CN104355542A - Preparation method of glass ceramic - Google Patents
Preparation method of glass ceramic Download PDFInfo
- Publication number
- CN104355542A CN104355542A CN201410568183.7A CN201410568183A CN104355542A CN 104355542 A CN104355542 A CN 104355542A CN 201410568183 A CN201410568183 A CN 201410568183A CN 104355542 A CN104355542 A CN 104355542A
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- CN
- China
- Prior art keywords
- quality
- preparation
- magnesia
- borosilicate glass
- powder
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Classifications
-
- 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
- C03C10/0036—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 containing SiO2, Al2O3 and a divalent metal oxide as main constituents
- C03C10/0045—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 containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
Abstract
The invention relates to a preparation method of glass ceramic. The method comprises the following steps: (1) preparing the following raw materials by mass percent: 30%-40% of magnesia borosilicate glass powder, 30%-50% of aluminum oxide filler powder, 10%-30% of Y2O3 and 10%-15% of rare earth ions, wherein the magnesia borosilicate glass powder contains 40%-70% of SiO2, 8%-25% of B2O3, 5%-30% of Al2O3 and 20%-30% of MgO; (2) performing heat treatment for the first time at 650-750 DEG C and performing heat treatment for the second time at 700-750 DEG C. A glass ceramic substrate prepared by the method is high in reflection rate, low in glass phase crystallization rate and excellent in luminous performance.
Description
Technical field
The present invention relates to a kind of preparation method of glass-ceramic, especially a kind of preparation method that can be applicable to the glass-ceramic of opticglass.
Background technology
Along with the develop rapidly of information technology and photoelectric technology, the property of phosphor is subject to people's attention day by day, and its existing forms has polycrystal powder, monocrystalline, film, pottery, glass etc.Because glass has even, transparent, to be easy to be processed into different shape advantage, and can carry out the doping of higher concentration, therefore become the good substrate material of inorganic light-emitting gradually, its purposes is also more and more extensive.
Light source is divided into discharge lamp and solid state lamp usually, and in solid state lamp, heat radiator is occupied an leading position in general illumination and automobile application, such as halogen lamp.In addition, the solid state light emitter of light emitting deivce form, such as a kind of common form of inorganic light-emitting diode (LED).
LED has the performance of many excellences, and electric energy can be converted into luminous energy by it, and therefore have higher efficiency, volume is little, and has multiple different colours, therefore becomes a kind of luminescent material of widespread use.
Rare earth ion has good fluorescent characteristic due to its special 4f electronic structure, and as pure in luminescent chromaticity, physico-chemical property is stablized, efficiency of conversion is high.In recent years, rare earth ion doped Novel luminous glass becomes the focus of R and D, and its application covers the fields such as fluorescence equipment, laser, fiber amplifier, white light LEDs.Ground state level due to rare earth Eu2+ is 4f7 (8S7/2), in ultraviolet to infrared band, Eu2+ all can be excited, so the luminescent properties of the ceramic that adulterates about Eu2+, lot of domestic and international scholar has carried out a large amount of fundamental research [2-10].The Rare-earth Optic Glass being matrix with B2O3-SiO2 system has the solubilize rare earth ions ability of higher chemical strength, good dielectricity, higher chemical stability and excellence, is the Major Systems that current people study Rare-earth Optic Glass.
At present, the research for the luminescent properties of single rare earth ion pair pyrex is comparatively general, but, seldom there is bibliographical information that the combination of multiple rare earth ion can be utilized to study its impact on the luminescent properties of pyrex; In addition, for the preparation method of glass-ceramic, also the melting technology that adopts is carried out more, seldom has bibliographical information that heat treated mode can be adopted repeatedly to carry out the preparation of glass-ceramic.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of glass-ceramic, the glass-ceramic that this glass-ceramic prepares is suitable for higher level doping with rare-earth ions completely, thus the luminescent properties of the conversion of the light be conducive to as far as possible from cold light source (LED or discharge lamp) can be obtained, the glass ceramic baseplate that this glass-ceramic preparation method makes has high-reflectivity and the percent crystallization in massecuite of glassy phase is low.
For reaching this goal of the invention, the present invention by the following technical solutions:
First aspect, the invention provides a kind of glass-ceramic preparation method, described method comprises the steps:
(1) preparation of raw material: the magnesia borosilicate glass powder of 30 ~ 40 quality %, the alumina packing powder of 30 ~ 50 quality %, 10 ~ 30 quality %Y
2o
3with the rare earth ion of 10-15%, described magnesia borosilicate glass powder converts containing 40 ~ 70 quality %SiO with oxide compound
2, 8 ~ 25 quality %B
2o
3, 5 ~ 30 quality %Al
2o
3, 20 ~ 30 quality %MgO;
(2) carry out first time thermal treatment at 650 ~ 750 DEG C, carry out second time thermal treatment at 700 ~ 750 DEG C and obtain.
