WO2013146953A1 - 多孔質材料、ハニカム構造体及び多孔質材料の製造方法 - Google Patents
多孔質材料、ハニカム構造体及び多孔質材料の製造方法 Download PDFInfo
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- WO2013146953A1 WO2013146953A1 PCT/JP2013/059143 JP2013059143W WO2013146953A1 WO 2013146953 A1 WO2013146953 A1 WO 2013146953A1 JP 2013059143 W JP2013059143 W JP 2013059143W WO 2013146953 A1 WO2013146953 A1 WO 2013146953A1
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- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 78
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims abstract description 15
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Definitions
- the present invention relates to a porous material, a honeycomb structure, and a method for manufacturing the porous material. More specifically, the present invention relates to a porous material and a honeycomb structure having high thermal shock resistance, and a method for producing a porous material capable of producing such a porous material.
- a porous material in which silicon carbide particles are bonded with an oxide phase or the like is excellent in thermal shock resistance, and thus is used as a material for a catalyst carrier, a material for a DPF (diesel particulate filter), or the like (for example, Patent Document 1). 2).
- the present invention has been made to solve such a problem, and has a porous material and a honeycomb structure having high thermal shock resistance, and a porous material capable of producing such a porous material of the present invention.
- the main purpose is to provide a manufacturing method.
- the present invention provides the following porous material, honeycomb structure, and method for producing the porous material.
- the lower limit of the content of the composite binder is 12% by mass with respect to the total mass of the aggregate, the composite binder, and the metal silicon, and the upper limit of the content of the composite binder is 50%. % Of the porous material according to [1].
- the lower limit of the content of the mullite particles is 0.5% by mass, and the upper limit of the content of the mullite particles is 15% by mass with respect to the total mass of the aggregate, the composite binder, and the metal silicon. % Of the porous material according to [1] or [2].
- the lower limit of the aspect ratio of the mullite particles that are reinforcing particles is 1.5, and the upper limit of the aspect ratio of the mullite particles is 4.7. Porous material.
- the pores having a pore diameter of less than 10 ⁇ m are 20% or less of the whole pores, and the pores having a pore diameter of more than 40 ⁇ m are 10% or less of the whole pores, Porous material.
- a honeycomb structure provided with partition walls, which is formed of the porous material according to any one of [1] to [10], and which partitions and forms a plurality of cells extending from one end face to the other end face.
- honeycomb structure according to [11] further comprising a plugged portion disposed in an opening of the predetermined cell on the one end face and an opening of the remaining cell on the other end face.
- the metal silicon content in the porous material is less than 15 mass%
- metal silicon is not contained, or metal silicon is contained in such an amount that the metal silicon content in the obtained porous material is less than 15% by mass.
- the aluminum oxide component contained in the composite binder generating raw material is aluminum oxide, and the average particle diameter of the aluminum oxide is a lower limit of 2.5 ⁇ m and an upper limit of 15.0 ⁇ m.
- the porous material of the present invention is superior in thermal shock resistance as compared with conventional porous materials.
- Porous material As shown in FIG. 1, one embodiment of the porous material of the present invention is an aggregate 1 and “a cordierite which is a binder 3 and mullite particles which are reinforcing particles 2 are dispersed. And a composite binder 5 ”that bonds the aggregates 1 in a state where the pores 4 are formed.
- the content of metal silicon is less than 15% by mass.
- the content of metallic silicon is the value of the remaining amount of Si by identifying the amounts of SiC and SiO 2 from Si, C, and O measured by ICP (Inductively Coupled Plasma) -AES (Emission Spectroscopy) method.
- FIG. 1 is a schematic view showing an enlarged cross section of one embodiment (porous material 100) of the porous material of the present invention.
- the porous material of the present invention Since the porous material of the present invention has the above-described configuration, it has high strength and a high “strength / Young's modulus ratio” value. Therefore, the porous material of the present invention is excellent in thermal shock resistance.
- the “strength” in the “strength / Young's modulus ratio” is bending strength.
- mullite particles function as reinforcing particles. For example, when a crack occurs in the porous material, the mullite particles can prevent the crack from progressing.
- Cordierite can contain spinel particles and forsterite particles in addition to mullite particles. However, since spinel particles and forsterite particles have lower strength than mullite particles, they cannot function as reinforcing particles.
- mullite particles have higher strength than spinel particles and forsterite particles, and therefore can prevent the progress of cracks generated in the porous material and function as reinforcing particles.
- spinel particles and forsterite particles have a high thermal expansion coefficient, the thermal expansion coefficient of the entire porous material is increased when present in the binder, and the thermal shock resistance of the porous material is lowered. Therefore, spinel particles and forsterite particles are not suitable as reinforcing particles.
- the composite binder is obtained by dispersing mullite particles as reinforcing particles in cordierite as a binder. Further, a form in which a part of the aggregate is dispersed in the binder may be used.
- the composite binder preferably has a crystalline component of more than 50% by mass. That is, the composite binder preferably has an amorphous component of less than 50% by mass. The amorphous component in the composite binder can be quantified by analyzing the X-ray diffraction data.
- the amount of amorphous when “the maximum height of the background is 25% in the range of 2 ⁇ of 20 ° to 30 ° with respect to the diffraction peak height of (100) plane of hexagonal cordierite” Is 50 mass% with respect to the entire composite binder. Then, the amorphous amount when the maximum background height is 2.8% when 2 ⁇ is in the range of 20 ° to 30 ° with respect to the diffraction peak height of the (100) plane of hexagonal cordierite. And 0% by mass relative to the entire composite binder. And the measurement result of a sample is applied to the said relationship (calibration curve), and the amorphous component in a composite binder is calculated
- the measurement can be performed using a powder obtained by pulverizing a porous material as a measurement sample and using a rotating counter electrode X-ray diffractometer (RINT, manufactured by Rigaku Corporation).
- the aggregate preferably contains at least one of silicon carbide (SiC) particles and silicon nitride (Si 3 N 4 ) particles.
- the aggregate is preferably silicon carbide (SiC) particles or silicon nitride (Si 3 N 4 ) particles, and more preferably silicon carbide (SiC) particles.
- SiC silicon carbide
- SiC silicon carbide
- SiC silicon carbide
- the porous material of the present invention has a metal silicon content of less than 15% by mass, preferably 10% by mass or less, more preferably 9% by mass or less, and particularly preferably 2.5% by mass or less.
