EP0934553A1 - Procede permettant de preparer la production de couches metalliques structurees a l'aide de proteines - Google Patents

Procede permettant de preparer la production de couches metalliques structurees a l'aide de proteines

Info

Publication number
EP0934553A1
EP0934553A1 EP97945795A EP97945795A EP0934553A1 EP 0934553 A1 EP0934553 A1 EP 0934553A1 EP 97945795 A EP97945795 A EP 97945795A EP 97945795 A EP97945795 A EP 97945795A EP 0934553 A1 EP0934553 A1 EP 0934553A1
Authority
EP
European Patent Office
Prior art keywords
metal
layer
proteins
protein
substrate
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Withdrawn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
EP97945795A
Other languages
German (de)
English (en)
Inventor
Stefan Fiedler
Dieter Oesterhelt
Heinrich Meyer
Wolfgang Scheel
Herbert Reichl
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.)
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Atotech Deutschland GmbH and Co KG
Original Assignee
Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV filed Critical Fraunhofer Gesellschaft zur Forderung der Angewandten Forschung eV
Publication of EP0934553A1 publication Critical patent/EP0934553A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C5/00—Photographic processes or agents therefor; Regeneration of such processing agents
    • G03C5/58—Processes for obtaining metallic images by vapour deposition or physical development
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00—Photosensitive materials
    • G03C1/72—Photosensitive compositions not covered by the groups G03C1/005 - G03C1/705
    • G03C1/73—Photosensitive compositions not covered by the groups G03C1/005 - G03C1/705 containing organic compounds
    • G03C1/731—Biological compounds

