EP1558518A2 - Method for production of a component with a micro-joint and component produced by said method - Google Patents

Method for production of a component with a micro-joint and component produced by said method

Info

Publication number
EP1558518A2
EP1558518A2 EP03767900A EP03767900A EP1558518A2 EP 1558518 A2 EP1558518 A2 EP 1558518A2 EP 03767900 A EP03767900 A EP 03767900A EP 03767900 A EP03767900 A EP 03767900A EP 1558518 A2 EP1558518 A2 EP 1558518A2
Authority
EP
European Patent Office
Prior art keywords
micro
substrate
transfer substrate
structured
joint
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.)
Withdrawn
Application number
EP03767900A
Other languages
German (de)
French (fr)
Inventor
Olivier Constantin
Frédérique Mittler
Philippe Combette
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.)
Commissariat a lEnergie Atomique et aux Energies Alternatives CEA
Original Assignee
Commissariat a lEnergie Atomique CEA
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 Commissariat a lEnergie Atomique CEA filed Critical Commissariat a lEnergie Atomique CEA
Publication of EP1558518A2 publication Critical patent/EP1558518A2/en
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
    • B29C65/52—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive
    • B29C65/526—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the way of applying the adhesive by printing or by transfer from the surfaces of elements carrying the adhesive, e.g. using brushes, pads, rollers, stencils or silk screens
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • 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
    • B01L3/502707—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 characterised by the manufacture of the container or its components
    • 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
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
    • B29C66/112—Single lapped joints
    • 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
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
    • B29C66/112—Single lapped joints
    • B29C66/1122—Single lap to lap joints, i.e. overlap joints
    • 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
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/13—Single flanged joints; Fin-type joints; Single hem joints; Edge joints; Interpenetrating fingered joints; Other specific particular designs of joint cross-sections not provided for in groups B29C66/11 - B29C66/12
    • B29C66/131—Single flanged joints, i.e. one of the parts to be joined being rigid and flanged in the joint area
    • 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
    • B29C66/50—General aspects of joining tubular articles; General aspects of joining long products, i.e. bars or profiled elements; General aspects of joining single elements to tubular articles, hollow articles or bars; General aspects of joining several hollow-preforms to form hollow or tubular articles
    • B29C66/51—Joining tubular articles, profiled elements or bars; Joining single elements to tubular articles, hollow articles or bars; Joining several hollow-preforms to form hollow or tubular articles
    • B29C66/53—Joining single elements to tubular articles, hollow articles or bars
    • B29C66/534—Joining single elements to open ends of tubular or hollow articles or to the ends of bars
    • B29C66/5346—Joining single elements to open ends of tubular or hollow articles or to the ends of bars said single elements being substantially flat
    • 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
    • B29C66/50—General aspects of joining tubular articles; General aspects of joining long products, i.e. bars or profiled elements; General aspects of joining single elements to tubular articles, hollow articles or bars; General aspects of joining several hollow-preforms to form hollow or tubular articles
    • B29C66/51—Joining tubular articles, profiled elements or bars; Joining single elements to tubular articles, hollow articles or bars; Joining several hollow-preforms to form hollow or tubular articles
    • B29C66/54—Joining several hollow-preforms, e.g. half-shells, to form hollow articles, e.g. for making balls, containers; Joining several hollow-preforms, e.g. half-cylinders, to form tubular articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/12—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by using adhesives
    • B32B37/1284—Application of adhesive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
    • B81C1/00119—Arrangement of basic structures like cavities or channels, e.g. suitable for microfluidic systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00349—Creating layers of material on a substrate
    • B81C1/00357—Creating layers of material on a substrate involving bonding one or several substrates on a non-temporary support, e.g. another substrate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C3/00—Assembling of devices or systems from individually processed components
    • B81C3/008—Aspects related to assembling from individually processed components, not covered by groups B81C3/001 - B81C3/002
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00833—Plastic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/0086—Dimensions of the flow channels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/06—Fluid handling related problems
    • B01L2200/0689—Sealing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2200/00—Solutions for specific problems relating to chemical or physical laboratory apparatus
    • B01L2200/12—Specific details about manufacturing devices
    • 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
    • B01L2300/04—Closures and closing means
    • B01L2300/041—Connecting closures to device or container
    • B01L2300/044—Connecting closures to device or container pierceable, e.g. films, membranes
    • 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
    • B01L2300/0809—Geometry, shape and general structure rectangular shaped
    • B01L2300/0819—Microarrays; Biochips
    • 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
    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • 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
    • B29C66/024—Thermal pre-treatments
    • B29C66/0242—Heating, or preheating, e.g. drying
    • 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
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/756—Microarticles, nanoarticles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00—Specific applications of microelectromechanical systems
    • B81B2201/02—Sensors
    • B81B2201/0214—Biosensors; Chemical sensors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00—Specific applications of microelectromechanical systems
    • B81B2201/05—Microfluidics
    • B81B2201/058—Microfluidics not provided for in B81B2201/051 - B81B2201/054
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00—Manufacture or treatment of microstructural devices or systems
    • B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0174—Manufacture or treatment of microstructural devices or systems in or on a substrate for making multi-layered devices, film deposition or growing
    • B81C2201/019—Bonding or gluing multiple substrate layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00—Manufacture or treatment of microstructural devices or systems
    • B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0174—Manufacture or treatment of microstructural devices or systems in or on a substrate for making multi-layered devices, film deposition or growing
    • B81C2201/0191—Transfer of a layer from a carrier wafer to a device wafer

