WO2003053848A1 - Reversible speicherung von wasserstoff mit hilfe von dotierten alkalimetallaluminiumhydriden - Google Patents
Reversible speicherung von wasserstoff mit hilfe von dotierten alkalimetallaluminiumhydriden Download PDFInfo
- Publication number
- WO2003053848A1 WO2003053848A1 PCT/EP2002/014383 EP0214383W WO03053848A1 WO 2003053848 A1 WO2003053848 A1 WO 2003053848A1 EP 0214383 W EP0214383 W EP 0214383W WO 03053848 A1 WO03053848 A1 WO 03053848A1
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- WO
- WIPO (PCT)
- Prior art keywords
- hydrogen storage
- storage materials
- doped
- materials according
- titanium
- Prior art date
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Classifications
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- 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
- C01B3/0078—Composite solid storage mediums, i.e. coherent or loose mixtures of different solid constituents, chemically or structurally heterogeneous solid masses, coated solids or solids having a chemically modified surface region
-
- 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
- C01B3/0031—Intermetallic compounds; Metal alloys; 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 relates to improved materials for the reversible storage of hydrogen using alkali metal aluminum hydrides (alkali metal alanates) or mixtures of aluminum metal with alkali metal (hydrides) by doping these materials with catalysts having a high degree of distribution or a large specific surface area.
- the alkali metal alanates are doped with transition metal and rare metal compounds or their combinations in catalytic amounts.
- the alanates NaAlH 4 , Na 3 AlH 6 and Na 2 LiAlH 6 are particularly useful.
- the properties of the substances mentioned as hydrogen storage materials can be significantly improved if the catalysts used for doping, namely transition metals of groups 3, 4, 5, 6, 7, 8, 9, 10, 11, or Alloys or mixtures of these metals with each other or with aluminum, or compounds of these metals in the form of very small particles with a high degree of distribution (e.g. particle size 0.5 to 1000 nm) or large specific surfaces (e.g. 50 to 1000 m Ig) can be used.
- the improvements in storage properties refer to
- titanium, iron, cobalt and nickel have been found to be suitable transition metals, for example in the form of titanium, titanium-iron and titanium-aluminum catalysts.
- the metals titanium, iron and aluminum can be used in elemental form, in the form of Ti-Fe or Ti-Al alloys, or in the form of their compounds for doping. Suitable metal compounds for this purpose are, for example, hydrides, carbides, nitrides, oxides, fluorides and alcoholates of titanium, iron and aluminum.
- alkali metal and aluminum are preferably present in a molar ratio of 3.5: 1 to 1: 1.5, the catalysts used for doping in amounts of 0.2 to 10 mol%, based on the alkali alanates, particularly preferably in amounts of 1 to 5 mol%.
- An excess of aluminum based on Formula I has an advantageous effect.
- the hydrogenation can be carried out at pressures between 0.5 and 15 MPascal (5 and 150 bar) and at temperatures between 20 and 200 ° C, and the dehydrogenation at temperatures between 20 and 250 ° C.
- Sodium alanate (example la) doped by grinding with the conventional, technical titanium nitride (TiN) with a specific surface area of 2 m 2 / g provides only 0.5% by weight of hydrogen after a dehydrogenation-rehydration cycle.
- sodium alanate (Example 1) is ground in the same way with a titanium nitride, which has a specific surface area of 150 m 2 / g and a grain size in the nanometer range (according to TEM), a storage material is obtained which is tested in a cycle test ( Table 1) has a reversible storage capacity of up to 5% by weight H 2 .
- Comparably high reversible hydrogen storage capacities (4.9% by weight, example 2) also shows NaAlH 4 , which is doped with colloidal titanium nanoparticles (H. Bönnemann et al, J. Am. Chem. Soc. 118 (1996) 12090).
- Table 1 Comparably high reversible hydrogen storage capacities (4.9% by weight, example 2) also shows NaAlH 4 , which is doped with colloidal titanium nanoparticles (H. Bönnemann et al, J. Am. Chem. Soc. 118 (1996) 12090).
- the rate of hydrogen charging and discharging of the reversible alanate systems can be increased many times over by doping them with finely divided titanium-iron catalysts instead of just such titanium catalysts.
