CN101712533B - Lead-free glass powder for glass-ceramics adhesion, preparation method and application thereof - Google Patents
Lead-free glass powder for glass-ceramics adhesion, preparation method and application thereof Download PDFInfo
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- CN101712533B CN101712533B CN2009101029472A CN200910102947A CN101712533B CN 101712533 B CN101712533 B CN 101712533B CN 2009101029472 A CN2009101029472 A CN 2009101029472A CN 200910102947 A CN200910102947 A CN 200910102947A CN 101712533 B CN101712533 B CN 101712533B
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Abstract
The invention provides lead-free glass powder for glass-ceramics adhesion, a preparation method and application thereof, which belongs to the technical field of chemical engineering and electrons. The powder is formed by proportioning and processing the following raw materials in percentage by mass: 20 to 50 percent of stannous phosphate, 40 to 70 percent of zinc phosphate, 1 to 5 percent of aluminum phosphate, 0.5 to 2 percent of calcium phosphate, 0.5 to 1 percent of strontium phosphate, 1 to 3 percent of iron phosphate, and 2 to 6 percent of barium phosphate. The powder has fire-retarding temperature between 280 and 600 DEG C, low expansion coefficient between 20 and 300 DEG C, average linear expansion coefficient of 90+/-3*10-7/DEG C, transformation temperature of 240+/-3 DEG C and softening temperature of 280+/-3 DEG C. The glue is suitable for mutual adhesion between soda-lime glass and ceramics.
Description
Technical field: the invention belongs to chemical industry, electronic technology field, specifically a kind of low-melting point lead-less glasses powder and its production and application.
Background technology: China's Ministry of Information Industry stipulates that clearly it is 0.1% (1000ppm) that the maximum of six kinds of poisonous and harmful element lead (Pb), mercury (Hg), sexavalent chrome (Cr6+), Polybrominated biphenyl (PBB), polybromodiphenyl ether (PBDE) in the glass powder allows content, cadmium (cd) is 0.01% (100ppm), require to implement lead-free process, the content of poisonous and harmful element will be up to state standards in all electronic products.Face the restriction of unleaded policy of China and international environmental protection policy threshold, the new low-melting point lead-less glasses powder of our numerous and confused developments is about patent application has: " low-melting point lead-less glasses powder for frit slurry and preparation method thereof and purposes " application number 200810200747.6; " a kind of with metal or alloy lead-free glass powder with low melting point for sealing and preparation method thereof " application number 200710043182.0 " a kind of no-lead RE doped sealing glass powder with low smelting point and manufacture method thereof " application number 200710111386.3, " a kind of low-melting point leadless borophosphate seal glass powder and preparation method thereof " application number 200810060990.2, the present invention is according to the application purpose difference, from having created a kind of low-melting point leadless adhesion glass powder, performance is suitable with low melting point flint glass powder, can replace low melting point flint glass powder and be applied in inter-adhesive between soda-lime glass and the pottery.Aspect formulation ratio unlike the prior art.
Summary of the invention: the objective of the invention is to, 1. according to industry or this enterprise to the different glass powder of developing a series of different ingredients of adhesion object, satisfy different adhesion objects to different glass powder performance demands.The present invention is exactly one of serial different ingredients glass powder, and glass powder of the present invention is suitable for inter-adhesive between soda-lime glass and the pottery; 2. the product of the present invention's development meets the requirement of not having six kinds of harmful elements in China's Ministry of Information Industry's regulation glass powder; 3. the compound method of glass powder of the present invention is disclosed.
A kind of glass of the present invention and ceramics adhesion lead-free glass powder, be to be the phosphoric acid stannous chloride of 20-50% by mass percent, the 40-70% zinc phosphate, 1-5% aluminum phosphate, 0.5-2% calcium phosphate, the 0.5-1% strontium phosphate, the 1-3% tertiary iron phosphate, 2-6% barium phosphate formulated forms refractory temperature: 280～600 ℃, the lower coefficient of expansion is arranged, at 20～300 ℃ of averages coefficient of linear expansion 90 ± 3 * 10
-7/ ℃, 240 ± 3 ℃ of invert points, 280 ± 3 ℃ of softening temperatures.