- the content of metal silicon is most preferably 0% by mass. Since the specific heat capacity is maintained high because the content of metallic silicon is less than 15% by mass, the thermal shock resistance is improved. When the content of metal silicon is 15% by mass or more, the specific heat capacity is lowered, and the thermal shock resistance may be lowered, which is not preferable.
- the lower limit of the porosity is preferably 40%, and more preferably 50%.
- the upper limit value of the porosity is preferably 90%, and more preferably 70%.
- the porosity is less than 40%, the pressure loss may increase.
- the porosity is 50% or more, a low pressure loss is preferable for use in a DPF or the like.
- the porosity exceeds 90%, the strength may be lowered.
- the porosity is 70% or less, high strength is preferable for use in a DPF or the like.
- the porosity is calculated from the total pore volume (unit: cm 3 / g) by the mercury intrusion method (based on JIS R 1655) and the apparent density (unit: g / cm 3 ) measured by the Archimedes method. It is the value.
- the porosity can be adjusted by, for example, the amount of a pore-forming material used when producing the porous material, the amount of sintering aid, the firing atmosphere, and the like.
- the porosity can also be adjusted by the ratio between the aggregate and the composite binder.
- the lower limit value of the average pore diameter is preferably 10 ⁇ m, and more preferably 15 ⁇ m.
- the upper limit value of the average pore diameter is preferably 40 ⁇ m, and more preferably 30 ⁇ m.
- the average pore diameter is less than 10 ⁇ m, the pressure loss may increase.
- the average pore diameter exceeds 40 ⁇ m, when the porous material of the present invention is used as a DPF or the like, a part of the particulate matter in the exhaust gas may pass through the DPF or the like without being collected.
- the average pore diameter is a value measured by a mercury intrusion method (based on JIS R 1655).
- pores having a pore diameter of less than 10 ⁇ m are 20% or less of the whole pores, and pores having a pore diameter of more than 40 ⁇ m are preferably 10% or less of the whole pores. If the pores having a pore diameter of less than 10 ⁇ m exceed 20% of the total pores, the pores having a pore diameter of less than 10 ⁇ m are likely to be clogged when the catalyst is loaded, so that the pressure loss tends to increase. When the pores with a pore diameter of less than 40 ⁇ m exceed 10% of the whole pores, the pores with a pore diameter of less than 40 ⁇ m may easily pass through a particulate substance, and thus it may be difficult to sufficiently exert a filter function such as DPF. .
- the lower limit of the content of the composite binder with respect to the total mass of the aggregate, the composite binder and the metal silicon is preferably 12% by mass. Moreover, it is preferable that the upper limit of content of a composite binder with respect to the total mass of an aggregate, a composite binder, and metal silicon is 50 mass%. Furthermore, the lower limit of the content of the composite binder with respect to the total mass of the aggregate, the composite binder, and the metal silicon is more preferably 17% by mass, and particularly preferably 20% by mass. Further, the upper limit of the content of the composite binder with respect to the total mass of the aggregate, the composite binder, and the metal silicon is more preferably 40% by mass, and particularly preferably 35% by mass.
- the content of the composite binder is less than 12% by mass, the bending strength is lowered, the “strength / Young's modulus ratio” is further lowered, and the thermal shock resistance may be lowered.
- the content of the composite binder exceeds 50% by mass, the porosity may be reduced.
- the lower limit of the ratio of the content of “mullite particles contained in the composite binder and acting as reinforcing particles” to the total mass of the aggregate, composite binder, and metal silicon is 0.5% by mass. preferable. Moreover, it is preferable that the upper limit of the ratio with respect to the total mass of aggregate, a composite binder, and a metal silicon of the content of the said mullite particle is 15 mass%.
- the lower limit of the mullite particle content is more preferably 0.9% by mass. Further, the upper limit of the content of the mullite particles is more preferably 8.0% by mass, and particularly preferably 4.5% by mass.
- the content ratio of “mullite particles contained in the composite binder” with respect to the total mass of the aggregate, composite binder, and metal silicon (hereinafter, sometimes referred to as “content ratio of mullite particles”) is 0.5. If it is less than% by mass, the strength / Young's modulus ratio may be lowered, and the thermal shock resistance may be lowered. Moreover, when the content rate of a mullite particle exceeds 15 mass%, strength / Young's modulus ratio will become low and a thermal shock resistance may fall.
- the “content ratio of mullite particles” is a value obtained based on a value obtained by X-ray diffraction analysis. Specifically, it is calculated by simple quantitative analysis “analyzing X-ray diffraction data and quantifying each component using RIR (Reference Intensity Ratio) method”.
- the analysis of X-ray diffraction data is preferably performed using, for example, “X-ray data analysis software JADE7” manufactured by MDI.
- X-ray diffractometer used for X-ray diffraction analysis a rotating counter-cathode X-ray diffractometer (RINT, manufactured by Rigaku Corporation) can be exemplified.
- the lower limit of the average particle diameter of the silicon carbide particles as the aggregate is preferably 5 ⁇ m, and more preferably 10 ⁇ m.
- the upper limit value of the average particle diameter of the silicon carbide particles as the aggregate is preferably 100 ⁇ m, and more preferably 40 ⁇ m. If it is smaller than 5 ⁇ m, the firing shrinkage amount becomes large, and the porosity of the fired product may be less than 40%. In addition, pores of less than 10 ⁇ m in the fired body may exceed 20% of the entire pores. When it is larger than 100 ⁇ m, pores exceeding 40 ⁇ m in the fired body may be 10% or more of the whole pores. Furthermore, when a honeycomb structure is formed, the die may be clogged, resulting in a molding failure.
- the average particle diameter of silicon carbide as an aggregate is larger than the average particle diameter of mullite particles as reinforcing particles. Moreover, it is preferable that the average particle diameter of the silicon carbide which is an aggregate is 1.5 times or more the average particle diameter of the mullite particles which are reinforcing particles.
- the upper limit of the magnification of the average particle diameter of silicon carbide as an aggregate to the average particle diameter of mullite particles as reinforcing particles is preferably 40 times. If the average particle size of silicon carbide is smaller than 1.5 times the average particle size of mullite particles, the number of contacts with the binder is reduced, which may cause firing failure. As a result, the bending strength is greatly reduced, and the thermal shock resistance may be inferior.
- the aspect ratio of mullite particles is preferably 1.5 or more.
- the lower limit value of the aspect ratio of the mullite particles is more preferably 1.8, and particularly preferably 2.1.
- the upper limit of the aspect ratio of the mullite particles is preferably 4.7, and more preferably 4.2.
