperature 3 hours, after obtaining glass dust by above-mentioned steps, adds in the Ce of 3wt%：YAG fluorescence micro mists are used after mixing
Crucible is held, and is directly placed into 600 DEG C of resistance furnace, keeps the temperature 30min aftershapings, and 300 DEG C of annealing temperature obtains fluorescent glass
Piece.
Fluorescent glass piece such as Fig. 1, observation show that material homogeneity prepared by the technique is good, contain yttrium-aluminium-garnet crystalline phase
(YAG) it has been evenly distributed in glass matrix.Fluorescent glass piece encapsulates after grinding and polishing together with blue chip, in kind
Such as Fig. 2.Fig. 3 is blue spectrum figure, and peak wavelength 450nm, under blue light excitation, which emits yellow light,
White light is combined into the blue light of blue chip transmitting, as shown in Fig. 4 spectrograms.From Fig. 5 chromaticity diagrams it is found that positioned at positive white light area
Domain belongs to positive white light.
Embodiment 2
By 48%PbO：33%B2O3：14%ZnO：5%SiO2(mol ratios) weighs powder material, is melted after mixing, temperature
It is 800 DEG C to spend, and keeps the temperature 3 hours, after obtaining glass dust by above-mentioned steps, adds in the Ce of 5wt%：YAG fluorescence micro mists are used after mixing
Crucible is held, and is directly placed into 600 DEG C of resistance furnace, keeps the temperature 30min aftershapings, and 300 DEG C of annealing temperature obtains fluorescent glass
Piece.Blue light after grinding and polishing with blue chip transmitting is combined into positive white light.
Embodiment 3
By 48%PbO：33%B2O3：14%ZnO：5%SiO2(mol ratios) weighs powder material, is melted after mixing, temperature
It is 800 DEG C to spend, and keeps the temperature 3 hours, after obtaining glass dust by above-mentioned steps, adds in the Ce of 2wt%：YAG fluorescence micro mists are used after mixing
Crucible is held, and is directly placed into 600 DEG C of resistance furnace, keeps the temperature 30min aftershapings, and 300 DEG C of annealing temperature obtains fluorescent glass
Piece.Blue light after grinding and polishing with blue chip transmitting is combined into positive white light.
Embodiment 4
By 52%PbO：33%B2O3：10%ZnO：5%SiO2(mol ratios) weighs powder material, is melted after mixing, temperature
It is 800 DEG C to spend, and keeps the temperature 3 hours, after obtaining glass dust by above-mentioned steps, adds in the Ce of 3wt%：YAG fluorescence micro mists are used after mixing
Crucible is held, and is directly placed into 600 DEG C of resistance furnace, keeps the temperature 30min aftershapings, and 300 DEG C of annealing temperature obtains fluorescent glass
Piece.Blue light after grinding and polishing with blue chip transmitting is combined into positive white light.
Embodiment 5
By 52%PbO：33%B2O3：10%ZnO：5%SiO2(mol ratios) weighs powder material, is melted after mixing, temperature
It is 800 DEG C to spend, and keeps the temperature 3 hours, after obtaining glass dust by above-mentioned steps, adds in the Ce of 5wt%：YAG fluorescence micro mists are used after mixing
Crucible is held, and is directly placed into 600 DEG C of resistance furnace, keeps the temperature 30min aftershapings, and 300 DEG C of annealing temperature obtains fluorescent glass
Piece.Blue light after grinding and polishing with blue chip transmitting is combined into positive white light.
Embodiment 6
By 52%PbO：33%B2O3：10%ZnO：5%SiO2(mol ratios) weighs powder material, is melted after mixing, temperature
It is 800 DEG C to spend, and keeps the temperature 3 hours, after obtaining glass dust by above-mentioned steps, adds in the Ce of 2wt%：YAG fluorescence micro mists are used after mixing
Crucible is held, and is directly placed into 600 DEG C of resistance furnace, keeps the temperature 30min aftershapings, and 300 DEG C of annealing temperature obtains fluorescent glass
Piece.Blue light after grinding and polishing with blue chip transmitting is combined into positive white light.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (1)
1. a kind of Ce：The preparation method of YAG fluorescent glass, which is characterized in that include the following steps：
By 48%PbO：33%B2O3：14%ZnO：5%SiO2Molar ratio weigh powder material, melt after mixing, temperature is
800 DEG C, 3 hours are kept the temperature, after obtaining glass dust by above-mentioned steps, adds in the Ce of 3wt%：YAG fluorescence micro mists use crucible after mixing
It holds, is directly placed into 600 DEG C of resistance furnace, keep the temperature 30min aftershapings, 300 DEG C of annealing temperature obtains fluorescent glass piece.
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| CN201510717960.4A CN105399325B (en) | 2015-04-17 | 2015-10-29 | For the Ce of white light LEDs：YAG fluorescent glass and preparation method thereof |
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| CN2015101840754 | 2015-04-17 | ||
| CN201510717960.4A CN105399325B (en) | 2015-04-17 | 2015-10-29 | For the Ce of white light LEDs：YAG fluorescent glass and preparation method thereof |
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| CN105399325B true CN105399325B (en) | 2018-06-22 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106542739A (en) * | 2016-10-24 | 2017-03-29 | 中国人民大学 | A kind of Ce:YAG yellow glass ceramics and preparation method and application |
| CN106816521B (en) * | 2016-12-26 | 2019-06-14 | 温州大学 | A kind of interlayer fluorescent glass and its preparation method and application |
| CN106800371B (en) * | 2017-01-25 | 2019-12-03 | 上海应用技术大学 | A kind of high thermal conductivity coefficient borosilicate fluorescent glass material and preparation method thereof |
| 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 |
| CN108281535A (en) * | 2018-02-02 | 2018-07-13 | 温州大学 | Composite fluorescence laminated glass and preparation method thereof and the application on white light LEDs |
| CN109111120B (en) * | 2018-10-26 | 2021-09-21 | 浙江工业大学 | Spontaneous crystallization fluorescent microcrystalline glass for warm white LED and preparation method thereof |
| JP2021081460A (en) * | 2019-11-14 | 2021-05-27 | 大電株式会社 | Optical wavelength conversion member and light source device |
| CN112645592B (en) * | 2020-12-23 | 2022-07-05 | 温州大学 | Preparation and application of efficient adjustable composite fluorescent glass material |
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|---|---|---|---|---|
| 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 |
| CN102121591A (en) * | 2010-12-23 | 2011-07-13 | 大连海事大学 | White LED light source and manufacturing method of phosphor thereof |
| CN102574727A (en) * | 2009-10-15 | 2012-07-11 | 旭硝子株式会社 | Glass for diffusion layer in organic led element, and organic led element utilizing same |
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2015
- 2015-10-29 CN CN201510717960.4A patent/CN105399325B/en active Active
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 |
| CN102574727A (en) * | 2009-10-15 | 2012-07-11 | 旭硝子株式会社 | Glass for diffusion layer in organic led element, and organic led element utilizing same |
| CN102121591A (en) * | 2010-12-23 | 2011-07-13 | 大连海事大学 | White LED light source and manufacturing method of phosphor thereof |
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Effective date of registration: 20220824 Address after: Room 702, Building 12, No. 2, Xingye Road, Songshan Lake Park, Dongguan City, Guangdong 523000 Patentee after: Zhongke Haoye (Dongguan) material technology Co.,Ltd. Address before: 100086 room 5A, Hing Fat mansion, 45 Zhongguancun Avenue, Haidian District, Beijing. Patentee before: Beijing Hui Yao Xingguang ceramic material technology Co.,Ltd. |
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