Method of using an array of electrodes for high throughput development and testing of materials

• US 6,937,002 B2
• Filed: 10/09/2003
• Issued: 08/30/2005
• Est. Priority Date: 12/22/1998
• Status: Expired due to Fees

• Current Assignee: Daniel Buttry, John Pope
• Original Assignee: Daniel Buttry, John Pope
• Inventors: Pope, John, Buttry, Daniel
• Primary Examiner(s): Deb, Anjan K.
• Application Number:
  US10/681,285
• Publication Number:
  US 20040100290A1
• Time in Patent Office: 691 Days
• Field of Search: 324/71.1, 324/444, 324/447, 324/425, 324/600, 205/81, 205/118, 205/687, 205/704, 205/82, 205/83, 205/67, 738/66, 436518-535, 148/518, 204/193, 204/412
• US Class Current: 324/71.1
• CPC Class Codes: B01J 19/0046 Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays synthesis methods per se C40B50/00
• CPC Class Codes: B01J 2219/00286 Reactor vessels with top and bottom openings
• CPC Class Codes: B01J 2219/00527 Sheets
• CPC Class Codes: B01J 2219/00533 essentially rectangular
• CPC Class Codes: B01J 2219/00585 Parallel processes
• CPC Class Codes: B01J 2219/0059 Sequential processes
• CPC Class Codes: B01J 2219/00596 Solid-phase processes
• CPC Class Codes: B01J 2219/00605 the compounds being directly bound or immobilised to solid supports
• CPC Class Codes: B01J 2219/00612 the surface being inorganic
• CPC Class Codes: B01J 2219/00614 Delimitation of the attachment areas
• CPC Class Codes: B01J 2219/0063 Other, e.g. van der Waals forces, hydrogen bonding
• CPC Class Codes: B01J 2219/00637 by coating it with another layer
• CPC Class Codes: B01J 2219/00653 the compounds being bound to electrodes embedded in or on the solid supports
• CPC Class Codes: B01J 2219/00659 Two-dimensional arrays
• CPC Class Codes: B01J 2219/00675 In-situ synthesis on the substrate
• CPC Class Codes: B01J 2219/00702 Processes involving means for analysing and characterising the products
• CPC Class Codes: B01J 2219/00713 Electrochemical synthesis
• CPC Class Codes: B01J 2219/00745 Inorganic compounds
• CPC Class Codes: B01J 2219/00747 Catalysts
• CPC Class Codes: B01J 2219/00752 Alloys
• CPC Class Codes: B01J 2219/00754 : Metal oxides
• CPC Class Codes: B01J 2219/00756 : Compositions, e.g. coatings, crystals, formulations
• CPC Class Codes: B82Y 30/00 : Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C40B 30/08 : by measuring catalytic activity
• CPC Class Codes: C40B 40/18 : Libraries containing only inorganic compounds or inorganic materials
• CPC Class Codes: C40B 50/14 : Solid phase synthesis, i.e. wherein one or more library building blocks are bound to a solid support during library creation; Particular methods of cleavage from the solid support
• CPC Class Codes: C40B 60/14 : for creating libraries
• CPC Class Codes: G01N 27/403 : Cells and electrode assemblies
• CPC Class Codes: H01M 4/921 : Alloys or mixtures with metallic elements
• CPC Class Codes: Y02E 60/50 : Fuel cells

Abstract

Methods and apparatus employ the use of arrays (301, 902) of two or more electronically-discrete electrodes (1, 2, 3 . . . ) to facilitate high-throughput preparation and testing of materials comprising two or more elements. High rates of deposition, synthesis and/or analysis of materials are achieved with the use of arrays of electrodes whereby desired materials are developed. The high rate synthesis and/or analysis of an array of materials uses deposition control techniques in conjunction with the electrode array to develop a meaningful array of materials and to analyze the materials for desired characteristics to develop one or more materials with desired characteristics. The use of an array of electrodes enables high-throughput development of materials having scientific and economic advantages.

Claims

1. An apparatus for rapidly applying at least one component of each of at least two materials to addressable predefined locations on an array of electrodes, the apparatus comprising:

at least two electrodes contained in said array; and

an assembly for applying an electrical potential or current from a power source to each of the electrodes, wherein the electrodes are addressable through the assembly, and wherein said at least one component of said each of said materials is operatively supplied to the array of electrodes, said electrical potential or current causing the components of the materials to deposit at said addressable predefined location, wherein the deposition is controllable.

