WO2009015654A1 - Composant poreux monolithique constitué de nanotubes sensiblement parallèles, procédé pour le fabriquer et son utilisation - Google Patents

Composant poreux monolithique constitué de nanotubes sensiblement parallèles, procédé pour le fabriquer et son utilisation Download PDF

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Publication number
WO2009015654A1
WO2009015654A1 PCT/DE2008/001250 DE2008001250W WO2009015654A1 WO 2009015654 A1 WO2009015654 A1 WO 2009015654A1 DE 2008001250 W DE2008001250 W DE 2008001250W WO 2009015654 A1 WO2009015654 A1 WO 2009015654A1
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Prior art keywords
template
monolithic
porous
tubes
pores
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PCT/DE2008/001250
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German (de)
English (en)
Inventor
Jörg Schneider
Alexander Popp
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Technische Universität Darmstadt
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Publication of WO2009015654A1 publication Critical patent/WO2009015654A1/fr

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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/2485—Monolithic reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00033—Continuous processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
    • B01J2219/00027—Process aspects
    • B01J2219/00036—Intermittent processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00788—Three-dimensional assemblies, i.e. the reactor comprising a form other than a stack of plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00822—Metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00824—Ceramic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00824—Ceramic
    • B01J2219/00826—Quartz
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00835—Comprising catalytically active material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00844—Comprising porous material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00846—Materials of construction comprising nanostructures, e.g. nanotubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/00864—Channel sizes in the nanometer range, e.g. nanoreactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange

