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• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
  • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
  • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
  • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
  • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
  • C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
  • C25B11/093—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds at least one noble metal or noble metal oxide and at least one non-noble metal oxide
• • 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
  • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
  • B01J37/02—Impregnation, coating or precipitation
  • B01J37/03—Precipitation; Co-precipitation
  • B01J37/031—Precipitation
  • B01J37/035—Precipitation on carriers
• • 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
  • B01J21/18—Carbon
• • 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
  • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
  • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
  • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
  • B01J23/56—Platinum group metals
  • B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
  • B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
  • B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
• • 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
  • B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
  • B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
• • 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
  • B01J35/393—Metal or metal oxide crystallite size
• • 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
  • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
  • B01J37/16—Reducing
• • 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
  • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
  • B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
  • B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
  • B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
  • B01J37/345—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of ultraviolet wave energy
• • 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
  • C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
  • C01B3/32—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
  • C01B3/34—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
  • C01B3/38—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts
  • C01B3/40—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using catalysts characterised by the catalyst
• • C—CHEMISTRY; METALLURGY
  • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
  • C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
  • C25B1/00—Electrolytic production of inorganic compounds or non-metals
  • C25B1/01—Products
  • C25B1/02—Hydrogen or oxygen
• • 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
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B82—NANOTECHNOLOGY
  • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
  • B82Y40/00—Manufacture or treatment of nanostructures
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/02—Processes for making hydrogen or synthesis gas
  • C01B2203/0205—Processes for making hydrogen or synthesis gas containing a reforming step
  • C01B2203/0227—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step
  • C01B2203/0238—Processes for making hydrogen or synthesis gas containing a reforming step containing a catalytic reforming step the reforming step being a carbon dioxide reforming step
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/10—Catalysts for performing the hydrogen forming reactions
  • C01B2203/1041—Composition of the catalyst
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/10—Catalysts for performing the hydrogen forming reactions
  • C01B2203/1041—Composition of the catalyst
  • C01B2203/1047—Group VIII metal catalysts
  • C01B2203/1064—Platinum group metal catalysts
  • C01B2203/107—Platinum catalysts
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
  • C01B2203/12—Feeding the process for making hydrogen or synthesis gas
  • C01B2203/1205—Composition of the feed
  • C01B2203/1211—Organic compounds or organic mixtures used in the process for making hydrogen or synthesis gas
  • C01B2203/1235—Hydrocarbons
  • C01B2203/1241—Natural gas or methane
• • 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
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P20/00—Technologies relating to chemical industry
  • Y02P20/141—Feedstock
• • 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
  • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
  • Y02P20/00—Technologies relating to chemical industry
  • Y02P20/50—Improvements relating to the production of bulk chemicals
  • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Definitions

• the field of the invention is that of H 2 / O 2 fuel cells.
• pressurized hydrogen tanks gas storage
• metal hydrides storage in solid form
• biofuels and gaseous hydrocarbons such as natural gas or liquids such as alcohol, gasoline or gas oil are potentially sources of hydrogen and an electrochemical cell connected to a low-power power supply.
• an electrochemical cell connected to a low-power power supply.
• Platinum is very often used as a reaction catalyst in electrochemical systems, but its use for a purification application as anode material is problematic although it is the best material used at low temperature for the reaction of electro-oxidation of hydrogen (H 2 -> 2H + + 2e " ).
• Pt platinum
• Pt platinum
• This poisoning is done by adsorption of CO on the surface of the Pt irreversibly by blocking the available adsorption sites, thus preventing the adsorption of hydrogen, and its oxidation.
• Pt-Ru platinum-ruthenium
• Pt-Sn platinum-tin
• Pt-Mo platinum-molybdenum
• Pt-Co platinum-cobalt
• the present invention relates to a method based on the optimization of the operating conditions of synthesis in order to limit the growth phase of the nanoparticles and to favor that of germination making it possible to increase the number of germs.
• the limitation of the growth phase makes it possible to obtain nanoparticles of small sizes, typically of the order of 2 to 5 nm and a larger number of particles.
• the subject of the present invention is a process for synthesizing particles of bimetallic catalyst based on platinum and at least one second metal, characterized in that it comprises the chemical reduction of a first salt or complex based on platinum and at least one second salt or complex based on said second metal, said chemical reduction comprising the following steps:
• the reducing agent is formic acid, the temperature of said chemical reduction being carried out at a temperature of between approximately 0 ° C. and 8 ° C., advantageously being of the order of 4 ° C. vs.
• the reducing agent is hydrazine, the temperature of said reduction being carried out at a temperature between 0 ° C. and 2 ° C.
