Micro and ultrafilters with controlled pore sizes and pore size distribution and methods for making

• US 6,309,546 B1
• Filed: 07/08/1999
• Issued: 10/30/2001
• Est. Priority Date: 01/10/1997
• Status: Expired due to Fees

• Current Assignee: Ellipsis Corporation
• Original Assignee: Ellipsis Corporation
• Inventors: Herrmann, Robert C., Landin, Steven M.
• Primary Examiner(s): FORTUNA, ANA M
• Application Number:
  US09/341,483
• Time in Patent Office: 845 Days
• Field of Search: 210/490, 210/500.25, 210/500.26, 210/499, 555/23, 555/24, 427/244, 427/245, 264/45.1
• US Class Current: 210/500.25
• CPC Class Codes: B01D 2239/0442 Antimicrobial, antibacterial, antifungal additives apparatus incorporating such gas filtering material B01D46/0028
• CPC Class Codes: B01D 2239/0471 Surface coating material
• CPC Class Codes: B01D 2239/0478 on a layer of the filter
• CPC Class Codes: B01D 2239/0654 Support layers
• CPC Class Codes: B01D 2239/083 Binders between layers of the filter
• CPC Class Codes: B01D 2239/10 Filtering material manufacturing
• CPC Class Codes: B01D 2239/1216 Pore size
• CPC Class Codes: B01D 2239/1241 Particle diameter
• CPC Class Codes: B01D 2323/08 Specific temperatures applied
• CPC Class Codes: B01D 2323/081 Heating
• CPC Class Codes: B01D 2325/04 Characteristic thickness
• CPC Class Codes: B01D 2325/12 Adsorbents being present on the surface of the membranes or in the pores
• CPC Class Codes: B01D 39/12 of wire gauze; of knitted wire; of expanded metal
• CPC Class Codes: B01D 39/2034 sintered or bonded by inorganic agents
• CPC Class Codes: B01D 39/2041 the material being filamentary or fibrous
• CPC Class Codes: B01D 39/2082 the material being filamentary or fibrous
• CPC Class Codes: B01D 67/0041 by agglomeration of particles in the dry state
• CPC Class Codes: B01D 67/00411 by sintering
• CPC Class Codes: B01D 69/141 Heterogeneous membranes, e.g. containing dispersed material; Mixed matrix membranes
• CPC Class Codes: B01D 69/1411 containing dispersed material in a continuous matrix
• CPC Class Codes: B01D 71/022 : Metals
• CPC Class Codes: B01D 71/02231 : Palladium
• CPC Class Codes: B01D 71/02232 : Nickel
• CPC Class Codes: B01J 37/0215 : Coating
• CPC Class Codes: B32B 15/02 : Layer formed of wires, e.g. mesh
• CPC Class Codes: B32B 15/16 : next to a particulate layer
• CPC Class Codes: B32B 2305/38 : Meshes, lattices or nets
• CPC Class Codes: B32B 2305/80 : Sintered
• CPC Class Codes: B32B 5/28 : impregnated with or embedded in a plastic substance not used

Abstract

A micro/ultrafiltering element (10) and method for making a filter element are provided. The filtering element comprises a multi-level support (26) having a filtering membrane layer (12) formed thereon comprising sintered particles (14) of uniform diameter. The filtering membrane preferably has an average pore size of from about 0.005-10 micrometers. The filter element is capable of being formed in a variety of geometrical shapes based on the shape of the porous support,

Claims

1. A method of making a micro/ultra-filter element comprising:

(a) masking a uniformly porous support resulting in the pores of said support to be substantially impenetrable;

(b) coating a solution of uniformly sized metallic particles dispersed in a fluid medium comprising a binding agent on the surface of said masked uniformly porous support, wherein said particles do not substantially penetrate the pores of said support; and

(c) heating said coated support to a temperature sufficiently high to (i) sinter said metallic particles resulting in metallurgical adhesion between said metallic particles and between said metallic particles and said surface of said porous support thereby producing a uniformly porous membrane on the surface of said support; and

(ii) volatize or burn off said mask.

2. The method of claim 1, wherein said porous support is metallic.

3. The method of claim 2, wherein said metallic porous support is comprised of a metal selected from the group consisting of titanium, iron, nickel, chromium, silver, and alloys thereof.

4. The method of claim 2, wherein said metallic porous support comprises stainless steel.

5. The method of claim 2, wherein said metallic support comprises

(a) a first wire mesh layer having an upper surface for supporting said particles and a lower surface, wherein said first layer supports said particles;

(b) a second wire mesh layer bonded to the lower surface of said first layer, wherein said second layer protects said first layer from possible deformation under high pressure;

(c) a third wire mesh layer bonded to said second layer, wherein said third layer lends support to said metallic support; and

(d) a fourth wire mesh layer bonded to said third layer, wherein said fourth layer lends support to said metallic support, and said first layer has a finer mesh size than said second, third and fourth layers.

6. The method of claim 5, wherein said first layer has an approximate weave count of 325×

2000.

7. The method of claim 1, wherein said metallic particles are comprised of a metal selected from the group consisting of titanium, iron, nickel, chromium, silver and alloys thereof.

