EP1534631A1 - Procede de production de cristaux hautement organises au moyen de procedes sol-gel - Google Patents

Procede de production de cristaux hautement organises au moyen de procedes sol-gel

Info

Publication number
EP1534631A1
EP1534631A1 EP03750426A EP03750426A EP1534631A1 EP 1534631 A1 EP1534631 A1 EP 1534631A1 EP 03750426 A EP03750426 A EP 03750426A EP 03750426 A EP03750426 A EP 03750426A EP 1534631 A1 EP1534631 A1 EP 1534631A1
Authority
EP
European Patent Office
Prior art keywords
crystal
analog
superstructure
particles
porous material
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Withdrawn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
EP03750426A
Other languages
German (de)
English (en)
Inventor
Wolfram Beier
Rupert Schnell
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.)
Schott AG
Original Assignee
Carl Zeiss AG
Schott Glaswerke AG
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
Priority claimed from DE2002141494 external-priority patent/DE10241494A1/de
Application filed by Carl Zeiss AG, Schott Glaswerke AG filed Critical Carl Zeiss AG
Priority to EP20060017325 priority Critical patent/EP1757662A3/fr
Publication of EP1534631A1 publication Critical patent/EP1534631A1/fr
Withdrawn legal-status Critical Current

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    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • 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
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
    • B01J21/063—Titanium; Oxides or hydroxides thereof
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/391—Physical properties of the active metal ingredient
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
    • C01B13/14—Methods for preparing oxides or hydroxides in general
    • C01B13/145—After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
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    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
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    • C01B33/1585—Dehydration into aerogels
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    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
    • C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid phase
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
    • 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
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C—CHEMISTRY; METALLURGY
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    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/36—Compounds of titanium
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    • C12N11/00—Carrier-bound or immobilised enzymes; Carrier-bound or immobilised microbial cells; Preparation thereof
    • C12N11/14—Enzymes or microbial cells immobilised on or in an inorganic carrier
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
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    • G02B5/20—Filters
    • G02B5/206—Filters comprising particles embedded in a solid matrix
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    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
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    • G02B6/1225—Basic optical elements, e.g. light-guiding paths comprising photonic band-gap structures or photonic lattices
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    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • 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
    • C08J2399/00—Characterised by the use of natural macromolecular compounds or of derivatives thereof not provided for in groups C08J2301/00 - C08J2307/00 or C08J2389/00 - C08J2397/00
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/10—Biological treatment of water, waste water, or sewage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00—Technologies for wastewater treatment
    • Y02W10/30—Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy

