EP1003973B1 - Mikropumpe mit einem einlasssteuerorgan zum selbstansaugen - Google Patents

Mikropumpe mit einem einlasssteuerorgan zum selbstansaugen Download PDF

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Publication number
EP1003973B1
EP1003973B1 EP98951326A EP98951326A EP1003973B1 EP 1003973 B1 EP1003973 B1 EP 1003973B1 EP 98951326 A EP98951326 A EP 98951326A EP 98951326 A EP98951326 A EP 98951326A EP 1003973 B1 EP1003973 B1 EP 1003973B1
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EP
European Patent Office
Prior art keywords
plate
orifice
valve
membrane
moving member
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Expired - Lifetime
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EP98951326A
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English (en)
French (fr)
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EP1003973A1 (de
Inventor
Didier Maillefer
Harald Van Lintel
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Debiotech SA
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Westonbridge International Ltd
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Publication of EP1003973A1 publication Critical patent/EP1003973A1/de
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B43/00—Machines, pumps, or pumping installations having flexible working members
    • F04B43/02—Machines, pumps, or pumping installations having flexible working members having plate-like flexible members, e.g. diaphragms
    • F04B43/04—Pumps having electric drive
    • F04B43/043—Micropumps
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B53/00—Component parts, details or accessories not provided for in, or of interest apart from, groups F04B1/00 - F04B23/00 or F04B39/00 - F04B47/00
    • F04B53/10—Valves; Arrangement of valves
    • F04B53/1037—Flap valves
    • F04B53/1047—Flap valves the valve being formed by one or more flexible elements
    • F04B53/106—Flap valves the valve being formed by one or more flexible elements the valve being a membrane
    • F04B53/1067—Flap valves the valve being formed by one or more flexible elements the valve being a membrane fixed at its whole periphery and with an opening at its centre

