CA2475906A1 - Tubular solid oxide fuel cell stack - Google Patents

Tubular solid oxide fuel cell stack Download PDF

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Publication number
CA2475906A1
CA2475906A1 CA002475906A CA2475906A CA2475906A1 CA 2475906 A1 CA2475906 A1 CA 2475906A1 CA 002475906 A CA002475906 A CA 002475906A CA 2475906 A CA2475906 A CA 2475906A CA 2475906 A1 CA2475906 A1 CA 2475906A1
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Prior art keywords
matrix
fuel cells
fuel cell
electrode layer
fuel
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CA002475906A
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French (fr)
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CA2475906C (en
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Hongsang Rho
Partho Sarkar
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Innotech Alberta Inc
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Individual
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/1286—Fuel cells applied on a support, e.g. miniature fuel cells deposited on silica supports
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
    • B01D63/02—Hollow fibre modules
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/12—Electroforming by electrophoresis
    • C25D1/14—Electroforming by electrophoresis of inorganic material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/02—Electrophoretic coating characterised by the process with inorganic material
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00—Electrophoretic coating characterised by the process
    • C25D13/12—Electrophoretic coating characterised by the process characterised by the article coated
    • C25D13/14—Tubes; Rings; Hollow bodies
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0232—Metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/023—Porous and characterised by the material
    • H01M8/0236—Glass; Ceramics; Cermets
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/06—Combination of fuel cells with means for production of reactants or for treatment of residues
    • H01M8/0606—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants
    • H01M8/0612—Combination of fuel cells with means for production of reactants or for treatment of residues with means for production of gaseous reactants from carbon-containing material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M8/1213—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material
    • H01M8/1226—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte characterised by the electrode/electrolyte combination or the supporting material characterised by the supporting layer
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H01M8/2404—Processes or apparatus for grouping fuel cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H01M8/241—Grouping of fuel cells, e.g. stacking of fuel cells with solid or matrix-supported electrolytes
    • H01M8/2425—High-temperature cells with solid electrolytes
    • H01M8/243—Grouping of unit cells of tubular or cylindrical configuration
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H01M8/2465—Details of groupings of fuel cells
    • H01M8/247—Arrangements for tightening a stack, for accommodation of a stack in a tank or for assembling different tanks
    • H01M8/2475—Enclosures, casings or containers of fuel cell stacks
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/24—Grouping of fuel cells, e.g. stacking of fuel cells
    • H01M8/2465—Details of groupings of fuel cells
    • H01M8/2484—Details of groupings of fuel cells characterised by external manifolds
    • H01M8/2485—Arrangements for sealing external manifolds; Arrangements for mounting external manifolds around a stack
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00853—Uses not provided for elsewhere in C04B2111/00 in electrochemical cells or batteries, e.g. fuel cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Abstract

This invention relates to a stack comprising a continuous solid-phase matrix and tubular fuel cells embedded in the matrix. Each fuel cell comprises an inner electrode layer, an outer electrode layer, and an electrolyte layer sandwiched between the inner and outer electrode layers. The matrix is sufficiently porous to allow a first reactant to flow through the matrix and to the outer electrode of each fuel cell, and have sufficient mechanical strength to support the fuel cells in the stack. The fuel cells are embedded such that a second reactant may be flowed through the inside of each tubular fuel cell and to the inner electrode thereof. Alternatively, a stack of tubular separation membranes or a stack of tubular membrane reactors may be embedded in the matrix. The matrix material may comprise solid state foam, metal filament, or metal, cermet, or ceramic wool.