Definitions

  • the invention relates to a method for producing a component, comprising a micro-structured substrate and a complementary element assembled by means of an assembly joint. It also relates to a component made by this method.
  • micro-structured components in particular micro-fluidic devices (bio-chips, "lab-on-chip”, etc.) or micro-mechanical devices (MEMS, OEMS, etc.), generally involves micro-structuring. at the surface or in volume of at least one substrate where free spaces are created which allow the circulation or the storage of fluids.
  • the cavities and channels thus created are open on at least one side and therefore need to be connected or assembled to another structure (open or closed hood, capillaries, other microfluidic substrate ).
  • micro-structured components require assembly joints and possibly microstructured seals.
  • manipulation and positioning of micro-structured joints is very difficult.
  • these techniques require high temperatures or chemical preparations which limit the possibility of functionalizing the components to be assembled (for example by biological grafting) and are limiting in the choice of materials.
  • thermal welding also limits the choice of materials.
  • pre-bonded adhesive films has the disadvantage of the presence of glue in contact with fluids to handle and poses problems of biological compatibility.
  • the object of the invention is to remedy these drawbacks and, more particularly, to propose a process for manufacturing micro-structured components, minimizing the problems of biological compatibility, while reducing the complexity and the manufacturing cost. According to the invention, this object is achieved by the fact that the method comprises the manufacture of the assembly joint by:
  • the transfer substrate is flexible and the withdrawal of the transfer substrate is carried out by pulling it at one end.
  • the method comprises a step of chemical activation of the complementary element and / or, after the third step, a step of chemical activation of the assembly joint disposed on the micro-structured substrate.
  • the invention also relates to a component, made by the above method, and comprising a complementary element assembled to the micro-structured substrate by the assembly joint, the element being a cover, another micro-structured substrate, a capillary or a matrix of capillaries integral with each other.
  • Figures 1 to 6 show different stages of a particular embodiment of a method according to the invention.
  • FIG. 7 represents a particular embodiment of the invention with support zones on the micro-structured substrate.
  • FIG. 8 represents a particular embodiment of a component according to the invention, in which the complementary element is a capillary.
  • Figure 9 shows an embodiment variation of a transfer substrate.
  • a thin layer of polymer 2 is deposited on a transfer substrate 1.
  • a deposition technique typically used is spinning.
  • the polymer of the thin layer 2 and the material of the transfer substrate 1 must have a chemical affinity for the second and third steps described below.
  • the materials of the transfer substrate 1 and the polymer thin film 2 are both polydimethylsiloxane (PDMS).
  • PDMS polydimethylsiloxane
  • An advantageous property of a transfer substrate 1 in PDMS is its flexibility.
  • an additional intermediate step of crosslinking for example by heating, can be added just after the deposit.
  • the second step (FIG. 3) consists of contacting the thin polymer layer 2 carried by the transfer substrate 1 with the micro-structured substrate.
  • the chemical affinity between the thin polymer layer 2 and the microstructured substrate 3 must be stronger than the chemical affinity between the thin polymer layer 2 and the transfer substrate 1.
  • the adaptation of the affinity between the thin polymer layer 2 and the micro-structured substrate 3 can be carried out, before the second step, by additional intermediate steps of chemical activation. As shown in FIG. 2, the chemical activation steps can be applied to the polymer layer 2 and / or the micro-structured substrate 3.
  • a chemical activation means used is an oxygen plasma.
  • FIG. 2 a simultaneous plasma oxidation of the thin polymer layer 2 and the micro-structured substrate 3 is shown.
  • the toughness of the thin polymer layer 2 decreases after plasma oxidation, facilitating the third step of the method described below.
  • the thin layer of polymer can be irreversibly bonded to the micro-structured substrate by suitably adapting the chemical affinity by chemical activation steps prior to the second step (Fig. 2).
  • the transfer substrate 1 is removed. Only the zones of the thin polymer layer 2 in contact with the micro-structured substrate 3 during the second step remain on the micro-structured substrate 3. In fact, the chemical affinity between the micro-structured substrate 3 and the thin layer of polymer 2 being stronger than the chemical affinity between the thin polymer layer and the transfer substrate 1, the thin polymer layer 2 tears, a part 4 remaining attached to the micro-structured substrate 3, the rest 6 leaving with the transfer substrate 1. The areas of the thin layer of polymer 2 which were not in contact with the micro-structured substrate 3 during the second step thus remain as residues 6 on the transfer substrate 1. The assembly joint 4 is thus formed by the zones of the layer remaining polymer on the micro-structured substrate 3.
  • the second step requires no alignment, the micro-structured substrate 3 itself defining the contact areas with the layer 2.
  • the toughness of the thin polymer layer 2 must be very low. The tenacity can be reduced in particular by plasma oxidation preceding the second step (FIG. 2).
  • the method described above allows the formation of an assembly joint 4 conforming to the micro-structured substrate 3 to be connected or assembled, without leaving a dead space and without adding material above cavities 5 formed in the substrate. micro-structured 3.
  • the surface of the joint 4 in contact with the materials (fluids, liquids, etc. ..) contained in the cavities 5 is minimized, which allows to minimize the possible interaction between the material of the assembly joint 4 and the materials contained in the cavities 5.
  • the biological compatibility of the component is thus optimized.
  • This method allows simultaneous formation of a multitude of assembly micro-joints, each of which can be very small ( ⁇ 20 ⁇ m), on micro-structured substrates of large area (treatment of a complete wafer), the micro-substrate structured delimiting itself the joint assembly.
  • the process is fast, inexpensive and requires no alignment for joint formation.
  • performing the third step is facilitated by the use of a flexible transfer substrate that can be removed by one end (Figure 4). This avoids the use of excessive force that can damage the component.
  • a complementary element 7 can be fixed on the micro-structured substrate 3 by means of the joint 4, possibly reversibly, by keeping the complementary element 7 by a device (not shown) providing contact intimate with the joint assembly 4. It is also possible to fix the complementary element 7 irreversibly on the micro-structured substrate 3 by adding one or more steps of chemical activation of the joint 4 and / or the complementary element 7, for example by plasma oxidation (FIG. 5).
  • the micro-structured substrate 3 comprises a support zone 8 serving to support the transfer substrate 1 during the second step in the case where zones intended to define the joint joint 4 are relatively distant from each other.
  • the bearing zones 8 thus prevent the polymer thin film 2 from sticking to lower surfaces 9 of the micro-structured substrate 3 between two zones defining the jointing joint, while ensuring the parallelism between the transfer substrate and the the micro-structured substrate during the second step.
  • the complementary element 7 is a cover 7 closing the cavities 5 of the microstructured substrate 3.
  • complementary element is constituted by a capillary 10 or a matrix of capillaries integral with each other.
  • the complementary element 7 is another micro-structured substrate.
  • the transfer substrate is a micro-structured substrate 11, making it possible to avoid the contact of the thin polymer layer 2 on certain zones 12 of the surface of the micro-structured substrate. 3.
  • the formation of such a microstructured transfer substrate 11 can be made by molding for example.
  • a micro-structured transfer substrate 11 requires alignment with the micro-structured substrate 3 during the second process step, making the process more complicated.
  • the material of the joining joint will be selected from thermo-hard resins, elastomers or elastomeric thermoplastics meeting the following criteria:
  • PDMS polydimethylsiloxane
  • rank Sylgard ® 184 Dow Corning ® is particularly suitable, thanks to its optical qualities and biological compatibility.
  • Dow Corning ® Sylgard ® 184 Grade PDMS can be activated with low energy oxygen plasma
  • the material of the transfer substrate is preferably chosen so as to form covalent bonds (free methacryl groups, for example, which bind to the methacryl groups of the PDMS of the thin layer) with the material of the jointing joint and for its flexibility. For this reason, a preferred choice is a PDMS transfer substrate, freshly made to avoid storage-related dusting problems, since PDMS is very dust-hungry.
  • the thin layer of PDMS is preferentially heat-cured to save time (4 hours at 60 °).
  • the use of a spinner makes it possible to choose the thickness of the joint (typically between a few micrometers and 50 ⁇ m).
  • the material of the micro-structured substrate to be assembled or connected, or at least of the surfaces dedicated to the formation of the joint, must be able to be activated to form covalent bonds with said jointing joint. Similarly, covalent bonds can be made between said seal and the complementary element. Under these conditions, the assembled final component can be fluid tight.
  • the micro-structured substrate In the manufacture of enzymatic digestion reactors on silicon, the micro-structured substrate consists of channels several millimeters long and 1 mm wide, in which are milled 5 ⁇ m or 10 ⁇ m diameter column matrices (several millions of columns). This makes it possible to increase the surface / volume ratio of said reactors, the enzymatic digestion reaction taking place between wall-grafted enzymes and proteins carried in these reactors.
  • the present invention has notably allowed the formation of an assembly joint on very small patterns (square columns of

