EP0672835B1 - Micro diode fluidique - Google Patents
Micro diode fluidique Download PDFInfo
- Publication number
- EP0672835B1 EP0672835B1 EP95101737A EP95101737A EP0672835B1 EP 0672835 B1 EP0672835 B1 EP 0672835B1 EP 95101737 A EP95101737 A EP 95101737A EP 95101737 A EP95101737 A EP 95101737A EP 0672835 B1 EP0672835 B1 EP 0672835B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- fluid
- micro
- silicon
- diode
- capillaries
- 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.)
- Expired - Lifetime
Links
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F15—FLUID-PRESSURE ACTUATORS; HYDRAULICS OR PNEUMATICS IN GENERAL
- F15C—FLUID-CIRCUIT ELEMENTS PREDOMINANTLY USED FOR COMPUTING OR CONTROL PURPOSES
- F15C4/00—Circuit elements characterised by their special functions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/30—Injector mixers
- B01F25/31—Injector mixers in conduits or tubes through which the main component flows
- B01F25/314—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit
- B01F25/3142—Injector mixers in conduits or tubes through which the main component flows wherein additional components are introduced at the circumference of the conduit the conduit having a plurality of openings in the axial direction or in the circumferential direction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/30—Micromixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/206—Flow affected by fluid contact, energy field or coanda effect [e.g., pure fluid device or system]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/206—Flow affected by fluid contact, energy field or coanda effect [e.g., pure fluid device or system]
- Y10T137/2224—Structure of body of device
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T137/00—Fluid handling
- Y10T137/8593—Systems
- Y10T137/87571—Multiple inlet with single outlet
- Y10T137/87652—With means to promote mixing or combining of plural fluids
Definitions
- the invention relates to a micro-fluid diode that is only permeable to fluid in one direction directional coupling of submicroliter amounts of one fluid medium into another standing or flowing target fluid in a closed system.
- Appropriate Requirements exist when dosing, mixing and injecting fluids in the sub-microliter range for applications in particular in the field of biomedical engineering and chemical microsensor technology.
- Liquid is a widely used procedure in the field of medical technology and Flow injection analysis. It is known to be by injecting through a rubber septum [P. W. Alexander et al., Analyst 107 (1982) 1335] or using rotary injection valves [M. D. Luque de Castro et al., Analyst 109 (1984) 413] or based on the hydrodynamic injection [J. Ruzicka et al., Anal. Chim. Acta, 145 (1983) 1].
- the devices that use these techniques and are currently commercially available are based exclusively on costly precision mechanical manufacturing technologies.
- the aim of the invention is to avoid adhering to the micromechanical valves Problems a technical solution for coupling a dosing fluid into a standing one or flowing target fluid can be found, which has a high dosing accuracy in the Has submicroliter range and maximum security against penetration of the target fluid into the dosing fluid.
- the object is achieved by a micro-fluid diode which is only permeable to fluid in one direction and which consists of one or a system of a plurality of microcapillaries which are open on both sides and are in direct contact on the output side with the target fluid and whose input side facing the metering fluid is provided by an air or gas cushion is separated from the metering fluid so that the target fluid that expands in the capillaries is prevented from advancing due to the surface tension with the formation of a meniscus.
- the metering fluid is applied to this meniscus discontinuously, preferably as a self-supporting fluid jet, and is coupled into the target fluid as a result of diffusion or convection processes.
- the micro-fluid diode according to the invention is preferably integrated into a microtechnical flow channel, whereby it reliably prevents the liquid (target fluid) standing or flowing in the flow channel from escaping and at the same time ensures the entry of a second liquid (metering fluid) to be applied to the micro-fluid diode from the outside.
- a coupling surface for the introduction of microdrops of a metering fluid is formed by the large number of open capillaries directed outwards.
- the gas-liquid interface at each end of the microcapillaries is a mandatory prerequisite for the maintenance of the micro-fluid diode function at all times for the component functions and thus part of the component.
- the microcapillaries have three-dimensional dimensions in the ⁇ m range and, due to the high precision requirements for their geometry, are preferably manufactured by anisotropic etching on ⁇ 100> or ⁇ 110> silicon substrates.
- the length of each individual microcapillary is to be dimensioned such that the target fluid extends up to the capillary ends, and there, under the influence of the surface tension and the acting fluidic gravity pressures, forms a defined liquid-gas interface in the form of a meniscus at each microcapillary end.
