EP4182262A1 - Production de surfaces structurées - Google Patents

Production de surfaces structurées

Info

Publication number
EP4182262A1
EP4182262A1 EP21739255.4A EP21739255A EP4182262A1 EP 4182262 A1 EP4182262 A1 EP 4182262A1 EP 21739255 A EP21739255 A EP 21739255A EP 4182262 A1 EP4182262 A1 EP 4182262A1
Authority
EP
European Patent Office
Prior art keywords
proposed
parameters
irradiation
surface structure
pattern
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.)
Pending
Application number
EP21739255.4A
Other languages
German (de)
English (en)
Inventor
Jens ELGETI
Gerhard GOMPPER
Stephan FÖRSTER
Lucas DE QUEIROZ DA COSTA CAMPOS
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.)
Forschungszentrum Juelich GmbH
Original Assignee
Forschungszentrum Juelich GmbH
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 Forschungszentrum Juelich GmbH filed Critical Forschungszentrum Juelich GmbH
Publication of EP4182262A1 publication Critical patent/EP4182262A1/fr
Pending 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
    • B29C53/00—Shaping by bending, folding, twisting, straightening or flattening; Apparatus therefor
    • B29C53/02—Bending or folding
    • B29C53/04—Bending or folding of plates or sheets
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/0037—Production of three-dimensional images
    • 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
    • B29C55/00—Shaping by stretching, e.g. drawing through a die; Apparatus therefor
    • B29C55/02—Shaping by stretching, e.g. drawing through a die; Apparatus therefor of plates or sheets
    • 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
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/14—Surface shaping of articles, e.g. embossing; Apparatus therefor by plasma treatment
    • 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
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/16—Surface shaping of articles, e.g. embossing; Apparatus therefor by wave energy or particle radiation, e.g. infrared heating
    • 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
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/18—Surface shaping of articles, e.g. embossing; Apparatus therefor by liberation of internal stresses, e.g. plastic memory
    • 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
    • B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
    • B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
    • B81C1/00492—Processes for surface micromachining not provided for in groups B81C1/0046 - B81C1/00484
    • 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
    • C08J7/12—Chemical modification
    • C08J7/123—Treatment by wave energy or particle radiation
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/16—Coating processes; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes

Definitions

  • the present invention relates to the targeted production of surface structures, in particular complex surface structures, and in particular down to the micro and nanometer range and also three-dimensionally structured surfaces starting from an elastic material by stretching, selective treatment of different surface areas and relaxation.
  • Surface technologies play an important role in almost all manufacturing processes, from the metalworking industry to the semiconductor industry to biomedicine, from mechanical engineering, plant and tool construction to optics, microelectronics, medical technology, the automotive industry and plastics processing to building technology and architecture.
  • the aim of surface technologies is to change surface properties such as corrosion resistance, wettability, biocompatibility, flow properties, etc., regardless of the actual material of a component. In most cases, new surface properties lead to better product quality or enable components and products to be used or used in the first place.
  • Such functional surfaces are created, for example, by microstructuring.
  • a wide range of manufacturing processes is available to create structured surfaces, such as simple folding techniques, X-ray lithography, 3D printing, laser ablation, various coating processes and classic lithographic techniques.
  • X-ray lithography allows the production of very fine structures, but it is very expensive and only possible on a relatively small scale. In addition, structures with overhangs are very expensive. 3D printing only allows relatively coarse structures and is not particularly fast in terms of throughput. Similar fine surface structures can be created using laser ablation. However, this method is relatively expensive and cannot produce structures with overhangs.
  • a method for ultra-precise surface structuring that has so far been relatively little used is based on the regular formation of folds when a prestressed elastic material (usually polymers) with a subsequently applied stiffer surface layer contracts. Since the surface layer can contract less than the substrate during relaxation, a very regular fold pattern of microscopically small folds is formed.
  • the object of the present invention is to provide options for structuring surfaces, in particular in the micrometer range.
  • An essential aspect of the present invention is to spatially vary the nature of a surface layer applied to a preferably elastic substrate, such as its thickness or elasticity, in a targeted manner. By controlling the inhomogeneity of these parameters, a very wide range of complex structures can be generated in one step.
  • the resulting textured material can be used directly, but it can also be used as a "mold” for various other materials, e.g. epoxy resins, thermoplastics or concrete, making the process available for a wide range of materials.
  • the subject matter of the present invention is therefore a method for producing three-dimensionally structured surfaces, in which an elastic material is provided in a first step. This material is then stretched by a predetermined value and the stretched state is initially retained. Thereafter, a two-dimensional pattern is then applied or transferred to the surface of the elastic material in the stretched state or introduced into the surface of the elastic material in the stretched state. After the stretch is then removed, the elastic material relaxes and, due to the pattern transferred or introduced to the surface, unfolds in a specific pattern.