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
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Abstract

The method for production of a component with a micro-joint comprises a first step of deposition of a layer of polymer (2) on a transfer substrate (1), for the embodiment of an assembly joint (4), a second step of bringing the polymer layer into contact with a micro-structured substrate (3) and a third step of withdrawing the transfer substrate. As a result of the difference of the chemical affinity between the polymer layer (2) and the transfer substrate (1) and the chemical affinity between the polymer layer (2) and the micro-structured substrate, the zones (4) of the polymer layer, which are in contact with the micro-structured substrate (3) during the second step, remain on the micro-structured substrate (3) after the third step. Said zones embody the assembly joint.

Description

Procédé de réalisation d'un composant comportant un micro-joint et composant réalisé par ce procédéProcess for producing a component comprising a micro-joint and component produced by this process
Domaine technique de l'inventionTechnical field of the invention
L'invention concerne un procédé de réalisation d'un composant, comportant un substrat micro-structuré et un élément complémentaire assemblés au moyen d'un joint d'assemblage. Elle concerne également un composant réalisé par ce procédé.The invention relates to a method for producing a component, comprising a micro-structured substrate and a complementary element assembled by means of an assembly joint. It also relates to a component made by this method.
État de la techniqueState of the art
La réalisation de composants micro-structurés, notamment les dispositifs micro- fluidiques (bio-puces, « lab-on-chip », etc..) ou micro-mécaniques (MEMS, OEMS, etc.), implique généralement la micro-structuration en surface ou en volume d'au moins un substrat où sont créés des espaces libres qui permettent la circulation ou le stockage de fluides. Les cavités et canaux ainsi créés sont ouverts sur au moins un côté et nécessitent donc d'être connectés ou assemblés à une autre structure ( capot ouvert ou fermé, capillaires, autre substrat micro-fluidique...).The production of micro-structured components, in particular micro-fluidic devices (bio-chips, "lab-on-chip", etc.) or micro-mechanical devices (MEMS, OEMS, etc.), generally involves micro-structuring. at the surface or in volume of at least one substrate where free spaces are created which allow the circulation or the storage of fluids. The cavities and channels thus created are open on at least one side and therefore need to be connected or assembled to another structure (open or closed hood, capillaries, other microfluidic substrate ...).
L'assemblage de composants micro-structurés nécessite des joints d'assemblage et des joints d'etancheité éventuellement micro-structurés. Or, la manipulation et le positionnement de joints micro-structurés est très difficile. Il existe des techniques utilisant en particulier le Polydiméthylsiloxane comme joint d'assemblage, avec des méthodes complexes pour définir la surface du joint. Il existe d'autres techniques d'assemblage de substrats dont les surfaces d'assemblage peuvent être localement très petites, mais ces techniques nécessitent des températures élevées ou des préparations chimiques limitant la possibilité de fonctionnaliser les composants à assembler (par exemple par greffage biologique) et sont limitatives dans le choix des matériaux. Dans le domaine de l'assemblage des polymères, la soudure thermique limite elle aussi le choix des matériaux. L'utilisation de films adhésifs pré-encollés présente l'inconvénient de présence de colle au contact de fluides à manipuler et pose des problèmes de compatibilité biologique.The assembly of micro-structured components requires assembly joints and possibly microstructured seals. However, the manipulation and positioning of micro-structured joints is very difficult. There are techniques using in particular Polydimethylsiloxane as an assembly joint, with complex methods for defining the joint surface. There are other techniques of assembling substrates whose surfaces However, these techniques require high temperatures or chemical preparations which limit the possibility of functionalizing the components to be assembled (for example by biological grafting) and are limiting in the choice of materials. In the field of polymer assembly, thermal welding also limits the choice of materials. The use of pre-bonded adhesive films has the disadvantage of the presence of glue in contact with fluids to handle and poses problems of biological compatibility.
Les techniques d'encollage plus classiques (distribution de colle par seringue, tampographie, rouleaux encolleurs, sérigraphie), outre les problèmes liés à la polymérisation de colles liquides en présence d'espèces biologiques, s'avèrent inadaptées à l'assemblage de micro-structures présentant des surfaces d'assemblage très petites (<20μm).The more conventional sizing techniques (glue dispensing by syringe, pad printing, gluing rolls, screen printing), in addition to the problems related to the polymerization of liquid glues in the presence of biological species, prove to be unsuitable for the assembly of microparticles. structures with very small joining surfaces (<20μm).
Ainsi, les techniques d'assemblage connues posent des problèmes de compatibilité biologique et/ou sont complexes, ce qui limite les possibilités d'application. De plus, certaines techniques ne permettent pas un assemblage réversible de deux composants.Thus, the known assembly techniques pose problems of biological compatibility and / or are complex, which limits the possibilities of application. In addition, some techniques do not allow a reversible assembly of two components.
Objet de l'inventionObject of the invention
L'invention a pour but de remédier à ces inconvénients et, plus particulièrement, de proposer un procédé de fabrication de composants micro-structurés, minimisant les problèmes de compatibilité biologique, tout en réduisant la complexité et le coût de fabrication. Selon l'invention, ce but est atteint par le fait que le procédé comporte la fabrication du joint d'assemblage par :The object of the invention is to remedy these drawbacks and, more particularly, to propose a process for manufacturing micro-structured components, minimizing the problems of biological compatibility, while reducing the complexity and the manufacturing cost. According to the invention, this object is achieved by the fact that the method comprises the manufacture of the assembly joint by:
- une première étape, de dépôt sur un substrat de transfert d'une couche mince d'un polymère, le substrat de transfert et la couche mince de polymère ayant une affinité chimique prédéterminée,a first step of deposition on a transfer substrate of a thin layer of a polymer, the transfer substrate and the thin layer of polymer having a predetermined chemical affinity,
- une seconde étape, de mise en contact du substrat micro-structuré et de la couche mince de polymère, le substrat micro-structuré et la couche mince de polymère ayant une affinité chimique plus forte que l'affinité chimique entre le substrat de transfert et la couche mince de polymère, - une troisième étape, de retrait du substrat de transfert, de manière à ce que le joint d'assemblage soit formé par les zones de la couche mince de polymère venant en contact avec le substrat micro-structuré au cours de la seconde étape.a second step of contacting the micro-structured substrate and the thin polymer layer, the micro-structured substrate and the thin polymer layer having a higher chemical affinity than the chemical affinity between the transfer substrate and the thin layer of polymer, - a third step of removing the transfer substrate, so that the joint is formed by the areas of the thin layer of polymer coming into contact with the micro-structured substrate during of the second step.
