CN101712531B - Lead-free glass powder for electronic component connection and preparation method thereof - Google Patents
Lead-free glass powder for electronic component connection and preparation method thereof Download PDFInfo
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- CN101712531B CN101712531B CN2009101029453A CN200910102945A CN101712531B CN 101712531 B CN101712531 B CN 101712531B CN 2009101029453 A CN2009101029453 A CN 2009101029453A CN 200910102945 A CN200910102945 A CN 200910102945A CN 101712531 B CN101712531 B CN 101712531B
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Abstract
The invention provides lead-free glass powder for electronic component connection and a preparation method thereof, belonging to the technical fields of chemical industry and electrons. The lead-free glass powder is prepared by processing the following components by mass percentage: 40-70% of stannous pyrophosphate, 0.15-0.5% of silica, 2-10% of aluminum oxide, 10-15% of copper oxide, 10-20% of calcium oxide, 5-10% of strontium oxide, 1-5% of vanadium pentoxide and 0.5-2% of barium oxide. The fire-retarding temperature of the glass powder is 320-550 DEG C, the inversion temperature thereof is 240+/-3 DEG C, and the softening temperature thereof is 300+/-3 DEG C; and the glass powder has a lower expansion coefficient, and the average linear expansion coefficient is 86+/-3*10<-7>/DEG C under the temperature of 20-300 DEG C, thus being applicable to connection between glass, ceramics, metals and semiconductors.
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 lead-free glass powder that electron device connects that is used for, performance is suitable with low melting point flint glass powder, can replace low melting point flint glass powder and be applied in glass, pottery, being connected between metal and the semi-conductor.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 being connected between glass, pottery, metal and the semi-conductor; 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 lead-free glass powder that is used for the electron device connection of the present invention, be to be the 40%-70% stannous pyrophosphate by mass percent, the silicon-dioxide of 0.15%-0.5%, 2%-10% aluminium sesquioxide, the 10%-15% cupric oxide, the 10%-20% calcium oxide, 5%-10% strontium oxide, 1%-5% Vanadium Pentoxide in FLAKES, 0.5%-2% barium oxide formulated forms, refractory temperature: 320～550 ℃, the lower coefficient of expansion is arranged, at 20～300 ℃ of averages coefficient of linear expansion 86 ± 3 * 10
-7/ ℃, 240 ± 3 ℃ of invert points, 300 ± 3 ℃ of softening temperatures.
The quality proportioning of above-mentioned formulation optimization is: 40%-60% stannous pyrophosphate, the silicon-dioxide of 0.15%-0.5%, 5%-10% aluminium sesquioxide, the 10%-15% cupric oxide, 15%-20% calcium oxide, 5%-10% strontium oxide, the 1%-5% Vanadium Pentoxide in FLAKES, 0.5%-2% barium oxide is formed.
A kind of compound method that is used for the lead-free glass powder of electron device connection of the present invention is characterized in that following these steps to process:
1. prepare compound, in proportion that stannous pyrophosphate, silicon-dioxide, aluminium sesquioxide, cupric oxide, calcium oxide, strontium oxide, Vanadium Pentoxide in FLAKES, barium oxide thorough mixing is even, make compound;
2. compound is melted at 1000～1200 ℃ of resistance furnace internal heating, be incubated 0.5 hour;
3. the liquid that melts is cooled off and forms the homogeneous particle of disordered structure fast in water, make powder after the taking-up drying and get product.
The present invention is a kind of to be used for the lead-free glass powder that electron device connects, and is meant to be suitable for being connected between glass, pottery, metal and the semi-conductor.
The glass of above-mentioned indication, pottery, metal, semi-conductor, its coefficient of expansion 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: this glass powder chemical stability 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 320-550 ℃, 20-300 ℃ of average coefficient of linear expansion 86 ± 3X 10
-7/ ℃, 240 ± 3 ℃ of transition temperatures, 300 ± 3 ℃ of softening temperatures are suitable for being connected between glass, pottery, metal and the semi-conductor, the cold-resistant thermal shocking of the device after the connection, and matching is good.
Glass powder of the present invention does not contain noble metal, and raw materials cost is low, and operating procedure is simple, realizes suitability for industrialized production easily, and no poisonous and harmful element does not constitute pollution to environment.
Embodiment: embodiment 1, press stannous pyrophosphate 48, silicon-dioxide 0.5g, aluminium sesquioxide 8g, cupric oxide 13g, calcium oxide 18g, strontium oxide 8g, Vanadium Pentoxide in FLAKES 3.5g, barium oxide 1g amount to that 100g divides the another name sample and by following step processing:
1. prepare compound, in proportion that stannous pyrophosphate, silicon-dioxide, alchlor, cupric oxide, calcium oxide, strontium oxide, Vanadium Pentoxide in FLAKES, barium oxide thorough mixing is even, make compound;
2. compound is melted at 1000 ℃ of resistance furnace internal heating, be incubated 0.5 hour;
3. the liquid that melts is cooled off and forms the homogeneous particle of disordered structure fast in water, make powder after the taking-up drying and get product.
Product of the present invention detects through testing laboratory of our company, and this glass powder chemical stability 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 320-550 ℃, 20-300 ℃ of average coefficient of linear expansion 86 ± 3X 10
-7/ ℃, 240 ± 3 ℃ of transition temperatures, 300 ± 3 ℃ of softening temperatures are suitable for being connected between glass, pottery, metal and the semi-conductor, the cold-resistant thermal shocking of the device after the connection, and matching is good.
