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WO2001057119A1 - Method for durable joining of polymer components - Google Patents

Method for durable joining of polymer components Download PDF

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Publication number
WO2001057119A1
WO2001057119A1 PCT/EP2001/000890 EP0100890W WO0157119A1 WO 2001057119 A1 WO2001057119 A1 WO 2001057119A1 EP 0100890 W EP0100890 W EP 0100890W WO 0157119 A1 WO0157119 A1 WO 0157119A1
Authority
WO
WIPO (PCT)
Prior art keywords
pressing
components
bar
functional groups
plates
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.)
Ceased
Application number
PCT/EP2001/000890
Other languages
German (de)
French (fr)
Inventor
Jürgen Behnisch
Andreas Holländer
Hartmut Blum
Ulf Heim
Lutz MÜLLER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jenoptik AG
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
Original Assignee
Jenoptik Jena GmbH
Jenoptik AG
Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV
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 Jenoptik Jena GmbH, Jenoptik AG, Fraunhofer Gesellschaft zur Foerderung der Angewandten Forschung eV filed Critical Jenoptik Jena GmbH
Publication of WO2001057119A1 publication Critical patent/WO2001057119A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/02—Preparation of the material, in the area to be joined, prior to joining or welding
    • B29C66/022—Mechanical pre-treatments, e.g. reshaping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
    • B29C66/71—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the composition of the plastics material of the parts to be joined
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/914—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux
    • B29C66/9141—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature
    • B29C66/91411—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature of the parts to be joined, e.g. the joining process taking the temperature of the parts to be joined into account
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/914—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux
    • B29C66/9141—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature
    • B29C66/91441—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature the temperature being non-constant over time
    • B29C66/91443—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature the temperature being non-constant over time following a temperature-time profile
    • B29C66/91445—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux by controlling or regulating the temperature, the heat or the thermal flux by controlling or regulating the temperature the temperature being non-constant over time following a temperature-time profile by steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/919—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges
    • B29C66/9192—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams
    • B29C66/91921—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature
    • B29C66/91931—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature in explicit relation to the fusion temperature or melting point of the material of one of the parts to be joined
    • B29C66/91935—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature in explicit relation to the fusion temperature or melting point of the material of one of the parts to be joined lower than said fusion temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/919—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges
    • B29C66/9192—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams
    • B29C66/91921—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature
    • B29C66/91941—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature in explicit relation to Tg, i.e. the glass transition temperature, of the material of one of the parts to be joined
    • B29C66/91945—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature in explicit relation to Tg, i.e. the glass transition temperature, of the material of one of the parts to be joined lower than said glass transition temperature
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/12—Bonding of a preformed macromolecular material to the same or other solid material such as metal, glass, leather, e.g. using adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/02—Preparation of the material, in the area to be joined, prior to joining or welding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/919—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/90—Measuring or controlling the joining process
    • B29C66/91—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux
    • B29C66/919—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges
    • B29C66/9192—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams
    • B29C66/91921—Measuring or controlling the joining process by measuring or controlling the temperature, the heat or the thermal flux characterised by specific temperature, heat or thermal flux values or ranges in explicit relation to another variable, e.g. temperature diagrams in explicit relation to another temperature, e.g. to the softening temperature or softening point, to the thermal degradation temperature or to the ambient temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
    • B29K2033/04—Polymers of esters
    • B29K2033/12—Polymers of methacrylic acid esters, e.g. PMMA, i.e. polymethylmethacrylate