Selon un mode de réalisation préférentiel, le substrat de transfert est flexible et le retrait du substrat de transfert est effectué en le tirant par une extrémité.According to a preferred embodiment, the transfer substrate is flexible and the withdrawal of the transfer substrate is carried out by pulling it at one end.
Selon un développement de l'invention, le procédé comporte une étape d'activation chimique de l'élément complémentaire et/ou, après la troisième étape, une étape d'activation chimique du joint d'assemblage disposé sur le substrat micro-structuré. Ainsi, un assemblage irréversible du substrat micro- structuré et de l'élément complémentaire peut être réalisé.According to a development of the invention, the method comprises a step of chemical activation of the complementary element and / or, after the third step, a step of chemical activation of the assembly joint disposed on the micro-structured substrate. Thus, an irreversible assembly of the micro-structured substrate and the complementary element can be realized.
L'invention a également pour objet un composant, réalisé par le procédé ci- dessus, et comportant un élément complémentaire assemblé au substrat micro- structuré par le joint d'assemblage, l'élément étant un capot, un autre substrat micro-structuré, un capillaire ou une matrice de capillaires solidaires entre eux. Description sommaire des dessinsThe invention also relates to a component, made by the above method, and comprising a complementary element assembled to the micro-structured substrate by the assembly joint, the element being a cover, another micro-structured substrate, a capillary or a matrix of capillaries integral with each other. Brief description of the drawings
D'autres avantages et caractéristiques ressortiront plus clairement de la description qui va suivre de modes particuliers de réalisation de l'invention donnés à titre d'exemples non limitatifs et représentés aux dessins annexés, dans lesquels :Other advantages and features will emerge more clearly from the following description of particular embodiments of the invention given by way of non-limiting example and represented in the accompanying drawings, in which:
Les figures 1 à 6 représentent différentes étapes d'un mode particulier de réalisation d'un procédé selon l'invention.Figures 1 to 6 show different stages of a particular embodiment of a method according to the invention.
La figure 7 représente un mode particulier de réalisation de l'invention avec des zones d'appui sur le substrat micro-structuré.FIG. 7 represents a particular embodiment of the invention with support zones on the micro-structured substrate.
La figure 8 représente un mode particulier de réalisation d'un composant selon l'invention, dans lequel l'élément complémentaire est un capillaire. La figure 9 représente une variation de réalisation d'un substrat de transfert.FIG. 8 represents a particular embodiment of a component according to the invention, in which the complementary element is a capillary. Figure 9 shows an embodiment variation of a transfer substrate.
Description de modes particuliers de réalisation.Description of particular embodiments.
Dans une première étape du procédé représenté aux figures 1 à 6, une couche mince de polymère 2 est déposée sur un substrat de transfert 1. Une technique de dépôt typiquement utilisée est l'étalement à la tournette. Le polymère de la couche mince 2 et le matériau du substrat de transfert 1 doivent avoir une affinité chimique permettant les seconde et troisième étapes décrites ci- dessous. Dans un mode de réalisation préféré, les matériaux du substrat de transfert 1 et de la couche mince de polymère 2 sont tous deux du Polydiméthylsiloxane (PDMS). Une propriété avantageuse d'un substrat de transfert 1 en PDMS est sa flexibilité. Selon le polymère utilisé pour la couche mince 2 et la technique de dépôt, une étape supplémentaire intermédiaire de réticulation, par exemple par échauffement, peut être rajoutée juste après le dépôt.In a first step of the process shown in Figures 1 to 6, a thin layer of polymer 2 is deposited on a transfer substrate 1. A deposition technique typically used is spinning. The polymer of the thin layer 2 and the material of the transfer substrate 1 must have a chemical affinity for the second and third steps described below. In a preferred embodiment, the materials of the transfer substrate 1 and the polymer thin film 2 are both polydimethylsiloxane (PDMS). An advantageous property of a transfer substrate 1 in PDMS is its flexibility. Depending on the polymer used for the thin layer 2 and the deposition technique, an additional intermediate step of crosslinking, for example by heating, can be added just after the deposit.
La seconde étape (figure 3) consiste à mettre en contact la couche mince de polymère 2, portée par le substrat de transfert 1 , avec le substrat micro-structuréThe second step (FIG. 3) consists of contacting the thin polymer layer 2 carried by the transfer substrate 1 with the micro-structured substrate.
3. L'affinité chimique entre la couche mince de polymère 2 et le substrat micro- structuré 3 doit être plus forte que l'affinité chimique entre la couche mince de polymère 2 et le substrat de transfert 1. L'adaptation de l'affinité chimique entre la couche mince de polymère 2 et le substrat micro-structuré 3 peut être effectuée, avant la seconde étape, par des étapes supplémentaires intermédiaires d'activation chimique. Comme représenté à la figure 2, les étapes d'activation chimique peuvent s'appliquer à la couche de polymère 2 et/ou au substrat micro-structuré 3. Un moyen d'activation chimique utilisé est un plasma d'oxygène. A la figure 2, une oxydation plasma simultanée de la couche mince de polymère 2 et du substrat micro-structuré 3 est représentée. De plus, la ténacité de la couche mince de polymère 2 diminue après l'oxydation plasma, facilitant la troisième étape du procédé décrite ci-dessous. La couche mince de polymère peut être irréversiblement collée au substrat micro-structuré en adaptant de manière appropriée l'affinité chimique par des étapes d'activation chimique avant la seconde étape (figure 2).3. The chemical affinity between the thin polymer layer 2 and the microstructured substrate 3 must be stronger than the chemical affinity between the thin polymer layer 2 and the transfer substrate 1. The adaptation of the affinity between the thin polymer layer 2 and the micro-structured substrate 3 can be carried out, before the second step, by additional intermediate steps of chemical activation. As shown in FIG. 2, the chemical activation steps can be applied to the polymer layer 2 and / or the micro-structured substrate 3. A chemical activation means used is an oxygen plasma. In FIG. 2, a simultaneous plasma oxidation of the thin polymer layer 2 and the micro-structured substrate 3 is shown. In addition, the toughness of the thin polymer layer 2 decreases after plasma oxidation, facilitating the third step of the method described below. The thin layer of polymer can be irreversibly bonded to the micro-structured substrate by suitably adapting the chemical affinity by chemical activation steps prior to the second step (Fig. 2).