- the aspect ratio is less than 1.5, the effect of acting as reinforcing particles is reduced, so that the bending strength is lowered, and further, the “bending strength / Young's modulus ratio” is lowered, and the thermal shock resistance may be lowered.
- the aspect ratio exceeds 4.7 the shape of the mullite particles is a plate shape or a fiber shape.
- the aspect ratio of mullite particles is a value measured using an SEM (scanning electron microscope). Specifically, the porous material of the present invention contained in a resin is mirror-polished using diamond slurry or the like as an observation sample, and this cross-sectional polished surface is observed at a magnification of 3000 times to obtain a microstructure photograph. . Measure the major axis and minor axis of all mullite particles in the obtained microstructure photograph, calculate the ratio “major axis / minor axis”, and average the number of mullite particles in the microstructure photograph. Aspect ratio.
- the lower limit of the long diameter of the mullite particles is preferably 0.5 ⁇ m, more preferably 1.8 ⁇ m, and particularly preferably 2.0 ⁇ m.
- the upper limit of the long diameter of the mullite particles is preferably 35 ⁇ m, and more preferably 30.1 ⁇ m. If the long diameter of the mullite particles is less than 0.5 ⁇ m, the strength does not act as reinforcing particles, so the bending strength is lowered, the “strength / Young's modulus ratio” is further lowered, and the thermal shock resistance may be lowered.
- the long diameter of the mullite particles exceeds 35 ⁇ m, it acts as a defect instead of reinforcing particles and the bending strength is lowered, the “strength / Young's modulus ratio” is further lowered, and the thermal shock resistance may be lowered.
- the porous material of the present invention preferably has a “bending strength (Pa) / Young's modulus (Pa) ratio” of 1.4 ⁇ 10 ⁇ 3 or more.
- the lower limit value of the bending strength is 7.0 MPa, and the lower limit value of the “bending strength (Pa) / Young's modulus (Pa) ratio” is more preferably 1.5 ⁇ 10 ⁇ 3 .
- the upper limit value of the bending strength is 14.0 MPa, and the upper limit value of the “bending strength (Pa) / Young's modulus (Pa) ratio” is more preferably 5.0 ⁇ 10 ⁇ 3 .
- the thermal shock resistance of the porous material can be improved.
- the upper limit is about 50 MPa in the configuration of the present invention.
- the bending strength is a value measured by a “bending test” based on JIS R1601.
- the Young's modulus is a value calculated from the stress-strain curve obtained in the “bending test”.
- the porous material of the present invention preferably has a linear thermal expansion coefficient of 40 ⁇ 800 ° C. or less of 4.2 ⁇ 10 ⁇ 6 / K or less.
- the lower limit value of linear thermal expansion coefficient of 40 ⁇ 800 ° C. is more preferably from 2.0 ⁇ 10 -6 / K, particularly preferably 2.0 ⁇ 10 -6 / K.
- the upper limit value of the linear thermal expansion coefficient at 40 to 800 ° C. is more preferably 3.9 ⁇ 10 ⁇ 6 / K. If it is larger than 4.2 ⁇ 10 ⁇ 6 / K, the thermal shock resistance may be lowered.
- 2.0 ⁇ 10 ⁇ 6 / K is the lower limit in the configuration of the present invention.
- a thermal expansion coefficient is the value measured by the method based on JISR1618. Specifically, a test piece of 3 cells long ⁇ 3 cells wide ⁇ 20 mm long was cut out from the honeycomb structure and thermally expanded in the A-axis direction (parallel to the flow path of the honeycomb structure) at 40 to 800 ° C. This is a value obtained by measuring a coefficient.
- the porous material of the present invention may contain less than 0.4% by mass of sodium (Na) in terms of oxide, with respect to the entire porous material. Moreover, the porous material of this invention may contain less than 0.4 mass% of potassium (K) by the oxide conversion mass with respect to the whole porous material. Moreover, the porous material of the present invention may contain calcium (Ca) in an oxide equivalent mass of less than 0.4 mass% with respect to the entire porous material.
- Terms of oxide weight of sodium is the Na 2 O mass when the sodium is assumed to be present as all Na 2 O.
- Oxide reduced mass of potassium is the K 2 O mass when it is assumed that the potassium is present as all K 2 O.
- the oxide equivalent mass of calcium is the mass of the CaO when it is assumed that all calcium is present as CaO.
- the contents of sodium (Na), potassium (K), and calcium (Ca) in the porous material are values measured by an ICP (Inductively Coupled Plasma) -AES (Emission Spectroscopy) method.
- the honeycomb structure of the present invention includes the partition wall that is formed of the above-described porous material of the present invention and that defines “a plurality of cells extending from one end surface to the other end surface”.
- the cell serves as a fluid flow path.
- the honeycomb structure preferably has a structure having an outer peripheral wall located at the outermost periphery.
- the lower limit of the partition wall thickness is preferably 30 ⁇ m, and more preferably 50 ⁇ m.
- the upper limit of the partition wall thickness is preferably 1000 ⁇ m, more preferably 500 ⁇ m, and particularly preferably 350 ⁇ m.
- the lower limit of the cell density is preferably 10 cells / cm 2, more preferably 20 cells / cm 2 , and particularly preferably 50 cells / cm 2 .
- the upper limit of the cell density is preferably 200 cells / cm 2 and more preferably 150 cells / cm 2 .
- the shape of the honeycomb structure is not particularly limited, and examples thereof include a cylindrical shape and a cylindrical shape having a polygonal bottom (triangle, quadrangle, pentagon, hexagon, etc.).
- the shape of the cells of the honeycomb structure is not particularly limited.
- examples of the cell shape in the cross section orthogonal to the cell extending direction include a polygon (triangle, quadrangle, pentagon, hexagon, heptagon, octagon, etc.), circle, or a combination thereof.
- the size of the honeycomb structure can be appropriately determined according to the application. Since the honeycomb structure of the present invention is composed of the porous substrate of the present invention, it has excellent thermal shock resistance. Therefore, it is possible to increase the size of the honeycomb structure. And as a lower limit of the magnitude
- the honeycomb structure of the present invention can be used as a DPF or a catalyst carrier. It is also a preferred embodiment that a catalyst is supported on the DPF.
- the honeycomb structure of the present invention is used as a DPF or the like, the following structure is preferable. That is, it is preferable that the honeycomb structure of the present invention includes a plugged portion disposed in an opening of a predetermined cell on one end face and an opening of a remaining cell on the other end face. On both end faces, it is preferable that cells having plugged portions and cells not having plugged portions are alternately arranged to form a checkered pattern.