Definitions

  • the invention relates to the production of thin metallic layers and structures on substrate carriers with a planar or three-dimensional structure, such as are required, for example, for imaging lettering or drawings.
  • the process avoids stamp printing techniques.
  • Known methods and processes for producing such metallic structures on the materials mentioned can be roughly classified into basic types.
  • the division into direct and indirect methods here relates to the first electrically conductive layer, which is structured or applied in a structured manner on a substrate with significantly lower conductivity.
  • the known processes work either directly and subtractively (e.g. laser-induced blation), directly and additively (chemical deposition from the gas phase - CVD, also laser-induced) or indirectly and with the help of a complex combination of different process steps from the range of microlithographic structuring processes (e.g.
  • Etching process in aqueous or gas phase are widely used in semiconductor technology. Those techniques that use only a few process steps are based on a closed metal layer or a closed metal film on the respective substrate. These can be, for example, layers obtained by lamination for thick layers (> 5 ⁇ m) or chemical and physical vapor deposition processes or combinations thereof for thin layers. The latter typically require vacuum conditions and high voltages or chemically aggressive gases and reagents.
  • Coarser structures can be obtained by simply cutting or punching them out of a metal foil and gluing them to the corresponding surface.
  • the negative image can be concealed, overprinted, pasted over or - covered differently, while the image elements stand out clearly in a metallic sheen.
  • the latter technique limits the applicability of the created patterns and structures solely for decoration and packaging purposes.
  • laser-induced chemical deposition can produce high-resolution planar and even three-dimensional metallic structures on different materials (laser-assisted deposition - LAD, synonymous chemical vapor deposition - CVD).
  • laser-assisted deposition - LAD synonymous chemical vapor deposition - CVD
  • these processes are subject to special pressure or atmospheric conditions and are reserved for the production of small series up to lot size 1.
  • Combined methods can also be used. These are either printing processes, such as screen printing techniques, in which a metal paste containing auxiliary substances is applied to the material and then attached to the substrate surface by remelting at an elevated temperature (about 200 - over 800 degrees Celsius). The resolution (smallest structure width) of such processes and thus the quality of the images obtained is limited. The relatively high temperature required for the remelting process for pastes to produce metallizations that can be subjected to permanent loads limits the range of materials usable here to correspondingly stable materials, such as ceramics and glasses.
  • Stamp printing and molding techniques have successfully found their way into the range of microstructuring processes via the LIGA technique (Becker, E.W., et al., Microelectronic Engineering 4: 35-56 (1986)). They are embedded in a complex cascade of individual steps. Their highest lateral resolution is also limited to structure widths in the m range due to the stamp materials to be used.
  • a microlithographically created stamp can be used to make chemical surface modifications with a lateral resolution in the ⁇ m range.
  • the use of environmentally harmful components should preferably be avoided.
  • the object is achieved in that a layer consisting of or containing proteins is applied to the substrate to be coated, the layer or proteins under exposure to light (exposure to light) in a corresponding environment causing a vectorial gradient of a physical or chemical property between two builds up the layer formed compartments and the resulting change in the physical or chemical property in one of the two compartments causes metal ions to be reduced to metal or accessible for later reduction, after which the substrate provided with the proteinaceous layer is exposed at those locations where the metal is to be deposited (positive exposure), or the change in property mentioned causes an already existing metal deposit on the exposed areas of the layer to be removed (etched away) (negative exposure).
  • proteins used according to the invention are those which as
  • Pulp can act to build up a gradient of a physical or chemical property directed against the usually established equilibrium.
  • the "property” can be physical, e.g. on
  • Electron gradient but is preferably chemical in nature.
  • the proteins can be natural proteins, naturally derived (e.g. - genetically or chemically modified) proteins or artificial proteins.
  • the structure of the concentration gradient should be inducible with the help of light (photons).
  • proteins are found in nature, for example.
  • Bacteriorhodopsin is a
  • мем ⁇ proteins that acts as a "proton pump” when exposed to light, while an example of an anion pump is halorhodopsin (see Oesterheld, D., Israel J. of Cheistry 1995, 35: 475-494).
  • Such proteins are commonly referred to as “retinal proteins”. In principle, they use a cis-trans transition of a chromophore with light absorption, as found in alkenals such as the retinal of rhodopsin (visual purple of mammals) or the retinal of bacteriorhodopsin o was.
  • Some "retinal proteins” use the energy obtained to build up a concentration gradient, for example the aforementioned, bacteriorhodopsin and halorhodopsin.
  • the proteins to be used according to the invention can be genetically modified proteins derived from natural proteins. Small changes in the structure of the amino acid chain of the protein can possibly already bring about a significant change in function here: for example, a bacterial mutant is known that produces a bacteriorhodopsin modified by only one amino acid, which transports chloride ions (Sasahi et al., Science ( 1995), 269: 73-75).
  • lipids as the carrier material. In principle, there are no restrictions on the selection thereof; phospholipids are preferred. For cost reasons, fabrics such as
  • Soybean lecithin or azolecitin Soybean lecithin or azolecitin.
  • Soybean lecithin or azolecitin Soybean lecithin or azolecitin.
  • all phosphatidylcholines and their derivatives are suitable.
  • the lipids can be deposited as a two-dimensional layer on the substrate, in which the protein (or different types of protein) are embedded.
  • the advantage of using lipids is their spatial composition of the hydrophilic head and hydrophobic tail, which causes the lipids to be arranged in parallel (head-head and tail-tail).
  • the protein for example bacteriorhodopsin, will be arranged in such a layer with a preferred direction.
  • the protein-containing layer consists of or comprises lipid vesicles (liposomes) in which the protein is embedded.
  • lipid vesicles liposomes
  • Bacteriorhodopsin gets into the
  • the vesicle is installed, it is arranged in the artificial membrane in such a way that the pump function - unlike in nature - can also be "inside-out".
  • metal ions can either be reduced either in the immediate vicinity of the vesicles or in their interior, or changed in such a way that they are amenable to reduction.
  • the result is the locally defined deposition of these metal atoms.
  • other methods which are customary in the technology of metal deposition can also be followed, e.g.
