EP2282824A1 - Filtre composite sic-vitroceramique - Google Patents

Filtre composite sic-vitroceramique

Info

Publication number
EP2282824A1
EP2282824A1 EP09766038A EP09766038A EP2282824A1 EP 2282824 A1 EP2282824 A1 EP 2282824A1 EP 09766038 A EP09766038 A EP 09766038A EP 09766038 A EP09766038 A EP 09766038A EP 2282824 A1 EP2282824 A1 EP 2282824A1
Authority
EP
European Patent Office
Prior art keywords
glass
phase
ceramic
filter
sic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP09766038A
Other languages
German (de)
English (en)
French (fr)
Inventor
Cécile JOUSSEAUME
Carine Dien-Barataud
Gilles Querel
Caroline Tardivat
Sébastien Rémi BARDON
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Original Assignee
Saint Gobain Centre de Recherche et dEtudes Europeen SAS
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
Application filed by Saint Gobain Centre de Recherche et dEtudes Europeen SAS filed Critical Saint Gobain Centre de Recherche et dEtudes Europeen SAS
Publication of EP2282824A1 publication Critical patent/EP2282824A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068—Other inorganic materials, e.g. ceramics
    • B01D39/2072—Other inorganic materials, e.g. ceramics the material being particulate or granular
    • B01D39/2075—Other inorganic materials, e.g. ceramics the material being particulate or granular sintered or bonded by inorganic agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • 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
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0036—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents
    • C03C10/0045—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and a divalent metal oxide as main constituents containing SiO2, Al2O3 and MgO as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0054—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing PbO, SnO2, B2O3
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
    • C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0006—Honeycomb structures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00793—Uses not provided for elsewhere in C04B2111/00 as filters or diaphragms
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    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6565—Cooling rate
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/74—Physical characteristics
    • C04B2235/77—Density
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/80—Phases present in the sintered or melt-cast ceramic products other than the main phase
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • C04B2235/9607—Thermal properties, e.g. thermal expansion coefficient

