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Nanostructured glass ceramics and its sol-gelatin preparation method

A technology of glass ceramics and nanostructures, applied in the field of glass ceramics, can solve the problems of uneven distribution of material components, deviation of material components from design values, inconvenience in research and production, etc., and achieve low cost, low preparation temperature and good uniformity Effect

Inactive Publication Date: 2006-12-20
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently preparing PbF 2 ·SiO2 2 The method of glass-ceramic materials is the melting and quenching method, and its preparation conditions require high temperature, which brings inconvenience to research and production; in addition, the distribution of material components prepared by this method is not uniform enough, and due to the evaporation of some raw materials during high-temperature melting, resulting in The final material composition deviates from the design value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0008] Example 1: Add 0.005mol of lead acetate (Pb(AC) 2 ·3H 2 O), 0.03mol of trifluoroacetic acid (TFA) and 0.02mol of water were mixed in a beaker and heated to dissolve to obtain a transparent solution (hereinafter referred to as Pb / TFA solution); in another beaker, add 0.1mol of ethyl orthosilicate ( TEOS), 0.4mol of absolute ethanol and 0.02mol of water, drip into the hydrolysis catalyst CH 3 COOH, mix and stir for 30min (hereinafter referred to as TEOS / H 2 O solution). Add Pb / TFA solution dropwise to TEOS / H 2 In the O solution, adjust the pH of the solution to 2, then cover with a plastic wrap and stir for 4 hours to obtain a uniform transparent sol.

[0009] Pour the uniform sol into a glass petri dish and cover with plastic wrap. Strictly control the drying speed-after aging at room temperature for 1 week, evenly pierce a number of small holes in the cling film to speed up the gel formation process while ensuring that the gel does not break; after another week of aging, Sl...

example 2

[0010] Example 2: Add 0.005mol of lead acetate (Pb(AC) 2 ·3H 2 O), 0.03mol trifluoroacetic acid (TFA), 0.00025mol erbium acetate (Er(AC) 3 ) And 0.02mol of water were mixed in a beaker and heated to dissolve to obtain a transparent solution (hereinafter referred to as Pb / TFA solution); in another beaker, add 0.1mol of ethyl orthosilicate (TEOS), 0.4mol of ethanol (CH 3 CH 2 OH) and 0.02mol water, drip into the hydrolysis catalyst CH 3 COOH, mix and stir for 30min (hereinafter referred to as TEOS / H 2 O solution). Add Pb / TFA solution dropwise to TEOS / H 2 In the O solution, adjust the pH of the solution to 2, then cover with a plastic wrap and stir for 4 hours to obtain a uniform transparent sol.

[0011] After the same drying and heat treatment process as in Example 1, PbF doped with 0.5% erbium ion is obtained 2 ·SiO 2 Nanostructured glass-ceramic block, its microstructure was observed under JEM2010 transmission electron microscope, its PbF 2 The grain size is about 5-20nm. The mic...

example 3

[0012] Example 3: Add 0.005mol of lead acetate (Pb(AC) 2 ·3H 2 O), 0.03mol trifluoroacetic acid (TFA), 0.0005mol erbium acetate (Er(AC) 3 ) And 0.02mol of water were mixed in a beaker and heated to dissolve to obtain a transparent solution (hereinafter referred to as Pb / TFA solution); in another beaker, add 0.1mol of ethyl orthosilicate (TEOS), 0.4mol of ethanol (CH 3 CH 2 OH) and 0.02mol water, drip into the hydrolysis catalyst CH 3 COOH, mix and stir for 30min (hereinafter referred to as TEOS / H 2 O solution). Add Pb / TFA solution dropwise to TEOS / H 2 In the O solution, adjust the pH of the solution to 2, then cover with a plastic wrap and stir for 4 hours to obtain a uniform transparent sol.

[0013] After the same drying and heat treatment process as in Example 1, PbF doped with 1% erbium ion is obtained 2 ·SiO 2 Nanostructured glass-ceramic block, its microstructure was observed under JEM2010 transmission electron microscope, its PbF 2 The grain size is about 5-15nm. The microh...

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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 [0001] The invention relates to the field of glass ceramics, in particular to a lead fluoride silica glass ceramic and its preparation. Background technique [0002] Glass ceramics are obtained through partial crystallization of the glass phase, which is a composite of glass and crystals; by controlling the crystallization process, transparent glass ceramics can be obtained, which is a good light-emitting substrate. PbF 2 ·SiO 2 Nanostructured glass ceramic is a new type of luminescent material with low phonon energy of fluoride and oxide mechanical strength and thermal stability. It has great application prospects in the field of optical communication and has attracted special attention from scholars at home and abroad. PbF is currently prepared 2 ·SiO 2 The method of glass ceramic materials is the melting quenching method, and its preparation conditions require high temperature, which brings inconvenience to research and production; in a...

Claims

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Application Information

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IPC IPC(8): C04B35/624C04B35/14C03C10/14
Inventor 周丽花王元生罗文钦陈大钦
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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