- each meniscus With the formation of each meniscus, the process of spreading the liquid in the corresponding microcapillary is completed and the coupling surface is thus brought into a reproducible state.
- This state represents the prevailing equilibrium between the static gravity pressures and, in the event that the target fluid moves in the flow channel, the dynamic hydrostatic pressures. As long as the equilibrium conditions of the pressures are met, the desired directional dependence exists on all menisci of the entire coupling area. This means that the target fluid moved or standing in the flow channel does not leave the microcapillaries in the direction of the droplet chamber, but a metering fluid sprayed through the gas space of the droplet chamber onto any meniscus can get into the interior of the microcapillary and thus the flow channel.
- the unhindered entry of the second liquid into the flow channel via the meniscus of the first liquid takes place via diffusion and / or convection mechanisms.
- the flow velocity in the flow channel is exactly zero or the microcapillaries of the micro fluid diode are chosen long enough, only the diffusion component comes into play when the metering and target fluids are mixed. All flow velocities other than zero in the channel lead directly to the formation of convection components in the microcapillary, which are also superimposed by diffusion components.
- the rate of inflow of the metering fluid through the microcapillaries of the coupling surface into the flow channel can be adjusted by choosing their geometric dimensions.
- the figure shows the sectional view of the planar construction of a complete MFD component containing the actual inventive micro fluid diode (hereinafter referred to as MFD).
- the MFD is a chip-shaped component 1 made entirely of ⁇ 100> or ⁇ 110> silicon. It is etched on one side as a lattice structure 6 and on the other side as a continuous flow channel 9.
- the MFD chip 1 is mounted with the spacer chip 2, which is also made of silicon, in the glass-silicon flow cell 3 in such a way that a target fluid 7 can move past the MFD unhindered, thereby forming 6 small micromenisci in the lattice structure.
- the lattice structure forms the coupling surface of the microfluidic diode in the direction of the spacer chip 2.
- the entire component of the MFD comprises the stack arrangement of fluidic flow cell 3, 4 with flow channel 7, 9 and channel stopper 8, the MFD chip 1 with its microcapillary array 6 and the spacer chip 2, which is connected to the adjacent gas or air cushion over the microcapillary array.
- the spacer chip 2, which forms the droplet chamber, is also produced by anisotropic etching in ⁇ 100> silicon. If the flow channel 7 is now flowed through by the target fluid, it wets the microcapillaries and spreads up to their opposite opening, where it forms a target fluid meniscus 6 independently of the flow speed depending on its surface tension and the system-internal gravity pressures, the total field of the capillary openings providing a coupling area for one Dosing fluid forms. If the metering fluid 5 is now sprayed onto this coupling surface 6 by means of a microtechnical pump, it can pass through the MFD arrangement 1 and directly reach the flow channel of the target fluid.
- the micro fluid diode according to the invention provides a new element for microfluid handling without mechanical valves.
- the construction of the micro fluid diode according to the invention is much simpler than that of the micromechanical valves, so that in addition to the smaller space requirement, the production is more cost-effective.
- they can be used to implement a new concept for coupling unsupported fluid jets into a flowing target fluid located in a closed system.
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Engineering & Computer Science (AREA)
- Fluid Mechanics (AREA)
- Physics & Mathematics (AREA)
- Theoretical Computer Science (AREA)
- Mechanical Engineering (AREA)
- Micromachines (AREA)
- Reciprocating Pumps (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
- Bipolar Transistors (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Thermistors And Varistors (AREA)
Claims (3)
- Micro-diode fluide (1) permettant l'introduction orientée d'un fluide doseur (5) dans un autre fluide récepteur (7) (lequel est en circulation ou au repos et se trouve dans un système fermé, spécialement dans le domaine des submicrolitres), caractérisée par la disposition planaire d'un microcapillaire ouvert des deux côtés ou d'un système de microcapillaires (6) ouverts des deux côtés, étroitement serrés l'un à côté de l'autre, se trouvant au contact direct du fluide récepteur du côté de la sortie et séparés du fluide de dosage du côté de l'entrée, le fluide de dosage devant être introduit de façon discontinue par un coussin d'air ou de gaz formant un ménisque courbé suivant la tension de surface.