  • This three-dimensionally structured surface produced in this way can in itself represent the desired product. However, it is just as possible to mold this surface, i.e. to apply other materials to the structured surface and then to carry out an inverse molding, i.e. to obtain a three-dimensionally structured surface in the second material, which represents a direct inversion of the surface of the elastic material.
  • all elastic materials can in principle be used for this method, which can be structured in any form, or on which a two-dimensional pattern can be applied in any form, such that the surface quality/elasticity of the pattern structure differs from that of the non-patterned surface areas.
  • all elastic materials can be used within the scope of the present invention.
  • materials can be used that have a tensile modulus of 10 Pa, such as very soft elastomers, to those that have tensile moduli of up to 1000 GPa, such as very hard metal and glass.
  • tensile modulus of 10 Pa such as very soft elastomers
  • tensile moduli of up to 1000 GPa such as very hard metal and glass.
  • elastic materials whose tensile moduli are in the range from about 100 kPa to 100 kPa; exemplary of such materials would be polydimethylsiloxanes (PDMS).
  • PDMS polydimethylsiloxanes
  • examples of elastic materials that can be used in the context of the present invention are rubber or elastomers, in particular elastomers based on silicone, such as polydimethylsiloxane (PDMS), polyurethane, polybutadiene, polyisoprene and copolymers such as SBR, NBR, EPM, EVA .
  • PDMS polydimethylsiloxane
  • polyurethane polyurethane
  • polybutadiene polyisoprene
  • copolymers such as SBR, NBR, EPM, EVA .
  • the two-dimensional pattern can be transferred to or introduced into the surface of the elastic material in the stretched state in principle in all conceivable ways.
  • an elastic material stretch it and then, for example by means of a laser, burn or melt structures into the surface, i.e. to remove the surface at precisely desired and defined points (in contrast to irradiation with laser light in the sense of exposure).
  • This procedure can be carried out in a similar way to direct laser writing, with the focus of the laser light being bundled onto certain desired areas in such a way that the elastic material can be liquefied or vaporized at this point.
  • a three-dimensional surface structure is then formed in accordance with the baked or removed pattern.
  • the introduction of the two-dimensional pattern into the surface of the elastic material in the stretched state is carried out by first covering or protecting specific surface areas of the material by covering or by applying a protective substance and then oxygen plasma on the surface is left to act.
  • the oxygen plasma would then reach the surface areas that are not covered or not protected by a protective substance and could change the surface there by chemical reactions.
  • the oxygen plasma supply is stopped, and then the cover or the protective substance (protective substance) is removed from the surface. If the stretching is then removed, the material relaxes and forms a defined three-dimensionally structured surface, depending on the surface areas changed by the oxygen plasma in relation to the unchanged surface areas.
  • the protective substance can be a protective lacquer, for example, which is applied to the stretched surface, for example, by means of pad printing or other printing methods, such as, for example, using an inkjet printer.
  • the protective lacquer can be removed, for example, by rinsing with suitable solvents.
  • suitable solvents Corresponding paints and solvents are known to those skilled in the art.
  • a reactive gas is used in place of oxygen plasma. The procedure otherwise remains the same. Examples of reactive gases are ozone, chlorine or hydrogen chloride.
  • a protective substance by means of oxygen plasma or a reactive gas, preferably selected from the group consisting of ozone, chlorine and hydrogen chloride, for a certain period of time,
  • the protected areas, the protective materials, the plasma or reactive gas and the duration of exposure and/or the degree of stretching of the elastic material are determined depending on the elastic material used.
  • the two-dimensional pattern is introduced onto the surface of the elastic material in the stretched state by irradiation using electromagnetic radiation.
  • an irradiation mask is first arranged between the radiation source and the elastic material.
  • This radiation mask can be placed anywhere on the radiation path between the radiation source and the surface of the material, but can also be placed in direct contact with the surface. Depending on the exact pattern desired, a person skilled in the art can select the most suitable distance between the surface, the radiation source and the radiation mask. In this context, the specialist will then - depending on the radiation used - take into account to what extent the radiation mask leads to diffraction effects or not and to what extent these are desired.
  • irradiation is then carried out by means of electromagnetic radiation with a radiation duration and radiation intensity required for the desired surface structure.
  • the irradiation mask is then removed and the stretched state is canceled.
  • folding to form the desired three-dimensionally structured surface takes place as a function of the irradiation pattern.
  • the radiation mask can either be a rigid mask that can be used multiple times, for example a metal or plastic template, or a protective lacquer that is applied to the stretched surface, for example by means of pad printing or other printing processes, such as an inkjet printer.
  • removing the protective mask would then mean removing the protective lacquer, for example by rinsing with suitable solvents.
  • suitable solvents for example by rinsing with suitable solvents.
  • this electromagnetic radiation will always have a certain penetration depth into the material, so that the surface change takes place down to a certain depth of the surface (for example crosslinking stimulated by UV rays).
  • this also applies to painting or printing the surface with glue, for example.
