CN106746516A - A kind of preparation method of fluorescent glass - Google Patents
A kind of preparation method of fluorescent glass Download PDFInfo
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- CN106746516A CN106746516A CN201611156777.2A CN201611156777A CN106746516A CN 106746516 A CN106746516 A CN 106746516A CN 201611156777 A CN201611156777 A CN 201611156777A CN 106746516 A CN106746516 A CN 106746516A
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- glass
- fluorescent
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- powder
- fluorescent glass
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
-
- 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
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/004—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of particles or flakes
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dispersion Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Luminescent Compositions (AREA)
Abstract
A kind of preparation method of fluorescent glass, belongs to zone material preparation field, it is characterised in that comprise the following steps：（1）Quartz test tube is broken into by required silica glass powder by ball-milling method first；（2）Take silicon-dioxide powdery and fluorescent material, drying for standby；（3）The powder for mixing is taken, is put into SPS devices after being fitted into graphite jig；（4）Then vacuumize, pressure regulation sintering；（5）Power supply is finally closed, mould is taken out after being cooled to room temperature；Sample is processed into glass wafer by twin polishing, completes to prepare.Ce is prepared for using a step SPS sintering process:Silica/the Ce of YAG fluorescent powder mixing:YAG fluorescent glass, optimal sintering temperature is 1200 DEG C, and whole sintering process only needs to 9 min, and fluorescent glass of the present invention preparation method preparation process is simple, it is easy to operate, be suitable to popularization and application.
Description
Technical field
The invention belongs to zone material preparation field, more particularly to a kind of preparation method of fluorescent glass.
Background technology
The pursuit of lighting source is always along with the development of human society.Before the eighties in 18th century, the mankind are also always
Using kerosene lamp as lighting source.Until Edison in 1879 is prepared for first incandescent lamp in the world using carbon fibre,
The mankind just calculate and actually enter the electric light source epoch.But the luminous efficiency of incandescent lamp is low, and more than 90% energy is damaged with form of heat
Consume, so producing great energy waste.As people are to the light efficiency of lamp and the pursuit of brightness, more supernumerary segment is occurred in that again in succession
The fluorescent lamp and gas-discharge lamp of energy.
Into 21 century, global energy crisis are increasingly severe.There is data to show, global electric consumption on lighting amount accounting is up to
22%.Therefore in the urgent need to finding more energy-conservation and environmentally friendly lighting source, to meet growth requirement.21 century is with semiconductor
The maturation of technology of preparing, light emitting diode is valued by people rapidly as the lighting source for rising, and applies to each
In individual field.LED is cold light source, and itself does not have any pollution to environment, and compared with incandescent lamp, fluorescent lamp, electric energy can
To reach more than 90%, therefore it is considered as the forth generation lighting source of energy-conserving and environment-protective.
Fluorescent glass is to substitute being preferably selected for current large power white light LED fluorescent material and epoxy encapsulation.Its system
Standby technique is relatively easy, and energy consumption is relatively low, and the machining property of glass is preferable, can be processed into variously-shaped and LED core
Piece is encapsulated.What wherein quartz glass had that the simple glasses such as low-expansion coefficient, high transmittance, high chemical stability do not have is excellent
Point, is wherein preferred host material.
In fact, to the research of fluorescent glass always for a long time.The fluorescent glass of rare earth ion or doped transition metal ionses,
As long-afterglow luminescent glass has many excellent optical properties, the research of early stage is used for laser, optical amplifier, light and leads to
The fields such as news, energy storage.Developing rapidly with LED industry in recent years, fluorescent glass is used as the another kind hair in addition to fluorescent material
Luminescent material is increasingly taken seriously in the potential application value of field of LED illumination.
The content of the invention
Present invention seek to address that above mentioned problem, there is provided a kind of preparation method of fluorescent glass.
The technical scheme is that：
A kind of preparation method of fluorescent glass, it is characterised in that comprise the following steps：（1）Pass through ball-milling method first by quartz test tube
It is broken into required silica glass powder；（2）Take the Ce of silicon-dioxide powdery and commercialization:YAG fluorescent powder, by mortar grinder
Drying for standby after uniform；（3）The powder for mixing is taken, is put into SPS devices after being fitted into the graphite jig of diameter 10mm；（4）
Then vacuumize, regulation pressure to 50MPa is sintered；（5）Power supply is finally closed, mould is taken out after being cooled to room temperature；Sample passes through
Twin polishing is processed into glass wafer, completes to prepare.
The preparation method of fluorescent glass of the present invention, 15 × 150mm of the quartz glass tube model.
The preparation method of fluorescent glass of the present invention, the LED fluorescent powder is BL304A.
