CN108503216A - A kind of preparation method and fluorescent glass of fluorescent glass - Google Patents
A kind of preparation method and fluorescent glass of fluorescent glass Download PDFInfo
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- CN108503216A CN108503216A CN201810462517.0A CN201810462517A CN108503216A CN 108503216 A CN108503216 A CN 108503216A CN 201810462517 A CN201810462517 A CN 201810462517A CN 108503216 A CN108503216 A CN 108503216A
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- glass
- fluorescent
- fluorescent glass
- preparation
- red fluorescence
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Classifications
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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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/10—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce uniformly-coloured transparent products
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
-
- 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
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
Abstract
The invention discloses a kind of preparation method of fluorescent glass and fluorescent glass, belong to the method for manufacturing fluorescent material fields LED, and preparation method includes the following steps：1. glass raw material and LuAG fluorescent powders are ground obtains fluorescent glass mixture；2. fluorescent glass mixture is sintered in Muffle furnace, melten glass material is obtained；3. melten glass material is made annealing treatment, fluorescent glass is obtained after cooling；4. adjusting the thickness of fluorescent glass；5. the uniform sizing material of red fluorescence powder and organic bond is carried out vacuum defoamation processing, slurry is coated in fluorescent glass surface using spin coating equipment；It is heat-treated 6. above-mentioned fluorescent glass is put into, is cut after cooling.The preparation method of the fluorescent glass of the present invention simplifies the technique for preparing fluorescent glass, easily mass produces.The fluorescent glass of the present invention inhibits harmful light scattering, improves the transparency and luminous efficiency of fluorescent glass.High color rendering index (CRI), the warm white of low color temperature are obtained.
Description
Technical field
The invention belongs to the method for manufacturing fluorescent material fields LED more particularly to a kind of use spin coating method to prepare LED
The fluorescent glass that encapsulation is extremely prepared with the method for high-color rendering fluorescent glass.
Background technology
White light LEDs are multi-party since high, small with brightness, response is fast, long lifespan, environmental protection and energy saving, designability are strong etc.
The advantages of face, is just gradually replacing the conventional illumination sources such as incandescent lamp, fluorescent lamp, it is considered to be 21 century most potential illumination light
Source.
Currently, commercial common white light LEDs are mainly by doping yellow YAG:The silica gel or epoxy resin of Ce fluorescent powders
It is encapsulated in and realizes on GaInN blue chips.The heat conductivility and thermal stability of this encapsulating material are poor, in permanent worker
Easily occur the problem of jaundice and aging under the conditions of work, and then the serious drift of the chromaticity coordinates of white light LEDs and service life can be caused
Shorten.In addition, yellow YAG:The refractive index of Ce fluorescent powder grains (n ≈ 1.84) and epoxy resin or silica gel (n ≈ 1.55) is less
Matching, when work, can cause harmful light scattering, influence the luminous efficiency of white light LEDs.Some scholar experts have proposed fluorescence
Powder, which is evenly distributed in the inorganic material such as glass, to be gone to solve problem above existing for white light LEDs.Have with epoxy resin or silica gel etc.
Machine adhesive is compared, and the thermal conductivity of glass is high, and stable chemical performance can make its photochromic stabilization with effective protection fluorescent powder grain,
Luminous efficiency improves, and service life extends.
The certain patented technologies for inorganic phosphors materials such as white-light LED fluorescence glass occurred at present are as follows：
102060441 A of Chinese patent CN disclose a kind of YAG of high-crystallinity：Ce fluorescent glass ceramics and its preparation
Method, it is characterized in that by Al2O3、Y2O3、Na2B4O7And R2O3Raw material is uniformly mixed, and then carries out high-temperature fusion, Annealing Crystallization, system
Obtain the fluorescent glass ceramics of high-crystallinity.Its melting temperature is higher (1500-1650 DEG C), and annealing, crystallization process need strictly
Technological parameter is controlled, large-scale commercial production is unfavorable for.
