EP0956449B1 - Mikroejektionspumpe - Google Patents
Mikroejektionspumpe Download PDFInfo
- Publication number
- EP0956449B1 EP0956449B1 EP97951842A EP97951842A EP0956449B1 EP 0956449 B1 EP0956449 B1 EP 0956449B1 EP 97951842 A EP97951842 A EP 97951842A EP 97951842 A EP97951842 A EP 97951842A EP 0956449 B1 EP0956449 B1 EP 0956449B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- pump according
- microejection
- silicon chip
- microejection pump
- pumping chamber
- 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.)
- Revoked
Links
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 53
- 239000010703 silicon Substances 0.000 claims abstract description 53
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000011521 glass Substances 0.000 claims abstract description 18
- 238000005086 pumping Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 238000005530 etching Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052715 tantalum Inorganic materials 0.000 claims description 3
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 239000012528 membrane Substances 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 description 35
- 239000000126 substance Substances 0.000 description 11
- 230000000694 effects Effects 0.000 description 10
- 238000011068 loading method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 238000011109 contamination Methods 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007639 printing Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 238000000206 photolithography Methods 0.000 description 2
- 150000003376 silicon Chemical class 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910001174 tin-lead alloy Inorganic materials 0.000 description 2
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- 229910001128 Sn alloy Inorganic materials 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000005297 pyrex Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002444 silanisation Methods 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
- F04B43/046—Micropumps with piezoelectric drive
-
- 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
- F04B53/08—Cooling; Heating; Preventing freezing
Definitions
- the invention relates to a micro ejection pump for generation of microdroplets consisting of at least one in one Silicon chip-formed pump chamber, one above the pump chamber arranged and piezoelectrically actuable silicon membrane, wherein the pump chamber with at least one inlet channel and an exhaust port provided with an exhaust port is connected and in which a glass chip opposite the silicon membrane at least closes the pump chamber.
- micro ejection pumps allow in connection with a suitable handling device, e.g. Manipulators that targeted delivery of these substances to the site of sample processing or a sample waste. With the help of a suitable positioning technology can take sampling and Sample storage location may be different.
- This sample storage location can be a liquid surface, a Solid surface or a gas-filled reaction chamber his.
- a micropump intended for the above applications is from the US 50 94 594 A become known.
- This micropump consists of a pump unit with an associated pump chamber and a deformable chamber segment on which an electrically controllable Piezo element is arranged.
- the liquid to be pumped the pump chamber via an inlet capillary (inlet channel) fed.
- By actuating the piezo element alternately exerted on the deformable chamber segment Force causes a constant change in pressure in the pump chamber, see above that alternately loading them via the inlet capillary and expelling the liquid via one with the pumping chamber related outlet capillary.
- the Inlet and the outlet capillary each piezoelectrically actuable Valves provided.
- Micropump With such a micropump it is possible to use small amounts of liquid to apply, but a relatively limited Frequency range and thus also a limited one Funding rate is available. With the one described above Micropump can, for example, a delivery rate of reach about 500 picoliters. To ensure the necessary Functional reliability of this micropump, it is necessary that the liquids or suspensions are as low as possible Have viscosity.
- a micropump can be seen from WO, A, 9419609, which a pump chamber with variable chamber volume and contains a liquid inlet and a liquid outlet.
- a pump chamber with variable chamber volume and contains a liquid inlet and a liquid outlet.
- a diffuser provided with a nozzle.
- the diffuser here is the liquid inlet and the nozzle associated with the liquid outlet.
- the invention has for its object a micro ejection pump to create the handling of liquids or Suspensions, or of liquefiable substances, in the volume range from a few picoliters to a few hundred Microliters, which has a high frequency stability and with which the generation of individually countable, directed, accelerated and impulsive defined their drop volume and reproducible microdrops is possible.
- the pumping chamber becomes the frequency stability of the microejection pump significantly improved.
- the anisotropy of the diffuser flow resistance supports drop formation in pump mode, i.e. there is a jet effect along the positive Pressure drop and in loading mode is the liquid afterflow into the pumping chamber, i.e. there is a diffuser effect along the positive pressure gradient.
- Micro ejection pump for printing can by the Diffuser a higher printing speed can be achieved.
- the outlet channel is also designed as a microcapillary, so that the sample delivery in the form of individually countable, directed, accelerated with impulses and in terms of their Drop volume of defined microdroplets is reproducible.
- the volume of the drops and the delivery rate are through the electrical parameters (frequency, amplitude, pulse shape) the pump control adjustable.
- the diffuser element Pump chamber is arranged immediately, or immediately extends to the pumping chamber, the diffuser element in a first variant of the invention a constant opening angle having.
- the opening angle of the diffuser element should preferably be 3 - 5 °.
- the diffuser element has a constantly changing opening angle.
- the opening angle can increase continuously.
- the pump chamber a floor plan with straight or curved boundary lines on, with the diffuser element in an entrance zone the pump chamber opens.
- the microcapillary is between the pumping chamber and the discharge opening can be connected to further inlet channels. This makes it possible for the pumped through the pumping chamber Add liquid to other substances in a targeted manner.
