CN1880277A - Nanostructured glass ceramics and its sol-gelatin preparation method - Google Patents
Nanostructured glass ceramics and its sol-gelatin preparation method Download PDFInfo
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- CN1880277A CN1880277A CN 200510078781 CN200510078781A CN1880277A CN 1880277 A CN1880277 A CN 1880277A CN 200510078781 CN200510078781 CN 200510078781 CN 200510078781 A CN200510078781 A CN 200510078781A CN 1880277 A CN1880277 A CN 1880277A
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Abstract
This invention relates to a nanostructured pyroceram and the sol-gal process thereof, concretely to a lead fluoride silica dioxide pyroceram and method for making same. The produced PbF2 .SiO2 nanostructured pyroceram body is characterized of high purity, good homogeneity, up to 30mm diameter, up to 1-5mm thickness, good transparency, and good mechanical property(microhardness up to 150kg/mm2).
Description
Technical field
The present invention relates to the glass-ceramic field, especially relate to a kind of plumbous fluoride silica glass pottery and preparation thereof.
Background technology
Glass-ceramic is that glassy phase passes through partially-crystallized getting, and is glass and crystalline complex body; By the control crystallization process, can obtain transparent glass-ceramic, it is a kind of good luminous host.PbF
2SiO
2Nanostructured glass ceramics is a kind of advanced luminescent material that has fluorochemical low phonon energy and oxide compound machinery intensity and thermostability concurrently, has great application prospect in the optical communication field, is subjected to the special concern of Chinese scholars.Prepare PbF at present
2SiO
2The method of glass ceramic material is a melt quenching method, and its preparation condition requires high temperature, all makes troubles for research and production; In addition, it is even inadequately to distribute with the material component of this method preparation, and because part material evaporation during high-temperature fusion causes final material component off-design value.
Summary of the invention
The present invention proposes a kind of PbF
2SiO
2Nanostructured glass ceramics and sol-gel preparation technology thereof.
The PbF of the present invention's preparation
2SiO
2The component of nanostructured glass ceramics is: XPbF
2-YSiO
2-ZErF
3(X=5-10mol%, Y=(100-X-Z) mol%, Z=0-1mol%).
The present invention adopts and is prepared as follows technology: with plumbic acetate (Pb (AC)
23H
2O), acetic acid erbium (Er (AC)
3), trifluoroacetic acid (TFA) and water mixes in beaker, and heating for dissolving obtains clear solution (following abbreviation Pb/TFA solution); In another beaker, add tetraethoxy (TEOS), dehydrated alcohol and water mix and stir (below be called for short TEOS/H
2O solution), then splash into hydrolyst, as HNO
3, CH
3COOH etc.The Pb/TFA drips of solution is added to TEOS/H
2In the O solution, stir the colloidal sol that obtains homogeneous transparent.This colloidal sol slowly is warming up to 120 ℃ after the room temperature ageing, drying obtains transparent xerogel; Xerogel speed with 1-10 ℃/min in process furnace is warming up to 350 ℃-550 ℃, obtains PbF
2SiO
2The nanostructured glass ceramics block.
The PbF for preparing
2SiO
2Nanostructured glass ceramics block purity height, good uniformity, diameter reaches 30mm, and thickness reaches 1-5mm, is heigh clarity, and (microhardness reaches 150kg/mm to have the favorable mechanical performance
2).Mix behind a spot of luminescence rare earth erbium ion, the outward appearance and the mechanical property of glass-ceramic block remain unchanged substantially.
Material preparation process of the present invention is simple, and not strict to the requirement of required equipment, cost is lower, can obtain the various shapes that meet service requirements such as circular or square; Process for preparing sol-gel of the present invention is with present preparation PbF
2SiO
2The melt quenching method that glass ceramic material adopts is compared, and preparation temperature reduces greatly, and glass-ceramic block purity height, the good uniformity prepared; Since no raw materials evaporate, final component and design load basically identical.So PbF of the present invention
2SiO
2The nanostructured glass ceramics block will become a kind of good novel light-emitting matrix.
Embodiment
Example 1: with 0.005mol plumbic acetate (Pb (AC)
23H
2O), 0.03mol trifluoroacetic acid (TFA) and 0.02mol water mixes in beaker, and heating for dissolving obtains clear solution (following abbreviation Pb/TFA solution); In another beaker, add 0.1mol tetraethoxy (TEOS), 0.4mol dehydrated alcohol and 0.02mol water, splash into hydrolyst CH
3COOH mixes and stirs 30min (following abbreviation TEOS/H
2O solution).The Pb/TFA drips of solution is added to TEOS/H
2In the O solution, the pH value to 2 of regulator solution covers preservative film then and stirred 4 hours, obtains homogeneous transparent colloidal sol.
