Method for producing a vacuum measuring cell of the membrane type
Method for producing a vacuum measuring cell having a pressure transducer diaphragm with housing plates sealed on opposite sides to form reference and measuring vacuum chambers. An opening in one plate communicates with the measuring vacuum chamber and has a sealed connection for joining to medium to be measured. The diaphragm and plates are aluminum oxide ceramic and at least one of the seals is aluminum with a thickness of 0.5 μm to 30 μm. The ceramic parts are pressed together at increased temperature of 600° C. to 680° C. in a process gas atmosphere including a reducing gas, during a time of 30 to 90 minutes, and subsequently a tempering step is carried out in a second process gas atmosphere including oxygen, tempering taking place at a temperature of 450° C. to 575° C. such that the metallic aluminum is oxidized into aluminum oxide.
1. A method for the production of a vacuum measuring cell ( 8 ) for measuring a medium, the vacuum measuring cell comprising first and second housing plates ( 1 , 4 ) and a diaphragm ( 2 ) for functioning as a pressure transducer, one side of the diaphragm ( 2 ) being spaced apart from a portion of the first housing plate ( 1 ) around a margin region of the first housing plate that is engaged against a margin region of the diaphragm in a first joining region by joining means ( 3 ) forming a seal, so that between the margin regions of the first housing plate and the diaphragm, a reference vacuum chamber ( 7 ) is formed, an opposite side of the diaphragm ( 2 ) being spaced apart from a portion of the second housing plate ( 4 ) around a margin region of the second housing plate that is engaged against the margin region of the diaphragm in a second joining region by joining means ( 3 ) forming a seal, so that between the margin region of the second housing plate and the diaphragm, a measuring vacuum chamber ( 9 ) is formed, the second housing plate ( 4 ) including an opening for communicating the measuring vacuum chamber ( 9 ) to the medium, the vacuum measuring cell including connection means ( 5 ) with joining means ( 6 ) connected to the second housing part for forming a seal for joining the measuring vacuum chamber ( 9 ) with the medium to be measured in a third joining region, wherein at least the diaphragm ( 2 ) and the two housing plates ( 1 , 4 ) are ceramic parts ( 1 , 2 , 4 ) of an aluminum oxide, the method comprising: forming at least one of the joining means ( 3 , 6 ) of metallic aluminum having a thickness in the range of 0.5 μm to 30 μm; disposing the at least one joining means in one of the joining regions between the ceramic parts ( 1 , 2 , 4 ); and joining the ceramic parts by pressing the ceramic parts ( 1 , 2 , 4 ) to be joined together at increased temperature in the range of 600° C. to 680° C. in a process gas atmosphere encompassing the parts to be joined, the process gas atmosphere including a reducing gas, and the pressing occurring during a time in the range of 30 to 90 minutes; and subsequently to the pressing step, performing a tempering step in a second process gas atmosphere which includes oxygen, wherein the tempering step takes place in a temperature range of 450° C. to 575° C. so that the metallic aluminum is substantially oxidized to aluminum oxide.
2. The method as claimed in claim 1 , wherein each ceramic part comprises one of an alpha and gamma aluminum oxide.
3. The method as claimed in claim 1 , wherein surfaces to be joined of the ceramic parts ( 1 , 2 , 4 ) have a mean surface roughness of less than 500 nm.
4. The method as claimed in claim 1 , wherein the tempering is performed for a time in the range from 2.0 to 12 hours.
5. The method as claimed in claim 1 , including cleaning at least surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined of foreign material before the joining step.
6. The method as claimed in claim 5 , wherein the cleaning step is a chemical cleaning step carried out using a solution containing HNO 3 .
7. The method as claimed in claim 1 , wherein the ceramic parts ( 1 , 2 , 4 ) have a purity of better than 99%.
8. The method as claimed in claim 1 , including depositing an adhesion promoting metallic layer on at least one of the surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined.
9. The method as claimed in claim 1 , including the joining means of metallic aluminum ( 3 , 6 ) being deposited as a layer on at least one of the surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined.
10. The method as claimed in claim 8 , wherein the adhesion promoting metallic layer has a thickness in the range of 0.2 μm to 15 μm.
11. The method as claimed in claim 1 , wherein, as the joining means ( 3 , 6 ), a foil of aluminum is utilized with a thickness in the range of 10 μm to 50 μm.
12. The method as claimed in claim 1 , wherein the joining step is performed with a shearing strength in the range of 5 N/mm 2 to 35 N/mm 2 .
13. The method as claimed in claim 1 , wherein, after the joining step, in a further step at least in the joining regions, an additional layer ( 13 ) is deposited as a vacuum tightening means, which covers and overlaps the joining regions and at least one subregion of the joined ceramic parts ( 1 , 2 , 4 ).
14. The method as claimed in claim 1 , including applying, as a sealing means ( 13 ) around the cell, a glass solder.
15. The method as claimed in claim 1 , including applying an additional covering ( 14 ) for improved sealing with a material only in the joining region as additional sealing means ( 14 ), wherein such covering is only applied on an outer surface of the measuring cell ( 8 ) forming the seal at the margin region of the diaphragm.
16. The method as claimed in claim 1 , wherein the vacuum measuring cell ( 8 ) comprises a capacitive diaphragm measuring cell.
17. The method as claimed in claim 1 , wherein the vacuum measuring cell ( 8 ) comprises an optically readable diaphragm measuring cell.
18. The method as claimed in claim 1 , wherein the ceramic parts each at least partly comprise sapphire and have different shapes.
19. The method as claimed in claim 1 , wherein surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined have a mean surface roughness of less than 500 nm and are planar.
20. The method as claimed in claim 1 , wherein the tempering is performed for a time in the range from 6.0 to 10 hours.
21. The method as claimed in claim 1 , wherein at least the surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined are cleaned of foreign material before the joining process, through at least one of: chemical etching; plasma etching; and ion etching.
22. The method as claimed in claim 5 , including a further treatment step carried out using a solution containing HF on the surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined.
23. The method as claimed in claim 1 , wherein the ceramic parts ( 1 , 2 , 4 ) have a purity of better than 99.5%.
24. The method as claimed in claim 1 , including depositing an adhesion promoting metallic layer on at least one of the surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined which comprises at least one of Ti and Cr.
25. The method as claimed in claim 1 , including the joining means of metallic aluminum ( 3 , 6 ) being deposited as a layer on at least one of the surfaces of the ceramic parts ( 1 , 2 , 4 ) to be joined using a vacuum process comprising sputtering.
26. The method as claimed in claim 8 , wherein the adhesion promoting metallic layer has a thickness in the range of 0.5 μm to 6.0 μm.
27. The method as claimed in claim 1 , wherein, as the joining means ( 3 , 6 ), a foil of aluminum is utilized with a thickness in the range of 10 μm to 30 μm.
28. The method as claimed in claim 1 , wherein the joining step is performed with a shearing strength in the range of 14 N/mm 2 to 42 N/mm 2 .
29. The method as claimed in claim 1 , including applying, as a sealing means ( 13 ) around the cell, a glass solder in the form of a layer deposited using an ALD method.
30. The method as claimed in claim 1 , including applying an additional covering ( 14 ) for improved sealing with a material only in the joining region as additional sealing means ( 14 ), wherein said covering is only applied on an outer surface of the measuring cell ( 8 ) forming the seal at the margin region of the diaphragm, the additional covering ( 14 ) being a glass solder.