EP1210593A2 - Capteur de gaz et procede de fabrication correspondant - Google Patents

Capteur de gaz et procede de fabrication correspondant

Info

Publication number
EP1210593A2
EP1210593A2 EP00954786A EP00954786A EP1210593A2 EP 1210593 A2 EP1210593 A2 EP 1210593A2 EP 00954786 A EP00954786 A EP 00954786A EP 00954786 A EP00954786 A EP 00954786A EP 1210593 A2 EP1210593 A2 EP 1210593A2
Authority
EP
European Patent Office
Prior art keywords
substrate
electrolyte
electrodes
electrode
gas sensor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP00954786A
Other languages
German (de)
English (en)
Inventor
John Robert Dodgson
Malcolm Trayton Austin
John Edward Andrew Shaw
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Central Research Laboratories Ltd
Original Assignee
Central Research Laboratories Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Central Research Laboratories Ltd filed Critical Central Research Laboratories Ltd
Publication of EP1210593A2 publication Critical patent/EP1210593A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/403—Cells and electrode assemblies
    • G01N27/404—Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid, e.g. Clark-type oxygen sensors
    • G01N27/4045—Cells with anode, cathode and cell electrolyte on the same side of a permeable membrane which separates them from the sample fluid, e.g. Clark-type oxygen sensors for gases other than oxygen
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416—Systems
    • G01N27/4163—Systems checking the operation of, or calibrating, the measuring apparatus
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/0004—Gaseous mixtures, e.g. polluted air
    • G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
    • G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
    • G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
    • G01N33/004—CO or CO2

