Electrochemical sensor/detector system and method

• US 5,296,125 A
• Filed: 03/30/1992
• Issued: 03/22/1994
• Est. Priority Date: 08/31/1990
• Status: Expired due to Fees

• Current Assignee: Regents of the University of California (University of California)
• Original Assignee: The United States of America As Represented By The Secretary of Agriculture
• Inventors: Perone, Sam P., Glass, Robert S., Ciarlo, Dino R., Kimmons, James F.
• Primary Examiner(s): Niebling, John
• Assistant Examiner(s): Phasge, Arun S.
• Application Number:
  US07/860,329
• Time in Patent Office: 722 Days
• Field of Search: 29/829, 430/311, 430/312, 430/313, 430/319, 204/153.21
• US Class Current: 430/311
• CPC Class Codes: G01N 27/27 Association of two or more measuring systems or cells, each measuring a different parameter, where the measurement results may be either used independently, the systems or cells being physically associated, or combined to produce a value for a further parameter
• CPC Class Codes: Y10T 29/49124 On flat or curved insulated base, e.g., printed circuit, etc.

Abstract

An electrochemical detection system is described comprising in combination:

(a) a multielement, microelectrode array detector containing means for acquiring a plurality of signals;

(b) electronic means for receiving said signals and converting said signals into a readout or display providing information with respect to the nature and concentration of elements present in a solution being tested.

Also described is the means of making the above described microelectrode detector.

Claims

1. A method for preparing an electrochemical detector containing microelectrodes embedded in an insulating matrix which comprises:

(a) selecting a silicon wafer of predetermined size;

(b) coating one side of said wafer with silicon nitride;

(c) applying a photo-resist composition to the top of said silicon nitride;

(d) applying to said photo-resist a mask which selects a predetermined electronic circuit pattern;

(e) developing said photo-resist;

(f) evaporating a metal onto the surface of said photo-resist covered wafer to a thickness of about 1000Å

.

(g) lifting off the metal coated photo-resist, leaving a metal circuit pattern on said silicon nitride, and repeating steps (c) through (g) a predetermined number of times with a different metal each time.

2. The method claim 1 wherein said metal evaporated onto the surface of said photo-resist is selected from the group consisting of platinum, gold, carbon, iridium, vanadium, nickel, silver, titanium or copper.

3. The method of claim 1 wherein said photo-resist is deposited to a thickness of 1.25 μ

m.

4. The method of claim 1 wherein evaporated niobium serves as an adhesion layer between the sensor materials are conductor pattern.

5. The method of claim 1 wherein said unwanted metal is lifted off with acetone.

6. A method of preparing an electrochemical detector containing microelectrodes embedded in an insulating matrix which comprises:

a. selecting an alumina-ceramic wafer of predetermined size,

b. coating said wafer on one side with a layer of chromium,

c. coating said layer of chromium with a layer of gold,

d. coating said layer of gold with a positive photo-resist composition,

e. placing a photo-mask with a desired conductor pattern thereon over said photo-resist coated wafer,

f. exposing said photo-resist coating with ultraviolet light through said photo-mask, and dissolving away those areas of photo-resist not protected from exposure by said photo-mask in a chemical developer bath, exposing said gold,

g. etching away said gold not covered by said photo-resist, leaving a photo-resist covered gold circuit pattern,

h. removing the balance of said photo-resist exposing said gold circuit pattern,

i. depositing a plurality of sensor materials at pre-determined areas on said gold circuit pattern, at least one of said sensor materials being platinum,

j. applying a negative photo-resist over said sensor materials and said wafer,

k. applying a shadow-mask over said photo-resist covered wafer which has opaque dots corresponding in location with said sensor materials,

l. exposing said negative photo-resist to ultraviolet light through said shadow-mask,

m. dissolving the unexposed portions of said negative photo-resist corresponding in location with said opaque dots in said shadowmask,

thereby leaving exposed to the environment those specific areas of said sensor materials in register with the opaque dots in said shadow mask, thus forming arrays of microelectrodes.

