WO2010053122A1 - チタン酸アルミニウム系セラミックスの製造方法 - Google Patents
チタン酸アルミニウム系セラミックスの製造方法 Download PDFInfo
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- WO2010053122A1 WO2010053122A1 PCT/JP2009/068904 JP2009068904W WO2010053122A1 WO 2010053122 A1 WO2010053122 A1 WO 2010053122A1 JP 2009068904 W JP2009068904 W JP 2009068904W WO 2010053122 A1 WO2010053122 A1 WO 2010053122A1
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
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- C04B2235/5481—Monomodal
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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
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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
- C04B2235/81—Materials characterised by the absence of phases other than the main phase, i.e. single phase materials
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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 present invention relates to a method for producing an aluminum titanate ceramic.
- Aluminum titanate-based ceramics are known as ceramics that contain titanium and aluminum as constituent elements and have a crystal pattern of aluminum titanate in the X-ray diffraction spectrum, and have excellent heat resistance.
- Aluminum titanate-based ceramics have been used as a sintering tool such as a crucible, but in recent years, fine carbon particles contained in exhaust gas discharged from internal combustion engines such as diesel engines are collected. As a material constituting a ceramic filter for industrial use, industrial utility value is increasing.
- an aluminum titanate ceramic there is known 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 (Patent Document 1). In order to be able to withstand use in the field, those having a small thermal expansion coefficient are required.
- An object of the present invention is to provide a new method capable of producing an aluminum titanate ceramic having a small thermal expansion coefficient.
- the present invention is a method for producing an aluminum titanate-based ceramics by firing a raw material mixture containing a titanium source powder, an aluminum source powder and a silicon source powder,
- the particle size (D50) equivalent to 50% of the cumulative percentage of the silicon source powder on a volume basis is 5 ⁇ m or less.
- the raw material mixture further contains a magnesium source powder.
- the firing temperature is preferably 1300 ° C. or higher and 1650 ° C. or lower.
- the silicon source powder has a 90% cumulative particle diameter (D90) of 17% or less on a volume basis, and the silicon source powder is preferably a glass frit.
- the particle size (D50) equivalent to 50% of the cumulative percentage on the volume basis of the titanium source powder is preferably 0.1 ⁇ m or more and 20 ⁇ m or less, and the particle diameter equivalent to 50% of the cumulative percentage on the volume basis of the aluminum source powder. (D50) is preferably 1 ⁇ m or more and 100 ⁇ m or less.
- the 50% cumulative particle size (D50) on a volume basis of the magnesium source powder is 0.5 ⁇ m or more and 20 ⁇ m or less.
- the amount of titanium source powder converted to titania is 30 to 70 parts by mass
- the amount of aluminum source powder converted to alumina is 30 to 70 parts by mass
- silica SiO 2
- the amount of silicon source powder used in conversion is preferably 0.1 parts by mass or more and 20 parts by mass or less.
- the raw material mixture contains a magnesium source powder
- the usage-amount of the magnesium source powder of magnesia (MgO) conversion is 0.1 mass part or more and 10 mass parts or less.
- the raw material mixture is preferably mixed dry or wet, and when dry or wet mixing, it is also preferable to pulverize and mix in a pulverization container in the presence of pulverization media.
- the grinding media is preferably alumina beads or zirconia beads having a diameter of 1 mm to 100 mm. Moreover, it is preferable to vibrate the pulverization container with an amplitude width of 2 mm or more and 20 mm or less.
- the method of the present invention preferably further includes a step of crushing the aluminum titanate ceramic fired product obtained after firing the raw material mixture.
- an aluminum titanate ceramic having a low thermal expansion coefficient can be produced using a raw material mixture containing a titanium source powder, an aluminum source powder, and a silicon source powder such as glass frit.
- the raw material mixture used in the present invention is a mixture containing one or more titanium source powders, one or more aluminum source powders, and one or more silicon source powders as raw material powders, and further one or more magnesium source powders. It is preferable to contain.
- the raw material mixture may contain aluminum titanate or aluminum magnesium titanate itself.
- the aluminum magnesium titanate is a titanium source powder or an aluminum source powder.
- a raw material mixture containing a magnesium source powder is a magnesium source powder.
- titanium source powder The titanium source powder used in the present invention is not particularly limited as long as it contains a titanium element and can synthesize an aluminum titanate ceramic by firing, but is preferably a titanium oxide powder.
- titanium oxide examples include titanium (IV) oxide, titanium (III) oxide, and titanium (II) oxide, and titanium (IV) oxide is preferably used. Titanium oxide may be crystalline or amorphous. When the titanium (IV) oxide is crystalline, examples of its crystal form include anatase, rutile, and brookite, and more preferred are anatase and rutile.
- titanium source powder a powder of a substance that is led to titania (titanium oxide) by firing in air can also be used.
- examples of such substances include titanium salts, titanium alkoxides, titanium hydroxide, titanium nitride, titanium sulfide, and titanium.
- Specific examples of the titanium salt include titanium trichloride, titanium tetrachloride, titanium (IV) sulfide, titanium sulfide (VI), titanium sulfate (IV), and the like.
- 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.
- the titanium source powder may contain inevitable impurities derived from the raw material or mixed in the manufacturing process.
