WO2009154219A1 - 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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- WO2009154219A1 WO2009154219A1 PCT/JP2009/061006 JP2009061006W WO2009154219A1 WO 2009154219 A1 WO2009154219 A1 WO 2009154219A1 JP 2009061006 W JP2009061006 W JP 2009061006W WO 2009154219 A1 WO2009154219 A1 WO 2009154219A1
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Definitions
- the present invention relates to a method for producing an aluminum titanate ceramic (such as an aluminum titanate-containing ceramic or an aluminum magnesium titanate-containing ceramic).
- an aluminum titanate ceramic such as an aluminum titanate-containing ceramic or an aluminum magnesium titanate-containing ceramic.
- Aluminum titanate ceramics contain titanium and aluminum as constituent elements and have a crystal pattern of aluminum titanate in the X-ray diffraction spectrum, and are known as ceramics having excellent heat decomposition resistance. It is used as a sintering jig such as a crucible. In recent years, the industrial utility value has increased as a material constituting a ceramic filter for collecting fine carbon particles contained in exhaust gas discharged from an internal combustion engine such as a diesel engine.
- Patent Document 1 As a method for producing such an aluminum titanate-based ceramic, 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. It is disclosed in WO 2005/105704 (Patent Document 1) that an aluminum titanate-based ceramic with improved thermal decomposition resistance can be obtained by firing a raw material mixture to which alkali feldspar powder is added.
- the present inventors have intensively studied to develop a method capable of producing an aluminum titanate-based ceramic having excellent thermal decomposition resistance and a smaller thermal expansion coefficient. As a result, the present inventors have reached the present invention.
- the present invention is characterized by firing a raw material mixture containing a titanium source compound, an aluminum source compound, and a glass frit having a yield point of 700 ° C. or higher and / or 900 ° C. of a viscosity value of 1.0 ⁇ 10 6 poise or higher.
- a method for producing an aluminum titanate-based ceramic is provided.
- the amount of titania-converted titanium source compound used is 30 to 70 parts by mass per 100 parts by mass of the total amount of titania-converted titanium source compound and alumina-converted aluminum source compound.
- the amount of glass frit used is preferably 0.1 to 20 parts by mass.
- the raw material mixture further contains a magnesium source compound.
- the amount of magnesium source compound converted to magnesia is 0.1 to 10 parts by mass per 100 parts by mass of the total amount of titanium source compound converted to titania and the amount of aluminum source compound converted to alumina. Is preferred.
- the titanium source compound is preferably titanium oxide
- the aluminum source compound is preferably aluminum oxide and / or magnesia spinel.
- the glass frit is preferably silicate glass containing 50 mass% or more of SiO 2
- the magnesium source compound is preferably magnesium oxide and / or magnesia spinel.
- the raw material mixture is preferably mixed in a dry or wet manner. Further, in the mixing, it is also preferable to pulverize and mix in a pulverization container in the presence of a pulverization medium.
- the grinding media is preferably alumina balls or zirconia balls having a diameter of 1 mm to 100 mm. It is also preferable to vibrate the pulverization container with an amplitude width of 2 mm to 20 mm.
- the present invention also includes a method for producing an aluminum titanate ceramic powder by obtaining an aluminum titanate ceramic by any one of the production methods described above and crushing the obtained aluminum titanate ceramic.
- the manufacturing method of the present invention since glass frit is used as a silicon source, it is possible to manufacture an aluminum titanate-based ceramic having a smaller thermal expansion coefficient than that according to the conventional manufacturing method.
- the viscosity value of 700 ° C. or higher and / or 900 ° C. is used 1.0 ⁇ 10 6 poises or more glass frits, it is possible to produce an excellent aluminum titanate-based ceramics in thermal decomposition resistance.
- a raw material mixture containing a titanium source compound, an aluminum source compound, and a glass frit having a yield point of 700 ° C. or higher and / or 900 ° C. of 1.0 ⁇ 10 6 poise or higher is used.
- titanium source compound examples include titanium oxide powder.
- examples of titanium oxide include titanium (IV) oxide, titanium (III) oxide, and titanium (II) oxide.