Definitions

  • the invention relates to the field of filters. More particularly, the present invention is in the field of porous materials for obtaining honeycomb structures.
  • honeycomb structures are used in particular as a catalyst support or as a particulate filter in automotive gas treatment systems in an exhaust line of an internal combustion engine.
  • pollutants such as gaseous and / or solid pollutants, in particular the soot produced by the combustion of a gasoline or diesel fuel.
  • Filtration structures for soot contained in the exhaust gas of an internal combustion engine are well known in the prior art. These structures have a honeycomb structure, one of the faces of the structure for the admission of the exhaust gases to be filtered and the other side the exhaust of the filtered exhaust gases.
  • the structure comprises, between the intake and discharge faces, a set of adjacent ducts of axes parallel to each other separated by porous filtration walls, which ducts are closed at one or the other of their ends to delimit entry chambers opening on the admission face and exit chambers opening on the evacuation face.
  • the peripheral part of the structure can be surrounded by a coating cement.
  • the channels are alternately closed in an order such that the exhaust gases, during the crossing of the honeycomb body, are forced to pass through the sidewalls of the inlet channels to join the outlet channels. In this way, the particles or soot are deposited and accumulate on the porous walls of the filter body.
  • the filter bodies are based on a porous ceramic material, for example cordierite, silicon carbide or aluminum titanate.
  • a particulate filter is subjected to a succession of filtration phases (accumulation of soot) and regeneration
  • the elements are most often assembled together by bonding by means of a cement of a ceramic nature, called in the following description seal cement or cement joint.
  • seal cement or cement joint examples of such filter structures are for example described in patent applications EP 816,065, EP 1 142 619, EP 1 455 923, WO 2004/090294, or WO 2005/063462.
  • the soot filters as previously described are mainly used on a large scale in the gas depollution devices exhaust of a diesel engine in automobiles or trucks or a stationary system.
  • the filtration structures are not yet entirely reliable over the life of the motor vehicle.
  • radial cracks may appear during poorly controlled regeneration or during spontaneous regeneration in the filter.
  • the local temperature of the filter can reach temperatures higher than 1000 0 C, with a strong spatial inhomogeneity of the temperatures leading to the appearance of cracks whose impact is more or less important on the integrity and the filtration capabilities of the filter.
  • experience has shown that, in the most severe cases, large radial cracks may appear which may cover the entire filter.
  • the additional cost of manufacturing an R-SiC particle filter is currently mainly related to the energy expended and the equipment necessary to reach the sintering temperature of the recrystallized SiC, most often between 2100 and 2300 ° C.
  • the costs related to other manufacturing parameters such as the cost of raw materials, the extrusion process, are minimal.
  • the object of the present invention is thus to provide a filter whose manufacturing cost is lowered, but having thermomechanical resistance properties at least comparable to those observed for an R-SiC filter.
  • the work carried out by the applicant and reported below has made it possible to obtain SiC-glass-ceramic composite filters making it possible to achieve such an objective.
  • the invention relates to a filter whose filtering portion consists of an inorganic material comprising SiC grains bonded by a phase of the glass-ceramic type, to form a porous structure whose open porosity is between 20 and 70%, said glass-ceramic binder phase comprising at least the following constituents, in molar percentage of all the oxides present in said phase: SiO 2 : from 30% to 80% Al 2 O 3 : from 5% to 45% MO : from 10% to 45%,
  • MO representing an oxide of a divalent cation or the sum of the oxides of the divalent cations present in said glass-ceramic phase, M being preferably chosen from Ca, Ba, Mg or Sr, said glass-ceramic phase having a residual glass volume percentage lower than 20%.
  • M represents at least one divalent cation selected from Ca, Ba, Mg.
  • the glass-ceramic phase comprises between 40 and 60 mol% of SiO 2 , preferably between 45 and 55 mol% of SiO 2 .
  • the glass-ceramic phase comprises between 15 and 30 mol% of Al 2 O 3 .
  • the glass-ceramic phase may further comprise between 5 and 20 mol% of oxide A 2 O in which A represents an alkali or the sum of alkali present in said phase, the alkali or alkali being selected from Na, K or preferably Cs.
  • the glass-ceramic phase may further comprise between 1 and 5 mol% of boron oxide.
  • the mass ratio between the glass-ceramic phase and the SiC phase in the porous material is between 10/90 and 40/60, preferably between 20/80 and 30/70.
  • the glass-ceramic phase comprises at least the following constituents, in molar percentage of all the oxides present in said phase: SiO 2 : from 40% to 70% Al 2 O 3 : from 10% to 30% MgO: from 15% to at 35%.
  • the glass-ceramic phase crystallizes in the cordierite structure, said phase comprising the following constituents, in molar percentage of the oxides:
  • SiO 2 from 40% to 55% - Al 2 O 3 : from 20% to 30% MgO: from 18 to 30%
  • the glass-ceramic phase crystallizes in the Anorthite Celsian structure, said phase comprising the following constituents, in molar percentage of the oxides: SiO 2 : from 40% to 55% Al 2 O 3 : from 15% to 30% - CaO : 5 to 15%
  • the invention relates particularly to a honeycomb particle filter having a structure as previously described, suitable for filtering the exhaust gas of a motor vehicle.
  • a filter may comprise a single monolithic element or be obtained by the association, by bonding with a joint cement, of a plurality of monolithic elements in honeycomb.
  • recrystallized silicon carbide rods have been synthesized according to the conventional techniques already well known in the art and for example described in the patent application EP 1 142 619 A1. Initially, it was first realized in a kneader a mixture of silicon carbide particles of greater than 98% purity according to the method of manufacturing an R-SiC structure described in WO 1994/22556. The mixture is obtained from a coarse fraction of SiC particles (75% by weight) whose median particle diameter is greater than 10 micrometers and a fine particle size fraction (25% by weight) whose median particle size is less than 1 micron.