- the particle size of the titanium source powder is not particularly limited, but the particle size (D50) equivalent to a cumulative percentage of 50% on a volume basis before being mixed with another powder is preferably 0.1 ⁇ m or more and 20 ⁇ m or less. More preferably 0.1 ⁇ m to 10 ⁇ m, and most preferably 0.1 ⁇ m to 1 ⁇ m. Further, the 90% cumulative particle diameter (D90) on a volume basis is preferably 0.1 ⁇ m or more and 20 ⁇ m or less, more preferably 0.1 ⁇ m or more and 10 ⁇ m or less, and most preferably 0.2 ⁇ m or more and 1.5 ⁇ m or less. It is.
- the aluminum source powder used in the present invention is not particularly limited as long as it contains an aluminum element and can synthesize an aluminum titanate ceramic by firing, but is preferably alumina.
- Alumina may be crystalline or amorphous. When alumina is crystalline, examples of the crystal type include ⁇ -type, ⁇ -type, ⁇ -type, ⁇ -type, and the like, preferably ⁇ -type.
- the aluminum source powder a powder of a substance introduced into alumina by firing in air can be used.
- examples of such substances include aluminum salts, aluminum alkoxides, aluminum hydroxides, and aluminum.
- the aluminum source powder may be derived from the raw material or contain inevitable impurities mixed in the manufacturing process.
- the aluminum salt may be an inorganic acid salt (inorganic salt) or an organic acid salt (organic salt).
- inorganic salt include nitrates such as aluminum nitrate and ammonium aluminum nitrate, carbonates such as ammonium aluminum carbonate, and the like.
- organic salt include aluminum oxalate, aluminum acetate, aluminum stearate, aluminum lactate, and aluminum laurate.
- Examples of the aluminum alkoxide include aluminum isopropoxide, aluminum ethoxide, aluminum sec-butoxide, aluminum tert-butoxide and the like.
- Aluminum hydroxide may be crystalline or amorphous.
- examples of its crystal form include a gibbsite type, a bayerite type, a norosotrandite type, a boehmite type, and a pseudoboehmite type.
- examples of 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 particle size (D50) equivalent to 50% of the cumulative percentage of the aluminum source powder before mixing with other powders is preferably 1 ⁇ m or more and 100 ⁇ m or less, more preferably 10 ⁇ m or more and 80 ⁇ m or less, and most preferably It is 20 ⁇ m or more and 60 ⁇ m or less.
- the 90% cumulative particle size (D90) on a volume basis is preferably 1 ⁇ m or more and 200 ⁇ m or less, more preferably 10 ⁇ m or more and 150 ⁇ m or less, and most preferably 30 ⁇ m or more and 100 ⁇ m or less.
- the silicon source powder used in the present invention is not particularly limited as long as it contains a silicon element and can synthesize an aluminum titanate ceramic by firing, but is preferably a silicon oxide powder.
- silicon oxide include silicon dioxide and silicon monoxide.
- silicon source powder contained in the raw material mixture a powder of a substance introduced into silicon oxide (silica) by firing in air can be used.
- a powder of a substance introduced into silicon oxide (silica) by firing in air examples include silicic acid, silicon carbide, silicon nitride, silicon sulfide, silicon tetrachloride, silicon acetate, sodium silicate, sodium orthosilicate, feldspar, and glass frit.
- glass frit and the like are preferably used from the viewpoint of industrial availability and stable component composition.
- Glass frit refers to flakes or powdered glass obtained by pulverizing glass.
- the glass constituting the glass frit include silicate glass and the like, and silicate glass containing general silicic acid (silicon dioxide, SiO 2 ) as a main component (50% by mass or more in all components) is preferably used. It is done.
- silicate glass similarly to general silicate glass, alumina (Al 2 O 3 ), sodium oxide (Na 2 O), potassium oxide (K 2 O), calcium oxide (CaO), Magnesia (MgO) may be included.
- ZrO 2 is preferably contained, and the addition amount is preferably 0.1% by mass or more and 10% by mass or less. Moreover, it is preferable to use a glass frit having a yield point of 700 ° C. or higher from the viewpoint of improving the heat decomposition resistance of the obtained aluminum titanate ceramic.
- the silicon source powder a powder that also serves as the aluminum source powder can be used.
- examples of such powder include feldspar powder.
- the silicon source powder may contain inevitable impurities derived from the raw material or mixed in the manufacturing process.
- the particle size (D50) equivalent to 50% of the cumulative percentage of the silicon source powder before mixing with other powder is 5 ⁇ m or less, preferably 1 ⁇ m or more and 5 ⁇ m or less, more preferably 2 ⁇ m or more and 4 ⁇ m or less. Most preferably, it is 3 ⁇ m or more and 4 ⁇ m or less.
- the coefficient of thermal expansion is 1 ⁇ 10 ⁇ 6 (K ⁇ 1 ) even when firing at a temperature of 1650 ° C. or less, preferably 1600 ° C. or less.
- the following aluminum titanate ceramics can be obtained.
- the 90% cumulative particle size (D90) of the silicon source powder on a volume basis before being mixed with other powders is preferably 17 ⁇ m or less, more preferably 10 ⁇ m or more and 16 ⁇ m or less, and most preferably Is 12 ⁇ m or more and 16 ⁇ m or less.
- the silicon source powder having the particle size distribution as described above is usually smaller than the particle size of commercially available powders, it is prepared by pulverizing commercially available powders in advance.