- Micro-diodes fluides (1) selon la spécification 1, dont les composants sont formés de silicium, verre, céramique, métal ou d'une combinaison de ces matériaux, fabriquées selon un procédé microtechnique et les techniques de montage et de connexion de la technique des microsystèmes.
- Micro-diode fluide (1) selon la spécification 1, caractérisée par une fabrication à base de silicium orienté à <100> -ou- <110>.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE4405005A DE4405005A1 (de) | 1994-02-17 | 1994-02-17 | Mikro-Fluiddiode |
DE4405005 | 1994-02-17 |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0672835A1 EP0672835A1 (fr) | 1995-09-20 |
EP0672835B1 true EP0672835B1 (fr) | 1999-05-12 |
Family
ID=6510442
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP95101737A Expired - Lifetime EP0672835B1 (fr) | 1994-02-17 | 1995-02-09 | Micro diode fluidique |
Country Status (7)
Country | Link |
---|---|
US (1) | US5730187A (fr) |
EP (1) | EP0672835B1 (fr) |
JP (1) | JP3786421B2 (fr) |
AT (1) | ATE180044T1 (fr) |
DE (2) | DE4405005A1 (fr) |
DK (1) | DK0672835T3 (fr) |
WO (1) | WO1995022696A1 (fr) |
Families Citing this family (54)
Publication number | Priority date | Publication date | Assignee | Title |
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DE19530886C1 (de) * | 1995-08-11 | 1996-10-02 | Inst Bioprozess Analysenmesst | Vorrichtung zur sterilen Entnahme von Proben über eine Filtermembran |
DE19611270A1 (de) * | 1996-03-22 | 1997-09-25 | Gesim Ges Fuer Silizium Mikros | Mikromischer zur Handhabung kleinster Flüssigkeitsmengen |
US6033544A (en) * | 1996-10-11 | 2000-03-07 | Sarnoff Corporation | Liquid distribution system |
US5964997A (en) * | 1997-03-21 | 1999-10-12 | Sarnoff Corporation | Balanced asymmetric electronic pulse patterns for operating electrode-based pumps |
US6117396A (en) * | 1998-02-18 | 2000-09-12 | Orchid Biocomputer, Inc. | Device for delivering defined volumes |
JP2981547B1 (ja) * | 1998-07-02 | 1999-11-22 | 農林水産省食品総合研究所長 | クロスフロー型マイクロチャネル装置及び同装置を用いたエマルションの生成または分離方法 |
JP3012608B1 (ja) * | 1998-09-17 | 2000-02-28 | 農林水産省食品総合研究所長 | マイクロチャネル装置及び同装置を用いたエマルションの製造方法 |
US6591852B1 (en) | 1998-10-13 | 2003-07-15 | Biomicro Systems, Inc. | Fluid circuit components based upon passive fluid dynamics |
EP1125129A1 (fr) * | 1998-10-13 | 2001-08-22 | Biomicro Systems, Inc. | Composants de circuit fluidique bases sur la dynamique passive des fluides |
US6637463B1 (en) | 1998-10-13 | 2003-10-28 | Biomicro Systems, Inc. | Multi-channel microfluidic system design with balanced fluid flow distribution |
US6601613B2 (en) | 1998-10-13 | 2003-08-05 | Biomicro Systems, Inc. | Fluid circuit components based upon passive fluid dynamics |
US6360775B1 (en) | 1998-12-23 | 2002-03-26 | Agilent Technologies, Inc. | Capillary fluid switch with asymmetric bubble chamber |
US6481453B1 (en) * | 2000-04-14 | 2002-11-19 | Nanostream, Inc. | Microfluidic branch metering systems and methods |
US6561208B1 (en) * | 2000-04-14 | 2003-05-13 | Nanostream, Inc. | Fluidic impedances in microfluidic system |
US6296452B1 (en) | 2000-04-28 | 2001-10-02 | Agilent Technologies, Inc. | Microfluidic pumping |
US6615856B2 (en) * | 2000-08-04 | 2003-09-09 | Biomicro Systems, Inc. | Remote valving for microfluidic flow control |
JP3511238B2 (ja) | 2000-10-13 | 2004-03-29 | 独立行政法人食品総合研究所 | マイクロスフィアの製造方法および製造装置 |
