CN104386917A - Glass ceramic material and preparation method thereof - Google Patents
Glass ceramic material and preparation method thereof Download PDFInfo
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- CN104386917A CN104386917A CN201410568827.2A CN201410568827A CN104386917A CN 104386917 A CN104386917 A CN 104386917A CN 201410568827 A CN201410568827 A CN 201410568827A CN 104386917 A CN104386917 A CN 104386917A
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Abstract
The invention relates to a glass ceramic material and a preparation method thereof. The preparation method comprises the following steps: (1) preparing raw materials according to the following mass ratio: 30-40% of a glass material, 30-50% of oxide ceramic powders and 10-30% of alkaline earth metal oxide; (2) carrying out a first heat treatment on the raw materials at 650-700 DEG C, carrying out a second heat treatment at 680-750 DEG C and carrying out a third heat treatment at 700-750 DEG C to obtain the glass ceramic material. The glass ceramic baseplate prepared by adopting the preparation method is high in reflectivity and low in crystallization rate of the glass phase, and has the excellent luminescence property.
Description
Technical field
The present invention relates to a kind of glass-ceramic material and preparation method thereof, particularly relate to a kind of glass-ceramic material that can be applicable to opticglass and preparation method thereof.
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.
At present, comparatively general to the research of the luminescent properties of pyrex for rare earth ion, but, seldom there is bibliographical information that the ceramic oxide containing rare earth ion and glass material can be utilized to carry out combining the luminescent properties etc. studying glass-ceramic material, and existing glass-ceramic preparation method many employings melting is carried out.
Summary of the invention
The object of the present invention is to provide a kind of glass-ceramic material and preparation method thereof, 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, and luminescent properties is excellent.
For reaching this goal of the invention, the present invention by the following technical solutions:
First aspect, the invention provides a kind of preparation method of glass-ceramic material, comprises the steps:
(1) preparation of raw material is carried out by following proportioning: the alkaline earth metal oxide of the glass material of 30-40 quality %, the ceramic oxide powders of 30-50 quality %, 10-30 quality %;
(2) at 650-700 DEG C, first time thermal treatment is carried out to above-mentioned glass-ceramic, carry out second time thermal treatment at 680-750 DEG C, carry out third 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 glass material 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 ceramic oxide powders 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 %.
The content of the alkaline earth metal oxide in the present invention is 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 %.
In advantageous modification of the present invention, the proportioning raw materials of described preparation method can comprise the glass material of 32 ~ 38 quality %, the ceramic oxide powders of 35 ~ 45 quality %, the alkaline earth metal oxide of 12 ~ 25 quality %.
In another advantageous modification of the present invention, in step (1), described glass material converts containing 8-20 quality %B with oxide compound
2o
3, 15-25 quality %La
2o
3, 10-20 quality %SiO
2, 5-10 quality %Al
2o
3, 10-15 quality %MgO and 12-25 quality %ZrO
2.
In the present invention, the ceramic oxide powder powder of step (1) is BaRek
2ti
4o
12ceramic oxide; Wherein, rare earth metal Rek is the mixture of any one or at least two kinds in Ce, Eu, Ho, Tm, Tb, Dy or Yb, and preferably, described rare earth ion is any one mixture in Ce/Eu, Ho/Tm/Yb or Tb/Dy.
In the present invention, the alkaline earth metal oxide of step (1) is the mixture of any one or at least two kinds in aluminium sesquioxide, magnesium oxide, calcium oxide, strontium oxide or barium oxide.
Described in step of the present invention (2) is 10 ~ 30h at 650 ~ 700 DEG C of first time heat treatment times carried out, can be such as 10h, 12h, 15h, 20h, 22h, 25h, 30h, be 15 ~ 25h at 680 ~ 750 DEG C of second time heat treatment times carried out, can be such as 15h, 20h, 22h, 25h, being 60 ~ 80h at 700 ~ 750 DEG C of third time heat treatment times carried out, such as, can be 60h, 62h, 65h, 70h, 72h, 75h, 80h.
The present invention adopts point three thermal treatment 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 that glass-ceramic preparation method of the present invention makes has 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 glass material of 30 quality %, the ceramic oxide powders of 40%, 30 quality % alkaline earth metal oxides;
(2) the first time heat treatment time 10h carried out at 650 DEG C, at the second time heat treatment time 20h that 680 DEG C are carried out, at the third 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 glass material of 35 quality %, the ceramic oxide powders of 45%, 20 quality % alkaline earth metal oxides;
(2) the first time heat treatment time 12h carried out at 660 DEG C, at the second time heat treatment time 25h that 680 DEG C are carried out, at the third 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 glass material of 30 quality %, the ceramic oxide powders of 50%, 20 quality % alkaline earth metal oxides;
(2) the first time heat treatment time 15h carried out at 680 DEG C, at the second time heat treatment time 20h that 700 DEG C are carried out, at the third 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 glass material of 35 quality %, the ceramic oxide powders of 48%, 17 quality % alkaline earth metal oxides;
(2) the first time heat treatment time 20h carried out at 650 DEG C, at the second time heat treatment time 15h that 750 DEG C are carried out, at the third time heat treatment time 75h 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 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 glass material of 30 quality %, the ceramic oxide powders of 42%, 28 quality % alkaline earth metal oxides;
(2) the first time heat treatment time 22h carried out at 700 DEG C, at the second time heat treatment time 10h that 720 DEG C are carried out, at the third time heat treatment time 72h 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 55% with volume basis, and high refractive index filler powder is the pottery of specific refractory power more than 1.98.
