Chemical preconcentrator

• US 6,171,378 B1
• Filed: 08/05/1999
• Issued: 01/09/2001
• Est. Priority Date: 08/05/1999
• Status: Expired due to Term

• Current Assignee: National Technology & Engineering Solutions Of Sandia LLC (Honeywell International Inc.)
• Original Assignee: Sandia Corporation (Martin Marietta Corporation)
• Inventors: Manginell, Ronald P., Frye-Mason, Gregory C.
• Primary Examiner(s): Spitzer, Robert H.
• Application Number:
  US09/369,664
• Time in Patent Office: 523 Days
• Field of Search: 95/82, 95/87, 95/89, 95/90, 951/16, 951/48, 96/4, 96/11, 961/01, 961/02, 961/05, 961/26, 961/43, 961/46, 961/54, 555/24, 55D/IG.5
• US Class Current: 96/143
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/121 cooling; cold traps
• CPC Class Codes: G01N 2030/623 by modulation of sample feed or detector response
• CPC Class Codes: G01N 30/12 by evaporation
• CPC Class Codes: Y10S 55/05 Methods of making filter

Abstract

A chemical preconcentrator is disclosed with applications to chemical sensing and analysis. The preconcentrator can be formed by depositing a resistive heating element (e.g. platinum) over a membrane (e.g. silicon nitride) suspended above a substrate. A coating of a sorptive material (e.g. a microporous hydrophobic sol-gel coating or a polymer coating) is formed on the suspended membrane proximate to the heating element to selective sorb one or more chemical species of interest over a time period, thereby concentrating the chemical species in the sorptive material. Upon heating the sorptive material with the resistive heating element, the sorbed chemical species are released for detection and analysis in a relatively high concentration and over a relatively short time period. The sorptive material can be made to selectively sorb particular chemical species of interest while not substantially sorbing other chemical species not of interest. The present invention has applications for use in forming high-sensitivity, rapid-response miniaturized chemical analysis systems (e.g. a “chem lab on a chip”).

Claims

1. A chemical preconcentrator apparatus, comprising:

(a) a substrate having a suspended membrane formed thereon;

(b) a resistive heating element disposed on a surface of the membrane; and

(c) a sorptive material disposed on at least one surface of the membrane to sorb and concentrate at least one chemical species of interest from a vapor over time, with the chemical species being releasable from the sorptive material upon heating of the sorptive material by the resistive heating element.

2. The apparatus of claim 1 wherein the substrate is selected from the group consisting of semiconductors and dielectrics.

3. The apparatus of claim 2 wherein the substrate comprises silicon.

4. The apparatus of claim 1 wherein the membrane comprises a material selected from the group consisting of silicon nitride, polycrystalline silicon, silicon oxynitride and silicon carbide.

5. The apparatus of claim 1 wherein the resistive heating element comprises a circuitous metal trace.

6. The apparatus of claim 5 wherein the metal comprises a metal selected from the group consisting of platinum, molybdenum, titanium, chromium, palladium, gold, tungsten and combinations thereof.

7. The apparatus of claim 5 further including a heat-spreading layer disposed over the resistive heating element to provide a more uniform heating of the sorptive material.

8. The apparatus of claim 7 wherein the heat-spreading layer comprises aluminum or silicon.

9. The apparatus of claim 1 wherein the sorptive material comprises a microporous material.

10. The apparatus of claim 1 wherein the sorptive material comprises a sol-gel oxide.

11. The apparatus of claim 10 wherein a surface of the sol-gel oxide is chemically modified to enhance sorption of the chemical species of interest.

12. The apparatus of claim 1 wherein the sorptive material comprises a polymer.

13. A method for forming a chemical preconcentrator apparatus for sorbing a chemical species of interest from a vapor over time and releasing the chemical species of interest upon demand, comprising steps for:

(a) forming a suspended membrane on a substrate;

(b) forming a resistive heating element on a surface of the suspended membrane; and

(c) coating at least one surface of the suspended membrane with a sorptive material capable of sorbing the chemical species of interest.

14. The method of claim 13 wherein the suspended membrane comprises a material selected from the group consisting of silicon nitride, polycrystalline silicon, silicon oxynitride and silicon carbide.