105399325 A of Chinese patent CN disclose the Ce for white light LEDs:YAG fluorescent glass and preparation method thereof,
It is characterized in that by PbO, B2O3, ZnO and SiO2Raw material is uniformly mixed, and then carries out high-temperature fusion (1000 DEG C or so), water quenching obtains
Glass disintegrating slag, then glass disintegrating slag powder and YAG that will smash to pieces:Ce fluorescent powder mixed sinterings are at fluorescent glass.The fluorescent glass is given birth to
Toxic raw materials PbO has been used in production, has been unfavorable for keeping the safety in production, and preparation process is more complex time-consuming, in addition, the fluorescent glass encapsulates
White light be cool white light, colour temperature is higher, show refer to it is relatively low, may not apply to room lighting field.
107265873 A of Chinese patent CN disclose a kind of white-light LED encapsulation low-melting-point fluorescent glass piece and its preparation
Method, it is characterized in that by B2O3、ZnO、SiO2、Na2CO3、CaCO3And Al2O3Raw material is uniformly mixed, and then carries out high-temperature fusion
(1100-1200 DEG C), glass metal is poured on grinding tool and obtains host glass, then host glass is ground into micron-sized glass
Powder, with YAG：Ce yellow fluorescent powders are sintered obtain fluorescent glass after evenly mixing.The transparency of the fluorescent glass is relatively low, and fluorescence
Glass ingredient is more, and preparation process is cumbersome to be taken, and the cost is relatively high, and light is obtained by addition adulterating single yellow fluorescent powder
Cool white light may not apply to require the high aobvious lighting area for referring to low color temperature.
Therefore, develop a kind of fluorescent glass encapsulating material for high aobvious index, low color warm white light LEDs have it is great
Commercial value.
Invention content
In order to solve deficiencies of the prior art, LED is prepared using spin coating method the present invention provides a kind of
The method of encapsulation high-color rendering fluorescent glass.By selecting the oxide raw material of low melting point, glass ingredient type, matching are reduced
The refractive index of raw mixture and fluorescent powder simplifies preparation process and has prepared low transparency height, fusing point, safety and environmental protection, shone
Uniformly, the fluorescent glass for the features such as easy processing, luminous efficiency are high, thermal conductivity is good recycles spin coating process addition red glimmering
Light powder goes compensation emitting red light defect, obtain showing high aobvious index, low color temperature warm white fluorescent glass, be applied to indoor photograph
Bright equal fields.
To achieve the above object, the technical scheme is that：A kind of preparation method of fluorescent glass, it is characterised in that：
Include the following steps：
(1) glass raw material and LuAG fluorescent powders are sufficiently mixed in mortar, grind and obtains fluorescent glass mixture；It is described
Glass raw material is by TeO2、H3BO3, ZnO and Na2CO3Composition；
(2) the fluorescent glass mixture is poured into after crucible and is sintered in Muffle furnace, obtain melten glass material；
(4) the melten glass material is made annealing treatment, is cooled to room temperature to form transparent fluorescent glass；
(4) thickness of the fluorescent glass is adjusted；
(5) uniform sizing material of red fluorescence powder and organic bond is subjected to vacuum defoamation processing, is set using rotary coating
It is standby that slurry is coated in green fluorescence glass surface；
(6) fluorescent glass coated with red fluorescence powder is put into drying box and is heat-treated, is cooled to room temperature
After cut, be then encapsulated on LED blue chips and generate warm white.
Further, glass components described in the step (1) are calculated as by mole percent：TeO240-
60mol%, H3BO35-20mol%, ZnO 5-25%, Na2CO310-35%.
Further, LuAG fluorescent powders described in the step (1) are Lu3Al5O12：Ce3+Fluorescent powder, the LuAG fluorescence
The quality of powder is the 5-20% of glass raw material gross mass.
Further, muffle furnace described in the step (2) is set as 400-750 DEG C, and the crucible is corundum earthenware
Crucible, described to be sintered to Isothermal sinter, the Isothermal sinter time is 0.5-2.5 hours.
Further, the step (3) is specially that the melten glass material is poured into the mold that temperature is 150-450 DEG C
On, the mold is pig mold, is placed in and keeps the temperature 2-4 hours in Muffle furnace and anneal, is cooled to room temperature to obtain later transparent glimmering
Light glass.
Further, the step (4) is machined into the thickness of method adjustment fluorescent glass between 0.5-2mm.
