WO2004113222A1 - Procede pour stocker de maniere reversible de l'hydrogene atomique sur/dans un micromateriau et/ou un nanomateriau carbone, et dispositif de stockage d'hydrogene - Google Patents

Procede pour stocker de maniere reversible de l'hydrogene atomique sur/dans un micromateriau et/ou un nanomateriau carbone, et dispositif de stockage d'hydrogene Download PDF

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Publication number
WO2004113222A1
WO2004113222A1 PCT/DE2004/001190 DE2004001190W WO2004113222A1 WO 2004113222 A1 WO2004113222 A1 WO 2004113222A1 DE 2004001190 W DE2004001190 W DE 2004001190W WO 2004113222 A1 WO2004113222 A1 WO 2004113222A1
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WO
WIPO (PCT)
Prior art keywords
nanomaterial
hydrogen
atomic hydrogen
carbon
storage
Prior art date
Application number
PCT/DE2004/001190
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German (de)
English (en)
Inventor
Thomas Zecho
Original Assignee
Future Camp Gmbh
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from DE10347237A external-priority patent/DE10347237A1/de
Application filed by Future Camp Gmbh filed Critical Future Camp Gmbh
Priority to EP04738642A priority Critical patent/EP1644283A1/fr
Publication of WO2004113222A1 publication Critical patent/WO2004113222A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
    • C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
    • C01B3/0021—Carbon, e.g. active carbon, carbon nanotubes, fullerenes; Treatment thereof
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