In step of the present invention (1), for the preparation of raw material, the content of the magnesia borosilicate glass powder in the present invention is 30 ~ 40 quality %, can be such as 30 quality %, 31 quality %, 32 quality %, 33 quality %, 34 quality %, 35 quality %, 36 quality %, 37 quality %, 38 quality %, 39 quality %, 40 quality %, be preferably 32 ~ 38 quality %, more preferably 35 quality %.
The content of the alumina packing powder in the present invention is 30 ~ 50 quality %, can be such as 30 quality %, 32 quality %, 35 quality %, 38 quality %, 40 quality %, 45 quality %, 48 quality %, 50 quality %, be preferably 35 ~ 45 quality %, more preferably 35 quality %.
Y in the present invention
2o
3content be 10 ~ 30 quality %, can be such as 10 quality %, 12 quality %, 15 quality %, 18 quality %, 20 quality %, 22 quality %, 25 quality %, 28 quality %, 30 quality %, be preferably 12 ~ 25 quality %, more preferably 15 quality %.
Rare earth ion in the present invention is 10-15 quality %, such as, can be 10 quality %, 11 quality %, 12 quality %, 13 quality %, 14 quality %, 15 quality %, is preferably 12-15 quality %, more preferably 15 quality %.
In advantageous modification of the present invention, the proportioning raw materials of this preparation method can for comprising magnesia borosilicate glass powder, the alumina packing powder of 30 ~ 45 quality %, 10 ~ 28 quality %Y of 32 ~ 40 quality %
2o
3with the rare earth ion of 10-15 quality %, described magnesia borosilicate glass powder converts containing 40 ~ 70 quality %SiO with oxide compound
2, 8 ~ 25 quality %B
2o
3, 5 ~ 30 quality %Al
2o
3, 20 ~ 30 quality %MgO.
In advantageous modification of the present invention, the proportioning raw materials of described preparation method can comprise the magnesia borosilicate glass powder of 32 ~ 38 quality %, the alumina packing powder of 35 ~ 45 quality %, 12 ~ 25 quality %Y
2o
3with the rare earth ion of 12-15 quality %, described magnesia borosilicate glass powder converts containing 48 ~ 68 quality %SiO with oxide compound
2, 10 ~ 20 quality %B
2o
3, 10 ~ 25 quality %Al
2o
3, 22 ~ 28 quality %MgO.
In another advantageous modification of the present invention, the proportioning raw materials of described preparation method can comprise the magnesia borosilicate glass powder of 35 quality %, the alumina packing powder of 35 quality %, 15 quality %Y
2o
3with the rare earth ion of 15 quality %, described magnesia borosilicate glass powder converts containing 50 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 15 quality %Al
2o
3, 25 quality %MgO.
Rare earth ion in the present invention is selected from the mixture of any one or at least two kinds in Ce, Pr, Nd, Sm, Eu, Gd, Tb, Er, Tm, Yb, Ho, Dy or La.
In an advantageous modification of the present invention, described rare earth ion is the mixture of any one or at least two kinds in Ce, Eu, Ho, Tm, Tb, Dy or Yb.
In another advantageous modification of the present invention, described rare earth ion is any one mixture in Ce/Eu, Ho/Tm/Yb or Tb/Dy, is preferably the mixture of Ho/Tm/Yb.
Described in step of the present invention (2) is 20 ~ 60h at 650 ~ 750 DEG C of first time heat treatment times carried out, can be such as 20h, 22h, 25h, 30h, 35h, 40h, 45h, 50h, 55h, 60h, being 60 ~ 90h at 700 ~ 750 DEG C of second time heat treatment times carried out, such as, can be 60h, 62h, 65h, 70h, 72h, 75h, 80h, 85h, 90h.
The present invention adopts thermal treatment at twice to carry out the preparation of glass-ceramic, and glass-ceramic can be made to obtain more excellent optical property.
Second aspect, present invention also offers a kind of preparation method as described in relation to the first aspect and the glass-ceramic obtained.
The third aspect, present invention also offers a kind of fluorescent glass, and described light source comprises LED and the glass-ceramic as described in second aspect.
Compared with prior art, the present invention has following beneficial effect:
The glass ceramic baseplate insulating reliability that glass-ceramic preparation method of the present invention makes is high, have high-flexural strength and high-reflectivity and the percent crystallization in massecuite of glassy phase is low, wherein, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches less than 60% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.95.
Embodiment
Technical scheme of the present invention is further illustrated below by embodiment.
Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment 1
(1) preparation comprises the first glass of following composition (quality %, with oxide basis):
The magnesia borosilicate glass powder of 30 quality %, the alumina packing powder of 30%, 30 quality %Y
2o
3with the mixture of the rare earth ion Ce/Eu of 10 quality %, described magnesia borosilicate glass powder converts containing 68 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 10 quality %Al
2o
3, 22 quality %MgO.Wherein, the molar fraction of Ce and Eu is 0.5%.