Definitions

  • the present invention relates to a gas sensor and its method of manufacture. It relates particularly, but not exclusively, to a gas sensor for detecting carbon monoxide.
  • Electrochemical gas sensors typically comprise two electrodes in contact with an electrolyte. Usually a liquid electrolyte is used, the electrolyte being kept in contact with one or more of the electrodes by means of a wick.
  • An electrochemical gas cell which utilises liquid electrolyte is described in US Patent US-A-4100048 (Pompei et al).
  • a polarographic cell having thin film metal electrodes supported on a solid, rigid matrix, which acts as a wick is disclosed.
  • a liquid electrolyte is partially absorbed into the rigid matrix, the pores of the matrix define reaction sites between the gas, the electrodes and the electrolyte.
  • the reaction area of this cell is low compared with sensor cells which use porous gas diffusion electrodes. This means that the polarographic cell may have a shorter life due to poisoning.
  • the cell is also unsuitable for mass production techniques, as the electrodes are deposited, rather than screen printed, onto the matrix.
  • a highly viscous or solid electrolyte is used, in which case no wick is required.
  • gas sensors incorporating a solid electrolyte are disclosed in US Patents US-A-4820386 (LaConti and Griffith) and US- A-4900405 (Otagawa and Madou).
  • LaConti and Griffith use a sheet of solid polymer electrolyte (SPE) with electrodes placed on either side of this sheet.
  • a humidifying reservoir is also included in the sensor.
  • the humidifying reservoir contains a liquid to keep the solid electrolyte wet.
  • Otagawa and Madou use a planar array of electrodes with a layer of SPE cast over the electrodes. Gas reaches the electrodes either through the SPE film, or at the interface between the SPE film and parts of the electrodes projecting above the film.
  • the LaConti and Griffith gas sensor employs an SPE membrane with electrodes separately fabricated and pressed onto the membrane.
  • the fabrication of this sensor is a complex process, and the polymer membrane and electrodes are also relatively expensive.
  • An additional disadvantage of this sensor is that heat treatment of the SPE membrane is not possible as it tends to decompose. This limits the way in which the electrodes can be mounted on the membrane.
  • electrodes are pressed onto the polymer membrane, and are urged into contact, for example, by the cell housing structure or by cold welding of the electrode and the membrane.
  • the design of the gas sensor also means that the electrodes must be contacted using expensive noble metals.
  • the Otagawa gas sensor requires only a relatively small amount of SPE, but the area of electrode available for gas reaction is small. Therefore, unless complex fabrication procedures are used, the cell output will be low and problems with short life through poisoning tend to occur.
  • An aim of the present invention is to provide a gas sensor with a simpler structure than existing gas sensors, and a gas sensor that is simpler and cheaper to manufacture than existing gas sensors.
  • a method of manufacturing a gas sensor including the steps of: a) forming at least first and second electrodes on a substantially planar porous substrate, the substrate having a first major surface, and a second major surface; b) introducing a first electrolyte into at least a portion of the substrate, said first electrolyte being solid and defining a conductive path between the electrodes; c) providing a housing containing a reservoir, which, in use receives a second electrolyte; said second electrolyte maintaining the first electrolyte in a wetted state and d) bonding the substrate to the housing.
  • the first electrolyte preferably contains a polymer and may be introduced into the substrate in liquid form, or as a melted solid. Such an electrolyte is hereinafter referred to as a polymer electrolyte.
  • the first electrolyte is in the form of a solution, when it is applied, so that, upon evaporation of the solvent, the electrolyte is deposited in the substrate.
  • the polymer electrolyte preferably has a high concentration of attached acid groups and which therefore conducts hydrogen ions such as, for example, NafionTM produced by Dupont.
  • the substrate has an open-cell structure, thus ensuring that gas may pass through the substrate to reach the electrodes.
  • the first electrolyte may be introduced into, and supported by, the substrate.
  • Electrodes Use of a porous substrate to contain the first electrolyte also allows the electrodes to be formed on the substrate in a rapid, efficient manner.
  • the electrodes may then, for example, be sintered to the substrate to give a robust structure. This permits the electrode material to be taken through the region where the housing and substrate are bonded (the seal) to form external electrical contacts.
  • the use of electrode material as electrical contacts means that the use of expensive noble metal contacts is avoided.
  • the first electrolyte may be introduced into the substrate via the first major surface of the substrate and/or via the electrode(s) (if any) formed thereon. It is also possible to introduce the first electrolyte into the substrate via the second major surface of the substrate and/or via the electrode(s) (if any) formed thereon.
  • the housing is preferably a two-part housing comprising a first housing portion and a second housing portion.
  • the substrate is disposed between the first housing portion and the second housing portion, the second housing portion containing the reservoir into which the second electrolyte is introduced.
  • the second electrolyte is preferably aqueous electrolyte, and most preferably a hygroscopic liquid (such as concentrated sulphuric acid) so that there is a high relative humidity in the vicinity of the first electrolyte. This allows the first electrolyte to maintain a relatively constant conductivity, and removes the need for a wick.
  • electrodes are preferably sintered onto the substrate, they may be deposited onto the substrate by, for example, screen printing; filtering in selected areas from a suspension placed onto the substrate; by spray coating, or any other method suitable for producing a patterned deposition of solid material onto a substrate.
  • Deposition might be of a single material or more than one material in layers so as, for example, to vary the properties of the electrode material through its thickness, or to add a second layer of increased electrical conductivity above or below the layer which is the main site of gas reaction.
  • the first electrode may be formed on the first or second major surface of the substrate.
  • the second electrode may also be formed on the first or second major surface of the substrate.
  • Some, or all, of the electrodes may extend past the first and/or second housing portions so as to form electrical contacts. This may be achieved by having a substrate in the form of a disc which has a larger diameter than the first and/or second housing portions.
  • pins, metal strips or wires may be used to form the electrical contacts.
