Sensor array for rapid materials characterization

• US 20020032531A1
• Filed: 05/23/2001
• Published: 03/14/2002
• Est. Priority Date: 12/11/1998
• Status: Active Grant

• Current Assignee: Freeslate Inc. (Unchained Labs Inc.)
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Bennett, James, Mansky, Paul
• Granted Patent: US 6,535,822 B2
• Time in Patent Office: Days
• US Class Current: 702/21
• 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 2219/00605 the compounds being directly bound or immobilised to solid supports
• CPC Class Codes: B01J 2219/00612 the surface being inorganic
• CPC Class Codes: B01J 2219/00621 by physical means, e.g. trenches, raised areas
• 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 2219/00707 separated from the reactor apparatus
• CPC Class Codes: B01J 2219/00745 Inorganic compounds
• CPC Class Codes: B01J 2219/00747 Catalysts
• 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: G01N 25/005 by investigating specific heat
• CPC Class Codes: G01N 25/18 by investigating thermal conductivity by calorimetry G01N25/20; by measuring change of resistance of an electrically-heated body G01N27/18
• CPC Class Codes: G01N 27/72 by investigating magnetic variables

Abstract

A sensor-array based materials characterization apparatus includes a sensor array disposed on a substrate; electronic test circuitry for sending electrical signals to and receiving electrical signals from the sensor array; electronic circuitry for routing signals between selected sensors and the electronic test circuitry; and a computer or processor. All or part of the electronic test and signal routing circuitry is contained on the same substrate as the sensor array, comprising an integrated apparatus disposed on a substrate. Additional circuitry and a processor or computer may be physically separate from the substrate carrying the sensor array, and connected to the sensor array substrate by a standardized interconnection method. The method of using the apparatus comprises applying multiple samples to the multiple sensors in the array, and sending and receiving signals to and from selected sensors, where the signals correspond to the material properties of samples in contact with the sensors. The sensor array is preferably arranged in a standardized format used in combinatorial applications for rapid deposition of sample materials on the sensor array. By integrating the electronic test and signal routing circuitry onto the same substrate as the sensor array, a high density of sensors can be situated on a single substrate, permitting the rapid analysis of libraries containing thousands of material samples or more.

Claims

1. An apparatus for characterizing one or more material properties for each of 5 or more samples, comprising:

a substrate;

5 or more sensors disposed on said substrate to form a sensor array, wherein each sensor is associated with one of said 5 or more samples and characterizes at least one material property of its associated sample; and

means for coupling said sensor array with electronic circuitry that sends signals to and receives signals from said plurality of sensors, wherein said signals received from said sensors correspond with at least one material property.

2. The apparatus of claim 1, further comprising a multiplexer disposed on said substrate for selectively coupling a sensor or a group of sensors in said sensor array to an electronic platform.

3. The apparatus of claim 1, further comprising electronic test circuitry disposed on said substrate that communicates with the electronic device and generates data corresponding with the material property.

4. The apparatus of claim 2, further comprising electronic test circuitry disposed on said substrate that communicates with the electronic device via said multiplexer and generates data corresponding with the material property.

5. The apparatus of claim 3 or 4, wherein the electronic test circuitry receives and collects data from said sensor array, and wherein the apparatus further includes a computer or processor including software that controls data collection, data viewing, and user interface between the sensor array and the electronic device.

6. The apparatus of claim 1, 2, 3 or 4, wherein the property characterized by said sensors in said sensor array is a thermal property.

7. The apparatus of claim 6, wherein the thermal property characterized by said sensor array is at least one selected from the group consisting of heat capacity, specific heat, thermal conductivity, and thermal stability.

8. The apparatus of claim 6, wherein each sensor in said sensor array comprises:

a microthin film membrane supported by said substrate such that said sensor array is an array of microthin film windows; and

a heater/thermometer pattern disposed on said microthin film membrane.