- the pulverization method in this case is not particularly limited as long as it is a method capable of obtaining the above particle size distribution, but a method of pulverization by stirring in the presence of pulverization media in a pulverization container is preferably used. be able to.
- the silicon source powder alone or in combination with other raw material powders (especially all raw material powders) in the pulverization container is put together with the pulverization media, and then the pulverization container is vibrated. Or can be pulverized by rotating.
- the silicon source powder and other raw material powders are added, the raw material powders are mixed and pulverized at the same time.
- a container made of a metal material such as stainless steel is usually used, and the inner surface may be coated with a fluorine resin, a silicon resin, a urethane resin, or the like.
- the internal volume of the pulverization container is usually 1 to 4 times, preferably 1.2 to 3 times the total volume of the raw material powder and pulverization media.
- the grinding media examples include alumina beads and zirconia beads having a diameter of 1 mm to 100 mm, preferably 5 mm to 50 mm.
- the amount of grinding media used is usually relative to the total amount of raw material powder (when using powders of complex oxides such as aluminum magnesium titanate as raw material powder, the total amount including them). It is 1 to 1000 times, preferably 5 to 100 times.
- a normal pulverizer such as a vibration mill, a ball mill, a planetary mill, a high-speed rotary pulverizer (pin mill, etc.) can be used.
- a vibration mill is preferably used because it is easy.
- the amplitude is usually 2 mm or more and 20 mm or less, preferably 12 mm or less.
- the pulverization may be performed continuously or batchwise, but is preferably performed continuously because it is easy to implement on an industrial scale.
- the time required for pulverization is usually from 1 minute to 6 hours, preferably from 1.5 minutes to 2 hours, more preferably from 10 minutes to 2 hours, and most preferably from 20 minutes to 1.5 hours. is there. Moreover, you may add additives, such as a grinding aid and a peptizer, in a grinding
- the magnesium source powder used in the present invention is not particularly limited as long as it contains a magnesium element and can synthesize an aluminum titanate ceramic by firing.
- it is magnesia (magnesium oxide).
- magnesia magnesium oxide
- the magnesium source powder a powder of a substance introduced into magnesia by firing in air can be mentioned, and magnesia is preferable.
- Examples of substances introduced to magnesia by firing in air include magnesium salts, magnesium alkoxides, magnesium hydroxide, magnesium nitride, and magnesium metal.
- Specific examples of 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, and magnesium stearate.
- Specific examples of the magnesium alkoxide include magnesium methoxide and magnesium ethoxide.
- magnesium source powder a powder containing an aluminum source powder in addition to the magnesium source powder can also be used.
- examples of such powder include magnesia spinel (MgAl 2 O 4 ) powder.
- the magnesium source powder may include inevitable impurities that are derived from the raw material or mixed in the manufacturing process.
- the particle size (D50) equivalent to 50% of the cumulative percentage of the magnesium source powder before mixing with other powders is preferably 0.5 ⁇ m or more and 20 ⁇ m or less, more preferably 1 ⁇ m or more and 10 ⁇ m or less.
- the 90% cumulative particle diameter (D90) on a volume basis is preferably 1 ⁇ m or more and 50 ⁇ m or less, and more preferably 5 ⁇ m or more and 30 ⁇ m or less.
- the amount of titanium source powder converted to titania is the total amount of titanium source powder converted to titania (TiO 2 ) and aluminum source powder converted to alumina (Al 2 O 3 ) contained in the raw material mixture ( (Hereinafter referred to as “total titania / alumina amount”) per 100 parts by mass, it is usually 30 parts by mass or more and 70 parts by mass or less, and preferably 40 parts by mass or more and 60 parts by mass or less. Moreover, the usage-amount of the aluminum source powder of alumina conversion is 30 to 70 mass parts normally, Preferably it is 40 to 60 mass parts.
- the amount of the silicon source powder converted to silica is usually 0.1 parts by mass or more and 20 parts by mass or less, preferably 0.1 parts by mass or more with respect to 100 parts by mass of the total titania / alumina. It is 10 parts by mass or less.
- the amount of magnesium source powder converted to magnesia (MgO) is usually 0.1 parts by mass or more and 10 parts by mass or less with respect to 100 parts by mass of the total titania / alumina. Preferably, they are 0.1 mass part or more and 8 mass parts or less.
- a raw material mixture can usually be obtained by mixing the above raw material powders.
- a mixing method either a method of mixing in a dry atmosphere (dry mixing method) or a method of mixing in a wet atmosphere (wet mixing method) may be used.
- these raw material mixtures may contain fine aluminum titanate and the like.
- a container made of a metal material such as stainless steel is usually used, and the inner surface may be coated with a fluorine resin, a silicon resin, a urethane resin, or the like.
- the internal volume of the pulverization container is usually 1 to 4 times, preferably 1.2 to 3 times the total volume of the raw material powder and pulverization media.
- the grinding media examples include alumina beads and zirconia beads having a diameter of 1 mm to 100 mm, preferably 5 mm to 50 mm.
- the amount of grinding media used is usually relative to the total amount of raw material powder (when using powders of complex oxides such as aluminum magnesium titanate as raw material powder, the total amount including them). It is 1 to 1000 times, preferably 5 to 100 times.