US6644944B2 (en) | 2000-11-06 | 2003-11-11 | Nanostream, Inc. | Uni-directional flow microfluidic components |
US6649078B2 (en) | 2000-12-06 | 2003-11-18 | The Regents Of The University Of California | Thin film capillary process and apparatus |
US20020186263A1 (en) * | 2001-06-07 | 2002-12-12 | Nanostream, Inc. | Microfluidic fraction collectors |
US20020195343A1 (en) * | 2001-06-20 | 2002-12-26 | Coventor, Inc. | Microfabricated separation device employing a virtual wall for interfacing fluids |
US20030015425A1 (en) * | 2001-06-20 | 2003-01-23 | Coventor Inc. | Microfluidic system including a virtual wall fluid interface port for interfacing fluids with the microfluidic system |
US20020197733A1 (en) * | 2001-06-20 | 2002-12-26 | Coventor, Inc. | Microfluidic system including a virtual wall fluid interface port for interfacing fluids with the microfluidic system |
US7179423B2 (en) * | 2001-06-20 | 2007-02-20 | Cytonome, Inc. | Microfluidic system including a virtual wall fluid interface port for interfacing fluids with the microfluidic system |
US7211442B2 (en) * | 2001-06-20 | 2007-05-01 | Cytonome, Inc. | Microfluidic system including a virtual wall fluid interface port for interfacing fluids with the microfluidic system |
EP1314479A3 (fr) * | 2001-11-24 | 2004-03-24 | GeSIM Gesellschaft für Silizium-Mikrosysteme mbH | Dispositif pour le transfert d' échantillons liquides |
US6932502B2 (en) * | 2002-05-01 | 2005-08-23 | Hewlett-Packard Development Company, L.P. | Mixing apparatus |
US20050032238A1 (en) * | 2003-08-07 | 2005-02-10 | Nanostream, Inc. | Vented microfluidic separation devices and methods |
KR100540143B1 (ko) * | 2003-12-22 | 2006-01-10 | 한국전자통신연구원 | 미소 유체 제어소자 및 미소 유체의 제어 방법 |
JP4520166B2 (ja) * | 2004-02-02 | 2010-08-04 | 独立行政法人農業・食品産業技術総合研究機構 | 樹脂製マイクロチャネル基板及びその製造方法 |
WO2006016519A1 (fr) * | 2004-08-12 | 2006-02-16 | National Agriculture And Food Research Organization | Ensemble de microcanaux |
US8685711B2 (en) * | 2004-09-28 | 2014-04-01 | Singulex, Inc. | Methods and compositions for highly sensitive detection of molecules |
US7572640B2 (en) * | 2004-09-28 | 2009-08-11 | Singulex, Inc. | Method for highly sensitive detection of single protein molecules labeled with fluorescent moieties |
US9040305B2 (en) * | 2004-09-28 | 2015-05-26 | Singulex, Inc. | Method of analysis for determining a specific protein in blood samples using fluorescence spectrometry |
US20060088449A1 (en) * | 2004-10-26 | 2006-04-27 | Massachusetts Institute Of Technology | Systems and methods for transferring a fluid sample |
EP3156799B1 (fr) | 2006-04-04 | 2024-01-24 | Novilux, LLC | Analyseur et procédé hautement sensible de détection d'analytes |
JP5308328B2 (ja) | 2006-04-04 | 2013-10-09 | シングレックス,インコーポレイテッド | トロポニンの分析のための高感度のシステムおよび方法 |
US7838250B1 (en) | 2006-04-04 | 2010-11-23 | Singulex, Inc. | Highly sensitive system and methods for analysis of troponin |
US8524173B2 (en) * | 2006-09-01 | 2013-09-03 | Tosoh Corporation | Microchannel structure and fine-particle production method using the same |
EP2111551A1 (fr) * | 2006-12-20 | 2009-10-28 | Applied Biosystems, LLC | Dispositifs et procédés de gestion de l'écoulement dans des structures microfluidiques |
US20090087860A1 (en) * | 2007-08-24 | 2009-04-02 | Todd John A | Highly sensitive system and methods for analysis of prostate specific antigen (psa) |