The preparation method of fluorescent glass of the present invention, the sintering process reaches 600 DEG C for 3min, and 4min reaches
1200 DEG C, it is incubated 2min.
The preparation method of fluorescent glass of the present invention, the specification of the glass wafer is Φ 10mm × 1mm.
The technical effects of the invention are that：
The preparation method of fluorescent glass of the present invention, Ce is prepared for using a step SPS sintering process:YAG fluorescent powder mixing
Silica/Ce:YAG fluorescent glass, have studied sintering characteristic, microstructure, the optical property of fluorescent glass, obtain optimal
Sintering temperature is 1200 DEG C, and whole sintering process only needs to 9 min.And the preparation method system of fluorescent glass of the present invention
Standby process is simple, it is easy to operate, be suitable to popularization and application.
Specific embodiment
Embodiment
A kind of preparation method of fluorescent glass, it is characterised in that comprise the following steps：（1）Pass through ball-milling method first by quartz
Test tube is broken into required silica glass powder；（2）Take the Ce of silicon-dioxide powdery and commercialization:YAG fluorescent powder, by mortar
Drying for standby after grinding is uniform；（3）The powder for mixing is taken, is put into SPS devices after being fitted into the graphite jig of diameter 10mm；
（4）Then vacuumize, regulation pressure to 50MPa is sintered；（5）Power supply is finally closed, mould is taken out after being cooled to room temperature；Sample is passed through
Cross twin polishing and be processed into glass wafer, complete to prepare.
The preparation method of fluorescent glass of the present invention, 15 × 150mm of the quartz glass tube model.
The preparation method of fluorescent glass of the present invention, the LED fluorescent powder is BL304A.
The preparation method of fluorescent glass of the present invention, the sintering process reaches 600 DEG C for 3min, and 4min reaches
1200 DEG C, it is incubated 2min.
The preparation method of fluorescent glass of the present invention, the specification of the glass wafer is Φ 10mm × 1mm.
With Ball-milling Time from 4h, 8h, 12h, 24h to 48h when, particle diameter distribution is broadened by narrow；When Ball-milling Time reaches 12h
More than, diameter of particle distribution starts widthization, therefore Ball-milling Time is preferable within 12h.With milling time from 4h, 8h, 12h,
24h to 48h increases, and powder median reduces first, and when more than 12h is reached, particle diameter increases on the contrary, it may occur however that reunite existing
As.In sum, quartz glass powder that Ball-milling Time obtained for 12h is chosen as raw material, now the grain of quartz glass powder
Footpath distribution is also narrower, and median is in 2.95um or so.
When sintering temperature increases to during 1200 DEG C from 1000 DEG C, glass sample gradually bleach, but transparency is simultaneously
It is bad.Also there is spike in 1000 DEG C of glass samples for sintering out, when temperature is gradually increased to 1200 DEG C, spike gradually disappears
Lose, typical glass steamed bun peak is presented.Therefore glass is formed to ensure sample, experimental part below employs 1200 DEG C of burning
It is prepared by junction temperature.
Based on sintering temperature system obtained above, then mix Ce:YAG fluorescent powder is prepared for various concentrations
Fluorescent glass sample.As phosphor concentration increases, the color of fluorescent glass is gradually deepened, and transparency also declines.Sintering temperature
600 DEG C are reached in 3min, 4min reaches 1200 DEG C, be then incubated 2min at 1200 DEG C.In 3min, sample occurs somewhat swollen
Swollen, this is mainly and is caused by the expanded by heating of glass powder；In 7min or so, sample drastically shrinks, and is then received in 8min or so
Contracting stops, and this represents glass sintering and is basically completed, and at 1200 DEG C or so, this sinters situation to corresponding temperature with previously reported SPS
Unanimously.
Sintering does not destroy Ce:The structure of YAG crystal, and sample main body is still glass.Then test further to glass
Glass structure is analyzed, Ce:YAG fluorescent powder particle is uniformly distributed in glass matrix, and destroyed phenomenon is not occurred,
Granular size is between 15 ~ 20um.
With Ce:YAG fluorescent powder concentration from 1wt% increase to 5wt% when, fluorescent glass is interval in wavelength 500nm-780nm
Transmitance is reduced to 5% or so from 10%.But all concentration fluorescent glass have strong absorption at 460nm, and this belongs to Ce3+'s
5d-4f transition.Lower fluorescent glass is excited to possess the emission peak of 550nm in 460nm blue lights.As phosphor concentration increases, light
Intensity first rises and declines afterwards, this be probably due to starting caused by the concentration too big transparency of too low and later concentration is greatly reduced, its
The luminous intensity of middle 3wt% fluorescent glass is maximum.