- Titanium (IV) oxide is preferably used.
- the titanium oxide (IV) may be crystalline or amorphous.
- examples of the crystal type include anatase type, rutile type and brookite type, and anatase type and rutile type are preferable.
- titanium source compounds include compounds that are led to titania (titanium oxide) by firing in air.
- examples of such compounds include titanium salts, titanium alkoxides, titanium hydroxide, titanium nitride, titanium sulfide, and titanium metal.
- titanium salts include titanium trichloride, titanium tetrachloride, titanium sulfide (IV), titanium sulfide (VI), and titanium sulfate (IV).
- titanium alkoxide include titanium (IV) ethoxide, titanium (IV) methoxide, titanium (IV) tert-butoxide, titanium (IV) isobutoxide, titanium (IV) n-propoxide, titanium (IV) tetraiso Examples thereof include propoxides and chelating products thereof.
- titanium source compound only one kind of titanium source compound may be used, or two or more kinds may be used in combination.
- the titanium source compound may be derived from raw materials or contain inevitable impurities mixed in during the manufacturing process.
- Examples of the aluminum source compound include alumina (aluminum oxide) powder.
- Examples of the crystal type of alumina include ⁇ type, ⁇ type, ⁇ type, and ⁇ type, and may be amorphous.
- the aluminum source compound is preferably ⁇ -type alumina.
- Aluminum source compounds include compounds that are led to alumina by firing in air.
- Examples of such a compound include an aluminum salt, aluminum alkoxide, aluminum hydroxide, and metal aluminum.
- the aluminum salt may be a salt with an inorganic acid (inorganic salt) or a salt with an organic acid (organic salt).
- specific examples of the aluminum inorganic salt include aluminum nitrates such as aluminum nitrate and ammonium nitrate, and aluminum carbonates such as ammonium aluminum carbonate.
- examples of 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.
- the crystal type include a gibbsite type, a bayerite type, a norosotrandite type, a boehmite type, and a pseudoboehmite type.
- 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 aluminum alkoxide.
- a compound containing an aluminum source and a magnesium source can also be used.
- examples of such a compound include magnesia spinel [MgAl 2 O 4 ] powder.
- only one type of aluminum source compound may be used, or two or more types may be used in combination.
- the aluminum source compound may contain inevitable impurities that are derived from raw materials or mixed in the manufacturing process.
- the raw material mixture used in the method for producing an aluminum titanate ceramic of the present invention preferably further contains a magnesium source compound in addition to the titanium source compound and the aluminum source compound.
- a magnesium source compound examples include magnesia (magnesium oxide).
- magnesium source compounds include compounds that are led to magnesia by firing in air.
- examples of such a compound include magnesium salt, magnesium alkoxide, magnesium hydroxide, magnesium nitride, and magnesium metal.
- the magnesium salt may be a salt with an inorganic acid (inorganic salt) or a salt with an organic acid (organic salt).
- the magnesium inorganic salt include magnesium chloride, magnesium perchlorate, magnesium phosphate, magnesium pyrophosphate, magnesium nitrate, magnesium carbonate, magnesium sulfate and the like.
- the magnesium organic salt include magnesium oxalate, magnesium acetate, magnesium citrate, magnesium lactate, magnesium stearate, magnesium salicylate, magnesium myristate, magnesium gluconate, magnesium dimethacrylate, and magnesium benzoate.
- magnesium alkoxide examples include magnesium methoxide and magnesium ethoxide.
- magnesium source compound a compound containing a magnesium source and an aluminum source can also be used.
- An example of such a compound is magnesia spinel [MgAl 2 O 4 ] powder.
- magnesium source compound only one kind may be used, or two or more kinds may be used in combination.
- the magnesium source compound may be derived from raw materials or contain unavoidable impurities mixed in during the manufacturing process.
- the raw material mixture may contain aluminum titanate or aluminum magnesium titanate itself.
- aluminum magnesium titanate as a raw material mixture corresponds to a raw material mixture comprising a titanium source, an aluminum source and a magnesium source.
- the amount of the titanium source compound and aluminum source compound is determined based on the result in terms of titania [TiO 2] and alumina [Al 2 O 3].
