Method of making electrochemical detectors based on iridium oxide

• US 6,863,792 B1
• Filed: 10/11/2001
• Issued: 03/08/2005
• Est. Priority Date: 10/11/2001
• Status: Expired due to Fees

• Current Assignee: Ohio State University
• Original Assignee: Ohio State University
• Inventors: Yao, Sheng, Madou, Marc J.
• Primary Examiner(s): King, Roy
• Assistant Examiner(s): Leader, William T.
• Application Number:
  US09/975,475
• Time in Patent Office: 1,244 Days
• Field of Search: 205/86, 205/229, 205/230, 205/231, 205/333, 205/538, 205/543, 205/704
• US Class Current: 205/86
• CPC Class Codes: C25D 11/34 of metals or alloys not provided for in groups C25D11/04 - C25D11/32

Abstract

A conductive oxide solid formed through an electrochemical process. The resulting solid predominantly contains oxides of the highest oxidation state. Additionally, the solid can be thick, uniform, stable across a wide range of acidity and temperature, fully hydrated, and conductive with a very low redox potential. A preferred embodiment is an iridium solid formed at high temperature in molten carbonate, said solid containing intercalated lithium. The solid has application as an electrode with reduced drift. An electrochemical acidity sensor is disclosed which pairs an electrode bearing the solid with a reference electrode. Additionally, sensor apparatuses for measuring carbon dioxide and other materials as well as methods for measuring materials using an embedded acidity sensor are disclosed.

Claims

1. A method for forming an iridium oxide solid, said method comprising the steps of:

exposing iridium metal to an alkali metal carbonate at a temperature sufficient to oxidize said iridium metal; and

applying a voltage between said iridium metal and said alkali metal carbonate so as to drive said oxidizing iridium metal toward a maximum oxidation state.

2. The method for forming an iridium oxide solid of claim 1, wherein said exposing of said iridium metal to said alkali metal carbonate is accomplished by a technique selected from the group consisting of:

immersing said iridium metal in a bath of liquid alkali metal carbonate, applying liquid alkali metal carbonate to said iridium metal, depositing said iridium metal and said alkali metal carbonate sequentially and heating until one liquefies, bombarding said alkali metal carbonate with ions containing said iridium metal, bombarding said iridium metal with ions containing said alkali metal carbonate, condensing said alkali metal carbonate from a vapor phase onto said iridium metal, and condensing said iridium metal from a vapor phase onto said alkali metal carbonate.

3. The method for forming an iridium oxide solid of claim 1, wherein said application of a voltage between said iridium metal and said alkali metal carbonate is accomplished by a technique selected from the group consisting of:

applying a galvanic potential across a bimetallic junction, utilizing the potential from a voltage-regulated power source connecting said iridium metal and said alkali metal carbonate in a circuit, and utilizing the potential from a battery connecting said iridium metal and said alkali metal carbonate in a circuit.

4. The method for forming an iridium oxide solid of claim 1, further comprising the step of cleaning said iridium metal.

5. The method for forming an iridium oxide solid of claim 4, wherein said cleaning is accomplished by application of chemicals selected from the group consisting of:

acetone, hydrochloric acid and de-ionized water.

6. The method for forming an iridium oxide solid of claim 1, further comprising the step of drying said iridium metal wire.

7. The method for forming an iridium oxide solid of claim 6, wherein said drying consists of drying said wire in an electric oven.

8. The method for forming an iridium oxide solid of claim 1, wherein said alkali metal carbonate is in powder form.

9. The method for forming an iridium oxide solid of claim 1, wherein said alkali metal carbonate is selected from the group consisting of:

lithium carbonate and sodium carbonate.

10. The method for forming an iridium oxide solid of claim 1, further comprising the step of descumming said oxidized iridium metal.

11. The method for forming an iridium oxide solid of claim 1, wherein said iridium metal is oxidizes by ambient oxygen.

12. The method for forming an iridium oxide solid of claim 11, wherein said ambient oxygen is atmospheric oxygen.

13. A method for forming an iridium oxide solid electrode, said method comprising the steps of:

forming an iridium oxide solid, said iridium oxide solid formed by the method of;

(i) exposing iridium metal to an alkali carbonate at a temperature sufficient to oxidize said iridium metal;

(ii) applying a voltage between said iridium metal and said alkali metal carbonate so as to drive said oxidizing iridium metal toward a maximum oxidation state; and

depositing said iridium oxide solid on at least one surface of an electrical lead, said electrical lead conductively attached to said iridium oxide solid.

14. A method for forming an iridium oxide solid electrode according to claim 13, wherein said electrical lead is gold.

15. A method for forming an iridium oxide solid electrode according to claim 13, wherein said iridium metal is oxidized by ambient oxygen.

16. A method for forming an iridium oxide solid electrode according to claim 15, wherein said ambient oxygen is atmospheric oxygen.

17. A method for forming an iridium oxide solid electrode, said method comprising the steps of:

forming an iridium oxide solid, said iridium oxide solid formed by the method of;

(i) exposing iridium metal to an alkali carbonate at a temperature sufficient to oxidize said iridium metal;

(ii) applying a voltage between said iridium metal and said alkali metal carbonate so as to drive said oxidizing iridium metal toward a maximum oxidation state; and

depositing said iridium oxide solid on at least one surface of a metal substrate, said metal substrate conductively attached to said iridium oxide solid; and

conductively connecting an electrical lead to said metal substrate, so as to form an iridium oxide electrode.

18. A method for forming an iridium oxide solid electrode according to claim 17, wherein said metal substrate is iridium.

19. A method for forming an iridium oxide solid electrode according to claim 17, wherein said electrical lead is gold.