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Definitions

• the present invention relates to a method for producing a fired body made of an aluminum titanate ceramic, and more specifically, a fired body made of an aluminum titanate ceramic by firing a molded body of a raw material mixture containing an aluminum source powder and a titanium source powder. It relates to a method of manufacturing.
• Aluminum titanate ceramics are known as ceramics containing titanium and aluminum as constituent elements and having a crystal pattern of aluminum titanate in an X-ray diffraction spectrum, having excellent heat resistance and low thermal expansion. Yes.
• Aluminum titanate-based ceramics have been used as a sintering tool such as a crucible, and in recent years, fine carbon particles contained in exhaust gas discharged from internal combustion engines such as diesel engines have been collected.
• a ceramic filter Diesel particulate filter
• Patent Document 1 a method of firing a raw material mixture containing a powder of a titanium source compound such as titania and an aluminum source compound such as alumina is known (Patent Document 1).
• the present invention provides a method for producing an aluminum titanate-based ceramic fired body in which cracking of the ceramic molded body in the degreasing process is suppressed and the ceramic molded body has sufficient strength for handling when the ceramic molded body is moved to the firing process. For the purpose.
• the present invention provides a molding step of forming a raw material mixture containing an inorganic component containing an aluminum source powder and a titanium source powder and an organic component to obtain a ceramic molded body, A degreasing step of removing the organic component contained in the ceramic molded body under a temperature condition where the maximum temperature is 700 ° C. or higher and 1100 ° C. or lower in an atmosphere having an oxygen concentration of 0.1% or less; and Including a firing step of firing the ceramic molded body at a maximum temperature of 1300 ° C. or higher in this order,
• the atmosphere in the temperature raising process up to 1300 ° C. in the firing step is an oxygen concentration of 1% to 6%.
• the ceramic formed body is held at the highest temperature in the degreasing step, and in the firing step, the ceramic formed body is held at the highest temperature in the firing step.
• the ceramic molded body is fired in an atmosphere having an oxygen concentration higher than 5% after the temperature raising process up to 1300 ° C. in the firing step.
• the inorganic component preferably further contains a magnesium source powder and / or a silicon source powder.
• the total amount of organic components contained in the ceramic molded body is preferably 10 parts by mass or more and less than 50 parts by mass with respect to 100 parts by mass of the total amount of the ceramic molded body.
• the organic component preferably contains a pore-forming agent, and the pore-forming agent is preferably polyethylene, corn starch or potato starch.
• the ceramic molded body has a honeycomb shape, the cross-sectional area of the bottom surface in the arrangement in the degreasing step is 78.5 cm 2 or more, and the height is 5 cm or more.
• the degreasing step it is preferable that a part of the organic component is removed and the remainder is carbonized.
• the molar ratio of the Al 2 O 3 converted aluminum source powder to the TiO 2 converted titanium source powder is 35:65 to 45:55, or (ii) Al 2 O of 3 converted to aluminum source powder and the total amount of the titanium source powder in terms of TiO 2, the molar ratio of the magnesium source powder in terms of MgO is, and it is 0.03 ⁇ 0.15, (iii) silicon in terms of SiO 2
• the content of the source powder is preferably 0.1 to 10 parts by mass with respect to 100 parts by mass of the total amount of the aluminum source powder converted to Al 2 O 3 and the titanium source powder converted to TiO 2 .
• the oxygen concentration at the time of temperature rise (degreasing step) to a concentration of 0.1% or less
• heat generation of organic substances can be suppressed and cracking after degreasing can be suppressed.
• a small amount of carbon remains in the ceramic formed body after the degreasing process (before firing), the strength of the formed body is improved, and the ceramic formed body can be easily moved to the firing process.
• the strength of the ceramic formed body after the degreasing process is improved by grain growth. Transfer to the process becomes easy.
• the aluminum titanate-based ceramic fired body of the present invention is manufactured by degreasing and firing a formed body of a raw material mixture containing an inorganic component containing an aluminum source powder and a titanium source powder and an organic component.
• the aluminum titanate-based ceramic fired body obtained using such a raw material mixture is a fired body made of aluminum titanate-based crystals.
• the aluminum source powder contained in the raw material mixture used in the present invention is a powder of a substance that becomes an aluminum component constituting the aluminum titanate-based ceramic fired body.
• the aluminum source powder include alumina (aluminum oxide) powder.
• Alumina may be crystalline or amorphous (amorphous).
