Method of stabilizing the surface properties of objects to be thermally treated in a vacuum

• US 5,400,489 A
• Filed: 10/30/1992
• Issued: 03/28/1995
• Est. Priority Date: 11/30/1991
• Status: Expired due to Term

• Current Assignee: Frank Hegner, Ulfert Drewes
• Original Assignee: Frank Hegner, Ulfert Drewes
• Inventors: Hegner, Frank, Drewes, Ulfert
• Primary Examiner(s): ECHOLS, PERCY W
• Application Number:
  US07/968,811
• Time in Patent Office: 879 Days
• Field of Search: 29/621.1, 29/25.41, 228/121, 228/122, 228/124, 73/718, 338/2, 338/5, 427/240
• US Class Current: 29/25.41
• CPC Class Codes: C03C 17/25 by deposition from the liquid phase
• CPC Class Codes: C03C 2217/213 SiO2
• CPC Class Codes: C03C 2218/113 by sol-gel processes
• CPC Class Codes: C04B 2235/6581 Total pressure below 1 atmosphere, e.g. vacuum
• CPC Class Codes: C04B 2237/062 based on silica or silicates
• CPC Class Codes: C04B 2237/10 Glass interlayers, e.g. frit or flux
• CPC Class Codes: C04B 2237/122 based on refractory metals
• CPC Class Codes: C04B 2237/125 based on noble metals, e.g. silver
• CPC Class Codes: C04B 2237/127 The active component for bonding being a refractory metal
• CPC Class Codes: C04B 2237/343 Alumina or aluminates
• CPC Class Codes: C04B 2237/40 Metallic
• CPC Class Codes: C04B 2237/592 whereby the interlayer is not continuous, e.g. not the whole surface of the smallest substrate is covered by the interlayer
• CPC Class Codes: C04B 2237/708 of one or more of the interlayers
• CPC Class Codes: C04B 2237/72 Forming laminates or joined articles comprising at least two interlayers directly next to each other
• CPC Class Codes: C04B 37/006 consisting of metals or metal salts
• CPC Class Codes: C04B 37/026 consisting of metals or metal salts
• CPC Class Codes: G01L 9/0055 bonded on a diaphragm
• CPC Class Codes: G01L 9/0075 using a ceramic diaphragm, e.g. alumina, fused quartz, glass
• CPC Class Codes: Y10T 29/43 Electric condenser making
• CPC Class Codes: Y10T 29/49103 Strain gauge making

Abstract

To avoid any deterioration of the surface properties of objects of ceramic, glass, or a single-crystal insulating material which are subjected to a vacuum temperature process, a thin layer of a spin-on glass solution with a silicon-dioxide equivalent of not more than 10% is applied to the objects by spinning or spraying prior to the vacuum temperature process. This is particularly important to avoid the strong moisture dependence of capacitive or resistive pressure sensors having a substrate and a diaphragm to be joined together, forming a chamber sealed at least at the edge. The diaphragm is covered with a layer of silicon carbide, niobium, or tantalum serving as one capacitor electrode, or the surface portion of the diaphragm which will lie within the chamber is coated with at least one strain gage; the portion of the substrate surface which will lie within the chamber is coated with at least one additional capacitor electrode or, in the case of the resistive pressure sensor, not coated therewith; over the entire surface portion of the substrate and diaphragm thus coated, a thin layer of the spin-on glass solution is applied and dried; contact is made to the capacitor electrodes or strain gages through the substrate and/or diaphragm, and substrate and diaphragm are brazed together by a ring-shaped part of active brazing material, which also serves as a spacer, or by a sufficient amount of active brazing paste.

Claims

1. A method of providing a protective barrier on an object made of ceramic, glass, or a single-crystal insulating material which is subsequently subjected to a heating process, the method including the steps of applying a thin layer of a spin-on glass solution with a silicon-dioxide equivalent content of not more than 10% to the object, and drying the object before the object subjected to the heating process.

2. The method of claim 1, wherein the spin-on glass solution is applied to the surface of the object by spinning.

3. The method of claim 1, wherein the spin-on glass solution is applied to the surface of the object by spraying.

4. The method of claim 1, wherein the vacuum is at least 10^-5 mbar.

5. The method of claim 1, wherein the vacuum is at least 10^-6 mbar.

6. A method of manufacturing a capacitive pressure sensor having a substrate and a diaphragm to be joined together, particularly in a defined spaced relationship and parallel to each other, forming a chamber sealed at least at the edge, with the substrate and/or the diaphragm made of ceramic, glass, or a single-crystal insulating material, the method comprising the following steps:

the diaphragm is covered with a layer of a conductive material including silicon carbide, niobium, or tantalum serving as a first capacitor electrode;

a portion of the substrate surface which will lie within the chamber is covered with at least one additional layer of said conducting material serving as a second capacitor electrode;

over the entire surface portion of the substrate and diaphragm thus covered, a thin layer of a spin-on glass solution with a silicon-dioxide equivalent content of not more than 10% is applied by spinning or spraying, and dried;

a first electrical lead is coupled to the first capacitor electrode, and a second electrical lead is coupled to the second capacitor electrode, and

the substrate and the diaphragm are high-vacuum-brazed together by means of a ring-shaped part of active brazing material, which also services as a spacer, or by means of an amount of active brazing paste sufficient for holding the two parts at the desired distance from each other.