- the aggregate raw material preferably contains at least one of silicon carbide (SiC) and silicon nitride (Si 3 N 4 ).
- the raw material for producing the composite binder is a material in which “mullite particles that are reinforcing particles” and “cordielite that is a binder” are produced by firing. Note that mullite powder and cordierite forming raw material may be mixed instead of the composite binder generating raw material powder.
- the cordierite forming raw material means a raw material from which cordierite crystals are generated by firing.
- the raw material for producing the composite binder preferably contains an aluminum oxide (Al 2 O 3 ) component of more than 34.9% by mass and less than 71.8% by mass.
- the raw material for producing a composite binder preferably contains more than 28.2% by mass and less than 52.0% by mass of a silicon dioxide (SiO 2 ) component.
- the raw material for composite binder production contains a magnesium oxide (MgO) component of more than 5.0% by mass and less than 13.8% by mass.
- the aluminum oxide component is aluminum oxide or “aluminum and oxygen” which is a composition ratio of aluminum oxide in a raw material containing aluminum and oxygen such as aluminum hydroxide, kaolin, boehmite, and feldspar.
- the "mass of the aluminum oxide component” is a terms of oxide weight of aluminum in the aluminum oxide component (mass of Al 2 O 3).
- the lower limit value of the average particle diameter is preferably 2.5 ⁇ m
- the upper limit value of the average particle diameter is preferably 15.0 ⁇ m.
- the aluminum oxide is preferably ⁇ -alumina.
- the silicon dioxide component is silicon dioxide or “silicon and oxygen” which is a composition ratio of silicon dioxide in a raw material containing silicon and oxygen such as “talc, kaolin, and feldspar”.
- the magnesium oxide component is magnesium oxide or “magnesium and oxygen” which is a composition ratio of magnesium oxide in a raw material containing magnesium and oxygen such as magnesium hydroxide and talc.
- Examples of the raw material powder for generating a composite binder include a mixed powder of 35.9% by mass of talc, 44.3% by mass of aluminum hydroxide, and 19.8% by mass of silica powder.
- the raw material powder for producing the composite binder includes Al—Si fiber, Al 2 O 3 fiber, plate-like alumina, coarse-grained Al 2 O 3 , kaolin, etc.
- the lower limit value of the major axis of the plate-like alumina is preferably 0.5 ⁇ m.
- the upper limit of the major axis of the plate-like alumina is preferably 15 ⁇ m.
- the lower limit value of the minor axis (thickness) of the plate-like alumina is 0.01 ⁇ m.
- the upper limit of the minor axis (thickness) of the plate-like alumina is preferably 1 ⁇ m.
- variety of plate-like alumina is 0.05 micrometer.
- variety of plate-like alumina is 70 micrometers.
- the lower limit of the aspect ratio of the plate-like alumina is preferably 5.
- the upper limit of the aspect ratio of the plate-like alumina is preferably 70.
- the alumina fiber preferably has a length of 200 ⁇ m or less. Further, the alumina fiber preferably has a minor axis of 3 ⁇ m or less.
- the alumina fiber preferably has an aspect ratio of 3 or more.
- the average particle diameter of the coarse Al 2 O 3 is preferably 2.5 to 15 ⁇ m.
- the minor axis and the major axis are values measured using a scanning electron microscope. Specifically, it is a value obtained by measuring the major axis and the minor axis of all the particles in the microstructure photograph that can be observed at a magnification of 3000 times, and averaging each by the number of particles.
- the average particle diameter is a value measured by a laser diffraction method.
- a raw material (magnesium (Mg) source) of a magnesium (Mg) component MgO or Mg (OH) 2 is preferable.
- a raw material (silicon (Si) source) of Si (silicon) component kaolin, powdered silica, and colloidal silica are preferable.
- the raw material for producing the composite binder contains no metallic silicon or contains an amount of metallic silicon such that the metallic silicon content in the resulting porous material is less than 15% by mass. Thereby, metal silicon content in the porous material obtained can be made into less than 15 mass%.
- the aggregate material is silicon carbide (SiC) powder or silicon nitride (Si 3 N 4 ) powder.
- the lower limit of the average particle diameter of the aggregate raw material is preferably 5 ⁇ m, and more preferably 10 ⁇ m.
- the upper limit of the average particle diameter of the aggregate raw material is preferably 100 ⁇ m, and more preferably 40 ⁇ m.
- the average particle diameter is a value measured by a laser diffraction method.
- binder examples include organic binders such as methyl cellulose, hydroxypropoxyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose, and polyvinyl alcohol. Among these, it is preferable to use methyl cellulose and hydroxypropoxyl cellulose in combination.
- the binder content is preferably 2 to 10% by mass with respect to the entire forming raw material.
- ethylene glycol, dextrin, fatty acid soap, polyalcohol or the like can be used as the surfactant. These may be used individually by 1 type and may be used in combination of 2 or more type.
- the content of the surfactant is preferably 2% by mass or less with respect to the whole forming raw material.
- the pore former is not particularly limited as long as it becomes pores after firing, and examples thereof include graphite, starch, foamed resin, water absorbent resin, silica gel and the like.
- the pore former content is preferably 10% by mass or less based on the entire forming raw material.
- the lower limit of the average particle diameter of the pore former is preferably 10 ⁇ m.
- the upper limit of the average particle diameter of a pore former is 30 micrometers. If it is smaller than 10 ⁇ m, pores may not be formed sufficiently. If it is larger than 30 ⁇ m, the die may be clogged during molding.
- the average particle diameter of the pore former is a value measured by a laser diffraction method. When the pore former is a water absorbent resin, the average particle diameter is a value after water absorption.
- the water content is appropriately adjusted so that the clay hardness is easy to mold, but is preferably 20 to 80% by mass with respect to the entire forming raw material.
- the forming raw material is kneaded to form a clay.
- molding raw material and forming a clay For example, the method of using a kneader, a vacuum clay kneader, etc. can be mentioned.
- honeycomb formed body formed body
- clay is also included in the concept of forming raw materials.
- extrusion molding it is preferable to use a die having a desired overall shape, cell shape, partition wall thickness, cell density and the like.
- a cemented carbide which does not easily wear is preferable.
- the honeycomb formed body has a structure having porous partition walls that define and form a plurality of cells serving as fluid flow paths and an outer peripheral wall located at the outermost periphery.
- the partition wall thickness, cell density, outer peripheral wall thickness, and the like of the honeycomb formed body can be appropriately determined according to the structure of the honeycomb structure to be manufactured in consideration of shrinkage during drying and firing.