- the raw material powder is pulverized simultaneously with the mixing, for example, the raw material powder is mixed into the pulverization container together with the pulverization medium, and then the pulverization container is vibrated or rotated to simultaneously mix the raw material powder. It is crushed.
- a normal pulverizer such as a vibration mill, a ball mill, a planetary mill, a high-speed rotary pulverizer (pin mill, etc.) can be used, and the implementation on an industrial scale is easy. Therefore, a vibration mill is preferably used.
- the amplitude is usually 2 mm or more and 20 mm or less, preferably 12 mm or less.
- the pulverization may be performed continuously or batchwise, but is preferably performed continuously because it is easy to implement on an industrial scale.
- the time required for pulverization is usually 1 minute to 6 hours, preferably 1.5 minutes to 2 hours.
- additives such as a pulverizing aid and a peptizer may be added.
- the grinding aid examples include monohydric alcohols such as methanol and ethanolpropanol, dihydric alcohols such as propylene glycol, polypropylene glycol and ethylene glycol, amines such as triethanolamine, palmitic acid, stearic acid and oleic acid. Higher fatty acids, carbon black, carbon materials such as graphite, and the like. These may be used alone or in combination of two or more.
- the total amount used is usually 0.1 parts by mass or more and 10 parts by mass or less, preferably 0.5 parts by mass or more and 5 parts by mass with respect to 100 parts by mass of the total amount of raw material powder.
- it is more preferably 0.75 parts by mass or more and 2 parts by mass or less.
- raw material powder such as silicon source powder may be mixed with other raw material powder in a state of being dispersed in a solvent. In a dispersed state, it is mixed with other raw material powders. At that time, water is usually used as the solvent, and ion-exchanged water is preferably used in terms of few impurities.
- the usage-amount of a solvent is 20 mass parts or more and 1000 mass parts or less normally with respect to 100 mass parts of total amounts of raw material powder, Preferably it is 30 mass parts or more and 300 mass parts or less.
- a dispersing agent may be added to the solvent during wet mixing.
- the dispersant 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, and interfaces such as ammonium polycarboxylate. An active agent etc. are mentioned.
- the amount of the dispersant used is usually 0.1 parts by mass or more and 20 parts by mass or less, and preferably 0.2 parts by mass or more and 10 parts by mass or less with respect to 100 parts by mass of the total amount of the solvent.
- raw material powders other than the silicon source powder may be mixed after being dissolved in a solvent depending on the type.
- the raw material powder is precipitated again as a solid by evaporation of the solvent.
- a pulverizer such as a medium stirring mill, a ball mill, or a vibration mill.
- a titanium source powder, an aluminum source powder, a magnesium source powder and a silicon source powder such as glass frit are mixed together while being pulverized to obtain a raw material mixture having a more uniform composition.
- examples of the wet mixing method include a method of performing only a stirring process in a normal liquid solvent.
- the liquid solvent for example, monohydric alcohols such as methanol, ethanol, butanol, and propanol, dihydric alcohols such as propylene glycol, polypropylene glycol, and ethylene glycol, or ion-exchanged water can be used, and more preferably. Ion exchange water.
- the raw material powder may be simultaneously pulverized by stirring in a pulverization container in the presence of pulverization media.
- the grinding may be performed by vibrating or rotating the grinding container.
- the internal volume of the pulverization container is usually 1 to 4 times, preferably 1.2 to 3 times the total volume of the raw material powder, pulverization media, and solvent.
- the type, size, and amount of grinding media used can be the same as in the dry mixing method.
- the pulverizer used to vibrate or rotate the pulverization container, the pulverization conditions (amplitude width, etc.), and the time required for pulverization can be the same as in the dry mixing method.
- additives such as a pulverizing aid and a peptizer may be added separately from the pulverizing media.
- the type of grinding aid used and the amount used can be the same as in the dry mixing method.
- the raw material mixture used in the present invention can be obtained by removing the solvent. Removal of the solvent is usually performed by distilling off the solvent.
- the temperature condition and the pressure condition are not limited, and may be air-dried at room temperature, vacuum-dried, or heat-dried.
- the drying method may be stationary drying or fluidized drying. Although the temperature at the time of heat-drying is not specified in particular, it is usually from 50 ° C to 250 ° C. Examples of the equipment used for heat drying include a shelf dryer, a slurry dryer, and a spray dryer.
- the powdery raw material mixture obtained as described above may be fired as it is in a powder form, and then formed into a molded body. After the powdery raw material mixture is molded, the powdery raw material mixture is fired. May be performed. Alternatively, a molded body may be obtained after firing the powdery raw material mixture, and the molded body may be further fired.
- Calcination temperature is usually 1300 ° C. or higher, preferably 1400 ° C. or higher, and is usually 1650 ° C. or lower, preferably 1600 ° C. or lower, more preferably 1550 ° C. or lower.
- the temperature raising rate up to the firing temperature is not particularly limited, but is usually 1 ° C./hour or more and 500 ° C./hour or less. Moreover, you may provide the process hold
- Firing is usually performed in the atmosphere, but depending on the type and amount ratio of the raw material powder used, that is, titanium source powder, aluminum source powder and magnesium source powder, and silicon source powder, nitrogen gas, argon gas, etc. It may be fired in an inert gas or may be fired in a reducing gas such as carbon monoxide gas or hydrogen gas. Further, the firing may be performed by lowering the water vapor partial pressure in the atmosphere.