Dans une troisième étape, le substrat de transfert 1 est retiré. Seules les zones de la couche mince de polymère 2 en contact avec le substrat micro-structuré 3 pendant la seconde étape restent sur le substrat micro-structuré 3. En effet, l'affinité chimique entre le substrat micro-structuré 3 et la couche mince de polymère 2 étant plus forte que l'affinité chimique entre la couche mince de polymère et le substrat de transfert 1 , la couche mince de polymère 2 se déchire, une partie 4 restant fixée au substrat micro-structuré 3, le reste 6 partant avec le substrat de transfert 1. Les zones de la couche mince de polymère 2 qui n'étaient pas en contact avec le substrat micro-structuré 3 lors de la seconde étape restent ainsi en tant que résidus 6 sur le substrat de transfert 1. Le joint d'assemblage 4 est ainsi formé par les zones de la couche mince de polymère 2 restant sur le substrat micro-structuré 3. Dans le cas d'un substrat de transfert 1 plan, la seconde étape ne nécessite aucun alignement, le substrat micro-structuré 3 définissant lui-même les zones de contact avec la couche mince de polymère 2. Pour que la couche mince de polymère se déchire au bord des motifs usinés dans le substrat micro-structuré 3, la ténacité de la couche mince de polymère 2 doit être très faible. La ténacité peut être diminuée notamment par une oxydation plasma précédant la seconde étape (figure 2).In a third step, the transfer substrate 1 is removed. Only the zones of the thin polymer layer 2 in contact with the micro-structured substrate 3 during the second step remain on the micro-structured substrate 3. In fact, the chemical affinity between the micro-structured substrate 3 and the thin layer of polymer 2 being stronger than the chemical affinity between the thin polymer layer and the transfer substrate 1, the thin polymer layer 2 tears, a part 4 remaining attached to the micro-structured substrate 3, the rest 6 leaving with the transfer substrate 1. The areas of the thin layer of polymer 2 which were not in contact with the micro-structured substrate 3 during the second step thus remain as residues 6 on the transfer substrate 1. The assembly joint 4 is thus formed by the zones of the layer remaining polymer on the micro-structured substrate 3. In the case of a transfer substrate 1 plane, the second step requires no alignment, the micro-structured substrate 3 itself defining the contact areas with the layer 2. In order for the thin polymer layer to tear at the edge of the patterns machined in the micro-structured substrate 3, the toughness of the thin polymer layer 2 must be very low. The tenacity can be reduced in particular by plasma oxidation preceding the second step (FIG. 2).
Le procédé décrit ci-dessus permet la formation d'un joint d'assemblage 4 conforme au substrat micro-structuré 3 à connecter ou à assembler, sans laisser de volume mort et sans apport de matière au-dessus de cavités 5 formées dans le substrat micro-structuré 3. La surface du joint d'assemblage 4 en contact avec les matériaux (fluides, liquides, etc..) contenus dans les cavités 5 est donc minimisée, ce qui permet d'atténuer au maximum une éventuelle interaction entre le matériau du joint d'assemblage 4 et les matériaux contenus dans les cavités 5. La compatibilité biologique du composant est ainsi optimisée.The method described above allows the formation of an assembly joint 4 conforming to the micro-structured substrate 3 to be connected or assembled, without leaving a dead space and without adding material above cavities 5 formed in the substrate. micro-structured 3. The surface of the joint 4 in contact with the materials (fluids, liquids, etc. ..) contained in the cavities 5 is minimized, which allows to minimize the possible interaction between the material of the assembly joint 4 and the materials contained in the cavities 5. The biological compatibility of the component is thus optimized.
Ce procédé permet une formation simultanée d'une multitude de micro-joints d'assemblage, chacun pouvant être très petit (<20μm), sur des substrats micro- structurés de grande surface (traitement d'une plaquette complète), le substrat micro-structuré délimitant lui-même le joint d'assemblage. Le procédé est rapide, peu coûteux et ne nécessite aucun alignement pour la formation des joints.This method allows simultaneous formation of a multitude of assembly micro-joints, each of which can be very small (<20 μm), on micro-structured substrates of large area (treatment of a complete wafer), the micro-substrate structured delimiting itself the joint assembly. The process is fast, inexpensive and requires no alignment for joint formation.
Dans un mode de réalisation préférentiel, la réalisation de la troisième étape est facilitée par l'utilisation d'un substrat de transfert flexible qui peut être retiré par une extrémité (figure 4). Ceci permet d'éviter l'utilisation d'une force trop importante pouvant endommager le composant.In a preferred embodiment, performing the third step is facilitated by the use of a flexible transfer substrate that can be removed by one end (Figure 4). This avoids the use of excessive force that can damage the component.
Après la troisième étape, un élément complémentaire 7 peut être fixé sur le substrat micro-structuré 3 au moyen du joint d'assemblage 4, éventuellement de manière réversible, en maintenant l'élément complémentaire 7 par un dispositif (non représenté) assurant un contact intime avec le joint d'assemblage 4. Il est aussi possible de fixer l'élément complémentaire 7 de manière irréversible sur le substrat micro-structuré 3 en rajoutant une ou plusieurs étapes d'activation chimique du joint d'assemblage 4 et/ou de l'élément complémentaire 7, par exemple par oxydation plasma (figure 5). Un composant ainsi obtenu, comportant un substrat micro-structuré 3 et un élément complémentaire 7 assemblés au moyen d'un joint d'assemblage 4, est représenté à la figure 6.After the third step, a complementary element 7 can be fixed on the micro-structured substrate 3 by means of the joint 4, possibly reversibly, by keeping the complementary element 7 by a device (not shown) providing contact intimate with the joint assembly 4. It is also possible to fix the complementary element 7 irreversibly on the micro-structured substrate 3 by adding one or more steps of chemical activation of the joint 4 and / or the complementary element 7, for example by plasma oxidation (FIG. 5). A component thus obtained, comprising a micro-structured substrate 3 and a complementary element 7 assembled by means of an assembly joint 4, is represented in FIG.
Dans un mode de réalisation particulier, représenté à la figure 7, le substrat micro-structuré 3 comporte une zone d'appui 8 servant d'appui au substrat de transfert 1 au cours de la seconde étape dans le cas où des zones destinées à définir le joint d'assemblage 4 se trouvent relativement distantes l'une de l'autre. Les zones d'appui 8 empêchent ainsi un collage de la couche mince de polymère 2 sur des surfaces inférieures 9 du substrat micro-structuré 3 comprises entre deux zones définissant le joint d'assemblage, tout en assurant le parallélisme entre le substrat de transfert et le substrat micro-structuré pendant la seconde étape.In a particular embodiment, represented in FIG. 7, the micro-structured substrate 3 comprises a support zone 8 serving to support the transfer substrate 1 during the second step in the case where zones intended to define the joint joint 4 are relatively distant from each other. The bearing zones 8 thus prevent the polymer thin film 2 from sticking to lower surfaces 9 of the micro-structured substrate 3 between two zones defining the jointing joint, while ensuring the parallelism between the transfer substrate and the the micro-structured substrate during the second step.
Dans la variante de réalisation représentée à la figure 6, l'élément complémentaire 7 est un capot 7 fermant les cavités 5 du substrat micro- structuré 3. Selon un autre mode particulier de réalisation de l'invention, représenté à la figure 8, l'élément complémentaire est constitué par un capillaire 10 ou une matrice de capillaires solidaires entre eux. Dans un autre mode de réalisation, l'élément complémentaire 7 est un autre substrat micro-structuré.In the variant embodiment shown in FIG. 6, the complementary element 7 is a cover 7 closing the cavities 5 of the microstructured substrate 3. According to another particular embodiment of the invention, represented in FIG. complementary element is constituted by a capillary 10 or a matrix of capillaries integral with each other. In another embodiment, the complementary element 7 is another micro-structured substrate.