  • this two-dimensional structure designated in this way or the two-dimensional surface pattern has a surface structure that is orders of magnitude smaller than the three-dimensional surface structure subsequently obtained by folding.
  • a pattern can also be produced by targeted, precise application of chemical compounds that react with the surface molecules of the substrate to the surface.
  • the application must take place with very fine nozzles so that the fine structuring desired within the scope of the present invention is made possible.
  • the application can be done using printers based on "inkjet technology", i.e. printers are used that have very fine application nozzles, with nozzle openings, the droplets of less than 100 picoliters, preferably less than 50 picoliters, particularly preferably less than 20 Picoliters can be generated.
  • printers instead of the inks, a chemical or chemical mixture can be used in the printer cartridges, which reacts with the molecules on the substrate surface. After this solution has been "printed” onto the substrate surface, the molecules react with each other and the jetted or printed pattern results from the surface molecules transformed by chemical reaction.
  • this can be in the Polymer chemistry in principle take place in a known manner by reacting a substance with a suitable hardening substance or crosslinking substance.
  • the substance to be printed/sprayed on can either be used in its pure form or as a mixture with co-crosslinkers or dissolved in a solvent; this is known to the person skilled in the art and accordingly does not need to be discussed in more detail here.
  • the substrate itself must be sufficiently stable and, above all, elastically stretchable so that after printing, reaction and removal of the stretching it can contract again and form the desired surface structure.
  • PDMS is often offered already premixed with the appropriate crosslinker, a commercially available example of this being Sylgard® 184. Such prefabricated mixtures can be printed on and cured directly using this variant of the present invention.
  • the PDMS or the hardeners are dissolved in suitable solvents; preferred examples of such solvents are methyl isobutyl ketone, toluene, isobutyl acetate and octyl acetate (mainly for PDMS) and acetonitrile (mainly for the crosslinkers).
  • the stretched elastic material is only one layer of a multi-layer workpiece.
  • This multi-layer workpiece can consist of at least two layers at least three or more layers. It is possible that the different layers consist of different materials, or that the different layers consist of the same materials that are arranged one above the other. The latter can be useful, for example, if an anisotropic material is used whose properties have preferred directions. In such a case, this material could be rotated in layers relative to one another, for example arranged rotated by 90°, layers one on top of the other. In embodiments, the multi-layer material can also be obtained after structuring the uppermost layer by applying this layer to the remaining layer(s).
  • the irradiation mask, the duration of the irradiation, the radiation intensity and the precise form of the electromagnetic radiation and/or the degree of stretching of the elastic material are determined as a function of the elastic material used.
  • This determination can be made based on experimental data and appropriately created databases or calculated based on computer simulations.
  • the exact shape and structure of the radiation mask, the duration of the radiation, the radiation intensity and/or the degree of stretching, or analogous to the type and shape of the protective materials, the protected areas and the plasma or reactive gas, are determined accordingly in embodiments of the present invention experimentally, in other embodiments experimentally iteratively, in other embodiments iteratively using machine learning, and in further embodiments using computer simulations. It is also possible to combine these selection processes. For example, part of the parameters such as the shape of the radiation mask may have been determined experimentally and another part, eg the radiation intensity, determined experimentally iteratively, whereas the degree of stretching may come from machine learning or computer simulations. The exact selection and the precise application of these methods result from the specifications for the respective desired project.
  • the experimentally iterative determination can take place as follows:
  • a desired three-dimensional surface structure is specified, which is to be achieved for a defined elastic material.
  • a two-dimensional surface pattern is proposed, which should fold into a structure that is as similar as possible to that of the specification after irradiation through a proposed irradiation mask or treatment with plasma or reactive gas of unprotected surface areas.
  • parameters for the duration of the irradiation, the radiation intensity, or the duration and intensity of the plasma/gas treatment, and/or the degree of stretching are then proposed.
  • the product obtained with this method is compared with the specified surface structure with regard to the three-dimensional surface structure obtained. If the surface structure obtained shows sufficient agreement with the specified structure, the product obtained is dispensed.
  • this output means that the product obtained is suitable as an end product and can easily be used or further processed. If the method is carried out in a closed system, the method can also be stopped for this purpose and the user can be notified, for example by an optical or acoustic signal or by e-mail or in another conventional manner.
  • the suggested structure or the suggested parameters for the irradiation, the shape of the irradiation mask and the suggested pattern as well as the three-dimensional surface structure obtained can then optionally be saved;
  • the type and form of the protective materials, the protected areas and the plasma or reactive gas can be stored analogously.
  • this data is stored in the form of a parameter set that is given an accurate, unambiguous designation and in context can form a corresponding manufacturing database with other such parameter sets.
  • this method described with a view to irradiating the surface can also be applied analogously to the other methods described above for applying a pattern to the surfaces, in particular treatment with oxygen plasma.
  • the iterative determination using machine learning can take place as follows:
  • a desired three-dimensional surface structure is specified, which is to be achieved for a defined elastic material.