Definitions

  • the invention relates to a fluidic device such as a micropump.
  • a fluidic device such as a micropump.
  • a fluidic device such as a micropump.
  • a fluidic device such as a micropump.
  • said inlet control member being a non-return valve composed of a mobile body and a membrane-shaped part connecting said movable member to the rest of said intermediate plate, interposed between the inlet duct and the pumping chamber and allowing by its elasticity, the movement of said valve between a closed position and a open position, said movable member being traversed by an orifice, between the first and second ends, said valve being shaped so that, in said open position, the movable member does not prevent the flow of the liquid from said port to said pumping chamber and the second end of the movable member being shaped to ensure, in said closed position, tight contact with that of the pads
  • such a device constitutes a micropump for medical use which regularly delivers a quantity controlled drug.
  • the manufacturing of these micropumps is based on micro-machining technologies for silicon or any other material machinable by etching using photolithographic techniques.
  • the micropump is controlled by varying the volume of the pumping chamber (alternating decreases and increases), for example by means of an order by a piezoelectric actuator.
  • European patent application 95904674.9 presents such a self-priming micropump.
  • the inlet valves described in this document cannot be made easily.
  • European patent application 90 810272.6 describes a micropump comprising an inlet member, forming a non-return valve, which does not allow however, not to ensure self-priming of the pump.
  • the object of the present invention is to provide a fluidic device such a micropump comprising an input control member allowing to obtain in a secure manner the self-priming of said device, this member being able to be easily manufactured.
  • this objective is achieved by the fact that the movable member is located over most of the thickness of said intermediate plate, that the membrane-shaped part is located near the other of the platelets and that said orifice has a limited volume.
  • the liquid inlet control member included in the device according to the present invention constitutes a non-return valve of the seat valve type.
  • This non-return valve has a shaped part membrane allowing, by its elasticity, the opening and closing of the valve and a movable member surrounding an orifice intended for the flow of liquid.
  • the movable member also comprises at one of its ends means ensuring the tightness of this inlet valve in its closed position, that is to say that the movable member is in sealed contact support against one plates adjacent to the valve, this plate forming the seat of the valve.
  • the first end of the movable member adjacent to said membrane-shaped part is provided with at least one stop element intended to limit the movement of said valve from the closed position towards the open position, the free end of said abutment element coming to contact of the plate located near the membrane-shaped part in said open position without said stop member preventing the flow of liquid from said orifice to said pumping chamber.
  • the micropumps 10 and 100 comprise a base plate 12, preferably made of glass, traversed right through by two conduits 14, 16 respectively forming an inlet conduit and a micropump outlet duct.
  • An intermediate plate 18 surmounts the base plate 12, this intermediate plate preferably being made of silicon and connected to the base plate 12 by the technique, known per se, of anodic welding.
  • the intermediate plate 18 is surmounted by an upper plate 20 or second plate, preferably glass, the intermediate plate and the second plate being linked together by the same technique as the base plate 12 and the intermediate plate 18.
  • the first plate 12 and the second plate 20 have a substantially equal thickness of the order of 1 mm while the intermediate plate also has a substantially constant thickness but more low, between 0.1 and 0.5 mm, preferably between 0.3 and 0.5 mm and advantageously of the order of 0.3 mm.
  • a portion of the intermediate plate 18 constitutes a membrane pump 22 of substantially circular shape and delimiting, with the face upper of the first plate 12, the pumping chamber 24.
  • the pumping membrane 22 constitutes a movable wall controlled by a actuator 26, 126.
  • the inlet duct 14 is connected to the pumping chamber 24 by one or more several input control members 28 which will be described in more detail below.
  • the pumping chamber 24 is connected to a device for controlling liquid outlet or outlet valve 30 which may be of structure similar to that described in the aforementioned European patent application 95 904674.9.
  • the outlet valve 30 shown includes the elements provided for in the above European patent application, namely an annular rib 32 placed opposite the duct of outlet 16 and in sealing contact with the upper surface of the first plate 12 in the closed position of the outlet valve 30, a membrane flexible 34, and thin layers of silicon oxide 36 and 38 allowing, respectively, to avoid adhesion between the annular rib 32 and the first plate 12, and, on the side of the membrane 34 opposite the first plate 12, to create a preload stressing the top of the rib 32 against the first plate 12.