Definitions

  • the invention relates to a method for permanently connecting polymer components to other components, which can consist of polymers, glasses, metals or semiconductors.
  • Such methods can be used, for example, to provide a lid on the surface of microstructured polymer components so that the resulting microstructured, typically microfluidic cavities are hermetically sealed.
  • microchannels are designed as cavities, liquids can be transported continuously electrokinetically or by pressure. Closed cavities are used to enclose precisely defined sample volumes and prevent the very small sample quantities from evaporating.
  • plate-shaped microfluidic components with branching channel structures have become increasingly common. The channel structures were first introduced into the silicon wafer by etching, as is the case with the Semiconductor technology for the production of integrated circuits is known, one now wants to switch to using plastics. The motivation for their use is determined not only by the inexpensive fabrication, but also by the advantageous material properties such as optical transparency, biocompatibility and low fluorescence in certain wavelength ranges.
  • the substances introduced into the channels as liquids and reacting with one another at channel branches are to be analyzed in a continuous channel area using optical means. Since defined cross-sectional dimensions for the channels in the range from previously 10 ⁇ m to 100 ⁇ m are required for this purpose, high demands are placed on the production of such products.
  • the device which is essentially composed of two parts, contains in a base plate
  • Microstructures in the form of microchannels are described.
  • an adhesive should be applied to one of the panels before joining.
  • the microstructured channels remain unchanged in their functional characteristics.
  • the auxiliary substances used could undesirably modify the existing microstructures on the surface or fill or otherwise influence the structure itself, a temperature increase above the glass transition temperature T G for amorphous polymers or the melting temperature T M for crystalline polymers can lead to material deformation.
  • the object of the invention is to rule out structural influences and undesirable modifications to the surfaces to be connected and thereby meet increased accuracy requirements even in the case of inexpensive production in large numbers.
  • the object is achieved by a method for permanently connecting polymer components to components made of the same or different type of material, the surfaces of which are to be connected first cleaned and then activated to generate reactive functional groups and in which the activated surfaces are brought into contact with one another to initiate bonds between the generated reactive functional groups under the action of pressure, exclusion of moisture and heating up to the glass transition or melting temperature of the polymer parts to reach these temperatures.
  • the use of this procedure results in a permanent connection of the parts below the glass transition or melting temperature, so that deformations due to thermal stress can be excluded.
  • the surface activation can e.g. B. by a plasma treatment or by photocnemics. After this treatment, the surfaces modified by the generation of functional groups have a high concentration of functional groups which are capable of a chemical interaction (bonds through acid-base interactions up to covalent bonds).
  • the interaction partners should be brought into atomic contact through the physical connection under pressure. To achieve this, in addition to the previous cleaning, it is also necessary to exclude new contaminations. In particular, an adsorbate layer that forms due to moisture must also be prevented.
  • connection mechanisms are used in the invention in which the formation of chemical compounds and intermolecular interactions serve as a functional principle , This also has the consequence that not only the same or similar but also very different materials can now be joined together. These no longer have to be adjusted in their melting point and also not be compatible.
  • An exemplary embodiment includes the connection of two planar plates, at least one of which can have a microstructured surface.
  • Both plates can be made of the same polymeric material, such as. B. polymethyl methacrylate (PMMA) or other materials, especially thermoplastics, such as. B. polycarbonate (PC) or polyethylene (PE) exist.
  • PMMA polymethyl methacrylate
  • PC polycarbonate
  • PE polyethylene
  • another polymer material or else glass, metal or a semiconductor material can also be used for one of the plates.
  • the two plates Before the two plates can be connected to each other, they are first cleaned in an ultrasonic bath filled with a cleaning liquid into which the plates are dipped.
  • the cleaning time is about 5 minutes at room temperature.
  • ethanol absolute
  • aqueous surfactant solutions which contain nonionic and / or ionic surfactants in concentrations between 0.01% and 5% are also suitable for this purpose, the cleaning process being carried out at a process temperature of 60.degree.
  • the two parts are then dried and subjected to a treatment in a low-pressure plasma with oxygen as the reaction gas, in which reactive functional groups are generated on the surfaces of the two plates to be joined or their concentration is increased on the surfaces.
  • the plasma treatment can be carried out in a plasma reactor with an inductively coupled high frequency of 13.56 MHz in a remote position, in which the surfaces to be activated are arranged some distance from the actual plasma zone.
  • the process time can range from 1 to 10 seconds, with two seconds being preferred.
  • the plasma treatment can also be carried out in a reactor which, for. B. works with a kHz or GHz excitation.
  • the times and the other reaction conditions can also vary within such a range sufficient surface functionalization takes place without degradation occurring.
  • the plasma effect must be dosed in a very defined manner.
  • other gases for example nitrogen, ammonia and also layer-forming gases such as methane or acetylene, can be used as process gases.
  • the treatment can also be carried out differently for each of the two parts to be connected, in particular with different process gases.
  • the activated plates which are absolutely dry after the plasma treatment, are then brought into contact with one another and pressed with an increase in temperature.
  • the temperature is increased in a range below the glass transition temperature T G or up to this temperature, but without reaching it. Since any access of moisture of any kind can be excluded in this process step, the connection and pressing should ideally take place in the plasma chamber (vacuum chamber), in which the activation step is also carried out.
  • the following process conditions are suitable for pressing PMMA sheets.
  • the temperature range of the holding elements for the PMMA plates used for pressing should be between room temperature and 80 ° C, the pressure between 80 bar and 500 bar and the pressing time between 0.5 min and 10 min. Optimal results can be achieved at 60 ° C, 200 bar and 1 min.
  • the two plates After cooling, the two plates are already permanently connected to each other. Nevertheless, annealing has had an advantageous effect on the strength of the connection produced, in which the two plates connected to one another at an elevated temperature be stored dry below the glass transition temperature T G. For example, a two-hour storage in a drying cabinet at a temperature of 60 ° C is suitable for this. Storage for a long time at room temperature also leads to a similar result.
  • the two plates can no longer be separated without being destroyed; there is a break in cohesion, which leads to a white coloring of both delaminated surfaces.
  • the two plates can only be separated with effort; the two delaminated surfaces show none visible changes / damage. Even extending the plasma treatment tent up to 60 s, for example, does not improve bond adhesion any further.
  • Two PMMA plates became 5 mm. m ethanol cleaned with ultrasound. The cleaned areas were placed on one another without further pretreatment and 1 mm. pressed at 60 ° C with 200 bar. The two plates can be easily separated; the two delaminated surfaces show no visible changes / damage.
  • Example 5 Two PMMA plates became 5 mm. ultrasonically cleaned in ethanol and then in an oxygen plasma for 2 s

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Plasma & Fusion (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Abstract

The aim of the invention is to preclude structural effects and undesired modifications of the joint surfaces in a method for durable joining of polymer components, with components made from homogeneous or heterogeneous materials and thus achieve increased precision requirements, even with cheap production in high quantities. Said aim is achieved, whereby the surfaces to be joined are first cleaned and then activated for the production of reactive functional groups. The activated surfaces are then brought into contact with each other, to initiate the bonding between the reactive functional groups, by means of pressure effects, exclusion of moisture and heating up towards the glass transition or meting point of the polymer components without achieving said temperature.

