Optical systems and methods for rapid screening of libraries of different materials

• US 6,373,570 B1
• Filed: 12/29/1999
• Issued: 04/16/2002
• Est. Priority Date: 10/09/1996
• Status: Expired due to Fees

• Current Assignee: Freeslate Inc. (Unchained Labs Inc.)
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: McFarland, Eric W., Danielson, Earl, Archibald, William
• Primary Examiner(s): Font, Frank G.
• Assistant Examiner(s): Punnoose, Roy M.
• Application Number:
  US09/474,344
• Time in Patent Office: 839 Days
• Field of Search: 356/364, 356/369, 356/370, 356/382, 356/368, 324/223, 324/212, 324/96
• US Class Current: 506/11
• 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 2219/00315 Microtiter plates
• CPC Class Codes: B01J 2219/00317 Microwell devices, i.e. having large numbers of wells
• CPC Class Codes: B01J 2219/00364 Pipettes
• CPC Class Codes: B01J 2219/00378 Piezoelectric or ink jet dispensers
• CPC Class Codes: B01J 2219/0043 for direct application of reagents, e.g. through openings in a shutter
• CPC Class Codes: B01J 2219/00443 Thin film deposition
• CPC Class Codes: B01J 2219/00497 Features relating to the solid phase supports
• CPC Class Codes: B01J 2219/005 Beads
• CPC Class Codes: B01J 2219/00511 Walls of reactor vessels
• CPC Class Codes: B01J 2219/00515 in the shape of strings
• CPC Class Codes: B01J 2219/0052 in the shape of elongated tubes
• CPC Class Codes: B01J 2219/00527 Sheets
• CPC Class Codes: B01J 2219/00536 in the shape of disks
• CPC Class Codes: B01J 2219/00583 Features relative to the processes being carried out
• 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 2219/0061 The surface being organic
• 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 2219/00626 : Covalent
• CPC Class Codes: B01J 2219/00628 : Ionic
• CPC Class Codes: B01J 2219/00637 : by coating it with another layer
• CPC Class Codes: B01J 2219/00641 : the porous medium being continuous, e.g. porous oxide substrates
• 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 2219/00689 : using computers
• CPC Class Codes: B01J 2219/00702 : Processes involving means for analysing and characterising the products
• CPC Class Codes: B01J 2219/00704 : integrated with the reactor apparatus
• CPC Class Codes: B01J 2219/00722 : Nucleotides
• CPC Class Codes: B01J 2219/00738 : Organic catalysts
• CPC Class Codes: B01J 2219/00745 : Inorganic compounds
• CPC Class Codes: B01J 2219/00747 : Catalysts
• CPC Class Codes: B01J 2219/0075 : Metal based compounds
• CPC Class Codes: B01J 2219/00754 : Metal oxides
• CPC Class Codes: B82Y 30/00 : Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C07F 15/0066 : without a metal-carbon linkage
• CPC Class Codes: C07F 15/045 : without a metal-carbon linkage
• CPC Class Codes: C40B 20/08 : Direct analysis of the library members per se by physical methods, e.g. spectroscopy
• CPC Class Codes: C40B 30/08 : by measuring catalytic activity
• CPC Class Codes: C40B 40/14 : Libraries containing macromolecular compounds and not covered by groups C40B40/06 - C40B40/12
• 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 60/12 : for screening libraries
• CPC Class Codes: C40B 60/14 : for creating libraries
• CPC Class Codes: G01H 13/00 : Measuring resonant frequency
• CPC Class Codes: G01J 4/00 : Measuring polarisation of light
• CPC Class Codes: G01N 11/16 : by measuring damping effect upon oscillatory body