- the total amount of titania-converted titanium source compound and alumina-converted aluminum source compound used per 100 parts by mass is typically 30 to 70 parts by mass of titania-converted titanium source compound.
- the amount of the aluminum source compound used is usually 70 to 30 parts by mass, preferably 40 to 60 parts by mass of the titanium source compound converted to titania, and the amount of the aluminum source compound converted to alumina 60 Parts by mass to 40 parts by mass.
- the amount of magnesium source compound converted to magnesia [MgO] is the amount of titanium source compound converted to titania [TiO 2 ] and the amount of alumina [Al 2 O 3 ] converted
- the amount is usually 0.1 to 10 parts by weight, preferably 8 parts by weight or less per 100 parts by weight of the total amount of the aluminum source compound used.
- glass frit is used as the silicon source compound.
- Glass frit refers to glass crushed into flakes or powder.
- the silicon source also acts as a reaction aid.
- the melting point of the silicon source is lowered.
- the silicon source becomes a liquid phase from a lower temperature and the synthesis of the aluminum titanate ceramic becomes easier. The expansion coefficient can be reduced.
- the glass frit has a bending point of 700 ° C. or higher and / or a viscosity value of 900 ° C. of 1.0 ⁇ 10 6 poise or higher.
- the yield point of glass is also called the yield point and refers to the temperature at which the amount of thermal expansion of the glass, which increases with temperature, suddenly begins to decrease. If a glass frit with a glass frit yield point of less than 700 ° C. and a viscosity value at 900 ° C. of less than 1.0 ⁇ 10 6 poise is used, the thermal decomposition resistance of the aluminum titanate-based ceramics obtained by sintering is not good. It will be enough.
- the glass frit yield point is less than 700 ° C.
- the glass phase contained in the aluminum titanate ceramics obtained by sintering is likely to soften, so that the heat resistance of the aluminum titanate ceramics obtained by sintering is high. Degradability is reduced.
- the reason why the viscosity value at 900 ° C. of the glass frit is defined is that the temperature range in which the conventional aluminum titanate ceramics are thermally decomposed is taken into account.
- the viscosity value in this temperature range is the aluminum titanate ceramic grain boundary. Affects the molten state of the glass phase present in the glass. That is, when the glass phase existing in the aluminum titanate-based ceramic is melted when the viscosity value at 900 ° C. is less than 1.0 ⁇ 10 6 poise, the constituent elements of the aluminum titanate-based ceramic into the molten glass phase Since diffusion is promoted, the thermal decomposition resistance of the aluminum titanate-based ceramics obtained by sintering becomes insufficient.
- a general silicate glass containing silicate [SiO 2 ] as a main component is used as the glass constituting the glass frit.
- Other components include alumina [Al 2 O 3 ], sodium oxide [Na 2 O], potassium oxide [K 2 O], calcium oxide [CaO], magnesia [MgO], as in general silicate glass. May be included.
- the glass frit preferably contains zirconia [ZrO 2 ] in order to improve the hot water resistance of the glass itself, and the content is preferably 0.1 wt% or more and 10 wt% or less. .
- the glass frit used in the production method of the present invention does not contain boric acid [B 2 O 3 ]. This is because boric acid is a factor that lowers the yield point of glass, and it is difficult to make the yield point of glass 700 ° C. or higher.
- the amount of the glass frit used is preferably 0.1 parts by mass or more and 20 parts by mass or less with respect to 100 parts by mass of the total amount of the titania converted titanium source compound and the alumina converted aluminum source compound. More preferably, it is 10 mass parts or less.
- the particle size of the glass frit used in the present invention is preferably small so that it can be uniformly distributed in the mixture, and the center particle size is usually 15 ⁇ m or less, preferably 10 ⁇ m or less.
- each metal source compound that is the titanium source compound, the aluminum source compound, and the magnesium source compound is a powder
- the respective metal source compound and the glass frit are mixed.
- a raw material mixture used in the production method of the present invention is obtained.
- a non-powdered metal source compound such as a lump is included, or when it is desired to further uniformly mix
- a mixture of each metal source compound and the glass frit may be pulverized and mixed.
