WO2001051208A1 - Systeme de microbuses - Google Patents

Systeme de microbuses Download PDF

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Publication number
WO2001051208A1
WO2001051208A1 PCT/EP2000/011689 EP0011689W WO0151208A1 WO 2001051208 A1 WO2001051208 A1 WO 2001051208A1 EP 0011689 W EP0011689 W EP 0011689W WO 0151208 A1 WO0151208 A1 WO 0151208A1
Authority
WO
WIPO (PCT)
Prior art keywords
nozzle
micro
hollow channel
opening
nozzle body
Prior art date
Application number
PCT/EP2000/011689
Other languages
German (de)
English (en)
Inventor
Thomas Kinkopf
Hansjörg BEUTEL
Original Assignee
Fraunhofer Gesellschaft zur Förderung der angewandten Forschung e.V.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fraunhofer Gesellschaft zur Förderung der angewandten Forschung e.V. filed Critical Fraunhofer Gesellschaft zur Förderung der angewandten Forschung e.V.
Publication of WO2001051208A1 publication Critical patent/WO2001051208A1/fr

Links

Classifications

    • 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
    • B01L3/02—Burettes; Pipettes
    • B01L3/0241—Drop counters; Drop formers
    • B01L3/0268—Drop counters; Drop formers using pulse dispensing or spraying, eg. inkjet type, piezo actuated ejection of droplets from capillaries
    • 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
    • B01L3/02—Burettes; Pipettes
    • B01L3/021—Pipettes, i.e. with only one conduit for withdrawing and redistributing liquids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0861—Configuration of multiple channels and/or chambers in a single devices
    • B01L2300/0867—Multiple inlets and one sample wells, e.g. mixing, dilution
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/08—Geometry, shape and general structure
    • B01L2300/0861—Configuration of multiple channels and/or chambers in a single devices
    • B01L2300/0874—Three dimensional network
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N2035/1027—General features of the devices
    • G01N2035/1034—Transferring microquantities of liquid
    • G01N2035/1039—Micropipettes, e.g. microcapillary tubes

