CN109650725A - A kind of production method of blue-fluorescence glass ceramics - Google Patents
A kind of production method of blue-fluorescence glass ceramics Download PDFInfo
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- CN109650725A CN109650725A CN201811637912.4A CN201811637912A CN109650725A CN 109650725 A CN109650725 A CN 109650725A CN 201811637912 A CN201811637912 A CN 201811637912A CN 109650725 A CN109650725 A CN 109650725A
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- salt
- oxide
- glass ceramics
- blue
- cerium
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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
- 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
-
- 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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7715—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing cerium
- C09K11/7721—Aluminates
Abstract
The present invention provides a kind of production methods of blue-fluorescence glass ceramics, it is characterized in that, it include: to weigh barium salt or ba oxide, pink salt or tin-oxide, silicon salt or Si oxide, cerium salt or cerium oxide and be uniformly mixed, gained mixture is transferred in graphite crucible, graphite crucible is placed in the alumina crucible for filling C powder, 4h~7h is calcined under 1350 DEG C~1450 DEG C environment, it is cooling, obtain blue-fluorescence glass ceramics.The present invention has many advantages, such as that production method is simple, and technological operation is easy.
Description
Technical field
The present invention relates to fluorescent glass field of ceramic preparation more particularly to a kind of BaO-SnO2-SiO2-Ce2O3System is blue
The production method of color fluorescent glass ceramics.
Background technique
The advantages that white light LEDs are high-efficient with its, small in size, the service life is long, environment friendly and pollution-free and be known as forth generation illumination light
Source.In recent years, with the development of illumination market, the demand to great power LED is constantly soaring[1-2].However, most at present
The mode that LED product uses silica gel/epoxy resin and fluorescent powder to mix encapsulates, and the power of LED itself is higher, produced by causing
Heat can not effectively shed, there are silica gel/epoxy resin aging, brightness decline, color drift, losts of life etc. in practical application
Problem.The presence of these problems, also puts forward new requirements Light-conversion Materials for White-light LED: (1) solving the painting of fluorescent material
Apply homogeneity question；(2) fluorescent material stable with high coefficient of thermal conductivity, physical and chemical performance.In these fluorescent materials
In, fluorescent glass ceramics are concerned because having both both performances[3].Fluorescent glass ceramics refer to will be added with the spy of nucleating agent
Surely the parent glass formed, the composite material for by controlling crystallization becoming that there are one or more microcrystals and residual glass phase,
The small ceramic crystal of a large amount of random orientation is uniform-distribution in amorphous glass.With existing epoxy resin block
Fluorescent material is compared, and fluorescent glass ceramics also have the advantage that (1) is dilute other than the natural characteristic with high-temperature corrosion resistance
Native ion is evenly distributed in glass ceramics, will have better color stability and Color uniformity than phosphor material powder；(2) rare earth
The glass block materials of doping are fixed easily, and are conducive to device, replace traditional phosphor material powder, and it is contour can to reduce epoxy resin
The dosage of molecular material alleviates the problems such as aging[4-8].Therefore, a kind of alternative silica gel/epoxy resin and fluorescent powder mixing are developed
Encapsulation and light conversion material of the fluorescent glass ceramics of object as power type white light LED have important practical significance.
Bibliography
[1] Luo Qun, rare earth doped luminescent glass ceramic system is standby with optical property research [D], Zhejiang University, and 2011.
[2]Kim J K,Schubert E F.Transcending the replacement paradigm of
solid-state lighting[J].Optics Express,2008,16(26):21835.
[3] Yang Liang, preparation, characterization and its application [D] in great power LED of fluorescent powder glass composite material, Central China
University of Science and Technology, 2013.
[4] Zhang Yan, preparation and performance study [D] of great power LED fluorescent glass, Donghua University, 2015.
[5] Chen great Qin, Wang Yuansheng can be used for the CeF of burst of ultraviolel white light LEDs3Base transparent glass ceramics [J], laser with
Photoelectronics progress, 2010.
[6] Sun Jiaju, the rear-earth-doped synthesis comprising gallate, aluminate and silicate nano crystal glass ceramics and shine
Property [D], University Of Nanchang, 2016.
[7] Liu Shujie, Guan Rongfeng, for white light LEDs doping Ce-YAG fluorescent glass development [J], electronic component with
Material, 2007,26 (12): 8-9.
[8] Tian Hua, Lu Qifei, Wang Dajian, the CaO-SiO for white light LEDs2The optics of system mixed crystal fluorescent glass ceramics
Property [C], the meeting of national rare earth luminescent material scientific seminar, 2011.
Summary of the invention
The object of the present invention is to provide a kind of production methods of blue-fluorescence glass ceramics.
In order to achieve the above object, the present invention provides a kind of production method of blue-fluorescence glass ceramics, feature exists
In, comprising: it weighs barium salt or ba oxide, pink salt or tin-oxide, silicon salt or Si oxide, cerium salt or cerium oxide and mixes
Uniformly, gained mixture is calcined under 1350 DEG C~1450 DEG C environment to 4h~7h under CO reducing atmosphere condition, it is cooling, it obtains
Blue-fluorescence glass ceramics.
