WO2009087912A1 - チタン酸アルミニウムセラミックスの製造方法 - Google Patents
チタン酸アルミニウムセラミックスの製造方法 Download PDFInfo
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- WO2009087912A1 WO2009087912A1 PCT/JP2008/073596 JP2008073596W WO2009087912A1 WO 2009087912 A1 WO2009087912 A1 WO 2009087912A1 JP 2008073596 W JP2008073596 W JP 2008073596W WO 2009087912 A1 WO2009087912 A1 WO 2009087912A1
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Definitions
- the present invention relates to a method for producing aluminum titanate ceramics, and more particularly to a method for producing aluminum titanate ceramics in a dry manner.
- Aluminum titanate ceramics are obtained by firing a titanium source powder and an alumina source powder, and are known as ceramics having excellent heat resistance.
- Non-Patent Document 1 Key Engineering Materials Vol. 336-338 (2007) P1327-1330
- titania source powder and alumina source powder are pulverized in water and evaporated to dryness.
- a method for firing the obtained precursor mixture is disclosed.
- Patent Document 1 discloses that a titania source powder and an alumina source powder are pulverized in the presence of various auxiliaries composed of a small amount of organic components, and the resulting powdery precursor mixture is calcined. A method is disclosed.
- the present inventors have intensively studied to develop a method capable of producing an aluminum titanate ceramic by firing the precursor mixture in a shorter time, and as a result, the present invention has been achieved.
- a titania source powder and an alumina source powder are mixed, and pulverized under a pulverization condition of acceleration 2G or higher in the presence of pulverization media to obtain a precursor mixture, and the obtained precursor mixture is fired.
- the manufacturing method of the aluminum titanate ceramics characterized by the above-mentioned is provided.
- the amount of titania-converted titania source powder used is 30 to 70 parts by mass per 100 parts by mass of the total amount of titania-converted titania source powder and alumina-converted alumina source powder. Preferably there is.
- the titania source powder and the alumina source powder are preferably mixed together with the magnesia source powder, and the titania source powder and the alumina source powder may be mixed together with the silica source powder.
- the silica source powder is also preferably feldspar or glass frit powder.
- the vibration mill preferably has an amplitude of 2 to 20 mm and a vibration frequency of 500 to 5000 times / minute.
- the amount of magnesia-converted magnesia source powder used is 10 parts by mass or less per 100 parts by mass of the total amount of titania-converted titania source powder and alumina-converted alumina source powder. It is preferable. Further, the amount of silica source powder converted to silica is preferably 20 parts by mass or less per 100 parts by mass of the total amount of titania source powder used and titania source powder used.
- the present invention also includes a method for producing an aluminum titanate ceramic powder characterized in that the aluminum titanate ceramic is obtained by any one of the production methods described above and the obtained aluminum titanate ceramic is crushed.
- the present invention is a method for producing a precursor mixture containing a titania source powder and an alumina source powder and being led to an aluminum titanate ceramic by firing.
- the titania source powder and the alumina source powder are mixed and dried.
- an aluminum titanate ceramic can be produced by firing the precursor mixture in a short time.
- titania source powder used in the production method of the present invention examples include titanium oxide powder.
- titanium oxide examples include titanium (IV) oxide, titanium (III) oxide, and titanium (II) oxide. Titanium (IV) oxide is preferably used.
- examples of the crystalline form of titanium oxide (IV) include anatase type, rutile type, brookite type and the like, and it may be amorphous, more preferably anatase type and rutile type.
- the titania source powder includes a powder of a compound that is led to titania (titanium oxide) by firing alone 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).
- the titania source powder may be used alone or in combination of two or more.
- the titanium source powder is preferably a titanium oxide powder.
- the titania source powder may contain inevitable impurities derived from raw materials or mixed in the manufacturing process.
- Examples of the alumina source powder include alumina (aluminum oxide) powder.
- Examples of the crystal type of alumina include ⁇ type, ⁇ type, ⁇ type, and ⁇ type, and may be amorphous.
- the alumina source powder is preferably ⁇ -type alumina.