Definitions

  • the invention relates to a micro-nozzle system with at least one nozzle body that encloses a nozzle opening that has a nozzle opening cross section in the micrometer range and through which a gaseous or liquid material flow can be introduced or removed.
  • a method for producing such a micro-nozzle system is also described.
  • Micro-nozzle systems of the type mentioned above are preferably suitable for handling and manipulating small objects, such as biological cells.
  • small objects such as biological cells.
  • optical sighting with the aid of a microscope focused on the plane of the nozzle opening, it is also possible to observe or manipulate the spatially fixed biological cell in the desired manner.
  • micro-nozzle systems In addition to the examination and handling of the smallest objects, micro-nozzle systems also allow a specific substance deposition into the smallest space areas by discharging a certain material flow through the nozzle opening.
  • a field-like or array-like arrangement of a large number of individual nozzles also makes it possible to inject a wide variety of material flows into one another Bring mixture to generate material mixtures in even the smallest of spaces.
  • micro-nozzle systems do not allow different material flows to be discharged separately from one another through adjacent nozzle openings, especially since known micro-nozzle systems are limited only to membranes perforated with the smallest holes, through which either a uniform material flow can be discharged or on which a uniform vacuum can be created. In this case, only the perforated membrane spans a closed volume, which in turn is connected to a corresponding pressure source, by means of which either a material flow can be introduced into the volume or a negative pressure can be created in the volume.
  • the invention is based on the object of designing a micro-nozzle system with at least one, a nozzle opening, which has a nozzle opening cross section in the micrometer range and through which a gaseous or liquid material flow can be introduced or removed, in such a way that a finely metered It is possible to discharge different material flows through a large number of micro-nozzles arranged next to one another. Through each individual nozzle opening, it should be possible to locally discharge a stream of material from the nozzle arrangement or to introduce it into the nozzle opening by means of negative pressure.
  • the construction of each individual nozzle arrangement should be as simple as possible and with the cheapest possible means that also meet the requirements of mass production.
  • a micro-nozzle system with at least one nozzle body which has a nozzle opening cross-section in the micrometer range and through which a gaseous or liquid material flow can be introduced or removed, is designed in such a way that the nozzle body encloses a volume into which at least one one end of a hollow channel opens, and that another end of the hollow channel is connected to a connection area to which a pressure source for transporting the material flow through the hollow channel can be connected.
  • each individual nozzle opening is surrounded by a nozzle body, which encloses a volume into which at least one hollow channel opens.
  • a nozzle body is designed in the manner of a chamber, which is surrounded by chamber walls and into which one or more hollow channels open.
  • the connection of the hollow duct to a pressure source by means of which either a controlled one, is required Negative pressure is generated within the hollow channel or a certain material flow is specifically fed into the hollow channel, special attention.
  • the end of the hollow channel facing away from the nozzle body opens into a connection area which, as will be shown in more detail below, is designed as a flat section, on the surface of which holes are drilled, which act as connecting openings to each serve single hollow channel.
  • An adapter unit is releasably fixed in a fluid-tight manner to the flat connection area, which in turn is penetrated with openings whose opening diameters increase from the size of the connection openings to macroscopically large opening widths, which allow a connection that is easy to handle mechanically and to which a corresponding pressure source can be connected ,
  • each individual hollow channel to an individual pressure source or to supply all the hollow channels opening into the connection area with a single pressure source.
  • the nozzle body itself preferably has a pyramidal shape, which preferably has a three-sided or four-sided plan. In principle, however, any other spatial shape of the nozzle body is conceivable, such as, for example, cylindrical, in the form of a tube, cubic, etc. Opposite the floor plan, the nozzle body has a nozzle opening which is arranged at the pyramid tip. For the purpose of a stream of material oriented centrally to the nozzle opening through the nozzle body, regardless of whether the stream of material is directed out of the volume of the nozzle body through the nozzle opening or into the volume, the hollow channel connected to the volume of the nozzle body opens out centrally the footprint in the volume of the nozzle body.
  • micro-mixer units are suitable which are arranged in the flow before the volume enters the nozzle body and which ensures an improved mixing of the material flows flowing into the volume of the nozzle body.
  • the micro mixer unit preferably consists of a conically tapering micro column, on the contour of which vortices are arranged. The tapered end of the micro-mixer unit is directed in the direction of the volume of the nozzle body.
  • the nozzle body itself and the material surrounding the hollow channel are preferably made of light-transparent material, so that an examination of biological cells in the manner described at the beginning is possible with the aid of conventional light microscopes.
  • the term light-transparent is to be understood in such a way that the structure of the nozzle arrangement should not have a lasting effect on an optical analysis.