Dans un mode de réalisation particulier, représenté à la figure 9, le substrat de transfert est un substrat micro-structuré 11 , permettant d'éviter le contact de la couche mince de polymère 2 sur certaines zones 12 de la surface du substrat micro-structuré 3. La formation d'un tel substrat de transfert micro-stucturé 11 peut être effectué par moulage par exemple. Cependant, contrairement à un substrat de transfert plan, un substrat de transfert micro-structuré 11 nécessite un alignement avec le substrat micro-structuré 3 lors de la seconde étape du procédé, rendant le procédé plus compliqué.In a particular embodiment, represented in FIG. 9, the transfer substrate is a micro-structured substrate 11, making it possible to avoid the contact of the thin polymer layer 2 on certain zones 12 of the surface of the micro-structured substrate. 3. The formation of such a microstructured transfer substrate 11 can be made by molding for example. However, unlike a planar transfer substrate, a micro-structured transfer substrate 11 requires alignment with the micro-structured substrate 3 during the second process step, making the process more complicated.
Le matériau du joint d'assemblage sera choisi parmi les résines thermo-dures, les élastomères ou les thermoplastiques élastomères répondant aux critères suivants :The material of the joining joint will be selected from thermo-hard resins, elastomers or elastomeric thermoplastics meeting the following criteria:
- être suffisamment souple une fois le joint formé pour assurer sa fonction d'etancheité et d'assemblage, permettant par exemple de compenser des défauts de rugosité ou de planéité du substrat micro-structuré (comportement visco-élastique), - former, éventuellement après un traitement adéquat, des liaisons covalentes avec le substrat micro-structuré et le substrat de transfert,- Be sufficiently flexible once the seal formed to ensure its tightness and assembly function, allowing for example to compensate for roughness defects or flatness of the micro-structured substrate (visco-elastic behavior), - to form, possibly after a suitable treatment, covalent bonds with the micro-structured substrate and the transfer substrate,
- être peu tenace, éventuellement après un traitement adéquat, pour se déchirer facilement lors du transfert. Les familles de polymères précitées voient leur ténacité diminuer sur une profondeur généralement de 100μm à 150μm après une oxydation plasma. La gamme d'épaisseur du joint décrit étant inférieure, il sera oxydé et donc fragilisé sur toute son épaisseur, favorisant ainsi l'opération de transfert,- Be somewhat stubborn, possibly after adequate treatment, to tear easily during transfer. The aforementioned polymer families have their toughness decrease over a depth generally of 100 .mu.m to 150 .mu.m after plasma oxidation. Since the thickness range of the gasket described is lower, it will be oxidized and thus embrittled throughout its thickness, thereby favoring the transfer operation,
- préférentiellement, être disponible sous forme liquide pour pouvoir être étalé à la tournette. Le Polydiméthylsiloxane (PDMS), et plus particulièrement le grade 184 Sylgard® de Dow Corning®, est particulièrement adapté, notamment grâce à ses qualités optiques et de compatibilité biologique. Le PDMS du grade 184 Sylgard® de Dow Corning® peut être activé par un plasma d'oxygène à faible énergie- Preferably, be available in liquid form to be spread by spin. The polydimethylsiloxane (PDMS), especially the rank Sylgard ® 184 Dow Corning ®, is particularly suitable, thanks to its optical qualities and biological compatibility. Dow Corning ® Sylgard ® 184 Grade PDMS can be activated with low energy oxygen plasma
(création de sites SiOH et OH ; hydroxylation) lui permettant d'être irréversiblement collé au silicium, au verre, à une large gamme de plastiques, à lui-même, etc.. Il est disponible sous forme non réticulée, livré avec un agent durcissant, et donc suffisamment liquide pour être étalé à la tournette. L'hydroxylation de surface pourrait éventuellement être faite en plongeant le polymère choisi dans de l'eau bouillante. Cette voie s'avère cependant moins simple à mettre en œuvre.(creation of SiOH and OH sites, hydroxylation) allowing it to be irreversibly bonded to silicon, glass, a wide range of plastics, to itself, etc. It is available in non-crosslinked form, delivered with an agent hardening, and therefore liquid enough to be spread by spin. The surface hydroxylation could possibly be made by dipping the selected polymer in boiling water. This path is however less simple to implement.
Le matériau du substrat de transfert est préférentiellement choisi pour pouvoir former des liaisons covalentes (groupes méthacryl libres par exemple, qui se lient aux groupes méthacryl du PDMS de la couche mince) avec le matériau du joint d'assemblage et pour sa souplesse. Pour cette raison, un choix préférentiel est un substrat de transfert en PDMS, fraîchement fabriqué pour éviter tout problème d'empoussièrement lié au stockage, le PDMS étant très avide de poussière.The material of the transfer substrate is preferably chosen so as to form covalent bonds (free methacryl groups, for example, which bind to the methacryl groups of the PDMS of the thin layer) with the material of the jointing joint and for its flexibility. For this reason, a preferred choice is a PDMS transfer substrate, freshly made to avoid storage-related dusting problems, since PDMS is very dust-hungry.
La couche mince de PDMS est préférentiellemnt réticulée à chaud pour gagner du temps (4 heures à 60°). L'utilisation d'une tournette permet de choisir l'épaisseur du joint d'assemblage (typiquement entre quelques micromètres et 50μm).The thin layer of PDMS is preferentially heat-cured to save time (4 hours at 60 °). The use of a spinner makes it possible to choose the thickness of the joint (typically between a few micrometers and 50 μm).
Le matériau du substrat micro-structuré à assembler ou à connecter, ou du moins des surfaces dédiées à la formation du joint d'assemblage, doit pouvoir être activé pour former des liaisons covalentes avec ledit joint d'assemblage. De manière analogue, des liaisons covalentes peuvent être réalisées entre ledit joint et l'élément complémentaire. Dans ces conditions, le composant final assemblé peut être étanche aux fluides.The material of the micro-structured substrate to be assembled or connected, or at least of the surfaces dedicated to the formation of the joint, must be able to be activated to form covalent bonds with said jointing joint. Similarly, covalent bonds can be made between said seal and the complementary element. Under these conditions, the assembled final component can be fluid tight.
Dans la fabrication de réacteurs de digestion enzymatique sur silicium, le substrat micro-structuré se compose de canaux longs de plusieurs millimètres et larges de 1 mm, dans lequel sont micro-usinées des matrices de colonnes de 5 μm ou 10 μm de diamètre (plusieurs millions de colonnes). Ceci permet d'augmenter le rapport surface/volume desdits réacteurs, la réaction de digestion enzymatique ayant lieu entre des enzymes greffées aux parois et des protéines véhiculées dans ces réacteurs.In the manufacture of enzymatic digestion reactors on silicon, the micro-structured substrate consists of channels several millimeters long and 1 mm wide, in which are milled 5 μm or 10 μm diameter column matrices (several millions of columns). This makes it possible to increase the surface / volume ratio of said reactors, the enzymatic digestion reaction taking place between wall-grafted enzymes and proteins carried in these reactors.
La présente invention, telle que décrite ci-dessus, a notamment permis la formation d'un joint d'assemblage sur des motifs très petits (colonnes carrées deThe present invention, as described above, has notably allowed the formation of an assembly joint on very small patterns (square columns of
5 μm de côté et colonnes hexagonales de 10 μm de diamètre), et sur des composants de surface relativement grande (4x2cm2), sans volume mort au- dessus des colonnes, et en minimisant la surface de PDMS en regard des fluides (problèmes d'adsorption des protéines sur le PDMS). 5 μm side and hexagonal columns 10 μm in diameter), and relatively large surface components (4x2cm 2 ), with no dead volume above the columns, and minimizing the surface area of PDMS against fluids adsorption of proteins on PDMS).