Description

VERFAHREN ZUM DAUERHAFTEN VERBINDEN VON POLYMERBAUTEILEN METHOD FOR PERMANENTLY CONNECTING POLYMER COMPONENTS

Die Erfindung betrifft ein Verfahren zum dauerhaften Verbinden von Polymerbauteilen mit anderen Bauteilen, die aus Polymeren, Gläsern, Metallen oder Halbleitern bestehen können .The invention relates to a method for permanently connecting polymer components to other components, which can consist of polymers, glasses, metals or semiconductors.

Derartige Verfahren sind beispielsweise einsetzbar, um oberflächlich mikrostrukturierte Polymerbauteile mit einem Deckel so zu versehen, dass ein hermetischer Abschluss der entstehenden mikrostrukturierten, typischerweise mikrofluidischen Kavitäten erfolgt.Such methods can be used, for example, to provide a lid on the surface of microstructured polymer components so that the resulting microstructured, typically microfluidic cavities are hermetically sealed.

Eine Vielzahl bekannt gewordener technischer Lösungen unterstreicht das bestehende große Interesse an mikrostrukturierten Disposables für mikrofluidische Anwendungen zum vorwiegenden Einsatz in der Biotechnologie, Medizin und Pharmakologie. Ein besonderes Augenmerk bei derartigen Anwendungen ist auf die genaue Kenntnis des umschlossenen Flüssigkeitsvolumens gerichtet, das hier im Mengenbereich von Pikolitern liegt. Sind die Mikrokanäle als Hohlräume ausgebildet, können Flüssigkeiten kontinuierlich elektrokinetisch oder durch Druck hindurch transportiert werden. Geschlossene Hohlräume werden zum Einschluss genau definierter Probenvolumina benutzt und verhindern das Verdunsten der sehr kleinen Probenmengen. Für die durchzuführenden Analysen haben sich in zunehmendem Maße plattenförmige mikrofluidische Bauelemente mit sich verzweigenden Kanalstrukturen durchgesetzt. Wurden die Kanalstrukturen zunächst durch Ätzen in Siliziumwafer eingebracht, wie es aus der Halbleitertechnik zur Herstellung integrierter Schaltkreise bekannt ist, will man nunmehr dazu übergehen, Kunststoffe einzusetzen. Die Motivation für deren Verwendung ist nicht nur durch die preiswerte Fabrikation bestimmt, sondern auch durch die vorteilhaften Materialeigenschaften wie optische Transparenz, Biokompatibilität und niedrige Fluoreszenz in bestimmten Wellenlängenbereichen .A variety of known technical solutions underlines the existing great interest in microstructured disposables for microfluidic applications for predominant use in biotechnology, medicine and pharmacology. In such applications, particular attention is paid to the precise knowledge of the enclosed liquid volume, which is in the range of picoliters here. If the microchannels are designed as cavities, liquids can be transported continuously electrokinetically or by pressure. Closed cavities are used to enclose precisely defined sample volumes and prevent the very small sample quantities from evaporating. For the analyzes to be carried out, plate-shaped microfluidic components with branching channel structures have become increasingly common. The channel structures were first introduced into the silicon wafer by etching, as is the case with the Semiconductor technology for the production of integrated circuits is known, one now wants to switch to using plastics. The motivation for their use is determined not only by the inexpensive fabrication, but also by the advantageous material properties such as optical transparency, biocompatibility and low fluorescence in certain wavelength ranges.

Die als Flüssigkeiten in die Kanäle eingebrachten und an Kanalverzweigungen miteinander reagierenden Substanzen sollen in einem fortlaufenden Kanalbereich mit optischen Mitteln analysiert werden. Da zu diesem Zweck definierte Querschnittsabmessungen für die Kanäle im Bereich von bisher 10 μm bis 100 μm erforderlich sind, werden hohe Anforderungen an die Herstellung derartiger Produkte gestellt .The substances introduced into the channels as liquids and reacting with one another at channel branches are to be analyzed in a continuous channel area using optical means. Since defined cross-sectional dimensions for the channels in the range from previously 10 μm to 100 μm are required for this purpose, high demands are placed on the production of such products.

Eine bekannte Lösung in Form einer integrierten Einrichtung zu elektrophoretischen Zwecken wird in der USA known solution in the form of an integrated device for electrophoretic purposes is described in the US

5 770 029 beschrieben. Die im wesentlichen aus zwei Teilen zusammengesetzte Einrichtung enthält in einer Grundplatte5 770 029. The device, which is essentially composed of two parts, contains in a base plate

MikroStrukturen in Form von Mikrokanälen, zu derenMicrostructures in the form of microchannels

Abdichtung eine Deckplatte verwendet wird. Als kostengünstige Variante für den einmaligen Gebrauch wird vorgeschlagen, alle Bestandteile aus Plastik zu fertigen.Sealing a cover plate is used. As a cost-effective variant for single use, it is proposed to manufacture all components from plastic.