- the micro ejection pump preferably consists of a composite from a micromechanically structured silicon chip and a glass chip.
- the micro ejection pump i.e. the combination of the silicon chip and the Glass chip, in the direction of the discharge opening of the outlet duct in tapered x and / or y direction. This ensures that when immersing the micro ejection pump in a liquid has very little surface contamination takes place, which then takes place in one cleaning step can be easily removed accordingly. So that can can be prevented in a simple manner that substances unintentionally and can be carried away unnoticed.
- the invention Micro ejection pump is therefore also for manipulation smallest amounts of liquid particularly suitable.
- the taper in the x direction can be advantageous during the sawing of the silicon chip are formed, whereas the taper in the y direction during the anisotropic Structure etching can be formed.
- the silicon chip heated directly and temperature-controlled i.e. it will the ohmic resistance of the silicon is exploited by the Heating effect due to Joule heat generated in the silicon material becomes.
- the heater is preferably integrated in the silicon membrane, or acts directly on them, the electrical contacts arranged laterally opposite on the silicon chip are.
- liquids can e.g. containing glucose or be oily substances that are then exploited the advantages of the diffuser element are promoted can.
- Metals e.g. Tin or tin-lead alloys, or other substances that are otherwise due to their viscosity in the Micro ejection pump are not eligible, easily promoted become. These substances can then be thermally activated promoted and also printed.
- the electrical contacts and the temperature sensor should be off a chemically neutral material, with photolithography structured platinum or tantalum layers for this are particularly suitable.
- a particularly advantageous continuation of the invention is through a parallel arrangement of several pumping chambers an associated inlet diffuser and outlet channels.
- the micro ejection pump 1 shown in FIGS. 1 to 3 consists of a composite of a silicon chip 2 and a Glass chip 3 connected by anodic bonding are.
- the silicon chip 2 is structured on two sides, wherein a flat one on the side opposite the glass chip 3
- Pump chamber 4 is formed by a silicon membrane 5 is closed to the outside (Fig. 2).
- a piezoelectric plate actuator 6 On this silicon membrane 5 is a piezoelectric plate actuator 6, for example attached by means of the known chip bonding technology. This plate actuator is used to deflect the Silicon membrane 5, so that the volume of the pump chamber 4 alternately is enlarged or reduced, which increases the pumping effect is achieved.
- the control of the piezoelectric plate actuator 6 can by an electronic control, not shown predetermined frequency and amplitude. It did proved to be useful for the switch-on pulse high slope, i.e. a sudden switch-on pulse pretend.
- the subsequent switch-off pulse can be a damped one have a flat course, e.g. corresponding to an e-function.
- the pump behavior of the invention is thus Micro ejection pump further improved.
- the piezoelectric plate actuator 6 with a bias voltage before the switch-on pulse apply.
- the bias should be the polarity of the Switching impulse be opposite.
- the pump chamber 4 with an inlet channel 7 and provided an outlet channel 8, the outlet channel 8 with an ejection opening 9 for ejecting individual microdroplets 10 is provided.
- the pump chamber 4 essentially has one square or rectangular plan, with the an inlet channel 7 in connected to a fluid inlet 16 (FIGS. 8, 9) an entrance zone of the pump chamber 4 opens.
- the outlet duct 8 is arranged on the opposite side of the pump chamber.
- the pump chamber 4 can also have a floor plan have curved boundary lines and, for example, round (Fig. 4), or also oval (Fig. 9).
- the inlet channel 7 is designed as a diffuser element 11, i.e. the inlet channel 7, or part of the same widens in Direction to the pump chamber 4.
- the diffuser element 11 can be designed such that the opening angle over the entire length of the diffuser element 11 is constant. Of course it is also possible to use the diffuser element 11 in this way to design that the opening angle changes constantly. So the opening angle can be within predetermined limits also increase continuously (Fig. 9)
- microcapillary Outlet channel 8 between the pump chamber 4 and the discharge opening 9 it is possible to use the microcapillary Outlet channel 8 between the pump chamber 4 and the discharge opening 9 to be connected to other inlet channels.
- other substances are added, which is the possible uses the micro ejection pump has been expanded considerably.
- the diffuser element 11 enables stable operation via a large frequency range, or the delivery rate over the excitation frequency for the plate actuator 6 is regulated be, with a particularly steep switch-on pulse and a flat switch-off pulse are particularly advantageous because the formation of gas bubbles in the pump chamber 4 also is prevented.
- Micro ejection pump Another extension of the application possibilities for the Micro ejection pump enables heating to be integrated at least into the silicon membrane 5 of the silicon chip 2.
- the micro ejection pump 1 can therefore not only be used for handling of liquids or suspensions with low viscosity are used, but also for such materials that with an increase in temperature low or low viscosity become. Another aspect of integrated heating is in it to see that this also results in a simple drying of the wetted Areas of the micro ejection pump 1 is made possible. For example can result in outer wetted areas of the micro ejection pump 1 can be dried quickly, causing a carryover of liquids can be safely prevented.
- the integration of the heater can be done easily take place that the electrical resistance of the silicon chip 2nd is used directly for heating. These are for electrical Contacting electrical contacts 17, 18 provided which are laterally opposite on the silicon chip 2 extend (Fig. 8).