- the mixing method may be dry mixing or wet mixing.
- the raw material mixture may be mixed and stirred in a pulverization container without being dispersed in a liquid medium.
- stirring is performed in the pulverization container in the presence of a pulverization medium.
- 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 grinding container is usually 1 to 4 times, preferably 1.2 to 3 times the volume of the total volume of the raw material mixture and grinding media.
- the grinding media examples include alumina balls and zirconia balls having a diameter of 1 mm to 100 mm, preferably 5 mm to 50 mm.
- the amount of the grinding media used is usually 1 to 1000 times, preferably 5 to 100 times, the amount of the raw material mixture used.
- the pulverization is performed, for example, by putting the raw material mixture and the pulverization medium into the pulverization container, and then vibrating the pulverization container, rotating it, or both.
- the raw material mixture is stirred and mixed with the grinding media and then ground.
- a normal pulverizer such as a vibration mill, a ball mill, and a planetary mill can be used. It is done.
- the amplitude is usually 2 mm to 20 mm, 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 include alcohols such as methanol, ethanol and propanol, glycols such as propylene glycol, polypropylene glycol and ethylene glycol, amines such as triethanolamine, and higher fatty acids such as palmitic acid, stearic acid and oleic acid.
- Carbon materials such as carbon black and graphite, and these are used alone or in combination of two or more.
- the total amount used is usually 0.1 to 10 parts by weight, preferably 0.5 to 5 parts by weight, more preferably 0.75 per 100 parts by weight of the raw material mixture. Parts by mass to 2 parts by mass.
- these raw material mixtures may be mixed and dispersed in a liquid medium.
- the mixer is not particularly limited, and may be stirred in a common container in the presence of a liquid solvent, or may be pulverized and stirred in a pulverization container in the presence of a liquid medium and a pulverizing medium.
- the same container and pulverization medium as in the case of dry mixing can be used.
- the internal volume of the pulverization container is usually 1 to 4 volume times, preferably 1.2 to 3 volume times with respect to the total volume of the raw material mixture, the pulverization medium, and the liquid medium.
- the amount of the grinding media used is usually 1 to 1000 times, preferably 5 to 100 times, the amount of the raw material mixture used.
- water is usually used as a solvent, and ion-exchanged water is preferable from the viewpoint of few impurities.
- organic solvents such as alcohols such as methanol, ethanol, butanol, and propanol, and glycols such as propylene glycol, polypropylene glycol, and ethylene glycol can be used as the solvent.
- the amount of the solvent used is usually 20 parts by mass to 1000 parts by mass, preferably 30 parts by mass to 300 parts by mass with respect to 100 parts by mass of the mixture.
- 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 used is usually 0.1 to 20 parts by weight, preferably 0.2 to 10 parts by weight per 100 parts by weight of the solvent.
- pulverization for example, a raw material mixture, a liquid medium, and a pulverization medium, and a dispersant as necessary may be added into a pulverization container, and then the raw material mixture may be mixed and pulverized in the same manner as in dry mixing.
- the solvent can be removed (eg, distilled off) to obtain a uniformly mixed mixture.
- the temperature and pressure conditions are not limited, and may be air-dried at room temperature, vacuum-dried, or heat-dried.
- the stirring conditions are not limited, either stationary drying or fluidized drying may be used.
- the temperature at the time of heat-drying is not specified in particular, it is usually from 50 ° C to 250 ° C. Examples of equipment used for heat drying include a shelf dryer, a slurry dryer, and a spray dryer.
- the raw material mixture such as the aluminum source compound used in the wet mixing
- the raw material mixture such as the aluminum source compound dissolved in the solvent may be solidified again by distilling off the solvent. To be deposited.
- a raw material mixture is obtained by mixing a titanium source compound, an aluminum source compound and a glass frit, preferably a magnesium source, and the raw material mixture is sintered to sinter aluminum titanate ceramics.
- a titanium source compound, aluminum source compound, glass frit and the like are usually contained in the raw material mixture in powder form.