  • Suitable materials for the nozzle body are, for example, silicon nitride, which is applied to a glass substrate into which a recess is formed which is open on one side and which is also covered by the silicon nitride layer and in this way delimits the hollow channel.
  • micro-nozzle system is produced using microsystem technology processes, such as, for example, deposition processes from the plasma phase, reactive ion etching (RIE), metal etching, lithographic processes, sputtering or anisotropic silicon etching.
  • RIE reactive ion etching
  • metal etching metal etching
  • lithographic processes lithographic processes
  • sputtering anisotropic silicon etching.
  • a glass substrate which serves both as a carrier medium for the pyramid-shaped nozzle bodies and as a channel-forming material for the hollow channels.
  • the nozzle body and the layer covering the hollow channels are preferably made of silicon nitrite.
  • these can also be produced using technically fully controllable machining processes in a cost-effective framework and on a large industrial scale. It is also possible, in addition to the individual production of the nozzle bodies according to the invention, to arrange them in a plurality in an array, next to one another, on large-area substrates. In particular, this makes it possible to produce micro-nozzle systems with a large number of individual nozzle bodies, which are used, for example, to examine biological cells in large-scale laboratories.
  • 1 is a perspective view of two nozzle bodies
  • FIG. 1 shows the schematic perspective illustration of two nozzle bodies 3, of which the nozzle body upstream in FIG. 1 is shown in a cut-away manner for better clarification of shape and geometry.
  • the pyramid-shaped pyramid body 3 has a square base.
  • the nozzle body 3, like the layer 6, is made of silicon nitrite and is integrally connected to it.
  • the so-called nozzle opening At the tip of each individual nozzle body 3 there is an opening 4, the so-called nozzle opening, which typically has an opening diameter of a few ⁇ m to approximately 50 ⁇ m.
  • micromechanical techniques which will be discussed in more detail in particular with reference to FIG. 8, it is also possible to round the sharp edges of the four-sided pyramid, so that the nozzle opening 4 also has the square outline shape shown in FIG. 1 a round nozzle opening shape can be converted.
  • Each individual nozzle body 3, which encloses a volume inside, is connected to a hollow channel 1, which runs orthogonally to the exit direction of the nozzle opening 4.
  • the connection between the hollow channel 1 and the volume of the nozzle body 3 is typically made centrally through the base from below.
  • Each individual hollow channel is preferably located in a glass substrate 5, on the surface of which the aforementioned silicon nitride layer 6, from which the walls of each individual nozzle body 3 are made, is deposited.
  • the silicon nitride layer 6 also closes the hollow channel 1 at the top.
  • FIG. 2 shows an array-like arrangement of four nozzle bodies 3, all of which are arranged on one and the same glass substrate with a uniform silicon nitride layer 6 covering the glass substrate.
  • nozzle bodies 3 all of which are arranged on one and the same glass substrate with a uniform silicon nitride layer 6 covering the glass substrate.
  • FIG. 3 shows a nozzle body 9 shown in perspective with a nozzle opening 10 which, in contrast to the embodiment according to FIG. 1, is fed by the merging of three partial hollow channels 11, 12.
  • the original hollow channel 1 branches off in a branching node into three partial hollow channels 11, 12 which collide in a star shape below the base area of the nozzle body 9.
  • the subchannels 12 are designed somewhat thinner in flow cross-section than the partial hollow channel 11.
  • the three subchannels open into the volume of the nozzle body 9, as a result of which they operate in a mode of operation of the nozzle arrangement in which a material flow through the hollow channel 1 via the partial channels 11, 12 get into the volume of the nozzle body 9, ensure an almost central exit of the material flow through the nozzle opening 10.
  • the volume of the nozzle body 9 also serves for better mixing of the material flow before it leaves the nozzle opening 10.
  • a suction flow is achieved through the nozzle opening 10 into the nozzle opening, which, with the aid of the arrangement of the three partial hollow channels shown in FIG. runs vertically from top to bottom through the nozzle opening 10, cells in front of the nozzle opening 10 being able to be drawn as centrally as possible to the nozzle opening 10.
  • the nozzle opening 10 and nozzle body 9 receives a kind of container effect.
  • the largely closed volume ensures that the cell remains spatially fixed, especially since the passage opening through which the hollow channels open is dimensioned such that biological cells cannot be transported through the hollow channels.
  • the dimensions of the micro nozzle system can, however, be individually designed depending on the application. So it is also possible to rinse or treat a volume inserted cell with a special material flow, so that the volume inside the nozzle body can also be viewed as a kind of mini laboratory unit.
  • FIG. 4 shows an array-like arrangement, consisting of a large number of individual nozzle bodies 9, according to the exemplary embodiment in FIG. 3.
  • All individual nozzle bodies 9, which have a nozzle opening 10, are each supplied and located by three partial hollow channels 11 and 12 all on a single carrier substrate 5, which is covered by the aforementioned layer 6, preferably a silicon nitride layer.
  • the hollow channel 1 can be split into partial or secondary channels as desired in diameter.
  • a single nozzle body 9 can also be connected to different hollow channels, so that different material flows can be mixed in the interior of the nozzle body 9. This requires a correspondingly different design of the hollow duct feed compared to the embodiment shown in FIG. 4.
  • FIG. 5 shows an overall view of the micro-nozzle system designed according to the invention, which is applied to a carrier substrate 5, preferably a glass substrate.
  • the hollow channels 1, which are connected to nozzle bodies 3, run inside the glass substrate 5.
