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Oxynitride sealing glass and preparation method thereof

A technology for sealing glass and nitrogen oxides, which is applied in glass manufacturing equipment, glass molding, manufacturing tools, etc., can solve the problem of low nitrogen doping, and achieve the effects of stable preparation process, easy access to raw materials, and simple raw materials

Active Publication Date: 2018-11-13
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional method of doping nitrogen in molten glass with anhydrous ammonia gas has a low nitrogen doping amount (Journal of the European Ceramic Society, 2012(32) 1389-94)

Method used

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  • Oxynitride sealing glass and preparation method thereof
  • Oxynitride sealing glass and preparation method thereof
  • Oxynitride sealing glass and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] 1. Add 30 ml H to 2.13 g trichloroborazine 2 O, add 1 M / L NH dropwise 3 •H 2 0 to pH=8, stirred at 45 °C for 24 h to obtain solution A, and set aside;

[0035] 2. Take 4.92 g of ATSB, add 2.6 g of EAA, add IPA to make the overall weight 24 g, and stir for 1 hour to obtain solution B, set aside;

[0036] 3. Take 3.22 g of TMB, add IPA to the total mass of 24 g, stir for 1 h to obtain solution C, and set aside;

[0037] 4. Take TEOS 14.11 g, add H 2 O 2.82 ml, 1 M / mol HNO 3 2.83g, add IPA to make the overall mass 24g, magnetic stirrer for 1 h, obtain solution D, set aside;

[0038] 5. After mixing solutions B, C, and D and stirring them magnetically for 1 h, add 10.65 g of Sr(NO 3 ) 2 , after the complete dissolution, continue magnetic stirring for 30 min, add 11.88 g Ca(NO 3 ) 2 • 4H 2 O, after completely dissolving, stir for 30 min to obtain solution F;

[0039] 6. Add solution A dropwise to the obtained homogeneous solution F, and magnetically stir for 30 ...

Embodiment 2

[0045] 1. Add 50 ml H to 12.45 g trichloroborazine 2 O, add 1 M / L NH dropwise 3 •H 2 O to pH=8, stirred at 45 °C for 24 h, A obtained solution A, set aside;

[0046] 2. Take 4.92 g of ATSB, add 2.6 g of EAA, add IPA to make the overall weight 24 g, and stir for 1 hour to obtain solution B, set aside;

[0047] 3. Take TEOS 14.11 g, add H 2 O 2.82 ml, 1 M / mol HNO 3 2.83g, add IPA to make the overall mass 24g, magnetic stirrer for 1 h, obtain solution D, set aside;

[0048] 4. Mix solutions B, C, and D and stir them magnetically for 1 h, then add 10.65 g of Sr(NO 3 ) 2 , and continued magnetic stirring for 30 min after complete dissolution, then added 11.88 g Ca(NO 3 ) 2 • 4H 2 O, stirred for 30 min after complete dissolution to obtain solution F;

[0049] 5. Add solution A dropwise to the obtained homogeneous solution F, and magnetically stir for 30 min to obtain solution H;

[0050] 6. Add 1 M / L NH dropwise to Solution H 3 •H 2O until the pH = 11, stirring contin...

Embodiment 3

[0055] 1. Add 50 ml H to 16 g trichloroborazine 2 O, add 1 M / L NH dropwise 3 •H 2 O to PH=8, stirred at 45 °C for 24 h, A obtained solution A, set aside;

[0056] 2. Take 4.92 g ATSB, add 2.6 g EAA, add IPA to make the overall weight 24 g, stir magnetically for 1 hour, and obtain solution B, set aside;

[0057] 3. Take TEOS 14.11 g, add H 2 O 2.82 ml, 1 M / mol HNO 3 2.83g, add IPA to make the overall mass 24g, magnetic stirrer for 1 h, obtain solution D, set aside;

[0058] 4. Mix solutions B, C, and D and stir them magnetically for 1 h, then add 10.65 g of Sr(NO 3 ) 2 , after the complete dissolution, continue magnetic stirring for 30 min, add 11.88 g Ca(NO 3 ) 2 • 4H 2 O, after completely dissolving, stir for 30 min to obtain solution F;

[0059] 5. Add solution A dropwise to the obtained homogeneous solution F, and magnetically stir for 30 min to obtain solution H;

[0060] 6. Add 1 M / L NH dropwise to Solution H 3 •H 2 O until PH = 11, stirring continuously fo...

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PUM

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Abstract

The invention discloses an oxynitride sealing glass and a preparation method thereof, and belongs to the technical field of preparation of low-temperature sealing glass. The nitrogen oxide sealing glass is prepared from the following raw materials: Ca(NO3)2.4H2O, aluminum tri-tert-butoxide, trimethyl borate, tetraethoxysilane, Sr(NO3)2, trichloroborazine and a solvent; and a glass network structure is obtained by a sol-gel method. Compared with a method for doping nitrogen in a molten state of glass by anhydrous ammonia gas, the preparation method provided by the invention selects trichloroborazine as an organic nitrogen source to prepare oxynitride glass in a solution state, not only can obtain a higher nitrogen content, but also can significantly improve sealing performance of glass by the introduced boron element, has the advantages of simple and readily available preparation raw materials and stable process, and achieves industrialization conditions.

Description

technical field [0001] The invention belongs to the technical field of sealing glass preparation, and in particular relates to a nitrogen oxide sealing glass and a sol-gel preparation method thereof. Background technique [0002] Based on the structural characteristics of the stacked fuel cell (SOFC), in order to prevent fuel gas from leaking and mixing with air at high temperature, the cell structure must be strictly sealed. In order to prevent leakage, the sealing material is required to have high insulation; the operating temperature of high-temperature fuel cells is 800-1000 ° C, and the operating time is long, the sealing material is required to have long-term high-temperature chemical stability and thermal stability, even Sufficient heat cycle resistance is required. Glass has attracted widespread attention at home and abroad because of its high insulation, thermal stability, chemical stability and good mechanical properties. [0003] On the other hand, previous stud...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03B19/12C03C4/00
CPCC03B19/12C03C4/00
Inventor 张腾李曾艳姜晓婷林铭雄
Owner FUZHOU UNIV
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