- the powdery raw material mixture may be fired as it is, or the raw material mixture may be formed into a molded body and fired.
- the formation of aluminum titanate can be promoted by firing after forming the molded body.
- the molding machine used for molding include an extrusion molding machine, a uniaxial press machine, a tableting machine, and a granulator.
- a raw material mixture can be molded by adding a pore-forming agent, a binder, a lubricant, a plasticizer, a dispersant, a solvent, and the like.
- pore-forming agent 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.
- binder examples include celluloses such as methylcellulose, carboxymethylcellulose, and sodium carboxymethylcellulose; 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. Some substances have both a pore-forming agent and a binder. As such a substance, any substance can be used as long as it can adhere particles to each other at the time of molding to shape the molded body, and can burn itself to form pores at the time of subsequent firing. In particular, polyethylene may be applicable.
- lubricant examples include alcohol-based lubricants such as glycerin, higher fatty acids such as caprylic acid, lauric acid, palmitic acid, alginic acid, oleic acid and stearic acid, and metal stearates such as aluminum stearate. .
- alcohol-based lubricants such as glycerin
- higher fatty acids such as caprylic acid, lauric acid, palmitic acid, alginic acid, oleic acid and stearic acid
- metal stearates such as aluminum stearate.
- Such a lubricant usually also functions as a plasticizer.
- alcohols such as methanol and ethanol are usually used in addition to ion-exchanged water.
- the firing temperature is usually 1300 ° C. or higher, preferably 1400 ° C. or higher.
- the sintering temperature is usually 1650 ° C. or lower. Preferably it is 1600 degrees C or less.
- the rate of temperature increase up to the firing temperature is not particularly limited, but is usually 1 ° C./hour to 500 ° C./hour.
- Firing is usually carried out in the air, but depending on the components of the raw material mixture and the ratio of the amount used, it may be fired in an inert gas such as nitrogen gas or argon gas, or carbon monoxide gas, hydrogen gas, etc. You may bake in such reducing gas. Further, the firing may be performed by lowering the water vapor partial pressure in the atmosphere.
- an inert gas such as nitrogen gas or argon gas, or carbon monoxide gas, hydrogen gas, etc. You may bake in such reducing 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 mixture transitions to an aluminum titanate ceramic (such as aluminum titanate or aluminum magnesium titanate).
- a sintered body of the target aluminum titanate ceramic can be obtained as a fired product.
- the final product may be formed by grinding the sintered body.
- the ceramic powder can be obtained by pulverizing the ceramic sintered body in a massive shape. 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 ceramic powder obtained by crushing may be classified by a usual method. Since the ceramic powder thus obtained has a generally spherical shape, the handling container or the like is not worn when the ceramic powder is handled.
- the ceramic powder can be granulated or formed by a known powder molding technique.
- the aluminum titanate-based ceramics obtained by the production method of the present invention includes a crystal pattern of aluminum titanate or magnesium aluminum titanate in the X-ray diffraction spectrum. In addition, crystal patterns 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 a titanium source compound, an aluminum source compound, and magnesium. It can control by the usage-amount of a source compound.
- the value of x is 0.01 or more, preferably 0.01 or more and 0.7 or less, more preferably 0.02 or more and 0.5 or less.
- the aluminum titanate conversion rate (hereinafter referred to as “AT conversion rate”) in the aluminum titanate-based ceramics obtained in each Example and Comparative Example was calculated from the following formula (2).
- AT conversion rate (%) 100 ⁇ I AT / (I AT + I T ) (2)
- the thermal decomposition rate of the aluminum titanate ceramics obtained in each Example and Comparative Example was measured as follows.
- Aluminum titanate ceramic powder was charged into an alumina crucible and held at 1100 ° C. for 48 hours in a box-type electric furnace to obtain aluminum magnesium titanate for thermal decomposition evaluation.