Claims

Revendications claims
1. Procédé de réalisation d'un composant, comportant un substrat micro- structuré (3) et un élément complémentaire (7, 10) assemblés au moyen d'un joint d'assemblage (4), procédé caractérisé en ce qu'il comporte la fabrication du joint d'assemblage par :1. Method for producing a component, comprising a micro-structured substrate (3) and a complementary element (7, 10) assembled by means of an assembly joint (4), characterized in that it comprises the manufacture of the joint by:
- une première étape, de dépôt sur un substrat de transfert (1 , 11) d'une couche mince d'un polymère (2), le substrat de transfert et la couche mince de polymère ayant une affinité chimique prédéterminée,a first step of depositing on a transfer substrate (1, 11) a thin layer of a polymer (2), the transfer substrate and the thin layer of polymer having a predetermined chemical affinity,
- une seconde étape, de mise en contact du substrat micro-structuré (3) et de la couche mince de polymère (2), le substrat micro-structuré et la couche mince de polymère ayant une affinité chimique plus forte que l'affinité chimique entre le substrat de transfert (1 , 11) et la couche mince de polymère, - une troisième étape, de retrait du substrat de transfert (1 , 11), de manière à ce que le joint d'assemblage (4) soit formé par les zones de la couche mince de polymère (2) venant en contact avec le substrat micro-structuré (3) au cours de la seconde étape.a second step of contacting the micro-structured substrate (3) and the thin polymer layer (2), the micro-structured substrate and the thin polymer layer having a higher chemical affinity than the chemical affinity between the transfer substrate (1, 11) and the thin polymer layer, - a third step of removing the transfer substrate (1, 11), so that the joining joint (4) is formed by the areas of the thin polymer layer (2) coming into contact with the micro-structured substrate (3) during the second step.
2. Procédé de réalisation selon la revendication 1 , caractérisé en ce qu'il comporte une étape de réticulation de la couche mince de polymère (2) entre les première et seconde étapes.2. Production method according to claim 1, characterized in that it comprises a step of crosslinking the thin polymer layer (2) between the first and second steps.
3. Procédé de réalisation selon l'une des revendications 1 et 2, caractérisé en ce qu'il comporte une étape d'activation chimique de la couche mince de polymère (2) déposée sur le substrat de transfert (1 , 11) entre les première et seconde étapes. 3. Production method according to one of claims 1 and 2, characterized in that it comprises a step of chemical activation of the thin polymer layer (2) deposited on the transfer substrate (1, 11) between the first and second steps.
4. Procédé de réalisation selon l'une quelconque des revendications 1 à 3, caractérisé en ce qu'il comporte une étape d'activation chimique du substrat micro-structuré (3) entre les première et seconde étapes.4. Production method according to any one of claims 1 to 3, characterized in that it comprises a step of chemical activation of the micro-structured substrate (3) between the first and second steps.
5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce que le substrat de transfert (1 , 11 ) est flexible et le retrait du substrat de transfert est effectué en le tirant par une extrémité.5. Method according to any one of claims 1 to 4, characterized in that the transfer substrate (1, 11) is flexible and the removal of the transfer substrate is carried out by pulling at one end.
6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que le substrat de transfert (1 , 11 ) est en Polydiméthylsiloxane (PDMS).6. Method according to any one of claims 1 to 5, characterized in that the transfer substrate (1, 11) is polydimethylsiloxane (PDMS).
7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce qu'il comporte, après la troisième étape, une étape d'activation chimique du joint d'assemblage (4) disposé sur le substrat micro-structuré (3).7. Method according to any one of claims 1 to 6, characterized in that it comprises, after the third step, a step of chemical activation of the joint (4) disposed on the micro-structured substrate (3). ).
8. Procédé selon l'une quelconque des revendications 1 à 7, caractérisé en ce qu'il comporte une étape d'activation chimique de l'élément complémentaire (7, 10).8. Method according to any one of claims 1 to 7, characterized in that it comprises a chemical activation step of the complementary element (7, 10).
9. Procédé selon l'une quelconque des revendications 1 à 8, caractérisé en ce que le substrat micro-structuré (3) comporte au moins une zone d'appui (8) servant d'appui au substrat de transfert (1 , 11) au cours de la seconde étape.9. Method according to any one of claims 1 to 8, characterized in that the micro-structured substrate (3) comprises at least one bearing zone (8) serving to support the transfer substrate (1, 11) during the second stage.
10. Procédé selon l'une des revendications 1 à 9, caractérisé en ce que le substrat de transfert (1) est plan.10. Method according to one of claims 1 to 9, characterized in that the transfer substrate (1) is plane.
11. Procédé selon l'une des revendications 1 à 9, caractérisé en ce que le substrat de transfert est micro-structuré (11). 11. Method according to one of claims 1 to 9, characterized in that the transfer substrate is micro-structured (11).
12. Procédé selon l'une des revendications 1 à 11 , caractérisé en ce que le matériau polymère de la couche mince de polymère (2) est choisi parmi les résines thermo-dures, les élastomères et les thermoplastiques élastomères.12. Method according to one of claims 1 to 11, characterized in that the polymer material of the thin polymer layer (2) is selected from thermo-hard resins, elastomers and elastomeric thermoplastics.
13. Procédé selon la revendication 12, caractérisé en ce que le matériau polymère de la couche mince de polymère (2) est du Polydiméthylsiloxane (PDMS).13. The method of claim 12, characterized in that the polymer material of the thin layer of polymer (2) is polydimethylsiloxane (PDMS).
14.Composant, réalisé par le procédé selon l'une quelconque des revendications 1 à 13, caractérisé en ce que l'élément complémentaire est un capot (7).14.Component, produced by the method according to any one of claims 1 to 13, characterized in that the complementary element is a cover (7).
15.Composant, réalisé par le procédé selon l'une quelconque des revendications 1 à 13, caractérisé en ce que l'élément complémentaire (7) est un autre substrat micro-structuré.15.Component, produced by the method according to any one of claims 1 to 13, characterized in that the complementary element (7) is another micro-structured substrate.
16.Composant, réalisé par le procédé selon l'une quelconque des revendications 1 à 13, caractérisé en ce que l'élément complémentaire est un capillaire (10) ou une matrice de capillaires solidaires entre eux. 16.Composer produced by the method according to any one of claims 1 to 13, characterized in that the complementary element is a capillary (10) or a matrix of capillaries integral with each other.
EP03767900A 2002-11-08 2003-11-04 Method for production of a component with a micro-joint and component produced by said method Withdrawn EP1558518A2 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
FR0213998 2002-11-08
FR0213998A FR2846906B1 (en) 2002-11-08 2002-11-08 METHOD FOR PRODUCING A COMPONENT COMPRISING A MICRO-SEAL AND COMPONENT PRODUCED THEREBY
PCT/FR2003/003288 WO2004043849A2 (en) 2002-11-08 2003-11-04 Method for production of a component with a micro-joint and component produced by said method