Definitions

  • the present invention first relates to a method for the reversible storage of atomic hydrogen on / in carbon micro- and / or nanomaterial.
  • the invention further relates to a corresponding hydrogen storage.
  • the present invention consequently relates to the technical field of hydrogen storage, which has recently gained considerably in importance.
  • Hydrogen is regarded as a zero-emission fuel (with regard to emissions of toxic or climate-influencing process gases) because only water is generated when it is used, for example in thermal internal combustion engines, in fuel cell applications or the like. Consequently, the creation of suitable storage means for the efficient storage of hydrogen is an important goal which must be achieved before widespread use of hydrogen as a fuel can occur.
  • molecular hydrogen (H 2 ) on carbon nanomaterial can be reversibly stored in the form of so-called single-walled nanotube material (SWNT material).
  • “reversible” means that the hydrogen molecules can be attached to the carbon nanomaterial, that is to say stored, but that the hydrogen molecules can also be detached and released from the carbon nanomaterial.
  • the known solution provides that that the molecular hydrogen attach to the surfaces of the SWNT material that means can adsorb, and that this is released again at certain temperature conditions, that is, desorbed.
  • Hydrogen storage in carbon nanotubes (carbon nanotubes) with molecular hydrogen as the medium to be stored comprises the steps that suitable carbon nanomaterial must first be produced and cleaned, that the carbon nanomaterial is subsequently exposed to molecular hydrogen at or above atmospheric pressure, that the external hydrogen pressure is increased and that the stored hydrogen molecules have to be kept in the carbon nanomaterial.
  • the carbon nanomaterial is heated to an elevated temperature, the so-called desorption temperature.
  • a disadvantage of the known solution is, inter alia, that because of the low bond strength between the hydrogen molecules and the carbon nanomaterial, only a limited amount of hydrogen molecules can be stored in / on the carbon nanomaterial under normal ambient conditions. In addition, the bond strength between the hydrogen molecules and the carbon nanomaterial in the storage state is relatively low.
  • the present invention is based on the object of providing a method for the reversible storage of hydrogen on / in carbon micro- and / or nanomaterial and a hydrogen storage device with which the disadvantages described can be avoided.
  • the present invention is based on the knowledge that it is no longer molecular hydrogen (H 2 ) but atomic hydrogen (H) that is stored on / in the carbon micro- and / or nanomaterial.
  • the storage of hydrogen is according to the generation of atomic hydrogen
  • the bond strength between the hydrogen atoms and carbon atoms is high, so that the hydrogen is stored stably in the carbon micro- and / or nanomaterial under normal ambient conditions and beyond up to the desorption temperature.
  • a method for the reversible storage of atomic hydrogen on / in carbon micro- and / or - nanomaterial is provided, which is characterized by the following steps:
  • a) for storing atomic hydrogen attaching the atomic hydrogen to the carbon micro- and / or - nanomaterial by means of adsorption, in particular by means of chemisorption;
  • the method according to the invention initially provides that the atomic hydrogen is to be reversibly stored on / in the carbon micro- and / or nanomaterial.
  • the carbon can both be attached to the carbon micro- and / or nanomaterial, that is, stored, and detached from the carbon micro- and / or nanomaterial, that is, removed.
  • Carbon micromaterial is a material that has particles whose dimensions are in the range of micrometers.
  • Carbon nanomaterial is a material that has particles whose dimensions are in the range of nanometers.
  • atomic hydrogen is deposited on the carbon micro- and / or nanomaterial, which takes place according to the invention by means of adsorption, in particular by means of chemisorption.
  • Adsorption generally means the accumulation of gases or solutes at the interface of a solid or liquid phase.
  • Chemisorption is a special case of adsorption, in which the adsorbed atoms are held on the surface of a solid, here the carbon micro- and / or nanomaterial, by chemical bonds.
  • atomic hydrogen is generated from molecular hydrogen using energy.
  • the carbon micro and / or nanomaterial is heated to a certain temperature, the so-called desprotion temperature, for the purpose of thermal desorption, so that the stored atomic hydrogen is separated from the carbon micro and / or or nanomaterial.
  • Desorption is generally the back reaction of the Adsorption / chemisorption, but usually with a much higher activation energy.
  • the carbon micro and / or -Nanomaterial consequently heated to at least the desorption temperature at which the atomic hydrogen can be recovered.
  • the hydrogen atoms detach from the carbon micro- and / or nanomaterial, that is, they are released, and then recombine to form hydrogen molecules (H 2 ).
  • energy is released which can be used further, in particular for increasing the temperature of the storage medium itself. This will be discussed in more detail later in the description.
  • the present invention is based on the knowledge that hydrogen atoms can be adsorbed / chemisorbed on the surfaces of carbon micro- and / or nanomaterials. Hydrogen remains adsorbed on the surfaces of the carbon micro- and / or nanomaterials up to the desorption temperature. By heating the hydrogen-coated / coated carbon micro- and / or nanomaterials to elevated temperatures greater than / equal to the desorption temperature, atomic hydrogen can be recovered and recombined to molecular hydrogen.