Veränderungen der Form und des Querschnitts der Kanäle sind bei der dort beschriebenen Herstellungstechnik dann zu erwarten, wenn Breiten- und Tiefenabmessungen in einer Größe von 10 μm und kleiner gefordert sind und wenn insbesondere die Schwankungsbreite dieser Abmessungen weniger als 5 % betragen soll. Derartige Probleme treten auch auf, wenn von der Lehre nach der WO 98/45693 Gebrauch gemacht wird. Es wird ein Verfahren zur Herstellung polymerer MikroStrukturen auf der Basis plattenformiger Grundkorper beschrieben, von denen mindestens einer eine Mikrokanalstruktur enthalt, die durch Verbinden der beiden Platten geschlossen wird. Sind die beiden Platten aus Kunststoff hergestellt, wird vorgeschlagen, diese soweit zu erhitzen, dass durch Schmelzkleben oder einen dazu analogen Mechanismus eine direkte Verbindung infolge einer Interpenetπerung von Polymerketten hergestellt wird. Ansonsten soll auf eine der Platten vor dem Zusammenfugen ein Klebemittel aufgebracht werden. Bei beiden Verfahrensweisen st nicht gewährleistet, dass die mikrostrukturierten Kanäle m ihren Funktionsmerkmalen unverändert bleiben. Wahrend die eingesetzten Hilfssubstanzen die vorhandenen MikroStrukturen an der Oberflache unerwünscht modifizieren bzw. die Struktur selbst verfullen oder anderweitig beeinflussen konnten, kann eine Temperaturerhöhung über die Glasubergangstemperatur TG bei amorphen Polymeren oder der Schmelztemperatur TM bei kristallinen Polymeren zur Materialverformung fuhren.Changes in the shape and cross-section of the channels can be expected in the manufacturing technology described there if width and depth dimensions in a size of 10 μm and smaller are required and if in particular the fluctuation range of these dimensions should be less than 5%. Problems of this type also arise when use is made of the teaching according to WO 98/45693. A method for producing polymeric microstructures based on plate-shaped base bodies is described, at least one of which contains a microchannel structure which is closed by connecting the two plates. If the two plates are made of plastic, it is proposed to heat them to such an extent that a direct connection as a result of an interpenetration of polymer chains is produced by hot melt gluing or a mechanism analogous thereto. Otherwise, an adhesive should be applied to one of the panels before joining. In both procedures it is not guaranteed that the microstructured channels remain unchanged in their functional characteristics. While the auxiliary substances used could undesirably modify the existing microstructures on the surface or fill or otherwise influence the structure itself, a temperature increase above the glass transition temperature T G for amorphous polymers or the melting temperature T M for crystalline polymers can lead to material deformation.

Aufgabe der Erfindung ist es, Strukturbeeinflussungen sowie unerwünschte Modifizierungen der zu verbindenden Oberflachen auszuschließen und dadurch erhöhten Genauigkeitsanforderungen auch bei einer kostengünstigen Produktion in großen Stuckzahlen gerecht zu werden.The object of the invention is to rule out structural influences and undesirable modifications to the surfaces to be connected and thereby meet increased accuracy requirements even in the case of inexpensive production in large numbers.

Gemäß der Erfindung wird die Aufgabe durch ein Verfahren zum dauerhaften Verbinden von Polymerbauteilen mit Bauteilen aus gleichartigem oder andersartigem Material gelost, deren zu verbindende Oberflachen zunächst gereinigt und anschließend zur Erzeugung von reaktiven funktionellen Gruppen aktiviert werden und bei dem die aktivierten Oberflachen zur Initiierung von Bindungen zwischen den erzeugten reaktiven funktionellen Gruppen unter Druckeinwirkung, Ausschluss von Feuchtigkeit und Erwärmung bis zur Glasubergangs- oder Schmelztemperatur der Polymerteile in Kontakt miteinander gebracht werden, ohne dabei diese Temperaturen jedoch zu erreichen.According to the invention, the object is achieved by a method for permanently connecting polymer components to components made of the same or different type of material, the surfaces of which are to be connected first cleaned and then activated to generate reactive functional groups and in which the activated surfaces are brought into contact with one another to initiate bonds between the generated reactive functional groups under the action of pressure, exclusion of moisture and heating up to the glass transition or melting temperature of the polymer parts to reach these temperatures.