The quality proportioning of above-mentioned formulation optimization is: the phosphoric acid stannous chloride of 30-40%, and the 50-60% zinc phosphate, the 1-5% aluminum phosphate, 0.5-2% calcium phosphate, the 0.5-1% strontium phosphate, the 1-3% tertiary iron phosphate, the 2-6% barium phosphate is formed.
A kind of glass of the present invention and the ceramics adhesion compound method of lead-free glass powder is to follow these steps to process:
1. according to above-mentioned formulation ratio all phosphoric acid salt are mixed;
2. with phosphate mixt 1000-1200 ℃ of time fusing, be incubated 0.5-1 hour;
3. the liquid that melts is cooled off the homogeneous particle that forms disordered structure fast in water, take out drying and be finely ground to glass powder.
A kind of glass of the present invention and ceramics adhesion be with the application of lead-free glass powder, is suitable for inter-adhesive between soda-lime glass and the pottery, the cold-resistant thermal shocking of adhesion device, and matching is good.
Its coefficient of expansion of the pottery of above-mentioned indication will be complementary with glass powder of the present invention, promptly is that its coefficient of linear expansion is identical or close with glass powder coefficient of linear expansion of the present invention.
The invention effect: glass powder chemical stability of the present invention is good, and acid resistance is good, is that stable existence is not corroded in 3 the acid solution at pH value, and refractory temperature is at 280-600 ℃, 20-300 ℃ of average coefficient of linear expansion 90 ± 3X10
-7/ ℃, 240 ± 3 ℃ of invert points, 280 ± 3 ℃ of softening temperatures are particularly suitable for inter-adhesive between soda-lime glass and the pottery, the cold-resistant thermal shocking of the device after the adhesion, matching is good.
This glass powder kind does not contain noble metal, and no poisonous and harmful element does not constitute pollution to environment, and raw materials cost is low, and operating procedure is simple, realizes suitability for industrialized production easily.
Embodiment: embodiment 1, press phosphoric acid stannous chloride 40g, zinc phosphate 50g, aluminum phosphate 2g, calcium phosphate 1g, strontium phosphate 1g, tertiary iron phosphate 2g, barium phosphate 4g amount to 100g and divide the another name sample to process according to following steps:
1. according to above-mentioned formulation ratio all phosphoric acid salt are mixed;
2. with phosphate mixt 1000-1200 ℃ of time fusing, be incubated 0.5 hour;
3. the liquid that melts is cooled off the homogeneous particle that forms disordered structure fast in water, take out drying and be finely ground to glass powder.
Product of the present invention is measured through testing laboratory of our company, and refractory temperature has the lower coefficient of expansion for 280～600 ℃, at 20～300 ℃ of averages coefficient of linear expansion 90 ± 3 * 10
-7/ ℃, 240 ± 3 ℃ of invert points, 280 ± 3 ℃ of softening temperatures.
Embodiment 2, press phosphoric acid stannous chloride 30g, zinc phosphate 60g, aluminum phosphate 2g, calcium phosphate 1g, strontium phosphate 1g, tertiary iron phosphate 2g, barium phosphate 4g amount to 100g respectively weighing process by following step:
1. according to above-mentioned formulation ratio all phosphoric acid salt are mixed;
2. with phosphate mixt 1200 ℃ of time fusings, be incubated 1 hour;
3. the liquid that melts is cooled off the homogeneous particle that forms disordered structure fast in water, take out drying and be finely ground to glass powder.
Product of the present invention detects through testing laboratory of our company: refractory temperature: 280～600 ℃, the lower coefficient of expansion is arranged, at 20～300 ℃ of averages coefficient of linear expansion 90 ± 3 * 10
-7/ ℃, 240 ± 3 ℃ of invert points, 280 ± 3 ℃ of softening temperatures.
