CN102584012A - Low-melting-point optical glass and preparation method thereof - Google Patents
Low-melting-point optical glass and preparation method thereof Download PDFInfo
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- CN102584012A CN102584012A CN2012100300948A CN201210030094A CN102584012A CN 102584012 A CN102584012 A CN 102584012A CN 2012100300948 A CN2012100300948 A CN 2012100300948A CN 201210030094 A CN201210030094 A CN 201210030094A CN 102584012 A CN102584012 A CN 102584012A
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Abstract
The invention provides a low-melting-point optical glass, which is prepared by a chemical raw materials containing 20-65% of P2O5, 23-40% of ZnO, 7-36% of B2O3 and 3-8% of (Li2O+Na2O+K2O) by the mass mole percent, wherein the Li2O accounts for at least 2%. Oxide or carbonate raw materials containing the components are weighed by proportion, mixed evenly in a platinum crucible, melted in an electric furnace of 900-1300 DEG C for 1-3 hours and then quenched to obtain the low-melting-point optical glass. The low-melting-point optical glass has the advantages that the optical glass does not contain Bi2O3, is colorless and transparent and has high transmissivity to visible light.
Description
Technical field
The invention belongs to optical glass material, particularly a kind of low-melting point optical glass and preparation method thereof.
Background technology
White light LEDs has plurality of advantages such as energy-saving and environmental protection and long lifetime as the novel illumination light source, and its principle of work is to utilize blue chip and xanchromatic phosphor combination (or other array mode) to obtain white light.Current mainly is to utilize silica gel or resin to mix with fluorescent material to encapsulate.One of shortcoming of this packaged type (especially for high-power LED encapsulation) is through long illumination and thermal environment silica gel or resin meeting flavescence, to influence the light extraction efficiency of LED.
To the problems referred to above, use glass to mix and encapsulate and effectively to address this problem, because glass has under illumination than silica gel or resin excellent chemical stability with fluorescent material.Based on above-mentioned application background, the glass that above-mentioned background needs must have following characteristic: low fusing point (package temperature is lower than blue chip growth temperature (600 ℃)) and high visible light wave range transmitance.Though CN201010117674.1LED element (2) contain glass Al2O3 substrate (3), it is low melting glass that P2O5-ZnO is set abreast, still has room for improvement on the prescription, especially has aspect the high transmitance index at visible light wave range.
Summary of the invention
The present invention seeks to, the fusing point that reduces glass with and make it have high transmitance at visible light wave range, thereby address the above problem.
The method that the present invention solves the problems of the technologies described above is in glass, not use the raw material Bi that can reduce glass transition temp usually
2O
3And WO
3Above-mentioned two kinds of raw materials can make glass coloring when reducing glass transition temp, influence the transmitance of glass at visible light wave range.
The method that the present invention solves the problems of the technologies described above is that low-melting point optical glass does not use the raw material PbO that can reduce glass transition temp usually in glass.Above-mentioned raw materials can reduce glass transition temp, but pollutes the environment.
Technical scheme of the present invention is: a kind of low-melting point optical glass that provides, the shared quality x of each component is respectively: P
2O
5: 20-65%, ZnO:23-40%, B
2O
3: 7%-36%, (Li
2O+Na
2O+K
2O): 3-8%.More than be molar percentage.Li wherein
2O will account for 2% at least.The present invention especially adopts following prescription: P
2O
5: 33-41%, ZnO:34-40%, B
2O
3: 18-22%, (Li
2O3%+Na
2O 1%+K
2O 1%): 5-8%.
P
2O
5For forming the staple of glass network structure, be necessary.Component is lower than at 20% o'clock can not form glass, and component is higher than at 65% o'clock, its unstable chemcial property.
ZnO can reduce the second-order transition temperature of glass, is neccessary composition.It is relatively poor that component is lower than 23% o'clock chemicalstability, is higher than 40% o'clock easy crystallization of glass.
B
2O
3Can improve the glass melting effect, also help to reduce the second-order transition temperature of glass, be neccessary composition.Component is lower than 7% and is reducing DeGrain aspect the second-order transition temperature of glass, and it is relatively poor that component is higher than the chemicalstability of 36% o'clock glass.
[010] Li
2O, Na
2O, K
2O can destroy the network structure of glass, reduces the second-order transition temperature of glass.Total component is lower than at 3% o'clock, reduces the second-order transition temperature DeGrain, and total component is higher than at 8% o'clock, and the chemicalstability of glass is relatively poor.