Im Gegensatz zum herkömmlichen Schmelzkleben wird mit der Anwendung dieser Verfahrensweise ein dauerhaftes Verbinden der Teile bereits unterhalb der Glasubergangs- oder Schmelztemperatur erreicht, so dass Verformungen infolge einer thermischen Belastung ausgeschlossen werden können. Die Oberflachenaktivierung kann z. B. durch eine Plasmabehandlung oder aber auch auf photocnemischem Wege erfolgen. Die durch die Erzeugung von Funktionalgruppen modifizierten Oberflachen weisen nach dieser Behandlung eine hohe Konzentration funktioneller Gruppen auf, die zu einer chemischen Wechselwirkung (Bindungen durch Saure- Base-Wechselwirkungen bis hin zu kovalenten Bindungen) fähig sind. Durch die körperliche Verbindung unter Druckeinwirkung sollen die Wechselwirkungspartner in atomaren Kontakt gebracht werden. Um das zu erreichen, ist neben der vorherigen Reinigung auch ein Ausschluss erneuter Kontaminationen erforderlich. Insbesondere ist auch eine sich durch Feuchtigkeit bildende Adsorbatschicht zu verhindern. Wahrend durch die für eine optimale dauerhafte Verbindung unbedingt erforderlichen Schritte der Reinigung, der Aktivierung und des Verpressens bereits eine erhebliche Festigkeit der Verbindung erreicht wird, kann ein Tempern bzw. eine Lagerung der verbundenen Teile die erreichte Festigkeit noch erstarken. Im Unterschied zu den direkten Verbindungsmethoden, bei denen eine gegenseitige Durchdringung der Polymerketten infolge einer Temperaturerhöhung über die Glasubergangstemperatur TG bzw. die Schmelztemperatur TM erfolgt, werden bei der Erfindung Verbindungsmechanismen ausgenutzt, bei denen die Bildung von chemischen Verbindungen und zwischenmolekularen Wechselwirkungen als Funktionsprinzip dienen. Das hat auch zur Folge, dass nunmehr nicht nur gleiche oder ähnliche sondern auch sehr unterschiedliche Materialien miteinander verbunden werden können. Diese müssen nicht mehr in ihrem Schmelzpunkt angepasst und auch nicht kompatibel sein.In contrast to conventional hotmelt gluing, the use of this procedure results in a permanent connection of the parts below the glass transition or melting temperature, so that deformations due to thermal stress can be excluded. The surface activation can e.g. B. by a plasma treatment or by photocnemics. After this treatment, the surfaces modified by the generation of functional groups have a high concentration of functional groups which are capable of a chemical interaction (bonds through acid-base interactions up to covalent bonds). The interaction partners should be brought into atomic contact through the physical connection under pressure. To achieve this, in addition to the previous cleaning, it is also necessary to exclude new contaminations. In particular, an adsorbate layer that forms due to moisture must also be prevented. While the steps of cleaning, activation and pressing, which are absolutely necessary for an optimal permanent connection, already achieve a considerable strength of the connection, tempering or storage of the connected parts can further increase the strength achieved. In contrast to the direct connection methods, in which the polymer chains penetrate one another as a result of an increase in temperature above the glass transition temperature T G or the melting temperature T M , connection mechanisms are used in the invention in which the formation of chemical compounds and intermolecular interactions serve as a functional principle , This also has the consequence that not only the same or similar but also very different materials can now be joined together. These no longer have to be adjusted in their melting point and also not be compatible.

Der Verzicht auf haftvermittelnde Hilfssubstanzen gewahrleistet, dass vorhandene MikroStrukturen an der Oberflache nicht unerwünscht modifiziert, verfullt oder anderweitig beeinflusst werden.The absence of auxiliary substances that promote adhesion ensures that existing microstructures on the surface are not undesirably modified, filled or otherwise influenced.

Weitere vorteilhafte Ausgestaltungen sind m den Unteranspruchen enthalten. Die Erfindung soll nachstehend anhand von Beispielen naher erläutert werden.Further advantageous configurations are contained in the subclaims. The invention will be explained in more detail below with the aid of examples.

Ein Ausfuhrungsbeispiel beinhaltet die Verbindung zweier planarer Platten, von denen mindestens eine über eine mikrostrukturierte Oberflache verfugen kann. Selbstverständlich beschrankt sich die Anwendung des erfmdungsgemaßen Verfahrens nicht auf planare Platten und auch nicht auf solche mit mikrostrukturierter Oberflache. Beide Platten können aus dem gleichen polymeren Werkstoff, wie z. B. Polymethylmethacrylat (PMMA) oder anderen Materialien, insbesondere thermoplastischen Kunststoffen, wie z. B. Polycarbonat (PC) oder Polyethylen (PE) bestehen . Abweichend von der Gleichartigkeit der Werkstoffe kann für eine der Platten auch ein anderer polymerer Werkstoff oder aber auch Glas, Metall oder ein Halbleitermaterial verwendet werden.An exemplary embodiment includes the connection of two planar plates, at least one of which can have a microstructured surface. Of course, the application of the method according to the invention is not restricted to planar plates and also not to those with a microstructured surface. Both plates can be made of the same polymeric material, such as. B. polymethyl methacrylate (PMMA) or other materials, especially thermoplastics, such as. B. polycarbonate (PC) or polyethylene (PE) exist. In a departure from the uniformity of the materials, another polymer material or else glass, metal or a semiconductor material can also be used for one of the plates.