  • the method for the reversible storage of atomic hydrogen is in the form of hydrogen atoms (H) and / or deuterium atoms (D).
  • the method can preferably be used to store atomic hydrogen on the carbon micro- and / or nanomaterial with a maximum storage capacity of one hydrogen atom per carbon atom, equivalent to 8% by weight.
  • the present invention is not restricted to certain types of carbon nanomaterials.
  • the method can be used for the reversible storage of atomic hydrogen on / in carbon nanomaterial in the form of nanotubes, in particular single-walled nanotubes (SWNT) or multi-walled nanotubes (MWNT) and / or nanofibers (nanofibers). and / or nanoshells (nanoscale) can be used.
  • the carbon nanomaterial can be in the form of a powder, for example.
  • the method for the reversible storage of atomic hydrogen on / in carbon micro- and / or nanomaterial in the form of oriented carbon micro- and / or nanomaterial can advantageously be used.
  • the carbon micro- and / or nanomaterials can have a directional structure.
  • the carbon micro- and / or nanomaterials are helical.
  • This helical structure can be described, for example, in the form of a “spiral staircase”.
  • the helical nanostructures can advantageously be designed as helical carbon nanofibers, which thus initially have an outer structure in the longitudinal direction in the form of the helical line and additionally an inner structure
  • Inner structure which in the exemplary example of the "spiral staircase" would form the individual "stair steps"
  • Such a structure has considerable advantages because of its many edges.
  • the atomic hydrogen can first be generated in at least one atomic source.
  • the atomic hydrogen produced can be thermal (2000 K) hydrogen.
  • the atomic hydrogen is generated in at least one atom source known as a plasma source.
  • Suitable plasma sources include, for example, low temperature DC (low temperature DC), microwave, HF plasma sources and the like.
  • the atomic hydrogen is generated in an atom source designed as a particularly heated tungsten capillary.
  • molecular hydrogen flows through it, whereby the molecular hydrogen is split into atomic hydrogen.
  • the carbon micro- and / or nanomaterial for depositing atomic hydrogen is exposed to a stream of gaseous atomic hydrogen.
  • the carbon micro- and / or nanomaterial is bombarded with hydrogen atoms, which then attach to the carbon micro- and / or nanomaterial.
  • the carbon micro- and / or nanomaterial for depositing atomic hydrogen is immersed in the at least one atom source.
  • a metal is applied to the carbon material and that the atomic hydrogen bound to the metal, for example by dissociative adsorption of molecular Hydrogen according to H 2 + 2 * metal ⁇ 2 ⁇ metal
  • the atomic hydrogen can preferably be adsorbed on the carbon micro- and / or nanomaterial at a temperature between 150 and 300 K, in particular at a temperature around 200 K.
  • the atomic hydrogen is recombined into hydrogen molecules after the desorption step. It is advantageously provided that the desorbed atomic hydrogen is recombined in the gas phase.
  • the carbon micro- and / or nanomaterial is advantageously heated to temperatures above 350 K, in particular to temperatures in the range from 350 to 1000 K, preferably to a range from 750 to 800 K.
  • the hydrogen atoms first detach from the carbon micro and / or nanomaterial.
  • the hydrogen atoms recombine to form hydrogen molecules at these temperatures.
  • This reaction releases energy.
  • the energy released in the recombination of the atomic hydrogen can advantageously be made available to further processes or process steps.
  • a hydrogen storage for the reversible storage of atomic hydrogen comprising a storage medium for storing the atomic hydrogen.
  • this hydrogen storage device is characterized in that the storage medium is in the form of carbon micro- and / or nanomaterial.
  • the storage medium is arranged in a pressure container. This ensures particularly safe storage of hydrogen.
  • a solid filling can be formed from the storage medium in a storage container, but at least the storage medium can be part of such a filling.
  • the storage medium can be in any form, for example in the form of powder and / or conglomerates and / or pellets or the like.
  • the carbon micro- and / or nanomaterial can therefore preferably be in the form of conglomerates, the invention not being restricted to certain forms of conglomerates.
  • the conglomerates can be, for example, bundles of carbon micro- and / or nanomaterial, as described, for example, in the already mentioned WO 01/53199 A2, the disclosure content of which is included in the present description.
  • An increase in the storage capacity for the gas can also be generated if the carbon micro- and / or nanomaterials are designed as coherent conglomerates. As a result, more material can be introduced into a given storage volume of a storage container than would be possible by simply filling in carbon particles with a micro- and / or nanostructure.
  • At least individual conglomerates are advantageously compressed with an apparent density higher than the apparent density of the originally loose carbon micro- and / or nanomaterials.
  • the apparent density refers to the weight based on the volume of the conglomerate.