Definitions

  • the invention relates to materials with a crystal-analog superstructure, in particular photonic crystals, which are obtained by self-organization, either by self-organization of the particles which form the photory crystal itself or by sol-gel infiltration into a preform, a so-called template; a method for producing the same and the use of such crystals.
  • Photonic crystals are materials with a crystal-like superstructure with a photonic band gap, ie forbidden or inadequate energy states for photons, ie light of a certain frequency cannot propagate in all spatial directions.
  • Photonic crystals which have such an optical band gap are characterized by a regular three-dimensional periodic grating structure, which consist of regions with strongly changing refractive indices.
  • One way of producing photonic crystals is by using micromechanical processes.
  • a silicon wafer can be coated with silicon dioxide, even trenches can be scratched therein and these can be filled with polysilicon.
  • the surface can be ground flat, covered again with SiO 2 and regular polysilicon strips can also be structured therein, albeit at right angles to that in the layer below. By repeating this several times, double layers can be produced crosswise in this way.
  • the Si0 2 can be extracted as a support material with hydrogen fluoride, so that there is a cross-lattice structure made of polysilicon with regular cavities.
  • a completely different way of producing photonic crystals is the construction of photonic crystals by self-organizing or induced-controlled processes.
  • Such self-organizing or induced-controlled processes are in the field of colloidal crystals, which are composed, for example, of titanium dioxide or
  • colloidal crystals form spontaneously under suitable temperature and pressure conditions. They have a three-dimensional regular superstructure with submicron periodicity.
  • the structural elements of the colloidal crystals are, for example, polymer z.
  • polystyrene beads with a size of 10 nm to
  • colloidal crystals are produced by sedimentation, which lead to thick polycrystalline samples within a liquid.
  • the liquid in the sedimented colloidal structures consisting of the aforementioned structural elements is then drawn off, so that voids between the structural elements, i.e. for example, the polymer beads.
  • Photonic crystals produced in this way have domains up to a few centimeters (cm) in size.
  • the capillary forces on the meniscus of a colloidal solution and a substrate are used to pull colloids into densely packed structures through self-organization.
  • the disadvantage of the method known from the prior art for producing highly organized, in particular photonic, crystals using micromechanical methods is the high outlay.
  • sol-gel processes which are used in the sol-gel infiltration of a preform, for the production of glasses, glass ceramics, ceramics and
  • Sols are colloidal suspensions of solid and liquid substances in a liquid or gaseous dispersion medium, the particle size being between 5 x 10 "10 and 2 x 10 " 7 m.
  • catalyst supports materials which have a wide size distribution of the cavities are used as catalyst supports.
  • Such catalyst supports for example made of zeolites, have a high flow resistance.
  • open-pore sintered glasses are used for immobilizing bacteria and other biological, microbiological, bioprocessing and medical expenses and for cleaning and treating water.
  • Such sintered glasses are sold by SCHOTT GLAS, Mainz, under the brand name SIRAN® and are described, for example, in the article "Bioreactors in Wastewater Technology” by M. Radke in Disposal Practice 10/89
  • Paints as color effect coatings according to the prior art of metal, glass or plastic surfaces usually contain, in addition to the coloring pigments, metallic particles, for example aluminum powder, in order to achieve a metallic luster.
  • a brilliant effect can also be brought about by the size variation of these particles and in particular by the addition of large aluminum particles and plastic particles.
  • the color pigments can be flake-like and vaporized with metal.
  • Lacquer coatings according to the prior art with high light dynamics ie lacquers with gloss effects or those that give a color impression that depends on the incidence of light and the direction of view, are characterized by a particularly complex production and by a limitation in the design of the color effects.
  • additives with an iridescent color effect can be incorporated into the material during manufacture.
  • a traditional example of this is the rainbow-colored, shiny metallic Tiffany glass from the Art Berlin period, which was mostly produced by vapors from various mixed metal salts.
  • the disadvantage here is that the color effect can usually not be precisely controlled, since it depends on the details of the formation of metal colloids in the glass matrix. The restrictions that result from this for the selection of the glass materials and the manufacturing conditions are to be regarded as disadvantageous.
  • Coloring the surface consists in the use of interference layer systems, which are characterized by wavelength-selective reflection.
  • interference layer systems are complex to manufacture, since each layer has to be applied or vapor-deposited on its own.
  • the layer sequence alternating in only one direction enables one
  • a first object of the invention is to provide a method for producing highly organized, in particular photonic crystals, with which the disadvantages of the prior art can be overcome, in particular the drying of the self-organized crystal-like superstructures and the inverse produced by sol-gel infiltration crystal-like superstructures take place without damage and faster than in the prior art. Especially should damage to inverse crystal-analog superstructures produced by the sol-gel process can be prevented during drying.
  • Another object of the invention is to overcome the disadvantages of conventional materials used as IR blockers or UV blockers.
  • IR blockers and / or UV blockers should be able to be produced in a simple manner, for example, by applying a dispersion which is applied once to a substrate, for example window glass, for example sprayed on or spun on.
  • Another object of the invention is to overcome the disadvantages of conventional porous materials as catalyst supports in chemical and process engineering applications, as materials for the purification and treatment of water and for the immobilization of bacteria and for other biological, microbiological, bioprocess and medical