Definitions

  • a monolithic porous member of substantially parallel nanotubes method of making and using same
  • the present invention relates to a monolithic, porous member of substantially parallel nanotubes, a method for its production and uses thereof.
  • Reactors for chemical synthesis, structured on a micrometer scale, are known as microreactors. They have been increasingly used in process development and optimization in recent years and are gaining more and more industrial interest. Such reactors are characterized by three-dimensional reaction spaces, which represent a container of only a few milliliters in volume and below. These reaction spaces, which have hitherto been produced mainly by various lithography and etching methods, usually have channels in the order of several micrometers, through which a fluid flows and in which a reaction takes place. Numerous reaction types - catalyzed and non-catalyzed, single- or multi-phase - have been realized in microreactors to date. In addition, there is enormous potential for bioprocess engineering using microorganisms and cells as biocatalysts.
  • the ratio of surface to volume is a key parameter and has a size of about 1,000 m 2 / m 3 in conventional industrial reactors, with microstructured Realctoren an increase in a range of 10,000 to 50,000 m 2 / m 3 is possible.
  • microreactors are known in the art, in whose channels nanotubes are generated. These nanotubes are typically in the range between about 10-200 nm in diameter. They offer the advantage of increasing the inner surface of the reaction space in order to apply catalyst particles therein and to allow better heat supply and removal, with simultaneously increased mass transfer. However, these have not been aligned very parallel to each other, have varying lengths in diameter and have material-side differences from the reactor material, which may be disadvantageous for the purposes of such microreactors.
  • the ratio of surface to volume should be significantly increased.
  • a further object of the invention is to provide a method for producing such a component and to identify possible uses.
  • the object is achieved by a method for producing a monolithic, porous member from substantially parallel nanotubes with a diameter in the range of 1 to 1000 nm, comprising the steps of: (i) providing a substantially parallel pore-containing template material; (ii) depositing at least one solid in the pores to form tubes and outer surfaces of the template at least substantially perpendicular to the pores to form cover layers, the solid being formed from an atomic / molecular precursor; (iii) optionally shaping the template coated in step (ii) to a predetermined shape and size; and (iv) removing the template.
  • the removal of the template by etching with bases or acids, preferably hydrofluoric acid, is performed.
  • the template material is selected from alumina, titania, silica, silica, and Group 12/16 compound semiconductors of the periodic table, such as CdS, CdSe, and CdTe.
  • the solid to be deposited is selected from carbon, metals, elements of groups 13-16 of the periodic table, polymers and combinations of said substances, optionally with the addition of hydrogen. Combinations with hydrogen allow hydrocarbons and polymers.
  • the solid is precipitated from the gas phase or condensed phase.
  • the deposition by chemical vapor deposition (CVD), metal evaporation, via polymers, sol-gel process or electrochemical deposition takes place.
  • CVD chemical vapor deposition
  • the deposition via sol-gel processes or polymers has already been described many times and should therefore be well known to the person skilled in the art, see, for example, CJ. Brinker and G.W. Scherer, "Sol-Gel Science - The Physics and Chemistry of Sol-Gel Processing", Academic Press, New York, 1990; Lu & Schüth, “Nanocasting: A Versatile Strategy for Creating Nanostructured Porous Materials” Adv.Matr. 2006, 18, 1793-1805.
  • Electrochemical deposition is described, for example, by C. Martin, Chem. Mater 1996, 8, 1739-1746.
  • a flow carrying the solids to be deposited is substantially parallel to the longitudinal axis of the pores of the template. The parallel flow is particularly important for vapor phase deposition processes (such as CVD processes), but of less importance for liquid phase depositions (such as sol-gel processes) or electrochemical deposition.
  • the template is heated in step (ii), preferably to a temperature of 700 to 1000 ° C.
  • cover layers and nanotubes be produced in one step.
  • a plurality of outer surfaces of the template can be coated with at least one solid to form a cover layer shell.
  • the coating of the outer surfaces can also be made variable. For example, the coating of two opposite side surfaces may be useful. The coating of all outer surfaces would close the reaction space.
  • the removal of the template is preferably carried out by etching with acid.
  • the etching is usually carried out with the aid of hydrofluoric acid (HF).
  • HF hydrofluoric acid
  • other mineral acids e.g. Phosphoric acid
  • bases such as KOH or NaOH may also be used.
  • the interior of the tubes is open to the outside surface. It is also proposed that the tubes of the component be filled, preferably with a compact or other porous material.
  • the interior of the tubes is completely filled.
  • the filling material may also be porous. It is therefore also proposed that the pores of the component are preferably filled with a compact or other porous material.
  • the component preferably has a surface to volume ratio of 50,000 to 100,000,000 m 2 / m 3 , preferably 500,000 to 10,000,000 m 2 / m 3 .
  • Tubes and cover layers can be constructed of similar or different materials.
  • the entire outer surface is provided with the cover layer.
  • the outer surface can be selectively removed again in defined areas.
  • the monolithic, porous component has a length and / or width of 0.1 mm to 5 cm and a thickness of 1 .mu.m to 1 mm.
  • the component according to the invention can absorb substances or be flowed through by them.
  • the component according to the invention can therefore be used as a flow or reaction space, wherein deposited cover surfaces limit the flow spatially. Therefore, a continuous or discontinuous operation of the component according to the invention is particularly preferably possible.
  • the use may be provided as a nanoreactor, sensor, heat exchanger or a combination thereof. It should be emphasized that when using the inventive component of the previously filled with template space and not the interior of the nanotubes is flowed through.
  • a flow guidance is made possible in which the flow runs perpendicular to the tube axes of the component and the individual tubes of the component flow around the outside. Due to the generated cover layers, the flow can also be limited in space.
  • the use as a component with system and integration reference can be provided to provide an interface between typical dimensions of nanotechnology and those of microstructure technology.
  • the structure of the device has a high degree of order since the nanotubes can be made very straight by the template. Furthermore, the nanotubes have a defined length, since the length of the nanotubes is determined by the thickness of the template and is uniform.
  • the outer diameter of the nanotubes produced in the component corresponds to the pore diameter of the template, the inner diameter of the tubes can be easily varied over the deposition time, so that defined diameter and wall thicknesses are adjustable. Also, the so-called aspect ratio, d. H. the ratio of length to diameter, very well adjustable.
  • a scale-spanning nano-macro-macro transition can be achieved and ensured from substantially macroscopically arranged parallel nanotubes.
  • Particularly preferred can be provided for use of the component with system and integration reference to create a Thomas Abbott between nanotechnology and microstructure technology. This may be provided in particular in the form of a sensor, heat soak, chemical reactor or a combination thereof.
  • the nanotubes end in an at least upper and lower cover layer, which extend substantially perpendicular to the longitudinal axis of the tubes. This makes possible a three-dimensional arrangement of the tubes, holds the tubes together and also offers a contacting possibility through the two cover layers. Furthermore, by providing the cover layers, the tubes can be handled well and flow within the component can be limited by the cover layers.
  • the degree of graphitization of the carbon via the temperature control during deposition is adjustable, which can control additional later functionalization of the formed tubes. Furthermore, the degree of graphitization can be changed even after deposition by temperature treatment.
  • the arrangement of the tubes and their distances are adjustable via the shape of the template, in particular its porosity.