- temperature sensor 19 with associated Control circuit 20 can thus also be highly viscous per se Liquids or suspensions, such as oils, fats or Liquids containing glucose by the micro ejection pump 1 be promoted. If the heating is designed accordingly this way, even fusible metals can be extracted, so that the micro ejection pump 1 also for printing Metals such as tin or lead-tin alloys or others Is suitable.
- the area of application of the micro ejection pump 1 is basically is not restricted, all parts must be filled with liquids can come into contact, be chemically neutral. Out for this reason it is advisable to have the electrical contacts 17, 18 and the temperature sensor 19 from a photolithographic structured platinum or tantalum layer.
- the composite from the silicon chip 2 and the glass chip 3 towards the discharge opening 9 of the Outlet channel 8 is tapered in the x and / or y direction, such as this is shown in principle in FIGS. 6 to 9. That can in that the taper 14 in the x direction during of sawing the silicon chip 2 is formed.
- the Taper 15 in the y direction can be easily during the anisotropic structure etching of the semiconductor chip 2 form.
- the taper 14; 15 also through a final grinding process are formed, wherein in this case also a taper of the glass chip 3 in the y direction can be manufactured.
- the immersion area of the Micro ejection pump 1 with a hydrophobic surface treatment is another way to keep this contamination to a minimum to be able to hold.
- This can be done by silanization or by coating e.g. with a layer that is a Teflon coating is similar.
- This layer of carbon and fluorine can be made using the plasma polymerization process getting produced.
- the internal channel and Chamber area of the micro ejection pump 1 not coated with becomes.
- the advantages of the invention can be seen in the fact that Diffuser element 11 a significant improvement in frequency stability the micro ejection pump 1 is reached.
- the anisotropy the flow resistance of the diffuser element 11 supports the formation of the microdrops 10 in the pump mode, i.e. there is a nozzle effect along the positive pressure gradient.
- the liquid afterflow supported i.e. there is a diffuser effect along the positive pressure gradient.
- the generation by the diffuser effect in loading mode of air bubbles in the pump chamber 4 especially at high ones Excitation frequencies of the plate actuator 6 effectively suppressed. So that the micro ejection pump 1 is large Frequency spectrum can be used and it can also be extremely high Delivery rates up to approx. 750 ⁇ l / min, with an excitation frequency up to approx. 6500 Hz.
- the micro ejection pump 1 for any liquids, Suspensions also of higher viscosity and also meltable Metals and the like be used when these materials in a reasonable temperature range sufficiently low viscosity can be made. As already explained, a quick drying of wetted areas of the micro ejection pump 1 bring about.
- the supply of the materials to be handled from a storage container to the pumping chamber 4 can be via conventional hose lines respectively.
- the application of the design of the micro ejection pump according to the invention 1 with the diffuser element 11 is not on it limited that only one pump chamber 4 is present. It is easily possible to create micro ejection pumps, the one Parallel arrangement of pumping chambers 4 in connection with the Have diffuser elements 11 according to the invention (FIG. 5).
- micro ejection pump according to the invention 1 can by the application of the known microtechnical Microforming take place and the connection of the Silicon chips 2 with the glass chip 3 using the anodic Bonding.
- Silicon chip 2 In a first preparation process, consisting of the sub-steps thermal oxidation, photolithography and anisotropic Structural etching is first the two-sided structure Silicon chip 2 manufactured.
- This silicon chip 2 receives the structures of a micro ejection pump 1 with the outlet channel 8, the pump chamber 4 with associated silicon membrane 5 and the inlet channel 7 with the diffuser element 11.
- the structured in this way Silicon chip 2 is used after a multi-stage cleaning a glass chip 3, consisting of a Pyrex 7740 glass plate, through anodic bonding to a solid silicon-glass composite together.
- the production of the parallel arrangement can done in the same manner as described above.
- the thickness of the glass plate is, for example, 1 mm and the silicon membrane between 50 - 190 ⁇ m.
- the thickness of the piezoelectric Plate actuators 6 should be in the range of 100 - 260 ⁇ m.
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Reciprocating Pumps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
- Fig. 1
- eine schematisch im Schnitt dargestellte Draufsicht auf die Mikroejektionspumpe;
- Fig. 2
- eine im Schnitt dargestellte Seitenansicht der Mikroejektionspumpe nach Fig. 1;
- Fig. 3
- die Draufsicht auf die Mikroejektionspumpe nach Fig. 1 und 2;
- Fig. 4
- eine schematische Darstellung einer Variante der Mikroejektionspumpe mit runder Pumpkammer;
- Fig. 5
- eine Mikroejektionspumpe mit einem Mehrkanalsystem;
- Fig. 6
- eine Mikroejektionspumpe mit Verjüngungen in x-Richtung;
- Fig. 7
- eine Mikroejektionspumpe mit Verjüngungen in y-Richtung;
- Fig. 8
- die Rückansicht des Siliziumchips für eine Mikroejektionspumpe mit Temperatursensor und Steuerschaltung; und
- Fig. 9
- die Vorderansicht des Siliziumchips nach Fig. 8 mit ovaler Pumpkammer.