(2) the first time heat treatment time 20h carried out at 650 DEG C, at the second time heat treatment time 68h that 700 DEG C are carried out.
After tested, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches 55% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.95.
Embodiment 2
(1) preparation comprises the first glass of following composition (quality %, with oxide basis):
The magnesia borosilicate glass powder of 32 quality %, the alumina packing powder of 35%, 20 quality %Y
2o
3with the mixture of the rare earth ion Ce/Eu of 13 quality %, described magnesia borosilicate glass powder converts containing 68 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 10 quality %Al
2o
3, 22 quality %MgO.Wherein, the molar fraction of Ce and Eu is 1.0%.
(2) the first time heat treatment time 22h carried out at 660 DEG C, at the second time heat treatment time 60h that 750 DEG C are carried out.
After tested, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches 52% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.95.
Embodiment 3
(1) preparation comprises the first glass of following composition (quality %, with oxide basis):
The magnesia borosilicate glass powder of 34 quality %, the alumina packing powder of 38%, 16 quality %Y
2o
3with the mixture of the rare earth ion Ho/Tm/Yb of 12 quality %, described magnesia borosilicate glass powder converts containing 60 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 10 quality %Al
2o
3, 20 quality %MgO.Wherein, the molar fraction of Ho, Tm and Yb is 1.0%.
(2) the first time heat treatment time 25h carried out at 680 DEG C, at the second time heat treatment time 70h that 750 DEG C are carried out.
After tested, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches 53% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.97.
Embodiment 4
(1) preparation comprises the first glass of following composition (quality %, with oxide basis):
The magnesia borosilicate glass powder of 35 quality %, the alumina packing powder of 35%, 15 quality %Y
2o
3with the mixture of the rare earth ion Ho/Tm/Yb of 15 quality %, described magnesia borosilicate glass powder converts containing 68 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 10 quality %Al
2o
3, 22 quality %MgO.Wherein, the molar fraction of Ho, Tm, Yb is 1.5%.
(2) the first time heat treatment time 28h carried out at 650 DEG C, at the second time heat treatment time 75h that 750 DEG C are carried out.
After tested, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches 50% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.95.
Embodiment 5
(1) preparation comprises the first glass of following composition (quality %, with oxide basis):
The magnesia borosilicate glass powder of 38 quality %, the alumina packing powder of 32%, 20 quality %Y
2o
3with the mixture of the rare earth ion Tb/Dy of 10 quality %, described magnesia borosilicate glass powder converts containing 68 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 10 quality %Al
2o
3, 22 quality %MgO.Wherein, the molar fraction of Tb and Dy is 0.5%.
(2) the first time heat treatment time 60h carried out at 700 DEG C, at the second time heat treatment time 90h that 720 DEG C are carried out.
After tested, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches 55% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.98.
Embodiment 6
(1) preparation comprises the first glass of following composition (quality %, with oxide basis):
The magnesia borosilicate glass powder of 37 quality %, the alumina packing powder of 30%, 22 quality %Y
2o
3with the mixture of the rare earth ion Tb/Dy of 11 quality %, described magnesia borosilicate glass powder converts containing 68 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 10 quality %Al
2o
3, 22 quality %MgO.Wherein, the molar fraction of Tb and Dy is 2.0%.
(2) the first time heat treatment time 45h carried out at 650 DEG C, at the second time heat treatment time 80h that 720 DEG C are carried out.
After tested, the percent crystallization in massecuite of the glassy phase in the ceramic sintered bodies obtained by burning till reaches 51% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.96.
As can be seen from above-described embodiment 1-6, the glass ceramic baseplate utilizing glass-ceramic preparation method of the present invention to make has high-reflectivity and the percent crystallization in massecuite of glassy phase is low, has excellent luminescent properties, can be widely used in industrial production.
Applicant states, the present invention illustrates processing method of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned processing step, does not namely mean that the present invention must rely on above-mentioned processing step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of raw material selected by the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. a preparation method for glass-ceramic, is characterized in that, described method comprises the steps:
(1) preparation of raw material: the magnesia borosilicate glass powder of 30 ~ 40 quality %, the alumina packing powder of 30 ~ 50 quality %, 10 ~ 30 quality %Y
2o
3with the rare earth ion of 10-15%, described magnesia borosilicate glass powder converts containing 40 ~ 70 quality %SiO with oxide compound
2, 8 ~ 25 quality %B
2o
3, 5 ~ 30 quality %Al
2o
3, 20 ~ 30 quality %MgO;
(2) carry out first time thermal treatment at 650 ~ 750 DEG C, carry out second time thermal treatment at 700 ~ 750 DEG C and obtain.