Further, red fluorescence powder described in the step (5) is CaAlSiN3：Eu2+, the matter of the red fluorescence powder
Amount is the 5-20% of organic bond gross mass, and the vacuum defoamation time is 0.5-2 hours.
Further, the temperature setting of drying box described in the step (6) is 100-200 DEG C, the heat treatment time
It is 0.5-1.5 hours.
Further, a length of 2-10mm, width 2-10mm of glass sample described in the step (6).
Fluorescent glass made from preparation method by above-mentioned fluorescent glass.
The above-mentioned fluorescent glass coated with red fluorescence powder is encapsulated on LED blue chips and generates warm white, can be applicable to
The fields such as room lighting.
The present invention has the advantages that：
First, the method that the present invention first uses the low temperature co-fired knot of a step prepares LuAG fluorescent glass, then uses rotary coating
Method coated red fluorescent powder.The technique for preparing fluorescent glass is simplified, the production cycle is shortened, is easily mass produced.
Second, the present invention, as major glass raw material, is reduced melting temperature, reduces life using the tellurate of low melting point
Produce cost；By using the tellurate raw material of high refractive index, make the refractive index of glass raw material and the refractive index close of fluorescent powder, presses down
Harmful light scattering has been made, the transparency and luminous efficiency of fluorescent glass are improved.
Red fluorescence powder is deposited on green fluorescence glass surface using spin coating method, passes through adjusting by third, the present invention
The concentration of red fluorescence powder has obtained high color rendering index (CRI), the warm white of low color temperature.
Description of the drawings
The electroluminescent light spectrogram of fluorescent glass made from Fig. 1 embodiments 1, example 2 and example 3；
The CIE chromaticity coordinates figures of Fig. 2 embodiments 1, example 2, fluorescent glass made from example 3.
Specific implementation mode
With reference to specific embodiments and the drawings 1 and 2 the present invention will be further described, to help understanding in the present invention
Hold.
Embodiment 1
By analytically pure TeO2、Na2CO3、ZnO、H3BO3Each component is calculated as 60mol%TeO according to molar fraction2、
20mol%Na2CO3, 10mol%ZnO, 10mol%H3BO3And mass fraction 8wt%LuAG fluorescent powders are (with TeO2,
Na2CO3, ZnO, H3BO3Gross mass meter) be precisely weighed after, be placed in agate mortar, grinding be uniformly placed in corundum crucible,
It is put into 600 DEG C of Muffle furnace and melts 0.5 hour, glass melts are poured on 250 DEG C of pig mold make annealing treatment later,
Wait for that temperature is down to room temperature and takes out fluorescent glass.Gained fluorescent glass is machined, grinding and polishing to 1mm thickness, it will
After 12wt% red fluorescence powders and 4g organic bond accurate weighings, it is placed in beaker, stirs evenly and be placed on vacuum degasing machine
Middle processing 0.5 hour, recycles spin coating process that homogeneous mixture is coated in fluorescent glass surface, is put into 150 DEG C dry
Constant temperature 0.5 hour in dry case, it is long 4mm, the sheet glass of wide 3mm to cut into size after cooling.
Fluorescent glass piece is encapsulated on blue chip, it can using Hangzhou distant place STC4000 rapid spectrometers and LED300E
Program the equipment such as LED testing light sources and carry out optical performance test, the electroluminescent spectrum of fluorescent glass as shown in Figure 1, and
Under the operating current excitation of 20mA, luminous efficiency 95.70lm/W, colour temperature 4829K, colour rendering index 83.4.
Embodiment 2
By analytically pure TeO2、Na2CO3、ZnO、H3BO3Each component is calculated as 60mol%TeO according to molar fraction2、
20mol%Na2CO3, 10mol%ZnO, 10mol%H3BO3And mass fraction 8wt%LuAG fluorescent powders are (with TeO2,
Na2CO3, ZnO, H3BO3Gross mass meter) be precisely weighed after, be placed in agate mortar, grinding be uniformly placed in corundum crucible,
It is put into 600 DEG C of Muffle furnace and melts 0.5 hour, glass melts are poured on 250 DEG C of pig mold make annealing treatment later,
Wait for that temperature is down to room temperature and takes out fluorescent glass.Gained fluorescent glass is machined, grinding and polishing to 1mm thickness, it will
After 16wt% red fluorescence powders and 4g organic bond accurate weighings, it is placed in beaker, stirs evenly and be placed on vacuum degasing machine
Middle processing 0.5 hour, recycles spin coating process that homogeneous mixture is coated in fluorescent glass surface, is put into 150 DEG C dry
Constant temperature 0.5 hour in dry case, it is long 4mm, the sheet glass of wide 3mm to cut into size after cooling.