- 1
- Mikroejektionspumpe
- 2
- Siliziumchip
- 3
- Glaschip
- 4
- Pumpkammer
- 5
- Siliziummembran
- 6
- Plattenaktuator
- 7
- Zulaufkanal
- 8
- Auslaßkanal
- 9
- Ausstoßöffnung
- 10
- Mikrotropfen
- 11
- Diffusorelement
- 12
- Zulaufkanal
- 13
- Zulaufkanal
- 14
- Verjüngung in x-Richtung
- 15
- Verjüngung in y-Richtung
- 16
- Fluideinlaß
- 17
- Rontakt
- 18
- Kontakt
- 19
- Temperatursensor
- 20
- Steuerschaltung
- 21
- Absaugkanal
- 22
- Austrittsebene
Claims (18)
- Mikroejektionspumpe zur Generation von Mikrotropfen, bestehend aus mindestens einer in einem Siliziumchip ausgebildeten Pumpkammer, einer über der Pumpkammer angeordneten und piezoelektrisch betätigbaren Siliziummembran, wobei die Pumpkammer mit wenigstens einem Zulaufkanal und einem mit einer Ausstoßöffnung versehenen Auslaßkanal verbunden ist und bei der ein Glaschip gegenüber der Siliziummembran die Pumpkammer verschließt, wobei sich der Zulauf- und der Auslaßkanal (7, 8) auf gegenüberliegenden Seiten der Pumpkammer (4) befinden, dadurch gekennzeichnet, daß der im Siliziumchip (2) befindliche Zulaufkanal (7) in Richtung zur Pumpkammer (4) zumindest teilweise als Diffusorelement (11) mit einem Öffnungswinkel bis 10° ausgebildet ist und daß der Auslaßkanal (8) als Mikrokapillare ausgebildet ist, die mit einer Ausstoßöffnung (9) in einer Austrittsebene (22) mündet.
- Mikroejektionspumpe nach Anspruch 1, dadurch gekennzeichnet, daß das Diffusorelement (11) der Pumpkammer (4) unmittelbar vorgeordnet ist.
- Mikroejektionspumpe nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß das Diffusorelement (11) einen konstanten Öffnungswinkel aufweist.
- Mikroejektionspumpe nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß der Öffnungswinkel bevorzugt 3 - 5 ° beträgt.
- Mikroejektionspumpe nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß das Diffusorelement (11) einen sich stetig verändernden Öffnungswinkel aufweist.
- Mikroejektionspumpe nach den Ansprüchen 1 bis 5, dadurch gekennzeichnet, daß die Pumpkammer (4) einen Grundriß mit geraden oder gekrümmten Begrenzungslinien aufweist.
- Mikroejektionspumpe nach den Ansprüchen 1 bis 6, dadurch gekennzeichnet, daß der Auslaßkanal (8) zwischen der Pumpkammer (4) und der Ausstoßöffnung (9) mit weiteren Zulaufkanälen verbindbar ist.
- Mikroejektionspumpe nach den Ansprüchen 1 bis 7, gekennzeichnet durch einen Verbund aus einem mikromechanisch strukturierten Siliziumchip (2) und einem Glaschip (3).
- Mikroejektionspumpe nach Anspruch 8, dadurch gekennzeichnet, daß der Verbund aus dem Siliziumchip (2) und dem Glaschip (3) in Richtung zur Ausstoßöffnung (9) des Auslaßkanales (8) in x- und/oder y-Richtung verjüngt ist.
- Mikroejektionspumpe nach Anspruch 9, dadurch gekennzeichnet, daß die Verjüngung (14) in x-Richtung während des Trennsägens des Siliziumchips (2) ausgebildet worden ist.
- Mikroejektionspumpe nach Anspruch 9, dadurch gekennzeichnet, daß die Verjüngung (15) in y-Richtung während des anisotropen Strukturätzens ausgebildet worden ist.
- Mikroejektionspumpe nach Anspruch 9, dadurch gekennzeichnet, daß die Verjüngung (14; 15) durch einen abschließenden Schleifprozeß ausgebildet worden ist.
- Mikroejektionspumpe nach einem der Ansprüche 1 bis 12, dadurch gekennzeichnet, daß das Siliziumchip (2) direkt und temperaturgeregelt beheizbar ist.
- Mikroejektionspumpe nach Anspruch 13, dadurch gekennzeichnet, daß die Heizung in die Siliziummembran (5) des Siliziumchips (2) integriert ist und daß die elektrischen Kontakte (17, 18) einander seitlich gegenüberliegend am Siliziumchip (2) angeordnet sind.
- Mikroejektionspumpe nach Anspruch 13 und 14, dadurch gekennzeichnet, daß auf dem Siliziumchip (2) ein Temperatursensor (19) mit zugehöriger Steuerschaltung (20) angeordnet ist.
- Mikroejektionspumpe nach den Ansprüchen 13 bis 15, dadurch gekennzeichnet, daß die elektrischen Kontakte (17, 18) und der Temperatursensor (19) aus einer fotolithografisch strukturierten Platin- oder Tantalschicht bestehen.