Further, the barium salt or ba oxide, pink salt or tin-oxide, silicon salt or Si oxide and cerium salt or
The dosage of cerium oxide meets: when the barium salt or ba oxide, pink salt or tin-oxide, silicon salt or Si oxide and cerium
Salt or cerium oxide are completely converted into BaO, SnO2、SiO2And Ce2O3When, by percentage to the quality, BaO content be 30.36%~
31.01%, SnO2Content is 31.09%~31.10%, SiO2Content is 37.18%~37.20%, Ce2O3Content is
0.69%~1.37%.(with BaCO3, SnO2, SiO2, CeO2On the basis of gross mass)
Further, the mixed method is to aoxidize barium salt or ba oxide, pink salt or tin-oxide, silicon salt or silicon
Object, cerium salt or cerium oxide are placed in grinding 20min~40min in mortar.
Further, the barium salt or ba oxide are BaCO3。
Further, the pink salt or tin-oxide are SnO2。
Further, the silicon salt or Si oxide are SiO2。
Further, the cerium salt or cerium oxide are CeO2。
The present invention also provides blue-fluorescence glass ceramics made by above-mentioned production method.
Compared with prior art, the beneficial effects of the present invention are:
The present invention provides a kind of BaO-SnO2-SiO2-Ce2O3The production method of system blue-fluorescence glass ceramics.Have
The advantages that production method is simple, and technological operation is easy.As far as we know, it is there is no at present using BaO-SnO2-SiO2-Ce2O3System
Blue-fluorescence glass ceramics report.
The present invention is obtained complete by calcining a certain proportion of raw material under the CO reducing atmosphere that C powder high-temperature calcination is formed
The blue-fluorescence glass ceramics of new system.Fluorescent glass ceramics of the invention can be with ultraviolet chip and other fluorescence transition materials
Matching, makes long-range white light LEDs, thus the problems such as overcoming traditional dispensing formula packaged type colloid easy to aging, yellow.Of the invention
Fluorescent glass ceramics are suitable for high stable, high power LED device.
Detailed description of the invention
Fig. 1 is BaO-SnO2-SiO2-Ce2O3System blue-fluorescence glass ceramics XRD spectrum；
Fig. 2 .BaO-SnO2-SiO2-Ce2O3System blue-fluorescence glass ceramics excites (λem=414nm) and transmitting (λex=
346nm) spectrum.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Case study on implementation 1:
1) prepared by powder: accurately weighing the BaCO that gross mass is 5g3, SnO2, SiO2, CeO2It is placed in agate mortar and grinds
30min is allowed to be transferred in graphite crucible after being sufficiently mixed uniformly；When the barium salt or ba oxide, pink salt or tin aoxidize
Object, silicon salt or Si oxide and cerium salt or cerium oxide are completely converted into BaO, SnO2、SiO2And Ce2O3When, with BaCO3,
SnO2, SiO2, CeO2On the basis of gross mass, by percentage to the quality, BaO:31.01%, SnO2: 31.10%, SiO2:
37.20%, Ce2O3: 0.69%.
2) graphite crucible is placed in the alumina crucible for the 1L capacity for filling C powder, alumina crucible is placed in high temperature
1400 DEG C of calcining 6h in furnace, powder described in calcination process are in the CO reducing atmosphere of C powder formation, and being cooled to room temperature can obtain
To the system fluorescent glass ceramics.
3) obtained sample is tested using the X-ray diffractometer of model D/max 2200PC, obtains the XRD of sample
Spectrum, by XRD spectrum it can be seen that (see Fig. 1), this sample are glass ceramics phase.
4) Fluorescence Spectrometer for using model HITACHI F-7000, tests the spectrum of the system fluorescent glass ceramics
Matter, the results showed that the most strong excitation peak of (see Fig. 2), the system fluorescent glass ceramics are located at 346nm, in swashing for the excitation wavelength light
It gives, shows that best launch wavelength is located at the blue emission of 414nm, show that the system fluorescent glass ceramics are excited in 346nm
Under blue-fluorescence glass ceramics (being shown in Table 1).
Case study on implementation 2:
1) prepared by powder: accurately weighing the BaCO that gross mass is 5g3, SnO2, SiO2, CeO2It is placed in agate mortar and grinds
30min is allowed to be transferred in graphite crucible after being sufficiently mixed uniformly；When the barium salt or ba oxide, pink salt or tin aoxidize
Object, silicon salt or Si oxide and cerium salt or cerium oxide are completely converted into BaO, SnO2、SiO2And Ce2O3When, with BaCO3,
SnO2, SiO2, CeO2On the basis of gross mass, by percentage to the quality, BaO:30.68%, SnO2: 31.09%, SiO2:
37.19%, Ce2O3: 1.04%.