  • impurities by catalyst particles do not occur in the deposited tubes when they are produced by non-catalytic gas phase deposition processes.
  • the tubes can be made open on both sides, so that the interior of the tubes is accessible after the manufacture of the component. Also tubes and cover layers can be made of the same material or of different materials.
  • Figures 1.1-1.3 show sectional views of a porous template or component according to the invention during the manufacturing process
  • FIG. 2.1-2.2 show further sectional views through a porous template and components according to the invention.
  • FIG. 3 shows a scanning electron micrograph of a component according to the invention.
  • the process according to the invention can be carried out in a reactor as follows:
  • the reactor head consists of two nested carbon parts, which can be heated by induction.
  • a feed gas carrier gas and gas containing the solids intended for separation
  • a disk-shaped membrane of alumina which serves as a template for the production of the inventive component.
  • the disk is arranged so that the gas flow impinges substantially perpendicular to the flat disk surface.
  • Excess gas species are extracted by a pump.
  • the reactor has the peculiarity that, as already stated, the flow is perpendicular to the membrane surface, ie the flow is guided in the same direction as the longitudinal axis of the pores of the template. Furthermore, high temperatures occur only locally, since the membrane rests directly on the heated carbon elements of the reactor head. Temporally different temperature profiles can be represented by the induction heating used.
  • the entire surface of the component is provided with a cover layer. In this case, in the production process, the upper and lower outer layers and, in a further working step, the lateral outer layers to be brought. Further, the materials of the top, bottom and side cover layers may be different.
  • Porous alumina is preferably used as a template, which is characterized by its cylindrical pores with a narrow pore distribution.
  • the solid on the template Before or after the deposition of the solid on the template, it may be sized and shaped by suitable means (e.g., laser or plasma techniques). Subsequently, further solids can be applied to the template brought into the desired shape. Subsequently, the original template is made accessible by removing the deposited solids at least at one point and removing the template via this opening, which can be achieved, for example, by etching with acid or alkali.
  • suitable means e.g., laser or plasma techniques.
  • the provided opening (s) may or may later serve for introducing or removing the substances intended to receive the component according to the invention or through which the component according to the invention is intended to flow.
  • the template may be brought by suitable • designated agent in a desired size and shape before separation of the solid and the solids are then deposited. Subsequently, the deposited cover layer must also be removed at least one location in order to make accessible and remove the original template. Finally, the outer surface of the generated tubes can be further functionalized (eg, coating with catalysts) to promote reactions of molecules or species of interest to flow through the device with the higher surface area.
  • Figure 1.1 shows a sectional view through a porous template 1, which has a plurality of continuous pores 2.
  • the porous template 1 has been coated with a cover layer 3, while in FIG. 1.3, the porous template 1 has been removed by etching.
  • the individual tubes are connected via a cover layer.
  • Figure 2.1 shows a further schematic sectional view, starting from a porous template 1 with continuous pores 2.
  • Figure 2.2 shows on the left side parallel tubes, which are interconnected by an upper cover layer 4 and a lower cover layer 5 and closed to the outer surface. In an alternative embodiment shown on the right, it is possible that the pores of the template are completely filled by deposited solid 6.
  • FIG. 3 shows a scanning electron micrograph of a component according to the invention, from which upper and lower cover layers as well as, substantially parallel tubes disposed therebetween can be clearly seen.
  • the erf ⁇ ndungshiele component can be used for example as a nanostructured micro-reactor, wherein reactant species can be introduced to the target of a chemical reaction in the component, as it is implemented in a known microreactor comparable.
  • Such nanostructured microreactors are particularly suitable for reactions with a high risk potential, for example highly exothermic or very toxic substances. of equipment already in operation or for screening functions, for example for catalysts or in the pharmaceutical industry.
  • the inventive component can be used, for example, as a nano-microstructure integrated reactor, wherein one or more reactant species are introduced into the component, the aim of a reaction of these species with each other, on the surface of the (possibly functionalized) tubes or a combination thereof.
  • An integrated reaction monitoring of microreactors is usually carried out by means of UV / VIS, IR 5 NMR, MS and LC / MS.
  • the component according to the invention offers an observation of the processes taking place in the component, in which a contacting of the upper and lower cover layer is carried out simultaneously.
  • the lateral cover layers must be removed or consist of different materials compared to the contacted cover layers.
  • a measurement of the running processes then takes place exclusively over the tubes of the component, e.g. by a time resolved view of the electrical resistance / conductance.
  • the component is also intended for use as a chemical sensor for gases or condensed phase reactants.
  • Screening functions for example, for catalysts or in the pharmaceutical industry or for the detection of biomolecules, for example via the key-lock principle by molecules applied to the tube surface, which favor a preferred docking of specific species from the fluid space.
  • Another use is as a heat exchanger.
  • the component according to the invention can be used for heat supply and removal since the heat transfer coefficient is inversely proportional to the dimensions of the structure of the heat exchanger.
  • the component according to the invention for example as a sensor is possible.
  • the component can be used as a sensor for characterization purposes.
  • a need for such chemical sensors is required, inter alia, for environmental observations, for the control of chemical processes and for agricultural and medical applications.
  • carbon tubes as a sensor element, show an increased sensitivity and a faster system response compared to conventional solid-state sensors.
  • the molecules to be studied absorb on the carbon nanotube wall and cause a strong, molecule-specific change in the electrical conductivity of the carbon structure, which can be measured.
  • the component according to the invention makes it possible, in particular, to achieve extremely precise positioning of the carbon nanotubes and easy contacting of the tubes over the cover layers, which has hitherto been technically extremely problematic and has hitherto largely prevented economical use of such components.
  • a reaction can take place within the component and at the same time the heat can be dissipated. Furthermore, a reaction can take place and be characterized simultaneously. In addition, a parallel connection and / or series connection of several Funitechnischsakuen is possible.
  • the component according to the invention is characterized by a special compactness by its nano-microstructured construction and thus also a possibility of a simple, scale-spanning system integration and significantly improved structural properties by the special arrangement of the nanotubes in the component and their direct connection with the cover layer. This also allows improved properties for handling and assembly techniques of such a nano-microstructure integrated component.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'un composant poreux monolithique constitué de nanotubes sensiblement parallèles ayant un diamètre dans la plage de 1 à 1000 nm, comprenant les étapes consistant à : (i) préparer un matériau de matrice présentant des pores sensiblement parallèles ; (ii) déposer au moins un solide dans les pores afin de former des tubes et au moins sur les surfaces extérieures de la matrice qui s'étendent sensiblement perpendiculairement aux pores afin de former des couches de couverture, le solide étant généré à partir d'un précurseur atomique/ moléculaire ; (iii) le cas échéant, façonner la matrice revêtue à l'étape (ii) à une forme et une taille prédéterminées ; et (iv) éliminer la matrice.
PCT/DE2008/001250 2007-07-30 2008-07-28 Composant poreux monolithique constitué de nanotubes sensiblement parallèles, procédé pour le fabriquer et son utilisation WO2009015654A1 (fr)