- the molding process is a process for producing a molded body by extruding a molding raw material containing an aggregate raw material, a composite binder generating raw material, a pore former, and a binder.
- the honeycomb molded body thus obtained is preferably dried before firing.
- the drying method is not particularly limited, and examples thereof include an electromagnetic heating method such as microwave heating drying and high-frequency dielectric heating drying, and an external heating method such as hot air drying and superheated steam drying.
- an electromagnetic heating method such as microwave heating drying and high-frequency dielectric heating drying
- an external heating method such as hot air drying and superheated steam drying.
- the entire molded body can be dried quickly and uniformly without cracks, and after drying a certain amount of moisture with an electromagnetic heating method, the remaining moisture is dried with an external heating method. It is preferable to make it.
- As drying conditions it is preferable to remove water of 30 to 99% by mass with respect to the amount of moisture before drying by an electromagnetic heating method, and then to make the moisture to 3% by mass or less by an external heating method.
- the electromagnetic heating method dielectric heating drying is preferable, and as the external heating method, hot air drying is preferable.
- the length of the honeycomb formed body in the cell extending direction is not a desired length, it is preferable to cut both end surfaces (both end portions) to a desired length.
- the cutting method is not particularly limited, and examples thereof include a method using a circular saw cutting machine.
- the honeycomb formed body (formed body) is fired to produce a honeycomb structure (porous material) (firing step).
- the calcination is preferably performed in an air atmosphere at 200 to 600 ° C. for 0.5 to 20 hours. Firing is preferably performed in a non-oxidizing atmosphere (inert atmosphere) such as nitrogen or argon (the oxygen partial pressure is 10 ⁇ 4 atm or less).
- the lower limit of the firing temperature is preferably 1300 ° C.
- the upper limit of the firing temperature is preferably 1600 ° C.
- the firing temperature is preferably 1400-1500 ° C.
- the pressure during firing is preferably normal pressure.
- the lower limit of the firing time is preferably 1 hour.
- the upper limit of the firing time is preferably 20 hours.
- the process of producing a porous material by firing the molded body at a predetermined temperature in an inert atmosphere is a firing process.
- an oxidation treatment may be performed in the atmosphere (which may contain water vapor) in order to improve durability.
- the lower limit of the oxidation treatment temperature is preferably 1100 ° C.
- the upper limit of the temperature of the oxidation treatment is preferably 1400 ° C.
- the lower limit of the oxidation treatment time is preferably 1 hour.
- the upper limit of the oxidation treatment time is preferably 20 hours.
- calcination and baking can be performed using an electric furnace, a gas furnace, etc., for example.
- the metal silicon content in the obtained porous material is less than 15% by mass.
- Example 1 The silicon carbide (SiC) powder and the composite binder producing raw material powder were mixed at a ratio of 7: 3 (volume ratio) to produce a “mixed powder”.
- a raw material powder for producing a composite binder a powder containing 45.1% by mass of aluminum hydroxide, 32.8% by mass of talc, and 22.1% by mass of silica was used.
- the content rate of the aluminum oxide component in the raw material (powder) for producing the composite binder was 35.6% by mass.
- the content rate of the silicon dioxide component in the raw material (powder) for composite binder production was 51.8% by mass.
- the content rate of the magnesium oxide component in the raw material (powder) for composite binder production was 12.6% by mass.
- hydroxypropylmethylcellulose as a binder, starch as a pore former, and a water-absorbing resin were added to the “mixed powder”, and water was added to obtain a molding raw material.
- the content of the binder was 7 parts by mass when the mixed powder was 100 parts by mass.
- the content of the pore former was 12 parts by mass when the mixed powder was 100 parts by mass.
- the water content was 70 parts by mass when the mixed powder was 100 parts by mass.
- the average particle diameter of the silicon carbide powder was 22.0 ⁇ m.
- the average particle diameter of the pore former was 20 ⁇ m.
- the average particle diameter of the silicon carbide powder and the pore former is a value measured by a laser diffraction method.
- the forming raw materials were kneaded and kneaded to prepare a columnar clay.
- the obtained cylindrical clay was formed into a honeycomb shape using an extrusion molding machine to obtain a honeycomb formed body.
- the obtained honeycomb formed body was dielectrically heated and dried, and then dried at 120 ° C. for 2 hours using a hot air dryer to obtain a honeycomb dried body.
- honeycomb dried body was degreased at 550 ° C. for 3 hours in an air atmosphere, and then fired at about 1450 ° C. for 2 hours in an Ar inert atmosphere to obtain a honeycomb fired body.
- honeycomb fired body was oxidized at 1200 ° C. for 4 hours to obtain a porous material having a honeycomb structure (honeycomb structure).
- the honeycomb structure at this time had a partition wall thickness of 300 ⁇ m and a cell density of 46.5 (cell / cm 2 ). Further, the bottom surface of the honeycomb structure was a square having a side of 35 mm, and the length of the honeycomb structure in the cell extending direction was 50 mm.
- the silicon carbide, mullite, and cordierite of the honeycomb structure were identified. Identification of silicon carbide, mullite and cordierite was performed based on the results of qualitative and quantitative analysis by EPMA and element mapping as well as identification of constituent phases by powder X-ray diffraction. Thereby, it was confirmed that the honeycomb structure includes silicon carbide, mullite, and cordierite.
- the aspect ratio of mullite particles was 4.7.
- the major axis length of the mullite particles was 2.5 ⁇ m.
- the “mullite content” was 0.5% by mass.
- the content of the composite binder in the porous material was 29.9% by mass.
- the major axis and aspect ratio of mullite particles were measured by the following methods. Moreover, the content rate of the mullite particle was measured by the method mentioned later.
- the resulting porous material (honeycomb structure) having a honeycomb structure had a porosity of 58.2% and an average pore diameter of 17.0 ⁇ m.
- the honeycomb structure had a bending strength of 6.5 MPa, a Young's modulus of 4.5 GPa, and a “strength / Young's modulus ratio” of 1.4 ⁇ 10 ⁇ 3 .
- the “strength” of “strength / Young's modulus ratio” is “bending strength”.
- the thermal expansion coefficient (40-800 ° C.) of the honeycomb structure was 3.2 ⁇ 10 ⁇ 6 K ⁇ 1 .
- the specific heat capacity of the honeycomb structure was 2.09 J / (cm 3 ⁇ K). The obtained results are shown in Table 1. Each measured value is a value obtained by the method shown below.
- the column “Binder” indicates the mass ratio (mass%) of the composite binder to the total mass of the silicon carbide particles, the composite binder, and the metal silicon.
