Methods for identifying and optimizing materials in microfluidic systems

• US 6,737,026 B1
• Filed: 11/28/2000
• Issued: 05/18/2004
• Est. Priority Date: 03/03/1999
• Status: Expired due to Fees

• Current Assignee: Freeslate Inc. (Unchained Labs Inc.)
• Original Assignee: Symyx Technologies Incorporated (Dassault Systemes SA)
• Inventors: Guan, Shenheng, Bergh, H. Sam
• Primary Examiner(s): Warden, Jill
• Assistant Examiner(s): Quan, Elizabeth
• Application Number:
  US09/728,209
• Time in Patent Office: 1,267 Days
• Field of Search: 422/99-104, 422/129-131, 436/37
• US Class Current: 422/130
• CPC Class Codes: B01F 25/41 Mixers of the fractal type
• CPC Class Codes: B01F 35/7182 with means for feeding the material with a fractal or tree-type distribution in a surface
• 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 19/0093 Microreactors, e.g. miniaturised or microfabricated reactors laboratory containers with capillary fluid transport in microfabricated channels or chambers B01L3/5027
• CPC Class Codes: B01J 2219/00286 Reactor vessels with top and bottom openings
• CPC Class Codes: B01J 2219/00306 Reactor vessels in a multiple arrangement
• CPC Class Codes: B01J 2219/00308 interchangeably mounted in racks or blocks
• CPC Class Codes: B01J 2219/00313 the reactor vessels being formed by arrays of wells in blocks
• CPC Class Codes: B01J 2219/00317 Microwell devices, i.e. having large numbers of wells
• CPC Class Codes: B01J 2219/00337 Valves
• CPC Class Codes: B01J 2219/00351 Means for dispensing and evacuation of reagents
• CPC Class Codes: B01J 2219/00353 Pumps
• CPC Class Codes: B01J 2219/00389 Feeding through valves
• CPC Class Codes: B01J 2219/00418 using pressure
• CPC Class Codes: B01J 2219/00452 Means for the recovery of reactants or products
• CPC Class Codes: B01J 2219/00479 Means for mixing reactants or products in the reaction vessels
• CPC Class Codes: B01J 2219/00495 Means for heating or cooling the reaction vessels
• CPC Class Codes: B01J 2219/00585 Parallel 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 2219/00635 : by reactive plasma treatment
• 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 2219/00657 : One-dimensional arrays
• CPC Class Codes: B01J 2219/00659 : Two-dimensional arrays
• CPC Class Codes: B01J 2219/00704 : integrated with the reactor apparatus
• CPC Class Codes: B01J 2219/00707 : separated from the reactor apparatus
• CPC Class Codes: B01J 2219/0072 : Organic compounds
• CPC Class Codes: B01J 2219/00745 : Inorganic compounds
• CPC Class Codes: B01J 2219/00747 : Catalysts
• CPC Class Codes: B01J 2219/00759 : Purification of compounds synthesised
• CPC Class Codes: B01L 2200/0689 : Sealing
• CPC Class Codes: B01L 2200/146 : Employing pressure sensors
• CPC Class Codes: B01L 2300/0864 : comprising only one inlet and multiple receiving wells, e.g. for separation, splitting
• CPC Class Codes: B01L 2300/0874 : Three dimensional network
• CPC Class Codes: B01L 2300/0887 : Laminated structure
• CPC Class Codes: B01L 2300/14 : Means for pressure control
• CPC Class Codes: B01L 2300/18 : Means for temperature control
• CPC Class Codes: B01L 2400/0487 : fluid pressure, pneumatics
• CPC Class Codes: B01L 3/5025 : for parallel transport of multiple samples
• CPC Class Codes: B01L 3/5027 : by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip B01L3/5023 takes precedence; micromixers B01F33/30; microreactors for synthesis B01J19/0093; microcapillary devices in general B81B1/00
• CPC Class Codes: B01L 3/502707 : characterised by the manufacture of the container or its components by shaping or joining plastic parts B29C59/00, B29C65/00; by laminating B32B37/00; manufacture of microstructural devices in general B81C
• CPC Class Codes: B01L 3/502715 : characterised by interfacing components, e.g. fluidic, electrical, optical or mechanical interfaces
• CPC Class Codes: B01L 7/54 : using spatial temperature gradients
• CPC Class Codes: C01B 3/40 : characterised by the catalyst
• CPC Class Codes: C07C 17/23 : by dehalogenation
• CPC Class Codes: C07C 45/34 : in unsaturated compounds
• CPC Class Codes: C07C 45/35 : in propene or isobutene
• CPC Class Codes: C07C 45/38 : being a primary hydroxyl group
• CPC Class Codes: C07C 45/46 : Friedel-Crafts reactions
• CPC Class Codes: C07C 45/54 : of compounds containing doubly bound oxygen atoms, e.g. esters
• CPC Class Codes: C07C 45/72 : by reaction of compounds containing >C = O groups with the same or other compounds containing >C = O groups
• CPC Class Codes: C07C 47/04 : Formaldehyde
• CPC Class Codes: C07C 47/06 : Acetaldehyde
• CPC Class Codes: C07C 47/127 : Glyoxal
• CPC Class Codes: C07C 47/22 : Acryaldehyde; Methacryaldehyde
• CPC Class Codes: C07C 49/403 : of a six-membered ring
• 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 2035/00158 : Elements containing microarrays, i.e. "biochip"
• CPC Class Codes: G01N 30/466 : with separation columns in parallel
• CPC Class Codes: G01N 30/90 : Plate chromatography, e.g. thin layer or paper chromatography
• CPC Class Codes: G01N 31/10 : using catalysis
• CPC Class Codes: G01N 35/028 : having reaction cells in the form of microtitration plates
• CPC Class Codes: Y10T 137/87885 : Sectional block structure
• CPC Class Codes: Y10T 436/117497 : with a continuously flowing sample or carrier stream
• CPC Class Codes: Y10T 436/118339 : with formation of a segmented stream
• CPC Class Codes: Y10T 436/2575 : Volumetric liquid transfer