• examples of the crystal type include ⁇ -type, ⁇ -type, ⁇ -type, and ⁇ -type. Of these, ⁇ -type alumina is preferably used.
• the aluminum source powder used in the present invention may be a powder of a substance led to alumina by firing in air.
• a substance led to alumina by firing in air examples include an aluminum salt, aluminum alkoxide, aluminum hydroxide, and metal aluminum.
• the aluminum salt may be a salt with an inorganic acid or a salt with an organic acid.
• the inorganic salt include nitrates such as aluminum nitrate and ammonium aluminum nitrate; aluminum carbonates such as ammonium aluminum carbonate and the like.
• the aluminum organic salt include aluminum oxalate, aluminum acetate, aluminum stearate, aluminum lactate, and aluminum laurate.
• aluminum alkoxide examples include aluminum isopropoxide, aluminum ethoxide, aluminum sec-butoxide, aluminum tert-butoxide, and the like.
• Aluminum hydroxide may be crystalline or amorphous (amorphous).
• the crystal type include a gibbsite type, a bayerite type, a norosotrandite type, a boehmite type, and a pseudoboehmite type.
• the amorphous aluminum hydroxide include an aluminum hydrolyzate obtained by hydrolyzing an aqueous solution of a water-soluble aluminum compound such as an aluminum salt or an aluminum alkoxide.
• the aluminum source powder only one kind may be used, or two or more kinds may be used in combination.
• alumina powder is preferably used as the aluminum source powder, and more preferably ⁇ -type alumina powder.
• the aluminum source powder can contain trace components derived from the raw materials or inevitably contained in the production process.
• a commercially available aluminum source powder is classified by sieving or the like.
• B A commercially available aluminum source powder is granulated using a granulator or the like.
• the volume-based cumulative percentage 50% equivalent particle diameter (D50) measured by a laser diffraction method of the aluminum source powder to be used is preferably 20 ⁇ m or more and 60 ⁇ m or less.
• D50 of the aluminum source powder is more preferably 25 ⁇ m or more and 60 ⁇ m or less, and further 30 ⁇ m or more and 60 ⁇ m or less.
• the titanium source powder contained in the raw material mixture is a powder of a substance that becomes a titanium component constituting the aluminum titanate-based ceramic fired body.
• a substance include titanium oxide powder.
• titanium oxide include titanium (IV) oxide, titanium (III) oxide, and titanium (II) oxide, and titanium (IV) oxide is preferably used.
• Titanium (IV) oxide may be crystalline or amorphous (amorphous). When the titanium (IV) oxide is crystalline, examples of the crystal form include anatase type, rutile type, brookite type, and the like. More preferred is anatase type or rutile type titanium (IV) oxide.
• the titanium source powder used in the present invention may be a powder of a substance that is led to titania (titanium oxide) by firing in air.
• titania titanium oxide
• examples of such substances include titanium salts, titanium alkoxides, titanium hydroxide, titanium nitride, titanium sulfide, and titanium metal.
• titanium salt examples include titanium trichloride, titanium tetrachloride, titanium sulfide (IV), titanium sulfide (VI), and titanium sulfate (IV).
• titanium alkoxide examples include titanium (IV) ethoxide, titanium (IV) methoxide, titanium (IV) tert-butoxide, titanium (IV) isobutoxide, titanium (IV) n-propoxide, titanium (IV) tetraiso Examples thereof include propoxide and chelates thereof.
• titanium source powder only one kind may be used, or two or more kinds may be used in combination.
• the titanium source powder a titanium oxide powder is preferably used, and a titanium (IV) oxide powder is more preferable.
• the titanium source powder may contain a trace component derived from the raw material or inevitably contained in the production process.
• the particle size of the titanium source powder is not particularly limited, but a titanium source powder having a volume-based cumulative percentage 50% equivalent particle size (D50) of 0.1 to 25 ⁇ m as measured by a laser diffraction method is usually used. In order to achieve a low firing shrinkage ratio, it is preferable to use a titanium source powder having a D50 of 1 to 20 ⁇ m.
• the titanium source powder may exhibit a bimodal particle size distribution. When using a titanium source powder exhibiting such a bimodal particle size distribution, the particle size measured by a laser diffraction method is used.
• the particle diameter of the particle forming the larger peak is preferably 20 to 50 ⁇ m.