  • a sensitization example: tin (II) chloride is converted into tin (II) hydroxide, which precipitates in a pallidum (II) salt bath with the oxidation of palladium metal).
  • Suitable metal layers on the substrate instead of direct etching, a metallic or non-metallic auxiliary, for example another alkali or acid-unstable compound, can also be activated in this variant, which in turn then causes the etching.
  • a metallic or non-metallic auxiliary for example another alkali or acid-unstable compound, can also be activated in this variant, which in turn then causes the etching.
  • the protein molecules must remain fixed in place from the time of exposure. This can be ensured by embedding them in the layer applied to the substrate.
  • the proteins additionally have an "anchor", i.e. they are replaced by Van der Waals or other, e.g. chemical forces held on the substrate.
  • the layer consisting of or containing proteins must be arranged in an environment which allows the concentration gradient to be formed. When using a proton pump, it is necessary that a sufficient amount of water molecules is present in both compartments.
  • An aqueous solution which contains the metal ions in is preferably located within the vesicles or below the two-dimensional layer (by "two-dimensional” is meant a layer which consists only of particles which are essentially arranged next to one another, but which can be formed both in one layer and in multiple layers) Contains form of a metal salt.
  • the outside of the vesicles (or the side of the two-dimensional layer facing away from the substrate) should also be covered by an aqueous solution which can contain the corresponding metal ions. It is sufficient if this solution covers the vesicles in a thin layer, which can be ensured - if necessary with the help of a "moist chamber".
  • Concentration gradient as described above depending on the selected conditions inside or on the outside of the vesicles, be suitable for effecting or preparing for the reduction or etching. If the former is the case, of course they have to
  • Vesicles are destroyed or opened so that the desired one
  • the metal ions which can be used according to the invention can be selected depending on the material to be deposited. Tin or transition metals, which can be complexed, for example, are preferably selected.
  • organometallic compounds can also be used. Protonation of such compounds leads to radicals that decompose to metal or metal oxide. Such radicals may be hydrolyzed relatively slowly, so they may be relatively long-lived. Otherwise, or in addition, they can be stabilized, for example by packing them in micelles.
  • the viscosity of the metal ion solution can contribute to the stability of the proteins.
  • the viscosity can be increased using conventional means, e.g. by adding polyvinyl pyrrolidone or polyvinyl alcohol.
  • the surface of the substrate can be electrically conductive or non-conductive; the effect of metal deposition or etching is independent of this.
  • the metal deposition that prepares the production of structured metal layers does not have to be a comprehensive deposition. It is sufficient to deposit crystal nuclei of the metal on the substrate surface. Here are high
  • the crystal nuclei can be catalytically active in the subsequent steps in the deposition of further material.
  • the substrate surface is covered with a light-sensitive protein layer as stated above, followed by the desired imaging pattern or the desired one Structure is written / drawn by appropriate exposure, if necessary with a focused light source or projected with a suitable photo mask.
  • the process according to the invention can in many cases be carried out at room temperature. If proteins occurring in nature are used, it is preferred to carry them out at a temperature which corresponds to the natural environment of the protein.
  • a metallic layer is deposited from the liquid at the locations (picture elements) of the material which have been changed by the exposure.
  • the method of metallization with the aid of molecules whose properties can be changed optically or complex mixtures of these is also suitable for generating spatial structures.
  • These structures which can be viewed from several complexly interconnected individual planes or components thereof, can be produced by specifically guiding focused light on the three-dimensional substrate that is homogeneous or inhomogeneous in its material composition and / or structure for metal deposition.
  • a substrate can be, for example, a sol, a gel, a glass or a monolithic or porous solid, such as, for example, a crystal compact similar to a piece of sugar cubes. From a complex, three-dimensional one created in this way
  • Layer structure in the sense described can completely or partially remove the underlying substrate, the surface of which was used for the layer deposition (for example by Dissolve in a suitable solvent). What remains - in the case of simply removing a planar substrate - is a finely structured planar layer of the deposited material, or else a spatially complex structure. This structure then consists of a metallic material or a material containing a metallic component.
  • this embodiment of the invention there is a layer of molecules and possibly auxiliary substances applied to the surface or in the substrate, which leads to the formation of locations of preferred metal deposition in the course of subsequent processes by means of a light-addressed change in the properties of an essential component of this layer .
  • a further embodiment of the invention uses the special properties of a substance which acts as a molecular pump, for example the bacteriorhodopsin molecule, which can be obtained from bacterial biomass.
  • the directional deposition of a monolayer of such molecules is used for locally high-resolution corrosion or modification of the substrate used as a base in a liquid medium.
  • the molecule referred to here as the "pump" has the property of selectively transporting substances such as - for example protons (H + ) or ions from the solution side to the substrate side through a layer which simultaneously serves as a support and barrier, under the action of light. These factors are structured in close proximity to the substrate surface. The structuring can lead to the creation of otherwise undetectable defects.
  • a further structuring or other modification of the material is carried out.
  • This can be isotropic or anisotropic etching or the formation of a layer, for example by crystallization a substance that comes into contact with the substrate from • a solution, a suspension or a gas.
  • the locally high-resolution deposition of the primary metallic layer which is later to act catalytically or directly as a nucleation at the location of previously optically modified molecules allows precision in the range of the wavelength of the light used, but at least in the range of if necessary Vesicle size.
  • the use of focused light, such as that of a laser beam, and the simplicity of the process control also allow metallization to be carried out in and under porous layers.
  • the same or different planar metallizations, one on top of the other in several levels, can be electrically conductively connected to one another via predetermined bridges. By combining suitable parameters, structures made of two or more different metals can be constructed planar and three-dimensional.
  • Such complex metallization structures can be used as high-density wiring structures.
  • Process-determining parameters result from the optical absorption properties of various proteins or other light-sensitive substances in their mixture, and / or the time-delayed incubation with solutions of different metals, or the controlled reaction kinetics in complex solutions and mixtures.