2. preparation method as claimed in claim 1, is characterized in that, the raw material packet described in step (1) is containing magnesia borosilicate glass powder, the alumina packing powder of 30 ~ 45 quality %, 10 ~ 28 quality %Y of 32 ~ 40 quality %
2o
3with the rare earth ion of 10-15 quality %, described magnesia borosilicate glass powder converts containing 40 ~ 68 quality %SiO with oxide compound
2, 8 ~ 24 quality %B
2o
3, 8 ~ 30 quality %Al
2o
3, 20 ~ 28 quality %MgO.
3. preparation method as claimed in claim 1 or 2, is characterized in that, the raw material packet described in step (1) is containing magnesia borosilicate glass powder, the alumina packing powder of 35 ~ 45 quality %, 12 ~ 25 quality %Y of 32 ~ 38 quality %
2o
3with the rare earth ion of 12-15 quality %, described magnesia borosilicate glass powder converts containing 48 ~ 68 quality %SiO with oxide compound
2, 10 ~ 20 quality %B
2o
3, 10 ~ 25 quality %Al
2o
3, 22 ~ 28 quality %MgO.
4. the preparation method as described in any one of claim 1-3, is characterized in that, the raw material packet described in step (1) is containing magnesia borosilicate glass powder, the alumina packing powder of 35 quality %, the 15 quality %Y of 35 quality %
2o
3with the rare earth ion of 15 quality %, described magnesia borosilicate glass powder converts containing 50 quality %SiO with oxide compound
2, 10 quality %B
2o
3, 15 quality %Al
2o
3, 25 quality %MgO.
5. the preparation method as described in any one of claim 1-4, is characterized in that, described rare earth ion is the mixture of any one or at least two kinds in Ce, Eu, Ho, Tm, Tb, Dy or Yb.
6. the preparation method as described in any one of claim 1-5, is characterized in that, described rare earth ion is any one mixture in Ce/Eu, Ho/Tm/Yb or Tb/Dy.
7. the preparation method as described in any one of claim 1-6, is characterized in that, described in step (2) to carry out the first time heat treated time at 650 ~ 750 DEG C be 20-60h, carrying out the second time heat treated time at 700 ~ 750 DEG C is 60-90h.
8. the preparation method as described in any one of claim 1-7, is characterized in that, described in step (2) is 20h at 650 ~ 750 DEG C of first time heat treatment times carried out, and is 80h at 700 ~ 750 DEG C of second time heat treatment times carried out.
9. the glass-ceramic that the preparation method as described in any one of claim 1-8 obtains.
10. a fluorescent glass, is characterized in that, described light source comprises LED and glass-ceramic as claimed in claim 9.
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CN201410568183.7A CN104355542A (en) | 2014-10-22 | 2014-10-22 | Preparation method of glass ceramic |
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CN201410568183.7A CN104355542A (en) | 2014-10-22 | 2014-10-22 | Preparation method of glass ceramic |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114735939A (en) * | 2022-05-17 | 2022-07-12 | 金湖万迪光电科技有限公司 | Preparation method of low-expansion-coefficient transparent microcrystalline glass |
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---|---|---|---|---|
CN1769231A (en) * | 2004-09-29 | 2006-05-10 | 肖特股份公司 | Glass or glass ceremic |
CN1955131A (en) * | 2005-10-25 | 2007-05-02 | 株式会社小原 | Glass-ceramics and a method for manufacturing the same |
CN101543151A (en) * | 2007-04-20 | 2009-09-23 | 株式会社村田制作所 | Multilayered ceramic substrate, process for producing the multilayered ceramic substrate, and electronic component |
CN102030477A (en) * | 2009-10-07 | 2011-04-27 | 旭硝子株式会社 | Ceramic material composition |
-
2014
- 2014-10-22 CN CN201410568183.7A patent/CN104355542A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1769231A (en) * | 2004-09-29 | 2006-05-10 | 肖特股份公司 | Glass or glass ceremic |
CN1955131A (en) * | 2005-10-25 | 2007-05-02 | 株式会社小原 | Glass-ceramics and a method for manufacturing the same |
CN101543151A (en) * | 2007-04-20 | 2009-09-23 | 株式会社村田制作所 | Multilayered ceramic substrate, process for producing the multilayered ceramic substrate, and electronic component |
CN102030477A (en) * | 2009-10-07 | 2011-04-27 | 旭硝子株式会社 | Ceramic material composition |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114735939A (en) * | 2022-05-17 | 2022-07-12 | 金湖万迪光电科技有限公司 | Preparation method of low-expansion-coefficient transparent microcrystalline glass |
CN114735939B (en) * | 2022-05-17 | 2024-02-20 | 金湖万迪光电科技有限公司 | Preparation method of transparent glass ceramics with low expansion coefficient |
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