  • a two-dimensional surface pattern is proposed, which should fold into a structure that is as similar as possible to that of the specification after irradiation through an irradiation mask that is also proposed, or treatment by means of plasma or reactive gas of unprotected surface areas.
  • a simulation program This is preferably a simulation program based on the finite element method.
  • the data used for the calculation for the specified three-dimensional surface structure, proposed two-dimensional surface pattern, proposed radiation mask, proposed radiation parameters or proposed protected areas of the surface and duration and intensity of the plasma/gas treatment are transferred to the algorithm or the neural network as a learning data set.
  • the result of a three-dimensional surface structure obtained from this calculation is then compared with the specified surface structure. If the calculated three-dimensional surface structure is sufficiently consistent with the specified structure, the result obtained is output. With this result and the associated parameters, a real, physical conversion and production of the desired product can then take place.
  • Said output can take place in the usual way.
  • a display on a monitor as a printout, or as a direct transmission of the data, e.g. as control data, to a connected production unit.
  • a notification can also be sent to the user, for example by an optical or acoustic signal or by e-mail or in some other customary manner.
  • the suggested/calculated structure or the suggested/calculated parameters for the irradiation, the shape of the irradiation mask and the suggested/calculated pattern as well as the one obtained as the result of the calculation three-dimensional surface structure can then optionally be saved;
  • the type and form of the protective materials, the protected areas and the plasma or reactive gas can be stored analogously.
  • this data is stored in the form of a parameter set, which is given a precise, unambiguous designation and can form a corresponding production database in conjunction with other such parameter sets.
  • the steps just described of suggesting a two-dimensional surface pattern, an irradiation mask and parameters for the irradiation, or type and shape the protective materials, the protected areas and the plasma or reactive gas, as well as the calculation as described above and the comparison of the calculated and the specified structures is repeated, with the data of the learning data set being included in the calculation.
  • one or more of the parameters and suggestions mentioned are changed. It is preferred to change only one parameter or suggestion in each case in order to obtain reproducibility and a result that is as meaningful as possible and that can be traced back to a specific parameter or its change.
  • the changes are preferably specified by the program/algorithm. In principle, however, it is also possible to have these specified by the experimenter. The results obtained in this way are optionally saved again as just described.
  • the first start data set for the proposal of surface patterns, radiation masks or Irradiation parameters, or the type and shape of the protective substances, the protected areas and the plasma or reactive gas are either specified by a computer program or caninely entered by the user, for example on the basis of previous experimental results.
  • this method described with a view to irradiation of the surface can also be applied analogously to the other methods described above of applying a pattern to the surfaces, in particular treatment with oxygen plasma.
  • the proposed two-dimensional surface pattern corresponds to at least one, preferably exactly one, defined exposure or irradiation mask.
  • the three-dimensionally structured surfaces resulting from the method of the present invention have hierarchical folds, overhangs, channels, microfluidic channels, in particular with a smooth, rounded cross section, knobs and/or combinations thereof.
  • the resulting three-dimensionally structured surface has smooth, rounded cross-section microfluidic channels.
  • the present invention also relates to workpieces with a three-dimensionally structured surface, the surfaces having hierarchical folds, overhangs and/or microfluidic channels with a smooth, rounded cross section, in particular workpieces that were produced using one of the methods described above.
  • the subject matter of the present invention is also workpieces with a three-dimensionally structured surface structure, which were produced using a method of the present invention.
  • the present invention also includes corresponding workpieces, these workpieces comprising at least two layers and the top layer being formed by a correspondingly three-dimensionally structured surface.
  • the subject matter of the present invention is a method for optimizing three-dimensionally structured surfaces by means of machine learning, the machine learning being carried out according to the specification of a desired three-dimensional target
  • a desired three-dimensional surface structure is specified, which is to be achieved for a defined elastic material.
  • a simulation program This is preferably a simulation program based on the finite element method.
  • the "program for determining the folding of the human brain in the course of embryonic development", optionally with adaptation, can be used.
  • the data used for the calculation for the given three-dimensional surface structure, proposed two-dimensional surface pattern, proposed irradiation mask, proposed irradiation parameters are transferred to the algorithm or the neural network as a learning data set.
  • the result of a three-dimensional surface structure obtained from this calculation is then compared with the specified surface structure. If the calculated three-dimensional surface structure is sufficiently consistent with the specified structure, the result obtained is output. With this result and the associated parameters, a real, physical conversion and production of the desired product can then take place.
  • Said output can take place in the usual way.
  • a display on a monitor as a printout, or as a direct transmission of the data, e.g. as control data, to a connected production unit.
  • a notification can also be sent to the user, for example by an optical or acoustic signal or by e-mail or in some other customary manner.
  • the suggested/calculated structure or the suggested/calculated parameters for the irradiation, the shape of the irradiation mask and the suggested/calculated pattern as well as the three-dimensional surface structure obtained as the result of the calculation can then optionally be saved.