  • catalyst supports with a lower flow resistance are to be made available, as are open-porous materials whose functionality can be influenced in such a way that colonization with specific, selected microorganisms is achieved and so these microorganisms can be immobilized.
  • the first object is achieved in that the highly organized, crystal-analog superstructures or inverse crystal-analog superstructures are subjected to hypercritical drying.
  • the crystal-analog superstructures are also referred to as a structure or heap structure.
  • Hypercritical drying enables the liquid to be drawn off from the crystal-analog superstructures more quickly. Furthermore, damage to the structure, in particular the inverse structures during drying, is prevented.
  • Fricke J. "Aerogels - a spectacular class of highly porous materials” in Umschau 1986, Issue 7, pp. 374 - 377 and Fricke J., "Aerogels - highly tenuous solids with beautiful properties", Journal of
  • Hypercritical drying takes advantage of the fact that the solid / liquid phase boundary is removed above the critical point and that a single phase still exists, i. H. that above the critical temperature, for example, a gas can no longer be liquefied by the highest pressure.
  • hypercritical drying means that there are no longer any voltage differences in the solid to be dried. This prevents the solid from tearing.
  • US 5795557 From US 5795557 the production of aerogels from silica is known. US 5795557 refers to the fact that aerogels can be obtained by sol-gel processes. The airgel is dried after drying. H. received after separating the alcohol.
  • US 6139626 describes the production of templates, ie synthetic opals and the filling of the pores of the template with colloidal nanocrystals described.
  • the colloidal nanocrystal solution contains at least one solvent, which is extracted.
  • the hypercritical drying according to a first aspect of the invention is carried out in such a way that non-destructive drying of regularly arranged self-organized or controlled organized particle arrangements, in particular inverse crystal-analog superstructures, which are produced by sol-gel infiltration, is made possible.
  • Inorganic, organic or hybrid processes such as the Ormocer process are conceivable as sol-gel processes.
  • Hypercritical drying can also take place in several stages, for example by solvent exchange.
  • Hypercritical drying will be used in particular to dry the self-organized or induced organized crystal-analog superstructures made of, for example, polymer beads, which in turn can serve as templates for high-index materials. These templates can be infiltrated with high refractive index materials using the sol-gel method, resulting in an inverse crystal structure. Hypercritical drying of the infiltrated gel enables low-shrinkage, crack-free inverse photonic crystals to be obtained by molding.
  • the particles which form the tempiate for example the polymer beads, can be used to enlarge the Difference in refraction from the inverse crystal structure can be removed, for example, by burning out.
  • the method according to the invention does not quickly extract a solvent, as described, for example, in US Pat. No. 6,261,469, but instead solidifies the structure by means of hypercritical drying and stabilizes the tempiate, for example. It is then possible, for example, to obtain photonic crystals or templates which form stable, superordinate, periodic structures without neck formation. In the past, such necks were necessary in photonic crystals to hold the superstructures together, for example, and to ensure mechanical stability.
  • the method according to the invention enables the production of optical components with a photonic crystal superstructure with large dimensions and of three-dimensional, optical components with a photonic crystal superstructure of complex shape and / or structuring.
  • templates which can serve as a preform for the formation of crystal-analogous superstructures of solids with a higher refractive index and which are referred to as so-called inverse opals
  • Hypercritical drying of a gel can be achieved, for example, by the following procedure in the case of tetra-methyl-orthosilicate Si (OCH 3 ) (TMOS) for the production of Si0 2 aerogels which are introduced into the tempiate to form an inverse crystal-analogous superstructure become:
  • the pressure P is increased very strongly at a constant temperature, for example in TMOS for the production of SiO 2 aerogels to approximately 80 bar.
  • the temperature is then increased to approximately 270 ° C. while the pressure is kept constant.
  • the fluid can be forced out of the gel structure without the gel structure breaking down or shrinks because such a process control always takes place above the critical temperature TK and only a liquid or gaseous phase is present.
  • the liquid or gaseous phase is extracted when the pressure is reduced to atmospheric pressure.
  • the temperature is lowered to room temperature.
  • the method according to the invention achieves hypercritical drying.
  • the procedure for the supercritical fluid extraction is chosen so that the fluid is quickly drawn off, i. H. is extracted; in the case of hypercritical drying, the process is chosen in such a way that the superstructure of the photonic crystal is stabilized so that, for example, neck attachments as in the prior art can be avoided with photonic crystals and the superstructure is stable even without such neck attachments.
  • a porous material in the form of a photonic crystal which is used as an IR blocker, can be produced in various ways.
  • particles for example polymer, silicon dioxide or titanium dioxide particles
  • the particles organize themselves in the dispersant by slow sedimentation to crystal-like superstructures themselves or under controlled control.
  • the middle of the dispersion! by drying, for example hypercritical drying,. deducted and the self-organized crystal stabilized.
  • Self-organization in crystal-analog superstructures in a dispersion medium is particularly advantageous in the case of silicon dioxide or titanium dioxide particles, since there is a large refractive index difference between the particles themselves and the air-filled cavities in such crystal-analog superstructures.
  • the photonic crystal can be produced by sol-gel infiltration in a preform, a so-called tempiate.