Bevor die beiden Platten miteinander verbunden werden können, erfolgt zunächst eine Reinigung in einem, mit einer Remigungsflussigkeit gefüllten Ultraschallbad, in das die Platten getaucht werden. Die Reinigungszeit betragt bei Raumtemperatur ca. 5 Minuten. Als Remigungsflussigkeit wird im vorliegenden Beispiel Ethanol (absolut) verwendet. Es sind jedoch auch wassrige Tensidlosungen für diesen Zweck geeignet, die nichtionische und/oder ionische Tenside m Konzentrationen zwischen 0,01% und 5% enthalten, wobei der Reinigungsprozess bei einer Prozesstemperatur von 60 °C erfolgen sollte.Before the two plates can be connected to each other, they are first cleaned in an ultrasonic bath filled with a cleaning liquid into which the plates are dipped. The cleaning time is about 5 minutes at room temperature. In the present example, ethanol (absolute) is used as the cleaning liquid. However, aqueous surfactant solutions which contain nonionic and / or ionic surfactants in concentrations between 0.01% and 5% are also suitable for this purpose, the cleaning process being carried out at a process temperature of 60.degree.

Danach werden die beiden Teile getrocknet und einer Behandlung m einem Niederdruckplasma mit Sauerstoff als Reaktionsgas ausgesetzt, bei der reaktive funktioneile Gruppen an den zu verbindenden Oberflachen der beiden Platten erzeugt bzw. in ihrer Konzentration auf den Oberflachen erhöht werden. Die Plasmabehandlung kann in einem Plasmareaktor mit einer induktiv gekoppelten Hochfrequenz von 13,56 MHz in einer Remote-Position erfolgen, bei der die zu aktivierenden Oberflachen m einiger Entfernung zur eigentlichen Plasmazone angeordnet sind. Die Prozessdauer kann in einem Zeitintervall von 1 bis 10 Sekunden liegen, wobei zwei Sekunden bevorzugt werden sollten.The two parts are then dried and subjected to a treatment in a low-pressure plasma with oxygen as the reaction gas, in which reactive functional groups are generated on the surfaces of the two plates to be joined or their concentration is increased on the surfaces. The plasma treatment can be carried out in a plasma reactor with an inductively coupled high frequency of 13.56 MHz in a remote position, in which the surfaces to be activated are arranged some distance from the actual plasma zone. The process time can range from 1 to 10 seconds, with two seconds being preferred.

Die Plasmabehandlung kann auch in einem Reaktor erfolgen, der z. B. mit einer kHz - oder GHz - Anregung arbeitet. Auch die Zeiten und die anderen Reaktionsbedingungen können in einem solchen Bereich variieren, m dem eine ausreichende Oberflächenfunktionalisierung erfolgt, ohne dass ein Abbau eintritt. Zu diesem Zweck muss die Plasmawirkung sehr definiert dosiert werden. Als Prozessgase können außer Sauerstoff auch andere Gase, z.B. Stickstoff, Ammoniak und auch schichtbildende Gase wie Methan oder Acetylen verwendet werden. Schließlich kann die Behandlung auch für jedes der beiden zu verbindenden Teile unterschiedlich, insbesondere mit unterschiedlichen Prozessgasen erfolgen.The plasma treatment can also be carried out in a reactor which, for. B. works with a kHz or GHz excitation. The times and the other reaction conditions can also vary within such a range sufficient surface functionalization takes place without degradation occurring. For this purpose, the plasma effect must be dosed in a very defined manner. In addition to oxygen, other gases, for example nitrogen, ammonia and also layer-forming gases such as methane or acetylene, can be used as process gases. Finally, the treatment can also be carried out differently for each of the two parts to be connected, in particular with different process gases.

Die nach der Plasmabehandlung absolut trockenen, aktivierten Platten werden dann in Kontakt miteinander gebracht und unter Temperaturerhöhung verpresst. Die Erhöhung der Temperatur erfolgt in einem Bereich unterhalb der Glasübergangstemperatur TG bzw. bis zu dieser Temperatur, ohne diese jedoch zu erreichen. Da bei diesem Verfahrensschritt ein Zutritt von Feuchtigkeit jeglicher Art auszuschließen ist, sollte das Verbinden und Verpressen idealerweise in der Plasmakammer (Vakuumkammer) erfolgen, in der auch der Aktivierungsschritt vollzogen wird.The activated plates, which are absolutely dry after the plasma treatment, are then brought into contact with one another and pressed with an increase in temperature. The temperature is increased in a range below the glass transition temperature T G or up to this temperature, but without reaching it. Since any access of moisture of any kind can be excluded in this process step, the connection and pressing should ideally take place in the plasma chamber (vacuum chamber), in which the activation step is also carried out.

Für das Verpressen von PMMA-Platten eignen sich die folgenden Prozessbedingungen. Der Temperaturbereich der zum Verpressen dienenden Halteelemente für die PMMA- Platten sollte zwischen Raumtemperatur und 80 °C, der Druck zwischen 80 bar und 500 bar und die Presszeit zwischen 0,5 min und 10 min liegen. Optimale Ergebnisse können bei 60 °C, 200 bar und 1 min erzielt werden.The following process conditions are suitable for pressing PMMA sheets. The temperature range of the holding elements for the PMMA plates used for pressing should be between room temperature and 80 ° C, the pressure between 80 bar and 500 bar and the pressing time between 0.5 min and 10 min. Optimal results can be achieved at 60 ° C, 200 bar and 1 min.