- hydrogenation is required of the dehydrated sodium malanate ground with 2 mol% titanium tetrabutylate (Ti (OBu n ) 4 ) at 115-105 ° C / 134-118 bar (Example 3a, FIG. 2) ⁇ 15 h.
- the reduction in the weight of the hydrogen tank amounts to an increase in the weight-related hydrogen storage capacity of the hydrogen store, which increases the range of the vehicles in the case of hydrogen-powered vehicles.
- the decisive criteria for assessing the suitability of metal hydrides for hydrogen storage purposes also include the level of the hydrogen desorption temperature. This applies in particular to those applications in which the waste heat from the hydrogen-consuming unit (gasoline engine, fuel cell) is to be used to desorb the hydrogen from the hydride. In general, the lowest possible hydrogen desorption temperature, at the same time as high as possible desorption rate of the hydrogen, is desired.
- example 3a shows, the hydrogen desorption of the Ti-doped alanate at normal pressure up to the first stage (Eq. La) at> 80-85 ° C and up to the second (Eq. Lb) at> 130- 150 ° C possible.
- Example 4 shows, when using titanium metal nanoparticles as dopants in direct synthesis, reversible hydrogen storage capacities of 4.6% H 2 are achieved after only 2 cycles, which is in relation to the previous process (SGK, PCT / EP01 / 02363) means a significant improvement.
- aluminum can optionally be used in excess or inferior amounts based on Gl, 1 or 2.
- Example 1 NaAlH 4 doped with titanium nitride with a large specific surface area as a reversible hydrogen storage
- TiN titanium nitride
- TiN titanium nitride
- Elemental analysis Ti 60.13, N 13.76, C 12.86, H 1.24, Cl ⁇ 1%.
- the determination of the specific surface area according to the BET method on a 0.17 g sample of the TiN resulted in 152.4 m 2 / g.
- the isothermal shape indicates the presence of nanoparticles.
- the width of the reflections indicates particle size in the nanometer range.
- NaAlH 4 is doped in the same way as in Example 1, but with 2 mol% of a commercial TiN (from Aldrich, specific surface area 2 m 2 / g).
- a commercial TiN from Aldrich, specific surface area 2 m 2 / g.
- H 2 was desorbed.
- the sample provided only 0.5% by weight H 2 within 3 h when dehydrated at 180 ° C.
- Example 2 (NaAlH 4 doped with Ti nanoparticles as reversible hydrogen storage)
- Example 2 The test was carried out analogously to Example 2, with commercially available titanium powder (325 mesh) being used for doping the NaAlH. In the first dehydrogenation, a sample (-1.1 g) gave 3.6% by weight H within 8 h at 160 ° C.
- Example 3 NaAlH doped by milling with 2 mol% of Ti (OBu n ) 4 and Fe (OEt) 2 as a reversible hydrogen storage
- the grinding vessel was provided with 2 steel balls (6.97 g, 12 mm diameter) and then the mixture was ground for 3 hours at 30 s "1 in a vibratory mill (Retsch, MM 200, Haan, Germany). After the grinding process was complete Grinding vessel hot and the originally colorless mixture dark brown.
- the representation of the Ti-Fe-doped NaAlH was repeated, starting from 1.70 g NaAlH 4 , in the same way as described above.
- a mixed sample (1.72 g) of the Ti-Fe-doped alanate from the two batches was subjected to a 17-cycle test (see Example 1).
- Table 3 contains the data on the cycle test carried out.
- a comparison of the hydrogenation rates of the Ti-Fe-doped NaAlH 4 with a corresponding Ti-doped sample (example 3a) at 104 ° C./134-135 bar is given in FIG. 1.
- the temperature was first raised to 84-86 and then to 150-152 ° C. in order to bring about the dehydration up to the first (Eq. La) and second (Eq. Lb) dissociation stage.
- the sample was rehydrated at 100 ° C / 10 MPascal (100 bar) / 12 h.
- FIG. 2 shows, the dehydrogenations in the 1st and 2nd stages proceed at almost constant speeds; the 2nd dehydration is faster than the 1st and the same as the 3rd .. dehydration.
