Devitrification type lead-free low-temperature sealing glass as well as preparation method and application method thereof

A technology for sealing glass and devitrification type, which is applied in the field of devitrification type lead-free low temperature sealing glass, which can solve the problems of not completely solving environmental protection problems, not well satisfied with low temperature sealing and rapid sintering, etc., and achieves low cost and high price. Inexpensive, lower softening temperature effect

Active Publication Date: 2014-03-12
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Patent application 201310259302.6 discloses a low-temperature lead-free glass powder and its preparation method, but another toxic substance Sb is introduced into the system, which still does not completely solve the environmental protection problem
And patent application 201210366375.0 also discloses lead-free glass material and preparation method thereof, through P 2 o 5 、K 2 O, Na 2 O, ZrO 2 、TiO 2 The composition design of the raw materials and other materials avoids environmental pollution, but the softening temperature range of the glass is 500~600°C, which still does not meet the requirements of low temperature sealing, especially the low temperature and rapid sintering of electronic components.

Method used

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  • Devitrification type lead-free low-temperature sealing glass as well as preparation method and application method thereof
  • Devitrification type lead-free low-temperature sealing glass as well as preparation method and application method thereof
  • Devitrification type lead-free low-temperature sealing glass as well as preparation method and application method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: Preparation and sealing of materials

[0032] According to the ratio of each component in Table 1, weigh a certain amount of analytically pure raw materials (CaO, SrO, SiO 2 、Al 2 o 3 , B 2 o 3 、 Bi 2 o 3 ), 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 1300°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 at the part to be sealed, heat up at a rate of 2°C / min in an electric furnace,...

Embodiment 2

[0033] Embodiment 2: Preparation and sealing of materials

[0034] According to the ratio of each component in Table 1, weigh a certain amount of analytically pure raw materials (CaO, SrO, SiO 2 、Al 2 o 3 , B 2 o 3 、 Bi 2 o 3 ), 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 at 3°C / min to 1280°C, 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, raising the temperature in an electric...

Embodiment 3

[0035] Embodiment 3: Preparation and sealing of materials

[0036] According to the ratio of each component in Table 1, weigh a certain amount of analytically pure raw materials (CaO, SrO, SiO 2 、Al 2 o 3 , B 2 o 3 、 Bi 2 o 3 ), 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 at 3°C / min to 1250°C, 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 Forming, 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 in a...

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Abstract

The invention discloses devitrification type lead-free low-temperature sealing glass as well as a preparation method and application method thereof. The devitrification type lead-free low-temperature sealing glass includes the following raw materials with the molar ratio of (0-10):(0-5):(20-40):(30-60):(5-30): B2O3, Al2O3, SiO2, MO (one or a mixture of MgO, CaO, SrO and BaO), and Bi2O3. Through the synergy between the Bi2O3 and the B2O3, the softening temperature range of the glass is reduced to 370-420 DEG C, and the coefficient of thermal expansion within the range of 150-300 DEG C reaches 1.2 minus 1.4*10<-5>/K, so that the sealing performance of the glass is remarkably improved; meanwhile, the sealing glass has good stability while being placed in hot water with the temperature of 80 DEG C for 1,000 hours, so that the sealing glass is applicable to electronic material and other low-temperature sealing fields. The raw materials for preparation of the sealing glass are simple and easy to get, the process is stable, simple and feasible, the cost is low, and the requirements for practicality and industrialization are met.

Description

technical field [0001] The invention belongs to the field of sealing glass, in particular to a crystallization type lead-free low-temperature sealing glass and its preparation and use method. 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 affects the actual performance of the battery. Sealing glass can also be used for mutual sealing between glass, ceramics, metals, and semiconductors. However, currently domestic and foreign research generally uses sealing materials containing Pb, which will pollute the environment. Since Bi and Pb are adjacent in the periodic table of elements and have similar ph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C8/24
Inventor 张腾陈斌邹培超方丽花
Owner FUZHOU UNIV
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