As can be seen from above-described embodiment 1-5, 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 (9)
1. a preparation method for glass-ceramic material, is characterized in that, described method comprises the steps:
(1) preparation of raw material is carried out by following proportioning: the alkaline earth metal oxide of the glass material of 30-40 quality %, the ceramic oxide powders of 30-50 quality %, 10-30 quality %;
(2) at 650-700 DEG C, first time thermal treatment is carried out to above-mentioned glass-ceramic, carry out second time thermal treatment at 680-750 DEG C, carry out third 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 the alkaline earth metal oxide of the glass material of 32-38 quality %, the ceramic oxide powders of 35-45 quality % and 12-25 quality %.
3. preparation method as claimed in claim 1 or 2, is characterized in that, in step (1), described glass material converts containing 8-20 quality %B with oxide compound
2o
3, 15-25 quality %La
2o
3, 10-20 quality %SiO
2, 5-10 quality %Al
2o
3, 10-15 quality %MgO and 12-25 quality %ZrO
2.
4. the preparation method as described in any one of claim 1-3, is characterized in that, in step (1), described ceramic oxide powders is BaRek
2ti
4o
12ceramic oxide;
Preferably, described alkaline earth metal oxide is the mixture of any one or at least two kinds in aluminium sesquioxide, magnesium oxide, calcium oxide, strontium oxide or barium oxide.
5. the preparation method as described in any one of claim 1-4, it is characterized in that, in step (1), the rare earth metal Rek contained in described ceramic oxide powders is the mixture of any one or at least two kinds in Ce, Eu, Ho, Tm, Tb, Dy or Yb, preferably, described rare earth ion is any one mixture in Ce/Eu, Ho/Tm/Yb or Tb/Dy.
6. the preparation method as described in any one of claim 1-5, it is characterized in that, described in step (2) is 10 ~ 30h at 650 ~ 700 DEG C of first time heat treatment times carried out, being 15 ~ 25h at 680 ~ 750 DEG C of second time heat treatment times carried out, is 60 ~ 80h at 700 ~ 750 DEG C of third time heat treatment times carried out.
7. the preparation method as described in any one of claim 1-6, it is characterized in that, described in step (2) is 15h at 650 ~ 700 DEG C of first time heat treatment times carried out, being 20h at 680 ~ 750 DEG C of second time heat treatment times carried out, is 80h at 700 ~ 750 DEG C of third time heat treatment times carried out.
8. the glass-ceramic that the preparation method as described in any one of claim 1-7 obtains.
9. a fluorescent glass, is characterized in that, described light source comprises LED and glass-ceramic as claimed in claim 8.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410568827.2A CN104386917A (en) | 2014-10-22 | 2014-10-22 | Glass ceramic material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410568827.2A CN104386917A (en) | 2014-10-22 | 2014-10-22 | Glass ceramic material and preparation method thereof |
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| CN104386917A true CN104386917A (en) | 2015-03-04 |
Family
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| CN201410568827.2A Pending CN104386917A (en) | 2014-10-22 | 2014-10-22 | Glass ceramic material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776871A (en) * | 2016-03-04 | 2016-07-20 | 北京科技大学 | Method for regulating emission cross section of Nd3+/ Na2Ca2Si3O9 laser glass ceramic |
| CN111940894A (en) * | 2019-04-30 | 2020-11-17 | 财团法人金属工业研究发展中心 | Processing method of lithium disilicate glass ceramic |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040121165A1 (en) * | 2002-12-20 | 2004-06-24 | Laird Ronald E. | Coated article with reduced color shift at high viewing angles |
| CN1556775A (en) * | 2000-09-01 | 2004-12-22 | W��C�������Ϲɷ��������Ϲ�˾ | Glass ceramic mass and use thereof |
| CN1807301A (en) * | 2006-01-10 | 2006-07-26 | 桂林迪华特种玻璃有限公司 | Preparation method of crystallite glass |
-
2014
- 2014-10-22 CN CN201410568827.2A patent/CN104386917A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1556775A (en) * | 2000-09-01 | 2004-12-22 | W��C�������Ϲɷ��������Ϲ�˾ | Glass ceramic mass and use thereof |
| US20040121165A1 (en) * | 2002-12-20 | 2004-06-24 | Laird Ronald E. | Coated article with reduced color shift at high viewing angles |
| CN1807301A (en) * | 2006-01-10 | 2006-07-26 | 桂林迪华特种玻璃有限公司 | Preparation method of crystallite glass |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776871A (en) * | 2016-03-04 | 2016-07-20 | 北京科技大学 | Method for regulating emission cross section of Nd3+/ Na2Ca2Si3O9 laser glass ceramic |
| CN105776871B (en) * | 2016-03-04 | 2019-10-18 | 北京科技大学 | A kind of Nd3+/Na2Ca2Si3O9 laser glass ceramics emission cross section regulation method |
| CN111940894A (en) * | 2019-04-30 | 2020-11-17 | 财团法人金属工业研究发展中心 | Processing method of lithium disilicate glass ceramic |
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Application publication date: 20150304 |