Nach dem Abkühlen sind die beiden Platten bereits dauerhaft miteinander verbunden. Dennoch hat sich ein Tempern vorteilhaft auf die Festigkeit der hergestellten Verbindung ausgewirkt, bei dem die beiden miteinander verbundenen Platten bei einer erhöhten Temperatur unterhalb der Glasubergangstemperatur TG trocken gelagert werden. Beispielsweise ist eine zweistündige Aufbewahrung in einem Trockenschrank bei einer Temperatur von 60 °C dafür geeignet. Auch eine Lagerung über eine längere Zeit bei Raumtemperatur fuhrt zu einem ahnlichen Ergebnis.After cooling, the two plates are already permanently connected to each other. Nevertheless, annealing has had an advantageous effect on the strength of the connection produced, in which the two plates connected to one another at an elevated temperature be stored dry below the glass transition temperature T G. For example, a two-hour storage in a drying cabinet at a temperature of 60 ° C is suitable for this. Storage for a long time at room temperature also leads to a similar result.

Die Vorteile des erfmdungsgemaßen Verfahrens sollen zusätzlich anhand von weiteren Ausfuhrungs- und Vergleichsbeispielen demonstriert werden.The advantages of the method according to the invention are also to be demonstrated on the basis of further exemplary embodiments and comparative examples.

Beispiel 1example 1

Zwei PMMA-Platten, die 1 mm. bei 60 °C mit 200 bar verpreßt wurden, fallen nach dem Pressen ohne besondere Krafteinwirkung wieder auseinander.Two PMMA sheets that are 1 mm. were pressed at 60 ° C with 200 bar, fall apart again after pressing without any special force.

Beispiel 2Example 2

Zwei PMMA-Platten wurden 5 mm. Ethanol mit Ultraschall gereinigt und anschließend 2 s in einem Sauerstoffplasma (20 W; 0,5 mbar) behandelt. Die behandelten Flachen wurden aufeinandergelegt und 1 min. bei 60 °C mit 200 bar verpreßt .Two PMMA plates became 5 mm. Ethanol cleaned with ultrasound and then treated in an oxygen plasma (20 W; 0.5 mbar) for 2 s. The treated areas were placed on one another and 1 min. pressed at 60 ° C with 200 bar.

Die beiden Platten lassen sich nicht mehr zerstörungsfrei trennen; es tritt ein Kohasionsbruch auf, der zu einer Weißfarbung beider delaminierter Oberflachen fuhrt.The two plates can no longer be separated without being destroyed; there is a break in cohesion, which leads to a white coloring of both delaminated surfaces.

Beispiel 3Example 3

Zwei PMMA-Platten wurden ohne vorherige Reinigungsoperation 2 s in einem Sauerstoffplasma (20 W; 0,5 mbar) behandelt. Die behandelten Flachen wurden aufeinandergelegt und 1 mm. bei 60 °C mit 200 bar verpreßt .Two PMMA plates were treated in an oxygen plasma (20 W; 0.5 mbar) for 2 s without prior cleaning operation. The treated areas were placed on top of each other and 1 mm. pressed at 60 ° C with 200 bar.

Die beiden Platten lassen sich nur mit Kraftaufwand trennen; die beiden delam ierten Oberflachen zeigen keine sichtbaren Veränderungen / Schädigungen. Auch eine Verlängerung der Plasmabehandlungszelt bis z.B. 60 s bringt keine weitere Verbesserung der Verbundhaftung.The two plates can only be separated with effort; the two delaminated surfaces show none visible changes / damage. Even extending the plasma treatment tent up to 60 s, for example, does not improve bond adhesion any further.

Beispiel 4Example 4

Zwei PMMA-Platten wurden 5 mm. m Ethanol mit Ultraschall gereinigt. Die gereinigten Flachen wurden ohne weitere Vorbehandlung aufeinandergelegt und 1 mm. bei 60 °C mit 200 bar verpreßt. Die beiden Platten lassen sich leicht trennen; die beiden delammierten Oberflachen zeigen keine sichtbaren Veränderungen / Schädigungen.Two PMMA plates became 5 mm. m ethanol cleaned with ultrasound. The cleaned areas were placed on one another without further pretreatment and 1 mm. pressed at 60 ° C with 200 bar. The two plates can be easily separated; the two delaminated surfaces show no visible changes / damage.

Beispiel 5 Zwei PMMA-Platten wurden 5 mm. in Ethanol mit Ultraschall gereinigt und anschließend 2 s in einem SauerstoffplasmaExample 5 Two PMMA plates became 5 mm. ultrasonically cleaned in ethanol and then in an oxygen plasma for 2 s

(20 W; 0,5 mbar) behandelt. Die behandelten Flachen wurden aufeinandergelegt und 0,5 mm. bei 60 °C mit 200 bar verpreßt . Beide Platten lassen sich nur m t Kraftaufwand trennen; die beiden delammierten Oberflachen zeigen keine sichtbaren Veränderungen / Schädigungen.(20 W; 0.5 mbar) treated. The treated areas were placed on top of each other and 0.5 mm. pressed at 60 ° C with 200 bar. Both plates can only be separated with a t effort; the two delaminated surfaces show no visible changes / damage.