- the alumina source powder may be a powder of a compound led to alumina by firing alone in air.
- the compound to be applied include aluminum salts, aluminum alkoxides, aluminum hydroxide, metal aluminum and the like.
- the aluminum salt may be an inorganic salt with an inorganic acid or an organic salt with an organic acid.
- the aluminum inorganic salt include aluminum nitrates such as aluminum nitrate and ammonium nitrate, and aluminum carbonates such as ammonium aluminum carbonate.
- 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.
- Examples of the aluminum hydroxide crystal type include a gibbsite type, a bayerite type, a norosotrandite type, a boehmite type, and a pseudo-boehmite type, and may be amorphous (amorphous).
- 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.
- alumina source powder only one type of alumina source powder may be used, or two or more types may be used in combination.
- the alumina source powder is preferably an alumina powder.
- the alumina source powder may contain inevitable impurities derived from raw materials or mixed in the manufacturing process.
- the amount of titania source powder and alumina source powder used is determined based on the results converted to titania [TiO 2 ] and alumina [Al 2 O 3 ].
- the total amount of titania-converted titania source powder and alumina-converted alumina source powder used per 100 parts by weight is usually 30 to 70 parts by weight of titania-converted titania source powder.
- the amount of source powder used is 70 to 30 parts by mass, preferably 40 to 60 parts by mass of titania source powder converted to titania, and the amount of alumina source powder converted to alumina is 60 to 40 parts by mass. Part.
- the titania source powder and the alumina source powder are raw material powders. These raw material powders are mixed and pulverized in a dry process to obtain a precursor mixture.
- a titania source powder and an alumina source powder may be mixed with a magnesia source powder, and pulverized by a dry method to obtain a precursor mixture.
- magnesia source powder examples include magnesia (magnesium oxide) powder.
- the magnesia source powder also includes a compound that is led to magnesia by firing alone in air.
- a compound that is led to magnesia by firing alone in air examples include magnesium salt, magnesium alkoxide, magnesium hydroxide, magnesium nitride, and magnesium metal.
- 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.
- magnesium alkoxide examples include magnesium methoxide and magnesium ethoxide.
- magnesia source powder a powder that also serves as the alumina source powder can be used.
- magnesia spinel (MgAl 2 O 4 ) powder examples include magnesia spinel (MgAl 2 O 4 ) powder.
- magnesia source powder only one type of magnesia source powder may be used, or two or more types may be used in combination.
- the magnesia source powder may contain inevitable impurities derived from raw materials or mixed in during the manufacturing process.
- the amount of magnesia source powder used when converted to magnesia [MgO] is 100 mass of the amount of titania source powder converted to titania [TiO 2 ] and the amount of alumina source powder converted to alumina [Al 2 O 3 ].
- the amount is usually 0.1 to 10 parts by weight, preferably 8 parts by weight or less per part.
- the titania source powder and alumina source powder and in some cases, in addition to these, magnesia source powder is used as a raw material powder, and these raw material powders are mixed and pulverized in a dry process to obtain a precursor mixture.
- These raw material powders may be mixed with the silica source powder and pulverized in a dry process to obtain a precursor mixture.
- silica source powder examples include silicon oxide (silica) such as silicon dioxide and silicon monoxide.
- the silica source powder may be a powder of a compound led to silica by firing alone in air.
- examples of such compounds include silicic acid, silicon carbide, silicon nitride, silicon sulfide, silicon tetrachloride, silicon acetate, sodium silicate, sodium orthosilicate, glass frit and the like, and are preferably easily available industrially. At some point, glass frit and the like can be mentioned.
- silica source powder a powder that also serves as the alumina source powder can be used.
- An example of such a powder is feldspar powder.
- the silica source powder may be used alone or in combination of two or more.
- the silica source powder may contain inevitable impurities derived from raw materials or mixed in during the manufacturing process.
- the amount of silica source powder converted to silica [SiO 2 ] is 100 parts by mass of the total amount of titania source powder converted to titania [TiO 2 ] and alumina source powder converted to alumina [Al 2 O 3 ].