- Calcination is usually performed using a normal firing furnace such as a tubular electric furnace, a box-type electric furnace, a tunnel furnace, a far-infrared furnace, a microwave heating furnace, a shaft furnace, a reflection furnace, a rotary furnace, or a roller hearth furnace. Firing may be performed batchwise or continuously. Moreover, you may carry out by a stationary type and may carry out by a fluid type.
- a normal firing furnace such as a tubular electric furnace, a box-type electric furnace, a tunnel furnace, a far-infrared furnace, a microwave heating furnace, a shaft furnace, a reflection furnace, a rotary furnace, or a roller hearth furnace.
- Firing may be performed batchwise or continuously.
- you may carry out by a stationary type and may carry out by a fluid type.
- the time required for firing is sufficient as long as the raw material mixture transitions to the aluminum titanate-based ceramics, and varies depending on the amount of the raw material mixture, the type of firing furnace, firing temperature, firing atmosphere, etc. It is not less than 24 minutes.
- an aluminum titanate-based ceramic powder can be obtained by further crushing the fired product. Crushing can be performed using a normal crusher such as hand crushing, mortar, ball mill, vibration mill, planetary mill, medium stirring mill, pin mill, jet mill, hammer mill, roll mill, and the like.
- the aluminum titanate ceramic powder obtained by crushing may be classified by a usual method.
- the aluminum titanate-based ceramics (powder or molded body) obtained by the method of the present invention contains a crystal pattern of aluminum titanate in the X-ray diffraction spectrum, but in addition, a crystal pattern of silica, alumina, titania, etc. May be included.
- the aluminum titanate-based ceramic is aluminum magnesium titanate (Al 2 (1-x) Mg x Ti (1 + x) O 5 )
- the value of x is 0.01 or more, preferably 0.8. It is 01 or more and 0.7 or less, more preferably 0.02 or more and 0.5 or less.
- Molding process For forming the raw material mixture before firing or after firing, a commonly used molding method can be used, and uniaxial molding, extrusion molding, or the like is used.
- the molding machine used for molding include a uniaxial press, an extrusion molding machine, a tableting machine, and a granulator.
- a pore forming agent When performing extrusion molding, a pore forming agent, a binder, a lubricant, a plasticizer, a dispersing agent, a solvent, and the like can be added to the raw material mixture for molding.
- the pore-forming agent 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 or dry ice, and the like.
- Binders include celluloses such as methyl cellulose, carboxymethyl cellulose, 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 polymer And thermoplastic resins such as engineering plastics.
- lubricants and plasticizers include alcohols such as glycerin, caprylic acid, lauric acid, palmitic acid, higher fatty acids such as alginate, oleic acid and stearic acid, and stearic acid metal salts such as aluminum stearate.
- the solvent water such as ion-exchanged water is usually used, and it is preferable to use ion-exchanged water whose temperature is adjusted.
- the pore-forming agent or binder serves as both a pore-forming agent and a binder depending on the substance.
- any substance can be used as long as it can adhere particles to each other at the time of molding to retain the shape of the molded body, and can burn the substance itself to form pores at the time of subsequent firing.
- Specific examples of such a substance may include polyethylene.
- the shape of the molded body obtained by molding the raw material mixture is not particularly limited, and examples thereof include a honeycomb structure, a spherical structure, a cubic structure, a rectangular block structure, and the like. It is preferable that it is a body.
- the value of the thermal expansion coefficient of the aluminum sintered titanate ceramics was calculated by the following operation. After the specimen was cut out from the molded sintered body before being crushed in each Example and Comparative Example, the temperature was raised to 600 ° C. at 200 ° C./h, and then a thermomechanical analyzer (TMA (SII Technology Co., Ltd.). The sample was heated from room temperature to 1000 ° C. at 600 ° C./h using a TMA6300 manufactured by KK, and the thermal expansion coefficient (K ⁇ 1 ) was measured during that time.
- TMA thermomechanical analyzer
- the secondary particle size was measured using a laser diffraction particle size distribution measuring device ("Microtrac HRA (X-100)" manufactured by Nikkiso Co., Ltd.), a cumulative particle size equivalent to 50% (D50) and 90% equivalent particle size on a volume basis ( D90).
- Example 1 Glass frit (manufactured by Takara Standard Co., Ltd., model number “CK-0832M2”, D50: 6.0 ⁇ m, D90: 18.4 ⁇ m) 5000 g is put together with 80 kg of alumina beads (diameter 15 mm) into an alumina crushing container (internal volume 50 L). did. Then, the glass frit in the pulverization container was pulverized by vibrating the pulverization container with an oscillation mill at an amplitude of 10 mm, a vibration frequency of 1200 times / minute, and a power of 5.5 kW for 30 minutes to obtain a silicon source powder. The glass frit after pulverization had a D50 of 3.6 ⁇ m and a D90 of 14.6 ⁇ m.
- Titanium oxide powder (DuPont Co., Ltd., “R-900”; D50 0.49 ⁇ m, D90 0.63 ⁇ m) 3991 g, ⁇ alumina powder (BET specific surface area 0.6 m 2 / g, D50 40.2 ⁇ m, D90 70.2 ⁇ m) 5100 g, magnesia powder (manufactured by Saint-Gobain, magnesia spinel; D50 5.47 ⁇ m, D90 15.25 ⁇ m) 546 g, and 364 g of the above-mentioned glass frit pulverized with alumina beads (diameter 15 mm) Together with 80 kg, it was put into an alumina pulverization container (internal volume 50 L).