• the mode diameter of the titanium source powder measured by the laser diffraction method is not particularly limited, but a mode diameter of 0.1 to 60 ⁇ m can be used.
• the molar ratio of the aluminum source powder in terms of Al 2 O 3 (alumina) and the titanium source powder in terms of TiO 2 (titania) in the raw material mixture is set to 35:65 to 45:55. It is preferably 40:60 to 45:55. Within such a range, by increasing the ratio of the titanium source powder to the aluminum source powder, it becomes possible to more effectively reduce the firing shrinkage rate of the molded body of the raw material mixture.
• the raw material mixture may contain a magnesium source powder.
• the obtained aluminum titanate ceramic fired body is a fired body made of aluminum magnesium titanate crystals.
• the magnesium source powder include magnesia (magnesium oxide) powder and a powder of a substance introduced into magnesia by firing in air. Examples of the latter include magnesium salt, magnesium alkoxide, magnesium hydroxide, magnesium nitride, metal magnesium and the like.
• magnesium salts include magnesium chloride, magnesium perchlorate, magnesium phosphate, magnesium pyrophosphate, magnesium oxalate, magnesium nitrate, magnesium carbonate, magnesium acetate, magnesium sulfate, magnesium citrate, magnesium lactate, magnesium stearate, Examples include magnesium salicylate, magnesium myristate, magnesium gluconate, magnesium dimethacrylate, and magnesium benzoate.
• the magnesium alkoxide include magnesium methoxide and magnesium ethoxide.
• the magnesium source powder may contain a trace component derived from the raw material or unavoidably contained in the production process.
• the magnesium source powder a powder of a compound serving both as a magnesium source and an aluminum source can be used.
• An example of such a compound is magnesia spinel (MgAl 2 O 4 ).
• the magnesium source powder the case of using a powder of a compound serving both as a magnesium source and an aluminum source, Al 2 O 3 (alumina) in terms of the aluminum source powder, and a compound serving both as a magnesium source and aluminum source powder.
• the molar ratio of the total amount of Al 2 O 3 (alumina) equivalent of the Al component contained in the TiO 2 (titania) equivalent of the titanium source powder is adjusted to be within the above range in the raw material mixture.
• magnesium source powder only one kind may be used, or two or more kinds may be used in combination.
• the particle size of the magnesium source powder is not particularly limited, but a material having a volume-based cumulative percentage 50% equivalent particle size (D50) of 0.5 to 30 ⁇ m, usually measured by a laser diffraction method, is used. From the viewpoint of reducing the firing shrinkage rate of the mixture molded body, it is preferable to use a magnesium source powder having a D50 of 3 to 20 ⁇ m.
• the content of magnesium source powder in terms of MgO (magnesia) in the raw material mixture is based on the total amount of aluminum source powder in terms of Al 2 O 3 (alumina) and titanium source powder in terms of TiO 2 (titania).
• the molar ratio is preferably 0.03 to 0.15, more preferably 0.03 to 0.13, and still more preferably 0.03 to 0.12.
• the raw material mixture may further contain a silicon source powder.
• the silicon source powder is a powder of a substance contained in the aluminum titanate ceramic fired body as a silicon component, and by using the silicon source powder in combination, a heat-resistant aluminum titanate ceramic fired body is obtained. Is possible.
• Examples of the silicon source powder include powders of silicon oxide (silica) such as silicon dioxide and silicon monoxide.
• the silicon source powder may be a powder of a substance that is guided to silica by firing in air.
• examples of such substances include silicic acid, silicon carbide, silicon nitride, silicon sulfide, silicon tetrachloride, silicon acetate, sodium silicate, sodium orthosilicate, feldspar, and glass frit.
• feldspar, glass frit and the like are preferably used, and glass frit and the like are more preferably used because they are easily available industrially and have a stable composition.
• Glass frit means flakes or powdery glass obtained by pulverizing glass. It is also preferable to use a powder made of a mixture of feldspar and glass frit as the silicon source powder.
• the yield point of the glass frit is determined by measuring the expansion of the glass frit by raising the temperature from a low temperature using a thermomechanical analyzer (TMA: Thermo Mechanical Analysis), and then the shrinkage occurs. It is defined as the starting temperature (° C).
• a general silicate glass containing silicate [SiO 2 ] as a main component can be used as the glass constituting the glass frit.
• the glass constituting the glass frit includes, as other components, alumina [Al 2 O 3 ], sodium oxide [Na 2 O], potassium oxide [K 2 O], calcium oxide [ CaO], magnesia [MgO] and the like may be included.