  • this data is stored in the form of a parameter set, which is given a precise, unambiguous designation and can form a corresponding production database in conjunction with other such parameter sets.
  • the steps just described of suggesting a two-dimensional surface pattern, an irradiation mask and parameters for the irradiation and the calculation as described above and the comparison of the calculated and the predetermined structures is repeated, with the data of the learning data set being included in the calculation.
  • one or more of the parameters and suggestions mentioned are changed. It is preferred to change only one parameter or suggestion in each case in order to obtain reproducibility and a result that is as meaningful as possible and that can be traced back to a specific parameter or its change.
  • the changes are preferably specified by the program/algorithm. In principle, however, it is also possible to have these specified by the experimenter.
  • the results obtained in this way are optionally saved again as just described. This repetition of the steps continues until a sufficient correspondence between the specified three-dimensional structure and the calculated three-dimensional structure is achieved.
  • this method described with a view to irradiation of the surface can also be applied analogously to the other methods described above of applying a pattern to the surfaces, in particular treatment with oxygen plasma.
  • the aim is to have a high degree of edge sharpness for the patterns/patterning introduced into the surface.
  • the individual structural elements of which, such as channels, are less than 1 mm in preferred embodiments this means that direct incorporation of such structures into the surface by means of direct irradiation through plasma nozzles, in particular those with nozzle openings of 0.5 cm and more, is not possible, as this would lead to insufficient edge sharpness and inhomogeneous structures; the individual pattern elements would, on the one hand, merge into one another with such a procedure and, on the other hand, would not fold precisely enough due to the insufficiently sharp pattern edges when the tension was removed, so that an exact control of the pattern and thus the resulting fold would no longer be possible.
  • Preferred developments of the present invention are the methods according to the invention for producing structured surfaces with pattern sizes of less than 1 mm, pattern sizes between 100 nm and less than 1 mm being preferred.
  • these variables are the widths of the structures; the length of a respective structure can, of course, be greater.
  • channels are accordingly obtainable, for example, which have a width of 100 nm to less than 1 mm, preferably 100 nm to 0.5 mm, particularly preferably 1 pm to 100 pm or 50 mil to 500 mil or 300 mil to 500 mil, and which may be several cm in length.
  • the depth results from the desired structure and can be, for example, 50 ⁇ m to 0.5 ⁇ m in some preferred embodiments.
  • tolerances are already specified when specifying the target structure, within which the result may deviate from the target structure. For example, for a microchannel with a width of 0.5 gm, a tolerance of +0.001 gm may be acceptable in embodiments. In other embodiments, for a 50 gm wide microchannel, a tolerance of +5 gm may be acceptable.
  • the result obtained is examined by the user and he then decides whether the result is sufficient for the desired application. For example, if the structure is not intended to serve any practical purpose, but only to be aesthetically pleasing, a significant deviation may also be aesthetically pleasing and therefore acceptable.
  • the algorithm used or the user specifies which percentage deviation from the target value (for example the target width of a channel) is sufficient.
  • an elastomer is stretched and then selectively cured (crosslinked, for example, by UV light) in various areas, creating a surface pattern. If the stretching is then reversed, the elastomer contracts again. Due to the fact that there is a surface pattern of hardened and unhardened areas, the elastomer contracts unevenly and folding caused by the structure of the hardened and unhardened areas occurs. Because the areas are selectively hardened or not hardened, it is possible to specifically influence and control the surface structure and the structure of the fold. It is possible to produce defined "folded structures" in this way. Examples of elastomers that can be used are those based on polydimethylsiloxane (PDMS).
  • PDMS polydimethylsiloxane
  • PDMS itself is difficult to cure or crosslink via UV radiation
  • modified PDMS on the market that are chemically modified by the incorporation of vinyl groups, for example, and/or to which other substances are added for crosslinking, such as free-radical generators such as benzophenone or peroxides.
  • Examples of commercially available PDMS(systems) that can be cured or crosslinked via UV radiation are Dow Corning WL-5000 or Sylgard® 184 PDMS Kit.
  • the precise dimensions of the surface structures result from the precise material properties of the elastic material used, the thickness of the material layer, the irradiation parameters (eg radiation intensity, radiation duration) and the irradiated areas or the areas used Radiation masks or the conditions of exposure to oxygen plasma or reactive gas such as exposure time.
  • the irradiation parameters eg radiation intensity, radiation duration
  • the present invention it is possible to irradiate the most elastic materials used with radiation of different energies or wavelengths.
  • the exact selection of the radiation is made in coordination with the material to be irradiated.
  • the person skilled in the art is aware that and how the radiation is to be selected as a function of material properties. For example, there are a wide variety of networking mechanisms that differ in the energies required for activation.
  • the radiation used may range from infrared radiation to ultraviolet radiation.
  • UV radiation is used as the radiation; this can be applied to a large number of crosslinking systems and can then be adapted in individual cases by precisely selecting the wavelength, radiation intensity and duration of radiation.