- the amount is usually 0.1 to 20 parts by mass, preferably 10 parts by mass or less.
- the above-mentioned titania source powder and alumina source powder are mixed with magnesia source powder and / or silica source powder as necessary, and pulverized in a dry process to obtain a precursor mixture, and the obtained precursor mixture is obtained. It is what is fired.
- the raw material powder may be dispersed and pulverized in a small amount of liquid medium as long as a substantially dry state can be maintained.
- the raw material powder is usually pulverized without being dispersed in the liquid medium.
- a suitable grinding container is used for grinding. In this pulverization container, the raw material powder can be pulverized by colliding the container, the raw material powder and the 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 pulverization container is usually 1 to 4 times, preferably 1.2 to 3 times the volume of the total volume of the raw material powder and pulverization media.
- the grinding media include alumina beads and zirconia beads having a diameter of 1 to 100 mm, preferably 5 to 50 mm.
- the hardness of the grinding media is preferably 6 or more, more preferably 8 or more in terms of Mohs hardness.
- the amount of grinding media used is usually from 1 to 1000 times the total amount of raw material powder, that is, titania source powder, alumina source powder and magnesia source powder, and silica source powder when silica source powder is used. Times, preferably 5 to 100 times by mass.
- the pulverization is preferably performed by oscillating or rotating the pulverization container after putting the raw material powder and the pulverization medium into the pulverization container.
- the raw material powder is agitated and mixed together with the grinding media, and is pulverized by being sandwiched between the grinding media that collide with each other and between the grinding media and the inner wall of the grinding container.
- a normal pulverizer such as a vibration mill or a planetary mill can be used, and the vibration mill is preferably used because it can be easily implemented on an industrial scale. It is done.
- the raw material powder is pulverized under the pulverization condition with an acceleration of 2G or more, that is, an acceleration of 2 times or more of the gravitational acceleration (9.8 m / sec 2 ), usually 20G or less, that is, 20 times of the gravitational acceleration. Grind under the following grinding conditions.
- the acceleration is preferably about 3 to 17G, more preferably about 5 to 15G.
- the amplitude of vibration is usually 2 mm to 20 mm, preferably 12 mm or less, and the frequency is usually 500 times / minute to 5000 times. / Min.
- 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 grinding is usually 1 minute to 6 hours, preferably 1.5 minutes to 2 hours.
- additives such as a pulverizing aid and a peptizer may or may not be added.
- the additive is preferably not added in consideration of the ease of post-treatment, but may be added in a small amount as long as the dry state can be substantially maintained.
- the grinding aid examples include alcohols such as methanol, ethanol and propanol, glycols such as propylene glycol, polypropylene glycol and ethylene glycol, amines such as triethanolamine, 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 about 100 parts by mass of the total amount of raw material powder, ie, titania source powder, alumina source powder and magnesia source powder, and silica source powder when silica source powder is used.
- the amount is 0.1 to 10 parts by mass, preferably 0.5 to 5 parts by mass, and more preferably 0.75 to 2 parts by mass.
- a precursor mixture is obtained by pulverizing in a dry manner.
- the desired aluminum titanate ceramic is obtained by firing the precursor mixture.
- the calcination temperature is usually 1300 ° C. or higher, preferably 1400 ° C. or higher, and is usually 1600 ° C. or lower, preferably 1550 ° C. or lower in that the obtained aluminum magnesium titanate is easily crushed.
- the rate of temperature rise up to the firing temperature is not particularly limited, and is usually 2 ° C./hour to 500 ° C./hour.
- the rate of temperature rise is more preferably 10 ° C./hour to 450 ° C./hour, and further preferably 50 ° C./hour to 400 ° C./hour. In the middle of raising the temperature to the firing temperature, a process of maintaining a constant temperature may be provided.
- Firing is usually performed in the atmosphere, but when using raw material powders, ie, titania source powder, alumina source powder and magnesia source powder, and silica source powder, depending on the type and amount ratio of silica source powder, nitrogen may be used. It may be fired in an inert gas such as gas or argon 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.
- an inert gas such as gas or argon gas
- a reducing gas such as carbon monoxide gas or hydrogen gas.