• the reducing agent is formaldehyde, the temperature of said reduction being carried out at a temperature of between -19 ° C. and 0 ° C.
• the process comprises the mixture of salt or platinum complex and salt or complex of said second metal, in the presence of particles of carbon black or metal oxide or metal nitride or carbide metallic.
• the amount of reducing agent is greater than or equal to the amount necessary to carry out the chemical reduction of all platinum salts and complexes and those of the second metal.
• the reaction is carried out in the presence of an additional source of energy to accelerate the chemical reduction operation without promoting the growth of nanoparticles.
• the additional energy source is a source of ultraviolet radiation.
• the source of ultraviolet radiation emits in a wavelength range of between about 200 nm and 300 nm.
• the second metal is tin, or ruthenium, or molybdenum, or cobalt.
• the bimetallic catalyst particles are based on platinum and tin and their size distribution has a median value of 4 nm with a low dispersion: the standard deviation is of the order of 1 , 1.
• the subject of the invention is also the use of the process for synthesizing bimetallic catalyst particles according to the invention, for a method of electrochemical hydrogen production comprising a catalytic reforming reaction in the presence of said catalyst particles and a mixture gas comprising hydrocarbon compounds.
• the metal particles obtained by the synthesis method of the invention appear in fact less sensitive to pollution by the hydrocarbon compounds present in the gas mixture than the particles obtained according to the methods described in the state of the art.
• the gaseous mixture comprises carbon monoxide, carbon dioxide and methane.
• FIG. 1 illustrates the UV absorption spectra of the PtCl 6 2 - ions
• FIG. 2 illustrates the particle size distribution of the Pt 3 Sn / C catalysts synthesized at room temperature and at 4 ° C., according to the process of the invention
• FIG. 3 illustrates the cyclic voltammogram obtained on Pt 3 Sn / C synthesized at room temperature in an aqueous solution of H 2 SO 4 at a concentration of 0.5 M at 25 ° C .;
• FIG. 4 illustrates the cyclic voltammogram obtained on Pt 3 Sn / C synthesized at 4 ° C. in an aqueous solution of H 2 SO 4 at a concentration of 0.5 M at 25 ° C .;
• FIG. 5 illustrates the evolution of the electro-oxidation current of H 2 on Pt 3 Sn / C synthesized at ambient temperature and at 4 ° C. in an aqueous solution of H 2 SO 4 of concentration 0.5 M after having subjected the catalyst to a mixture of compound gas 50 ppm CO in H 2 and 0.24 V vs. ERH and reaches a quasi stationary state of evolution of the oxidation current of hydrogen over time.
• Pt-M platinum-metal alloy
• Applicant uses the method FAM (Formic Acid Method) as described in the article E.l. Santiago et al. "CO tolerance on PtMo / C electrocatalysts prepared by the formic acid method" Electrochimica Acta 48 (2003) 3527-3534.
• solutions of salts or complexes of Pt and a metal alloy as precursors of Pt-M catalysts supported or not on carbon black with a high specific surface area, a metal oxide (TiO 2 2 , ZrO 2 , Al 2 O 3 , ...) or metal nitrides (TiN, TaN, BN), metal carbides (TiC, WC, W 2 C, Mo 2 C, etc.).
• the solutions of salts or complexes of Pt and the alloy metal element M are mixed with the carbon support and the whole is shaken vigorously with ultrasound for at least half an hour , time necessary to obtain a homogeneous mixture.
• the volume of the solutions is determined from the concentration of the solutions and so as to obtain the atomic composition of the desired metal alloy.
• the support mass of metal nanoparticles useful for the synthesis is determined so that it represents 50% of the mass of the synthesized catalyst.
• Formic acid is used as a reducing agent and is added to the previously described mixture.
• the volume of the formic acid must be in excess so that the chemical reduction of the salts or metal complexes is completed.
• the whole mixture is then brought to a temperature between the freezing temperature of water and that of formic acid. After 12 to 72 hours, the chemical reduction is complete and a metal powder is obtained representing the catalyst.
• the lowering of the temperature favors the decrease of the growth rate of the nanoparticles and consequently lengthens the duration of chemical reduction of the metal salts. To overcome this lengthening of duration, it is appropriate to accelerate the chemical reduction reaction without increasing the rate of growth.
• the vial containing the mixture may advantageously be exposed to a source of energy, for example ultraviolet (UV) rays which make it possible, thanks to this energy supply, to accelerate the reaction (the germination of the particles), thus favoring the multiplicity of seeds. in the nanoparticular state without promoting their growth.
• a source of energy for example ultraviolet (UV) rays which make it possible, thanks to this energy supply, to accelerate the reaction (the germination of the particles), thus favoring the multiplicity of seeds. in the nanoparticular state without promoting their growth.