  • the median diameter refers to the diameter of the particles below which 50% by mass of the population is found.
  • To the portion of SiC particles are added, based on their total weight, 7% by weight of a polyethylene type porogen and 5% by weight of an organic binder of the cellulose derivative type.
  • the honeycomb monoliths and the recrystallized SiC bars are obtained, after firing in a neutral atmosphere at a temperature of 2200 ° C.
  • the optimal experimental conditions are as follows: temperature rise of 20 ° C. C / hour up to 2200 0 C then temperature plateau of 6 hours at 2200 0 C.
  • a first glass composition is prepared by melting a mixture of precursors, in suitable proportions, placed in platinum crucibles in a flame oven. After complete melting of the mixture, the glass is quenched with water to obtain granulation.
  • the analysis shows that the glass phase thus obtained has the following composition, in molar percentage of the oxides:
  • Example 2 In a similar manner to Example 1, it was possible to obtain, without difficulty, by the same conventional extrusion techniques, honeycomb monoliths, as well as SiC strips.
  • the monoliths and the bars were sintered at a temperature of 1420 ° C. for 1 hour, that is to say more than 700 ° C. below the normal formation temperature of R-SiC and with a very long cooking time. shorter.
  • the heat treatment was carried out in a conventional induction furnace under an N 2 atmosphere under the following conditions: rise in temperature from 20K / min to 1420 ° C. and then temperature plateau of 1 hour at 1420 ° C. and finally descent along a ramp of 20K / min and following the inertia of the oven.
  • a third step another glass composition is prepared by the same melting technique as that described in Example 2, a mixture of precursors, in suitable proportions, placed in platinum crucibles in a flame oven. After complete melting of the mixture, the glass is quenched with water to obtain granulation.
  • the analysis shows that the following composition for the glass phase thus obtained, in molar percentage of the oxides:
  • this glass composition is used, after fine grinding, to obtain extruded honeycomb bars and monoliths of the SiC-glass-ceramic type according to the invention.
  • honeycomb monoliths, as well as SiC bars without difficulty by conventional extrusion techniques.
  • the monoliths and the bars were sintered at a temperature of 1380 ° C. for 1 hour, that is to say about 800 ° C. below the formation temperature of the R-SiC and with a very long cooking time. shorter .
  • the heat treatment was carried out in a conventional induction furnace under an N 2 atmosphere under the following conditions: rise in temperature from 20 K / min to 1380 ° C. and then temperature plateau of 1 hour at 1380 ° C. and finally lowering temperature in a ramp of 20 K / min and following the inertia of the oven.
  • the performance of the materials thus obtained and in particular their resistance to thermal shocks, an essential factor for use as a particulate filter in an automobile exhaust line as described above, are evaluated according to the TSP (Thermal Shock Parameter) criterion. classically used.
  • TSP Thermal Shock Parameter
  • the TSP is representative of the thermomechanical resistance of a material, in the sense previously described. More specifically, it is generally accepted that the higher the TSP of a material, the better its thermomechanical resistance.
  • MoE expressed in Pa, represents the Young's modulus
  • MoR was measured according to ASTM C1161-02.
  • MoE was measured by RFDA (Resonant Frequency and Damping Analyzer) techniques. The measurement was performed according to ASTM C1259-94.
  • the open porosity and the median pore diameter are measured on the honeycomb-shaped honeycomb-shaped bars and monoliths by mercury porosimetry. The porosimetry results (open porosity and pore diameter) obtained appeared substantially identical for the same material on the bars and monoliths.
  • the TSP of the SiC / glass-ceramic composite material of Example 2 is of the order of magnitude of the TSP of an R-SiC, which reflects a similar resistance of the materials to thermal shocks, although that the SiC / vitroceramic material was obtained at a firing temperature of at least 700 ° C. lower than that of the exclusively R-SiC material.
  • the SiC / glass-ceramic composite material of Example 3 even has a TSP factor better than that of R-SiC, for very close porosity characteristics.
  • the microstructure of the materials was observed on backscattered electron mode SEM plates, respectively shown in FIG. 1 for example 2 and in FIG. 2 for example 3.
  • a three-dimensional porous structure consisting of large pores opening between the SiC grains is clearly visible on the plates. It is also visible on the plates that the glass-ceramic phase acts as a binder between the grains of SiC.
  • the interstitial phase between the SiC grains comprises an essentially crystalline phase, with however the presence of a residual glassy phase around polycrystalline clusters, the volume of said glassy phase representing between about 5% and about 20% of the total volume of the glass-ceramic phase.
  • Example 10 The duration of the plateau of the maximum cooking temperature (1380 ° C.) was raised to 2 hours to reduce the degree of crystallinity of the glass-ceramic phase (temperature greater than the solidus).
  • the glass-ceramic has a crystalline volume, as estimated on the SEM plates made on the material obtained, less than 80% of the total volume, that is to say that the residual vitreous phase is greater than 20% by volume.
  • the measured TSP is then much lower than 100 due to the significant decrease in MoR.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geology (AREA)
  • Combustion & Propulsion (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Filtering Materials (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Ceramic Products (AREA)
  • Glass Compositions (AREA)
EP09766038A 2008-05-22 2009-05-19 Filtre composite sic-vitroceramique Withdrawn EP2282824A1 (fr)

Applications Claiming Priority (2)

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FR0853341A FR2931366B1 (fr) 2008-05-22 2008-05-22 Filtre composite sic-vitroceramique
PCT/FR2009/050931 WO2009153476A1 (fr) 2008-05-22 2009-05-19 Filtre composite sic-vitroceramique

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FR2931366B1 (fr) 2011-01-21
JP2011520605A (ja) 2011-07-21

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