  • Holes or apertures which extend from the external surfaces of the housing portions to the electrodes may be formed in the first and/or second housing portions. These enable external electrical connections to be made to the electrodes by way, for example of contact pins of clips.
  • the substrate is bonded to the housing portions by the application of heat and/or pressure.
  • This has the advantage of causing impregnation of the electrode with the housing material to seal the electrode in the region of the electrical contact. Bonding may, however, be achieved using adhesives or ultrasonic bonding.
  • the porosity of the substrate may be modified in a region adjacent the first electrolyte.
  • the porosity of the substrate may be modified by the application of pressure to the substrate, or by filling the required area with a material which is impermeable to the second electrolyte.
  • selected regions of the substrate can be sealed so that electrolyte from the electrolyte reservoir does not pass into region(s) of the sensor where it is not required.
  • An electrochemical device having an electrolyte impregnated membrane is disclosed in European Patent Application No. EP-A1-0 862 232 (Asahi).
  • a foam with a closed- cell structure is impregnated with a non-aqueous electrolytic liquid.
  • the electrolyte remains in a liquid form as it is held within the cells of the foam.
  • This type of impregnated foam is not suitable for use in gas sensors where the electrodes are made using a print and sinter process as the latter techniques involve very high temperatures, and the foam is liable to leak.
  • a gas sensor comprising: a housing within which there is located: at least first and second sensing electrodes formed on a gas permeable substrate, at least one of the sensing electrodes, in use, contacts a first electrolyte; and two self test electrodes, at least one of which is formed on the same surface of the substrate on which a sensing electrode is formed, a hydrophobic envelope surrounds a volume of solid polymer electrolyte, which solid polymer electrolyte defines an electrical pathway between the first and second self test electrodes thereby defining a self test gas generator.
  • the hydrophobic envelope may be defined in the gas permeable substrate by for example impregnating suitable regions of the substrate.
  • the first electrode is preferably the working or sensing electrode for carrying out the desired electrochemical reaction between the electrolyte and the incoming gas to be sensed.
  • the second electrode is preferably the counter electrode required for performing a counterpart electrochemical reaction with oxygen, and for creating the required ionic and electronic flows through the electrolyte between the electrodes.
  • the gas sensor may also include a reference electrode.
  • Electrodes are porous so that they are partially permeable to the first and second electrolytes.
  • the electrodes are preferably formed of a porous electrically conductive material containing PTFE or similar polymeric binder and particles of catalyst.
  • the electrodes may optionally contain additional catalyst support material, and also material to enhance conductivity.
  • the catalyst may comprise, for example, ruthenium dioxide or platinum.
  • the electrodes are preferably operated by way of a potentiostat circuit. Such circuits are well-known in the art.
  • the housing may have a diffusion barrier in the form of a small aperture through which ambient gases can diffuse to contact the sensing electrode.
  • the housing may be composed of a material (such as a plastics material) which has a lower melting point than the substrate, so that if heat and pressure are applied to the housing through the substrate, housing material is forced upwards and impregnates the substrate thus forming a strong bond between the housing and the substrate. The bond may, if necessary, be cooled under pressure to prevent relaxation of the structure before the housing material solidifies.
  • the substrate includes a porous plastic such as, for example, a porous fluoropolymer such as PTFE, a glass fibre mat, or any other absorbent medium onto which electrodes can be deposited.
  • a porous plastic such as, for example, a porous fluoropolymer such as PTFE, a glass fibre mat, or any other absorbent medium onto which electrodes can be deposited.
  • This substrate is preferably permeable to gases, but impermeable to the second electrolyte.
  • Figure la shows a cross-sectional view of a first gas sensor
  • Figure lb shows the first gas sensor having contact pins
  • Figure 2 shows a cross-sectional view of a second gas sensor
  • Figure 3 shows a cross-sectional view of a third gas sensor
  • Figure 4a shows a cross-sectional view of a gas sensor having self-test capability
  • Figure 4b shows a plan view of the gas sensor of Figure 4a.
  • a generally circular gas sensor (10a) comprising a two-part housing (12a) and (12b), and sensing electrode (14) and counter electrode (16) formed on a porous membrane (18).
  • Housing part (12b) is cylindrical with a hollow interior defining an electrolyte reservoir (20) for receiving liquid electrolyte (30).
  • the housing parts (12a) and (12b) support the membrane (18), and also form an acid-tight seal so that electrolyte (30) cannot leak from the sensor assembly.
  • Housing part (12a) is a disc shaped cap member having an aperture (22) therein to permit atmospheric gas to diffuse to a recessed manifold area (24), and thence to sensing electrode (14).
  • Aperture (22) may be in the form of a diffusion barrier to control the amount of gas reaching sensing electrode (14).
  • Membrane (18) is disposed between housing parts (12a) and (12b) and is in the form of a disc. A portion of the membrane is impregnated with a solid polymer electrolyte (26). A hydrophobic perimeter surrounds the solid polymer electrolyte and prevents it from leaching into the electrolyte or into the from the membrane.
  • Electrodes (14) and (16) are formed of a mixture of electrically conductive catalyst particles in PTFE binder, and are sintered onto substrate (18). Sensing electrode (14) is formed on the upper surface of substrate (18), while counter electrode (16) is formed on the lower surface of the substrate and is in contact with electrolyte (30). Housing portions (12a) and (12b) have apertures (28a) and (28b) extending from the outer surface of the housing portions to the electrodes, so that external electrical contact may be made with respective electrodes (14) and (16). Apertures (28a) and (28b) are offset one from another in order that the assembly is not weakened.
  • Electrolyte (30) is hygroscopic.
  • Reservoir (20) is closed at the base by means of a base member (not shown) having a pressure relief aperture, or vent, (32) in order to allow equalisation of pressure across the substrate (18).
  • Vent (32) is closed by a porous membrane.
  • FIG. lb A method of making an external electrical connection with gas sensor (10a) is shown in Figure lb.
  • conductive contact pins (40a) and (40b) are mounted in housing portions (12a) and (12b) in order to make electrical connection with respective electrodes (14) and (16).