2) graphite crucible is placed in the alumina crucible for the 1L capacity for filling C powder, alumina crucible is placed in high temperature
1400 DEG C of calcining 6h in furnace, powder described in calcination process are in the CO reducing atmosphere of C powder formation, and being cooled to room temperature can obtain
To the system fluorescent glass ceramics.
3) obtained sample is tested using the X-ray diffractometer of model D/max 2200PC, obtains the XRD of sample
Spectrum, this sample is glass ceramics phase it can be seen from XRD spectrum.
4) Fluorescence Spectrometer for using model HITACHI F-7000, tests the spectrum of the system fluorescent glass ceramics
Matter, the results showed that, the most strong excitation peak of the system fluorescent glass ceramics is located at 346nm, under the excitation of the excitation wavelength light, shows
Show that best launch wavelength is located at the blue emission of 414nm, shows that the system fluorescent glass ceramics are the blues under 346nm excitation
Fluorescent glass ceramics (being shown in Table 1).
Case study on implementation 3:
1) prepared by powder: accurately weighing the BaCO that gross mass is 5g3, SnO2, SiO2, CeO2It is placed in agate mortar and grinds
30min is allowed to be transferred in graphite crucible after being sufficiently mixed uniformly；When the barium salt or ba oxide, pink salt or tin aoxidize
Object, silicon salt or Si oxide and cerium salt or cerium oxide are completely converted into BaO, SnO2、SiO2And Ce2O3When, with BaCO3,
SnO2, SiO2, CeO2On the basis of gross mass, by percentage to the quality, BaO:30.36%, SnO2: 31.09%, SiO2:
37.18%, Ce2O3: 1.37%.
2) graphite crucible is placed in the alumina crucible for the 1L capacity for filling C powder, alumina crucible is placed in high temperature
1400 DEG C of calcining 6h in furnace, powder described in calcination process are in the CO reducing atmosphere of C powder formation, and being cooled to room temperature can obtain
To the system fluorescent glass ceramics.
3) obtained sample is tested using the X-ray diffractometer of model D/max 2200PC, obtains the XRD of sample
Spectrum, this sample is glass ceramics phase it can be seen from XRD spectrum.
4) Fluorescence Spectrometer for using model HITACHI F-7000, tests the spectrum of the system fluorescent glass ceramics
Matter, the results showed that, the most strong excitation peak of the system fluorescent glass ceramics is located at 346nm, under the excitation of the excitation wavelength light, shows
Show that best launch wavelength is located at the blue emission of 414nm, shows that the system fluorescent glass ceramics are the blues under 346nm excitation
Fluorescent glass ceramics (being shown in Table 1).
The different case study on implementation of table 1.
Claims (8)
1. a kind of production method of blue-fluorescence glass ceramics characterized by comprising weigh barium salt or ba oxide, pink salt
Or tin-oxide, silicon salt or Si oxide, cerium salt or cerium oxide and be uniformly mixed, by gained mixture in CO reducing atmosphere item
4h~7h is calcined under part under 1350 DEG C~1450 DEG C environment, it is cooling, obtain blue-fluorescence glass ceramics.
2. the production method of blue-fluorescence glass ceramics as described in claim 1, which is characterized in that the barium salt or barium oxygen
Compound, pink salt or tin-oxide, silicon salt or Si oxide and cerium salt or the dosage of cerium oxide meet: when the barium salt or
Ba oxide, pink salt or tin-oxide, silicon salt or Si oxide and cerium salt or cerium oxide are completely converted into BaO, SnO2、
SiO2And Ce2O3When, by percentage to the quality, BaO content is 30.36%~31.01%, SnO2Content be 31.09%~
31.10%, SiO2Content is 37.18%~37.20%, Ce2O3Content is 0.69%~1.37%.
3. the production method of blue-fluorescence glass ceramics as described in claim 1, which is characterized in that the mixed method is
Barium salt or ba oxide, pink salt or tin-oxide, silicon salt or Si oxide, cerium salt or cerium oxide are placed in mortar and are ground
20min~40min.
4. the production method of blue-fluorescence glass ceramics as described in claim 1, which is characterized in that the barium salt or barium oxygen
Compound is BaCO3。
5. the production method of blue-fluorescence glass ceramics as described in claim 1, which is characterized in that the pink salt or tin oxygen
Compound is SnO2。
6. the production method of blue-fluorescence glass ceramics as described in claim 1, which is characterized in that the silicon salt or silicon oxygen
Compound is SiO2。
7. the production method of blue-fluorescence glass ceramics as described in claim 1, which is characterized in that the cerium salt or cerium oxygen
Compound is CeO2。
8. blue-fluorescence glass ceramics made by production method of any of claims 1-7.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116004227A (en) * | 2022-12-15 | 2023-04-25 | 上海应用技术大学 | Ultraviolet excited blue light emitting fluorescent powder and preparation method and application thereof |
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| CN116004227A (en) * | 2022-12-15 | 2023-04-25 | 上海应用技术大学 | Ultraviolet excited blue light emitting fluorescent powder and preparation method and application thereof |
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