- 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 precursor mixture transitions to the aluminum titanate ceramics, and varies depending on the amount of the precursor mixture, the type of firing furnace, firing temperature, firing atmosphere, etc. Min to 24 hours.
- the precursor mixture is usually fired in the form of a powder, but may be molded and fired as a molded body.
- the molding machine used for molding include a single screw extruder, a single screw press, a tableting machine, and a granulator.
- the precursor mixture can be molded by adding additives such as a pore-forming agent, a binder, a lubricant, a plasticizer, a dispersant, and a solvent.
- additives such as a pore-forming agent, a binder, a lubricant, a plasticizer, a dispersant, and a solvent.
- 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 or dry ice, and the like.
- 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 of these binders also serve as a pore-forming agent.
- the binder that also functions as a pore-forming agent functions as a binder that adheres particles to each other at the time of molding to retain the shape of the molded body, and functions as a pore-forming agent that burns itself to form pores during subsequent firing.
- polyethylene or the like 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 stearic acid metal salts such as Al stearate. Such lubricants usually also function as plasticizers.
- alcohols such as methanol and ethanol are usually used in addition to ion-exchanged water.
- the desired aluminum titanate ceramics can be obtained as a fired product.
- the calcined aluminum titanate ceramic is usually in the form of a lump, but the aluminum titanate ceramic powder can be obtained by crushing. 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 handling container or the like is not worn when it is handled.
- the obtained aluminum titanate ceramics may contain inevitable impurities derived from raw materials or mixed in the manufacturing process.
- An aluminum titanate ceramic molded body can be obtained by molding and firing the aluminum titanate ceramic powder thus obtained.
- molded bodies include 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, catalyst carriers, and food and drink such as beer. Filters used for the filtration of substances, gas components generated during oil refining, such as carbon monoxide, carbon dioxide, and selective permeation filters for selectively permeating nitrogen, oxygen, etc. Ceramic filters, substrates, capacitors, etc. Examples include electronic parts.
- the obtained aluminum titanate ceramic molded body may be shaped by polishing or the like if necessary. Moreover, the obtained aluminum titanate ceramic molded body may contain inevitable impurities derived from raw materials or mixed in the manufacturing process.
- the following formula (1) Calculated by The shape of the aluminum titanate was determined by observing with a scanning electron microscope [SEM].
- Example 1 19.6 g of titanium oxide powder [DuPont Co., Ltd., “R-900”], 27.0 g of ⁇ -alumina powder (manufactured by Sumitomo Chemical Co., Ltd., “AES-12”), magnesium carbonate powder [Kamishima Chemical Co., Ltd.] 1.6 g of “Venus” and 1.8 g of powdered feldspar (Ohira feldspar, model number “SS-300” obtained from Tokushu Seiki Co., Ltd.) together with 5 kg of alumina beads (diameter 15 mm) [contents] Product 3.3L].
- the total volume of the mixture of titanium oxide powder, ⁇ -alumina powder and feldspar 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 at an amplitude of 5.4 mm, a frequency of 1760 times / minute (equivalent to an acceleration of 10 G), and a power of 5.4 kW. Obtained. 5 g of this precursor 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. Then, it stood to cool to room temperature and obtained the baked product. The fired product was crushed in a mortar to obtain a powder.
- this powder When a diffraction spectrum of this powder was obtained by powder X-ray diffraction, this powder showed a crystal peak of aluminum magnesium titanate. The AT conversion rate of this powder was determined to be 100%. Further, when the shape of the powder was observed with an SEM, most of the particles constituting the powder were substantially spherical.
- Comparative Example 1 The same titanium oxide powder as used in Example 1 [DuPont Co., Ltd., “R-900”], ⁇ -alumina powder [manufactured by Sumitomo Chemical Co., Ltd., “AES-12”], magnesium carbonate powder [Kanjima Chemical Co., Ltd.] , “Venus”] and feldspar (Ohira feldspar obtained from Tokusei Seisaku Co., Ltd., model number “SS-300”) were weighed in the same amount as in Example 1 and mixed in a plastic bag to obtain a precursor mixture. Obtained. 5 g of this precursor mixture was weighed without being pulverized, fired in the same manner as in Example 1, and pulverized to obtain a powder.
