WO2005077859A1 - 導電性マイエナイト型化合物の製造方法 - Google Patents
導電性マイエナイト型化合物の製造方法 Download PDFInfo
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- WO2005077859A1 WO2005077859A1 PCT/JP2005/001848 JP2005001848W WO2005077859A1 WO 2005077859 A1 WO2005077859 A1 WO 2005077859A1 JP 2005001848 W JP2005001848 W JP 2005001848W WO 2005077859 A1 WO2005077859 A1 WO 2005077859A1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/653—Processes involving a melting step
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/16—Preparation of alkaline-earth metal aluminates or magnesium aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/164—Calcium aluminates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3213—Strontium oxides or oxide-forming salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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
Definitions
- the present invention relates to a method for producing a mayenite compound having conductivity.
- Ca or A1 is a general component of ceramic materials, and has been mainly used as one component of structural materials. Generally, oxides of metals before the third cycle containing the compound are electrically dielectric and do not show conductivity.
- the mayenite-type compound crystal has 12 microscopic voids (cage) having a diameter of 0.6 nm per unit lattice in its crystal lattice, and its representative composition, C12A7 crystal, is contained in the cage per unit lattice. Includes two ⁇ 2 ions. That is, C12A7 crystal has [Ca A1 ⁇
- Hosono et al. Have developed a method for producing a C12A7 single crystal, and have found that by exposing the crystal to an alkali vapor, electrons can be included in a cage to impart conductivity to the crystal.
- a patent application was filed for an invention relating to the compound itself, a method for producing the compound, and uses of the compound (see Patent Document 6).
- the reaction of drawing out free oxygen from the C12A7 crystal in the solid state is used.
- diffusion of oxygen inside the solid is a rate-determining process, so that a sufficient amount of electrons can be included. It took a long time.
- Non-Patent Document 4 Hosono et al., One of the present inventors, used a hydrostatic pressed body having a more compact structure as compared with powder to reduce the surface area of the raw material, which is a reaction that occurs on the surface during the heating process. Having obtained the knowledge that the oxygen abstraction reaction can be slowed and the generation of decomposition products can be suppressed, the isostatic press body of C12A7 powder was melted in a reducing atmosphere or a carbon crucible with a lid, and the inside of the cage was melted. Preparation of C12A7 compounds in which oxygen is replaced by electrons Invented the law and filed a patent application (see Patent Document 6).
- Non-Patent Document 4 R.W.Nurse, J.H Welch, A.J.Majumdar, Transactions of the British Ceramic Society (1965), 64 (9), 409-18.
- the present invention is to adjust the electric conductivity by keeping the conductive mayenite type compound produced by the production method in air at a temperature of 500 ° C or more and a melting point or less of the compound. And a method for producing a conductive mayenite compound.
- the conductive mayenite type compound contained in the solidified product is less than 25%, so that conductivity is not provided. Especially when the content is 35-39%, the yield of the conductive mayenite type compound is the best.
- the raw material contains less than 1% of each of the typical metal elements or the transition metal elements, each of which is less than 1%.
- a raw material containing at least one selected from the group consisting of Ca and Sr and A1 is melted.
- the melting temperature is 1415 ° C. or higher, lower than the boiling point of the raw material, and is preferably 1550 ° C. to 1650 ° C. If the temperature is lower than 1415 ° C, a dense solidified product cannot be obtained because the raw material does not melt. If the boiling point is higher than the boiling point, the initial composition cannot be maintained due to the difference in the vapor pressure of the constituent elements, so that a conductive mayenite compound cannot be obtained.
- a temperature of 1550 ° C-1650 ° C is appropriate for rapid melting using a normal electric furnace.
- the oxygen partial pressure in a sealed atmosphere at 1600 ° C is about 10-15 Pa.
- the atmosphere of the oxygen partial pressure lOPa following low oxygen partial pressure particularly preferably in the range of about 10- 18 Pa one 10- 2 Pa.
- the oxygen partial pressure is less 10- 2 Pa, results oxidation of the conductive My Enaito type compound is suppressed, resulting in an increase in conductivity of the solidified product Wear. Further, in the following 10- 18 Pa, it is necessary expensive equipment.
- a carbon crucible with a lid is preferably used when the crucible is held in a normal electric furnace.
- an oxide crucible such as magnesia or alumina, a noble metal crucible such as platinum or molybdenum, or an industrially advantageous brick material can be used.
- the oxygen partial pressure in the case of cooling in an atmosphere of the low oxygen partial pressure and more preferably specifically shall be the range of about 10- 18 Pa- 10- 2 Pa.
- the oxygen partial pressure is less 10- 2 Pa, it is possible to increase the conductivity of the solidified product. Further, in the following 10- 18 Pa, it is necessary expensive equipment.
- the cooling rate is generally preferably more than 500 ° C / hour and 1000 ° CZ minutes or less, more preferably more than 500 ° C / hour and 1000 ° CZ hours or less. If the heating time is less than 500 ° CZ, the coating with the glassy portion may not be formed sufficiently, and the amount of electrons included in the mayenite-type compound to be produced may not be sufficient. When the temperature exceeds 1000 ° C / sec, the entire melt becomes vitreous, and the yield of the conductive mayenite compound decreases.