The concrete using method of product: in resistance furnace, populated this glass powder between soda-lime glass and pottery rises to 280-600 ℃ of scope insulation outage after 10-120 minute with resistance furnace temperature, treats that temperature is cold really to below 100 ℃, opens fire door and takes out this adhesion article
Claims (5)
1. glass and ceramics adhesion lead-free glass powder, it is characterized in that by mass percent being the phosphoric acid stannous chloride of 20-50%, the 40-70% zinc phosphate, 1-5% aluminum phosphate, 0.5-2% calcium phosphate, the 0.5-1% strontium phosphate, the 1-3% tertiary iron phosphate, 2-6% barium phosphate formulated forms refractory temperature: 280～600 ℃, the lower coefficient of expansion is arranged, at 20～300 ℃ of averages coefficient of linear expansion 90 ± 3 * 10
-7/ ℃, 240 ± 3 ℃ of invert points, 280 ± 3 ℃ of softening temperatures.
2. a kind of glass according to claim 1 and ceramics adhesion lead-free glass powder, the quality proportioning that it is characterized in that its formulation optimization is: the phosphoric acid stannous chloride of 30-40%, the 50-60% zinc phosphate, the 1-5% aluminum phosphate, 0.5-2% calcium phosphate, the 0.5-1% strontium phosphate, the 1-3% tertiary iron phosphate, the 2-6% barium phosphate is formed.
3. according to the compound method of claim 1 or 2 described a kind of glass and ceramics adhesion usefulness lead-free glass powder, it is characterized in that following these steps to process:
1. according to above-mentioned formulation ratio all phosphoric acid salt are mixed;
2. with phosphate mixt 1000-1200 ℃ of time fusing, be incubated 0.5-1 hour;
3. the liquid that melts is cooled off the homogeneous particle that forms disordered structure fast in water, take out drying and be finely ground to glass powder.
4. according to the application of claim 1 or 2 described a kind of glass and ceramics adhesion with lead-free glass powder, it is characterized in that being used for inter-adhesive between soda-lime glass and the pottery, the cold-resistant thermal shocking of adhesion device, matching is good.
5. a kind of glass according to claim 4 and ceramics adhesion is characterized in that with the application of lead-free glass powder its coefficient of expansion of indication pottery will be complementary with glass powder, promptly are that its coefficient of linear expansion is identical with the glass powder coefficient of linear expansion or close.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101029472A CN101712533B (en) | 2009-12-16 | 2009-12-16 | Lead-free glass powder for glass-ceramics adhesion, preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101029472A CN101712533B (en) | 2009-12-16 | 2009-12-16 | Lead-free glass powder for glass-ceramics adhesion, preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101712533A CN101712533A (en) | 2010-05-26 |
| CN101712533B true CN101712533B (en) | 2011-12-07 |
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| CN2009101029472A Expired - Fee Related CN101712533B (en) | 2009-12-16 | 2009-12-16 | Lead-free glass powder for glass-ceramics adhesion, preparation method and application thereof |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113035975A (en) * | 2021-03-03 | 2021-06-25 | 中国科学院电工研究所 | Glass powder and preparation method thereof, conductive silver paste and preparation method and application thereof |
| CN113003940A (en) * | 2021-04-23 | 2021-06-22 | 贵州国锐鑫节能科技有限公司 | Low-melting-point low-expansion-coefficient glass powder and preparation method thereof |
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| C14 | Grant of patent or utility model | ||
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Owner name: GUIZHOU JINGYU SILICON MATERIAL CO., LTD. Free format text: FORMER OWNER: GUIYANG HUALIMEI CHEMICAL CO., LTD. Effective date: 20131114 |
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Free format text: CORRECT: ADDRESS; FROM: 550002 GUIYANG, GUIZHOU PROVINCE TO: 550008 GUIYANG, GUIZHOU PROVINCE |
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Effective date of registration: 20131114 Address after: 550008 B315 room, standard workshop auxiliary room, Jinyang science and Technology Industrial Park, Guiyang hi tech Zone, Guizhou Patentee after: Guizhou Jing Yu silicon material Co., Ltd. Address before: 550002 No. 15 middle Sha Chong Road, Guizhou, Guiyang Patentee before: Guiyang Hualimei Chemical Co., Ltd. |
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| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20111207 Termination date: 20161216 |
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| CF01 | Termination of patent right due to non-payment of annual fee |