- Mikroejektionspumpe nach den Ansprüchen 1 bis 16, gekennzeichnet durch eine Parallelanordnung von mehreren Pumpkammern (4) mit jeweils einem Einlaßdiffusor (11) und Auslaßkanälen (8).
- Mikroejektionspumpe nach Anspruch 17, dadurch gekennzeichnet, daß zwischen den Auslaßkanälen (8) in der Austrittsebene (22) Absaugkanäle (21) münden.
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19651568 | 1996-12-11 | ||
DE19651568 | 1996-12-11 | ||
PCT/DE1997/002874 WO1998026179A1 (de) | 1996-12-11 | 1997-12-11 | Mikroejektionspumpe |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0956449A1 EP0956449A1 (de) | 1999-11-17 |
EP0956449B1 true EP0956449B1 (de) | 2002-05-29 |
Family
ID=7814406
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP97951842A Revoked EP0956449B1 (de) | 1996-12-11 | 1997-12-11 | Mikroejektionspumpe |
Country Status (6)
Country | Link |
---|---|
US (1) | US6179584B1 (de) |
EP (1) | EP0956449B1 (de) |
JP (1) | JP2001505640A (de) |
AT (1) | ATE218194T1 (de) |
DE (2) | DE59707378D1 (de) |
WO (1) | WO1998026179A1 (de) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010149595A1 (de) | 2009-06-25 | 2010-12-29 | Tecan Trading Ag | Funktionskontrolle bzw. varianzenkompensation in der massenspektrometrie |
Families Citing this family (51)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
RU2143596C1 (ru) * | 1998-09-08 | 1999-12-27 | Попов Сергей Анатольевич | Жидкостно-газовый эжектор |
DE19913076A1 (de) | 1999-03-23 | 2000-10-19 | Hahn Schickard Ges | Vorrichtung und Verfahren zum Aufbringen von Mikrotröpfchen auf ein Substrat |
EP1128075A3 (de) * | 2000-02-24 | 2003-10-29 | Fraunhofer-Gesellschaft Zur Förderung Der Angewandten Forschung E.V. | Mikropumpe und/oder Mikromischer mit integriertem Sensor und Verfahren zu dessen Herstellung |
AUPQ669000A0 (en) * | 2000-04-04 | 2000-05-04 | Cooke, Richard | Screen display device |
US6530755B2 (en) | 2000-04-07 | 2003-03-11 | Tecan Trading Ag | Micropump |
KR20030034192A (ko) * | 2000-09-18 | 2003-05-01 | 클리포드 엔. 로젠 | 압전 액추에이터 및 이를 사용하는 펌프 |
US7198250B2 (en) * | 2000-09-18 | 2007-04-03 | Par Technologies, Llc | Piezoelectric actuator and pump using same |
EP1332000B1 (de) | 2000-10-30 | 2012-06-20 | Sequenom, Inc. | Verfahren zur aufbringung von submikroliter fluid-volumina auf ein substrat |
US20040073175A1 (en) * | 2002-01-07 | 2004-04-15 | Jacobson James D. | Infusion system |
US6869275B2 (en) * | 2002-02-14 | 2005-03-22 | Philip Morris Usa Inc. | Piezoelectrically driven fluids pump and piezoelectric fluid valve |
US20030163111A1 (en) * | 2002-02-26 | 2003-08-28 | Daellenbach Keith K. | End effector for needle-free injection system |
FR2839662B1 (fr) * | 2002-05-16 | 2005-12-02 | Centre Nat Rech Scient | Dispositif de depot localise d'au moins une solution biologique |
US8080221B2 (en) | 2002-08-05 | 2011-12-20 | Palo Alto Research Center Incorporated | Capillary-channel probes for liquid pickup, transportation and dispense using stressy metal |
US7241420B2 (en) | 2002-08-05 | 2007-07-10 | Palo Alto Research Center Incorporated | Capillary-channel probes for liquid pickup, transportation and dispense using stressy metal |
MXPA05011246A (es) * | 2003-04-21 | 2006-07-06 | Stratagen Life Sciences Inc | Metodos y aparatos para la administracion repetitiva de farmacos por microchorro. |
FR2861814B1 (fr) * | 2003-11-04 | 2006-02-03 | Cit Alcatel | Dispositif de pompage par micropompes a transpiration thermique |
WO2005060593A2 (en) * | 2003-12-10 | 2005-07-07 | Purdue Research Foundation | Micropump for electronics cooling |
US7290993B2 (en) * | 2004-04-02 | 2007-11-06 | Adaptivenergy Llc | Piezoelectric devices and methods and circuits for driving same |
US7312554B2 (en) * | 2004-04-02 | 2007-12-25 | Adaptivenergy, Llc | Piezoelectric devices and methods and circuits for driving same |
US7287965B2 (en) * | 2004-04-02 | 2007-10-30 | Adaptiv Energy Llc | Piezoelectric devices and methods and circuits for driving same |
US20050225201A1 (en) * | 2004-04-02 | 2005-10-13 | Par Technologies, Llc | Piezoelectric devices and methods and circuits for driving same |
CN1583541B (zh) * | 2004-05-27 | 2010-09-29 | 哈尔滨工程大学 | 采用多层驱动膜结构的微驱动器及其制作方法 |