9. The apparatus of claim 8, wherein said microthin film membrane forming said sensors is a silicon nitride membrane, and wherein said substrate supporting said silicon nitride membranes in said sensor array is a silicon wafer.

10. The apparatus of claim 6, wherein each sensor in said sensor array comprises:

a microthin film membrane supported by said substrate such that said sensor array is an array of microthin film windows;

a first wire disposed on said microthin film membrane, said first wire acting as a heater and a first thermometer; and

a second wire spaced apart from said first wire and disposed on said substrate, said second wire acting as a second thermometer.

11. The apparatus of claim 10, wherein said microthin film membrane forming said sensors is a silicon nitride membrane, and wherein said substrate supporting said silicon nitride membranes in said sensor array is a silicon wafer.

12. The apparatus of claim 11, wherein said substrate is made of a polymer sheet, and wherein said sensor array includes a plurality of heater/thermometers disposed on said polymer sheet.

13. The apparatus of claim 12, wherein said polymer sheet is a polyimide.

14. The apparatus of claim 12, wherein said heater/thermometer is printed on said polymer sheet via lithography.

15. The apparatus of claim 6, wherein said substrate is made of a glass plate, and wherein said sensor array includes a plurality of heater/thermometers disposed on said glass plate.

16. The apparatus of claim 15, wherein said heater/thermometer is printed on said glass plate via lithography.

17. The apparatus of claim 11, wherein said sensor array includes a plurality of thermometers disposed on a top surface of said substrate, and wherein said substrate includes a large area heater disposed on a bottom surface of said substrate.

18. The apparatus of claim 8, wherein said substrate is made of a polymer sheet.

19. The apparatus of claim 6, wherein said substrate is made from a material having poor thermal conductivity and is placed on a heater block, and wherein said sensor array includes a plurality of temperature sensors disposed on the substrate such that a temperature difference between a first portion and a second portion of the substrate can be determined.

20. The apparatus of claim 19, wherein said substrate is a glass plate.

21. The apparatus of claim 6, wherein at least one sensor in said sensor array comprises:

a sample support having a thermal measurement pattern disposed thereon;

a gap between said sample support and said substrate for thermally isolating said sample support from said substrate; and

a plurality of bridges connecting said sample support to said substrate over said gap.

22. The apparatus of claim 1, 2, 3 or 4, wherein the property characterized by said sensor array is a dielectric constant.

23. The apparatus of claim 22, wherein each sensor in said sensor array comprises interdigitated electrodes disposed on said substrate.

24. The apparatus of claim 22, wherein each sensor in said sensor array further comprises a thermometer such that each sensor can conduct a dielectric constant measurement and a thermal measurement simultaneously.

25. The apparatus of claim 1, 2, 3 or 4, wherein the property characterized by said sensor array is an electrical transport property.

26. The apparatus of claim 25, wherein the electrical transport property characterized by said sensor array is at least one selected from the group of electrical resistance, Hall coefficient, magnetoresistance, current-voltage characteristics and thermoelectric power.

27. The apparatus of claim 25, wherein each sensor on the sensor array comprises a plurality of electrical leads disposed on the substrate, said leads on each sensor contacting a plurality of locations on said material sample.

28. The apparatus of claim 27, wherein said leads are deposited on said substrate, and wherein said material samples in said materials library are deposited on top of said leads.

29. The apparatus of claim 27, wherein said material samples in said materials library are deposited on said substrate, and wherein said leads are deposited on top of said samples.

30. The apparatus of claim 25, further comprising means for generating a magnetic field pointing perpendicular to said substrate.

31. The apparatus of claim 30, wherein said generating means comprises a magnet that generates a magnetic field over the entire sensor array.

32. The apparatus of claim 30, wherein said generating means comprises a magnet array having a plurality of magnets arranged in the same format as said plurality of sensors in said sensor array, wherein each magnet in said magnet array corresponds with a sensor in said sensor array to generate a magnetic field over the corresponding sensor.

33. The apparatus of claim 25, further comprising means for imposing a temperature gradient across said samples in said sensor array.

