CA2643369A1 - Titanium oxide, conductive titanium oxide, and processes for producing these - Google Patents

Titanium oxide, conductive titanium oxide, and processes for producing these Download PDF

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CA2643369A1
CA2643369A1 CA002643369A CA2643369A CA2643369A1 CA 2643369 A1 CA2643369 A1 CA 2643369A1 CA 002643369 A CA002643369 A CA 002643369A CA 2643369 A CA2643369 A CA 2643369A CA 2643369 A1 CA2643369 A1 CA 2643369A1
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titanium dioxide
titanium
electro
compound
axis length
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CA2643369C (en
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Kaoru Isobe
Katsuichi Chiba
Takanori Sakamoto
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Ishihara Sangyo Kaisha Ltd
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    • C01G23/047—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
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    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C—CHEMISTRY; METALLURGY
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    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/628—Coating the powders or the macroscopic reinforcing agents
    • C04B35/62886—Coating the powders or the macroscopic reinforcing agents by wet chemical techniques
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/20—Light-sensitive devices
    • H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
    • H01G9/2031—Light-sensitive devices comprising an oxide semiconductor electrode comprising titanium oxide, e.g. TiO2
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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
    • C04B2235/30—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
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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    • C04B2235/38—Non-oxide ceramic constituents or additives
    • C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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    • C04B2235/5436—Particle size related information expressed by the size of the particles or aggregates thereof micrometer sized, i.e. from 1 to 100 micron
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E10/542—Dye sensitized solar cells
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
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    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2991—Coated

Abstract

Titanium dioxide and a conductive titanium oxide which each includes particles having a large major-axis length in a large proportion and comprises columnar particles having a satisfactory particle size distribution. A titanium compound, an alkali metal compound, and an oxyphosphorus compound are heated/burned in the presence of titanium dioxide nucleus crystals having an aspect ratio of 2 or higher to grow the titanium dioxide nucleus crystals. Subsequently, a titanium compound, an alkali metal compound, and an oxyphosphorus compound are further added and heated/burned in the presence of the grown titanium dioxide nucleus crystals. Thus, titanium dioxide is produced which comprises columnar particles having a weight-average major-axis length of 7.0-15.0 µm and in which particles having a major-axis length of 10 µm or longer account for 15 wt.% or more of all the particles. A solution of a tin compound and a solution of compounds of antimony, phosphorus, etc. are added to a suspension obtained by suspending the titanium dioxide. The particles are sedimented. Subsequently, the product obtained is heated/burned to produce a conductive titanium oxide which comprises the titanium dioxide and a conductive coating film formed on the surface thereof.

Claims (23)