7. The method as claimed in claim 6 wherein prior to the application of the spin-on glass solution, the capacitor electrodes are covered with a protective layer.

8. A method of manufacturing a resistive pressure sensor having a substrate and a diaphragm to be joined together, particularly in a defined spaced relationship and parallel to each other, forming a chamber sealed at least at the edge, with the substrate and/or the diaphragm made of ceramic, glass or a single-crystal insulating material, the method comprising the following steps:

the surface portion of the diaphragm which will lie within the chamber is covered with at least one strain gage;

over the entire surface portion of the diaphragm thus covered and over an entire surface portion of the substrate which will lie opposite said surface portion of the diaphragm, a thin layer of a spin-on glass solution with a silicon-dioxide equivalent content of not more than 10% is applied by spinning or spraying, and dried;

contact is made between first and second electrical leads and the at least one strain gage through the diaphragm, and

the substrate and the diaphragm are high-vacuum-brazed together by means of a ring-shaped part of active brazing material, which also serves as a spacer, or by means of an amount of active brazing paste sufficient for holding the two parts at the desired distance from each other.

9. A method for manufacturing a capacitive pressure sensor having a substrate and a diaphragm coupled to the substrate in a spaced apart and parallel relation to form a chamber therebetween, the substrate and the diaphragm being made of ceramic, glass, or a single-crystal insulating material, the method comprising the steps of:

covering a surface of the diaphragm configured to face the substrate with a layer of silicon carbide, niobium, or tantalum to form a first capacitor electrode;

covering a portion of a substrate surface configured to face the diaphragm with at least one layer of silicon carbide, niobium, or tantalum to form a second capacitor electrode;

applying a layer of a spin-on glass solution having a silicon-dioxide equivalent content of not more than 10% to said diaphragm surface and said substrate surface;

drying the spin-on glass solution;

coupling first and second electrical leads to the first and second capacitor electrodes, respectively;

positioning an active brazing material between the substrate and the diaphragm for coupling the substrate to the diaphragm so that the substrate is spaced apart from the diaphragm by a predetermined distance; and

heating the substrate, the diaphragm, and the active brazing material in a vacuum to seal the substrate to the diaphragm.

10. The method of claim 9, wherein the spin-on glass solution is applied to the surface of the object by spinning.

11. The method of claim 9, wherein the spin-on glass solution is applied to the surface of the object by spraying.

12. The method of claim 9, wherein the vacuum is at least 10^-5 mbar.

13. The method of claim 9, wherein the vacuum is at least 10^-6 mbar.

14. The method of claim 9, wherein the heating step heats the substrate, the diaphragm, and the active brazing material to a temperature of about 30°

C. to about 100°

C. above a liquidous temperature of the active brazing material.

15. The method of claim 9, wherein prior to the step of applying the spin-on glass solution, the method includes the step of covering the first and second capacitor electrodes with a protective layer.

16. A method of manufacturing a resistive pressure sensor having a substrate and a diaphragm coupled to the substrate in a spaced apart, parallel relation to form a chamber therebetween, the substrate and the diaphragm being made of ceramic, glass or a single-crystal insulating material, the method comprising the steps of:

covering a surface portion of the diaphragm configured to lie within the chamber with at least one strain gage;

applying a layer of a spin-on glass solution having a silicon-dioxide equivalent content of not more than 10% to the surface portion of the diaphragm and to a surface portion of the substrate configured to lie within the chamber opposite said surface portion of the diaphragm;

drying the spin-on glass solution;

coupling first and second electrical leads to the at least one strain gage through the diaphragm;

positioning an active brazing material between the substrate and the diaphragm for coupling the substrate to the diaphragm so that the substrate is spaced apart from the diaphragm by a predetermined distance; and

heating the substrate, the diaphragm, and the active brazing material in a vacuum to bond the active brazing material to the substrate and the diaphragm.

17. The method of claim 16, wherein the spin-on glass solution is applied to the surface of the object by spinning.

18. The method of claim 16, wherein the spin-on glass solution is applied to the surface of the object by spraying.

19. The method of claim 16, wherein the vacuum is at least 10^-5 mbar.

20. The method of claim 16, wherein the vacuum is at least 10^-6 mbar.

21. The method of claim 16, wherein the heating step heats the substrate, the diaphragm, and the active brazing material to a temperature of about 30°

C. to about 100°

C. above a liquidous temperature of the active brazing material.

22. The method of claim 16, wherein active brazing material is a ring-shaped part.