7. The method of claim 6 wherein said sensor materials are selected from the group consisting of platinum, gold, carbon, iridium, vanadium, copper, silver, titanium or nickel.

8. The method of claim 6 wherein said positive photo-resist composition is a photoactive novolak resin in a solvent system.

9. The method of claim 6 wherein said negative photo-resist composition is a photoactive compound in a solvent system.

10. The method of claim 6 wherein said wafer is approximately 10 mil thick, and said chromium is applied to a depth of 0.01 micron.

11. The method of claim 6 wherein said wafer is about 10 mil thick, and said gold is applied to a depth of about 4 microns.

12. The method of claim 6 wherein said gold is etched away with a solution of potassium iodide and iodine crystals.

13. The method of claim 6 wherein said sensor materials are applied to a depth of 0.1-1.0 micron.

14. The method of claim 6 wherein said sensor materials comprise platinum and iridium.

15. The method of claim 6 wherein said sensor materials comprise platinum and vanadium.

16. The method of claim 6 wherein said sensor materials comprise platinum and carbon.

17. The method of claim 6 wherein said microelectrodes are formed of diameter 5 μ

m, separated by 14.5 μ

m, arranged in arrays of different materials, each comprising a block of approximately 77,000 electrically connected microelectrodes.

18. A method of preparing a wafer containing a plurality of microelectrodes which comprises:

a. selecting a thin alumina-ceramic or silicon wafer of predetermined size,

b. adhering to one side of said wafer a conducting material having a predetermined electronic circuit pattern,

c. depositing a plurality of different sensor materials at a plurality of predetermined locations on said conducting material, and

d. covering said wafer with an inert insulating substance leaving exposed a defined area of said sensor materials,

19. The method of claim 18 wherein the defined area is less than or equal to about 100 μ

m².

20. A method of preparing an electrochemical detector containing microelectrodes embedded in an insulating matrix which comprises:

a. selecting an insulated silicon wafer of predetermined size,

b. coating said wafer on one side with a layer of chromium,

c. coating said layer of chromium with a layer of gold,

d. coating said layer of gold with a positive photo-resist composition,

e. placing a photo-mask with a desired conductor pattern thereon over said photo-resist coated wafer,

f. exposing said photo-resist coating with ultraviolet light through said photo-mask, and dissolving away those areas of photo-resist not protected from exposure by said photo-mask in a chemical developer bath, exposing said gold,

g. etching away said gold not covered by said photo-resist, leaving a photo-resist covered gold circuit pattern,

h. removing the balance of said photo-resist exposing said gold circuit pattern,

i. depositing a plurality of sensor materials at pre-determined areas on said insulating substrate, at least one of said sensor materials being platinum,

j. applying a negative photo-resist over said sensor materials and said wafer,

k. applying a shadow-mask over said photo-resist covered wafer which has opaque dots corresponding in location with said sensor materials,

l. exposing said negative photo-resist through said shadowmask,

m. dissolving the unexposed portions of said negative photo-resist corresponding in location with said opaque dots in said shadowmask,

thereby leaving exposed to the environment those specific areas of said sensor materials in register with the opaque dots in said shadow mask, thus forming microelectrodes arrays.

21. The method of claim 20 wherein said sensor material is selected from the group consisting of platinum, gold, carbon, iridium, vanadium, copper, silver, nickel, titanium.

22. The method of claim 20 wherein said positive photo-resist composition is a photoactive novolak resin in a solvent system.

23. The method of claim 20 wherein said negative photo resist composition is a photoactive compound in a solvent system.

24. The method of claim 20 wherein said wafer is approximately 10 mil thick, and said chromium is applied to a depth of 0.01 micron.

25. The method of claim 20 wherein said wafer is about 10 mil thick, and said gold is applied to a depth of about 4 microns.

26. The method of claim 20 wherein said gold is etched away with a solution of potassium iodide and iodine crystals.

27. The method of claim 20 wherein said sensor materials are applied to a depth of 0.1-1.0 microns.

28. The method of claim 20 wherein said sensor materials comprise platinum and iridium.

29. The method of claim 20 wherein said sensor materials comprise platinum and vanadium.