  • the highly organized crystal-analog superstructures or inverse crystal-analog superstructures which are used for UV blockers or IR blockers become hypercritical
  • Hypercritical drying prevents damage to the structure, in particular the inverse structures, during drying.
  • Catalysts with such catalyst carriers are characterized by a very low flow resistance.
  • the reason for this is the extremely narrow distribution the characteristic dimensions of the cavities in photonic crystals.
  • such arrangements are distinguished by the fact that they can influence chemical reactions in a highly selective manner. This is due to the fact that the size of the cavities or the pore size can be adapted to the dimensions of the atoms, molecules or radicals involved in the reaction in question. Further, it is possible by controlling the size of the cavities in the superstructure krsitallanalogen to adjust the flow rate accurately ⁇ .
  • Reactions can be addressed using suitable structural parameters such as particle size, particle shape, particle spacing, porosity etc.
  • a porous material can be produced in the form of a photonic crystal, which acts as a catalyst carrier in chemical and process engineering
  • the hypercritical drying particularly damages the
  • Crystals for the immobilization of bacteria and for other biological, microbiological, bioprocess engineering and medical applications lies in the fact that such regular structures can be equipped with a larger loading capacity than the currently known subordinate porous materials and aggregates. Furthermore, it is possible to further develop and condition the colloidal crystals that have an optical band gap in such a targeted manner that very specific bacteria or viruses can be immobilized by suitable cavity sizes.
  • a porous material can be produced in the form of a photonic
  • Crystals that are used for the immobilization of bacteria and for other biological, microbiological, bioprocess engineering and medical applications, for example with the aid of slow sedimentation in a dispersant and subsequent hypercritical drying.
  • Water purification and treatment is such that such regular structures with a higher throughput capacity than the currently known disordered porous materials and piles allow. Furthermore, it is possible to specifically further develop and condition the colloidal crystals, which have an optical band gap, in such a way that the substrate material, the
  • a porous material in the form of a photonic crystal can be produced, which is used for the purification and treatment of water, for example with the aid of slow sedimentation in a dispersing agent and subsequent hypercritical drying, in which the dispersing agent is stripped off.
  • Such layers or coatings based on photonic crystals are characterized by an intensive development of the color effect and the color dynamics.
  • the color effect coating is particularly suitable for use on a large number of large and arbitrarily shaped substrates.
  • a porous, color effect-producing coating material in the form of a photonic crystal can be produced in various ways.
  • a first color effect coating according to the invention is obtained in that particles, for example polymer, silicon dioxide or
  • the crystal-analog superstructures Organize titanium dioxide particles into a dispersant controlled by slow sedimentation to crystal-analog superstructures themselves or induced.
  • the lattice periodicity of the resulting crystal-analog superstructure is determined by the choice of particle size.
  • the crystal-analog superstructures must have a lattice periodicity in the course of the refractive index in the range of the wavelength of the visible spectrum, i.e. in the range 380 nm ⁇ d ⁇ 780 nm.
  • Crucial for the optical quality of the color effect coating is the strict periodicity in the refractive index and the high symmetry of the photonic crystal.
  • the self-organization in crystal-analog superstructures in a dispersion medium is particularly in the case of silicon dioxide or titanium dioxide particles advantageous since there is a large refractive index difference between the particles themselves and the air-filled cavities in such crystal-analog superstructures.
  • the dispersant In order to create these air-filled cavities, the dispersant must be removed from the crystal-analog superstructure. Since this is problematic, as described above, due to the flatness of the coating and the capillary forces acting on it, it is particularly advantageous that the dispersant is removed by hypercritical drying, thus creating a highly ordered, crystal-analogous superstructure with air-filled spaces, the lattice structure of which is maintained evenly remains that the desired color effects come into their own.
  • the effect of the method with hypercritical drying is to be seen in the fact that porous coating material producing a color effect can be obtained in a sufficiently stable manner essentially without the neck-like material connections between the particles which disturb the optical properties of the coating.
  • the neck-like connections are, for example, disturbing for the optical properties of the photonic crystal when used in color effect layers, since the strict periodicity of the filter is adversely affected.
  • An alternative color effect layer or an alternative color effect coating based on photonic crystals represents an inverse structure to that described above.
  • a photonic crystal is produced as a coating by sol-gel infiltration in a preform, a so-called tempiate.
  • a highly ordered crystal-analog superstructure according to the invention without neck-like connections between the particles forming the superstructure, as described above, is used as a template.
  • Fig. 3 shows a color effect coating on a substrate comprising two porous material layers with different spatial
  • FIG. 4 shows a crystal-analog superstructure according to the prior art, with neck-shaped material connections for mechanical strengthening being formed between the particles forming the superstructure.
  • FIGS. 1a to 1c show the production of a crystal-analog superstructure by adding particles 1, preferably spheres with dimensions 10 nm to 10 ⁇ m in a dispersing agent 3 and stripping off the dispersing agent.
  • the particles can be polymer, Ti0 2 - or Si0 2 - beads or beads made of other organic or inorganic materials.