- cycles 2 and 3 the dehydrogenation is completed in the 1st stage after -1 h and in the 2nd stage after 20-30 min.
- the dehydrogenation of a corresponding Ti-doped sample is also shown in FIG.
- NaAlH 4 was made in the same manner as in the example . 3, but doped using Ti (OBu n ) 4 .
- the hydrogenation or dehydrogenation behavior of the sample of the Ti-doped alanate in comparison to the Ti-Fe-doped sample is shown in FIGS. 1 and 2.
- Example 4 directly synthesis of the Ti-doped NaAlH 4 from NaH, Al powder and Ti nanoparticles
- a 2 g sample of NaAlH 4 doped with 2.0 mol% of colloidal titanium (as in Example 2) was subjected to a 25 cycle hydrogen discharge and loading test. Cycle test conditions: dehydration, 120/180 ° C, normal pressure; Hydrogenation: 100 ° C / 100-85 bar. After the first cycles 2-5, with a storage capacity of 4.8% by weight H 2 , the capacity remained constant at 4.5-4.6% by weight H 2 until the end of the test.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
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Abstract
Description
Claims
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/499,526 US20040247521A1 (en) | 2001-12-21 | 2002-12-17 | Reversible storage of hydrogen using doped alkali metal aluminum hydrides |
CA002471362A CA2471362A1 (en) | 2001-12-21 | 2002-12-17 | Reversible storage of hydrogen using doped alkali metal aluminum hydrides |
EP02793042A EP1456117A1 (de) | 2001-12-21 | 2002-12-17 | Reversible speicherung von wasserstoff mit hilfe von dotierten alkalimetallaluminiumhydriden |
AU2002358732A AU2002358732A1 (en) | 2001-12-21 | 2002-12-17 | Reversible storage of hydrogen using doped alkali metal aluminum hydrides |
JP2003554572A JP2005512793A (ja) | 2001-12-21 | 2002-12-17 | ドープされた水素化アルミニウムアルカリ金属塩を用いた水素可逆吸蔵材料 |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE10163697A DE10163697A1 (de) | 2001-12-21 | 2001-12-21 | Reversible Speicherung von Wasserstoff mit Hilfe von dotierten Alkalimetallaluminiumhydriden |
DE10163697.0 | 2001-12-21 |
Publications (1)
Publication Number | Publication Date |
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WO2003053848A1 true WO2003053848A1 (de) | 2003-07-03 |
Family
ID=7710680
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2002/014383 WO2003053848A1 (de) | 2001-12-21 | 2002-12-17 | Reversible speicherung von wasserstoff mit hilfe von dotierten alkalimetallaluminiumhydriden |
Country Status (7)
Country | Link |
---|---|
US (1) | US20040247521A1 (de) |
EP (1) | EP1456117A1 (de) |
JP (1) | JP2005512793A (de) |
AU (1) | AU2002358732A1 (de) |
CA (1) | CA2471362A1 (de) |
DE (1) | DE10163697A1 (de) |
WO (1) | WO2003053848A1 (de) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005032709A2 (en) * | 2003-09-30 | 2005-04-14 | General Electric Company | Hydrogen storage compositions and methods of manufacture thereof |
EP1550634A2 (de) * | 2003-12-29 | 2005-07-06 | General Electric Company | Zusammensetzungen und Methoden zur Wasserstoffspeicherung und Zurückgewinnung |
WO2005068073A1 (de) * | 2004-01-14 | 2005-07-28 | Gkss-Forschungszentrum Geesthacht Gmbh | Metallhaltiger, wasserstoffspeichernder werkstoff und verfahren zu seiner herstellung |
WO2007041468A2 (en) * | 2005-10-03 | 2007-04-12 | General Electric Company | Hydrogen storage material and method for making |
EP1829820A1 (de) * | 2006-02-16 | 2007-09-05 | Sociedad española de carburos metalicos, S.A. | Verfahren zur Erzeugung von Wasserstoff |