Embodiment 2, press stannous pyrophosphate 54g, silicon-dioxide 0.5g, aluminium sesquioxide 6g, cupric oxide 12g, calcium oxide 15g, strontium oxide 8g, Vanadium Pentoxide in FLAKES 3.5g, barium oxide 1g amount to that 100g divides the another name sample and by following step processing:
1. prepare compound, in proportion that stannous pyrophosphate, silicon-dioxide, alchlor, cupric oxide, calcium oxide, strontium oxide, Vanadium Pentoxide in FLAKES, barium oxide thorough mixing is even, make compound;
2. compound is melted at 1100 ℃ of resistance furnace internal heating, be incubated 0.5 hour;
3. the liquid that melts is cooled off and forms the homogeneous particle of disordered structure fast in water, make powder after the taking-up drying and get product.
This glass powder chemical stability 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 320-550 ℃, 20-300 ℃ of average coefficient of linear expansion 86 ± 3X10
-7/ ℃, 240 ± 3 ℃ of transition temperatures, 300 ± 3 ℃ of softening temperatures are suitable for being connected between glass, pottery, metal and the semi-conductor, the cold-resistant thermal shocking of the device after the connection, and matching is good.
Concrete using method: in resistance furnace, populated this glass powder between glass, pottery, metal and semi-conductor, resistance furnace temperature is risen to 320-550 ℃ of scope insulation outage after 10-120 minute, treat that temperature is cold really to below 100 ℃, open fire door and take out this adhesion article.
Claims (4)
1. one kind is used for the lead-free glass powder that electron device connects, it is characterized in that it is the 40%-70% stannous pyrophosphate by mass percent, the silicon-dioxide of 0.15%-0.5%, the 2%-10% aluminium sesquioxide, the 10%-15% cupric oxide, 10%-20% calcium oxide, 5%-10% strontium oxide, the 1%-5% Vanadium Pentoxide in FLAKES, 0.5%-2% barium oxide formulated forms refractory temperature: 320～550 ℃, and at 20～300 ℃ of averages coefficient of linear expansion (86 ± 3) * 10
-7/ ℃, 240 ± 3 ℃ of invert points, 300 ± 3 ℃ of softening temperatures.
2. a kind of lead-free glass powder that electron device connects that is used for according to claim 1, the quality proportioning that it is characterized in that its formulation optimization is: the 40%-60% stannous pyrophosphate, the silicon-dioxide of 0.15%-0.5%, the 5%-10% aluminium sesquioxide, the 10%-15% cupric oxide, 15%-20% calcium oxide, 5%-10% strontium oxide, the 1%-5% Vanadium Pentoxide in FLAKES, 0.5%-2% barium oxide is formed.
3. according to claim 1 or 2 described a kind of compound methods that are used for the lead-free glass powder of electron device connection, it is characterized in that following these steps to process:
1. prepare compound, in proportion that stannous pyrophosphate, silicon-dioxide, aluminium sesquioxide, cupric oxide, calcium oxide, strontium oxide, Vanadium Pentoxide in FLAKES, barium oxide thorough mixing is even, make compound;
2. compound is melted at 1000～1200 ℃ of resistance furnace internal heating, be incubated 0.5 hour;
3. the liquid that melts is cooled off and forms the homogeneous particle of disordered structure fast in water, make powder after the taking-up drying and get product.
4. according to claim 1 or 2 described a kind of application that are used for the lead-free glass powder of electron device connection, it is characterized in that referring to being suitable for being connected between glass, pottery, metal and the semi-conductor, the glass of indication, pottery, semi-conductor, metal, its coefficient of expansion will be complementary with above-mentioned glass powder, promptly is that its coefficient of linear expansion is identical or close with above-mentioned glass powder coefficient of linear expansion.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101029453A CN101712531B (en) | 2009-12-16 | 2009-12-16 | Lead-free glass powder for electronic component connection and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101029453A CN101712531B (en) | 2009-12-16 | 2009-12-16 | Lead-free glass powder for electronic component connection and preparation method thereof |
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| CN101712531A CN101712531A (en) | 2010-05-26 |
| CN101712531B true CN101712531B (en) | 2011-09-28 |
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| CN109052965B (en) * | 2018-09-07 | 2021-12-24 | 苏州融睿电子科技有限公司 | Combination, mixture, sealing glass and manufacturing method thereof |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1428304A (en) * | 2001-12-25 | 2003-07-09 | 日本电气硝子株式会社 | Low temp. sealing lead-containingless tin phosphate series glass and composite material using the same |
| CN101522585A (en) * | 2006-10-06 | 2009-09-02 | 康宁股份有限公司 | Durable tungsten-doped tin-fluorophosphate glasses |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1428304A (en) * | 2001-12-25 | 2003-07-09 | 日本电气硝子株式会社 | Low temp. sealing lead-containingless tin phosphate series glass and composite material using the same |
| CN101522585A (en) * | 2006-10-06 | 2009-09-02 | 康宁股份有限公司 | Durable tungsten-doped tin-fluorophosphate glasses |
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| CN101712531A (en) | 2010-05-26 |
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