  • the outlet valve 30 also includes a limiting member 39 disposed at the level of the annular rib 32, on the face of the membrane flexible 34 opposite the first plate 12, this limiting member constituting a stop element coming to bear against the second plate 20 in the open position of the outlet valve 30 in order to limit the spacing of the annular rib 32 relative to the first plate 12.
  • the inlet control member or inlet valve 28 visible on the Figures 1 and 2 in its closed position, is illustrated in more detail in the Figure 3 in which the inlet valve is in its open position.
  • the inlet valve 28 is consists of a movable member 40 surrounded by a membrane-shaped part 42.
  • This membrane 42 is substantially circular with a diameter of on the order of 3 mm, its thickness, preferably substantially constant, is between 10 and 50 ⁇ m, preferably of the order of 25 ⁇ m.
  • the inlet valve (s) 28 constitute non-return valves, part of which abuts against one of the first and second pads, in the closed position of the valve.
  • the movable member 40 surrounds an orifice 44 which passes through the movable member 40 from its first end 45, adjacent to the first plate 12, towards its second end 46, adjacent to the second plate 20.
  • the movable member 40 preferably has an external shape of revolution, for example a substantially cylindrical outer shape with circular section or, as illustrated in Figures 1 to 3, in the shape of a trunk cone, the widest part being directed towards the first plate 12.
  • the orifice 44 its volume constituting a space of connection added to the volume of the pumping chamber 24, it is necessary that it is minimum so as not to constitute too much volume important in relation to the volume of the pumping chamber 24.
  • This orifice 44 can have various shapes such as cylindrical, circular, square or other, truncated cone or pyramid-shaped section. If the technique used to engrave the silicon plate constituting the intermediate plate 18 makes it possible to produce an orifice 44 of small diameter, we can make an orifice 44 having a small and substantially section equal over the entire length of this orifice 44.
  • the orifice 44 has a shape made up of two pyramids with square base whose bases constitute of the ends of said orifice, the central zone of this orifice belonging to the two pyramids.
  • This shape composed of two inverted pyramids having their vertices in contact makes it possible to obtain a shape for the orifice 44 of which the total volume is less than that of a single pyramid engraved from one of the two ends of the movable member 40.
  • an advantageous solution consists in carrying out anisotropic etching from the two ends 45 and 46 of the movable member 40.
  • anisotropic etching For this, we begins to dig hole 44 starting, for example, with the first end 45 of the movable member 40, the etching consisting of a square whose side length decreases as we dig more into the movable member 40.
  • an orifice 44 is produced having a cross section substantially constant over its entire length, for example thanks to a method of reactive ion etching or micro-machining, an orifice 44 of small is obtained diameter, this diameter possibly being of the order of 10 to 100 ⁇ m.
  • the volume of the orifice 40 has a volume at most equal to one fifth, preferably one tenth, of the unit volume of pumping, i.e. the volume moved at each open-close cycle of the pump or the volume moved by each cycle up and down of the pumping membrane 22.
  • the relationship between, on the one hand, the maximum distance between the membrane-shaped part of the nearest wafer and, on the other hand, the thickness of the wafer intermediate is less than 1/20, advantageously of the order of 7 ⁇ m.
  • said membrane-shaped part, the first end of the movable member and the outlet of the orifice are adjacent to the first plate and the outlet of the orifice opens directly into the pumping chamber.
  • annular rib 48 surrounding the inlet of the orifice 44 and allowing, when in contact against the lower surface of the second plate 20, to seal the inlet valve 28.
  • annular rib 48 having a surface of contact as small as possible so that, on the one hand, the surface in front present an optimum surface condition has the smallest surface area possible and, on the other hand, so as to produce an inlet valve 28 which can open for a difference in liquid pressure between the inlet pipe 14 and the relatively small pumping chamber 24.
  • the pressure difference allowing the opening of the inlet valve 28 corresponds to the pressure difference of liquid between the liquid present in the connection space 50 placed upstream of the inlet valve 28 and the liquid pressure in the orifice 44, this pressure being the same as in the pumping chamber 24.