- the density of the molded sintered body of the aluminum titanate ceramics obtained in each Example and Comparative Example was measured and evaluated by the following method. First, each metal source compound described in each example and comparative example was mixed or pulverized and mixed, and 3 g of the obtained raw material mixture was molded under a pressure of 0.3 t / cm 2 with a uniaxial press to form a molded body having a diameter of 20 mm. Was made. Next, this molded body was fired in a box-type electric furnace at a heating rate of 300 ° C./h for 4 hours at 1450 ° C. to obtain an aluminum titanate ceramic sintered body. The density of this sintered body was measured by the Archimedes method, and was set as the density of the molded sintered body of the aluminum titanate ceramics of each example and comparative example.
- thermomechanical analyzer TMA (TMA6300, manufactured by SII Technology Co., Ltd.)
- the viscosity of the glass frit used in each experimental example and comparative example was measured as follows.
- the glass frit is molded by a uniaxial press and then sintered, and this sintered body is analyzed by a parallel plate measurement method using a wide-range viscosity measuring device (WRVM-313, manufactured by Opto Corporation), and the glass viscosity at 900 ° C. Asked.
- WRVM-313 wide-range viscosity measuring device
- Example 1 Titania powder [DuPont Co., Ltd., “R-900”] 20.0 g, ⁇ -alumina powder (Sumitomo Chemical Co., Ltd., “AES-12”) 27.4 g, magnesia powder [Ube Material Co., Ltd., “UC -95M "] and glass frit (manufactured by Takara Standard Co., Ltd., model number” CK0832M2 ", center particle size 7.4 ⁇ m, deflection point 768 ° C (measured by the manufacturer), viscosity value 1.1 ⁇ 10 9 poise) 1.8 g was charged into an alumina crushing container [internal volume of 3.3 L] together with 5 kg of alumina beads [diameter: 15 mm]. The x value of aluminum magnesium titanate in this aluminum titanate ceramic is about 0.09.
- the total volume of the mixture of these titania powder, ⁇ -alumina powder, magnesia powder and glass frit was about 50 cm 3 .
- the mixture in the pulverization container is pulverized by vibrating the pulverization container with a vibration mill for 2 minutes under conditions corresponding to a gravitational acceleration of 10 G at an amplitude of 5.4 mm, a vibration frequency of 1760 times / minute, and a power of 5.4 kW.
- a raw material mixture was obtained. 5 g of this raw material mixture was placed in an alumina crucible, heated in the atmosphere to 1450 ° C. at a temperature increase rate of 300 ° C./hour with a box-type electric furnace, and fired by maintaining the same temperature for 4 hours.
- the obtained aluminum titanate ceramics were pulverized in a mortar to obtain aluminum titanate ceramic powders.
- a crystal peak of aluminum magnesium titanate was shown, and a crystal peak of ⁇ -alumina was slightly observed. No crystal peak of the titania alkyl phase was observed.
- the AT conversion rate of this powder was determined to be 100%.
- the thermal decomposition rate of the obtained aluminum titanate ceramic was measured and found to be 7.4%.
- the shape of the powder was observed with an SEM, most of the particles constituting the powder were almost spherical.
- the value of the sintered compact density was measured, the value of 3.40 g / cm 3 was shown, and the value of the thermal expansion coefficient was 2.2 ⁇ 10 ⁇ 6 K ⁇ 1 .
- Example 1 Titanic acid was operated in the same manner as in Example 1 except that feldspar (Ohira feldspar obtained from Tokushu Seisaku Co., Ltd., model number “SS-300”) was used instead of the glass frit used in Example 1.
- An aluminum ceramic powder was obtained. The AT conversion rate of this aluminum titanate ceramic was determined and found to be 100%. Further, the thermal decomposition rate of the obtained aluminum titanate ceramic was measured and found to be 3.7%. Further, when the shape of the aluminum titanate ceramic powder was observed with an SEM, most of the particles constituting the powder were substantially spherical. Moreover, when the value of the sintered compact density was measured, it was 3.21 g / cm 3 and the coefficient of thermal expansion was 2.6 ⁇ 10 ⁇ 6 K ⁇ 1 .
- Example 1 the components and the ratio of the glass frit used in Example 1 and Comparative Example 2 were confirmed with a fluorescent X-ray analyzer [Rigaku ZSX Primus II]. The results are shown in Table 1.