  • Polystyrene (PS) or polymethyl methacrylate (PMMA) particles, preferably polystyrene (PS) or polymethyl methacrylate (PMMA) beads, are particularly suitable as polymer particles.
  • FIG. 1a the particles in the solution 3 are distributed irregularly.
  • the particles arrange themselves in crystal-analogous, regular superstructures 5 through sedimentation and self-organization or induced controlled organization. This is shown in Figure 1 b.
  • the dispersant still present in FIG. 1b is drawn off, preferably by hypercritical drying.
  • the solid body 5 shown in FIG. 1c is then formed, which is a crystal analog
  • the solid 5 can itself be the photonic crystal, for example in the case of Ti0 2 or Si0 2 beads or as a tempiate for serve high-index materials. If the solid 5 consists of TiO 2 spheres, the solid 5 can be used as a porous material for the purification and treatment of water without further processing, for example coating.
  • the solid 5 is a crystal-analog superstructure, for example made of Si0 2 or polymer beads
  • the solid 5 forms the base material onto which a coating containing Ti0 2 or titanium oxide can be applied, which then forms the functional layer for cleaning and preparation of water.
  • the functionality can be tailored through the coating.
  • the photonic crystal with high refractive index material can be infiltrated with a high refractive index as shown in FIGS. 2a-2c
  • the polymer solid with a crystal-analog superstructure is placed in a colloidal solution or sol 10.
  • the colloidal solution comprises particles 12 with a size between 5-10 -10 and 2-10 -7 m, which agglomerate and form a gel structure.
  • a gel structure is formed in the spaces 14 of the polymer solid 5, which forms the tempiate for the high-index material.
  • the gel structure is dried hypercritically.
  • the hypercritically dried structure is shown in Figure 2c.
  • the dried high refractive index material is designated 20, the microstructure resulting from the microporosities is 22.
  • the particles 1 of the template can be removed, for example in the case of a solid made up of polymer beads as a tempiate by burning out.
  • FIG. 3 shows a color effect coating on a substrate 102 with two porous, layered layers 101.1, 101.2 arranged in a crystal-analogous manner, which differ in their lattice periodicity. Both grating periodicities of the refractive index should be selected so that only light of a wavelength in the range of the visible
  • a color effect coating according to the invention can also be provided by a porous layer with a uniform
  • Lattice periodicity or with more than two different lattice periodicities are formed.
  • FIGS. 1a-1c The production of a crystal-analog superstructure is shown in FIGS. 1a-1c and, for example, if a solid polymer with a crystal-analog
  • FIG. 4 shows in a schematically simplified manner a mechanical hardening of the crystal-analog superstructure by the formation of neck-like material connections 130 between the particles 101.
  • Structure is that their growth can usually not be controlled with sufficient accuracy, so that there is a deviation from the symmetrical
  • the structure and distortion of the grid result, for example, which reduces the color effects of the coating or has other disadvantages in other applications, such as, for example, reduced selectivity when used in the field of water treatment or in the immobilization of microorganisms.
  • the invention provides for the first time a process for the production of highly organized superstructure materials, with which photonic crystals with relatively large dimensions in the range of a few centimeters (cm) to decimeters (dm) for bulk materials and up to a few meters (m)
  • Coatings can be made.
  • the invention specifies porous materials which act highly selectively as IR blockers in the IR wave range, for example as IR-blocking coating material for window panes, automobile panes, spectacle lenses, technical and scientific components with IR filter function, components for solar systems, lamp glasses and for Finding electronic components, in solar systems, especially solar thermal systems, succeeds in significantly increasing the efficiency with such IR filters.
  • IR-blocking coating material for window panes, automobile panes, spectacle lenses, technical and scientific components with IR filter function, components for solar systems, lamp glasses and for Finding electronic components, in solar systems, especially solar thermal systems, succeeds in significantly increasing the efficiency with such IR filters.
  • the energy yield can also be increased considerably, since due to the reflection of the substrate coated with an IR-blocking material, the emitted IR light is focused back onto the light source, for example the filament.
  • an IR-blocking coating material can be used to protect such components from heat radiation or from excessive heating by adjacent hot ones
  • the IR blocking layer according to the invention can be applied to substrates by means of an immersion, a centrifugal or spray method. Any type of glass, transparent base materials or other transparent substrates, but also opaque substrates such as metals and ceramics are suitable as substrate materials for the IR-blocking layers. Furthermore, "the invention specifies porous materials which act in the UV wave range as highly selective UV blockers, for example as UV blocking coating material for window panes, automobile windows, spectacle lenses, in particular sunglasses lenses, technical and scientific components with UV filter function.
  • the UV blocking layer according to the invention can on
  • Photonic crystals are applied using a dipping, spinning or spraying method.
  • the photonic crystals can preferably be produced directly using sol-gel methods. Any type of glass, transparent base materials or other transparent substrates, but also opaque substrates such as metals and ceramics for reflective optics are suitable as substrate materials for the UV-blocking layers.
  • the invention provides for the first time a porous material and a method which can be immobilized in a highly specific manner in bio-process engineering and medical applications, in particular bacteria.
  • porous materials and a process for the production are specified with which catalyst supports with a very regular pore size can be produced, as well as porous materials with which highly specific immobilization can be carried out in biotechnological and medical applications, in particular bacteria.