Claims (45)

1. A fuel cell stack comprising (a) a plurality of tubular fuel cells, each fuel cell comprising an inner electrode layer, an outer electrode layer, and an electrolyte layer sandwiched between the inner and outer electrode layers; and, (b) a continuous solid phase porous matrix in which the fuel cells are embedded, wherein a first reactant is flowable through the matrix and to the outer electrode layer of at least one of the fuel cells, and a second reactant is flowable through the inside of at least one of the fuel cells and to the inner electrode thereof.
2. The fuel cell stack of claim 1 wherein the matrix is a solid state porous foam.
3. The fuel cell stack of claim 2 wherein the matrix has a porosity of between 25 and 95%.
4. The fuel cell stack of claim 3 wherein the matrix has a porosity of between 40 and 95%.
5. The fuel cell stack of claim 4 wherein the matrix has a porosity of about 60%.
6. The fuel cell stack of claim 1 wherein the inner electrode layer is an anode and the outer electrode layer is a cathode, and the first reactant is oxidant and the second reactant is fuel.
7. The fuel cell stack of claim 1, wherein the inner electrode layer is a cathode and the outer electrode layer is an anode, and the first reactant is fuel and the second reactant is oxidant.
8. The fuel cell stack of claim 1 wherein the fuel cells are of a solid-oxide type and the matrix composition includes an electronic or mixed (ionic and electronic) conductive ceramic, metal or cermet material.
9. The fuel cell stack of claim 8 wherein the matrix material is selected from the group consisting of: lanthanum strontium manganate, La1-x Sr x Cr0 3, La1-x Ca x Cr0 3, La1-x Mg x Cr0 3, LaCr(Mg)0 3, LaCa1-x Cr y0 3, stainless steel 316 and 316L, Ni-Yittria stabilized zirconia, Ni and doped zirconia cermet, Ni doped - Ce0 2 cermet, Cu doped-ceria cermet, silver-(Bi-Sr-Ca-Cu-O)-oxide cermet, silver-(Y-Ba-Cu-O)-oxide cermet; silver-alloy-(Bi-Sr-Ca-Cu-O)-oxide cermet; silver-alloy-(Y-Ba-Cu-O)-oxide cermet; silver and its alloys, Inconel steel and any super alloy, ferritic steel, SiC, and MoSi2.
10. The fuel cell stack of claim 1 wherein the diameter of at least one of the fuel cells is in the range of about 10 µm to 5000 µm.
11. The fuel cell stack of claim 10 wherein the inner electrode layer of at least one the fuel cells is produced by a process selected from the group consisting of electrophoretic deposition, metal electrodeposition, and composite electrodeposition.
12. A method of producing a fuel cell stack comprising:
(a) producing a plurality of tubular fuel cells, each fuel cell having an inner electrode layer, an outer electrode layer, and an electrolyte layer sandwiched between the inner and outer electrode layers;
(b) coating the fuel cells with a slurry having a composition that includes a matrix material that upon sintering, becomes a continuous solid phase porous matrix;

(c) stacking the fuel cells such that the slurry coating of each fuel cell is in contact with the slurry coating of adjacent fuel cells; and (d) sintering the coated and stacked fuel cells to solidify the matrix and embed the fuel cells therein, thereby producing a stack wherein a first reactant is flowable through the matrix and to the outer electrode layer of at least one of the fuel cells, and a second reactant is flowable through the inside of at least one of the fuel cells and to the inner electrode thereof.
13. The method of claim 12 wherein the step of producing the fuel cell comprises first forming an inner electrode layer on a combustible deposition cathode by a process selected from the group consisting of electrophoretic deposition, metal electrodeposition, and composite electrodeposition, then forming an electrolyte layer on the inner electrode layer by electrophoretic deposition, then forming an outer electrode layer onto the electrolyte layer, and then applying a sintering step that combusts the deposition cathode.
14. The method of claim 12 wherein the matrix material in the slurry is selected from the group consisting of lanthanum strontium manganate, La1-x Sr x Cr0 3, La1-x Ca x Cr0 3, La1-x Mg x Cr0 3, LaCr(Mg)0 3, LaCa1-x Cr y 0 3, stainless steel 316 and 316L, Ni-Yittria stabilized zirconia, Ni and doped zirconia cermet, Ni doped - Ce0 2 cermet, Cu doped-ceria cermet, silver-(Bi-Sr-Ca-Cu-O)-oxide cermet, silver-(Y-Ba-Cu-O)-oxide cermet; silver-alloy-(Bi-Sr-Ca-Cu-O)-oxide cermet; silver-alloy-(Y-Ba-Cu-O)-oxide cermet; silver and its alloys, Inconel steel and any super alloy, ferritic steel, SiC, and MoSi2.
15. The method of claim 14 wherein the slurry further includes a foaming agent, such that upon a selected heat treatment, a solid-state porous foam matrix is formed.
16. The method of claim 15 wherein the slurry further includes combustible particles that combust upon a selected heat treatment to form pores in the matrix.
17. The method of claim 14 wherein the slurry further includes combustible particles that combust upon a selected heat treatment to form pores in the matrix.
18. The method of claim 12 wherein the steps of coating the fuel cells with slurry and stacking the fuel cells comprise stacking the fuel cells in a container, then adding the slurry into the container such that the fuel cells in the container are immersed in the slurry.
19. The method of claim 12 wherein the steps of coating the fuel cells with slurry and stacking the fuel cells comprise coating each fuel cell then placing combustible spacers between the fuel cells before stacking.
20. The method of claim 12 wherein the steps of coating the fuel cells with slurry and stacking the fuel cells comprise coating each fuel cell then placing metal spacers between the fuel cells before stacking that remain after sintering to serve as current collectors and as mechanical support in the stack.
21. The method of claim 12 wherein the steps of coating the fuel cells with slurry and stacking the fuel cells comprise coating the fuel cells then placing the coated fuel cells on a flexible sheet, then manipulating the sheet such that the fuel cells are arranged into a desired stack configuration.
22. A method of producing a fuel cell stack comprising:
(a) producing a plurality of tubular fuel cells, each fuel cell having an inner electrode layer, an outer electrode layer, and an electrolyte layer sandwiched between the inner and outer electrode layers;