- Example 2 The amount of titanium oxide powder [R-900] used is 23.0 g, the amount of ⁇ -alumina powder [AES-12] is 19.6 g, the amount of magnesium carbonate powder [Venus] is 4.0 g, and feldspar.
- a calcined product was obtained by operating in the same manner as in Example 1 except that the amount of [SS-300] used was changed to 3.3 g.
- the obtained powder showed an X-ray diffraction peak of aluminum magnesium titanate, and its AT conversion was 100%. Further, in this powder, most of the particles constituting the powder were substantially spherical.
- Example 3 Titanium oxide powder [R-900] 20.0 g, ⁇ -alumina powder [Sumitomo Chemical Co., Ltd., “AES-12”] 27.4 g, magnesia powder [Ube Material Co., Ltd. “UC-95M”] 0 8 g and 1.8 g of glass frit (manufactured by Takara Standard Co., Ltd., “CK5431M2”) together with 5 kg of alumina beads (diameter: 15 mm) were put into an alumina crushing container (internal volume: 3.3 L). By operating in the same manner, a precursor mixture was obtained, a fired product was obtained, and a powder was obtained.
- this powder When a diffraction spectrum of this powder was obtained by powder X-ray diffraction, this powder showed a crystal peak of aluminum magnesium titanate. The AT conversion rate of this powder was determined to be 100%. Further, when the shape of the powder was observed with an SEM, most of the particles constituting the powder were substantially spherical.
- the aluminum titanate ceramics obtained by the production method of the present invention include, for example, exhaust gas filters used for exhaust gas purification of internal combustion engines such as crucibles, setters, mortars, furnace materials such as furnace materials, diesel engines, gasoline engines, etc.
- Filter filters used for filtering foods and drinks such as catalyst carriers, beer, gas components generated during petroleum refining, such as carbon monoxide, carbon dioxide, and selective permeation filters for selectively permeating nitrogen, oxygen, etc. It is suitable as an electronic component such as a ceramic filter, a substrate, or a capacitor.
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Abstract
Description
により算出した。チタン酸アルミニウムの形状は、走査型電子顕微鏡〔SEM〕により観察して判定した。
酸化チタン粉末〔デュポン(株)、「R-900」〕19.6g、αアルミナ粉末〔住友化学(株)製、「AES-12」〕27.0g、炭酸マグネシウム粉末〔神島化学(株)、「金星」〕1.6gおよび粉末状長石〔特殊精礦(株)より入手した大平長石、型番「SS-300」〕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。これら酸化チタン粉末、αアルミナ粉末および長石の混合物の合計容積は約50cm3であった。その後、粉砕容器を振動ミルにより振幅5.4mm、振動数1760回/分〔加速度10G相当〕、動力5.4kWにて2分間振動させることにより粉砕容器内の混合物を粉砕し、前駆体混合物を得た。この前駆体混合物のうち5gをアルミナ製ルツボに入れ、大気中、箱型電気炉により昇温速度300℃/時間で1450℃まで昇温し、同温度を4時間保持することにより焼成した。その後、室温まで放冷して、焼成物を得た。この焼成物を乳鉢にて解砕して粉末を得た。粉末X線回折法により、この粉末の回折スペクトルを得たところ、この粉末は、チタン酸アルミニウムマグネシウムの結晶ピークを示した。この粉末のAT化率を求めたところ、100%であった。また、この粉末の形状をSEMにて観察したところ、粉末を構成する粒子の殆どが概ね球形であった。