• UV rays which make it possible, thanks to this energy supply, to accelerate the reaction (the germination of the particles), thus favoring the multiplicity of seeds. in the nanoparticular state without promoting their growth.
• the wavelength of the UV rays is preferably chosen between 200 and 300 nm, corresponding to the absorption zone of the complex platinum of Pt, as shown in FIG.
• Embodiment Pt-Sn / C catalysts of 3: 1 molar composition were synthesized by chemical reduction with formic acid.
• Aqueous solutions of platinum and tin salts of 0.01 M concentration were mixed in the presence of carbon black and vigorously shaken with ultrasound for a period of about one hour.
• the volumes of K 2 PtCl 6 , 6H 2 0 and SnCl 2 , 2H 2 0 solutions mixed are respectively 15 ml and 5 ml so as to obtain an atomic ratio of 3: 1.
• a large amount of formic acid HCOOH (ACS reagent, greater than or equal to 98% Sigma-Aldrich) with a molar ratio of the order of 1000: 1, between formic acid and metal salts, used as a reducing agent is added to the mixture to allow a simultaneous reduction of the platinum and tin salts.
• the objective of carrying out the synthesis at this temperature is to reduce during the synthesis, the growth rate of the nanoparticles which has a growth dependence with temperature.
• the electro-active surface corresponds more precisely to the electro-chemically active surface for the reactions considered, which one seeks to increase.
• Figure 2 illustrates particle size distributions of Pt 3 Sn / C catalysts synthesized at room temperature (25 ° C) and at 4 ° C and demonstrates the high percentage of small particles, typically 3 to 4 nm. with the synthesis method of the invention.
• EDS Energy Dispersive X-ray Spectrometry
• the electroactive surface of the catalyst prepared at 4 ° C. is thus much larger than that of the same catalyst synthesized at 25 ° C.
• the Applicant has carried out the cyclic voltammograms in an electrochemical half-cell at 25 ° C. with a scanning speed of 10 mV / s, relative to the various catalysts prepared.
• cyclic voltammetry is a method of electrochemical analysis based on the measurement of the current flow resulting from the reduction or oxidation of the compounds which come into contact with a working electrode (the sample studied) under effect of a controlled variation of the potential difference with a fixed potential electrode, called the reference electrode. It helps identify and measure quantitatively a large number of compounds and also to study the chemical reactions including these compounds.
• the high absorption power can be characterized by the absence of oxidation peaks (positive current) on the voltammogram having the measured current density as a function of the applied potential E to the working electrode.
• the absence of these peaks on the voltammogram reflects the blocking of adsorption sites of the catalyst by another species.
• Figure 3 relates to the results obtained with Pt 3 Sn / C particles prepared at 25 ° C.
• Curve 3a is relative to the voltammetric curve (under N 2 , in 0.5 MH 2 SO 4 at 25 ° C. and 10 mV.s.sup.- 1 ) carried out after pollution of the catalyst by adsorption of CO.
• Figure 4 relates to the results obtained with Pt 3 Sn / C particles prepared at 4 ° C.
• curve 4a the same cyclic voltammetric curve after pollution of the catalyst by CO adsorption shows that the pollution of the catalyst is not complete: the hydrogen desorption peaks are still observed.
• curve 4a between 0.1 and 0.4 V vs. ERH and oxidation of CO starts at an electrode potential of 0.3 V vs. ERH.
• the gain, in terms of energy, for the oxidation of hydrogen in the presence of traces of polluting gases is nearly 30% (0.72 kWh / Nm 3 H 2 with the catalyst synthesized at 4 ° C, against 0, 96 kWi // Nm 3 H 2 with the catalyst synthesized at 25 ° C).
• the Applicant has also followed the evolution of the electro-oxidation current of H 2 on Pt 3 Sn / C synthesized at room temperature and at 4 ° C. in an electrochemical half-cell device, when the electrode is fed with a mixture gas composed of 50 ppm CO in H 2 and subjected to a potential of 0.24 V vs. ERH.
• FIG. 5 shows via the curves 5a and 5b the difference in behavior with a catalyst produced according to the present invention at a temperature of 4 ° C., compared to a catalyst produced at ambient temperature.

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• 2013
  • 2013-02-26 FR FR1351679A patent/FR3002464A1/fr active Pending
• 2014
  • 2014-02-24 JP JP2015558484A patent/JP2016513013A/ja active Pending
  • 2014-02-24 US US14/767,267 patent/US20160010229A1/en not_active Abandoned
  • 2014-02-24 WO PCT/EP2014/053535 patent/WO2014131724A1/fr active Application Filing
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