• the glass constituting the glass frit may contain ZrO 2 in order to improve the hot water resistance of the glass itself.
• silicon source powder only one type may be used, or two or more types may be used in combination.
• the particle size of the silicon source powder is not particularly limited, but a material having a volume-based cumulative particle size equivalent to 50% on a volume basis (D50) of 0.5 to 30 ⁇ m, usually measured by a laser diffraction method, is used. In order to further improve the filling rate of the molded body of the mixture and obtain a fired body having higher mechanical strength, it is preferable to use a silicon source powder having a D50 of 1 to 20 ⁇ m.
• the content of the silicon source powder in terms of SiO 2 (silica) in the raw material mixture is expressed in terms of Al 2 O 3 (alumina) in terms of aluminum source powder and TiO 2 (titania).
• the total amount with respect to 100 parts by weight of the titanium source powder is usually 0.1 to 10 parts by weight, preferably 5 parts by weight or less.
• the silicon source powder may contain trace components that are derived from the raw materials or inevitably contained in the production process.
• a compound containing two or more metal elements among titanium, aluminum, silicon and magnesium as a composite oxide such as magnesia spinel (MgAl 2 O 4 ) is used as a raw material powder.
• a compound containing two or more metal elements among titanium, aluminum, silicon and magnesium as a composite oxide such as magnesia spinel (MgAl 2 O 4 ) is used as a raw material powder.
• such a compound can be considered to be the same as the raw material mixture in which the respective metal source compounds are mixed, and based on such an idea, the aluminum source raw material, the titanium source raw material, the magnesium source in the raw material mixture are considered. Content of a raw material and a silicon source raw material is adjusted in the said range.
• the raw material mixture may contain aluminum titanate or aluminum magnesium titanate itself.
• the aluminum magnesium titanate when aluminum magnesium titanate is used as a constituent of the raw material mixture, contains a titanium source, It corresponds to a raw material having both an aluminum source and a magnesium source.
• an organic component such as a pore-forming agent, a binder, a lubricant and a plasticizer, a dispersant, and a solvent is further added to the raw material mixture.
• the pore former examples include carbon materials such as graphite; resins such as polyethylene, polypropylene and polymethyl methacrylate; plant materials such as starch, nut shells, walnut shells and corn; ice; and dry ice. It is done.
• polyethylene, corn starch, potato starch and the like generate a large amount of heat during combustion, and therefore the production method of the present invention is particularly effective when polyethylene, corn starch, potato starch or the like is used as a pore-forming agent.
• the amount of pore-forming agent added is usually 0 to 40 parts by mass, preferably 0 to 25 parts by mass with respect to 100 parts by mass of the total amount of aluminum source powder, titanium source powder, magnesium source powder and silicon source powder. It is.
• binder examples include celluloses such as methyl cellulose, carboxymethyl cellulose, and sodium carboxymethyl cellulose; alcohols such as polyvinyl alcohol; salts such as lignin sulfonate; waxes such as paraffin wax and microcrystalline wax; EVA, polyethylene, polystyrene, liquid crystal Examples thereof include thermoplastic resins such as polymers and engineering plastics.
• the addition amount of the binder is usually 20 parts by mass or less, preferably 15 parts by mass or less, with respect to 100 parts by mass of the total amount of the aluminum source powder, the titanium source powder, the magnesium source powder and the silicon source powder.
• the lubricant and plasticizer examples include alcohols such as glycerin; higher fatty acids such as caprylic acid, lauric acid, palmitic acid, alginic acid, oleic acid and stearic acid; and stearic acid metal salts such as Al stearate.
• the addition amount of the lubricant and the plasticizer is usually 0 to 10 parts by mass, preferably 1 to 7 parts per 100 parts by mass of the total amount of the aluminum source powder, titanium source powder, magnesium source powder and silicon source powder. Part by mass, more preferably 1 to 5 parts by mass.
• the dispersant examples include inorganic acids such as nitric acid, hydrochloric acid and sulfuric acid; organic acids such as oxalic acid, citric acid, acetic acid, malic acid and lactic acid; alcohols such as methanol, ethanol and propanol; ammonium polycarboxylate; Surfactants such as polyoxyalkylene alkyl ethers may be mentioned.