  • 6 shows a detailed view from the embodiment shown in FIG. 5.
  • 6 shows a plurality of nozzle bodies 3 arranged in a field-like manner, each of which is connected to hollow channels 1.
  • the hollow channels 1 branch into three partial hollow channels and open into the volume of each individual nozzle body 3 via a common opening.
  • each individual nozzle body 3 shows a layer 6, preferably consisting of silicon nitrite, covering the glass substrate 5, from which on the one hand each individual nozzle body 3 is made and on the other hand closes off the hollow channels 1 incorporated in the glass substrate 5 at the top.
  • the reference numeral 7 denotes a silicon layer in FIG. 5 and in FIG. 6, which can be broken off at the tapered end of the glass substrate 5 via a predetermined breaking line 8.
  • the individual hollow channels 1 open into a connection area in which each individual hollow channel has a connection opening 2 connected is.
  • Each individual connection opening 2 is to be connected in a fluid-tight manner to a suitable pressure source, so that a corresponding negative pressure can be applied via the connection opening 2 or corresponding material flows can be introduced in a targeted manner.
  • FIG. 7 shows how the micro-nozzle system 19 is connected for connection to a suitable pressure source.
  • a base body 13 is provided, as well as a counter plate 18, both of which are pressed against one another with a certain force by corresponding screws (not shown).
  • the base plate 13 has a recess 16 which is adapted to the contour of the micro-nozzle system and into which a silicone seal 17 and the micro-nozzle system 19 can be introduced for fluid-tight sealing.
  • the base plate 13 provides connection holes 15, which are precisely aligned with the connection openings 2 of the micro-nozzle system. The diameter of the connection holes 15 increases in the area of the connection points 14, which can each be connected to a pressure source.
  • FIG. 8 shows in sequence images a to d the production of a nozzle body, the side edges 20, 21 of which are successively rounded off. Suitable etching methods are suitable for this, which in particular result in the rounding of angular structures. With the edge rounding, it is also possible to round the nozzle opening 10. Depending on the design variation, round to square nozzle openings can be achieved.
  • a new manufacturing process makes it possible to build a three-dimensional micro-nozzle system that is optically transparent for conventional microscopes and adapts to a macro working pressure generator, inexpensively and in large numbers.
  • microsystem technology processes are Manufacturing and processing methods that are known from semiconductor manufacturing and that can be completely controlled and that allow cost-effective and large-scale production of the micro-nozzle systems of the highest quality.
  • a glass substrate 5 serves as a carrier medium for the pyramid-shaped nozzle bodies 3, 9 and as a channel-forming material.
  • the nozzles and the channel covers are preferably made of a silicon nitride. Glass or silicon oxide (SiÜ 2 ) can also be used, but a loss of mechanical stability has to be accepted.
  • the uniformity of the nozzle structures with one another can be considerably increased.
  • FIGS. 9 a) to k) show the process in which the novel micro-nozzle system can be produced.
  • a so-called SOI wafer serves as the starting material, which essentially consists of two Si substrates connected to one another by an SiO 2 layer.
  • the individual layers shown in FIG. 9a are briefly explained in detail: a) Si 3 N 4 layer, which serves as a protective layer for the etching steps that follow. b) Si0 2 layer, c) Si layer, which serves as a carrier layer, d) SiO 2 bond layer, serves as a connecting layer, e) Si layer, further serves as a sacrificial layer, f) Si0 2 layer, g) Si 3 N 4 layer, which serves as a mask for a subsequent KOH etching step, and h) positive resist layer, which represents a first mask.
  • the layer h) serves as a mask and defines the spatial positioning of the depressions to be introduced into the sacrificial layer e), into which the nozzle bodies are subsequently to be introduced.
  • RIE reactive ion etching
  • the layers g) and f) are deliberately removed (see FIG. 9b).
  • a glass substrate n) is coated with a chromium layer m), which is correspondingly structured by etching, and with a positive resist layer located above, which serves as mask 2.
  • a pyramid-shaped etching pit o) is introduced into the Si layer e) by means of KOH etching.
  • the glass substrate n) is processed with the help of Si0 2 -RIE, whereby a channel structure p) is created.
  • the edges of the pyramid-shaped etching pit are rounded using an isotropic Si-RIE process. In this way it is also possible to round the nozzle opening (see Fig. 8). This can be done optionally.
  • the glass substrate n) is then provided with holes r) by means of mechanical glass processing methods, such as drilling with diamond-tipped grinding pins or by means of an ultrasound drilling method.
  • the layer components are each cleaned from layers a), b), f), g) and m) using an AF-HF etching mixture.
  • the two layer components freed from layers a), b), f), g) and m) are subjected to appropriate oxidation by means of an oxide layer u) and using an Si 3 N 4 layer v) linked together.
  • the connection takes place by means of anodic bonding, so that the glass substrate n) is firmly and intimately connected to the structured SOI wafer.
  • the layers v) and u) are selectively opened using a positive resist mask x) (see FIG. 9g).
  • a deep etching process is then carried out using a KOH etching mixture and a subsequent ion etching, with which the SI0 2 layer d) is opened in a targeted manner.
  • the pyramid tip is deliberately exposed by deep etching using isotropic Sj ion etching.
  • the nozzle structure is opened by means of targeted Si 3 N 4 ion etching and subsequently, according to FIG. 9k, layer e) is removed by means of a KOH etching mixture, down to the oxide layer u).
  • the oxide layer u) can also be removed accordingly and replaced by a corresponding coating material which has certain hydrophilic or hydrophobic properties.