US7104767B2 (en) * | 2004-07-19 | 2006-09-12 | Wilson Greatbatch Technologies, Inc. | Diaphragm pump for medical applications |
JP4626224B2 (ja) * | 2004-08-27 | 2011-02-02 | 富士ゼロックス株式会社 | マイクロポンプ |
JP4645159B2 (ja) * | 2004-11-02 | 2011-03-09 | コニカミノルタホールディングス株式会社 | マイクロポンプ |
US7258533B2 (en) * | 2004-12-30 | 2007-08-21 | Adaptivenergy, Llc | Method and apparatus for scavenging energy during pump operation |
US20060147329A1 (en) * | 2004-12-30 | 2006-07-06 | Tanner Edward T | Active valve and active valving for pump |
EP1875525A2 (de) * | 2005-04-13 | 2008-01-09 | Par Technologies, LLC. | Piezoelektrische membranbaugruppe mit leitern auf flexiblem film |
US20060232166A1 (en) * | 2005-04-13 | 2006-10-19 | Par Technologies Llc | Stacked piezoelectric diaphragm members |
JP3896141B2 (ja) * | 2005-06-28 | 2007-03-22 | シャープ株式会社 | マイクロポンプおよびマイクロポンプシステム |
DE202006010293U1 (de) * | 2005-07-22 | 2006-08-31 | Tecan Trading Ag | Pipettiergerät mit Computerprogrammprodukt zum Akzeptieren oder Verwerfen von pipettierten Flüssigkeitsproben |
JP4779126B2 (ja) * | 2005-07-27 | 2011-09-28 | 国立大学法人九州工業大学 | バルブレスマイクロポンプ |
US8998881B2 (en) * | 2005-08-10 | 2015-04-07 | Alza Corporation | Method for delivering drugs to tissue under microjet propulsion |
EP1921648A1 (de) * | 2005-08-31 | 2008-05-14 | Matsushita Electric Works, Ltd. | Relaisvorrichtung mit leiterflüssigkeit |
US20070075286A1 (en) * | 2005-10-04 | 2007-04-05 | Par Technologies, Llc | Piezoelectric valves drive |
US20070129681A1 (en) * | 2005-11-01 | 2007-06-07 | Par Technologies, Llc | Piezoelectric actuation of piston within dispensing chamber |
US7345407B2 (en) * | 2005-11-18 | 2008-03-18 | Adaptivenergy, Llc. | Human powered piezoelectric power generating device |
KR100804686B1 (ko) | 2006-11-23 | 2008-02-18 | 한국에너지기술연구원 | 기포 동력 마이크로 펌프 |
US20080246367A1 (en) * | 2006-12-29 | 2008-10-09 | Adaptivenergy, Llc | Tuned laminated piezoelectric elements and methods of tuning same |
US20090180931A1 (en) | 2007-09-17 | 2009-07-16 | Sequenom, Inc. | Integrated robotic sample transfer device |
US8040022B2 (en) * | 2007-12-12 | 2011-10-18 | Aprolase Development Co., Llc | Forced vibration piezo generator and piezo actuator |
US8197235B2 (en) * | 2009-02-18 | 2012-06-12 | Davis David L | Infusion pump with integrated permanent magnet |
US20100211002A1 (en) * | 2009-02-18 | 2010-08-19 | Davis David L | Electromagnetic infusion pump with integral flow monitor |
US8353864B2 (en) * | 2009-02-18 | 2013-01-15 | Davis David L | Low cost disposable infusion pump |
US8579414B2 (en) | 2009-12-23 | 2013-11-12 | Xerox Corporation | Self-assembling structures for electrostatic extraction of pigments from liquid inks for marking |
KR101153613B1 (ko) * | 2010-05-25 | 2012-06-18 | 삼성전기주식회사 | 마이크로 이젝터 및 그 제조방법 |
CN103429348B (zh) | 2011-01-21 | 2016-03-09 | 拜奥-多特公司 | 具有纵向变换器和可替换毛细管的压电分配器 |
US10126264B2 (en) | 2014-07-14 | 2018-11-13 | Li-Cor, Inc. | Analyte separator with electrohydrodynamic Taylor cone jet blotter |
AU2017213725B2 (en) | 2016-02-01 | 2021-12-23 | Li-Cor, Inc. | Capillary electrophoresis inkjet dispensing |
CN109564188A (zh) | 2016-08-08 | 2019-04-02 | 利康公司 | 微芯片电泳喷墨式分配 |
AU2017311105A1 (en) | 2016-08-08 | 2019-02-21 | Li-Cor, Inc. | Multi-sheath flow and on-chip terminating electrode for microfluidic direct-blotting |
Family Cites Families (19)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4152098A (en) * | 1977-01-03 | 1979-05-01 | Clark Ivan P | Micropump |
EP0408306B1 (de) * | 1989-07-11 | 1996-05-01 | Ngk Insulators, Ltd. | Einen piezoelektrischen/elektrostriktiven Film enthaltende piezoelektrischer/elektrostriktiver Antrieb |
KR910012538A (ko) * | 1989-12-27 | 1991-08-08 | 야마무라 가쯔미 | 마이크로 펌프 및 그 제조 방법 |
US5094594A (en) | 1990-04-23 | 1992-03-10 | Genomyx, Incorporated | Piezoelectric pumping device |
DE69106240T2 (de) * | 1990-07-02 | 1995-05-11 | Seiko Epson Corp | Mikropumpe und Verfahren zur Herstellung einer Mikropumpe. |
US5277556A (en) * | 1990-07-10 | 1994-01-11 | Westonbridge International Limited | Valve and micropump incorporating said valve |
SE508435C2 (sv) * | 1993-02-23 | 1998-10-05 | Erik Stemme | Förträngningspump av membranpumptyp |