Even colloidal sol is poured in the glass culture dish, covered preservative film.Strict its rate of drying of control---after 1 week of room temperature ageing,, accelerate it and form gelation process, guarantee that again gel does not break simultaneously stinging several apertures on the preservative film equably; Through after 1 all ageings, slowly be warming up to 120 ℃ of dryings 7 days again, obtain transparent xerogel; Xerogel is warming up to 500 ℃ with 5 ℃/min speed in retort furnace, obtains PbF
2SiO
2The glass-ceramic block is observed its microstructure, its PbF under the JEM2010 transmission electron microscope
2Grain-size is about 10-30nm, reaches nanometer scale.Measuring its microhardness on the HX-1000 microhardness tester is 150kg/mm
2
Example 2: with 0.005mol plumbic acetate (Pb (AC)
23H
2O), 0.03mol trifluoroacetic acid (TFA), 0.00025mol acetic acid erbium (Er (AC)
3) and 0.02mol water in beaker, mix, and heating for dissolving obtains clear solution (following abbreviation Pb/TFA solution); In another beaker, add 0.1mol tetraethoxy (TEOS), 0.4mol ethanol (CH
3CH
2OH) and 0.02mol water, splash into hydrolyst CH
3COOH mixes and stirs 30min (following abbreviation TEOS/H
2O solution).The Pb/TFA drips of solution is added to TEOS/H
2In the O solution, the pH value to 2 of regulator solution covers preservative film then and stirred 4 hours, obtains homogeneous transparent colloidal sol.
After the drying and heat treatment process identical, obtain being mixed with the PbF of 0.5% erbium ion with example 1
2SiO
2The nanostructured glass ceramics block is observed its microstructure, its PbF under the JEM2010 transmission electron microscope
2Grain-size is about 5-20nm.Measuring its microhardness on the HX-1000 microhardness tester is 123kg/mm
2
Example 3: with 0.005mol plumbic acetate (Pb (AC)
23H
2O), 0.03mol trifluoroacetic acid (TFA), 0.0005mol acetic acid erbium (Er (AC)
3) and 0.02mol water in beaker, mix, and heating for dissolving obtains clear solution (following abbreviation Pb/TFA solution); In another beaker, add 0.1mol tetraethoxy (TEOS), 0.4mol ethanol (CH
3CH
2OH) and 0.02mol water, splash into hydrolyst CH
3COOH mixes and stirs 30min (following abbreviation TEOS/H
2O solution).The Pb/TFA drips of solution is added to TEOS/H
2In the O solution, the pH value to 2 of regulator solution covers preservative film then and stirred 4 hours, obtains homogeneous transparent colloidal sol.
Through wanting after drying identical and the heat treatment process, obtain being mixed with the PbF of 1% erbium ion with example 1
2SiO
2The nanostructured glass ceramics block is observed its microstructure, its PbF under the JEM2010 transmission electron microscope
2Grain-size is about 5-15nm.Measuring its microhardness on the HX-1000 microhardness tester is 112kg/mm
2
Claims (3)
1. the process for preparing sol-gel of a nanostructured glass ceramics is characterized in that:
(1) component of this glass-ceramic is: XPbF
2-YSiO
2-ZErF
3(X=5-10mol%, Y=(100-X-Z) mol%, Z=0-1mol%);
(2) with plumbic acetate (Pb (AC)
23H
2O), acetic acid erbium (Er (AC)
3), trifluoroacetic acid (TFA) and water mixes in beaker, and heating for dissolving obtains clear solution (following abbreviation Pb/TFA solution); In another beaker, add tetraethoxy (TEOS), dehydrated alcohol and water mix and stir (below be called for short TEOS/H
2O solution), then splash into hydrolyst; The Pb/TFA drips of solution is added to TEOS/H
2In the O solution, stir the colloidal sol that obtains homogeneous transparent; This colloidal sol slowly is warming up to 120 ℃ after the room temperature ageing, drying obtains transparent xerogel; Xerogel speed with 1-10 ℃/min in process furnace is warming up to 350 ℃-550 ℃, obtains PbF
2SiO
2The nanostructured glass ceramics block.
2. preparation method as claimed in claim 1 is characterized in that: described hydrolyst HNO
3Or CH
3COOH.
3. nanostructured glass ceramics by claim 1 or the preparation of 2 described methods.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510078781 CN1880277A (en) | 2005-06-13 | 2005-06-13 | Nanostructured glass ceramics and its sol-gelatin preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510078781 CN1880277A (en) | 2005-06-13 | 2005-06-13 | Nanostructured glass ceramics and its sol-gelatin preparation method |
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|---|---|
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ID=37518667
Family Applications (1)
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|---|---|---|---|
| CN 200510078781 Pending CN1880277A (en) | 2005-06-13 | 2005-06-13 | Nanostructured glass ceramics and its sol-gelatin preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101840011A (en) * | 2010-04-15 | 2010-09-22 | 上海聚恒太阳能有限公司 | Manufacture method for nanometer self-cleaning spotlight solar energy Fresnel lens |
| CN101641155B (en) * | 2007-02-14 | 2013-07-10 | 皮埃尔-玛丽-居里大学 | Hybrid material, and method for the production |
-
2005
- 2005-06-13 CN CN 200510078781 patent/CN1880277A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101641155B (en) * | 2007-02-14 | 2013-07-10 | 皮埃尔-玛丽-居里大学 | Hybrid material, and method for the production |
| CN101840011A (en) * | 2010-04-15 | 2010-09-22 | 上海聚恒太阳能有限公司 | Manufacture method for nanometer self-cleaning spotlight solar energy Fresnel lens |
| CN101840011B (en) * | 2010-04-15 | 2012-03-28 | 上海聚恒太阳能有限公司 | Manufacture method for nanometer self-cleaning spotlight solar energy Fresnel lens |
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Open date: 20061220 |