Fluorescent glass is encapsulated on blue chip, can be compiled using Hangzhou distant place STC4000 rapid spectrometers and LED300E
The equipment such as journey LED testing light sources carry out optical performance test, and the electroluminescent spectrum of fluorescent glass is as shown in Figure 1, and in 20mA
Operating current excitation under, luminous efficiency 92.54lm/W, colour temperature 3945K, colour rendering index 89.5.
Embodiment 3
By analytically pure TeO2、Na2CO3、ZnO、H3BO3Each component is calculated as 60mol%TeO according to molar fraction2、
20mol%Na2CO3, 10mol%ZnO, 10mol%H3BO3And mass fraction 8wt%LuAG fluorescent powders are (with TeO2,
Na2CO3, ZnO, H3BO3Gross mass meter) be precisely weighed after, be placed in agate mortar, grinding be uniformly placed in corundum crucible,
It is put into 600 DEG C of Muffle furnace and melts 0.5 hour, glass melts are poured on 250 DEG C of pig mold make annealing treatment later,
Wait for that temperature is down to room temperature and takes out fluorescent glass.Gained fluorescent glass is machined, grinding and polishing to 1mm thickness, it will
After 20wt% red fluorescence powders and 4g organic bond accurate weighings, it is placed in beaker, stirs evenly and be placed on vacuum degasing machine
Middle processing 0.5 hour, recycles spin coating process that homogeneous mixture is coated in fluorescent glass surface, is put into 150 DEG C dry
Constant temperature 0.5 hour in dry case, it is long 4mm, the sheet glass of wide 3mm to cut into size after cooling.
Fluorescent glass is encapsulated on blue chip, can be compiled using Hangzhou distant place STC4000 rapid spectrometers and LED300E
The equipment such as journey LED testing light sources carry out optical performance test, and the electroluminescent spectrum of fluorescent glass is as shown in Figure 1, and in 20mA
Operating current excitation under, luminous efficiency 90.65lm/W, colour temperature 3289K, colour rendering index 91.6.
The experimental results showed that with the increase of red fluorescence powder concentration, the luminous intensity of red light wave band gradually increases,
Related optical parameter colour temperature continuously decreases, and colour rendering index gradually increases.By adjusting the concentration of red fluorescence powder, can improve white
The coloration of light LED, finally obtains warm white.
Specific case used herein elaborates inventive concept, the explanation of above example is only intended to
Help understands core of the invention thought.It should be pointed out that for those skilled in the art, not departing from this
Under the premise of inventive concept, any obvious modification, equivalent replacement or the other improvements made should be included in the present invention
Protection domain within.
Claims (10)
1. a kind of preparation method of fluorescent glass, it is characterised in that：Include the following steps：
(1) glass raw material and LuAG fluorescent powders are sufficiently mixed in mortar, grind and obtains fluorescent glass mixture；The glass
Raw material is by TeO2、H3BO3, ZnO and Na2CO3Composition；
(2) the fluorescent glass mixture is poured into after crucible and is sintered in Muffle furnace, obtain melten glass material；
(3) the melten glass material is made annealing treatment, is cooled to room temperature to form transparent fluorescent glass；
(4) thickness of the fluorescent glass is adjusted；
(5) uniform sizing material of red fluorescence powder and organic bond is subjected to vacuum defoamation processing, it will using spin coating equipment
Slurry is coated in green fluorescence glass surface；
(6) fluorescent glass coated with red fluorescence powder is put into drying box and is heat-treated, is cooled to room temperature laggard
Row cutting, is then encapsulated on LED blue chips and generates warm white.
2. preparation method according to claim 1, it is characterised in that：Glass components are pressed described in the step (1)
Mole percent is calculated as：TeO240-60mol%, H3BO35-20mol%, ZnO 5-25%, Na2CO310-35%.