Applications Claiming Priority (2)

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DE102007035693.7 2007-07-30
DE200710035693 DE102007035693A1 (de) 2007-07-30 2007-07-30 Monolithisches, poröses Bauteil aus im wesentlichen parallelen Nanoröhren, Verfahren zu dessen Herstellung und Verwendung desselben

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DE102009056296A1 (de) 2009-11-30 2011-06-09 Günther Battenberg Sensor für die mechanische Druckmessung an Oberflächen
DE102009056072A1 (de) 2009-11-30 2011-06-01 Technische Universität Darmstadt Verfahren und Stoffgemische zur Herstellung von metallischen bzw. metalloxidischen Schichten

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WO2003050854A2 (fr) * 2001-12-12 2003-06-19 The Pennsylvania State University Gabarits de reacteur chimique: fabrication de couche sacrificielle et utilisation de gabarits

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WO2002043937A2 (fr) * 2000-12-02 2002-06-06 Aquamarijn Holding B.V. Procede de fabrication de produit a l'aide d'une micro- ou nano- structure et produit obtenu
WO2003050854A2 (fr) * 2001-12-12 2003-06-19 The Pennsylvania State University Gabarits de reacteur chimique: fabrication de couche sacrificielle et utilisation de gabarits

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A. TAGUCHI ET AL.: "Carbon Monoliths Possessing a Hierarchical, Fully Interconnected Porosity", ADVANCED MATERIALS, vol. 15, no. 14, 17 July 2003 (2003-07-17), pages 1209 - 1211, XP002506626 *
B-.H. HAN ET AL.: "Direct Preparation of Nanoporous Carbon by Nanocasting", JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, vol. 2003, no. 125, 3 April 2003 (2003-04-03), pages 3444 - 3445, XP002506638 *
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