• CPC Class Codes: G01N 2009/006 : vibrating tube, tuning fork
• CPC Class Codes: G01N 21/211 : Ellipsometry optical thickness measurement G01B11/06
• CPC Class Codes: G01N 21/253 : for batch operation, i.e. multisample apparatus analytical automats G01N35/00
• CPC Class Codes: G01N 21/6402 : Atomic fluorescence; Laser induced fluorescence
• CPC Class Codes: G01N 21/6452 : Individual samples arranged in a regular 2D-array, e.g. multiwell plates
• CPC Class Codes: G01N 21/66 : electrically excited, e.g. electroluminescence
• CPC Class Codes: G01N 2203/0094 : Visco-elasticity
• CPC Class Codes: G01N 2291/014 : Resonance or resonant frequency
• CPC Class Codes: G01N 2291/0224 : Mixtures of three or more liquids
• CPC Class Codes: G01N 2291/0255 : (Bio)chemical reactions, e.g. on biosensors
• CPC Class Codes: G01N 2291/0256 : Adsorption, desorption, surface mass change, e.g. on biosensors
• CPC Class Codes: G01N 2291/02818 : Density, viscosity
• CPC Class Codes: G01N 2291/02827 : Elastic parameters, strength or force
• CPC Class Codes: G01N 2291/02863 : Electric or magnetic parameters
• CPC Class Codes: G01N 2291/0422 : Shear waves, transverse waves, horizontally polarised waves
• CPC Class Codes: G01N 2291/0423 : Surface waves, e.g. Rayleigh waves, Love waves
• CPC Class Codes: G01N 2291/0427 : Flexural waves, plate waves, e.g. Lamb waves, tuning fork, cantilever
• CPC Class Codes: G01N 2291/106 : one or more transducer arrays
• CPC Class Codes: G01N 25/4813 : concerning the measuring means
• CPC Class Codes: G01N 29/022 : Fluid sensors based on microsensors, e.g. quartz crystal-microbalance [QCM], surface acoustic wave [SAW] devices, tuning forks, cantilevers, flexural plate wave [FPW] devices microdevices per se B81B
• CPC Class Codes: G01N 29/036 : by measuring frequency or resonance of acoustic waves
• CPC Class Codes: G01N 29/2418 : using optoacoustic interaction with the material, e.g. laser radiation, photoacoustics photoacoustic cells G01N21/1702; measuring characteristics of vibrations by using radiation-sensitive means G01H9/00; acousto-optical conversion techniques for short-range imaging G01S15/8965; sound-producing devices using laser bundle G10K15/046
• CPC Class Codes: G01N 29/2425 : optoacoustic fluid cells therefor
• CPC Class Codes: G01N 29/30 : Arrangements for calibrating or comparing, e.g. with standard objects
• CPC Class Codes: G01N 29/348 : with frequency characteristics, e.g. single frequency signals, chirp signals measuring frequency of mechanical vibrations or acoustic waves in general G01H1/06, G01H3/04; measuring frequency or analysing frequency spectra G01R23/00
• CPC Class Codes: G01N 29/42 : by frequency filtering or by tuning to resonant frequency
• CPC Class Codes: G01N 29/4418 : with a model, e.g. best-fit, regression analysis
• CPC Class Codes: G01N 29/4427 : with stored values, e.g. threshold values
• CPC Class Codes: G01N 31/10 : using catalysis
• CPC Class Codes: G01N 9/002 : using variation of the resonant frequency of an element vibrating in contact with the material submitted to analysis G01N9/34 takes precedence
• CPC Class Codes: H01J 49/0409 : Sample holders or containers containers for retaining a material to be analyzed, B01L3/50, for DNA, C12Q1/6834, for biological materials, G01N33/543
• CPC Class Codes: H01J 49/0468 : with means for heating or cooling the sample