• the addition amount of the dispersant is usually 0 to 20 parts by mass, preferably 2 to 8 parts by mass with respect to 100 parts by mass of the total amount of the aluminum source powder, titanium source powder, magnesium source powder and silicon source powder. is there.
• the solvent for example, alcohols such as monools (methanol, ethanol, butanol, propanol, etc.) and glycols (propylene glycol, polypropylene glycol, ethylene glycol, etc.); and water can be used. Of these, water is preferable, and ion-exchanged water is more preferably used from the viewpoint of few impurities.
• the amount of the solvent used is usually 10 parts by mass to 100 parts by mass, preferably 20 parts by mass to 80 parts by mass with respect to 100 parts by mass of the total amount of the aluminum source powder, titanium source powder, magnesium source powder and silicon source powder. It is.
• the total amount of organic components such as the pore-forming agent, binder, lubricant and plasticizer, dispersant, and solvent described above is based on 100 parts by mass of the ceramic molded body (that is, the total amount of the inorganic component and the organic component).
• the amount is preferably 10 parts by mass or more and less than 50 parts by mass, more preferably 15 parts by mass or more and 30 parts by mass or less.
• the raw material mixture to be used for molding is to mix (knead) the above-mentioned aluminum source powder, titanium source powder, inorganic components such as magnesium source powder and silicon source powder that are optionally used, and the above-mentioned various organic components. Can be obtained.
• a raw material mixture containing the above-mentioned aluminum source powder, titanium source powder, and inorganic components such as magnesium source powder and silicon source powder optionally used, and organic components (various additives) is molded.
• the formed body is subjected to a degreasing process and a firing process to obtain an aluminum titanate ceramic fired body.
• a porous aluminum titanate-based ceramic fired body having an aluminum titanate crystal whose pore shape is maintained can be obtained.
• the shape of the ceramic molded body is not particularly limited, and examples thereof include a honeycomb shape, a rod shape, a tube shape, a plate shape, and a crucible shape.
• the honeycomb shape is preferable, and the cross-sectional area of the bottom surface in the arrangement in the degreasing process described later is preferably 78.5 cm 2 or more and the height is preferably 5 cm or more.
• the molding machine used for molding the raw material mixture into a ceramic molded body include a uniaxial press, an extrusion molding machine, a tableting machine, and a granulator.
• the ceramic molded body is subjected to a degreasing step for removing organic components such as an organic binder contained in the ceramic molded body (in the raw material mixture) before being subjected to the firing step.
• the degreasing step is performed in an atmosphere having an oxygen concentration of 0.1% or less.
• “%” used as a unit of oxygen concentration means “volume%”.
• the degreasing step By performing the degreasing step in an atmosphere having an oxygen concentration of 0.1% or less, in the degreasing step, a part of the organic component is removed, and the remainder is carbonized and remains in the ceramic molded body. Thus, the trace amount of carbon remains in the ceramic molded body, whereby the strength of the molded body is improved and the ceramic molded body can be easily moved to the firing step.
• an atmosphere include an inert gas atmosphere such as nitrogen gas and argon gas, a reducing gas atmosphere such as carbon monoxide gas and hydrogen gas, and a vacuum.
• the oxygen concentration may be reduced by firing in an atmosphere with a low water vapor partial pressure or steaming with charcoal.
• the maximum temperature of the degreasing process is 700 ° C. or higher and 1100 ° C. or lower. More preferably, it is 800 degreeC or more and 1000 degrees C or less.
• the strength of the ceramic molded body after the degreasing process is improved by grain growth. Is easy to move.
• a temperature rising rate means each temperature rising rate in each temperature rising process except a holding process.
• Degreasing is usually used for normal firing of tubular electric furnaces, box-type electric furnaces, tunnel furnaces, far-infrared furnaces, microwave heating furnaces, shaft furnaces, reflection furnaces, rotary furnaces, roller hearth furnaces, gas combustion furnaces, etc. It is carried out using a furnace similar to the above. Degreasing may be performed batchwise or continuously. Moreover, you may carry out by a stationary type and may carry out by a fluid type.
• the ceramic molded body In the degreasing step, it is preferable to hold the ceramic molded body at the above-described maximum temperature (700 ° C. or higher and 1100 ° C. or lower).
• the time required for degreasing is sufficient as long as a part of the organic components contained in the ceramic molded body disappears.
• the organic component contained in the ceramic molded body that is, included in the raw material mixture. 90% by mass or more and 99% by mass or less of the total amount of organic components to be eliminated.
