Electrode assembly including iridium based mercury ultramicroelectrode array

• US 5,378,343 A
• Filed: 01/11/1993
• Issued: 01/03/1995
• Est. Priority Date: 01/11/1993
• Status: Expired due to Term

• Current Assignee: Board of Trustees of the Leland Stanford Junior University (Stanford University), Tufts University
• Original Assignee: Leland Standard University, Tufts University
• Inventors: Storment, Christopher W., Kovacs, Gregory T. A., Kounaves, Samuel P.
• Primary Examiner(s): Niebling, John
• Assistant Examiner(s): Bell, Bruce F.
• Application Number:
  US08/003,229
• Time in Patent Office: 722 Days
• Field of Search: 204/290 R, 204/413, 204/435, 204/153.23, 204/412
• US Class Current: 204/413
• CPC Class Codes: G01N 27/403 Cells and electrode assemblies

Abstract

An electrode assembly for use in quantifying the levels of various metals in an aqueous solution. In one embodiment, the electrode assembly comprises a substrate, the substrate being a silicon chip upon which a layer of silicon dioxide has been grown. A plurality of gold bond pads and gold interconnect traces are deposited by microphotolithography onto the silicon dioxide layer. An array of iridium deposits are then patterned by microphotolithography onto the interconnect traces at predefined locations. A passivation layer is deposited by plasma enhanced chemical vapor deposition over the finished metallization to electrically insulate it from external solutions. Plasma etching is then used to expose at least a portion of each of the iridium deposits. Just prior to analytical use, one or more of the exposed iridium elements are electroplated with mercury. The present invention is also directed to a field deployable sensor including the above-described electrode assembly.

Claims

1. An electrode assembly for use in quantifying the levels of various metals in an aqueous solution, said electrode assembly comprising:

a) a substrate; and

b) an array of ultramicroelectrodes arranged on said substrate, each of said ultramicroelectrodes comprising a layer of iridium and a layer of mercury, said mercury layer being disposed on said iridium layer.

2. The electrode assembly as claimed in claim 1 wherein said substrate has a non-conductive top surface and wherein said ultramicroelectrodes are arranged on said non-conductive top surface.

3. The electrode assembly as claimed in claim 2 wherein said substrate is a quantity of doped or undoped silicon upon which a layer of silicon dioxide or silicon nitride has been grown or deposited.

4. The electrode assembly as claimed in claim 1 further comprising means for interconnecting said ultramicroelectrodes to external electronics.

5. The electrode assembly as claimed in claim 4 wherein said interconnecting means comprises a plurality of interconnect traces and bond pads arranged on said substrate.

6. The electrode assembly as claimed in claim 5 wherein said interconnect traces and bond pads are made of gold.

7. The electrode assembly as claimed in claim 1 wherein said mercury layer is hemispherical or any other shape.

8. The electrode assembly as claimed in claim 1 wherein said iridium layer of two or more of said array of ultramicroelectrodes is formed from a single iridium deposit.

9. The electrode assembly as claimed in claim 1 wherein all of said ultramicroelectrodes are identical to one another.

10. The electrode assembly as claimed in claim 9 wherein two or more of said ultramicroelectrodes are electrically interconnected.

11. The electrode assembly as claimed in claim 10 wherein said ultramicroelectrodes have non-overlapping diffusion fields.

12. The electrode assembly as claimed in claim 9 wherein said ultramicroelectrodes have non-overlapping diffusion fields.

13. A method of making an electrode assembly comprising the steps of:

a) providing a substrate, said substrate having a non-conductive top surface;

b) depositing iridium onto said non-conductive top surface of said substrate; and

c) depositing a quantity of mercury onto at least a portion of said iridium deposit.

14. The method as claimed in claim 13 wherein said mercury depositing step comprises electroplating said quantity of mercury onto said portion of said iridium deposit.

15. A method of making an electrode assembly comprising the steps of:

a) providing a substrate, said substrate having a non-conductive top surface;

b) forming an array of iridium ultramicroelectrodes on said non-conductive top surface of said substrate; and

c) depositing a quantity of mercury on said iridium ultramicroelectrodes.

16. The method as claimed in claim 15 further comprising, prior to said iridium ultramicroelectrodes forming step, the step of forming an array of bond pads and interconnect traces on said non-conductive top surface of said substrate, wherein said iridium ultramicroelectrodes are formed at predefined locations on said interconnect traces.

17. An electrode assembly manufactured by the method of claim 15.

18. The method as claimed in claim 15 wherein said bond pads and said interconnect traces are made of gold.

19. The method as claimed in claim 15 wherein said bond pads, said interconnect traces and said iridium ultramicroelectrodes are deposited by microphotolithography.

20. An electrode assembly manufactured by the method of claim 19.

21. The method as claimed in claim 15 further comprising, prior to said mercury depositing step, the steps of depositing a passivation layer over the finished metallization and then exposing at least a portion of each of said iridium ultramicroelectrodes and said bond pads, wherein said deposited mercury is deposited over said exposed portions of said iridium ultramicroelectrodes.

22. An electrode assembly manufactured by the method of claim 21.

23. A portable sensor adapted to detect the levels of metals in an aqueous solution, said portable sensor comprising:

a) an elongated housing having a porous tip for permitting the passage therethrough of the aqueous solution being tested;

b) an electrode assembly appropriately disposed within said elongated housing to sample the aqueous solution, said electrode assembly comprising

i) a substrate; and

ii) an array of ultramicroelectrodes arranged on said substrate, each of said ultramicroelectrodes comprising a layer of iridium and a layer of mercury, said mercury layer being disposed on said iridium layer;

c) a reference electrode appropriately disposed within said elongated housing to sample the aqueous solution; and

d) electronics disposed within said elongated housing for performing simple or pulsed voltammetric techniques such as anodic stripping voltammetry.

24. The field deployable sensor as claimed in claim 23 further comprising a cable connected to said electronics for transmitting the results of said electrochemical measurements to a nearby or remote location.