Abstract

Methods and apparatus for screening diverse arrays of materials are provided. In particular, techniques for rapidly characterizing compounds in arrays of materials in order to discover and/or optimize new materials with specific desired properties are provided. The substrate can be screened for materials having useful properties, and/or the resulting materials can be ranked, or otherwise compared, for relative performance with respect to useful properties or other characterizations. In particular, systems and methods are provided for screening a library of magnetic materials for their bulk magnetization, saturation magnetization, and coercivity by imaging their individual optical Kerr rotation, screening a library of dielectric materials for their dielectric coefficients by imaging their individual electro-optical rotation and screening a library of luminescent materials by imaging their individual luminescent properties under a variety of excitation conditions. Optical or visible luminescence systems are also provided as well as their application to screening libraries of different materials.

Claims

1. A method of characterizing a combinatorial array of materials for use in the identification of new materials, comprising the steps of:

providing a substrate, wherein said substrate is of a low thermal mass;

synthesizing a combinatorial array of diverse materials on said substrate;

depositing a liquid crystal layer onto said array of materials;

applying a voltage across said combinatorial array of materials;

illuminating said liquid crystal layer;

monitoring said illuminated liquid crystal layer with an image detector for detecting the same material characteristic of each member of said array;

comparing members of said array with respect to said material characteristic; and

identifying materials for large scale preparation that satisfy said material characteristic.

21. The method of claim 1, further comprising maintaining said liquid crystal layer near its liquid crystal phase transition temperature.

22. The method of claim 1 wherein said image detector is a CCD.

24. The method of claim 1 wherein said combinatorial array of materials includes a plurality of candidates for screening for catalytic activity.

25. The method of claim 1 further comprising preparing large scale amounts of a material identified in said identifying step.

27. The method of claim 1, wherein said comparing step includes ranking members of said array according to said material characteristic.

2. A system for characterizing a combinatorial array of materials for use in the identification of new materials, comprising:

a low thermal mass substrate, wherein an array of diverse materials is deposited on a plurality of predefined regions of said substrate said array including at least nine different materials;

a liquid crystal layer deposited onto said array of materials;

a voltage source coupled to said combinatorial array, said voltage source applying a voltage across said combinatorial array;

a light source, wherein said light source directs a beam of light at said liquid crystal layer;

a detection array source for monitoring a common material characteristic of said illuminated liquid crystal layer, and providing data about each member of said array for ranking of said members with respect to said material characteristic.

3. A method of characterizing a combinatorial array of materials for temperature heterogeneity for use in the identification of new materials, comprising the steps of:

providing a substrate having thereon a combinatorial array of diverse materials with a liquid crystal layer on said array;

illuminating said liquid crystal layer; and

monitoring said illuminated liquid crystal layer with a detector for indicating temperature heterogeneity of said array of materials; and

ranking members of said array with respect to said temperature heterogeneity; and

identifying materials for large scale preparation based upon said temperature heterogeneity ranking.

4. The method of claim 3 wherein said combinatorial array has at least 9 different materials.

5. The method of claim 3 wherein said combinatorial array has at least 50 different materials.

6. The method of claim 3 wherein said combinatorial array has at least 10³ different materials.

7. The method of claim 3 wherein said combinatorial array has at least 10⁴ different materials.

8. The method of claim 3 wherein said combinatorial array has at least 10⁵ different materials.

9. The method of claim 3 wherein said combinatorial array has at least 10⁶ different materials.

10. The method of claim 3 wherein said materials in said array have at least 3 components therein.

11. The method of claim 3 wherein said materials in said array have at least 4 components therein.

12. The method of claim 3 wherein said materials in said array have at least 5 components therein.

13. The method of claim 3 wherein said materials in said array have at least 6 components therein.

14. The method of claim 3 wherein said materials in said array have at least 7 components therein.

15. The method of claim 3 wherein said materials in said array have at least 8 components therein.

16. The method of claim 3 wherein said combinatorial array of materials includes a plurality of candidates for screening for catalytic activity.

17. The method of claim 4 wherein said array includes organic array elements.

18. The method of claim 4 wherein said array includes organometallic array elements.

19. The method of claim 4 wherein said array includes heterogeneous array elements.

20. The method of claim 4 wherein said catalyst libraries include solid state inorganic array elements.

23. The method of claim 3, further comprising contacting a surface of said substrate with a reactant gas stream.

26. The method of claim 3 further comprising preparing large scale amounts of a material identified in said identifying step.