15. The method of claim 13 wherein the step for forming the suspended membrane comprises steps for depositing a film over a top surface of the substrate, and removing material from the substrate underneath a portion of the deposited film.

16. The method of claim 15 wherein the step for removing material from the substrate underneath the portion of the deposited film comprises at least one step for etching the substrate from a surface thereof.

17. The method of claim 16 wherein the step for etching the substrate from the surface thereof comprises etching the substrate using an etching method selected from the group of etching methods consisting of anisotropic wet etching, reactive ion etching, and combinations thereof.

18. The method of claim 16 wherein the surface is a bottom surface, and the step for etching the substrate comprises etching through a majority of the thickness of the substrate using reactive ion etching, and etching through the remainder of the thickness of the substrate using anisotropic wet etching.

19. The method of claim 13 wherein the step for forming the suspended membrane comprises steps for:

depositing a sacrificial layer over the substrate;

depositing a film over the sacrificial layer;

forming a plurality of openings through the film to expose the sacrificial layer; and

removing, at least in part, the sacrificial layer through the openings formed in the film.

20. The method of claim 19 wherein the film is selected from the group consisting of silicon nitride, polycrystalline silicon, silicon oxynitride and silicon carbide;

and the sacrificial layer is selected from the group consisting of silicon dioxide, silicate glasses and polymers.

21. The method of claim 20 wherein the step for removing the portion of the sacrificial layer comprises etching the sacrificial layer with a wet etchant comprising hydrofluoric acid.

22. The method of claim 20 wherein the step for removing the portion of the sacrificial layer comprises dissolving the sacrificial layer using a solvent.

23. The method of claim 13 wherein the step for forming the resistive heating element comprises depositing a metal layer and patterning the metal layer to form a circuitous metal trace.

24. The method of claim 23 wherein the metal layer comprises a metal selected from the group consisting of platinum, molybdenum, titanium, chromium, palladium, gold, tungsten and combinations thereof.

25. The method of claim 23 further including a step for annealing the circuitous metal trace for relieving any stress therein.

26. The method of claim 13 wherein the step for coating the surface of the suspended membrane comprises depositing a sorptive material selected from the group consisting of polymers, microporous materials, and sol-gel oxides.

27. The method of claim 26 further including a step for curing the deposited sorptive material by heating.

28. A method for forming a chemical preconcentrator apparatus for sorbing a chemical species of interest from a vapor over time and releasing the chemical species of interest upon demand, comprising steps for:

(a) depositing a film over a top surface of a substrate;

(b) forming a resistive heating element on a portion of the film;

(c) removing material from the substrate underneath the portion of the film and thereby forming a suspended membrane from the film; and

(d) coating at least one surface of the suspended membrane with a sorptive material capable of sorbing the chemical species of interest.

29. The method of claim 28 wherein the film comprises a material selected from the group consisting of silicon nitride, polycrystalline silicon, silicon oxynitride and silicon carbide.

30. The method of claim 28 wherein the step for removing material from the substrate comprises a step for etching the substrate.

31. The method of claim 30 wherein the step for etching the substrate comprises etching the substrate using an etching method selected from the group of etching methods consisting of anisotropic wet etching, reactive ion etching, and combinations thereof.

32. The method of claim 30 wherein the step for etching the substrate comprises etching through the substrate from a bottom surface thereof.

33. The method of claim 32 wherein the step for etching the substrate from the bottom surface thereof comprises etching through a majority of the thickness of the substrate using reactive ion etching, and etching through the remainder of the thickness of the substrate using anisotropic wet etching.

34. The method of claim 28 wherein the step for forming the resistive heating element comprises depositing a metal layer and patterning the metal layer to form a circuitous metal trace.

35. The method of claim 34 wherein the metal layer comprises a metal selected from the group consisting of platinum, molybdenum, titanium, chromium, palladium, gold, tungsten and combinations thereof.

36. The method of claim 34 further including a step for annealing the circuitous metal trace for relieving any stress therein.

37. The method of claim 28 wherein the step for coating the surface of the suspended membrane comprises depositing a sorptive material selected from the group consisting of polymers, microporous materials, and sol-gel oxides.

38. The method of claim 37 further including a step for curing the deposited sorptive material by heating.