(b) arranging a plurality of combustible members in a stack configuration then immersing the combustible members in a slurry having a composition that includes a matrix material that upon sintering, becomes a solid-state electronic or mixed (electronic and ionic) conductive porous matrix;
(c) sintering the slurry and combustible members such that the matrix is formed and the combustible members combust, thereby producing a plurality of channels in the matrix; and, (d) inserting at least one fuel cell into at least one channel;
thereby producing a stack wherein a first reactant is flowable through the matrix and to the outer electrode layer of at least one of the fuel cells, and a second reactant is flowable through the inside of at least one of the fuel cells and to the inner electrode thereof.
23. The method of claim 22 further comprising for at least one fuel cell, (e) adding bonding agent into the channel between the fuel cell and the matrix, then sintering the slurry such that the fuel cell is securely embedded in the matrix.
24. A method of producing a fuel cell stack comprising:
(a) producing a plurality of tubular fuel cells, each fuel cell having an inner electrode layer, an outer electrode layer, and an electrolyte layer sandwiched between the inner and outer electrode layers;
(b) embedding the fuel cells in a combustible template material;
(c) impregnating the template material with a slurry having a composition that includes a matrix material that upon sintering, becomes a continuous solid phase porous matrix; and (d) sintering the slurry-impregnated template material such that the template material combusts, and the matrix is formed;
thereby producing a stack wherein a first reactant is flowable through the matrix and to the outer electrode layer of at least one of the fuel cells, and a second reactant is flowable through the inside of at least one of the fuel cells and to the inner electrode thereof.
25. The method of claim 24 wherein the fuel cell is embedded in the template material before sintering.
26. The method of clam 24 wherein the fuel cell and a bonding agent are embedded in the matrix after sintering, then a heat treatment is applied to the bonding agent that is sufficient to bond the fuel cell to the matrix.
27. The method of claim 24 wherein the template material is selected from the group consisting of a sponge, carbon felt, and graphite felt.
28. A fluid separation apparatus comprising (a) a plurality of tubular fluid separation membrane assemblies, each assembly comprising a porous separation layer and a porous support layer in adjacent contact with the separation layer, wherein the porosity of the separation layer is selected according to the fluids to be separated; and, (b) a continuous solid phase porous matrix in which the assemblies are embedded, wherein an unseparated fluid is flowable through one of the matrix or the inside of at least one of the assemblies, and a separated fluid separated from the unseparated fluid by the separation layer is flowable through the other of the matrix and the inside of at least one of the assemblies.
29. The fluid separation apparatus of claim 28 wherein the separation layer has a thickness of between about 0.5 to 100 µm.
30. The fluid separation apparatus of claim 29 wherein the separation layer has a thickness of between about 0.5 to 30 µm.
31. The fluid separation apparatus of claim 28 wherein the average pore size of the separation layer is between 0.05 and 10 µm.
32. The fluid separation apparatus of claim 31 wherein the average pore size of the support layer is greater than or equal to the average pore size of the separation layer.