Families Citing this family (15)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7011768B2 (en) * | 2002-07-10 | 2006-03-14 | Fuelsell Technologies, Inc. | Methods for hydrogen storage using doped alanate compositions |
EP1551032A4 (de) * | 2002-10-11 | 2008-03-26 | Yoshiaki Arata | Wasserstoffkondensat und verfahren zur erzeugung von wärme damit |
US7004993B2 (en) * | 2003-06-13 | 2006-02-28 | Philip Morris Usa Inc. | Nanoscale particles of iron aluminide and iron aluminum carbide by the reduction of iron salts |
DE10332438A1 (de) * | 2003-07-16 | 2005-04-14 | Studiengesellschaft Kohle Mbh | In porösen Matrizen eingekapselte Materialien für die reversible Wasserstoffspeicherung |
US20060067878A1 (en) * | 2004-09-27 | 2006-03-30 | Xia Tang | Metal alanates doped with oxygen |
DE102005003623A1 (de) * | 2005-01-26 | 2006-07-27 | Studiengesellschaft Kohle Mbh | Verfahren zur reversiblen Speicherung von Wasserstoff |
US7837976B2 (en) * | 2005-07-29 | 2010-11-23 | Brookhaven Science Associates, Llc | Activated aluminum hydride hydrogen storage compositions and uses thereof |
DE102005037772B3 (de) * | 2005-08-10 | 2006-11-23 | Forschungszentrum Karlsruhe Gmbh | Verfahren zur Herstellung eines Wasserstoff-Speichermaterials |
US20070178042A1 (en) * | 2005-12-14 | 2007-08-02 | Gm Global Technology Operations, Inc. | Sodium Alanate Hydrogen Storage Material |
NO330070B1 (no) * | 2006-01-26 | 2011-02-14 | Inst Energiteknik | Hydrogenlagringssystem, fremgangsmate for reversibel hydrogenlagring og fremstilling av materiale derfor samt anvendelse |
US8673436B2 (en) * | 2006-12-22 | 2014-03-18 | Southwest Research Institute | Nanoengineered material for hydrogen storage |
US8784771B2 (en) * | 2007-05-15 | 2014-07-22 | Shell Oil Company | Process for preparing Ti-doped hydrides |
WO2009132036A1 (en) * | 2008-04-21 | 2009-10-29 | Quantumsphere, Inc. | Composition of and method of using nanoscale materials in hydrogen storage applications |
US8418841B2 (en) | 2010-05-14 | 2013-04-16 | Ford Global Technologies, Llc | Method of enhancing thermal conductivity in hydrogen storage systems |
DE102019211379A1 (de) * | 2019-07-30 | 2021-02-04 | Studiengesellschaft Kohle Mbh | Verfahren zur Entfernung von Kohlenmonoxid und/oder gasförmigen Schwefelverbindungen aus Wasserstoffgas und/oder aliphatischen Kohlenwasserstoffen |
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US20010018939A1 (en) * | 1998-10-07 | 2001-09-06 | Alicja Zaluska | Reversible hydrogen storage composition |
WO2001068515A1 (de) * | 2000-03-16 | 2001-09-20 | Studiengesellschaft Kohle Mbh | Verfahren zur reversiblen speicherung von wasserstoff auf der basis von alkalimetallen und aluminium |
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US4529580A (en) * | 1982-12-15 | 1985-07-16 | Ethyl Corporation | Alkali metal aluminum hydride production |
US6106802A (en) * | 1997-01-31 | 2000-08-22 | Intevep, S.A. | Stable synthetic material and method for preparing same |
CA2218271A1 (en) * | 1997-10-10 | 1999-04-10 | Mcgill University | Method of fabrication of complex alkali mental hydrides |
US6471935B2 (en) * | 1998-08-06 | 2002-10-29 | University Of Hawaii | Hydrogen storage materials and method of making by dry homogenation |
US6716525B1 (en) * | 1998-11-06 | 2004-04-06 | Tapesh Yadav | Nano-dispersed catalysts particles |
US6521212B1 (en) * | 1999-03-18 | 2003-02-18 | United Therapeutics Corporation | Method for treating peripheral vascular disease by administering benzindene prostaglandins by inhalation |