The blue-ray LED integrated chip of 10W on the market is used, the fluorescent glass of 20mm diameters is directly overlayed into chip
Above, around glued using heat-conducting glue, be prepared into a white light LEDs sample.Power supply is accessed, white light LEDs are lighted, and sample sends
Bright white light.Chromaticity coordinates figure of the packaged white light LED part sample under 8.80V, 800mA power drives.800mA's
Under electric current drives, the remaining blue light that chip sends is mixed to form white light with the gold-tinted that fluorescent glass sends, now white light LEDs sample
Chromaticity coordinates (x, y)=(0.33,0.38), fall near white light area just.This show using SPS prepare silica/
Ce:YAG fluorescent glass can be well matched with blue-light LED chip, form white light output, be expected to be applied to white light of new generation
LED component.
By studying quartz glass prepared by different temperatures, it is 1200 DEG C to obtain optimal sintering temperature, and is entirely burnt
Knot process only needs to 9 min.Silica/the Ce for obtaining is sintered by SPS:YAG fluorescent glass main body is still mutually vitreum, should
Fluorescent glass has strong absworption peak in 460 nm, and gold-tinted of the crest positioned at 550nm or so is launched in the case where this wavelength is excited.Pass through
Ce in regulation fluorescent glass:YAG fluorescent powder concentration, can obtain the fluorescent glass of different luminous intensities, 3wt% fluorescent glasses
Can be optimal, the white light LEDs sample encapsulated with this obtains white light output under the driving of 800mA electric currents, chromaticity coordinates (0.33,
0.38)。
Claims (5)
1. a kind of preparation method of fluorescent glass, it is characterised in that comprise the following steps：（1）Quartz is tried by ball-milling method first
Pipe is broken into required silica glass powder；（2）Take the Ce of silicon-dioxide powdery and commercialization:YAG fluorescent powder, is ground by mortar
Drying for standby after mill is uniform；（3）The powder for mixing is taken, is put into SPS devices after being fitted into the graphite jig of diameter 10mm；
（4）Then vacuumize, regulation pressure to 50MPa is sintered；（5）Power supply is finally closed, mould is taken out after being cooled to room temperature；Sample is passed through
Cross twin polishing and be processed into glass wafer, complete to prepare.
2. the preparation method of fluorescent glass according to claim 1, it is characterised in that：The quartz glass tube model 15
×150mm。
3. the preparation method of fluorescent glass according to claim 1, it is characterised in that：The LED fluorescent powder is BL304A.
4. the preparation method of fluorescent glass according to claim 1, it is characterised in that：The sintering process reaches for 3min
600 DEG C, 4min reaches 1200 DEG C, is incubated 2min.
5. the preparation method of fluorescent glass according to claim 1, it is characterised in that：The specification of the glass wafer is Φ
10mm×1mm。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611156777.2A CN106746516A (en) | 2016-12-15 | 2016-12-15 | A kind of preparation method of fluorescent glass |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611156777.2A CN106746516A (en) | 2016-12-15 | 2016-12-15 | A kind of preparation method of fluorescent glass |
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| CN106746516A true CN106746516A (en) | 2017-05-31 |
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| CN201611156777.2A Pending CN106746516A (en) | 2016-12-15 | 2016-12-15 | A kind of preparation method of fluorescent glass |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108329914A (en) * | 2018-04-17 | 2018-07-27 | 温州大学 | A kind of preparation method of fluorescent crystal particle |
| CN111253073A (en) * | 2020-01-21 | 2020-06-09 | 徐州凹凸光电科技有限公司 | Method for preparing gadolinium-aluminum-garnet-based white-light glass ceramic by adopting sol-gel method |
| CN113277715A (en) * | 2021-04-23 | 2021-08-20 | 华南师范大学 | Method for manufacturing quartz glass device with complex structure |
-
2016
- 2016-12-15 CN CN201611156777.2A patent/CN106746516A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108329914A (en) * | 2018-04-17 | 2018-07-27 | 温州大学 | A kind of preparation method of fluorescent crystal particle |
| CN111253073A (en) * | 2020-01-21 | 2020-06-09 | 徐州凹凸光电科技有限公司 | Method for preparing gadolinium-aluminum-garnet-based white-light glass ceramic by adopting sol-gel method |
| CN113277715A (en) * | 2021-04-23 | 2021-08-20 | 华南师范大学 | Method for manufacturing quartz glass device with complex structure |
| CN113277715B (en) * | 2021-04-23 | 2023-10-20 | 华南师范大学 | Method for manufacturing quartz glass device with complex structure |
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20170531 |
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| WD01 | Invention patent application deemed withdrawn after publication |