1. Titanium dioxide in the shape of columnar particles having a weight-average major-axis length of 7.0-15.0 µm and including particles having a major-axis length of 10 µm or larger in a proportion of 15% by weight or more.
2. Titanium dioxide according to claim 1, wherein the particles having a major-axis length of smaller than 5.0 µm are included in a proportion of 40%
by weight or less.
3. Titanium dioxide according to claim 1, wherein the weight-average minor-axis length of the particles is in the range of 0.25-1.0 µm.
4. Titanium oxide in the shape of columnar particles having a weight-average major-axis length of 7.0-15.0 µm and including particles having a major-axis length of 10 µm or larger in a proportion of 15% by weight or more and having a composition represented by TiO x (in the formula, Ti denotes a titanium atom, O
denotes an oxygen atom, and x can be a real number in the range of 1~x<=2) or TiN y O z (in the formula, Ti denotes a titanium atom, N denotes a nitrogen atom, O
denotes an oxygen atom, and y denotes a ratio of nitrogen atom to titanium atom, z denotes a ratio of oxygen atom to titanium atom, and y and z each can be a real number in the range of more than 0 and less than 2).
5. Titanium oxide according to claim 4, wherein the particles having a major-axis length of smaller than 5.0 µm are included in a proportion of 40% by weight or less.
6. Titanium oxide according to claim 4, wherein the weight-average minor-axis length of the particles is in the range of 0.25-1.0 µm.
7. Electro-conductive titanium oxide in the shape of columnar particles having a weight-average major-axis length of 7.0-15.0 µm and including particles having a major-axis length of 10 µm or larger in a proportion of 15% by weight or more, and havirig an electro-conductive coating on the surface of the particles.
8. Electro-conductive titanium oxide according to claim 7, wherein the particles having a major-axis length of smaller than 5.0 um are included in a proportion of 40% by weight or less.
9. Electro-conductive titanium oxide according to claim 7, wherein the weight-average minor-axis length of the particles is in the range of 0.25-1.0 µm.
10. Electro-conductive titanium oxide according to claim 7, wherein the electro-conductive coating contains tin oxide in which at least one element selected from antimony, phosphorus, tungsten, fluorine, niobium and tantalum is dissolved in solid state or tin oxide in which none of these elements is dissolved in solid state.
11. Electro-conductive titanium oxide according to claim 7, wherein the electro-conductive coating contains at least one member selected from metallic material, electro-conductive polymer and electro-conductive carbon.
12. A process for producing titanium dioxide which comprises heating and firing a titanium compound, an alkali metal compound and an oxyphosphorus compound in the presence of titanium dioxide nucleus crystals having an aspect ratio of 2 or higher and a weight-average major-axis length of 3.0-7.0 µm, thereby producing titanium dioxide in the shape of columnar particles having a weight-average major-axis length of 7.0-15.0 µm and including particles having a major-axis length of 10 µm or larger in a proportion of 15% by weight or more.
13. A process for producing titanium dioxide which comprises producing titanium dioxide in the shape of columnar particles through the first step of heating and firing a titanium compound, an alkali metal compound and an oxyphosphorus compound in the presence of titanium dioxide nucleus crystals having an aspect ratio of 2 or higher, thereby growing titanium dioxide nucleus crystals, and the second step of further adding a titanium compound, an alkali metal compound and an oxyphosphorus compound and heating and firing them in the presence of the grown titanium dioxide nucleus crystals.
14. A process for producing titanium dioxide according to claim 13, wherein at the first step, the titanium dioxide nucleus crystals are grown so that the ratio of weight-average major-axis length of the titanium dioxide nucleus crystals after growing to that of the titanium dioxide nucleus crystals reaches 3-7, and at the next second step, the titanium dioxide nucleus crystals are grown so that the ratio of weight-average major-axis length of the produced titanium dioxide to that of the titanium dioxide nucleus crystals reaches 2-5.
15. A process for producing titanium dioxide according to claim 13, wherein the weight-average major-axis length of the titanium dioxide nucleus crystals used at the first step is 1-4 µm, and that of the titanium dioxide nucleus crystals used at the second step is 3-7 µm.
16. A process for producing titanium dioxide according to claim 13, wherein the titanium dioxide nucleus crystals used at the first step are produced by heating and firing a titanium compound, an alkali metal compound and an oxyphosphorus compound.
17. A process for producing titanium dioxide, wherein the step of growing titanium dioxide nucleus crystals by heating and firing a titanium compound, an alkali metal compound and an oxyphosphorus compound in the presence of titanium dioxide nucleus crystals having an aspect ratio of 2 or higher is repeated twice or more to grow titanium dioxide nucleus crystals.
18. A process for producing titanium dioxide according to claim 17, wherein the titanium dioxide nucleus crystals are grown so that the ratio of weight-average major-axis length of the titanium dioxide nucleus crystals after growing to that of the titanium dioxide nucleus crystals used at each growing step reaches 1.2-7.
19. A process for producing titanium oxide which comprises heating and firing the titanium dioxide described in any one of claims 1-3 in the presence of a reducing compound or a nitrogen-containing compound, thereby producing titanium oxide in the shape of columnar particles having a composition represented by TiO x (in the formula, Ti denotes a titanium atom, O
denotes an oxygen atom, and x can be a real number in the range of 1 .ltorsim. × < 2) or TiN y O z (in the formula, Ti denotes a titanium atom, N denotes a nitrogen atom, O
denotes an oxygen atom, and y denotes a ratio of nitrogen atom to titanium atom, z denotes a ratio of oxygen atom to titanium atom, and y and z each can be a real number in the range of more than 0 and less than 2).
20. A process for producing electro-conductive titanium oxide which comprises forming an electro-conductive coating on the surface of the particles of the titanium dioxide described in any one of claims 1-3, thereby producing electro-conductive titanium oxide in the shape of columnar particles.
21. A process for producing electro-conductive titanium oxide according to claim 20, wherein a solution containing a tin compound or a solution containing a tin compound and a solution containing a compound of at least one element selected from antimony, phosphorus, tungsten, fluorine, niobium and tantalum are added to a suspension of the titanium dioxide described in any one of claims 1-3, to result in precipitation, and then the resulting product is heated and fired to form an electro-conductive coating containing a tin oxide in which at least one element selected from antimony, phosphorus, tungsten, fluorine, niobium and tantalum is dissolved in solid state or a tin oxide in which none of these elements is dissolved in solid state.
22. A process for producing electro-conductive titanium oxide according to claim 20, wherein a metallic compound and a reducing compound are added to a suspension of the titanium dioxide described in any one of claims 1-3 to reduce the metallic compound, thereby forming an electro-conductive coating containing a metallic material.
23. A process for producing electro-conductive titanium oxide according to claim 20, wherein an electro-conductive polymer or an electro-conductive carbon is synthesized in the presence of the titanium dioxide described in any one of claims 1-3, thereby to form an electro-conductive coating containing the electro-conductive polymer or the electro-conductive carbon.
CA2643369A 2006-03-07 2007-03-06 Titanium oxide, conductive titanium oxide, and processes for producing these Active CA2643369C (en)

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EP (1) EP1995216B1 (en)
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