US6680042B1 (en) * | 2000-11-07 | 2004-01-20 | Hydro-Quebec | Method of rapidly carrying out a hydrogenation of a hydrogen storage material |
US6680043B2 (en) * | 2001-11-29 | 2004-01-20 | General Motors Corporation | Process for enhancing the kinetics of hydrogenation/dehydrogenation of MAIH4 and MBH4 metal hydrides for reversible hydrogen storage |
US6793909B2 (en) * | 2002-01-29 | 2004-09-21 | Sandia National Laboratories | Direct synthesis of catalyzed hydride compounds |
US20040065171A1 (en) * | 2002-10-02 | 2004-04-08 | Hearley Andrew K. | Soild-state hydrogen storage systems |
WO2004041717A1 (en) * | 2002-11-01 | 2004-05-21 | Westinghouse Savannah River Company, Llc | Complex hydrides for hydrogen storage |
-
2001
- 2001-12-21 DE DE10163697A patent/DE10163697A1/de not_active Withdrawn
-
2002
- 2002-12-17 EP EP02793042A patent/EP1456117A1/de not_active Withdrawn
- 2002-12-17 AU AU2002358732A patent/AU2002358732A1/en not_active Abandoned
- 2002-12-17 US US10/499,526 patent/US20040247521A1/en not_active Abandoned
- 2002-12-17 WO PCT/EP2002/014383 patent/WO2003053848A1/de not_active Application Discontinuation
- 2002-12-17 CA CA002471362A patent/CA2471362A1/en not_active Abandoned
- 2002-12-17 JP JP2003554572A patent/JP2005512793A/ja active Pending
Patent Citations (4)
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US6106801A (en) * | 1995-07-19 | 2000-08-22 | Studiengesellschaft | Method for the reversible storage of hydrogen |
WO2000007930A1 (en) * | 1998-08-06 | 2000-02-17 | University Of Hawaii | Novel hydrogen storage materials and method of making by dry homogenation |
US20010018939A1 (en) * | 1998-10-07 | 2001-09-06 | Alicja Zaluska | Reversible hydrogen storage composition |
WO2001068515A1 (de) * | 2000-03-16 | 2001-09-20 | Studiengesellschaft Kohle Mbh | Verfahren zur reversiblen speicherung von wasserstoff auf der basis von alkalimetallen und aluminium |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2005032709A2 (en) * | 2003-09-30 | 2005-04-14 | General Electric Company | Hydrogen storage compositions and methods of manufacture thereof |
WO2005032709A3 (en) * | 2003-09-30 | 2005-08-11 | Gen Electric | Hydrogen storage compositions and methods of manufacture thereof |
EP1550634A2 (de) * | 2003-12-29 | 2005-07-06 | General Electric Company | Zusammensetzungen und Methoden zur Wasserstoffspeicherung und Zurückgewinnung |
EP1550634A3 (de) * | 2003-12-29 | 2005-10-26 | General Electric Company | Zusammensetzungen und Methoden zur Wasserstoffspeicherung und Zurückgewinnung |
US7175826B2 (en) | 2003-12-29 | 2007-02-13 | General Electric Company | Compositions and methods for hydrogen storage and recovery |
WO2005068073A1 (de) * | 2004-01-14 | 2005-07-28 | Gkss-Forschungszentrum Geesthacht Gmbh | Metallhaltiger, wasserstoffspeichernder werkstoff und verfahren zu seiner herstellung |
WO2007041468A2 (en) * | 2005-10-03 | 2007-04-12 | General Electric Company | Hydrogen storage material and method for making |
WO2007041468A3 (en) * | 2005-10-03 | 2007-05-24 | Gen Electric | Hydrogen storage material and method for making |
EP1829820A1 (de) * | 2006-02-16 | 2007-09-05 | Sociedad española de carburos metalicos, S.A. | Verfahren zur Erzeugung von Wasserstoff |
Also Published As
Publication number | Publication date |
---|---|
DE10163697A1 (de) | 2003-07-03 |
US20040247521A1 (en) | 2004-12-09 |
EP1456117A1 (de) | 2004-09-15 |
AU2002358732A1 (en) | 2003-07-09 |
CA2471362A1 (en) | 2003-07-03 |
JP2005512793A (ja) | 2005-05-12 |
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