- the total volume of the mixture of titanium oxide powder, ⁇ -alumina powder, magnesia powder and glass frit was about 10,000 cm 3 .
- the amount of the titanium source powder converted into titania is 43. 9 parts by mass
- the amount of aluminum source powder converted to alumina is 56.1 parts by mass
- the amount of magnesium source powder converted to magnesia is 6.0 parts by mass
- the amount of silica source powder converted to silica is 4.0 parts by mass Part.
- the mixture in the pulverization container was pulverized by vibrating the pulverization container with an oscillation mill at an amplitude of 10 mm, a vibration frequency of 1200 times / minute, and a power of 5.5 kW for 30 minutes to obtain a raw material mixture.
- 3 g of this raw material mixture is molded under a pressure of 0.3 t / cm 2 with a uniaxial press to produce a molded product having a diameter of 20 mm, and up to 1450 ° C. in a box-type electric furnace at a heating rate of 300 ° C./hour.
- the temperature was raised and firing was carried out by maintaining the same temperature for 4 hours. Then, it cooled to room temperature and obtained the shaping
- Example 2 Aluminum titanate ceramics in the same manner as in Example 1, except that the firing temperature of the raw material mixture was 1500 ° C. (the temperature was raised to 1500 ° C. at a heating rate of 300 ° C./hour and the temperature was maintained for 4 hours). A molded sintered body and a powder were obtained.
- Example 3 In the preparation of the silicon source powder, in the same manner as in Example 1, except that the grinding time (vibration time) of the glass frit (manufactured by Takara Standard Co., Ltd., model number “CK-0832M2”) with a vibration mill was 60 minutes. A molded sintered body and powder of an aluminum titanate ceramic were obtained. D50 of the glass frit after pulverization was 3.3 ⁇ m, and D90 was 13.3 ⁇ m.
- Example 4 Aluminum titanate ceramics in the same manner as in Example 3 except that the firing temperature of the raw material mixture was set to 1500 ° C. (the temperature was raised to 1500 ° C. at a heating rate of 300 ° C./hour and the temperature was maintained for 4 hours). A molded sintered body and a powder were obtained.
- Comparative Example 1 As a comparative example, an aluminum titanate-based ceramic shaped sintered body and powder were obtained in the same manner as in Example 1 except that the raw material powder was mixed without pre-grinding the glass frit.
- Comparative Example 2 As a comparative example, an aluminum titanate-based ceramic shaped sintered body and powder were obtained in the same manner as in Example 2 except that the raw material powder was mixed without pre-grinding the glass frit.
- the relationship between the thermal expansion coefficient of each aluminum titanate ceramic (molded fired body) and the secondary particle diameter (D90) of the glass frit is shown in FIG.
- the thermal expansion coefficient is 1 ⁇ 10 ⁇ 6 K ⁇ 1 or less.
- the aluminum titanate-based ceramic molded body obtained by using the method of the present invention is, for example, a furnace for firing furnaces such as crucibles, setters, mortars, furnace materials, exhaust gas purification of internal combustion engines such as diesel engines and gasoline engines.