SE501139C2 (sv) * | 1993-04-08 | 1994-11-21 | Sem Ab | Anordning vid fluidpump av membrantyp |
US5659171A (en) * | 1993-09-22 | 1997-08-19 | Northrop Grumman Corporation | Micro-miniature diaphragm pump for the low pressure pumping of gases |
CH689836A5 (fr) * | 1994-01-14 | 1999-12-15 | Westonbridge Int Ltd | Micropompe. |
DE4402119C2 (de) * | 1994-01-25 | 1998-07-23 | Karlsruhe Forschzent | Verfahren zur Herstellung von Mikromembranpumpen |
DE4422743A1 (de) * | 1994-06-29 | 1996-01-04 | Torsten Gerlach | Mikropumpe |
US5856174A (en) * | 1995-06-29 | 1999-01-05 | Affymetrix, Inc. | Integrated nucleic acid diagnostic device |
WO1997011275A1 (en) * | 1995-09-20 | 1997-03-27 | Philips Electronics N.V. | Pump and method for manufacturing the pump |
US5840062A (en) * | 1995-11-08 | 1998-11-24 | Gumaste; Anand V. | Solid state fluid delivery system |
US6054277A (en) * | 1996-05-08 | 2000-04-25 | Regents Of The University Of Minnesota | Integrated microchip genetic testing system |
US5779868A (en) * | 1996-06-28 | 1998-07-14 | Caliper Technologies Corporation | Electropipettor and compensation means for electrophoretic bias |
US5871336A (en) * | 1996-07-25 | 1999-02-16 | Northrop Grumman Corporation | Thermal transpiration driven vacuum pump |
DE19720482C5 (de) * | 1997-05-16 | 2006-01-26 | INSTITUT FüR MIKROTECHNIK MAINZ GMBH | Mikromembranpumpe |
-
1997
- 1997-12-11 EP EP97951842A patent/EP0956449B1/de not_active Revoked
- 1997-12-11 DE DE59707378T patent/DE59707378D1/de not_active Revoked
- 1997-12-11 DE DE29724735U patent/DE29724735U1/de not_active Expired - Lifetime
- 1997-12-11 JP JP52608798A patent/JP2001505640A/ja active Pending
- 1997-12-11 WO PCT/DE1997/002874 patent/WO1998026179A1/de not_active Application Discontinuation
- 1997-12-11 AT AT97951842T patent/ATE218194T1/de not_active IP Right Cessation
-
1999
- 1999-06-10 US US09/330,121 patent/US6179584B1/en not_active Expired - Fee Related
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2010149595A1 (de) | 2009-06-25 | 2010-12-29 | Tecan Trading Ag | Funktionskontrolle bzw. varianzenkompensation in der massenspektrometrie |
Also Published As
Publication number | Publication date |
---|---|
US6179584B1 (en) | 2001-01-30 |
WO1998026179A1 (de) | 1998-06-18 |
JP2001505640A (ja) | 2001-04-24 |
EP0956449A1 (de) | 1999-11-17 |
DE59707378D1 (de) | 2002-07-04 |
ATE218194T1 (de) | 2002-06-15 |
DE29724735U1 (de) | 2003-11-13 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
EP0956449B1 (de) | Mikroejektionspumpe | |
DE102005037401B4 (de) | Bildung einer Emulsion in einem fluidischen Mikrosystem | |
DE60216748T2 (de) | Flüssigkeitspumpsystem | |
DE10227593B4 (de) | Strömungsschaltungs-Mikrobauelemente | |
DE102005048259B4 (de) | Vorrichtung und Verfahren zur Erzeugung eines Gemenges von zwei ineinander unlösbaren Phasen | |
EP1270073B1 (de) | Mikrofluid-System mit Regler | |
DE60310997T2 (de) | Mikrofluides system mit stabilisierter flüssig-flüssig-grenzfläche | |
DE19720482A1 (de) | Mikromembranpumpe | |
DE19648458C1 (de) | Mikromechanische Ejektionspumpe zum Heraustrennen kleinster Fluidvolumina aus einem strömenden Probenfluid | |
DE69909753T2 (de) | Apparat zur abgabe einer vorherbestimmten flüssigkeitsmenge | |
WO2012048685A1 (de) | Flusszelle mit hohlraum und diaphragma | |
DE112005000445T5 (de) | Mikrochemisches System | |
DE10010208C2 (de) | Mikrodosiervorrichtung zur definierten Abgabe kleiner in sich geschlossener Flüssigkeitsvolumina | |
DE112017000632T5 (de) | Vertikaler Mikrofluidik-Sondenkopf mit Öffnungen für eine großmaßstäbliche Oberflächenbearbeitung | |
WO2004071660A1 (de) | Verfahren und vorrichtung zum kontaktieren einer mikrofluidikstruktur | |
EP2830764B1 (de) | Fluidisches system umfassend eine poröse membran mit veränderbarer porenoberfläche und verfahren zum betreiben desselben | |
EP2449296B1 (de) | Ventil | |
WO2002040165A1 (de) | Vorrichtung und system zur abgabe bzw. aufnahme/abgabe von flüssigkeitsproben | |
EP0672834B1 (de) | Mikro-Fluidmanipulator | |
DE10250406B4 (de) | Reaktionsvorrichtung und Mischsystem | |
WO2010054830A1 (de) | Vorrichtung und verfahren zum erzeugen eines tropfens einer flüssigkeit | |