- “composite binder” is simply indicated as “binder”.
- the column “mullite” indicates the mass ratio (mass%) of the mullite particles with respect to the total mass of the silicon carbide particles, the composite binder, and the metal silicon.
- the column “Metal Silicon” indicates the mass ratio (mass%) of metal silicon to the total mass of silicon carbide particles, composite binder, and metal silicon.
- the column “Mullite Aspect Ratio” indicates the aspect ratio of “Mullite Particles in Porous Material”.
- the column of “major diameter of mullite” indicates the major diameter of “mullite particles in the porous material”.
- the columns of “porosity” and “average pore diameter” indicate the porosity and average pore diameter of the porous material.
- the columns of “bending strength”, “Young's modulus” and “thermal expansion coefficient” indicate the bending strength, Young's modulus and thermal expansion coefficient of the porous material.
- the column “strength / Young's modulus ratio” indicates a value obtained by dividing the bending strength (Pa) by the Young's modulus (Pa).
- the column “Al source” in Table 4 indicates the type of aluminum source in the raw material for producing the composite binder.
- Each column of “Al source” and “Si source” in Table 7 indicates the type of aluminum source and the type of silicon source in the raw material for producing the composite binder.
- the column “Comprehensive evaluation” indicates that A to C are acceptable and D is unacceptable.
- a to C “A” indicates the most excellent thermal shock resistance.
- B indicates that the thermal shock resistance is excellent after “A”
- C indicates that the thermal shock resistance is excellent after “B”.
- D indicates poor thermal shock resistance.
- the conditions of the comprehensive evaluation A are: bending strength of 6.5 MPa or more, thermal expansion coefficient of 4.0 ⁇ 10 ⁇ 6 / K or less, “strength / Young's modulus ratio” of 1.6 or more, and specific heat capacity of 2.05 J / (cm 3 ⁇ K) All the conditions above are satisfied.
- the conditions of the comprehensive evaluation B were as follows: bending strength of 6.5 MPa or more, thermal expansion coefficient of 4.0 ⁇ 10 ⁇ 6 / K or less, “strength / Young's modulus ratio” of 1.2 or more, and specific heat capacity of 2.00 J / (Cm 3 ⁇ K) or more of all conditions are satisfied.
- the conditions of the comprehensive evaluation C are all the conditions in which the bending strength is 6.5 MPa or more, the thermal expansion coefficient is less than 4.5 ⁇ 10 ⁇ 6 / K, and the specific heat capacity is 1.95 J / (cm 3 ⁇ K) or more. It is to satisfy.
- the conditions of the comprehensive evaluation D are any of bending strength less than 6.5 MPa, thermal expansion coefficient of 4.5 ⁇ 10 ⁇ 6 / K or more, and specific heat capacity less than 1.95 J / (cm 3 ⁇ K). That one requirement is met.
- the mass ratio of each constituent crystal phase (composite binder, mullite particles, mass ratio of metal silicon) in the porous material (honeycomb structure) is determined as follows.
- An X-ray diffraction pattern of the porous material is obtained using an X-ray diffractometer.
- a rotating cathode type X-ray diffractometer RINT, manufactured by Rigaku Corporation
- the mass ratio of each constituent crystal phase is calculated by simple quantitative analysis “analyzing the obtained X-ray diffraction data using a RIR (Reference Intensity Ratio) method to quantify each component”.
- the analysis of the X-ray diffraction data was performed using “X-ray data analysis software JADE7” manufactured by MDI.
- the aspect ratio of mullite particles (the aspect ratio of mullite) is measured using an SEM (scanning electron microscope). Specifically, the major axis and minor axis of all the mullite particles in the microstructure photograph that can be observed at a magnification of 3000 times are measured, and the ratio “major axis / minor axis” is calculated to obtain the mullite in the microstructure photograph. The average value of the number of particles is defined as the mullite aspect ratio.
- the major axis of mullite particles is measured using a SEM (scanning electron microscope). Specifically, the major axis of all mullite particles in the microstructure photograph that can be observed at a magnification of 3000 times is measured, and the average value of the number of mullite particles in the microstructure photograph is taken as the major axis of mullite.
- total pore volume total pore volume
- the apparent density a test piece cut into a size of “20 mm ⁇ 20 mm ⁇ 0.3 mm” (corresponding to one partition wall having a size of 20 mm ⁇ 20 mm) is used.
- test piece having a size of “3 vertical cells ⁇ 3 horizontal cells ⁇ 20 mm length” is cut out from the honeycomb structure, and measured by a mercury intrusion method (JIS R 1655 compliant).
- Pore volume ratio The “pore volume ratio of 10 ⁇ m or less” and the “pore volume ratio of 40 ⁇ m or more” are measured as follows. Using a test piece similar to the case of the above “average pore diameter”, the total pore volume by the mercury intrusion method (according to JIS R 1655), the pore volume of the pore having a pore diameter of 40 ⁇ m or more, and the pore diameter is 10 ⁇ m. The pore volume of the following pores is measured.
- Pore volume ratio of 10 ⁇ m or less is calculated by the formula of pore volume of 10 ⁇ m or less / total pore volume
- pore volume ratio of 40 ⁇ m or more is calculated by the formula of pore volume of 40 ⁇ m or more / total pore volume.
- the honeycomb structure is processed into a test piece (length 0.3 mm ⁇ width 4 mm ⁇ length 40 mm) whose longitudinal direction is the cell penetration direction, and bending strength is calculated by a bending test according to JIS R1601.
- Examples 2 to 35 Comparative Examples 1 to 6
- a porous material was produced in the same manner as in Example 1 except that the conditions were as shown in Tables 1 to 8.
- Each evaluation was performed in the same manner as in Example 1.
- the results are shown in Tables 1-7.
- Table 8 shows the contents of the aluminum oxide component, the silicon oxide component, and the magnesium oxide component in the composite binder producing raw material.
- generation, a silicon oxide component, and a magnesium oxide component was computed from the chemical composition and content rate of each used raw material.
- the porous material of the present invention can be used as a catalyst carrier material, a DPF material, or the like.
- the honeycomb structure of the present invention can be used as a catalyst carrier, DPF, or the like.