- a furnace for firing furnaces such as crucibles, setters, mortars, furnace materials
- exhaust gas purification of internal combustion engines such as diesel engines and gasoline engines.
- filtration filters used for the filtration of food and drink such as beer
- gas components generated during petroleum refining such as carbon monoxide, carbon dioxide, nitrogen, oxygen, etc.
- Ceramic filters such as transmission filters, electronic parts such as substrates and capacitors.
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Abstract
Description
前記ケイ素源粉末の体積基準での累積百分率50%相当粒子径(D50)が5μm以下である方法である。
本発明で用いられる原材料混合物は、原材料粉末である1種以上のチタニウム源粉末、1種以上のアルミニウム源粉末および1種以上のケイ素源粉末を含む混合物であり、さらに1種以上のマグネシウム源粉末を含むことが好ましい。なお、本発明では、マグネシアスピネル(MgAl2O4)などの複合酸化物のように、チタニウム、アルミニウムおよびマグネシウムのうち2つ以上の金属元素を成分とする物質も、それぞれの金属源粉末を混合した原材料混合物に含まれるものとする。また、原材料混合物にはチタン酸アルミニウムやチタン酸アルミニウムマグネシウム自体が含まれていてもよく、例えば、原材料混合物としてチタン酸アルミニウムマグネシウムを使用する場合、チタン酸アルミニウムマグネシウムは、チタニウム源粉末、アルミニウム源粉末およびマグネシウム源粉末を含む原材料混合物に相当するものとする。
本発明に用いられるチタニウム源粉末は、チタン元素を含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、好ましくは酸化チタンの粉末である。酸化チタンとしては、例えば、酸化チタン(IV)、酸化チタン(III)、酸化チタン(II)などが挙げられ、酸化チタン(IV)が好ましく用いられる。酸化チタンは結晶性でもよく、アモルファスであってもよい。酸化チタン(IV)が結晶性である場合、その結晶型としては、アナターゼ型、ルチル型、ブルッカイト型などが挙げられ、より好ましくはアナターゼ型、ルチル型である。
本発明で用いられるアルミニウム源粉末は、アルミニウム元素を含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、好ましくはアルミナである。アルミナは結晶性であってもよく、アモルファスであってもよい。アルミナが結晶性である場合、その結晶型としては、γ型、δ型、θ型、α型などが挙げられ、好ましくはα型である。
本発明で用いられるケイ素源粉末は、ケイ素元素を含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、好ましくは酸化ケイ素の粉末である。酸化ケイ素としては、二酸化ケイ素、一酸化ケイ素などが挙げられる。
本発明で用いられるマグネシウム源粉末は、マグネシウム元素を含有し焼成によりチタン酸アルミニウム系セラミックスを合成できる粉末であれば特に限定されないが、例えば、マグネシア(酸化マグネシウム)である。また、マグネシウム源粉末として、空気中で焼成することによりマグネシアに導かれる物質の粉末が挙げられ、好ましくはマグネシアである。
チタニア換算のチタニウム源粉末の使用量は、原材料混合物中に含まれるチタニア(TiO2)換算のチタニウム源粉末の使用量およびアルミナ(Al2O3)換算のアルミニウム源粉末の使用量の合計量(以下、「全チタニア・アルミナ量」と呼ぶ)100質量部あたり、通常、30質量部以上70質量部以下であり、好ましくは40質量部以上60質量部以下である。また、アルミナ換算のアルミニウム源粉末の使用量は、通常、30質量部以上70質量部以下であり、好ましくは40質量部以上60質量部以下である。
本発明の方法においては、通常、上記各原材料粉末を混合することで原材料混合物を得ることができる。混合方法は、乾式雰囲気にて混合を行なう方法(乾式混合法)、湿式雰囲気で混合を行なう方法(湿式混合法)のいずれを用いてもよい。また、これらの原材料混合物には微粒チタン酸アルミニウム等が含まれていてもよい。
乾式雰囲気で混合する場合は、例えば、上記の各原材料粉末を混合し、液体媒体中に分散させること無く、粉砕容器内で撹拌すればよく、また粉砕メディアの共存下で撹拌することによって原材料粉末の粉砕を同時に行なってもよい。
湿式雰囲気で混合する場合は、例えば、ケイ素源粉末等の原材料粉末を溶媒中に分散させた状態で他の原材料粉末と混合すればよく、通常はケイ素源粉末が溶媒に分散された状態で他の原材料粉末と混合される。その際、溶媒として、通常は水が用いられ、不純物が少ない点で、イオン交換水が好適に用いられる。溶媒の使用量は、原材料粉末の合計量100質量部に対して、通常、20質量部以上1000質量部以下であり、好ましくは30質量部以上300質量部以下である。
本発明の方法においては、上述のようにして得られた粉末状の原材料混合物に対して、粉末状のままで焼成を行ってから成形体としてもよく、粉末状の原材料混合物を成形した後に焼成を行なってもよい。また、粉末状の原材料混合物を焼成した後に成形体を得て、さらに該成形体を焼成してもよい。
原材料混合物の焼成前または焼成後の成形には、通常用いられる成形方法を用いることができ、一軸成形や押出成形などが用いられる。成形に用いる成形機としては、一軸プレス、押出成形機、打錠機、造粒機などが挙げられる。
チタン酸アルミニウムのチタン酸アルミニウム化率(AT化率)は、粉末X線回折スペクトルにおける2θ=27.4°の位置に現れるピーク(チタニア・ルチル相(110)面)の積分強度(IT)と、2θ=33.7°の位置に現れるピーク(チタン酸アルミニウム相(230)面またはチタン酸アルミニウムマグネシウム相(230)面)の積分強度(IAT)とから、式(1)により算出した。
チタン酸アルミニウム系セラミックスの成形焼結体の熱膨張係数の値は、次の操作で算出した。各実施例、比較例において解砕される前の成形焼結体から検体を切り出した後、200℃/hで600℃まで昇温したのち、熱機械的分析装置(TMA (SIIテクノロジー(株)社製 TMA6300)を用いて、検体を室温から1000℃まで600℃/hで昇温させ、その間の熱膨張係数(K-1)を測定した。
二次粒子径は、レーザー回折式粒度分布測定装置(日機装社製「Microtrac HRA(X-100)」)により、体積基準での累積百分率50%相当粒子径(D50)および90%相当粒子径(D90)として算出した。