  • the liquid can pass from the orifice 44 to the pumping 24, in the open position of the inlet valve 28, provision is made, on the surface of the first end 45 of the movable member 40 placed in look of the first plate 12, a series of stop elements 52 under the shape of small pillars, one end of which is integral with the first end of the movable member 40 and whose second end, free, comes lean against the upper surface of the first plate 12.
  • these abutment elements 52 constitute limiters of movement for the inlet valve 28 when the latter opens so that, in its opening movement, when the movable member 40 approaches of the first plate 12, we are not in a situation where the surface of the first end of the movable member 40 which surrounds the outlet orifice 44 comes to bear on the first plate 12 by closing thus the exit from orifice 44.
  • the inlet valve 28 When the liquid pressure in the connection space 50 is equal to the liquid pressure in the pumping chamber 24, the inlet valve 28 is closes itself by a recall phenomenon whose origin is explained below. Then, the actuator 26, 126 controls the downward movement of the pumping membrane 22 so that one obtains a liquid pressure in the pumping chamber 24 which is higher than the liquid pressure in the connection space located downstream of the outlet valve 30. In this situation, the outlet valve opens as soon as the pressure difference is sufficient and the liquid flows out of the chamber pumping 24.
  • the inlet valve 28 further comprises a first layer of silicon oxide 54 covering at least the surface of the second end 46 of the movable member 40 capable of entering into contact with the second plate 20 in order to prevent a joining between the valve and the second plate in the closed position of the valve input 28.
  • This first layer of silicon oxide 54 covers at least the annular rib 48 in the area intended to come into contact with the second wafer 20, this thin layer of silicon oxide allowing avoid bonding between the movable member 40 and the second plate 20. So that the inlet valve 28 is closed in its rest position, we advantageously provides layers of silicon oxide 56, 58 arranged on the membrane 42 so that it is subjected to a certain prestressing up the figures.
  • the oxide layer 56 is arranged at the level of the region of the part form of membrane 42 which is adjacent to the movable member 40 and which is turned towards the second plate 20 and the oxide layer 58 is disposed in an area of the membrane 42 furthest from the organ mobile 40, on the opposite face of the first plate 12.
  • the inlet valve 28 being preferably machined within the wafer intermediate 18 in silicon using photolithographic techniques known, it is expected that, preferably, the surface of the first portion 42a turned towards the first plate 12 is parallel to the surface of the first plate 12 placed opposite the inlet valve 28 and either same level as the free end of the stop elements 52 because these two elements are machined simultaneously. So these two elements are placed at an identical distance from said first plate 12 when the valve 28 is closed.
  • the free end of the stop elements 52 is planar and parallel to the surface of the first plate 12 adjacent to the pumping chamber 24.
  • the inlet valve 28 in FIG. 5 does not have the layers of oxides 54, 56 and 58 of Figure 3 because it is shaped, during its manufacturing, to be naturally, that is to say in its rest position, in closed position. In the absence of layer 54, it is expected that at least the surface of the annular rib 48 facing the second plate 20 and / or at least the surface of the second plate 20 placed opposite the annular rib 48 is treated, for example coated with an anti-adhesion layer, to avoid the connection between the valve 28 in the closed position and the second plate 20.
  • an inlet valve 28 can be made with a membrane 42 in steps, such as that of FIG. 5, and comprising some or all of the silicon oxide layers 54, 56 and 58 in the figure 3. If a layer 58 is provided, it will preferably be limited to the first portion 42a of the membrane 42.
  • the variant embodiment illustrated in FIG. 6 corresponds to a non-return valve 28 in closed position whose position has been reversed with respect to that of FIG. 3.
  • the membrane 42 is located near the second plate 20 and the seat of the valve 28 is formed by the annular zone of the upper face of the first plate 12 facing the annular rib 48 directed towards the bottom of Figure 6 and placed on the second end 46 of the movable member 40.
  • the stop elements 52 On the side of the first end 45 of the movable member 40, adjacent to the second plate 20 and extended by the membrane 42, are arranged the stop elements 52 and the movable member is extended radially by the membrane 42.
  • the orifice 44 has the same characteristics and can be made of the same way as in the case of the embodiments presented previously.
  • the micropump comprising a inlet valve 28 according to one of the embodiments which have just been described, it remains identical to that of a micropump of the type of those which are described in the aforementioned European applications