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Abstract
Description
本発明の多孔質材料の一の実施形態は、図1に示されるように、骨材1と、「結合材3であるコージェライト中に強化粒子2であるムライト粒子が分散されたものであり細孔4を形成した状態で上記骨材1同士を結合する複合結合材5」と、を含有するものである。そして、本実施形態の多孔質材料は、金属珪素の含有量が15質量%未満である。また、金属珪素の含有量は、ICP(Inductively Coupled Plasma)-AES(発光分光分析)法で測定したSi、C、OからSiCとSiO2量を同定し、残りのSi量の値である。図1は、本発明の多孔質材料の一の実施形態(多孔質材料100)の断面を拡大して示す模式図である。
本発明のハニカム構造体は、上述した本発明の多孔質材料により構成され、「一方の端面から他方の端面まで延びる複数のセル」を区画形成する隔壁、を備えたものである。上記セルは、流体の流路となるものである。また、ハニカム構造体は、最外周に位置する外周壁を有する構造であることが好ましい。隔壁の厚さの下限値は、30μmが好ましく、50μmが更に好ましい。隔壁の厚さの上限値は、1000μmが好ましく、500μmが更に好ましく、350μmが特に好ましい。セル密度の下限値は、10セル/cm2が好ましく、20セル/cm2が更に好ましく、50セル/cm2が特に好ましい。セル密度の上限値は、200セル/cm2が好ましく、150セル/cm2が更に好ましい。
本発明の多孔質材料の製造方法について、以下に説明する。以下に説明する多孔質材料の製造方法は、多孔質材料によって構成される「ハニカム構造体」を、製造する方法でもある。
炭化珪素(SiC)粉末と複合結合材生成用原料粉末とを、7:3(体積比)の比率で混合して「混合粉末」を作製した。複合結合材生成用原料粉末としては、水酸化アルミニウムを45.1質量%、タルクを32.8質量%、シリカを22.1質量%含有する粉末を用いた。複合結合材生成用原料(粉末)中の酸化アルミニウム成分の含有率は、35.6質量%であった。また、複合結合材生成用原料(粉末)中の二酸化珪素成分の含有率は、51.8質量%であった。また、複合結合材生成用原料(粉末)中の酸化マグネシウム成分の含有率は、12.6質量%であった。そして、上記「混合粉末」に、バインダとしてヒドロキシプロピルメチルセルロース、造孔材としてデンプン、吸水性樹脂を添加すると共に、水を添加して成形原料とした。バインダの含有量は混合粉末を100質量部としたときに、7質量部であった。造孔材の含有量は混合粉末を100質量部としたときに、12質量部であった。水の含有量は混合粉末を100質量部としたときに、70質量部であった。炭化珪素粉末の平均粒子径は22.0μmであった。また、造孔材の平均粒子径は、20μmであった。なお、炭化珪素粉末及び造孔材の平均粒子径は、レーザー回折法で測定した値である。
多孔質材料(ハニカム構造体)における、各構成結晶相(複合結合材、ムライト粒子、金属珪素)の質量比率は以下のようにして求める。X線回折装置を用いて多孔質材料のX線回折パターンを得る。X線回折装置としては、回転対陰極型X線回折装置(理学電機製、RINT)を用いる。X線回折測定の条件は、CuKα線源、50kV、300mA、2θ=10~60°とする。そして、「RIR(Reference Intensity Ratio)法を用いて、得られたX線回折データを解析して、各成分を定量する」簡易定量分析により、各構成結晶相の質量比率を算出する。X線回折データの解析は、MDI社製の「X線データ解析ソフトJADE7」を用いて行った。
ムライト粒子のアスペクト比(ムライトのアスペクト比)は、SEM(走査型電子顕微鏡)を用いて測定する。具体的には、3000倍の倍率で観察し得た微構造写真中の全てのムライト粒子の長径と短径を測定し、その比率「長径/短径」を算出し、微構造写真中のムライト粒子の個数で平均した値を、ムライトのアスペクト比とする。
ムライト粒子の長径は、SEM(走査型電子顕微鏡)を用いて測定する。具体的には、3000倍の倍率で観察し得た微構造写真中の全てのムライト粒子の長径を測定し、微構造写真中のムライト粒子の個数で平均した値を、ムライトの長径とする。
気孔率は、水銀圧入法(JIS R 1655準拠)による全細孔容積[cm3/g]と、アルキメデス法により測定した見掛密度[g/cm3]から算出する。気孔率の算出に際しては、「開気孔率(%)=100×全細孔容積/{(1/見掛密度)+全細孔容積}」の式を用いる。「全細孔容積」の測定(水銀圧入法)には、ハニカム構造体から「縦3セル×横3セル×長さ20mm」の大きさに切り出した試験片を用いる。また、見掛密度の測定(アルキメデス法)には、「20mm×20mm×0.3mm」の大きさ(20mm×20mmの大きさの1枚の隔壁に相当)に切り出した試験片を用いる。
ハニカム構造体から、「縦3セル×横3セル×長さ20mm」の大きさの試験片を切り出し、水銀圧入法(JIS R 1655準拠)により測定する。
「10μm以下の細孔容積率」及び「40μm以上の細孔容積率」は、以下のようにして測定する。上記「平均細孔径」の場合と同様の試験片を用いて、水銀圧入法(JIS R 1655準拠)により全細孔容積、細孔径が40μm以上である細孔の細孔容積、細孔径が10μm以下である細孔の細孔容積を測定する。そして、「10μm以下の細孔容積率」は10μm以下の細孔容積/全細孔容積、「40μm以上の細孔容積率」は40μm以上の細孔容積/全細孔容積の式で算出する。
ハニカム構造体をセルが貫通する方向を長手方向とした試験片(縦0.3mm×横4mm×長さ40mm)に加工し、JIS R1601に準拠した曲げ試験により曲げ強度を算出する。
上記「曲げ強度」の測定方法により「応力-歪曲線」を作成し、当該「応力-歪曲線」の傾きを算出する。得られた「応力-歪曲線の傾き」をヤング率とする。
JIS R1618に準拠する方法で、ハニカム構造体から縦3セル×横3セル×長さ20mmの試験片を切り出し、40~800℃のA軸方向(ハニカム構造体の流路に対して平行方向)の平均線熱膨張係数(熱膨張係数)を測定する。
ハニカム構造体から、直径0.5mm×厚さ1.0mmの円盤状の測定試料を切り出す。得られた測定試料を用いてJIS R1611に準拠する方法で、室温における比熱を測定する。更に、測定試料について、アルキメデス法で、見かけ密度を測定する。そして、得られた比熱の値と見かけ密度との積を比熱容量(J/(cm3・K))とする。
各条件を表1~8に示すものとした以外は実施例1と同様にして多孔質材料(ハニカム構造体)を作製した。実施例1の場合と同様にして、各評価を行った。結果を表1~7に示す。また、複合結合材生成用原料中の酸化アルミニウム成分、酸化珪素成分及び酸化マグネシウム成分の含有率を表8に示した。尚、複合結合材生成用原料中の酸化アルミニウム成分、酸化珪素成分及び酸化マグネシウム成分の含有率は、使用した各原料の化学組成及び含有率から算出した。
Claims (15)
- 骨材と、結合材であるコージェライト中に強化粒子であるムライト粒子が分散されたものであり細孔を形成した状態で前記骨材同士を結合する複合結合材と、を含有し、