Abstract

A chemical processing microsystem useful for identifying and optimizing materials (e.g., catalysts) that enhance chemical processes or for characterizing and/or optimizing chemical processes is disclosed. The chemical processing microsystem comprises a plurality of microreactors 600 and, in a preferred embodiment, a plurality of microseparators 900 integral with the chemical processing microsystem 10. The microreactors 600 are preferably diffusion-mixed microreactors formed in a plurality of laminae that include a modular, interchangeable candidate-material array 100. The material array 100 comprises a plurality of different candidate materials (e.g., catalysts), preferably arranged at separate, individually addressable portions of a substrate (e.g., wafer). The microseparators 900 are similarly formed in a plurality of laminae that include a modular, interchangeable adsorbent array 700. The adsorbent array 700 comprises one or more adsorbents, preferably arranged at separate, individually addressable portions of a substrate to spatially correspond to the plurality of different candidate materials. Modular microfluidic distribution systems are also disclosed. The chemical processing microsystem can be integrated into a material evaluation system that enables a comprehensive combinatorial material science research program.

Claims

1. A chemical processing microsystem comprising

four or more microcomponents formed in a plurality of adjacent laminae, each of the four or more microcomponents comprising a surface defining a cavity having a volume of not more than about 3 ml for carrying out a chemical process of interest, an inlet port in fluid communication with the cavity, and optionally an outlet port in fluid communication with the cavity, and

a microfluidic distribution system for supplying one or more fluids from one or more external fluid sources to the inlet port of each of the four or more microcomponents and optionally for discharging an effluent from the outlet port of each of the four or more microcomponents to one or more external effluent sinks,

at least one of the plurality of laminae being a material-containing laminate that forms a portion of the cavity-defining surface of the four or more microcomponents, the material-containing laminate comprising a substrate for containing at least four materials arranged on the substrate such that they are individually resident in the cavities of the four or more microcomponents, the material-containing laminate having an essential absence of fluid distribution components, the four or more microcomponents being accessible for loading the material-containing laminate prior to carrying out the chemical process of interest, and for unloading the material containing laminate after the chemical process of interest.