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WO (1) WO2004043849A2 (en)

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0711430B2 (en) * 1985-09-13 1995-02-08 キヤノン電子株式会社 Encoder device
US7521292B2 (en) 2004-06-04 2009-04-21 The Board Of Trustees Of The University Of Illinois Stretchable form of single crystal silicon for high performance electronics on rubber substrates
US7622367B1 (en) 2004-06-04 2009-11-24 The Board Of Trustees Of The University Of Illinois Methods and devices for fabricating and assembling printable semiconductor elements
EP1652579A1 (en) * 2004-10-28 2006-05-03 CSEM Centre Suisse d'Electronique et de Microtechnique SA Recherche et Développement Fluidic systems comprising a capillary channel and process for their manufacture
WO2006061025A2 (en) * 2004-12-09 2006-06-15 Inverness Medical Switzerland Gmbh A method of producing a micro fluidic device and a micro fluidic device
US7473616B2 (en) * 2004-12-23 2009-01-06 Miradia, Inc. Method and system for wafer bonding of structured substrates for electro-mechanical devices
WO2006074665A2 (en) * 2005-01-12 2006-07-20 Inverness Medical Switzerland Gmbh A method of producing a microfluidic device and microfluidic devices
TWI306490B (en) * 2006-02-27 2009-02-21 Nat Applied Res Laboratoires Apparatus for driving microfluid driving the method thereof
WO2008083687A1 (en) 2007-01-10 2008-07-17 Scandinavian Micro Biodevices Aps A microfluidic device and a microfluidic system and a method of performing a test
JP5229215B2 (en) * 2007-03-02 2013-07-03 コニカミノルタアドバンストレイヤー株式会社 Microchip manufacturing method
US9195004B2 (en) * 2008-01-04 2015-11-24 Massachusetts Institute Of Technology Method and apparatus for forming structures of polymer nanobeads
WO2010017441A2 (en) * 2008-08-07 2010-02-11 Massachusetts Institute Of Technology Method and apparatus for simultaneous lateral and vertical patterning of molecular organic films
WO2010028390A2 (en) * 2008-09-08 2010-03-11 Massachusetts Institute Of Technology Method and apparatus for super radiant laser action in half wavelength thick organic semiconductor microcavities
US8739390B2 (en) * 2008-12-16 2014-06-03 Massachusetts Institute Of Technology Method for microcontact printing of MEMS
US8963262B2 (en) 2009-08-07 2015-02-24 Massachusettes Institute Of Technology Method and apparatus for forming MEMS device
KR101942967B1 (en) * 2012-12-12 2019-01-28 삼성전자주식회사 Bonded substrate structure using siloxane-based monomer and method of fabricating the same
CN103542956A (en) * 2013-09-29 2014-01-29 柳州市宏亿科技有限公司 Zigbee temperature sensor manufacturing method
US9105800B2 (en) 2013-12-09 2015-08-11 Raytheon Company Method of forming deposited patterns on a surface
US10986435B2 (en) 2017-04-18 2021-04-20 Massachusetts Institute Of Technology Electrostatic acoustic transducer utilized in a hearing aid or audio processing system
ES2775649B2 (en) * 2018-07-24 2020-12-01 Consejo Superior Investigacion PROCEDURE FOR THE TRANSFER OF MICRO- AND / OR NANO- STRUCTURED GROUNDS TO ARBITRARY SURFACES
FR3103805A1 (en) * 2019-12-02 2021-06-04 Commissariat A L'energie Atomique Et Aux Energies Alternatives LOCAL DEPOSIT PROCESS OF A MATERIAL ON AN ELEMENT
CN111250185B (en) * 2020-02-21 2022-11-04 京东方科技集团股份有限公司 Preparation method and preparation device of micro-fluidic chip
CN114308161B (en) * 2021-12-31 2023-07-25 上海中航光电子有限公司 Microfluidic chip and manufacturing method thereof

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4456570A (en) * 1982-07-26 1984-06-26 Ethyl Corporation Treatment of perforated film
US5147397A (en) * 1990-07-03 1992-09-15 Allergan, Inc. Intraocular lens and method for making same
SE501380C2 (en) * 1993-06-15 1995-01-30 Pharmacia Lkb Biotech Ways to manufacture microchannel / microcavity structures
JP3612945B2 (en) * 1997-07-08 2005-01-26 富士ゼロックス株式会社 Manufacturing method of microstructure
JP2002212529A (en) * 2000-06-28 2002-07-31 Sumitomo Chem Co Ltd Adhesive sheet
JP2002144300A (en) * 2000-07-27 2002-05-21 Toshiba Tec Corp Pipe joint, method of manufacturing the same, and fluid device using pipe joint
WO2002036485A1 (en) * 2000-11-02 2002-05-10 Biacore Ab Valve integrally associated with microfluidic liquid transport assembly
DE10056908A1 (en) * 2000-11-16 2002-05-23 Merck Patent Gmbh Method for joining plastic components involves application of an adhesive to a carrier foil, preliminary hardening of this adhesive, and transfer of the adhesive to at least one of the components
EP1467949A1 (en) * 2001-12-31 2004-10-20 Gyros AB A microfluidic device and its manufacture

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2004043849A2 *

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US20060048885A1 (en) 2006-03-09
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JP2006505418A (en) 2006-02-16
FR2846906A1 (en) 2004-05-14

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