金属珪素の含有量が15質量%未満である多孔質材料。 - 前記骨材、前記複合結合材及び前記金属珪素の合計質量に対する、前記複合結合材の含有量の下限値が12質量%であり、前記複合結合材の含有量の上限値が50質量%である請求項1に記載の多孔質材料。
- 前記骨材、前記複合結合材及び前記金属珪素の合計質量に対する、前記ムライト粒子の含有量の下限値が0.5質量%であり、前記ムライト粒子の含有量の上限値が15質量%である請求項1又は2に記載の多孔質材料。
- 強化粒子である前記ムライト粒子の長径の下限値が0.5μmであり、前記ムライト粒子の長径の上限値が35μmである請求項1~3のいずれかに記載の多孔質材料。
- 強化粒子である前記ムライト粒子のアスペクト比の下限値が1.5であり、前記ムライト粒子のアスペクト比の上限値が4.7である請求項1~4のいずれかに記載の多孔質材料。
- 前記骨材が、炭化珪素(SiC)粒子及び窒化珪素(Si3N4)粒子の中の少なくとも一方を含有するものである請求項1~5のいずれかに記載の多孔質材料。
- 気孔率の下限値が40%であり、気孔率の上限値が90%である請求項1~6のいずれかに記載の多孔質材料。
- 細孔径10μm未満の細孔が細孔全体の20%以下であり、細孔径40μmを超える細孔が細孔全体の10%以下である請求項1~7のいずれかに記載の多孔質材料。
- 曲げ強度が6.5MPa以上であり、曲げ強度/ヤング率比が1.4×10-3以上である請求項1~8のいずれかに記載の多孔質材料。
- 熱膨張係数が4.2×10-6/K以下である請求項1~9のいずれかに記載の多孔質材料。
- 請求項1~10のいずれかに記載の多孔質材料により構成され、
一方の端面から他方の端面まで延びる複数のセルを区画形成する、隔壁を備えたハニカム構造体。 - 前記一方の端面における所定の前記セルの開口部及び前記他方の端面における残余の前記セルの開口部、に配設された目封止部を備える請求項11に記載のハニカム構造体。
- 骨材原料、複合結合材生成用原料、造孔材及びバインダを含有する成形原料を押出成形して成形体を作製する成形工程と、
前記成形体を不活性雰囲気にて1400~1500℃で焼成して多孔質材料を作製する焼成工程とを有し、
前記複合結合材生成用原料が、34.9質量%超、71.8質量%未満の酸化アルミニウム成分、28.2質量%超、52.0質量%未満の二酸化珪素成分、及び5.0質量%超、13.8質量%未満の酸化マグネシウム成分を含有し、
前記多孔質材料中の金属珪素含有量が15質量%未満であり、
前記複合結合材生成用原料中に、金属珪素が含有されないか、又は得られる前記多孔質材料中の金属珪素含有量が15質量%未満となるような量の金属珪素が含有される、多孔質材料の製造方法。 - 前記複合結合材生成用原料に含有される前記酸化アルミニウム成分が酸化アルミニウムであり、前記酸化アルミニウムの平均粒子径が、下限値2.5μm、上限値15.0μmである請求項13に記載の多孔質材料の製造方法。
- 前記複合結合材生成用原料に含有される前記酸化アルミニウムが、α-アルミナである請求項14に記載の多孔質材料の製造方法。
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EP2784042A1 (en) * | 2013-03-27 | 2014-10-01 | NGK Insulators, Ltd. | Porous material, honeycomb structure, and method of manufacturing porous material |
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JP2015166573A (ja) * | 2014-03-04 | 2015-09-24 | 日本碍子株式会社 | ハニカム構造体 |
JP2015171981A (ja) * | 2014-03-12 | 2015-10-01 | 日本碍子株式会社 | ハニカム構造体 |
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DE102017009873A1 (de) | 2016-10-24 | 2018-04-26 | Ngk Insulators, Ltd. | Poröses Material, Wabenstruktur und Verfahren zur Herstellung eines porösen Materials |
CN107973618A (zh) * | 2016-10-24 | 2018-05-01 | 日本碍子株式会社 | 多孔质材料、蜂窝结构体、以及多孔质材料的制造方法 |
JP2018154546A (ja) * | 2016-10-24 | 2018-10-04 | 日本碍子株式会社 | 多孔質材料、ハニカム構造体および多孔質材料の製造方法 |
JP2018199608A (ja) * | 2016-10-24 | 2018-12-20 | 日本碍子株式会社 | 多孔質材料、ハニカム構造体、及び多孔質材料の製造方法 |
DE102017009873B4 (de) | 2016-10-24 | 2019-12-12 | Ngk Insulators, Ltd. | Gebranntes, poröses Material und Wabenstruktur |
US10557393B2 (en) | 2016-10-24 | 2020-02-11 | Ngk Insulators, Ltd. | Porous material, honeycomb structure, and method of producing porous material |
JP6991020B2 (ja) | 2016-10-24 | 2022-01-12 | 日本碍子株式会社 | 多孔質材料、ハニカム構造体、及び多孔質材料の製造方法 |
JP2019167278A (ja) * | 2018-03-26 | 2019-10-03 | 日本碍子株式会社 | 多孔質材料、セル構造体および多孔質材料の製造方法 |
JP7051524B2 (ja) | 2018-03-26 | 2022-04-11 | 日本碍子株式会社 | 多孔質材料、セル構造体および多孔質材料の製造方法 |
CN112430123A (zh) * | 2020-12-07 | 2021-03-02 | 重庆奥福精细陶瓷有限公司 | 一种窄孔径分布、大尺寸堇青石汽油颗粒过滤器及其制备方法 |
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US9358529B2 (en) | 2016-06-07 |
EP2832712B1 (en) | 2017-08-09 |
US20140370232A1 (en) | 2014-12-18 |
EP2832712A1 (en) | 2015-02-04 |
JP6043340B2 (ja) | 2016-12-14 |
JPWO2013146953A1 (ja) | 2015-12-14 |
EP2832712A4 (en) | 2015-12-16 |
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