• the time for holding the ceramic formed body at the maximum temperature is usually 1 minute to 10 hours, preferably 1-7 hours. After maintaining at the maximum temperature, it may be cooled to room temperature (for example, 20 ° C. to 25 ° C.), and the rate of temperature decrease is, for example, 70 to 120 ° C./hour.
• the ceramic molded body is subjected to a firing step after the above degreasing step.
• the maximum temperature (firing temperature) in the firing step is usually 1300 ° C. or higher, preferably 1400 ° C. or higher.
• the firing temperature is usually 1650 ° C. or lower, preferably 1550 ° C. or lower.
• the rate of temperature increase up to the firing temperature is not particularly limited, but is usually 1 ° C./hour to 500 ° C./hour.
• the temperature rise to 1300 ° C. is performed in an atmosphere having an oxygen concentration of 1% to 6%.
• the oxygen concentration By setting the oxygen concentration to 6% or less, combustion of residual carbides generated in the degreasing process can be suppressed, so that the ceramic molded body is less likely to crack in the firing process.
• the organic component of the finally obtained aluminum titanate ceramic fired body can be completely removed.
• the organic component carbide (soot) may remain in the obtained aluminum titanate ceramic fired body.
• raw material powder that is, aluminum source powder, titanium source powder, magnesium source powder, and silicon source powder and the usage ratio
• it may be fired in an inert gas such as nitrogen gas or argon gas, or may be oxidized.
• You may bake in reducing gas, such as carbon gas and hydrogen gas. Further, the firing may be performed in an atmosphere in which the water vapor partial pressure is lowered.
• the temperature is raised to 1300 ° C.
• firing in an atmosphere having an oxygen concentration higher than 5% that is, holding at the maximum temperature
• the atmosphere from 1300 ° C. to the firing temperature may have an oxygen concentration of 1% to 6% or higher than 5%.
• a firing furnace similar to the furnace used for degreasing described above can be used. Firing may be performed batchwise or continuously. Moreover, you may carry out by a stationary type and may carry out by a fluid type.
• the time required for firing may be sufficient time for the formed body of the raw material mixture to transition to the aluminum titanate crystal, and the amount of the raw material mixture, although it depends on the type, firing temperature, firing atmosphere, etc., it is usually 10 minutes to 24 hours.
• the desired aluminum titanate ceramic fired body can be obtained.
• Such an aluminum titanate-based ceramic fired body has a shape that substantially maintains the shape of the formed body immediately after forming.
• the obtained aluminum titanate-based ceramic fired body can be processed into a desired shape by grinding or the like.
• the aluminum titanate-based ceramic fired body obtained by the present invention may contain a crystal pattern of alumina, titania or the like in addition to the crystal pattern of aluminum titanate or aluminum magnesium titanate in the X-ray diffraction spectrum.
• the aluminum titanate-based ceramic fired body of the present invention is composed of aluminum magnesium titanate crystals, it can be represented by the composition formula: Al 2 (1-x) Mg x Ti (1 + x) O 5 , x Is 0.03 or more, preferably 0.03 or more and 0.15 or less, more preferably 0.03 or more and 0.12 or less.
• the aluminum titanate-based ceramic fired body obtained by the present invention can contain trace components that are derived from raw materials or inevitably contained in the production process.
• the aluminum titanate ceramic fired body of the present invention is a porous ceramic mainly composed of aluminum titanate crystals.
• “Mainly composed of an aluminum titanate-based crystal” means that the main crystal phase constituting the aluminum titanate-based ceramic fired body is an aluminum titanate-based crystal phase (for example, the aluminum titanate-based crystal phase is 80% or more).
• the aluminum titanate-based crystal phase may be, for example, an aluminum titanate crystal phase, an aluminum magnesium titanate crystal phase, or the like.
• the aluminum titanate-based ceramic fired body of the present invention may contain a phase (crystal phase) other than the aluminum titanate-based crystal phase.
• the phase (crystalline phase) other than the aluminum titanate-based crystal phase include a phase derived from a raw material used for producing an aluminum titanate-based ceramic fired body. More specifically, the raw material-derived phase refers to the aluminum source powder remaining without forming the aluminum titanate-based crystal phase when the aluminum titanate-based ceramic fired body of the present invention is manufactured according to the above-described manufacturing method. , A phase derived from a titanium source powder and / or a magnesium source powder. Further, when the raw material mixture containing a silicon source powder, an aluminum titanate-based ceramics fired body includes phase from the silicon source powder of glass phase or the like including a SiO 2 component.