US7914734B2 (en) | 2007-12-19 | 2011-03-29 | Singulex, Inc. | Scanning analyzer for single molecule detection and methods of use |
CN102016552A (zh) * | 2008-03-05 | 2011-04-13 | 神谷来克斯公司 | 用于分子的高灵敏性检测的方法和组合物 |
GB2464183A (en) * | 2008-09-19 | 2010-04-14 | Singulex Inc | Sandwich assay |
JP5678045B2 (ja) | 2009-06-08 | 2015-02-25 | シンギュレックス・インコーポレイテッド | 高感度バイオマーカーパネル |
JP2013525820A (ja) | 2010-05-06 | 2013-06-20 | シングレクス、インコーポレイテッド | 関節リウマチの発症に関するリスクを診断し、病期分類し、予測し、治療レスポンダーを同定するための方法 |
CN103240023B (zh) * | 2013-05-09 | 2015-01-07 | 四川大学 | 一种微手术刀触发液滴融合的方法 |
JP7356351B2 (ja) | 2016-12-12 | 2023-10-04 | エクセラ・バイオサイエンシーズ・インコーポレイテッド | マイクロキャピラリーアレイを使用したスクリーニングのための方法およびシステム |
US11085039B2 (en) | 2016-12-12 | 2021-08-10 | xCella Biosciences, Inc. | Methods and systems for screening using microcapillary arrays |
JP7208902B2 (ja) | 2016-12-30 | 2023-01-19 | エクセラ・バイオサイエンシーズ・インコーポレイテッド | マルチステージサンプル回収システム |
US20180304266A1 (en) * | 2017-04-24 | 2018-10-25 | miDiagnostics NV | Channel and a capillary trigger valve comprising the same |
WO2021144396A1 (fr) | 2020-01-17 | 2021-07-22 | F. Hoffmann-La Roche Ag | Dispositif microfluidique et procédé de synthèse automatisée par division de groupe |
EP4093543A2 (fr) | 2020-01-22 | 2022-11-30 | F. Hoffmann-La Roche AG | Dispositifs microfluidiques de piégeage de billes et procédés de préparation de banque de séquences de nouvelle génération |
JP2023545478A (ja) | 2020-10-15 | 2023-10-30 | カパ バイオシステムズ,インコーポレイティド | 次世代配列決定ライブラリ調製のための電気泳動デバイスおよび方法 |
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US3777344A (en) * | 1969-05-28 | 1973-12-11 | Cava Ind | Method of fabricating fluidic elements by assembling together a plurality of plastic strips |
US3865136A (en) * | 1971-04-29 | 1975-02-11 | Eke Verschuur | Oil/water pipeline inlet with oil supply via a large chamber |
US4027407A (en) * | 1975-11-24 | 1977-06-07 | Kiss Sandor G | Jet flow alternator |
US4761077A (en) * | 1987-09-28 | 1988-08-02 | Barrett, Haentjens & Co. | Mixing apparatus |
DE4003063A1 (de) * | 1990-01-24 | 1991-07-25 | Hopf Rolf | Ventilartige vorrichtungen |
US5094594A (en) * | 1990-04-23 | 1992-03-10 | Genomyx, Incorporated | Piezoelectric pumping device |
US5165440A (en) * | 1991-12-30 | 1992-11-24 | Conoco Inc. | Process and apparatus for blending viscous polymers in solvent |
-
1994
- 1994-02-17 DE DE4405005A patent/DE4405005A1/de not_active Withdrawn
-
1995
- 1995-02-09 EP EP95101737A patent/EP0672835B1/fr not_active Expired - Lifetime
- 1995-02-09 DK DK95101737T patent/DK0672835T3/da active
- 1995-02-09 DE DE59505877T patent/DE59505877D1/de not_active Expired - Fee Related
- 1995-02-09 AT AT95101737T patent/ATE180044T1/de not_active IP Right Cessation
- 1995-02-17 WO PCT/DE1995/000200 patent/WO1995022696A1/fr active Application Filing
- 1995-02-17 US US08/696,990 patent/US5730187A/en not_active Expired - Lifetime
- 1995-02-17 JP JP52150895A patent/JP3786421B2/ja not_active Expired - Lifetime
Also Published As
Publication number | Publication date |
---|---|
WO1995022696A1 (fr) | 1995-08-24 |
JPH09509466A (ja) | 1997-09-22 |
DK0672835T3 (da) | 1999-11-29 |
ATE180044T1 (de) | 1999-05-15 |
DE4405005A1 (de) | 1995-08-24 |
DE59505877D1 (de) | 1999-06-17 |
EP0672835A1 (fr) | 1995-09-20 |
US5730187A (en) | 1998-03-24 |
JP3786421B2 (ja) | 2006-06-14 |
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