3. preparation method according to claim 2, it is characterised in that：LuAG fluorescent powders are described in the step (1)
Lu3Al5O12：Ce3+Fluorescent powder, the quality of the LuAG fluorescent powders are the 5-20% of glass raw material gross mass.
4. preparation method according to claim 3, it is characterised in that：Muffle furnace described in the step (2) is arranged
It it is 400-750 DEG C, the crucible is corundum crucible, described to be sintered to Isothermal sinter, and the Isothermal sinter time is that 0.5-2.5 is small
When.
5. preparation method according to claim 4, it is characterised in that：The step (3) is specially by the melten glass
It is on 150-450 DEG C of mold that material, which pours into temperature, and the mold is pig mold, is placed in and keeps the temperature 2-4 hours in Muffle furnace and moved back
Fire is cooled to room temperature to obtain transparent fluorescent glass later.
6. preparation method according to claim 5, it is characterised in that：It is glimmering that the step (4) is machined into method adjustment
The thickness of light glass is between 0.5-2mm.
7. preparation method according to claim 6, it is characterised in that：Red fluorescence powder is described in the step (5)
CaAlSiN3：Eu2+, the quality of the red fluorescence powder is the 5-20% of organic bond gross mass, and when the vacuum defoamation
Between be 0.5-2 hours.
8. preparation method according to claim 7, it is characterised in that：The temperature of drying box described in the step (6) is set
It is set to 100-200 DEG C, the heat treatment time is 0.5-1.5 hours.
9. preparation method according to claim 8, it is characterised in that：Glass sample is a length of described in the step (6)
2-10mm, width 2-10mm.
10. a kind of fluorescent glass, which is characterized in that by the preparation method of fluorescent glass described in any one of claim 1-9
It is made.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810462517.0A CN108503216A (en) | 2018-05-15 | 2018-05-15 | A kind of preparation method and fluorescent glass of fluorescent glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810462517.0A CN108503216A (en) | 2018-05-15 | 2018-05-15 | A kind of preparation method and fluorescent glass of fluorescent glass |
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| CN108503216A true CN108503216A (en) | 2018-09-07 |
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| CN201810462517.0A Pending CN108503216A (en) | 2018-05-15 | 2018-05-15 | A kind of preparation method and fluorescent glass of fluorescent glass |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830587A (en) * | 2019-01-10 | 2019-05-31 | 徐煜 | A kind of full angle shines and the led lighting source production method of single side encapsulation |
| CN112851124A (en) * | 2021-02-04 | 2021-05-28 | 中国科学院福建物质结构研究所 | Glass ceramic membrane composite material for laser illumination |
| CN114133930A (en) * | 2021-12-01 | 2022-03-04 | 上海应用技术大学 | Warm white garnet type fluorescent glass ceramic and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084760A (en) * | 2014-05-06 | 2015-11-25 | 深圳市绎立锐光科技开发有限公司 | Preparation method for ultrathin light emitting glass and related light emitting device |
| CN107572777A (en) * | 2017-09-21 | 2018-01-12 | 上海应用技术大学 | A kind of preparation method of LED illumination tellurate transparent fluorescent glass |
-
2018
- 2018-05-15 CN CN201810462517.0A patent/CN108503216A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084760A (en) * | 2014-05-06 | 2015-11-25 | 深圳市绎立锐光科技开发有限公司 | Preparation method for ultrathin light emitting glass and related light emitting device |
| CN107572777A (en) * | 2017-09-21 | 2018-01-12 | 上海应用技术大学 | A kind of preparation method of LED illumination tellurate transparent fluorescent glass |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109830587A (en) * | 2019-01-10 | 2019-05-31 | 徐煜 | A kind of full angle shines and the led lighting source production method of single side encapsulation |
| CN112851124A (en) * | 2021-02-04 | 2021-05-28 | 中国科学院福建物质结构研究所 | Glass ceramic membrane composite material for laser illumination |
| CN114133930A (en) * | 2021-12-01 | 2022-03-04 | 上海应用技术大学 | Warm white garnet type fluorescent glass ceramic and preparation method thereof |
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