  • sensing electrode (14) On operation of sensor (10a), gas from the environment passes through the diffusion barrier (22) to recessed manifold area (24).
  • the diffusion barrier (22) controls the rate of arrival of atmospheric gas at sensing electrode (14). If the gas to be sensed is present, an electrochemical reaction is created at sensing electrode (14) on contact between the electrolyte and the gas. An electrochemical reaction also occurs at counter electrode (16) with oxygen from the atmosphere. Current is carried through the electrolyte by ions produced in the reactions, and by electrons in an external circuit. The current in the external circuit indicates the concentration of carbon monoxide in the atmosphere.
  • a gas sensor (10b) comprising a two-part housing (12a) and (12b), and sensing electrode (14) and counter electrode (16) both formed on the upper side of substrate (18).
  • lower housing part (12b) is cylindrical with a hollow interior forming an electrolyte reservoir
  • Electrolyte reservoir (20) contains electrolyte (30)
  • electrolyte (30) is permitted to directly contact the region of the substrate (18) which is impregnated with SPE (26) Atmosphe ⁇ c gas is permitted to diffuse to recessed manifold area (24) via aperture (22), and thence to sensing electrode (14) only Counter electrode (16) is covered by a portion of upper housing part (14a) so that gas from the atmosphere cannot directly diffuse thereto
  • substrate layer (18) is disposed between housing parts (12a) and (12b) and is in the form of a disc Co-planar electrodes (16) and (18) extend past opposite sides of housing portion (12a) to form elect ⁇ cal contact regions (28a) and (28b).
  • Gas sensor (10c) also comp ⁇ ses a two-part housing (12a) and (12b), and sensing electrode (14) and counter electrode (16) formed on substrate (18)
  • housing part (12a) permits atmosphe ⁇ c gas to diffuse to recessed manifold area (24), and thence to sensing electrode (14) only.
  • Electrodes (14) and (16) are formed on the lower surface of substrate layer (18), so that gas from the atmosphere diffuses through the substrate (18) before reaching the electrodes Electrodes (14,16) and the exposed lower surface of substrate layer (18) are coated with a layer of SPE (26) SPE layer (26) is kept wet by electrolyte (30) contained within electrolyte reservoir (20)
  • housing part (12a) is larger in diameter than housing part (12b) so that electrodes (14) and (16) extend past housing part (12b) to form respective elect ⁇ cal contact regions (28a) and (28b).
  • Gas sensor (lOd) comp ⁇ ses 1) a two-part housing (12a) and (12b), 2) a sensor cell comp ⁇ smg sensing electrode (14), reference electrode (15) and a counter electrode (16) (common to both the sensor cell and the test cell) formed on the lower surface of substrate (18); and 3) a self-test cell (36)
  • the self-test cell (36) includes a porous membrane or test electrode (17), loaded with a volume of SPE , and a bar ⁇ er region (34). Bar ⁇ er region (34) is formed by filling the outer edges of region (26) with a hydrophobic polymer Alternatively, the porosity of the outer edges of region (26) may be removed by, for example, compression. Barrier region (34) ensures that wicking of the electrolyte (20) from electrolyte reservoir (30) to recessed manifold area (24) does not occur.
  • Co-planar electrodes (14), (15) and (16) extend past opposite sides of housing portions (12a) and (12b) to form electrical contact regions (28a) (not shown), (28c) and (28b), respectively.
  • Test-cell electrode (17) also extends beyond housing portion (12a) to form an electrical contact (28d).
  • a wicking means (not shown) may be provided to keep the electrolyte (30) in contact with electrodes (14), (15), and (16).
  • gas sensors (10a) to (lOd) The manufacture of gas sensors (10a) to (lOd) will now be described.
  • the electrodes are sintered (at a temperature of between 300°C and 370°C for approximately 1 hour) onto porous substrate (18). These conditions fuse the binder particles to the substrate.
  • the polymer electrolyte (26) is then introduced into substrate (18) as a liquid.
  • the liquid polymer wets the porous substrate (18), flows into the substrate, fills the porous areas, and then solidifies.
  • the filling of the substrate might be complete or partial, depending on the properties of the chosen polymer and substrate.
  • the liquid polymer flows a little way into the electrodes, up to the interface with the substrate. This ensures that good electrical contact with the electrodes is made, while still enabling gas to access the area of reaction at the interface between the electrodes and the SPE (26).
  • the counter electrode is deposited on the lower surface of substrate
  • the electrode may be deposited on the substrate so that small holes are left in the electrode.
  • the polymer electrolyte is then introduced into the substrate through the holes.
  • the polymer electrolyte (26) may be introduced into substrate (18) through the electrodes (14, 16), or wicked through the side of the substrate.
  • the polymer may be introduced through the opposite side of the substrate from the electrodes, i.e., the lower surface of substrate (18).
  • the polymer electrolyte may be wicked through the side of the substrate.
  • the polymer (26) is introduced through the lower surface of substrate (18) - the surface of the substrate containing the electrodes (14, 16). However, it is only required to impregnate the region of the substrate in contact with the electrodes. This is achieved by using a polymer electrolyte (26) with a high viscosity, or by protecting a region of the substrate by first filling it with a substance which can later be removed while leaving the solidified electrolyte (26) in situ.
  • gas sensor (lOd) the polymer electrolyte (26) is introduced into substrate (18) in the same manner as for gas sensor (10a).
  • the SPE impregnated substrate is sandwiched between the housing parts (12a) and (12b). Heat and pressure are then applied to the peripheral parts of this structure in order to seal it. Electrolyte (30) is then introduced into reservoir (20) through a filling port (not shown) formed in lower housing portion (12b).
  • electrically conductive polymer may be positioned between the electrodes and the conductive contact pins (40a) and (40b), so that when heat and pressure are applied, the conductive polymer moulds itself around the heads of the contact pins and impregnates into the electrode material, thereby creating a stable and secure electrical coupling.
  • planar electrode assembly simplifies production of the sensor, as all electrodes can be produced in a single process
  • the cell assembly process is capable of automation.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Pathology (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Physics & Mathematics (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Food Science & Technology (AREA)
  • Medicinal Chemistry (AREA)
  • Measuring Oxygen Concentration In Cells (AREA)
  • Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)