• the shape of the aluminum titanate ceramic fired body of the present invention is not particularly limited, and may be a honeycomb shape, a rod shape, a tube shape, a plate shape (sheet shape), a crucible shape, or the like.
• a honeycomb shape is preferable.
• the open porosity of the aluminum titanate-based ceramic fired body By setting the open porosity of the aluminum titanate-based ceramic fired body to 35% or more, when the aluminum titanate-based ceramic fired body is used as a ceramic filter such as a DPF, collection of collected matter such as diesel particulates is collected. While the capacity (adsorption capacity) is improved, the pressure loss of the gas to be filtered (exhaust gas discharged from the diesel engine, etc.) is reduced, and a ceramic filter having excellent filter performance can be obtained.
• the upper limit of the open porosity of the aluminum titanate-based ceramic fired body is not particularly limited, but can be, for example, less than 45%.
• the open porosity of the ceramic fired body can be measured by, for example, the Archimedes method by immersion in water.
• the aluminum titanate ceramic fired body of the present invention may contain a glass phase.
• the glass phase refers to an amorphous phase in which SiO 2 is a main component.
• the glass phase content is preferably 5% by mass or less, and more preferably 2% by mass or more.
• the above-described method for producing an aluminum titanate-based ceramic fired body is preferably used.
• an aluminum source powder, a titanium source powder, and a raw material mixture containing optional magnesium source powder and silicon source powder are molded to obtain a molded body, and then the molded body is fired.
• An aluminum acid based ceramic fired body can be obtained.
• the aluminum titanate ceramic fired body obtained by this method is an aluminum titanate ceramic fired body mainly composed of aluminum titanate crystals.
• the raw material mixture preferably contains a silicon source powder.
• the silicon source powder those described above can be used, and among them, glass frit, feldspar, or a mixture thereof is preferably used.
• the content of the silicon source powder is 2% by mass or more and 5% by mass or less in the inorganic component contained in the raw material mixture. More preferably.
• the inorganic component contained in the raw material mixture is a component containing an element constituting the aluminum titanate-based ceramic fired body, and is typically an aluminum source powder, a titanium source powder, a magnesium source powder, and a silicon source powder.
• the organic component additive such as a pore forming agent, a binder, a lubricant, a plasticizer, and a dispersant included in the raw material mixture includes an inorganic component, these are also included.
• the raw material mixture preferably contains a magnesium source powder.
• the preferable content of the magnesium source powder in the raw material mixture is as described above.
• the volume-based cumulative percentage particle diameter equivalent to 10% (D10), cumulative percentage 50% equivalent particle diameter (D50), and cumulative percentage 90% equivalent particle diameter (D90) of the raw powder is determined by laser.
• the particle size distribution was measured using a diffraction type particle size distribution analyzer (“Microtrac HRA (X-100)” manufactured by Nikkiso Co., Ltd.).
• Aluminum source powder Aluminum oxide powder ( ⁇ -alumina powder) having a center particle size (D50) of 29 ⁇ m 25.23 parts by mass (2) Titanium source powder Titanium oxide powder having a D50 of 1.0 ⁇ m (rutile crystal) 43.00 parts by mass (3) Magnesia spinel powder having a D50 of 5.5 ⁇ m 16.06 parts by mass (4) Glass frit having a D50 of 8.5 ⁇ m (“CK0832” manufactured by Takara Standard) 3.51 parts by mass (5) pore former (polyethylene powder) 12.20 parts by mass Methyl cellulose as a binder with respect to 100 parts by mass of the above mixture of aluminum source powder, titanium source powder, magnesium source powder, silicon source powder and pore former (polyethylene powder) After adding 5.49 parts by mass, 2.35 parts by mass of hydroxypropylmethylcellulose, 0.40 parts by mass of glycerin and 4.64 parts by mass of Unilube as a lubricant, and further adding 29.22 parts by mass of water as a dispersion medium
• honeycomb-shaped ceramic molded body (cell density of 300 cpsi, cell wall thickness of 0.3 mm) having a columnar shape with a diameter of 160 mm and a height of 260 mm and having many communicating holes in the height direction. ) was produced.
• Each raw material component is shown in Table 1.
• the mode diameter of titanium oxide (IV) was about 1 ⁇ m.
• Unilube (registered trademark) is a polyoxyalkylene compound manufactured by NOF Corporation.