  • radiation power and intensities can be selected in order not to destroy the material or to achieve a targeted change in the material.
  • flat substrates made of elastic polymers in the uniaxially and biaxially stretched state are provided with a surface layer of specific thickness and crosslinking density by photocrosslinking and plasma treatment.
  • the modulus of elasticity can be set according to the specifications, for example from a simulation, via the crosslinking density. Wrinkling begins when the fabric is relaxed into the unstretched state and can be compared directly with the specifications or the predictions of the simulation.
  • the resulting structuring of the surface layer is an integral part of the surface layer and does not lie on the original surface, as would be the case with printing or pasting.
  • a cover, a protective material, or a mask is used, the recesses of which have a width of less than 1 mm, preferably between 1 ⁇ m and 0.5 mm, particularly preferably 50 ⁇ m to 500 ⁇ m or 300 ⁇ m to 500 ⁇ m pm, exhibit. This allows preferred structures to be created.
  • a detailed characterization of the surface structure can be carried out, for example, using profilometry (devices for this are available, for example, under the brand name Dektak®) and/or microscopic methods.
  • profilometry devices for this are available, for example, under the brand name Dektak®
  • microscopic methods With the help of scanning electron microscopy (SEM) and atomic force microscopy (AFM), surface structures, surface profiles and mechanical properties can be determined in detail and compared with the specifications or simulations. These methods can provide necessary structural information on length scales from nano- to micrometers, complemented if desired by optical microscopy, which can provide structural information on scales down to millimeters.
  • SEM scanning electron microscopy
  • AFM atomic force microscopy
  • surface structures, surface profiles and mechanical properties can be determined in detail and compared with the specifications or simulations.
  • These methods can provide necessary structural information on length scales from nano- to micrometers, complemented if desired by optical microscopy, which can provide structural information on scale
  • silicone that has been surface-structured by wrinkling can serve as a base for transferring the surface structure to polyurethane, epoxy resin or concrete. The structure is then transferred - inverted - to the hardening material, from the surface of which the silicone can be easily removed.
  • Microfluidic channel structures can, for example, also be integrated and used in a glass/elastomer sandwich structure in microfluidic chips.
  • microstructured surfaces can be produced with the aid of the present invention, such as self-cleaning surfaces or microfluidic channel systems.
  • Predicting the fold pattern is quite simple for the homogeneous layers previously used in the prior art, ie those that were stretched and relaxed as a whole without applying or introducing a pattern.
  • computer simulations are used in preferred embodiments, with which the structures formed can be predicted in silico—and thus in a versatile and automated manner.
  • this method of the present invention is associated with an automatic sharpening of the structure, the magnitude of which can be precisely determined: the resulting, folded 3D structure is usually around one magnitude finer than the previously applied layer inhomogeneity.
  • the method of the present invention has two other important advantages and unique selling points: It allows the relatively simple production of hierarchically structured surfaces - ie with small structures on larger structures on even larger structures, etc. - both uniaxially and biaxially.
  • the simulation software used within the framework of preferred embodiments of the present invention is based on extensive preliminary work in the Human Brain Project on the folding of the human brain in the course of embryonic development.
  • the software is used in one variant in such a way that it calculates the corresponding target structure from a surface pattern.
  • the software is used in another variant in such a way that it calculates the necessary surface pattern from a desired target structure. In this way, the present invention is of particular interest to the user as it enables the practical design of desired structures.
  • the present invention therefore relates, inter alia, to a manufacturing method with simulation software for ultra-precise surface structuring and thus for intelligent surface design.
  • a "finite element simulation” is used to calculate which surface pattern results in which fold.
  • a given target structure is used to predict which surface pattern results in fold results that correspond to the target structure. Since direct inversion is difficult, it is preferred a neural network is used: In the simulations, the parameters of the folding are systematically examined and it is determined which distribution patterns (thickness and elasticity of the surface layer) result in which structures.
  • these pattern-structure data are learned in reverse in a neural network, in order to then use the network to determine suitable surface patterns. Thanks to the simulations, the network can test itself and continue to improve: the determined pattern is translated back into a 3D structure by means of the simulations, and thus serves as a new learning data set. This creates an in-silico cycle that continuously improves the predictions and expands the realizable structural space.
  • a hyperelastic (“neo-Hookean”) material with a Poisson's ratio of 0.45, where the elastic modulus is irrelevant.
  • the substrate can be crosslinked in a controlled manner, for example using UV illumination or oxygen plasma (see above).
  • the present invention is applicable to many applications where tailored surface structures are required.
  • the market potential is correspondingly large.
  • microfluidic components for use in medical diagnosis often fail because of the costs, since the chips have to be manufactured using expensive, multi-stage lithography processes.
  • the present invention allows channel structures to be produced quickly and inexpensively in a single step.