2. The chemical processing microsystem of claim 1 further comprising a releasable seal between the material-containing laminate and one or more adjacent laminae in which the microcomponents are formed.

3. The chemical processing microsystem of claim 2 adapted for chemical process conditions that include a temperature above about 100°

C.

4. The chemical processing microsystem of claim 1 wherein the microfluidic distribution system is adapted for simultaneously supplying the one or more fluids from the one or more sources to the inlet port of each of the microcomponents.

5. The chemical processing microsystem of claim 1 wherein the microfluidic distribution system comprises a microfluidic fluid-supply manifold formed in a plurality of adjacent laminae.

6. The chemical processing microsystem of claim 5 wherein the microfluidic fluid-supply manifold is adapted for simultaneously supplying the one or more fluids from the one or more sources to the inlet port of each of the microcomponents.

7. The chemical processing microsystem of claim 5 wherein the microfluidic fluid-supply manifold is formed in a plurality of adjacent laminae comprising at least one laminate separate from the plurality of adjacent laminae in which the microcomponents are formed.

8. The chemical processing microsystem of claim 5 wherein the microfluidic fluid-supply manifold comprises a common port adaptable for fluid communication with the one or more sources, four or more terminal ports adapted for fluid delivery to the four or more microcomponents, and a distribution channel providing fluid communication between the common port and each of the four or more terminal ports, the flow paths defined between the common port and each microcomponent having substantially equal conductance.

9. The chemical processing microsystem of claim 5 wherein the microfluidic fluid-supply manifold comprises a common port adaptable for fluid communication with one or more sources, four or more terminal ports adapted for fluid delivery to the four or more microcomponents, and a distribution channel providing fluid communication between the common port and each of the four or more terminal ports, the distribution channels being adapted such that the pressure drop in each of the fluid distribution channels is larger than the pressure drop in its associated microcomponent.

10. The chemical processing microsystem of claim 5 wherein the plurality of adjacent laminae in which the four or more microcomponents are formed define a microcomponent structure, and the microfluidic fluid distribution manifold is releasably sealed with the microreactor structure, such that the manifold can be modularly interchanged with another microfluidic fluid distribution manifold.

11. The chemical processing microsystem of claim 5 wherein

ten or more microcomponents are formed in the plurality of adjacent laminae to define a microcomponent structure, and

the microfluidic fluid-supply manifold formed in a plurality of adjacent laminae is in sealed contact with the microcomponent structure and comprises one or more common ports adaptable for fluid communication with one or more fluid sources or one or more effluent sinks, ten or more terminal ports adaptable for fluid delivery to or fluid recovery from the ten or more microcomponents, and a distribution channel providing fluid communication between the one or more common ports and each of the ten or more terminal ports, the ratio of the number of terminal ports to the number of common ports being not less than about 10:

1.

12. The chemical processing microsystem of claim 1 wherein the cavity of the microcomponents has a volume of not more than about 100 μ

l and a geometry defined by ratios of distances X, Y, and Z measured within the cavity along three mutually orthogonal lines having a common point of intersection at midpoint of the longest line, Z, the X;

Z and Y;

Z ratios each ranging from about 1;

2 to about 1;

1.

13. The chemical processing microsystem of claim 1 wherein the volume of at least two of the four or more microcomponents is different.

14. The chemical processing microsystem of claim 1 wherein the four or more microcomponents are arranged in a substantially planar array and having a planar density of not less than about 5 microcomponents/cm².

15. The chemical processing microsystem of claim 1 wherein the material-containing laminate further comprises at least four candidate materials so that the candidate materials are individually resident in the cavity of separate microcomponents, each of the at least four candidate materials comprising an inorganic material, a metal-ligand or a non-biological organic material.