Identisch verpreßte PMMA-Platten wurden nach dem Pressen 2 h bei 60 °C m einem Trockenschrank gelagert. Die beiden Platten lassen sich nicht mehr zerstörungsfrei trennen; es tritt ein Kohasionsbruch auf, der zu einer Weißfarbung beider delammierter Oberflachen fuhrt. Identically pressed PMMA sheets were stored in a drying cabinet at 60 ° C. for 2 hours after the pressing. The two plates can no longer be separated without being destroyed; a break in cohesion occurs, which leads to a white coloring of both delaminated surfaces.

Claims

Patentanspr che Claims 1. Verfahren zum dauerhaften Verbinden von Polymerbauteilen mit Bauteilen aus gleichartigem oder andersartigem Material, deren zu verbindende Oberflachen zunächst gereinigt und anschließend zur Erzeugung von reaktiven funktionellen Gruppen aktiviert werden und bei dem die aktivierten Oberflachen zur Initiierung von Bindungen zwischen den erzeugten reaktiven funktionellen Gruppen unter Druckeinwirkung, Ausschluss von Feuchtigkeit und Erwärmung bis zur Glasubergangs- oder Schmelztemperatur der Polymerteile Kontakt miteinander gebracht werden, ohne dabei diese Temperaturen edoch zu erreichen.1. A process for the permanent connection of polymer components with components of the same or a different material, the surfaces to be connected are first cleaned and then activated to generate reactive functional groups, and the activated surfaces are used to initiate bonds between the generated reactive functional groups under pressure Exclusion of moisture and warming up to the glass transition or melting temperature of the polymer parts are brought into contact with one another without reaching these temperatures. 2. Verfahren nach Anspruch 1, bei dem die Reinigung in einem Ultraschallbad erfolgt.2. The method according to claim 1, wherein the cleaning is carried out in an ultrasonic bath. 3. Verfahren nach Anspruch 2, bei dem als Remigungsflussigkeit Ethanol dient.3. The method according to claim 2, in which ethanol serves as the cleaning liquid. 4. Verfahren nach Anspruch 2, bei dem als Remigungsflussigkeit Tensidlosungen dienen.4. The method according to claim 2, in which serve as cleaning liquid surfactant solutions. 5. Verfahren nach Anspruch 4, bei dem nichtionische und/oder ionische Tenside in wassπger Losung m einem Konzentrationsbereich von 0,01% bis 5 % enthalten sind.5. The method according to claim 4, in which nonionic and / or ionic surfactants are contained in a water solution in a concentration range of 0.01% to 5%. 6. Verfahren nach einem der Ansprüche 1 bis 5, bei dem die Aktivierung m einem Niederdruckplasma erfolgt.6. The method according to any one of claims 1 to 5, wherein the activation takes place in a low pressure plasma. 7. Verfahren nach Anspruch 6, bei dem für das Niederdruckplasma Sauerstoff als Prozessgas eingesetzt wird. 7. The method according to claim 6, in which oxygen is used as the process gas for the low-pressure plasma. 8. Verfahren nach einem der Ansprüche 1 bis 7, bei dem das Verbinden und Verpressen in derselben Vakuumkammer erfolgt, in der auch die Aktivierung vollzogen wird.8. The method according to any one of claims 1 to 7, in which the connection and pressing takes place in the same vacuum chamber in which the activation is also carried out. 9. Verfahren nach Anspruch 8, bei dem die zu verbindenden Bauteile als PMMA-Platten ausgebildet sind.9. The method according to claim 8, wherein the components to be connected are designed as PMMA plates. 10. Verfahren nach Anspruch 9, bei dem das Verpressen der PMMA-Platten bei Temperaturen zwischen Raumtemperatur und 80 °C, Drücken zwischen 80 bar und 500 bar und einer Presszeit zwischen 0,5 min und 10 min erfolgt.10. The method according to claim 9, wherein the pressing of the PMMA plates at temperatures between room temperature and 80 ° C, pressures between 80 bar and 500 bar and a pressing time between 0.5 min and 10 min. 11. Verfahren nach Anspruch 9, bei dem das Verpressen der PMMA-Platten bei einer Temperatur von 60 °C, einem Druck von 200 bar und einer Zeitdauer von 1 min erfolgt .11. The method according to claim 9, wherein the pressing of the PMMA plates is carried out at a temperature of 60 ° C, a pressure of 200 bar and a period of 1 min. 12. Verfahren nach einem der Ansprüche 1 bis 11, bei dem nach dem Verbinden ein Tempern erfolgt. 12. The method according to any one of claims 1 to 11, in which an annealing takes place after the connection.
PCT/EP2001/000890 2000-02-03 2001-01-27 Method for durable joining of polymer components Ceased WO2001057119A1 (en)

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