  • the present invention can also be used to create surfaces that are particularly non-slip or have a pleasant feel, for example for mobile phones or dashboards of luxury vehicles. By creating surface structures similar to the lotus leaf, self-cleaning surfaces can also be created in a simple manner.
  • the modification of mechanical properties such as adhesion (e.g. gecko effect) as well as optical properties such as absorption and reflection is also possible through suitable structuring and material selection.
  • Structure sizes of >100 nm can be achieved with X-ray lithography at a throughput of square centimeters per hour.
  • Organic photoresists and acrylates are suitable as materials. The process can be used in microtechnology and is very expensive.
  • Structure sizes of >50 pm can be achieved with 3D printing at a throughput of square centimeters per hour.
  • materials are hydrogels, cells and resins. The method can be used in medicine and microfluidics and is expensive.
  • structure sizes of >100 nm can be achieved at a throughput of square millimeters per minute.
  • Metals are suitable as materials. The process can be used in electronics and medical technology and is expensive.
  • Feature sizes of >100 nm can be achieved with the method of the present invention, in some cases at a throughput of up to square meters per second.
  • Elastic materials such as silicone (direct) are suitable as materials, but various other materials are also suitable indirectly via impressions. The process can be used anywhere where appropriate structures are required on surfaces and is inexpensive.
  • the surface structuring according to the present invention can be scaled well and can in principle be carried out quickly and over a large area in continuous roll-to-roll processes, which allow throughputs of up to square meters per second, which is a great advantage from the economic point of view.
  • FIG. 1 illustrates the manufacture of a workpiece using the method according to the invention.
  • the photocrosslinking of polymers and/or crosslinking via (oxygen) plasma treatment allows a controlled and local change in surface hardness.
  • 1 shows how an initially stretched (not shown here) material 1a, 1b, for example a vinyl group-terminated polydimethylsiloxane (Sylgard® 184 PDMS kit) is specifically exposed or cured in various areas using a mask 2 networked, will.
  • This is shown in FIG. 1 by means of lightning symbols 5, which are intended to illustrate the UV radiation (or oxygen plasma or the like) (in the case of oxygen plasma, the mask 2 must lie directly on the surface of the material, otherwise the hardening will be the same everywhere).
  • FIG. 1 illustrates the manufacture of a workpiece using the method according to the invention.
  • the photocrosslinking of polymers and/or crosslinking via (oxygen) plasma treatment allows a controlled and local change in surface hardness.
  • 1 shows how an initially stretched
  • FIG. 1 also illustrates the influence of the distance between the mask and the material surface; because directly under the parts of the mask 2 the material in the upper part of Figure 1 is also shown as hardened, but not to the same depth as in the areas not shielded by mask parts. This is because the mask cannot completely shield the areas below it from UV radiation at a greater distance.
  • the structure of the mask 2 illustrated here by bars of different widths, reduces the influence of the UV radiation (or the oxygen plasma, etc.) on certain areas of the surface and consequently creates a hardening pattern/crosslinking pattern in the material.
  • the degree of curing/crosslinking can be controlled by the duration and intensity of the radiation. Wrinkling begins upon relaxation to the unstretched state (not shown here.)
  • FIG. 2 illustrates in section a) a stretched polymer substrate with an unhardened zone 1a and a hardened and newly crosslinked, and therefore also more rigid, surface layer 1b (hatched).
  • the hardened layer lb is somewhat thinner in the central area.
  • Section d) illustrates how the structure can be transferred to other materials and inverted (here into sharp points) by molding with another material 3 (shown as a checkered pattern).
  • FIG. 3 shows an example of the structure of a channel cross that occurs when a cross-shaped weak point, i.e. a cross-shaped unexposed or less exposed area is obtained in the stretched state. Upon relaxation, this folds into a cross-shaped channel structure.
  • FIG. 3a shows a top view of the resulting cross-shaped channel structure, in which the various lines represent contour lines, starting from the deepest point in the middle of the figure.
  • FIG. 3b shows a lateral section through the structure obtained just below the top of the 3.3 ⁇ m contour line of FIG. 3a.
  • the surface forms a channel with the walls descending towards the center.
  • the areas shown in bold illustrate the hardened area, i.e. the material did not flatten in the middle.
  • FIG. 3c shows a three-dimensional representation of the cross-shaped channel structure shown in FIG. 3a, in which the deformations during relaxation are illustrated by the line grid.
  • FIG. 4 shows an example structure with knobs. Localized weak points result in a regular pattern of nubs, with the protuberances resulting from the weak points determined during irradiation (or plasma treatment).
  • FIG. 4a shows a plan view of the resulting nub structure, in which the various lines represent contour lines, starting from the lowest point in the middle of the figure.
  • FIG. 4b shows a lateral section through the structure obtained at the level of the middle of FIG. 4a. Here you can see that there is an unhardened area in the center. Two nubs are indicated towards the edges of FIG. 4 (partially shown). The areas shown in bold illustrate the hardened area, ie no hardening of the material took place in the middle.