  • the apparent density of the conglomerates produced from the originally loose particles of the carbon micro- and / or nanomaterial can advantageously be increased to at least 1.5 times, preferably at least to twice the original apparent density.
  • the original apparent density is approximately 1.0 g / cm 3 , so that the values to be aimed for in the compression are preferably at minimum densities of 1.5 and 2.0 g / cm 3 .
  • a further advantage is associated by densifying the carbon micro- and / or nanomaterials. This consists in that the individual particles are inevitably held together, so that when the storage container is unloaded, an undesired discharge of the smallest particles with the gas stream removed is counteracted. The escape of particles into downstream aggregates or the environment could, under certain circumstances, lead to technical problems or violate emission regulations with regard to very small particles.
  • the storage medium is advantageous in the form of carbon nanomaterials in the form of nanotubes, in particular single-walled nanotubes (SWNT) or multi-walled nanotubes (MWNT) and / or nanofibers and / or Nanoshells and / or oriented carbon nanomaterial.
  • SWNT single-walled nanotubes
  • MWNT multi-walled nanotubes
  • the storage medium can also be in the form of carbon micromaterials, which can advantageously also have a shape as described above.
  • a carbon micromaterial and / or a carbon nanomaterial in particular in the form of nanotubes, in particular single-walled nanotubes (SWNT) or multi-walled nanotubes (MWNT) and / or nanofibers and / or nanoshells and / or oriented carbon nanomaterial can be used as a storage medium for atomic hydrogen.
  • SWNT single-walled nanotubes
  • MWNT multi-walled nanotubes
  • nanofibers and / or nanoshells and / or oriented carbon nanomaterial can be used as a storage medium for atomic hydrogen.
  • Micromaterials and / or nanomaterials are coated with chemisorbed atomic hydrogen H (deuterium D)
  • Micromaterials and / or nanomaterials for example multi-walled carbon nanotubes - MWNT) with diameters, set according to a preferred bonding strength between the surface (tube surfaces) atoms and the chemisorbed atoms which are chemisorbed with atomic hydrogen H (deuterium D) are coated.
  • H or D coated micromaterials and / or nanomaterials such as SWNT, MWNT or the like
  • the micromaterials and / or nanomaterials being exposed to currents of H or D atoms on a suitable substrate.
  • H or D coated micromaterials and / or nanomaterials such as SWNT, MWNT or the like
  • the micromaterials and / or nanomaterials on a suitable substrate are exposed to streams of H or D atoms, the streams being in a suitable low temperature DC -, microwave - or HF plasma were generated.
  • Low temperature DC, microwave or HF plasma can be immersed.
  • H or D coated micromaterials and / or nanomaterials such as SWNT, MWNT or the like
  • the micromaterials and / or nanomaterials being used as a hydrogen electrode in an electrochemical cell.
  • H or D coated micromaterials and / or nanomaterials such as SWNT, MWNT or the like
  • metal is deposited / deposited on the micromaterials and / or nanomaterials and the so-called "spill-over phenomenon" (overflow phenomenon) is used to transfer H or D, which is dissociatively adsorbed on the metal component, to the surface of the micromaterials and / or nanomaterials.
  • Figures 1 to 5 each show diagrams in which results of different spectroscopy measurements are shown.
  • carbon nanomaterial in the form of single-walled carbon nanotubes was applied to a pyrolytic graphite sample (hereinafter referred to as the NT sample).
  • the NT sample was used as a substrate for the interaction with thermal hydrogen atoms.
  • the SWNT material had a purity of approximately 85 wt% (weight percent), the diameter of the nanotubes was between 1.2 to 1.4 nm, and their length was in the ⁇ m to a few 10 ⁇ m range.
  • the main contaminants are small amounts of nickel and cobalt catalyst particles.
  • the carbon nanomaterial showed a bundle structure. The purity was confirmed by EDX (in situ) and Auger electron spectroscopy (in situ) measurements, the results of which are shown in FIG. 1.
  • Electron loss spectra which detect the surface electron density by the ⁇ -plasmon excitation in the substrate, are in FIG. 3 for pure and D (deuterium) coated HOPG (FIG. 3a) and NT sample surfaces ( Figure 3b).
  • the decrease in the plasmon loss peak represents the formation of chemical C-D bonds on the sample surfaces.
  • Vibrational spectra which were obtained by means of high-resolution electron-energy loss spectroscopy (HREELS), are shown in FIG.
  • the HREELS spectrum of pure HOPG shows the graphite surface phonon losses (FIG. 4a).
  • the HREELS spectrum of HOPG covered with hydrogen additionally shows the losses caused by normal and parallel oscillations (vibrations) of Originate chemisorbed hydrogen on HOPG ( Figure 4b).
  • the HREELS spectrum of HOPG covered with D additionally shows the losses which result from normal and parallel oscillations (vibrations) of chemisorbed D onto HOPG (FIG. 4c).
  • the HREELS spectrum of pure NT sample surfaces shows only a broad background (FIG. 5a).
  • the HREELS spectra measured on H or D coated NT samples show the normal vibrations of H or D adsorbed on the nanotubes in the NT sample, and the respective parallel vibration of H.
  • H and D atoms adsorb on the surfaces of SWNTs.
  • the measured spectra reveal recombinant molecular H 2 (D 2 ) and atomic H (D) desorption between 350 K (400 K) and 950 K (1000 K), with a main peak at about 760 K (790 K).
  • the CH (D) bond strength is greater than that seen on the flat (0001) surfaces of graphite.