16. The chemical processing microsystem of claim 15 wherein

the microcomponent structure comprises two-hundred-fifty or more microcomponents, the microfluidic fluid distribution system comprises a microfluidic fluid-supply manifold formed in a plurality of laminae.

17. The chemical processing microsystem of claim 1 wherein the material-containing laminate further comprises at least four candidate materials so that the candidate materials are individually resident in the cavity of separate microcomponents, the at least four candidate materials being adsorbents that are selective for a particular species for enhancing the separation of the species from a mixture including the species.

18. The chemical processing microsystem of claim 1 wherein each of the four or more microcomponents further comprises an outlet port in fluid communication with the cavity, and the microfluidic distribution system is adapted for discharging an effluent from the outlet port of each of the four or more microcomponents to one or more external effluent sinks.

19. The chemical processing microsystem of claim 18 wherein the microfluidic fluid distribution system comprises a microfluidic effluent-distribution manifold for discharging the reactor effluent from the outlet port of each of the four or more microcomponents to one or more effluent sinks.

20. The chemical processing microsystem of claim 19 wherein the microfluidic effluent-distribution manifold is formed in a plurality of adjacent laminae.

21. The chemical processing microsystem of claim 18 wherein the microfluidic effluent-distribution manifold is adapted for simultaneously discharging the reactor effluent from the outlet port of each of the four or more microcomponents to one or more effluent sinks.

22. A chemical processing microsystem comprising

ten or more microcomponents formed in a plurality of adjacent laminae, each of the ten or more microcomponents comprising a surface defining a cavity for carrying out a chemical process of interest, an inlet port in fluid communication with the cavity, and an outlet port in fluid communication with the cavity, and

a microfluidic distribution system comprising a microfluidic fluid-supply for simultaneously supplying one or more fluids from one or more external fluid sources to the inlet port of each of the ten or more microcomponents and a microfluidic effluent-disfribution for simultaneously discharging an effluent from the outlet port of each of the ten or more microcomponents to one or more external effluent sinks,

at least one of the plurality of laminae being a material-containing laminate that forms a portion of the cavity-defining surface of the ten or more microcomponents, the material-containing laminate comprising a substrate for containing at least ten materials arranged on the substrate such that they are individually resident in the cavities of the ten or more microcomponents, the material-containing laminate having an essential absence of fluid distribution components, and

a releasable seal between the material-containing laminate and one or more adjacent laminae in which the microcomponents are formed, so that the ten or more microcomponents are accessible for loading the material-containing laminate prior to carrying out the chemical process of interest, and for unloading the material containing laminate after the chemical process of interest.

23. The chemical processing microsystem of claim 22 adapted for chemical process conditions that include a temperature above about 200°

C.

24. A chemical processing microsystem comprising

ten or more microcomponents formed in a plurality of adjacent laminae, each of the ten or more microcomponents comprising a surface defining a cavity for carrying out a chemical process of interest, an inlet port in fluid communication with the cavity, and an outlet port in fluid communication with the cavity, and

a microfluidic distribution system comprising a microfluidic fluid-supply for simultaneously supplying one or more fluids from one or more external fluid sources to the inlet port of each of the ten or more microcomponents and a microfluidic effluent-distribution for simultaneously discharging an effluent from the outlet port of each of the ten or more microcomponents to one or more external effluent sinks,

at least one of the plurality of laminae being a material-containing laminate that forms a portion of the cavity-defining surface of the ten or more microcomponents, the material-containing laminate comprising a substrate for containing at least ten materials arranged on the substrate such that they are individually resident in the cavities of the ten or more microcomponents, and

a releasable seal between the material-containing laminate and one or more adjacent laminae in which the microcomponents are formed, so that the ten or more microcomponents are accessible for loading the material-containing laminate prior to carrying out the chemical process of interest, and for unloading the material containing laminate after the chemical process of interest,

the chemical processing microsystem being adapted for chemical process conditions that include a temperature above about 200°

C.