  • FIG. 4c shows a three-dimensional representation of that shown in FIG. 4a Nub structure, in which the deformations during relaxation are illustrated by the line lattice.
  • FIG. 5 illustrates, in the form of a flow chart, a sequence for a machine learning design as can be used in the present invention.
  • a desired 3D structure is specified by the application or the user. It is illustrated how a neural network then proposes a surface pattern that should fold into a structure that is as similar as possible. A simulation is then used to calculate how the pattern should fold for a given exposure. The result is transferred to the neural network as a learning data set and, if necessary (if this result does not sufficiently match the 3D specification), a new suggestion is generated. This creates an in-silico cycle (ISC) in which new learning data sets are constantly generated for the neural network. In this way, the learning data set of the neural network is expanded each time, and the development of 3D structures is improved. The result pattern can then be checked or verified in the laboratory. The parameters of the simulation can be improved from deviations between experiment and simulation.
  • ISC in-silico cycle
  • UV radiation or oxygen plasma etc.
  • Example 1 Fabrication of a channel structure
  • a PDMS (Sylgard® 184) substrate block with an edge length of 4 ⁇ 4 cm and a thickness of 3 mm was stretched to 4.92 cm ⁇ 4.92 cm.
  • a shadow mask was placed thereon, with square holes of 0.4 mm x 0.4 mm.
  • the web width was 0.1 mm. Thereafter, the surface was exposed to an oxygen plasma (100 W; 0.2 bar) for a period of 10 minutes.
  • a workpiece was thereby obtained which consisted of a substrate block with a partially hardened but still stretched layer arranged on its uppermost surface.
  • the stretching was released and upon relaxation to the unstretched state, the PDMS layer folded into a regular, cross-shaped channel structure while shrinking to the original size of 4 ⁇ 4 cm.
  • the workpiece obtained in this way could be glued to a glass block.
  • Example 2 Analogously to Example 1, a polydimethylsiloxane layer was stretched using an isotropic stretcher. In contrast to example 1, however, the stretching was made to 5.2 cm and a round-hole mask with a hole diameter of 1 mm and a hole spacing of 5 mm was used. This hardened the surface in the non-shadowed area. Wrinkling started when the fabric was relaxed in the unstretched state and a regular nub pattern formed.
  • the knob pattern obtained in this way was transferred inversely by molding. To do this, the structure was filled with an epoxy resin and the epoxy resin was allowed to harden. The epoxy resin was then lifted off the "knob surface".

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Abstract

L'invention concerne des surfaces structurées tridimensionnelles obtenues à base d'un matériau élastique par étirement, traitement sélectif de diverses zones de surface et relaxation.
EP21739255.4A 2020-07-14 2021-06-11 Production de surfaces structurées Pending EP4182262A1 (fr)

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DE102020118555.3A DE102020118555A1 (de) 2020-07-14 2020-07-14 Herstellung strukturierter oberflächen
PCT/EP2021/065763 WO2022012825A1 (fr) 2020-07-14 2021-06-11 Production de surfaces structurées

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DE457484C (de) 1928-03-13 Us Imp House Emanuel Van Dam Druckvorrichtung zum Bedrucken von Gummiblasen
US7351346B2 (en) 2004-11-30 2008-04-01 Agoura Technologies, Inc. Non-photolithographic method for forming a wire grid polarizer for optical and infrared wavelengths
WO2006128189A2 (fr) * 2005-05-27 2006-11-30 The Regents Of The University Of California Retrecissements successifs d'elastomeres, un protocole de miniaturisation simple pour produire des microstructures et des nanostructures
WO2008121784A1 (fr) 2007-03-30 2008-10-09 The Trustees Of The University Of Pennsylvania Adhésifs à adhérence mécanique adaptable
US20140363610A1 (en) 2009-10-14 2014-12-11 Daniel Elliot Sameoto Compression, extrusion and injection molding of interlocking dry adhesive microstructures with flexible mold technology
EP2333749B1 (fr) 2009-12-10 2013-10-16 Universität Bayreuth Empreinte artificielle
US8792169B2 (en) 2011-01-24 2014-07-29 Arizona Board Of Regents On Behalf Of Arizona State University Optical diffraction gratings and methods for manufacturing same
WO2014011222A1 (fr) 2012-07-13 2014-01-16 Massachusetts Institute Of Technology Couches minces avec micro-topologies préparées par plissement séquentiel
US20170003594A1 (en) * 2014-03-17 2017-01-05 Northeastern University Elastomer-Assisted Manufacturing
US10472276B2 (en) 2014-12-04 2019-11-12 Electronics And Telecommunications Research Institute Composition for forming film having wrinkle structure and method of forming the film
DE102017218363A1 (de) 2017-10-13 2019-04-18 Leibniz-Institut Für Polymerforschung Dresden E.V. Oberflächenstrukturierte polymerkörper und verfahren zu ihrer herstellung

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JP2023535343A (ja) 2023-08-17

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