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  • Nanotechnology (AREA)
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  • Organic Chemistry (AREA)
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  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
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  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
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Abstract

L'invention concerne un procédé pour stocker de manière réversible de l'hydrogène atomique sur/dans un micromatériau et/ou un nanomatériau carboné, ainsi qu'un dispositif de stockage d'hydrogène. Le procédé selon l'invention est caractérisé par les étapes suivantes : a) stockage de l'hydrogène par accumulation de l'hydrogène atomique sur le micromatériau et/ou le nanomatériau carboné, notamment par chimisorption; b) libération de l'hydrogène atomique par chauffage du micromatériau et/ou du nanomatériau carboné pour réaliser une désorption thermique à une température de désorption déterminée, de sorte que l'hydrogène atomique se désolidarise du micromatériau et/ou du nanomatériau carboné, puis par recombinaison de l'hydrogène atomique libéré en molécules d'hydrogène.
PCT/DE2004/001190 2003-06-17 2004-06-09 Procede pour stocker de maniere reversible de l'hydrogene atomique sur/dans un micromateriau et/ou un nanomateriau carbone, et dispositif de stockage d'hydrogene WO2004113222A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
EP04738642A EP1644283A1 (fr) 2003-06-17 2004-06-09 Procede pour stocker de maniere reversible de l'hydrogene atomique sur/dans un micromateriau et/ou un nanomateriau carbone, et dispositif de stockage d'hydrogene

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
DE10327243.7 2003-06-17
DE10327243 2003-06-17
DE10347237A DE10347237A1 (de) 2003-06-17 2003-10-10 Verfahren zum reversiblen Speichern von atomarem Wasserstoff an/in Kohlenstoff-Mikro- und/oder -Nanomaterial sowie Wasserstoffspeicher
DE10347237.1 2003-10-10

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102018219720A1 (de) 2018-11-16 2020-05-20 Technische Universität Clausthal Verfahren und Vorrichtung zur Beladung von Wasserstoff-speichernden Feststoffen

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DE19757851C1 (de) * 1997-12-24 1999-04-29 Univ Bayreuth Vorrichtung zur Erzeugung von Radikalen und/oder Reaktionsprodukten
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WO2001053199A2 (fr) * 2000-01-19 2001-07-26 Midwest Research Institute Nanotubes de carbone a paroi simple pour stockage de l'hydrogene ou formation de superamas
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EP0025858A1 (fr) * 1979-09-18 1981-04-01 International Business Machines Corporation Matériel de fixation réversible pour hydrogène gazeux
DE19757851C1 (de) * 1997-12-24 1999-04-29 Univ Bayreuth Vorrichtung zur Erzeugung von Radikalen und/oder Reaktionsprodukten
US6159538A (en) * 1999-06-15 2000-12-12 Rodriguez; Nelly M. Method for introducing hydrogen into layered nanostructures
WO2001053199A2 (fr) * 2000-01-19 2001-07-26 Midwest Research Institute Nanotubes de carbone a paroi simple pour stockage de l'hydrogene ou formation de superamas
EP1209119A2 (fr) * 2000-11-22 2002-05-29 Air Products And Chemicals, Inc. Stockage d'hydrogène utilisant un composé hybride de carbone-métal
CA2459081A1 (fr) * 2001-09-11 2003-04-10 Sony Corporation Materiau d'occlusion de substance, dispositif electrochimique utilisant ce materiau et procede de production de ce materiau d'occlusion de substance

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102018219720A1 (de) 2018-11-16 2020-05-20 Technische Universität Clausthal Verfahren und Vorrichtung zur Beladung von Wasserstoff-speichernden Feststoffen
DE102018219720B4 (de) 2018-11-16 2023-03-16 Technische Universität Clausthal Verfahren und Vorrichtung zur Beladung von Wasserstoff in Wasserstoff-speichernden Feststoffen und Vorrichtung zum reversiblen Speichern von Wasserstoff

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