In addition as the inessential composition of glass, Sb
2O
3The finings that can be used as in preparation glass process uses, and consumption is below 1% of all raw material total mole numbers.
In addition as the inessential composition of glass, NaNO
3The skimmer that can be used as in preparation glass process uses, and consumption is below 1% of all raw material total mole numbers.
Preparing method of the present invention is: by the shared molecular fraction weighing raw materials P of each component
2O
5, ZnO, B
2O
3(or H
3BO
3), Li
2CO
3, Na
2CO
3, K
2CO
3And quality is the Sb below 1% of said mixture total mass
2O
3For finings and quality are the NaNO below 1% of said mixture total mass
3Be skimmer; 2) with above-mentioned load weighted starting material P
2O
5, ZnO, B
2O
3(H
3BO
3), Li
2CO
3, Na
2CO
3, K
2CO
3, Sb
2O
3, NaNO
3Put into behind the thorough mixing in the platinum crucible and in electric furnace and in 900 ℃-1300 ℃ electric furnace, melted 1-3 hour; The fused glass metal poured into be cooled in the mould below 600 ℃, and then put in the electric furnace and to be annealed to room temperature in 550 ± 50 ℃ and promptly to obtain the glass that needs.
With above-mentioned load weighted starting material P
2O
5, ZnO, B
2O
3(H
3BO
3), Li
2CO
3, Na
2CO
3, K
2CO
3, Sb
2O
3, NaNO
3Put into behind the thorough mixing in the platinum crucible and in electric furnace and in 900 ℃-1300 ℃ electric furnace, melted 1-3 hour.The fused glass metal poured into be cooled to it in the mould below the yield-point, and then put into and be annealed to room temperature in the electric furnace and promptly obtain the glass that needs.
The invention has the beneficial effects as follows: it is higher by about 2% than the glass of prior art that visible light wave range has high transmitance.Clear and bright limpid on the glass appearance, obviously high in the transmitance of visible light wave range.The chemicalstability and the temperature stability of annealing back glass are better.
Embodiment
Embodiment 1: by the shared molecular fraction of each component: P
2O
5: 20-65%, ZnO:23-40%, B
2O
3: 7%-36%, (Li
2O+Na
2O+K
2O): 3-8% weighing raw materials P
2O
5, ZnO, B
2O
3(or H
3BO
3), Li
2CO
3, Na
2CO
3, K
2CO
3, consumption is the Sb below 1% of all raw material total mole numbers
2O
3And consumption is the NaNO below 1% of all raw material total mole numbers
3
The prescription of low melting glass is (molar percentage):
1、P
2O
5:37%,ZnO:37%,B
2O
3:20%,(Li
2O3%+Na
2O1.5%+K
2O1.5%):6%。
2、P
2O
5:38%,ZnO:36%,B
2O
3:19%,(Li
2O2%+Na
2O2.5%+K
2O2.5%):7%。
3、P
2O
5:39%,ZnO:35%,B
2O
3:18%,(Li
2O3%+Na
2O2%+K
2O3%):8%。
4、P
2O
5:41%,ZnO:34%,B
2O
3:19%,(Li
2O3%+Na
2O1.5%+K
2O1.5%):6%。
5、P
2O
5:35%,ZnO:38%,B
2O
3:21%,(Li
2O3%+Na
2O1.5%+K
2O1.5%):6%。
6、P
2O
5:33%,ZnO:40%,B
2O
3:22%,(Li
2O3%+Na
2O?1%+K
2O?1%):5%。
7、P
2O
5:34%,ZnO:39%,B
2O
3:21%,(Li
2O3%+Na
2O1.5%+K
2O1.5%):6%。
8、P
2O
5:35%,ZnO:39%,B
2O
3:20%,(Li
2O3%+Na
2O1.5%+K
2O1.5%):6%。
Concrete preparation process is following: by the shared molecular fraction weighing raw materials P of each component
2O
5, ZnO, B
2O
3, Li
2CO
3, Na
2CO
3, K
2CO
3, 0.8% Sb
2O
3And 0.9% NaNO
3
[014] with above-mentioned load weighted starting material P
2O
5, ZnO, B
2O
3, Li
2CO
3, Na
2CO
3, K
2CO
3, Sb
2O
3, NaNO
3Put into behind the thorough mixing in the platinum crucible and in electric furnace and in 1150 ℃ electric furnace, melted 2 hours.The fused glass metal poured into be cooled to it in the mould below the yield-point, and then put into and be annealed to room temperature in the electric furnace and promptly obtain the glass that needs.
