Process for producing a glass-metal connection

• US 5,004,489 A
• Filed: 02/22/1990
• Issued: 04/02/1991
• Est. Priority Date: 02/22/1989
• Status: Expired due to Fees

• Current Assignee: L'Air Liquide Societe Anonyme Pour L'Etude et L'Exploitation Des Procedes Georges Claude (L'Air Liquide SA)
• Original Assignee: L'Air Liquide Societe Anonyme Pour L'Etude et L'Exploitation Des Procedes Georges Claude (L'Air Liquide SA)
• Inventors: Rotman, Frederic, Rancon, Yannick, Queille, Philippe, Olivier, Michel
• Primary Examiner(s): Lindsay, Robert L.
• Application Number:
  US07/483,177
• Time in Patent Office: 404 Days
• Field of Search: 65/32.2, 65/59.23, 65/59.1, 148/278
• US Class Current: 65/32.2
• CPC Class Codes: C01B 5/00 Water
• CPC Class Codes: C03C 27/02 by fusing glass directly to metal
• CPC Class Codes: C03C 27/046 of metals, metal oxides or metal salts only

Abstract

The invention concerns glass-metal sealing comprising effecting on a metallic piece, in particular an alloy based on iron and nickel or iron, nickel and cobalt, first of all a decarburization under an atmosphere, at a temperature of between 950° C. and 1,150° C., formed by hydrogen (10 to 99%), water vapor (1 to 8%), with a ratio hydrogen/water vapor higher than five, the possible remainder being nitrogen, then an oxidation under an atmosphere formed by an inert vector gas such as nitrogen, either at a temperature of 600° C. to 800° C. and with a water vapor content of 8% to 2%; or at a temperature of 900° C. to 1,100° C. and with a water vapor content of 4% to 0.5%; then establishing the connection. The gas mixture for a treatment atmosphere is obtained by mixing nitrogen and hydrogen conducted through pipes (13, 14), to which oxygen is added through a pipe (15) upstream of a catalytic chamber (11) permitting the elimination of the oxygen and the production of a content of water vapor.

Claims

1. A method of bonding together a glass part and a metal alloy part, said metal alloy part comprising iron and nickel, comprising the following successive steps:

subjecting said glass part and said metal alloy part to an oxidation phase under a first atmosphere which is substantially inert and contains from 2 to 8% of water vapor and less than 1% of hydrogen at a first temperature of from 600°

to 800°

C.;

bonding said glass part and said metal alloy part together under a second atmosphere at a second temperature greater than the first temperature,

wherein at least said first atmosphere is obtained by a catalytic reaction of a mixture of hydrogen and oxygen in proportions selected so as to obtain the desired content of water vapor and hydrogen.

2. The method according to claim 1 further including the preliminary step of subjecting said glass part and said metal alloy part to a decarburizing phase under a third atmosphere containing from 10 to 99% hydrogen, from 1 to 8% of water vapor, and a ratio of hydrogen/water vapor of not less than five;

wherein said third atmosphere is obtained by catalytic reaction of a mixture of hydrogen and oxygen in proportions selected so as to obtain the desired content of water vapor and hydrogen.

3. The method according to claim 1 wherein the ratio of water vapor to hydrogen is not less than 3.

6. The method of claim 1 wherein said catalytic reaction is achieved at ambient temperature with a catalyst having an energetic autonomy, said catalyst containing palladium on an aluminum substrate, the final content of oxygen in the resulting processing atmosphere being less than 10 vpm.

7. The method of claim 2, wherein said catalytic reaction is sequentially conducted in a single reactor for producing successively at least said first and third atmospheres.

8. A method for bonding together a glass part and a metal alloy part, said metal alloy part comprising iron and nickel, which comprises the following successive steps:

subjecting said glass part and said metal alloy part to an oxidation phase under a first atmosphere is substantially inert and contains from 0.5 to 4% of water vapor and less than 1% hydrogen, at a first temperature of from 900°

to 1100°

C.;

bonding said glass part to said metal alloy part under a second atmosphere at a second temperature which is greater than said first temperature,

wherein at least said first atmosphere is obtained by catalytic reaction of a mixture of hydrogen and oxygen in proportions selected so as to obtain the desired content of water vapor and hydrogen.

4. The method of claim 10 wherein said first atmosphere contains nitrogen, and the gaseous mixture subject to catalytic reaction contains nitrogen, hydrogen, and oxygen.

5. The method of claim 4 wherein said oxygen in the gaseous mixture is initially present in the nitrogen mixed with hydrogen, said nitrogen being raw nitrogen obtained by separation of air by adsorption or permeation.

9. The method of claim 8 further including the preliminary step of subjecting said glass part and said metal alloy part to a decarburizing phase under a third atmosphere containing from 10 to 99% of hydrogen, from 1 to 8% of water vapor, and a ratio of hydrogen/water vapor of not less than five, wherein said third atmosphere is obtained by catalytic reaction of a mixture of hydrogen and oxygen in proportions selected so as to obtain the desired content of water vapor and hydrogen.

10. The method of claim 8 wherein the ratio of water vapor to hydrogen is not less than 3.

11. The method of claim 8 wherein said first atmosphere contains nitrogen, and the gaseous mixture subject to catalytic reaction contains nitrogen, hydrogen, and oxygen.