  • the lateral extent of a metallic layer on the respective substrate can be specified with precision in the micrometer and sub-micrometer range.
  • Materials or layers is based on the same principle of optically addressable targeted modification of a suitable layer on a surface.
  • the method according to the invention it is possible, for example, to achieve a decorative metallic gloss for labeling surfaces.
  • the embodiments of the invention mentioned can be used to build up complex layers and structures.
  • the material that ultimately dominates the structure produced can be of a different material composition than the underlying substrate surface or the substrate itself.
  • FIG. 1 shows the sequence of steps of a photo-addressed metallicization
  • Figure 2 illustrates the precision of the layer deposition
  • FIG. 3 shows the sequence of steps of a fine etching technique mediated by a “molecular pump”.
  • 1 denotes a support / fixation auxiliary (e.g. lipid), 2 a photoactivatable molecule, such a molecular compound or cluster, 3 the substrate; 4 represents crystallization nuclei, and 5 a grown metal layer.
  • the sequence of steps shows, from top to bottom, the substrate 3 alone, the substrate with a layer of photoactivatable molecules deposited thereon in a supporting matrix, the selective exposure (hv) of a photoactivatable molecule or group of molecules (dry or wet), the primary metallization caused thereby with the formation of
  • the etching process is also illustrated in FIG. 3, from top to bottom, the substrate (drawn in dashed lines) with a metal layer deposited thereon ("primary layer", drawn as a continuous thicker black line) in the second row with monolayers of photoactivatable molecules in one Carrier (support function) are coated.
  • the selective exposure induces local pH gradients, recognizable by defects in the metal layer, which are enlarged by biomimetic corroding (4th row). The corrosion is stopped by removing the photoactivatable molecules (last row).
  • Liposomes are produced which contain metal ions stabilized in solution in the enclosed internal liquid pool and bacteriorhodopsin molecules (BR) oriented in a preferred direction (vectorially) in their lipid membrane.
  • a dispersion of such liposomes is applied as a closed thin layer to the substrate to be provided with a metal structure and partially exposed with the aid of an appropriate photomask.
  • the pH of the liquid encapsulated in the liposomes changes as a result of the activity of the molecular proton pump BR.
  • the temporary shifts in pH thus triggered are used to modify the solution of the encapsulated metal salt.
  • Metal salts of the type of complex compounds can be destabilized and partially or completely changed in this way.
  • the amount of lipid required for the preparation of a 0.1-0.5% lipid suspension is weighed into a test tube and together with a 0.01-1 mM salt or complex salt solution of a metal (for example 100 ⁇ M palladium (II) chloride ) in a 0.01 - 5 M salt solution of a chloride, sulfate, carbonate, nitrate or phosphate whose pH value can be adjusted to sizes around or below pH 8 (for example 0.5 M potassium sulfate) with the aid of a
  • a metal for example 100 ⁇ M palladium (II) chloride
  • Ultrasonic generator suspended according to common procedures. With constant cooling in the (tap water) cooling bath, depending on the power used, a clear, slightly opalescent liposome dispersion can be obtained within about 10 minutes.
  • a solution of the BR (bacteriorhodopsin) intended for reconstitution in the liposome membrane is added to the prepared liposome preparation.
  • the "incorporation" of the BR into the liposomes is again carried out using the titanium horn of an ultrasound generator within about 3 minutes, but can also be done - in other ways - as is common in biochemistry, biophysics or medicine in various variants.
  • polymers ⁇ for example, polyvinylpyrrolidone (PVP) or polyvinyl alcohol (PVA) may be added.
  • PVP polyvinylpyrrolidone
  • PVA polyvinyl alcohol
  • a 7.5% PVP - liposome dispersion can be applied to the substrate as a thin film - for example with one in the
  • microelectronic technologies commonly used spin coater The substrate prepared in this way is then exposed to yellow light (1> 500 nm) through the photomask in a moist atmosphere (so-called “moist chamber”). The exposed substrate is then dried in a hot air oven and is then available for conventional chemical metallization, for example with a nickel-boron layer (NiB).
  • Moist chamber a moist atmosphere
  • NiB nickel-boron layer
  • the substrate is dried in a hot air oven. This is followed by a conventional NiB deposition. lo
  • Metal layers on surfaces or their preparation in which, starting from protein molecules adhering to the surface of a solid, these properties change locally and thus compared to the unchanged protein molecules of the layer at the location of metal deposition from a solution or suspension and / or the binding of colloidal metal particles or become atomic clusters from a liquid or a gas or a gas mixture containing them, a protein layer ordered with molecular resolution or components thereof serves as an initiator of a reaction on a surface which is wetted by a solution or brought into contact with a defined gas composition, a local concentration gradient of at least one component in the liquid or gas phase in the immediate vicinity of certain protein molecules can be an important influencing variable for controlling the deposition process, light one Discrete wavelength from the spectrum of visible light is a factor that modifies the peculiarity of the protein molecules adhering to the surface
  • Conformational state of a polymeric component located at the location provided for metal deposition and which contains various amino acid residues as structural units represents a parameter determining the metallization process.
  • the invention further encompasses those configurations in which structured metal layers are produced on surfaces in contact with a liquid phase, as set out above, in which bacteriorhodopsin or a derivative derived therefrom or a variation thereof the protein component in represents the layer or constitutes an essential constituent thereof, a protein mixture or a mixture of proteins with other molecules capable of different conformational states is used for the layer structure,
  • the layer is stabilized by a type of molecule which is chemically inert under the other conditions, staggered or synchronously, discrete areas of the primary protein-containing layer absorb light of different wavelengths, discrete areas of a primary non-metallic layer are excited by light of a defined wavelength and / or their properties are changed locally ,
  • the liquid phase can contain the salt of a metal to be deposited in dissolved form, the liquid phase is a colloidal solution of the smallest ( ⁇ 200 nm diameter), a separate load of carrying particles, the liquid phase can contain a metal colloid, - the composition of the liquid Phase changes over the duration of contact with the substrate, the properties of the components in the liquid leading to the metal layer formation stabilized by the presence of other solutes or for the intended purpose of the layer Deposition is improved, the surface provided for metal layer deposition can be covered by a porous layer, the surface provided for metal layer deposition can represent the inner surface of a porous material, the surface provided for metal deposition represents the surface of a material which can be formed