Abstract

L'invention se rapporte à un capteur de gaz et à un procédé de fabrication correspondant. Les capteurs de gaz des techniques antérieures nécessitaient une mèche pour maintenir une électrode en état humide, ce qui demandait des structures et des techniques de fabrication complexes. Dans un mode de réalisation préféré, un capteur de gaz possède une première et une deuxième électrodes de détection formées sur un substrat perméable aux gaz, une au moins des électrodes étant en contact avec un électrolyte liquide. L'objet de l'invention comprend aussi deux électrodes d'autovérification dont au moins une est formée à la même surface du substrat sur laquelle est formée l'électrode de détection. Une enveloppe hydrophobe entoure un volume de l'électrode polymère solide, qui délimite une voie conductrice d'électricité entre les première et seconde électrodes d'autovérification et définit ainsi un générateur de gaz d'autovérification. Ainsi, l'invention permet de se passer de mèches devant être simultanément en contact avec une électrode et un électrolyte liquide.
EP00954786A 1999-08-24 2000-08-24 Capteur de gaz et procede de fabrication correspondant Withdrawn EP1210593A2 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
GB9919897 1999-08-24
GBGB9919897.0A GB9919897D0 (en) 1999-08-24 1999-08-24 A gas sensor and method of manufacture
PCT/GB2000/003285 WO2001014864A2 (fr) 1999-08-24 2000-08-24 Capteur de gaz et procede de fabrication correspondant

Publications (1)

Publication Number Publication Date
EP1210593A2 true EP1210593A2 (fr) 2002-06-05

Family

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Family Applications (1)

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EP00954786A Withdrawn EP1210593A2 (fr) 1999-08-24 2000-08-24 Capteur de gaz et procede de fabrication correspondant

Country Status (4)

Country Link
EP (1) EP1210593A2 (fr)
AU (1) AU6714100A (fr)
GB (1) GB9919897D0 (fr)
WO (1) WO2001014864A2 (fr)

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JP4140911B2 (ja) 2005-03-04 2008-08-27 フィガロ技研株式会社 液体電気化学ガスセンサ
JP2008164305A (ja) * 2006-12-26 2008-07-17 Yazaki Corp 電気化学式センサ、対象ガス監視装置、及び、電気化学式センサの濃度検出方法
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WO2016040771A1 (fr) 2014-09-12 2016-03-17 Spec Sensors, Llc Dispositifs d'échantillonnage de souffle et procédés d'échantillonnage de souffle utilisant des capteurs
JP6429193B2 (ja) * 2015-02-10 2018-11-28 光明理化学工業株式会社 アルコールセンサ
WO2016191552A1 (fr) 2015-05-26 2016-12-01 Spec Sensors, Llc Système de capteur de gaz sans fil en champ proche et ses procédés de fabrication
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Also Published As

Publication number Publication date
WO2001014864A2 (fr) 2001-03-01
AU6714100A (en) 2001-03-19
WO2001014864A3 (fr) 2001-05-31
GB9919897D0 (en) 1999-10-27

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