Sn-containing low-temperature seal glass and preparing and using methods thereof

Abstract

The invention discloses Sn-containing low-temperature seal glass and preparing and using methods thereof. The Sn-containing low-temperature seal glass is composed of B2O3, Bi2O3, ZnO and SnO2 according to a molar ratio of 10-50:20-40:5-30:0-30. Softening temperature of the glass is lowered through synergism of high-concentration Bi2O3 and B2O3 to realize low-temperature seal; Sn2+ in a glass network prepared through melting-quenching is converted into Sn4+ in the process of heating, conversion from Bi3+ in the glass to Bi5+ is stopped, and refractivity of the glass is stabilized; Sn can further lower the softening temperature of the seal glass and can adjust expansion coefficient of the glass, so that seal performance of the seal glass is improved remarkably; the glass is suitable for photoelectric materials and other low-temperature precise seal fields. The raw materials for preparation are simple and easy to obtain, the preparation method is stable, low in cost and simple and easy to implement, and practical and industrial conditions are met.

Description

technical field

[0001] The invention belongs to the field of low-temperature precision packaging glass, and in particular relates to a low-temperature sealing glass containing Sn and its preparation and use methods. Background technique

[0002] Low-temperature sealing glass (melting temperature and sealing temperature <600°C), due to its good heat resistance and chemical stability, high mechanical strength, is widely used in electronic paste, electric vacuum and microelectronics technology, energy, aerospace, In many fields such as automobiles, such as in solid oxide fuel cells (SOFC), the performance of the sealing material directly leads to the actual performance of the battery; in the application of electronic materials, the stability of the sealing glass also affects the LED The light decay rate has a great influence. At the same time, sealing glass can also be used for mutual sealing between glass, ceramics, metals and semiconductors. In view of the environmental ...

Examples

Embodiment 1

[0030] Embodiment 1: Preparation and sealing of materials

[0031] According to the proportioning of each component of embodiment 1 in table 1, take a certain amount of analytically pure raw material (B 2 o 3 、 Bi 2 o 3 , ZnO, SnO 2 ), use a planetary ball mill for 24 hours to mix evenly; then put the powder into a platinum crucible, place it in the air atmosphere of a box-type resistance furnace, heat it to 1000°C at 3°C / min, and keep it warm for 1 hour; then, take out the crucible, Pour the melt into deionized water for rapid cooling, and dry to obtain fragments of glass melt; grind and pass through a 100-mesh sieve to obtain glass powder. Mix glass powder with polyvinyl alcohol, fish oil, ethanol and toluene (80%, 2%, 1%, 10%, 7% by weight) to form a slurry, and disperse evenly in a ball mill; tape casting, natural Dry, then cut into the embryo body of the desired shape; place the embryo body on the part to be sealed, heat up in an electric furnace at a rate of 2°C / min...

Embodiment 2

[0032] Embodiment 2: Preparation and sealing of materials

[0033] According to the proportioning of each component of embodiment 2 in table 1, take a certain amount of analytically pure raw material (B 2 o 3 、 Bi 2 o 3 , ZnO, SnO 2 ), and mixed evenly with a planetary ball mill for 24 hours; then put the powder into a platinum crucible, place it in the air atmosphere of a box-type resistance furnace, heat it to 980°C at 3°C / min, and keep it warm for 1 hour; then, take out the crucible, Pour the melt into deionized water for rapid cooling, and dry to obtain fragments of glass melt; grind and pass through a 100-mesh sieve to obtain glass powder. Mix glass powder with methylcellulose, polyvinyl alcohol, n-butanol and acetone (82%, 2%, 2%, 8%, 6% by weight) to form a slurry, and disperse evenly in a ball mill; Stretching, drying naturally, and then cutting the embryo body into the desired shape; placing the embryo body on the part to be sealed, heating it in an electric furn...