33. The fluid separation apparatus of claim 28 wherein the composition of the support layer and the separation layer includes one or more material(s) selected from the group consisting of Al2O3, zirconia, SiO2, SiC, Si3N4, clay, mullite, Al2O3-zirconia composites and TiO2.
34. The fluid separation apparatus of claim 28 wherein the matrix is a solid-state porous foam.
35. The fluid separation apparatus of claim 34 wherein the matrix composition includes one or more material(s) selected from the group consisting of Al2O3, zirconia, Al2O3 - zirconia composites, steel, SiO2, SiC, Si3N4, clay, mullite, and TiO2.
36. The fluid separation apparatus of claim 35 wherein the matrix is coated with TiO2 photo catalyst.
37. The fluid separation apparatus of claim 28 wherein the separation layer is a membrane reactor separation membrane and has a composition that includes material that affects the conversion or selectivity of one or more chemical reactions of the fluids flowable through the apparatus.
38. The fluid separation apparatus of claim 37 wherein the membrane reactor separation membrane has a composition that includes material selected from the group of Pd and Sr-Fe-Co-O.
39. The fluid separation apparatus of claim 38 wherein the membrane reactor separation membrane has a composition that includes Pd and has a thickness of between about 0.5 and 10 µm.
40. The fluid separation apparatus of claim 38 wherein the membrane reactor separation membrane has a composition that includes Sr-Fe-Co-O and has a thickness of between 0.5 - 50 µm.
41. The fuel cell stack of claim 1 wherein the matrix comprises metal filament.
42. The fuel cell stack of claim 1 wherein the matrix comprises a metal, ceramic or cermet wool.
43. A fuel cell stack comprising (a) a plurality of tubular fuel cells, each fuel cell comprising an inner electrode layer, an outer electrode layer, and an electrolyte layer sandwiched between the inner and outer electrode layers;
and, (b) a continuous solid state porous foam matrix in which the fuel cells are embedded, wherein a first reactant is flowable through the matrix and to the outer electrode layer of at least one of the fuel cells, and a second reactant is flowable through the inside of at least one of the fuel cells and to the inner electrode thereof.
44. The fuel cell stack of claim 43 wherein the diameter of at least one of the fuel cells is in the range of about 10 µm to 5000 µm.
45. The fuel cell stack of claim 44 wherein the inner electrode layer of at least one the fuel cells is produced by a process selected from the group consisting of electrophoretic deposition, metal electrodeposition, and composite eiectrodeposition.
CA2475906A 2002-02-14 2003-02-14 Tubular solid oxide fuel cell stack Expired - Lifetime CA2475906C (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US10/078,548 2002-02-14
US10/078,548 US6824907B2 (en) 2002-01-16 2002-02-14 Tubular solid oxide fuel cell stack
PCT/CA2003/000216 WO2003069705A2 (en) 2002-02-14 2003-02-14 Tubular solid oxide fuel cell stack

Publications (2)

Publication Number Publication Date
CA2475906A1 true CA2475906A1 (en) 2003-08-21
CA2475906C CA2475906C (en) 2012-10-30

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US (1) US6824907B2 (en)
EP (1) EP1472755B1 (en)
JP (1) JP4672982B2 (en)
KR (1) KR101021341B1 (en)
CN (1) CN1312803C (en)
AT (1) ATE348410T1 (en)
AU (1) AU2003208194A1 (en)
BR (1) BR0307643A (en)
CA (1) CA2475906C (en)
DE (1) DE60310371T2 (en)
NO (1) NO20043823L (en)
RU (1) RU2004126863A (en)
WO (1) WO2003069705A2 (en)

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