- the aluminum titanate-based ceramics such as aluminum titanate or aluminum magnesium titanate obtained by the production method of the present invention can be used for various industrial applications.
- firing furnace jigs such as crucibles, setters, mortars, and furnace materials
- filters and catalyst carriers used for exhaust gas purification of internal combustion engines such as diesel engines and gasoline engines, filters for filtering food such as beer, and oil refining
- filters and catalyst carriers used for exhaust gas purification of internal combustion engines such as diesel engines and gasoline engines, filters for filtering food such as beer, and oil refining
- filters for filtering food such as beer
- oil refining examples thereof include electronic components such as ceramic filters, substrates, capacitors, and the like used for selective permeation filters for selectively permeating the generated gas components, carbon monoxide, carbon dioxide, nitrogen, oxygen, and the like.
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Abstract
Description
AT化率(%)=100×IAT/(IAT +IT)・・・(2)
熱分解率(%)=100-100×IAT2/(IAT2 +IT2)・・・(1)
チタニア粉末〔デュポン(株)、「R-900」〕20.0g、αアルミナ粉末〔住友化学(株)製、「AES-12」〕27.4g、マグネシア粉末〔宇部マテリアル(株)、「UC-95M」〕0.8gおよびガラスフリット〔タカラスタンダード(株)製、型番「CK0832M2」、中心粒径7.4μm、屈服点768℃(メーカー測定値)、粘度値1.1×109ポイズ〕1.8gを、アルミナビーズ〔直径15mm〕5kgと共にアルミナ製粉砕容器〔内容積3.3L〕に投入した。このチタン酸アルミニウム系セラミックス中のチタン酸アルミニウムマグネシウムのx値は約0.09である。
実施例1で用いた原料のガラスフリットの代わりに長石〔特殊精礦(株)より入手した大平長石、型番「SS-300」〕を用いた以外は実施例1と同様に操作し、チタン酸アルミニウム系セラミックスの粉末を得た。このチタン酸アルミニウム系セラミックスのAT化率を求めたところ100%であった。また、得られたチタン酸アルミニウム系セラミックスの熱分解率を測定したところ3.7%だった。またこのチタン酸アルミニウム系セラミックス粉末の形状をSEMにて観察したところ、粉末を構成する粒子のほとんどが概ね球形であった。また、焼結体密度の値を測定したところ3.21g/cm3の値を示し、熱膨張係数の値は2.6×10-6K-1の値を示した。
原料のガラスフリット〔タカラスタンダード(株)より入手したガラスフリット、型番「CK0314M2」、中心粒径7μm相当、屈服点610℃(メーカー測定値)、粘度値4.9×104ポイズ〕以外は実施例1と同様に操作し、チタン酸アルミニウム系セラミックスの粉末を得た。このチタン酸アルミニウム系セラミックスのAT化率を求めたところ100%であった。また、得られたチタン酸アルミニウム系セラミックスの熱分解率を測定したところ100%だった。またこのチタン酸アルミニウム系セラミックスの粉末の形状をSEMにて観察したところ、粉末を構成する粒子のほとんどが概ね球形であった。また、焼結体密度の値を測定したところ3.36g/cm3の値を示した。
Claims (14)
- チタン源化合物、アルミニウム源化合物、並びに屈服点が700℃以上および/または900℃の粘度値が1.0×106ポイズ以上のガラスフリットを含む原材料混合物を焼成することを特徴とするチタン酸アルミニウム系セラミックスの製造方法。
- チタニア換算のチタン源化合物の使用量は、チタニア換算のチタン源化合物の使用量およびアルミナ換算のアルミニウム源化合物の使用量の合計量100質量部あたり、30質量部~70質量部である請求項1に記載の製造方法。
- ガラスフリットの使用量は、チタニア換算のチタン源化合物の使用量およびアルミナ換算のアルミニウム源化合物の使用量の合計量100質量部あたり、0.1質量部~20質量部である請求項1または2に記載の製造方法。
- 前記原材料混合物が、さらにマグネシウム源化合物を含む請求項1~3のいずれか一項に記載のチタン酸アルミニウム系セラミックスの製造方法。