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  • Engineering & Computer Science (AREA)
  • General Physics & Mathematics (AREA)
  • Physics & Mathematics (AREA)
  • Biomedical Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemically Coating (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

L'invention concerne la production de minces couches métalliques et de structures de telles couches sur des substrats supports de différentes structures. L'expansion latérale d'une couche métallique sur le support en question peut être déterminée avec une précision de l'ordre du micron et du submicron. Le procédé décrit permet la fabrication de structures métalliques plates et tridimensionnelles sur des surfaces lisses, planes ou courbes, comme celles utilisées, par exemple, pour reproduire des lettres ou des dessins, sans faire intervenir de techniques d'impression par poiçons.
EP97945795A 1996-10-25 1997-10-27 Procede permettant de preparer la production de couches metalliques structurees a l'aide de proteines Withdrawn EP0934553A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19644516 1996-10-25
DE19644516 1996-10-25
PCT/DE1997/002494 WO1998019217A1 (fr) 1996-10-25 1997-10-27 Procede permettant de preparer la production de couches metalliques structurees a l'aide de proteines

Publications (1)

Publication Number Publication Date
EP0934553A1 true EP0934553A1 (fr) 1999-08-11

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Country Status (4)

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US (1) US6197387B1 (fr)
EP (1) EP0934553A1 (fr)
DE (1) DE19747377A1 (fr)
WO (1) WO1998019217A1 (fr)

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WO2002078906A2 (fr) * 2001-03-29 2002-10-10 Cellect Technologies Corp. Procedes, dispositifs et systemes de tri et de separation de particules
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US6197387B1 (en) 2001-03-06
DE19747377A1 (de) 1998-05-28
WO1998019217A1 (fr) 1998-05-07

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