34. The apparatus of claim 25, wherein said sensors in said sensor array measure temperature, and wherein said apparatus further comprises a plurality of temperature controlled elements to impose a temperature gradient across at least one of said samples in said sensor array.

35. The apparatus of claim 1, 2, 3 or 4, wherein the property characterized by said sensors in said sensor array is at least one selected from the group consisting of viscosity, density, conductivity, molecular weight, chemical concentration, capacitance, dielectric constant, mass loading, elasticity, damping, tensile strength, yield strength, ductility, toughness, hardness and magnetism.

36. The apparatus of claim 35, wherein said sensors are at least one selected from the group consisting of resonators, oscillators, and actuators.

37. The apparatus of claim 35, wherein each sensor in said sensor array comprises interdigitated electrodes disposed on said substrate.

38. The apparatus of claim 35, wherein each sensor in said sensor array comprises:

a mechanical resonator formed on said substrate; and

a piezoelectric material deposited on top of said sensor to form an acoustic wave sensing electrode.

39. The apparatus of claim 38, wherein said acoustic wave sensing electrode is operable in at least one of a surface acoustic wave resonance mode, a thickness shear mode, and a flexural plate wave resonance mode.

40. The apparatus of claim 38, wherein said acoustic wave sensing electrode acts as both a mechanical resonator and a materials characterization device.

41. The apparatus of claim 1, 2, 3 or 4, wherein said sensor array can characterize at least two material properties on the same array.

42. The apparatus of claim 41, wherein said sensor array includes at least a first sensor for characterizing a first material property and a second sensor for characterizing a second material property.

43. The apparatus of claim 41, wherein each sensor in said sensor array characterizes more than one material property.

44. The apparatus of claim 1, 2, 3 or 4, wherein said 5 or more sensors in said sensor array are arranged in a format compatible with combinatorial chemistry instrumentation.

45. The apparatus of claim 44, wherein said sensor array is an 8×

8 array with a 0.25 pitch.

46. The apparatus of claim 44, wherein said sensor array is an 8×

12 array with a 9 mm pitch.

47. The apparatus of claim 44, wherein said sensor array is a 16×

24 array.

48. The apparatus of claim 44, wherein said sensors in said sensor array are disposed on said substrate in a planar arrangement.

49. The apparatus of claim 44, wherein said sensors in said sensor array are attached to said substrate via a plurality of sensor plates disposed in an array format and extending generally perpendicularly from said substrate such that said plurality of sensors can be dipped into a plurality of wells having the same format as said sensor array simultaneously.

50. The apparatus of claim 1, 2, 3 or 4, wherein said plurality of sensors in said sensor array are arranged in a geometric shape.

51. The apparatus of claim 50, wherein said geometric shape is a closed shape having straight sides.

52. The apparatus of claim 50, wherein said geometric shape is a closed shape having curved sides.

53. The apparatus of claim 50, wherein said geometric shape is a closed shape having both straight and curved sides.

54. The apparatus of claim 50, wherein said geometric shape is an open shape having straight sides.

55. The apparatus of claim 50, wherein said geometric shape is an open shape having curved sides.

56. The apparatus of claim 50, wherein said geometric shape is an open shape having both straight and curved sides.

57. The apparatus of claim 50, wherein said sensor array contains at least 48 sensors.

58. The apparatus of claim 50, wherein said sensor array contains at least 96 sensors.

59. The apparatus of claim 50, wherein said sensor array contains at least 128 sensors.

60. The apparatus of claim 50, wherein said sensor array contains between 5 and 400 sensors.

61. The apparatus of claim 1, 2, 3 or 4, further comprising a plurality of contact pads associated with each sensor on said sensor array, wherein each contact pad is disposed next to its associated sensor.

62. The apparatus of claim 1, 2, 3 or 4, further comprising a plurality of contact pads associated with each sensor on said sensor array, wherein each contact pad is disposed at an edge of said sensor array.