実施例1で用いたと同じ酸化チタン粉末〔デュポン(株)、「R-900」〕、αアルミナ粉末〔住友化学(株)製、「AES-12」〕、炭酸マグネシウム粉末〔神島化学(株)、「金星」〕および長石〔特殊精礦(株)より入手した大平長石、型番「SS-300」〕をそれぞれ実施例1と同じ量だけ秤量し、ポリ袋中で混合して前駆体混合物を得た。この前駆体混合物を粉砕することなく5gを秤取し、実施例1と同様にして焼成し、解砕して、粉末を得た。この粉末の粉末X線回折スペクトルから、粉末を同定したところ、チタン酸アルミニウムマグネシウム、チタニア(ルチル型)の回折ピークが確認できた。この粉末のAT化率は50%であった。また、この粉末の形状をSEMにて観察したところ、殆どの粒子が不定形状であった。
酸化チタン粉末〔R-900〕の使用量を23.0gとし、αアルミナ粉末〔AES-12〕の使用量を19.6gとし、炭酸マグネシウム粉末〔金星〕の使用量を4.0gとし、長石〔SS-300〕の使用量を3.3gとした以外は実施例1と同様に操作して焼成物を得、粉末を得た。得られた粉末は、チタン酸アルミニウムマグネシウムのX線回折ピークを示し、そのAT化率は100%であった。また、この粉末は、粉末を構成する粒子の殆どが概ね球形であった。
酸化チタン粉末〔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)製、「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、「CK5431M2」〕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、その後、実施例1と同様に操作して前駆体混合物を得、焼成物を得、粉末を得た。粉末X線回折法により、この粉末の回折スペクトルを得たところ、この粉末は、チタン酸アルミニウムマグネシウムの結晶ピークを示した。この粉末のAT化率を求めたところ、100%であった。また、この粉末の形状をSEMにて観察したところ、粉末を構成する粒子の殆どが概ね球形であった。
Claims (11)
- チタニア源粉末およびアルミナ源粉末を混合し、粉砕メディアの共存下に乾式にて加速度2G以上の粉砕条件で粉砕して前駆体混合物を得、得られた前駆体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セラミックスの製造方法。
- チタニア換算のチタニア源粉末の使用量が、チタニア換算のチタニア源粉末の使用量とアルミナ換算のアルミナ源粉末の使用量の合計量100質量部あたり、30~70質量部である請求項1に記載の製造方法。
- チタニア源粉末およびアルミナ源粉末をマグネシア源粉末と共に混合する請求項1または2に記載の製造方法。
- マグネシア換算のマグネシア源粉末の使用量が、チタニア換算のチタニア源粉末の使用量とアルミナ換算のアルミナ源粉末の使用量の合計量100質量部あたり、10質量部以下である請求項3に記載の製造方法。
- チタニア源粉末およびアルミナ源粉末をシリカ源粉末と共に混合する請求項1~4のいずれかに記載の製造方法。
- シリカ換算のシリカ源粉末の使用量が、チタニア換算のチタニア源粉末の使用量とアルミナ換算のアルミナ源粉末の使用量の合計量100質量部あたり、20質量部以下である請求項5に記載の製造方法。
- シリカ源粉末が、長石またはガラスフリットの粉末である請求項5または6に記載の製造方法。
- 振動ミルにより粉砕する請求項1~7のいずれかに記載の製造方法。
- 振動ミルの振幅が2~20mm、振動数が500~5000回/分である請求項8に記載の製造方法。
- 請求項1~9のいずれかに記載の製造方法により得られたチタン酸アルミニウム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セラミックス粉末の製造方法。
- チタニア源粉末およびアルミナ源粉末を含み、焼成されることによりチタン酸アルミニウムセラミックスに導かれる前駆体混合物を製造する方法であり、チタニア源粉末およびアルミナ源粉末を混合し、乾式にて加速度2G以上の粉砕条件で粉砕することを特徴とする前記前駆体混合物の製造方法。
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US20110156323A1 (en) * | 2008-09-04 | 2011-06-30 | Sumitomo Chemical Company, Limited | Process for producing aluminum titanate-based ceramics |
WO2012101285A1 (de) * | 2011-01-28 | 2012-08-02 | Mann+Hummel Gmbh | Keramischer körper aus einer aluminiumtitanatmischung |
US9908260B2 (en) | 2013-05-20 | 2018-03-06 | Corning Incorporated | Porous ceramic article and method of manufacturing the same |
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