• all of the pore-forming agent, binder and lubricant in Table 1 are components (organic substances) combusted by firing.
• the total amount of components other than the above combusting components ie, raw material powder
• the compounding amount of the titanium source powder in terms of titania is 49.0 parts by mass
• the compounding amount of the source powder is 41.8 parts by mass
• the compounding amount of the magnesium source powder in terms of magnesia is 5.2 parts by mass
• the compounding amount of the silicon source powder in terms of silica is 4.0 parts by mass (that is, in the glass frit
• the SiO 2 component was 100% by mass).
• the output of the obtained honeycomb-shaped ceramic molded body was set to about 1 W / 1 g according to the weight of the sample, and microwave drying was performed for 10 minutes. At this time, the size of the molded body contracted to about 150 mm in diameter by drying. The dried ceramic formed body was cut to a height of 215 mm. The weight was 2970 g.
• the black ceramic molded body in which about 0.5% by mass of the unburned organic matter remains is heated to 900 ° C. at a temperature rising rate of 50 ° C./hour in an atmosphere having an oxygen concentration of 2% by volume for 5 hours. I kept it. After that, the temperature was raised to about 1300 ° C. at a rate of temperature increase of 20 ° C./hour, and then the oxygen concentration was switched to 21% by volume. . Thereafter, the temperature was lowered at 100 ° C./hour to obtain one aluminum titanate ceramic fired body.
• Example 2 An aluminum titanate ceramic fired body was obtained in the same manner as in Example 1 except that the temperature rising profile in the degreasing step was as follows.
• an unsintered ceramic molded body was heated to 170 ° C. at a temperature rising rate of 50 ° C./hour in a nitrogen atmosphere having an oxygen concentration of 0.1% by volume or less, and then heated at a temperature rising rate of 30 ° C./hour to 600 Then, the temperature was raised to 1000 ° C. at a heating rate of 50 ° C./hour and kept for 4 hours. Thereafter, the temperature was lowered to 20 ° C. at 100 ° C./hour.
• the crushing strength of the honeycomb-shaped ceramic molded body (diameter: 25.4 mm, cell density: 300 cpsi, cell wall thickness: 0.3 mm) after the degreasing step was 1N (Newton).
• the aluminum titanate ceramic fired bodies obtained in Examples 1 and 2 were crushed in a mortar and the diffraction spectrum of the obtained powder was measured by powder X-ray diffractometry. A crystal peak of aluminum magnesium was shown. Moreover, the firing shrinkage ratio with respect to the ceramic molded body which shape
• the values of x when the aluminum titanate-based ceramic fired bodies obtained in Examples 1 and 2 are expressed by the composition formula: Al 2 (1-x) Mg x Ti (1 + x) O 5 are both 0 .12.
• Example 1 A honeycomb-shaped ceramic molded body was produced in the same manner as in Example 1, and the degreasing step was performed with the temperature rising profile as described below. In addition, since the total number (4 pieces) of the ceramic molded bodies was cracked after the degreasing process, the subsequent firing process was not performed.
• Example 2 A honeycomb-shaped ceramic molded body was produced in the same manner as in Example 1 except that the oxygen concentration in the degreasing step was 1% by volume, and the same degreasing step as in Example 2 was performed. In addition, since all the ceramic molded bodies were cracked after completion of the degreasing process (five pieces), the subsequent firing process was not performed.
• Example 3 A honeycomb-shaped ceramic molded body was produced in the same manner as in Example 1 except that the oxygen concentration in the degreasing process was 2% by volume, and the same degreasing process as in Example 2 was performed. In addition, since all the ceramic molded bodies were cracked after completion of the degreasing process (five pieces), the subsequent firing process was not performed.
• An aluminum titanate-based ceramic fired body obtained by the present invention includes, for example, firing furnace jigs such as crucibles, setters, mortars, and furnace materials; exhaust gas filters used for exhaust gas purification of internal combustion engines such as diesel engines and gasoline engines And ceramics such as a selective permeation filter for selectively permeating gas components generated during petroleum refining, such as carbon monoxide, carbon dioxide, nitrogen, oxygen, etc. Filter: It can be suitably applied to electronic parts such as substrates and capacitors. Especially, when using as a ceramics filter etc., since the aluminum titanate ceramic sintered body of this invention has a high pore volume and open porosity, it can maintain favorable filter performance over a long period of time.

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