Embodiment 3

[0034] Embodiment 3: Preparation and sealing of materials

[0035] According to the proportioning of each component of embodiment 3 in table 1, take a certain amount of analytically pure raw material (B 2 o 3 、 Bi 2 o 3 , ZnO, SnO 2 ), use a planetary ball mill for 24 hours to mix evenly; then put the powder into a platinum crucible, place it in the air atmosphere of a box-type resistance furnace, heat it to 950°C at 3°C / min, and keep it warm for 1 hour; then, take out the crucible, Pour the melt into deionized water for rapid cooling, and dry to obtain fragments of glass melt; grind and pass through a 100-mesh sieve to obtain glass powder. Mix glass powder with epoxy resin, polyacrylamide, isopropanol and toluene (84%, 1.5%, 0.5%, 9%, 5% by weight) to form a slurry, and disperse evenly in a ball mill; casting Shaping, drying naturally, and then cutting into the embryo body of the desired shape; place the embryo body on the part to be sealed, heat up at a rate of 2°C / min ...

technical field

[0001] The invention belongs to the field of low-temperature precision packaging glass, and in particular relates to a low-temperature sealing glass containing Sn and its preparation and use methods. Background technique

[0002] Low-temperature sealing glass (melting temperature and sealing temperature <600°C), due to its good heat resistance and chemical stability, high mechanical strength, is widely used in electronic paste, electric vacuum and microelectronics technology, energy, aerospace, In many fields such as automobiles, such as in solid oxide fuel cells (SOFC), the performance of the sealing material directly leads to the actual performance of the battery; in the application of electronic materials, the stability of the sealing glass also affects the LED The light decay rate has a great influence. At the same time, sealing glass can also be used for mutual sealing between glass, ceramics, metals and semiconductors. In view of the environmental ...

Examples

Embodiment 1

[0030] Embodiment 1: Preparation and sealing of materials

[0031] According to the proportioning of each component of embodiment 1 in table 1, take a certain amount of analytically pure raw material (B 2 o 3 、 Bi 2 o 3 , ZnO, SnO 2 ), use a planetary ball mill for 24 hours to mix evenly; then put the powder into a platinum crucible, place it in the air atmosphere of a box-type resistance furnace, heat it to 1000°C at 3°C / min, and keep it warm for 1 hour; then, take out the crucible, Pour the melt into deionized water for rapid cooling, and dry to obtain fragments of glass melt; grind and pass through a 100-mesh sieve to obtain glass powder. Mix glass powder with polyvinyl alcohol, fish oil, ethanol and toluene (80%, 2%, 1%, 10%, 7% by weight) to form a slurry, and disperse evenly in a ball mill; tape casting, natural Dry, then cut into the embryo body of the desired shape; place the embryo body on the part to be sealed, heat up in an electric furnace at a rate of 2°C / min...

Embodiment 2

[0032] Embodiment 2: Preparation and sealing of materials

[0033] According to the proportioning of each component of embodiment 2 in table 1, take a certain amount of analytically pure raw material (B 2 o 3 、 Bi 2 o 3 , ZnO, SnO 2 ), and mixed evenly with a planetary ball mill for 24 hours; then put the powder into a platinum crucible, place it in the air atmosphere of a box-type resistance furnace, heat it to 980°C at 3°C / min, and keep it warm for 1 hour; then, take out the crucible, Pour the melt into deionized water for rapid cooling, and dry to obtain fragments of glass melt; grind and pass through a 100-mesh sieve to obtain glass powder. Mix glass powder with methylcellulose, polyvinyl alcohol, n-butanol and acetone (82%, 2%, 2%, 8%, 6% by weight) to form a slurry, and disperse evenly in a ball mill; Stretching, drying naturally, and then cutting the embryo body into the desired shape; placing the embryo body on the part to be sealed, heating it in an electric furn...

Embodiment 3

[0034] Embodiment 3: Preparation and sealing of materials

[0035] According to the proportioning of each component of embodiment 3 in table 1, take a certain amount of analytically pure raw material (B 2 o 3 、 Bi 2 o 3 , ZnO, SnO 2 ), use a planetary ball mill for 24 hours to mix evenly; then put the powder into a platinum crucible, place it in the air atmosphere of a box-type resistance furnace, heat it to 950°C at 3°C / min, and keep it warm for 1 hour; then, take out the crucible, Pour the melt into deionized water for rapid cooling, and dry to obtain fragments of glass melt; grind and pass through a 100-mesh sieve to obtain glass powder. Mix glass powder with epoxy resin, polyacrylamide, isopropanol and toluene (84%, 1.5%, 0.5%, 9%, 5% by weight) to form a slurry, and disperse evenly in a ball mill; casting Shaping, drying naturally, and then cutting into the embryo body of the desired shape; place the embryo body on the part to be sealed, heat up at a rate of 2°C / min ...

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