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Low temperature lead-free glass dust and preparation method thereof

A lead-free glass powder, low temperature technology, applied in the field of lead-free glass powder, low-temperature lead-free glass powder and its preparation, can solve the problems of poor wettability, easy crystallization, high softening temperature, etc., and achieve refiring stability Good, good wetting properties, high bond strength effect

Inactive Publication Date: 2013-09-25
SHANGHAI INTELLIGENT SENSOR ELECTRONICS TECHCO
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  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the aluminum oxide sealing and electronic paste glass powder for alumina substrates have the following shortcomings: (1) After sintering, due to the mismatch with the expansion coefficient of alumina or poor wettability, the stress is too large, and it is easy to crack after long-term use. lead to deterioration of electrical performance
(2) Although some glass powders have good performance, they contain chemical elements such as lead and chromium that are harmful to humans and the environment
(3) The refiring stability of the prepared electronic paste is relatively poor
[0006] The application number is US4362656, which discloses a glass powder for ruthenium oxide-based thick-film resistor paste. This glass contains a large amount of lead. Although it has excellent performance, it does not meet environmental protection requirements.
In order to meet the requirements of energy saving and environmental protection and improve the bonding performance with the substrate, the Chinese patent application number 201210446523.x discloses a Bi 2 o 3 , ZnO, B 2 o 3 , Kaolin, TiO 2 , SiO 2 Lead-free glass powder prepared as raw material, but since the glass contains TiO 2 , resulting in easy crystallization of the glass powder during secondary sintering, and poor refiring stability
The Chinese patent application number 200710041637.5 discloses a 2 o 3 , B 2 o 3 , SiO 2 , MgO, Li 2 O is used as a raw material to prepare lead-free glass powder, which has good chemical and thermal stability, low expansion coefficient, and high mechanical properties, but due to containing part of SiO 2 resulting in a higher softening temperature

Method used

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  • Low temperature lead-free glass dust and preparation method thereof

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preparation example Construction

[0024] A kind of low-temperature lead-free glass powder of the present invention and preparation method thereof, the raw material of lead-free glass powder comprises following component and weight percentage: Bi 2 o 3 30-80%, B 2 o 3 10~60%, ZnO 0~20%, Sb 2 o 3 0~20%,Al 2 o 3 0~10%, alkali metal oxide 0~7%; the basic oxide is Li 2 O.

[0025] The preparation method of low-temperature lead-free glass powder comprises the following steps:

[0026] (1) Weigh the raw materials according to the above components, use a planetary ball mill, and use ethanol as the medium to ball mill for 30 to 60 minutes and mix them evenly, and obtain uniformly mixed oxides after drying;

[0027] (2) After the mixture is melted, pour it into deionized water to obtain glass slag, then dry it, put it into a ball mill jar and mill it in a planetary ball mill;

[0028] (3) Pass through a 300-mesh sieve after ball milling to obtain low-temperature lead-free glass powder.

Embodiment 1

[0033] According to the weight percentage of the composition in Table 1, the ingredients are mixed evenly, and the raw materials are added into the corundum crucible, and heated and melted in a silicon-molybdenum rod resistance furnace at a melting temperature of 1200 ° C and a holding time of 30 minutes.

[0034] After the glass is evenly melted, part of it is poured into a preheated stainless steel mold with a size of 55mm×6mm×6mm for molding, and then placed in a muffle furnace for annealing at 450°C, kept for 2 hours and then cooled with the furnace, using a PCY horizontal dilatometer The expansion coefficient of the test sample is shown in Table 1, and the other part is quenched in high temperature water, and ball milled to powder, and sieved through a 300-mesh sieve, and a small amount of powder is taken to test the softening temperature of the glass with a HCT-1 / 2 differential thermal analyzer, as shown in the table 1, the resulting DTA curve is shown in the attached fi...

Embodiment 2

[0036] According to the weight percentage of the composition in Table 1, the ingredients are mixed evenly, and the raw materials are added into the corundum crucible, and heated and melted in a silicon-molybdenum rod resistance furnace at a melting temperature of 1250°C and a holding time of 40 minutes.

[0037] After the glass is evenly melted, part of it is poured into a preheated stainless steel mold with a size of 55mm×6mm×6mm for molding, and then placed in a muffle furnace for annealing at 450°C, kept for 2 hours and then cooled with the furnace, using a PCY horizontal dilatometer The expansion coefficient of the test sample is shown in Table 1, and the other part is quenched in high temperature water, and ball milled to powder, and sieved through a 300-mesh sieve, and a small amount of powder is taken to test the softening temperature of the glass with a HCT-1 / 2 differential thermal analyzer, as shown in the table 1, the resulting DTA curve is shown in the attached fig...

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Abstract

The invention relates to low temperature lead-free glass dust and a preparation method thereof. The glass dust comprise the following components as raw materials by weight percent: 30-80% of Bi2O3, 10-60% of B2O3, 0-20% of ZnO, 0-20% of Sb2O3, 0-10% of Al2O3 and 0-7% of alkali metal oxide, wherein the alkali metal oxide is Li2O. The preparation method comprises the following steps: (1) weighing the raw materials in ratio, carrying out ball-milling for 30-60 minutes by taking ethyl alcohol as a medium by using a planet ball grinding mill, then blending uniformly, drying to obtain a uniformly-mixed oxide; (2) after the mixture is melted, pouring the melted mixture into deionized water to obtain glass slag, then drying, and putting the glass slag into a ball-milling pot in the planet ball grinding mill and carrying out ball-milling to obtain a product; and (3) after the ball-milling, sieving the product with a 300-mesh mesh screen to obtain the low temperature lead-free glass dust. The lead-free glass dust prepared by the preparation method disclosed by the invention is low in softening in temperature, high in bonding strength and good in refiring stability.

Description

technical field [0001] The invention relates to a lead-free glass powder, in particular discloses a low-temperature lead-free glass powder and a preparation method thereof, which are applied to alumina sealing and electronic paste using alumina as a substrate, and belong to the technical field of electronic materials. Background technique [0002] Low-melting glass refers to the softening temperature (T s ) is a type of special-purpose glass below 600°C, widely used in vacuum electronics technology, microelectronics technology, laser and infrared technology, electric light source, high-energy physics and aerospace industry, energy, automobile industry, chemical industry, industrial testing and other fields, It can realize the sealing between glass, ceramics and various metals. Lead glass has outstanding low-temperature softening properties and excellent chemical stability, and has been used as a commercial low-melting glass for many years. However, this type of glass conta...

Claims

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Application Information

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IPC IPC(8): C03C12/00
Inventor 于小军
Owner SHANGHAI INTELLIGENT SENSOR ELECTRONICS TECHCO
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