DE19611270A1 (de) | Mikromischer zur Handhabung kleinster Flüssigkeitsmengen | |
EP2593231A1 (de) | Mikrofluidisches system und herstellungsverfahren für ein mikrofluidisches system | |
WO2010142471A1 (de) | Vorrichtung und verfahren zur erzeugung und/oder anordnung von sequenzen einer oder mehrerer fluidproben in einem trägerfluid | |
DE29708678U1 (de) | Mikromembranpumpe |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
17P | Request for examination filed |
Effective date: 19990528 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AT BE CH DE DK FI FR GB IT LI NL SE |
|
GRAG | Despatch of communication of intention to grant |
Free format text: ORIGINAL CODE: EPIDOS AGRA |
|
17Q | First examination report despatched |
Effective date: 20010718 |
|
GRAG | Despatch of communication of intention to grant |
Free format text: ORIGINAL CODE: EPIDOS AGRA |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAH | Despatch of communication of intention to grant a patent |
Free format text: ORIGINAL CODE: EPIDOS IGRA |
|
GRAA | (expected) grant |
Free format text: ORIGINAL CODE: 0009210 |
|
AK | Designated contracting states |
Kind code of ref document: B1 Designated state(s): AT BE CH DE DK FI FR GB IT LI NL SE |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: NL Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20020529 Ref country code: LI Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20020529 Ref country code: IT Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRE;WARNING: LAPSES OF ITALIAN PATENTS WITH EFFECTIVE DATE BEFORE 2007 MAY HAVE OCCURRED AT ANY TIME BEFORE 2007. THE CORRECT EFFECTIVE DATE MAY BE DIFFERENT FROM THE ONE RECORDED.SCRIBED TIME-LIMIT Effective date: 20020529 Ref country code: GB Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20020529 Ref country code: FR Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20020529 Ref country code: FI Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20020529 Ref country code: CH Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES Effective date: 20020529 |
|
REF | Corresponds to: |
Ref document number: 218194 Country of ref document: AT Date of ref document: 20020615 Kind code of ref document: T |
|
REG | Reference to a national code |
Ref country code: GB Ref legal event code: FG4D Free format text: NOT ENGLISH |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: EP |
|
REF | Corresponds to: |
Ref document number: 59707378 Country of ref document: DE Date of ref document: 20020704 |
|
PG25 | Lapsed in a contracting state [announced via postgrant information from national office to epo] |
Ref country code: SE Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20020829 Ref country code: DK Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT Effective date: 20020829 |
|
NLV1 | Nl: lapsed or annulled due to failure to fulfill the requirements of art. 29p and 29m of the patents act | ||
GBV | Gb: ep patent (uk) treated as always having been void in accordance with gb section 77(7)/1977 [no translation filed] |
Effective date: 20020529 |
|
PGFP | Annual fee paid to national office [announced via postgrant information from national office to epo] |
Ref country code: DE Payment date: 20030108 Year of fee payment: 6 |
|
EN | Fr: translation not filed | ||
PLBI | Opposition filed |
Free format text: ORIGINAL CODE: 0009260 |
|
PLBQ | Unpublished change to opponent data |
Free format text: ORIGINAL CODE: EPIDOS OPPO |
|
PLBF | Reply of patent proprietor to notice(s) of opposition |
Free format text: ORIGINAL CODE: EPIDOS OBSO |
|
26 | Opposition filed |
Opponent name: TECAN TRADING AG Effective date: 20030217 |
|
PLBF | Reply of patent proprietor to notice(s) of opposition |
Free format text: ORIGINAL CODE: EPIDOS OBSO |
|
RDAH | Patent revoked |
Free format text: ORIGINAL CODE: EPIDOS REVO |
|
RDAG | Patent revoked |
Free format text: ORIGINAL CODE: 0009271 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: PATENT REVOKED |
|
REG | Reference to a national code |
Ref country code: CH Ref legal event code: PL |
|
27W | Patent revoked |
Effective date: 20030424 |