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Lead-free superfine glass powder and synthetic method thereof

A technology of ultra-fine glass powder and synthesis method, which is applied in the field of electronic materials, can solve the problems of difficult uniformity of melt, high energy consumption of glass, and difficult refinement of powder, etc., and achieve large linear expansion coefficient and softening temperature range, chemical composition uniform effect

Inactive Publication Date: 2013-10-02
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these patents all use the melting-quenching method to prepare glass frit, and then crush it into powder by ball milling. Undoubtedly, the melting and quenching method consumes a lot of energy to synthesize glass, and the powder is difficult to refine. The particle size is generally 1-10 μm Even in the coarser range, the sintering activity is low, and there are disadvantages such as component volatilization and local difficulty in uniformity of the melt when melting at high temperature.

Method used

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  • Lead-free superfine glass powder and synthetic method thereof
  • Lead-free superfine glass powder and synthetic method thereof

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Select the glass oxide component precursor, bismuth nitrate, tetraethyl orthosilicate, boric acid, zinc acetate or zinc nitrate, aluminum isopropoxide or aluminum nitrate as the Bi 2 o 3 , SiO 2 , B 2 o 3 , ZnO, Al 2 o 3 Precursors, using deionized water and absolute ethanol, citric acid, and nitric acid as solvents, complexing agents, and catalysts;

[0033] (2) According to the glass composition oxide Bi 2 o 3, SiO 2 , B 2 o 3 , ZnO, Al 2 o 3 The weight percentages of 55%, 25%, 10%, 7%, and 3% are converted to the weight of the precursor.

[0034] (3) Weigh the precursor, prepare ethyl orthosilicate, absolute ethanol, A mixed solution of deionized water was placed in a constant temperature water bath at 55°C, nitric acid was added dropwise as a catalyst, the pH was controlled to be 2.5, and an electric stirrer was used to fully stir it to make it hydrolyze for 35 minutes.

[0035] (4) According to the weight ratio of bismuth nitrate: dilute nitric ac...

Embodiment 2

[0041] (1) Select the glass oxide component precursor, bismuth nitrate, tetraethyl orthosilicate, boric acid, zinc acetate or zinc nitrate, aluminum isopropoxide or aluminum nitrate as the Bi 2 o 3 , SiO 2 , B 2 o 3 , ZnO, Al 2 o 3 Precursors, using deionized water and absolute ethanol, citric acid, and nitric acid as solvents, complexing agents, and catalysts;

[0042] (2) According to the glass composition oxide Bi 2 o 3 , SiO 2 , B 2 o 3 , ZnO, Al 2 o 3 The weight percentages of 50%, 30%, 10%, 8%, and 2% are converted to the weight of the precursor.

[0043] (3) Weigh the precursor, prepare ethyl orthosilicate, absolute ethanol, The mixed solution of deionized water is placed in a constant temperature water bath at 50°C, nitric acid is added dropwise as a catalyst, the pH is controlled to be 3, and an electric stirrer is used to fully stir it to make it hydrolyze for 30 minutes.

[0044] (4) According to the weight ratio of bismuth nitrate:dilute nitric acid=1...

Embodiment 3

[0048] (1) Select the glass oxide component precursor, with bismuth nitrate, ethyl orthosilicate, boric acid, zinc acetate or zinc nitrate, aluminum isopropoxide or aluminum nitrate as Bi respectively 2 o 3 , SiO 2 , B 2 o 3 , ZnO, Al 2 o 3 Precursors, using deionized water and absolute ethanol, citric acid, and nitric acid as solvents, complexing agents, and catalysts;

[0049] (2) According to the glass composition oxide Bi 2 o 3 , SiO 2 , B 2 o 3 , ZnO, Al 2 o 3 The weight percentages of 45%, 25%, 25%, 4%, and 1% are converted to the weight of the precursor.

[0050] (3) Weigh the precursor, prepare ethyl orthosilicate, absolute ethanol, The mixed solution of deionized water is placed in a constant temperature water bath at 55°C, nitric acid is added dropwise as a catalyst, the pH is controlled to be 3.2, and an electric stirrer is used to fully stir it to make it hydrolyze for 35 minutes.

[0051] (4) According to the weight ratio of bismuth nitrate:dilute ...

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Abstract

The invention discloses lead-free superfine glass powder and a synthetic method thereof. The lead-free superfine glass powder comprises the following components in percentage by weight: 35-55% of Bi2O3, 5-30% of SiO2, 5-25% of B2O3, 2-10% of ZnO and 1-5% of Al2O3 and is synthesized by respectively taking bismuth nitrate, ethyl orthosilicate, boracic acid, zinc acetate or zinc nitrate and aluminum isopropoxide or aluminum nitrate as the precursors of Bi2O3, SiO2, B2O3, ZnO and Al2O3, respectively taking deionized water, anhydrous ethanol, citric acid and nitric acid as a solvent, a complexing agent and a catalyst and adopting a sol-gel method. The lead-free superfine glass powder disclosed by the invention has the advantages of no lead, environment friendliness, high chemical stability, small powder particle size and high sintering activity, can be used as the inorganic binder of various ceramics and glass substrates and also be used as an inorganic binder phase and added to electronic paste, is easy to improve the printing and sintering property of the electronic paste through a screen mesh due to small particle size and has a wide application prospect in the fields of electronics and electrical appliances.

Description

technical field [0001] The invention belongs to the field of electronic materials, in particular to a lead-free ultrafine glass powder and a synthesis method thereof. Background technique [0002] In recent years, with the development of microelectronics technology, electronic display, and optoelectronic technology, electronic glass, as the basic material in the electronic field, is widely used in the sealing between ceramics, metals and glass to achieve vacuum sealing and ensure the stability of electronic components and reliability purposes; at the same time, electronic glass powder can also be mixed with metal powder and organic solvents to make electronic paste, which is widely used in the production of conductive electrodes on silicon solar cells, integrated circuits, automobiles, and electric heaters, as a sintering flux , has achieved the purpose of promoting metallurgical bonding between metal powder and substrate materials such as silicon wafers. [0003] The tra...

Claims

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Application Information

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IPC IPC(8): C03C12/00
Inventor 袁鸽成刘华骆志捷李倩邓南林
Owner GUANGDONG UNIV OF TECH
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