2. The apparatus of claim 1, wherein said electrodes are the addressable predefined locations and wherein the depositings are controllable.

3. The apparatus of claim 2, wherein the assembly includes a controller to control the electrical potential or current for each said electrode.

4. The apparatus of claim 3, wherein the electrode array includes at least twenty said electrodes.

5. The apparatus of claim 4, wherein the electrode array includes at least one hundred said electrodes.

6. The apparatus of claim 5, wherein the electrode array includes at least ten thousand said electrodes.

7. The apparatus of claim 5, wherein said assembly includes a reference electrode.

8. The apparatus of claim 7, wherein the reference electrode is movable to operatively adjust depositions.

9. The apparatus of claim 5, wherein said assembly includes a counter electrode.

10. The apparatus of claim 9, wherein the counter electrode is movable to operatively adjust depositions.

11. The apparatus of claim 5, wherein the array of electrodes includes a highly resistive substrate below said electrodes, a highly conductive material above said highly resistive substrate and around said electrodes, and a second highly resistive material above said highly conductive material and around said electrodes wherein the second highly resistive material does not cover the electrodes.

12. The apparatus of claim 11, wherein the array of electrodes is a microelectrode array.

13. The apparatus of claim 12, wherein the electrodes are at most 1 mm in diameter.

14. The apparatus of claim 13, wherein the electrodes are at most 100 μ

m in diameter.

15. The apparatus of claim 5, wherein said at least one component of said each of at least two materials is entrained in a solution when operatively supplied to said assembly.

16. The apparatus of claim 15, wherein at least one of said at least one component is a kinetically sluggish precursor.

17. The apparatus of claim 15, wherein said solution includes at least two passivating agents.

18. The apparatus of claim 5, wherein the assembly includes a flow cell, whereby the at least one component of said each of the two at least two materials is supplied to the array of said electrodes in varying concentrations of said components.

19. A method of rapidly applying at least one component of each of at least two materials to addressable predefined locations on an array of electrodes, comprising:

applying a potential to at least one first electrode on said array of electrodes;

depositing at least said at least one component of each of the at least two materials onto said at least one first electrode;

applying a second potential to at least one second electrode on said array of electrodes;

depositing at least said at least one component of each of the at least two materials onto said at least one second electrode, said depositing being controllable

wherein said at least one component of each of the at least two materials deposited on the at least one second electrode varies in composition from the at least one component of each of the at least two materials deposited on the at least one first electrode.

20. A method of rapidly applying at least one respective component of each of at least two materials to addressable predefined locations on an array of electrodes, comprising:

varying concentrations of the components over time;

applying a potential to at least one first electrode on said array of electrodes;

depositing at least the components onto said at least one first electrode to form a respective deposit on each of said at least one first electrode;

applying a second potential to at least one second electrode on said array of electrodes;

depositing at least said components onto said at least one second electrode to form a respective deposit on each of said at least one second electrode,

wherein said components deposited on the at least one second electrode vary in composition from the components deposited on the at least one first electrode, and wherein the depositings are controllable.

21. The method of claim 20, wherein said components are supplied by a flow cell.

22. The method of claim 21, wherein said applying include adjusting the potential to operatively supply an overpotential at said at least one electrode whereby the depositing of said components leads to uniform morphologies at each said at least one electrode.

23. The method of claim 21, wherein said applying include controlling the potential at each said at least one electrode by pulse electrode position whereby a depositing potential is applied followed by a resting potential in cycles until said each at least one electrode is deposited with said respective composition.

24. The method of claim 21, wherein said applying include applying a second potential to the other electrodes in the array whereby the electrodes not being supplied a depositing potential are supplied a holding potential to prevent exchange reactions.

25. The method of claim 21, wherein said components are kinetically sluggish precursors.

26. The method of claim 21, wherein said varying includes moving a reference or counter electrode.

27. The method of claim 21, wherein said applying and said depositing step is repeated one thousand times in rapid sequence whereby at least one thousand different compositions are deposited onto the array of electrodes.

28. The method of claim 20, wherein said depositing include controlling the morphology of each of said deposits.