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Reciprocating Pumps (AREA)
  • Details Of Reciprocating Pumps (AREA)

Claims (17)

  1. Vorrichtung für Fluide wie eine Mikropumpe (10; 100) mit mindestens einem ersten Plättchen (12), einem zweiten Plättchen (20), einem zwischenliegenden Plättchen (18), das zwischen dem besagten ersten und zweiten Plättchen (12, 20) angeordnet ist, einer durch das besagte erste Plättchen (12) und das besagte zwischenliegende Plättchen (18) abgegrenzten Pumpkammer (24), sowie mit der besagten Pumpkammer (24) in Verbindung stehenden Einlass- und Auslasssteuerorganen (28, 30), mit Einlass- und Auslassleitungen (14, 16), die eines der besagten ersten und zweiten Plättchen (12, 20) völlig durchsetzen, wobei das besagte Einlasssteuerorgan (28) ein Rückschlag-Ventil ist, gebildet von einem beweglichen Organ (40) und einem das besagte bewegliche Organ (40) mit dem Rest des besagten zwischenliegenden Plättchens (18) verbindenden membranförmigen Teil (42), das zwischen der Einlassleitung (14) und der Pumpkammer (24) angeordnet ist und durch seine Elastizität die Bewegung des besagten Ventils (28) zwischen einer geschlossenen und einer geöffneten Position erlaubt, wobei das besagte bewegliche Organ (40) zwischen seinen ersten und zweiten Enden (45, 46) von einer Öffnung (44) durchsetzt ist, wobei das besagte Ventil (28) derartig gestaltet ist, dass in der besagten geöffneten Position das bewegliche Organ den Ausfluss der Flüssigkeit von der besagten Öffnung (44) in Richtung der besagten Pumpkammer (24) und des zweiten Endes (46) des beweglichen Organs (40) nicht verhindert, wobei dieses dafür ausgebildet ist, in der besagten geschlossenen Position einen dichten Kontakt mit demjenigen der Plättchen (12, 20), das den Ventilsitz bildet, sicherzustellen,
       dadurch gekennzeichnet, dass das bewegliche Organ auf dem größten Teil der Dicke des zwischenliegenden Plättchens (18) angeordnet ist, dass das membranförmige Teil in der Nähe des anderen der Plättchen (12, 20) angeordnet ist und dass die besagte Öffnung (44) ein geringeres Volumen als das Volumen der Pumpkammer (24) aufweist.
  2. Vorrichtung nach Anspruch 1, dadurch gekennzeichnet, dass das an das besagte membranförmige Teil (42) angrenzende erste Ende (45) des beweglichen Organs mit wenigstens einem Anschlagelement (52) versehen ist, das dazu dient, die Bewegung des besagten Ventils (28) von der geschlossenen Position zu der geöffneten Position hin zu begrenzen, wobei das freie Ende des besagten Anschlagelements in der besagten geöffneten Position in Kontakt mit dem in der Nähe des membranförmigen Teils (42) angeordneten Plättchen (12, 20) kommt, ohne dass das besagte Anschlagelement (52) den Ausfluss der Flüssigkeit von der besagten Öffnung (44) in Richtung der besagten Pumpkammer (24) verhindert.
  3. Vorrichtung nach Anspruch 2, dadurch gekennzeichnet, dass das besagte bewegliche Organ (40) eine äußere Form besitzt, die im Wesentlichen zylindrisch mit kreisförmigen Querschnitt oder kegelstumpfförmig ist.
  4. Vorrichtung nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die besagte Öffnung (44) eine zylindrische Form besitzt.
  5. Vorrichtung nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, dass die besagte Öffnung (44) eine Form besitzt, die aus zwei Pyramiden mit viereckigen Grundflächen gebildet ist, wobei die Grundflächen die Enden der besagten Öffnung bilden, wobei die zentrale Zone der besagten Öffnung den zwei Pyramiden zugeordnet ist.
  6. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass die besagte Öffnung (44) ein Volumen aufweist, das höchstens gleich einem Fünftel des Einheitsvolumens des Pumpvorgangs ist.
  7. Vorrichtung nach Anspruch 6, dadurch gekennzeichnet, dass das besagte zwischenliegende Plättchen (18) aus Silizium hergestellt ist und dass das Ventil (28) darüber hinaus eine erste Schicht (54) aus Siliziumoxid umfasst, die mindestens die Oberfläche des zweiten Endes (46) des beweglichen Organs bedeckt, geeignet zur Wiederaufnahme des Kontakts mit dem besagten Plättchen (12, 20), das den Ventilsitz bildet, um einen Zusammenschluss zwischen dem besagten Ventil (28) und dem besagten Plättchen (12, 20) während der geschlossenen Position des Ventils zu verhindern.
