Process for joining alumina ceramic bodies

• US 5,954,900 A
• Filed: 09/23/1997
• Issued: 09/21/1999
• Est. Priority Date: 10/04/1996
• Status: Expired due to Term

• Current Assignee: Envec Mess-Und Regeltechnik GmbH + Company
• Original Assignee: Envec Mess-Und Regeltechnik GmbH + Company
• Inventors: Voigtsberger, Barbel, Hegner, Frank, Rossberg, Andreas, Ludwig, Henry, Voigt, Ingolf, Schmidt, Elke Maria
• Primary Examiner(s): Mayes, Curtis
• Application Number:
  US08/935,417
• Time in Patent Office: 728 Days
• Field of Search: 156/89.11, 156/89.12, 156/306.6, 73/780, 361/283.3, 361/283.4
• US Class Current: 156/89.11
• CPC Class Codes: C04B 2235/656 characterised by specific heating conditions during heat treatment
• CPC Class Codes: C04B 2237/064 based on alumina or aluminates
• CPC Class Codes: C04B 2237/343 Alumina or aluminates
• CPC Class Codes: C04B 35/645 Pressure sintering
• CPC Class Codes: C04B 37/005 consisting of glass or ceramic material
• CPC Class Codes: G01L 9/0075 using a ceramic diaphragm, e.g. alumina, fused quartz, glass

Abstract

This process serves to form a long-time-vacuum-tight, high-strength, and corrosion-resistant joint, by means of a joining material, between a first body and a second body each made of sintered, polycrystalline alumina ceramic with a purity greater than 92 wt. % or of sapphire. The joining material is interposed in the form of a paste, a foil, or a slip between the first body and the second body. The joining material has been made from 1) an agglomerate-free, highly disperse, high-purity α-alumina powder with particles of as high a degree of calcination as possible and of a size not exceeding 100 nm (=10^-7 m), 2) an anorganic oxidic powder of an auxiliary sintering agent with particles of approximately the same size as the particle size of the α-alumina powder, 3) an organic vehicle which is dissolved or suspended in an organic or aqueous solvant and in which the particles of the respective powder are distributed as evenly as possible. Instead of the anorganic oxidic powder of an auxiliary sintering agent an anorganic oxidic auxiliary sintering agent produced chemically as envelopes around or attachment to the particles of the α-alumina powder can be used, the total α-alumina and auxiliary-sintering-agent content of the paste, the foil, or the slip ranging between 50% and 70%. After interposing the joining material the bodies are heated to a temperature of not more than 1,300° C. and then allowing them to cool down.

Claims

1. A process for forming a long-time-vacuum-tight, high-strength, and corrosion-resistant joint, by means of a joining material, between a first body and a second body each made of sintered, polycrystalline alumina ceramic with a purity greater than 92 wt. % or of sapphire, said process comprising steps of:

interposing the joining material in the form of a paste, a foil, or a slip between the first body and the second body,

the joining material having been made from

an agglomerate-free, high-purity α

-alumina powder with particles of a size not exceeding 100 nm (=10^-7 m),

an anorganic oxidic powder of an auxiliary sintering agent with particles of a size not exceeding 100 nm, and an organic vehicle which is dissolved or suspended in an organic or aqueous solvant and in which the particles of the respective powder are substantially evenly distributed,

with the total α

-alumina and auxiliary-sintering-agent content of the paste, the foil, or the slip ranging between 50% and 70%,

or with the joining material having been made from

an agglomerate-free, high-purity α

-alumina powder with particles of a size not exceeding 100 nm (=10^-7 m),

an anorganic oxidic auxiliary sintering agent produced chemically as envelopes around or attachment to the particles of the α

-alumina powder, and

an organic vehicle dissolved or suspended in an organic or aqueous solvant,

with the total α

-alumina and auxiliary-sintering-agent content of the paste, the foil, or the slip ranging between 50% and 70%; and

beating the bodies to a temperature of not more than 1,300°

C. and then allowing them to cool down,

with the alumina content of the joint after cooling being at least 95 wt. % and the auxiliary-sintering-agent content after cooling being not more than 5 wt. %.

2. A process as claimed in claim 1 wherein the total α

-alumina and auxiliary sintering agent is comprised of at least 99.9 wt. % α

-alumina.

3. A process as claimed in claim 2 wherein, in addition to the temperature, a pressure acts on the bodies.

4. A process as claimed in claim 1 wherein, in addition to the temperature, a pressure acts on the bodies.

5. A process as claimed in claim 1 wherein, the particles of the anorganic oxidic powder of the auxiliary sintering agent are the same size as the particles of the α

-alumina powder.

6. A process for forming a joint, by means of a joining material, in a ceramic absolute-pressure or differential-pressure sensor having a substrate and a diaphragm the substrate and diaphragm each made of sintered, polycrystalline alumina ceramic with a purity greater than 92 wt. % or of sapphire, the diaphragm being connected to the substrate with the joining material near its edge so as to form a long-time-vacuum-tight, high-strength, corrosion-resistant joint and an internal chamber, the process comprising the steps of:

interposing the joining material in the form of a paste, a foil, or a slip between the substrate and the diaphragm, the joining material being made from

an agglomerate-free, high-purity α

-alumina powder with particles of a size not exceeding 100 nm (=10^-7 m),

an anorganic oxidic powder of an auxiliary sintering agent with particles of a size not exceeding 100 nm, and

an organic vehicle which is dissolved or suspended in an organic or aqueous solvant and in which the particles of the respective powder are substantially evenly distributed,

wherein the total α

-alumina and auxiliary-sintering-agent content of the paste, the foil, or the slip ranges between 50% and 70%,

or with the joining material being made from

an agglomerate-free, high-purity α

-alumina powder with particles of a size not exceeding 100 nm (=10^-7 m),

an anorganic oxidic auxiliary sintering agent produced chemically as envelopes around or attachment to the particles of the α

-alumina powder, and

an organic vehicle dissolved or suspended in an organic or aqueous solvant,

wherein the total α

-alumina and auxiliary-sintering-agent content of the paste, the foil, or the slip ranges between 50% and 70%; and

heating the substrate and the diaphragm to a temperature of not more than 1,300°

C. and then allowing them to cool down,

wherein the alumina content of the joint after cooling is at least 95 wt. % and the auxiliary-sintering-agent content after cooling is not more than 5 wt. %.

7. The process of claim 6, wherein the total α

-alumina and auxiliary sintering agent is comprised of at least 99.9 wt. % α

-alumina.

8. The process of claim 7, further comprising the step of applying a pressure to the substrate and the diaphragm during the heating step.

9. The process of claim 6, further comprising the step of applying a pressure to the substrate and the diaphragm during the heating step.

10. The process of claim 6 wherein, the particles of the anorganic oxidic powder of the auxiliary sintering agent are the same size as the particles of the α

-alumina powder.