The glass of above-mentioned acquisition is as clear as crystal, has no color, does not have crackle and bubble, and is more excellent on routine 1 performance.
Utilize the second-order transition temperature and the yield-point of the above-mentioned glass of DSC experiment measuring.
The second-order transition temperature of above-mentioned glass is 491 ℃, and yield-point is 526 ℃.
Claims (4)
1. a low-melting point optical glass is characterized in that comprising P
2O
5, ZnO, B
2O
3And Li
2O, Na
2O and K
2The chemical feedstocks of O component is prepared from; The shared quality molecular fraction of each component is respectively: low-melting point optical glass, the shared quality molecular fraction of each component is respectively: P
2O
5: 20-65%, ZnO:23-40%, B
2O
3: 7%-36%, (Li
2O+Na
2O+K
2O): 3-8%; Li wherein
2O will account for 2% at least.
2. low-melting point optical glass according to claim 1 is characterized in that the shared quality molecular fraction of each component is respectively: P
2O
5: 33-41%, ZnO:34-40%, B
2O
3: 18-22%, (Li
2O3%+Na
2O 1%+K
2O 1%): 5-8%.
3. low-melting point optical glass according to claim 1 and 2 is characterized in that the shared quality molecular fraction of each component is respectively: P
2O
5: 37%, ZnO:37%, B
2O
3: 20%, (Li
2O3%+Na
2O1.5%+K
2O1.5%): 6%.
4. according to claim 1 described low melting glass preparation method one of so far, it is characterized in that comprising the steps: 1), by the shared molecular fraction weighing raw materials P of each component
2O
5, ZnO, B
2O
3(or H
3BO
3), Li
2CO
3, Na
2CO
3, K
2CO
3And quality is the Sb below 1% of said mixture total mass
2O
3For finings and quality are the NaNO below 1% of said mixture total mass
3Be skimmer; 2) with above-mentioned load weighted starting material P
2O
5, ZnO, B
2O
3(H
3BO
3), Li
2CO
3, Na
2CO
3, K
2CO
3, Sb
2O
3, NaNO
3Put into behind the thorough mixing in the platinum crucible and in electric furnace and in 900 ℃-1300 ℃ electric furnace, melted 1-3 hour; The fused glass metal poured into be cooled in the mould below 600 ℃, and then put in the electric furnace and to be annealed to room temperature in 550 ± 50 ℃ and promptly to obtain the glass that needs.
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CN2012100300948A CN102584012A (en) | 2012-02-10 | 2012-02-10 | Low-melting-point optical glass and preparation method thereof |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112830680A (en) * | 2019-11-22 | 2021-05-25 | 华北理工大学 | Heat-insulating glass glaze and preparation method thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007051055A (en) * | 2005-07-19 | 2007-03-01 | Ohara Inc | Optical glass |
CN101265024A (en) * | 2008-04-08 | 2008-09-17 | 中国计量学院 | Low-melting point leadless borophosphate seal glass powder and preparation method thereof |
CN102173582A (en) * | 2011-02-25 | 2011-09-07 | 东华大学 | Media glass used for infrared heating coating and preparation method thereof |
CN102190439A (en) * | 2010-03-16 | 2011-09-21 | 李胜春 | Blue phosphate glass used for high-power tube, and preparation method thereof |
-
2012
- 2012-02-10 CN CN2012100300948A patent/CN102584012A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2007051055A (en) * | 2005-07-19 | 2007-03-01 | Ohara Inc | Optical glass |
CN101265024A (en) * | 2008-04-08 | 2008-09-17 | 中国计量学院 | Low-melting point leadless borophosphate seal glass powder and preparation method thereof |
CN102190439A (en) * | 2010-03-16 | 2011-09-21 | 李胜春 | Blue phosphate glass used for high-power tube, and preparation method thereof |
CN102173582A (en) * | 2011-02-25 | 2011-09-07 | 东华大学 | Media glass used for infrared heating coating and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112830680A (en) * | 2019-11-22 | 2021-05-25 | 华北理工大学 | Heat-insulating glass glaze and preparation method thereof |
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Application publication date: 20120718 |