- the cooling rate and form were controlled using a twin roller, and the oxygen partial pressure of the melt was lOPa or less.
- a conductive mayenite-type compound in which oxygen in the cage is replaced with electrons at a high concentration can be produced. According to this method, it is possible to provide a method for producing a conductive mayenite-type compound by omitting a step of producing a crystal of a non-conductive mayenite-type compound which has been used as a precursor of a conductive mayenite-type compound. it can.
- C12A7 is a typical composition of a mayenite type compound, as an example.
- the degree of the oxygen abstraction reaction during the temperature raising process varies depending on the form of the raw material.
- the free oxygen extraction reaction proceeds near the surface of the raw material, and the amount of oxygen extracted depends on the surface area of the raw material.
- the reaction with the atmosphere or the crucible material promotes the oxygen extraction reaction from the melt and the accompanying donation of electrons to the melt.
- the proportion depends on the retention time and the mass of the melt.
- the decomposition product phase changes with an increase in the amount of substitution of oxygen and electrons as the melting time changes.
- the nucleation rate of the C12A7 crystal is shortly after the start of melting, because the nuclei of the C12A7 crystal nucleus are in a sufficient concentration, so that the C12A7 crystal is generated from the solidified product, but the amount of oxygen and electron exchange is small, so the generation rate is low. Almost all of the cages of the C12A7 dangling products are occupied by oxygen.
- the decomposition time phase and the C12A7 compound phase may be obtained as a coagulated product due to the change in the melting time, but the desired conductive mayenite type compound can be obtained by controlling the retention time and the melting temperature. .
- the obtained coagulated product was a dense solid having a black color.
- the powder had a dark green color. From the X-ray diffraction pattern, this solid was a mayenite type compound.
- the electrical conductivity was about 5 S / cm.
- the obtained coagulated product was a colorless solid, and from the X-ray diffraction pattern, was a mayenite-type compound, but did not exhibit conductivity.
- the obtained coagulated product was a dense solid having a black color.
- the powder had a dark green color.
- the solidified product was a mayenite type compound.
- the electrical conductivity was about 5S / cm.
- the obtained coagulated product was a dense solid having a black color.
- the powder had a dark green color.
- the solidified product was a mayenite type compound.
- the electrical conductivity was about 5SZcm.
- the conductive mayenite conjugate is an electron donor, the reducing agent or the nucleophilic As a reagent, it can be used for decomposition of organic substances. Also, by utilizing the property of taking in anions into the gauge, it can be used for recovery of chlorine, fluorine, bromine, iodine, etc. with high environmental load. These anions may be part of the compound. Also, iodine may be radioactive.
- the conductive mayenite conjugate is a field-effect type electron-emitting material, a small-sized electron-emitting device, display device, or X-ray source can be manufactured by using this property.
- an electrode material it can be used as a conductor requiring special bonding characteristics, such as a charge injection material in an organic EL device.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
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Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE602005015548T DE602005015548D1 (de) | 2004-02-13 | 2005-02-08 | Verfahren zur herstellung einer elektrisch leitfähigen verbindung vom mayenit-typ |
JP2005517942A JP4641946B2 (ja) | 2004-02-13 | 2005-02-08 | 導電性マイエナイト型化合物の製造方法 |
EP05709900A EP1717217B1 (en) | 2004-02-13 | 2005-02-08 | Method for preparing electroconductive mayenite type compound |
US11/503,244 US7465433B2 (en) | 2004-02-13 | 2006-08-14 | Method for preparing electroconductive mayenite type compound |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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JP2004037203 | 2004-02-13 | ||
JP2004-037203 | 2004-02-13 |
Related Child Applications (1)
Application Number | Title | Priority Date | Filing Date |
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US11/503,244 Continuation US7465433B2 (en) | 2004-02-13 | 2006-08-14 | Method for preparing electroconductive mayenite type compound |
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WO2005077859A1 true WO2005077859A1 (ja) | 2005-08-25 |
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PCT/JP2005/001848 WO2005077859A1 (ja) | 2004-02-13 | 2005-02-08 | 導電性マイエナイト型化合物の製造方法 |
Country Status (6)
Country | Link |
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US (1) | US7465433B2 (ja) |
EP (1) | EP1717217B1 (ja) |
JP (1) | JP4641946B2 (ja) |
DE (1) | DE602005015548D1 (ja) |
TW (1) | TWI283234B (ja) |
WO (1) | WO2005077859A1 (ja) |
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Also Published As
Publication number | Publication date |
---|---|
EP1717217A4 (en) | 2008-09-03 |
EP1717217A1 (en) | 2006-11-02 |
TWI283234B (en) | 2007-07-01 |
TW200536781A (en) | 2005-11-16 |
JPWO2005077859A1 (ja) | 2007-10-18 |
JP4641946B2 (ja) | 2011-03-02 |
DE602005015548D1 (de) | 2009-09-03 |
EP1717217B1 (en) | 2009-07-22 |
US7465433B2 (en) | 2008-12-16 |
US20060276326A1 (en) | 2006-12-07 |
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