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Abstract

L'invention concerne un procédé de production de matériaux présentant une surstructure cristalline ou une surstructure cristalline inverse, en particulier de cristaux photoniques. Selon ce procédé, lesdits matériaux à surstructure cristalline sont générés par auto-organisation ou au moyen de processus régulés et induits ainsi que par séchage hypercritique.
EP03750426A 2002-09-07 2003-08-22 Procede de production de cristaux hautement organises au moyen de procedes sol-gel Withdrawn EP1534631A1 (fr)

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EP20060017325 EP1757662A3 (fr) 2002-09-07 2003-08-22 Procédé de production de cristaux hautement organisés au moyen de procédé sol-gel

Applications Claiming Priority (15)

Application Number Priority Date Filing Date Title
DE2002141494 DE10241494A1 (de) 2002-09-07 2002-09-07 Verfahren zur Herstellung von hochorganisierten Kristallen mit Hilfe von Sol-Gel-Methoden
DE10241494 2002-09-07
DE20311943U 2003-08-02
DE20311942U DE20311942U1 (de) 2002-09-07 2003-08-02 Poröse Materialien für die Blockung von IR-Strahlung
DE20311939U 2003-08-02
DE20311944U DE20311944U1 (de) 2002-09-07 2003-08-02 Farbeffekt-Schichten und -Beschichtungen auf Basis photonischer Kristalle
DE20311944U 2003-08-02
DE20311940U 2003-08-02
DE20311937U DE20311937U1 (de) 2002-09-07 2003-08-02 Poröse Materialien für die Reinigung und Aufbereitung von Wasser
DE20311943U DE20311943U1 (de) 2002-09-07 2003-08-02 Poröse Materialien für die Blockung von UV-Strahlung
DE20311939U DE20311939U1 (de) 2002-09-07 2003-08-02 Poröse Materialien als Katalysatorträger in chemischen und verfahrenstechnischen Anwendungen
DE20311937U 2003-08-02
DE20311940U DE20311940U1 (de) 2002-09-07 2003-08-02 Poroese Materialien zur Immobilisierung von Bakterien
DE20311942U 2003-08-02
PCT/EP2003/009335 WO2004024627A1 (fr) 2002-09-07 2003-08-22 Procede de production de cristaux hautement organises au moyen de procedes sol-gel

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US7482610B2 (en) * 2005-01-13 2009-01-27 Massachusetts Institute Of Technology Vertical-cavity enhanced resonant thermal emitter
US8277943B2 (en) 2005-10-05 2012-10-02 Certainteed Corporation Thin films with high near-infrared reflectivity deposited on building materials
EP1827674B1 (fr) * 2005-11-08 2012-09-12 LG Chem, Ltd. Cristaux photoniques colloïdaux utilisant des nanoparticules colloïdales et procédé pour la préparation de ceux-ci
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