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  • Health & Medical Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Micromachines (AREA)

Abstract

Système de microbuses comportant au moins un corps (3) de buse entourant une ouverture (4) de buse qui possède une section transversale de l"ordre du micromètre et par laquelle peut être évacué ou introduit un flux de substance gazeuse ou liquide. La présente invention est caractérisée en ce que le corps (3) de buse définit un volume dans lequel débouche au moins une extrémité d"un canal creux (1) et en ce qu"une autre extrémité dudit canal est reliée à une zone de connexion à laquelle peut être raccordée une source de pression en vue du transport du flux de substance dans le canal creux (1).
PCT/EP2000/011689 2000-01-10 2000-11-23 Systeme de microbuses WO2001051208A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2000100691 DE10000691A1 (de) 2000-01-10 2000-01-10 Mikro-Düsen-System
DE10000691.4 2000-01-10

Publications (1)

Publication Number Publication Date
WO2001051208A1 true WO2001051208A1 (fr) 2001-07-19

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PCT/EP2000/011689 WO2001051208A1 (fr) 2000-01-10 2000-11-23 Systeme de microbuses

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DE (1) DE10000691A1 (fr)
WO (1) WO2001051208A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8845307B2 (en) 2010-05-25 2014-09-30 Samsung Electro-Mechanics Co., Ltd. Micro-ejector and method for manufacturing the same
EP3956672A4 (fr) * 2019-04-18 2022-06-08 Siemens Healthcare Diagnostics, Inc. Dispositif microfluidique intégré avec adaptation de pipette

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3877572B2 (ja) * 2001-08-09 2007-02-07 オリンパス株式会社 微細流路装置およびその使用方法
FR2862007B1 (fr) 2003-11-12 2005-12-23 Commissariat Energie Atomique Dispositif microfluidique muni d'un nez d'electronebulisation.

Citations (6)

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Publication number Priority date Publication date Assignee Title
EP0434149A2 (fr) * 1989-12-22 1991-06-26 Eastman Kodak Company Dispositif pour le transfert de liquides
EP0725267A2 (fr) * 1995-02-01 1996-08-07 Forschungszentrum Rossendorf e.V. Micro-pipette actionnée électriquement
JPH08219956A (ja) * 1995-02-17 1996-08-30 Hitachi Koki Co Ltd ピペット及びその使用方法
US5877580A (en) * 1996-12-23 1999-03-02 Regents Of The University Of California Micromachined chemical jet dispenser
US5904424A (en) * 1995-03-30 1999-05-18 Merck Patent Gesellschaft Mit Beschrankter Haftung Device for mixing small quantities of liquids
DE19911456A1 (de) * 1999-03-08 2000-09-14 Jenoptik Jena Gmbh Mehrkanal-Tropfengenerator

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US5992769A (en) * 1995-06-09 1999-11-30 The Regents Of The University Of Michigan Microchannel system for fluid delivery
US6154234A (en) * 1998-01-09 2000-11-28 Hewlett-Packard Company Monolithic ink jet nozzle formed from an oxide and nitride composition

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Publication number Priority date Publication date Assignee Title
EP0434149A2 (fr) * 1989-12-22 1991-06-26 Eastman Kodak Company Dispositif pour le transfert de liquides
EP0725267A2 (fr) * 1995-02-01 1996-08-07 Forschungszentrum Rossendorf e.V. Micro-pipette actionnée électriquement
JPH08219956A (ja) * 1995-02-17 1996-08-30 Hitachi Koki Co Ltd ピペット及びその使用方法
US5904424A (en) * 1995-03-30 1999-05-18 Merck Patent Gesellschaft Mit Beschrankter Haftung Device for mixing small quantities of liquids
US5877580A (en) * 1996-12-23 1999-03-02 Regents Of The University Of California Micromachined chemical jet dispenser
DE19911456A1 (de) * 1999-03-08 2000-09-14 Jenoptik Jena Gmbh Mehrkanal-Tropfengenerator

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Title
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PATENT ABSTRACTS OF JAPAN vol. 1996, no. 12 26 December 1996 (1996-12-26) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8845307B2 (en) 2010-05-25 2014-09-30 Samsung Electro-Mechanics Co., Ltd. Micro-ejector and method for manufacturing the same
EP3956672A4 (fr) * 2019-04-18 2022-06-08 Siemens Healthcare Diagnostics, Inc. Dispositif microfluidique intégré avec adaptation de pipette

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