8. The method of claim 1, wherein said metallic particles comprise stainless steel.

9. The method of claim 1, wherein said metallic particles have a uniform particle size ranging from about 1 μ

m to 10 μ

m.

10. The method of claim 1, wherein said particles consist essentially of the same material as said support.

11. The method of claim 1, wherein said solution of particles comprises said particles in the range of 50 to 75 weight percent and a binder system i the range of 25-50 weight percent.

12. A method of claim 11, wherein said binder system comprises a solvent in the range of 5 to 10 weight percent, a binder, a plasticizer and a dispersant.

13. The method of claim 12, wherein said binder is polyvinyl butyral.

14. The method of claim 12, wherein said solvent is toluene.

15. The method of claim 1, further comprising the step of applying a second mixture of particles dispersed in said binder system to said membrane surface.

16. The method of claim 15, wherein said particles in said second mixture have a smaller diameter than said particles in said first mixture.

17. The method of claim 1, wherein said heating step takes place in the presence of an oxygen gettering agent.

18. The method of claim 1, wherein said porous, membrane has an average pore size in the range of about 0.005 to 10 micrometers.

19. The method of claim 1, further comprising the step of applying a film coating over said membrane surface.

20. The method of claim 19, wherein said film is applied using a deposition process.

21. The method of claim 19, wherein said film has a thickness of about 0.2 μ

m.

22. The method of claim 1, wherein said filter element is planar.

23. The method of claim 1 , wherein said porous support is formed into a desired geometric shape prior to the coating step.

24. A method of making a micro/ultra-filter element comprising:

(a) masking a uniformly porous support resulting in, the pores of said support to be substantially impenetrable;

(b) depositing on the metallic, multi-layered porous support a plurality of uniformly sized metallic particles that are spherical in shape, wherein said particles do not substantially penetrate the pores of said support;

(c) sintering said metallic particles and said masked support to the extent that said particles and said support adhere forming a contiguous membrane on the surface of said support, said membrane having consistent uniform pore size and pore size distribution; and

(d) removing said mask from said masked metallic, multi-layered porous support.

25. A method of making a micro/ultra-filter element comprising:

(a) coating a solution of uniformly sized metallic particles dispersed in a fluid medium comprising a binding agent on the surface of said masked uniformly porous support, wherein said particles comprise metallic particles and ceramic particles at a ratio between greater than 0 volume percent and less than or equal to 50 volume percent ceramic particles; and

(b) heating said coated support to a temperature sufficiently high to sinter said metallic particles but below the sintering temperature of said ceramic particles, resulting in metallurgical adhesion between said metallic particles and between said metallic particles and said surface of said porous support, thereby producing a uniformly porous membrane on the surface of said porous support.

26. The method of claim 25, wherein said metallic particles are comprised of a metal selected An the group consisting of titanium, iron, nickel, chromium, silver and alloys thereof.

27. The method of claim 25, wherein said ceramic particles are comprised of an oxide.

28. The method of claim 27, wherein said oxide is selected from the group consisting of alumina (Al₂O₄), magnesia (MgO), titania (TiO₂), silica (SiO₂), zirconia (ZrO₂), yttria (Y₂O₃), magnesium aluminate (MgAl₂O₄), and nickel aluminate (NiAl₂O₄).

29. The method of claim 25, wherein said ceramic particles are comprised of a nitride.

30. The method of claim 29, wherein said nitride is selected from the group consisting of aluminum nitride (AlN), silicon nitride (Si₂N₃), and sialons (SiAlON).

31. The method of claim 25, wherein said ceramic particles are comprised of a carbide.

32. The method of claim 31, wherein said carbide is selected from the group consisting of silicon carbide.

33. The method of claim 25, wherein said ceramic particles are comprised of a boride.

34. The method of claim 33, wherein said boride is selected from the group consisting of titanium boride (TiB₂).

35. A method of making a micro/ultra filter element comprising:

(a) depositing on the surface of a metallic, multi-level porous support a plurality of uniformly sized particles that are spherical in shape, wherein said particles comprise metallic particles and ceramic particles at a ratio between greater than 0 volume percent and less than or equal to 50 volume percent ceramic particles; and

(b) sintering said metallic particles and said support at a sufficiently high temperature such that said particles and said support adhere but below the sintering temperature of the ceramic particles, thereby forming a contiguous membrane on the surface of said support, wherein said membrane has consistent uniform pore size and pore size distribution.

36. A filter element comprising

(a) a top porous membrane comprising ceramic particles and contiguous metallic particles, wherein said ceramic particles are present at a ratio of between greater than 0 volume percent and less than or equal to 50 volume percent, and wherein said metallic particles are sintered and form a metallic matrix and said ceramic particles are contained within said metallic matrix;

(b) a first layer Ar supporting said membrane, said first layer comprised of a first wire mesh for supporting said membrane;

(c) a second layer comprising a second wire mesh bonded to said first layer for protecting said first layer from deformation;

(d) a third layer comprising a third wire mesh bonded to said second layer for stabilizing the filter element; and

(e) a fourth layer comprising a fourth wire mesh bonded to said all layer for providing additional rigidity to the filter element,

wherein said metallic particles are further sintered to said first layer.