- マグネシア換算のマグネシウム源化合物の使用量は、チタニア換算のチタン源化合物の使用量およびアルミナ換算のアルミニウム源化合物の使用量の合計量100質量部あたり、0.1質量部~10質量部である請求項4に記載の製造方法。
- 前記マグネシウム源化合物が、酸化マグネシウムおよび/またはマグネシアスピネルである請求項4または5に記載の製造方法。
- 前記チタン源化合物が、酸化チタンである請求項1~6のいずれか一項に記載の製造方法。
- 前記アルミニウム源化合物が、酸化アルミニウムおよび/またはマグネシアスピネルである請求項1~7のいずれか一項に記載の製造方法。
- 前記ガラスフリットが、SiO2を50質量%以上含有するケイ酸ガラスである請求項1~8のいずれか一項に記載の製造方法。
- 前記原材料混合物を、乾式または湿式で混合する請求項1~9のいずれか一項に記載の製造方法。
- 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10に記載の製造方法。
- 前記粉砕メディアは、直径1mm~100mmのアルミナボールまたはジルコニアボールである請求項11に記載の製造方法。
- 前記粉砕容器を、2mm~20mmの振幅幅で振動させる請求項11または12に記載の製造方法。
- 請求項1~13のいずれか一項に記載の製造方法で、チタン酸アルミニウム系セラミックスを得、得られたチタン酸アルミニウム系セラミックスを解砕することを特徴とするチタン酸アルミニウム系セラミックス粉末の製造方法。
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- 2009-06-17 CN CN2009801228633A patent/CN102066287A/zh active Pending
- 2009-06-17 EP EP09766667A patent/EP2295388A4/en not_active Withdrawn
- 2009-06-17 WO PCT/JP2009/061006 patent/WO2009154219A1/ja active Application Filing
- 2009-06-17 KR KR1020107026227A patent/KR20110020235A/ko not_active Application Discontinuation
- 2009-06-17 JP JP2009144757A patent/JP5122527B2/ja not_active Expired - Fee Related
- 2009-06-18 TW TW098120459A patent/TW201010962A/zh unknown
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Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2011008938A1 (en) * | 2009-07-15 | 2011-01-20 | E.I. Du Pont De Nemours And Company | Aluminium magnesium titanate composite ceramics |
WO2011081217A1 (ja) * | 2009-12-28 | 2011-07-07 | 住友化学株式会社 | チタン酸アルミニウム系セラミックスの製造方法 |
WO2011111666A1 (ja) * | 2010-03-08 | 2011-09-15 | 住友化学株式会社 | グリーン成形体、及び、チタン酸アルミニウム焼成体の製造方法 |
WO2011118025A1 (ja) * | 2010-03-26 | 2011-09-29 | 大塚化学株式会社 | 柱状チタン酸アルミニウム及びその製造方法 |
CN102811972A (zh) * | 2010-03-26 | 2012-12-05 | 大塚化学株式会社 | 柱状钛酸铝及其制造方法 |
US8859447B2 (en) | 2010-03-26 | 2014-10-14 | Otsuka Chemical Co., Ltd. | Columnar aluminum titanate and method for producing same |
CN102811972B (zh) * | 2010-03-26 | 2015-03-25 | 大塚化学株式会社 | 柱状钛酸铝及其制造方法 |
EP2551251A4 (en) * | 2010-03-26 | 2015-06-17 | Otsuka Chemical Co Ltd | COLUMN ALUMINUM TITANATE AND MANUFACTURING METHOD THEREFOR |
WO2023157574A1 (ja) * | 2022-02-18 | 2023-08-24 | デンカ株式会社 | 粉末及び粉末の製造方法 |
Also Published As
Publication number | Publication date |
---|---|
EP2295388A1 (en) | 2011-03-16 |
EP2295388A4 (en) | 2011-11-02 |
TW201010962A (en) | 2010-03-16 |
US20110124484A1 (en) | 2011-05-26 |
JP2010159197A (ja) | 2010-07-22 |
JP5122527B2 (ja) | 2013-01-16 |
KR20110020235A (ko) | 2011-03-02 |
CN102066287A (zh) | 2011-05-18 |
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