ガラスフリット(タカラスタンダード(株)製、型番「CK-0832M2」、D50:6.0μm、D90:18.4μm)5000gをアルミナビーズ(直径15mm)80kgと共にアルミナ製粉砕容器(内容積50L)に投入した。その後、粉砕容器を振動ミルにより振幅10mm、振動数1200回/分、動力5.5kWにて30分間振動させることにより粉砕容器内のガラスフリットを粉砕し、ケイ素源粉末を得た。粉砕後のガラスフリットのD50は3.6μm、D90は14.6μmであった。
原材料混合物の焼成温度を1500℃とした(昇温速度300℃/時間で1500℃まで昇温し、同温度を4時間保持した)以外は、実施例1と同様にして、チタン酸アルミニウム系セラミックスの成形焼結体および粉末を得た。
ケイ素源粉末の調製において、ガラスフリット(タカラスタンダード(株)製、型番「CK-0832M2」)の振動ミルによる粉砕時間(振動時間)を60分間とした以外は、実施例1と同様にして、チタン酸アルミニウム系セラミックスの成形焼結体および粉末を得た。粉砕後のガラスフリットのD50は3.3μm、D90は13.3μmであった。
原材料混合物の焼成温度を1500℃とした(昇温速度300℃/時間で1500℃まで昇温し、同温度を4時間保持した)以外は、実施例3と同様にして、チタン酸アルミニウム系セラミックスの成形焼結体および粉末を得た。
比較例として、ガラスフリットの前粉砕処理を行なわずに原材料粉末を混合する以外は、実施例1と同様にして、チタン酸アルミニウム系セラミックスの成形焼結体および粉末を得た。
比較例として、ガラスフリットの前粉砕処理を行なわずに原材料粉末を混合する以外は、実施例2と同様にして、チタン酸アルミニウム系セラミックスの成形焼結体および粉末を得た。
Claims (15)
- チタニウム源粉末、アルミニウム源粉末およびケイ素源粉末を含む原材料混合物を焼成するチタン酸アルミニウム系セラミックスの製造方法であって、
前記ケイ素源粉末の体積基準での累積百分率50%相当粒子径(D50)が5μm以下である方法。 - 前記原材料混合物が、さらにマグネシウム源粉末を含む、請求項1記載の方法。
- 前記焼成の温度が1300℃以上1650℃以下である、請求項1記載の方法。
- 前記ケイ素源粉末の体積基準での累積百分率90%相当粒子径(D90)が17μm以下である、請求項1記載の方法。
- 前記ケイ素源粉末がガラスフリットである、請求項1記載の方法。
- 前記チタニウム源粉末の体積基準での累積百分率50%相当粒子径(D50)が0.1μm以上20μm以下である、請求項1記載の方法。
- 前記アルミニウム源粉末の体積基準での累積百分率50%相当粒子径(D50)が1μm以上100μm以下である、請求項1記載の方法。
- 前記マグネシウム源粉末の体積基準での累積百分率50%相当粒子径(D50)が0.5μm以上20μm以下である、請求項2記載の方法。
- 原材料混合物中に含まれるチタニア(TiO2)換算のチタニウム源粉末の使用量およびアルミナ(Al2O3)換算のアルミニウム源粉末の使用量の合計量100質量部に対して、チタニア換算のチタニウム源粉末の使用量は30質量部以上70質量部以下であり、アルミナ換算のアルミニウム源粉末の使用量は30質量部以上70質量部以下であり、かつ、シリカ(SiO2)換算のケイ素源粉末の使用量は、0.1質量部以上20質量部以下である、請求項1に記載の方法。
- チタニア(TiO2)換算のチタニウム源粉末の使用量とアルミナ(Al2O3)換算のアルミニウム源粉末の使用量との合計量100質量部に対して、マグネシア(MgO)換算のマグネシウム源粉末の使用量は0.1質量部以上10質量部以下である、請求項2に記載の方法。
- 前記原材料混合物を乾式または湿式で混合する請求項1記載の方法。
- 乾式または湿式での混合に際し、粉砕メディアの共存下に粉砕容器内で粉砕混合する請求項11記載の方法。
- 前記粉砕メディアは、直径1mm以上100mm以下のアルミナビーズまたはジルコニアビーズである請求項12記載の方法。
- 前記粉砕容器を、2mm以上20mm以下の振幅幅で振動させる請求項12記載の方法。
- さらに、原材料混合物の焼成後に得られたチタン酸アルミニウム系セラミックス焼成物を解砕する工程を含む、請求項1記載の方法。
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- 2009-11-05 EP EP09824821A patent/EP2360130A4/en not_active Withdrawn
- 2009-11-05 CN CN2009801443767A patent/CN102209698A/zh active Pending
- 2009-11-05 US US13/124,079 patent/US20110248106A1/en not_active Abandoned
- 2009-11-05 WO PCT/JP2009/068904 patent/WO2010053122A1/ja active Application Filing
- 2009-11-05 KR KR1020117009644A patent/KR20110083634A/ko not_active Application Discontinuation
- 2009-11-06 TW TW098137791A patent/TW201031616A/zh unknown
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2010138036A (ja) * | 2008-12-11 | 2010-06-24 | Sumitomo Chemical Co Ltd | チタン酸アルミニウム系焼成体の製造方法 |
WO2011008938A1 (en) * | 2009-07-15 | 2011-01-20 | E.I. Du Pont De Nemours And Company | Aluminium magnesium titanate composite ceramics |
JP2012020928A (ja) * | 2011-08-24 | 2012-02-02 | Sumitomo Chemical Co Ltd | チタン酸アルミニウム系焼成体の製造方法 |
CN103833072A (zh) * | 2014-03-20 | 2014-06-04 | 湖州巨力铝型材有限公司 | 利用铝型材改性废水处理产生的污泥制备钛酸铝的方法 |
Also Published As
Publication number | Publication date |
---|---|
EP2360130A1 (en) | 2011-08-24 |
TW201031616A (en) | 2010-09-01 |
US20110248106A1 (en) | 2011-10-13 |
CN102209698A (zh) | 2011-10-05 |
KR20110083634A (ko) | 2011-07-20 |
JP2010132527A (ja) | 2010-06-17 |
EP2360130A4 (en) | 2012-07-04 |
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