  8. Vorrichtung nach Anspruch 7, dadurch gekennzeichnet, dass das Ventil (28) darüber hinaus eine zweite Schicht (56) aus Siliziumoxid umfasst, die sich mindestens auf der Außenfläche des Ventils (28) erstreckt, auf Höhe der Zone des membranförmigen Teils (42), die an das bewegliche Organ (40) angrenzt und die in Richtung des Plättchens (12, 20) gewandt ist, das den Ventilsitz bildet, um eine Vorspannung zu erzeugen, die in der Ruheposition des Ventils das Ventil (28) zwingt, in gegen das besagte Plättchen (12, 20) geschlossener Position zu sein.
  9. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das besagte zwischenliegende Plättchen (18) eine im Wesentlichen konstante zwischen 0,3 und 0,5 mm liegende Dicke besitzt.
  10. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das besagte membranförmige Teil (42) eine im Wesentlichen konstante zwischen 10 und 50 µm liegende Dicke besitzt.
  11. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das besagte membranförmige Teil (42) einen Absatz (60) im Bereich seiner Oberfläche aufweist, der dem in der Nähe des membranförmigen Teils (42) angeordneten Plättchen (12, 20) zugewandt ist, wobei er einen ersten Bereich (42a) abgrenzt, der näher an dem besagten Plättchen (12, 20) ist als ein an das besagte bewegliche Organ (40) angrenzender zweiter Bereich (42b).
  12. Vorrichtung nach Anspruch 11, dadurch gekennzeichnet, dass der besagte Absatz (60) kreisförmig und zentriert um die besagte Öffnung (44) herum ist, wobei die besagten ersten und zweiten Bereiche (42a, 42b) des besagten membranförmigen Teils (42) konzentrische Ringe bilden.
  13. Vorrichtung nach Anspruch 11 oder 12, dadurch gekennzeichnet, dass die Oberfläche des besagten ersten Bereichs (42a), die dem besagten in der Nähe des membranförmigen Teils (42) angeordneten Plättchen (12, 20) zugewandt ist, und das freie Ende der besagten Anschlagelemente (52) gleich weit von dem besagten Plättchen (12, 20) entfernt sind.
  14. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass der das membranförmige Teil (42) von dem nächstgelegenen Plättchen (12, 20) trennende maximale Abstand zwischen 3 und 20 µm umfasst.
  15. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das Verhältnis zwischen dem maximalen Abstand einerseits, der das membranförmige Teil (42) von dem nächstgelegenen Plättchen (12, 20) trennt, und der Dicke des zwischenliegenden Plättchens (18) andererseits geringer ist als 1/20.
  16. Vorrichtung nach einem der vorhergehenden Ansprüche, dadurch gekennzeichnet, dass das besagte membranförmige Teil (42), das erste Ende des beweglichen Organs und der Ausgang der Öffnung (44) an das erste Plättchen (12) angrenzen, und dass der Ausgang der Öffnung (44) unmittelbar in die Pumpkammer (24) mündet.
  17. Vorrichtung nach einem der vorhergehenden Ansprüche 1 bis 15, dadurch gekennzeichnet, dass das besagte membranförmige Teil (42), das erste Ende des beweglichen Organs und der Ausgang der Öffnung (44) an das zweite Plättchen (20) angrenzen, und dass der Ausgang der Öffnung (44) mit der besagten Pumpkammer mittels einer zusätzlichen Öffnung (64) verbunden ist, welche die ganze Dicke des zwischenliegenden Plättchens (18) durchsetzt.
EP98951326A 1997-08-20 1998-08-19 Mikropumpe mit einem einlasssteuerorgan zum selbstansaugen Expired - Lifetime EP1003973B1 (de)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR9710497 1997-08-20
FR9710497 1997-08-20
PCT/EP1998/005471 WO1999009321A1 (fr) 1997-08-20 1998-08-19 Micropompe comprenant un organe de controle d'entree permettant son auto-amorcage

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Publication Number Publication Date
EP1003973A1 EP1003973A1 (de) 2000-05-31
EP1003973B1 true EP1003973B1 (de) 2003-04-16

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US (1) US6390791B1 (de)
EP (1) EP1003973B1 (de)
JP (1) JP2001515183A (de)
CN (1) CN1097168C (de)
AU (1) AU9739898A (de)
CA (1) CA2301878A1 (de)
DE (1) DE69813569T2 (de)
WO (1) WO1999009321A1 (de)

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DE69813569D1 (de) 2003-05-22
AU9739898A (en) 1999-03-08
WO1999009321A1 (fr) 1999-02-25
US6390791B1 (en) 2002-05-21
DE69813569T2 (de) 2004-04-08
CN1271407A (zh) 2000-10-25
CN1097168C (zh) 2002-12-25
JP2001515183A (ja) 2001-09-18
EP1003973A1 (de) 2000-05-31
CA2301878A1 (en) 1999-02-25

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