The present invention addresses the problem of providing a method for reducing impurities, e.g., aluminum, on element level in silicon oxide. The method for producing silicon oxide according to the present invention comprises a water treatment step, a reduced-pressure heating step and a sublimation step. In the water treatment step, silicon is brought into contact with water, and the resultant product is dried to produce water-treated silicon. In the reduced-pressure heating step, the water-treated silicon (a) is heated together with silicon dioxide (b1) and a mixture (b3) of a metal silicate (b2) or a metal oxide (b3) and silicon oxide under a reduced pressure to generate a gas. In the sublimation step, the gas is sublimated to produce a solid material.
In a method for continuously generating silicon monoxide (SiO) gas, wherein a silicon monoxide gas-generating raw material in a raw material supply unit is continuously charged into a reaction chamber RM, an inert gas is flowed through the raw material supply unit so as to be directed toward the charging direction of the silicon monoxide gas-generating raw material. The method for continuously generating silicon monoxide gas prevents a decrease in yield of the silicon monoxide (SiO) gas-generating raw material.
An object of the present invention is to provide a silicon monoxide gas generating raw material in which a reaction that generates a silicon monoxide (SiO) gas is hardly inhibited. The silicon monoxide gas generating raw material according to the present invention has a water content of 0.6 wt % or less.
Active metal particles in which the surface layer is hardly oxidized and a method for producing the active metal particles is provided. In the method for modifying the surface of active metal particles, heat is generated by moving active metal powder in a fluid, and the surface layer of the active metal particles is reacted with an arbitrary component in the fluid by the heat to modify the surface layer. Preferably, moving the active metal powder draws a substantially circular orbit while vibrating. A vibrating mill is preferably used when making such movement with respect to the active metal powder. Then, the powder obtained by the surface modification has a nitrogen-containing coating as a surface layer with a thickness more than 1 nm and less than or equal to 6 nm. The powder has a fluidity in the range of 25 seconds/50 g or more and 45 seconds/50 g or less.
An object of the present invention is to provide active material particles excellent in ion uptake ability. The silicon-based active material particles according to the present invention comprise a layer structure. Here, the “silicon-based active material particles” are, for example, active material particles for forming a negative electrode of a lithium ion secondary battery. Examples of the active material particles for forming the negative electrode of the lithium ion secondary battery include so-called Si-based active materials such as silicon (Si), silicon oxide (SiOx), metal element-containing silicon oxide containing alkaline metal elements such as lithium (Li) and alkaline earth metal elements such as magnesium (Mg), silicon alloys. The thickness of the layer in the active material particles is preferably 1 μm or less. Here, the thickness of the layer is preferably 0.01 μm or more.
An object of the present invention is to provide active material particles excellent in ion uptake ability. The silicon-based active material particles according to the present invention comprise a layer structure. Here, the “silicon-based active material particles” are, for example, active material particles for forming a negative electrode of a lithium ion secondary battery. Examples of the active material particles for forming the negative electrode of the lithium ion secondary battery include so-called Si-based active materials such as silicon (Si), silicon oxide (SiOx), metal element-containing silicon oxide containing alkaline metal elements such as lithium (Li) and alkaline earth metal elements such as magnesium (Mg), silicon alloys. The thickness of the layer in the active material particles is preferably 1 μm or less. Here, the thickness of the layer is preferably 0.01 μm or more.
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/58 - Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFySelection of substances as active materials, active masses, active liquids of polyanionic structures, e.g. phosphates, silicates or borates
H01M 4/1391 - Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/02 - Electrodes composed of, or comprising, active material
8.
SILICON MONOXIDE GAS GENERATING MATERIAL AND SILICON MONOXIDE GAS CONTINUOUS GENERATION METHOD
The present invention addresses the problem of providing a silicon monoxide gas generating material with which the reaction for generating silicon monoxide (SiO) gas is unlikely to be inhibited. The silicon monoxide gas generating material according to the present invention has a water content of 0.6 wt% or less.
xx), a metal element-containing silicon oxide which contains an alkali metal element such as lithium (Li) or an alkali earth metal element such as magnesium (Mg), and a silicon alloy. In addition, the layer thickness in the active material particles is preferably no greater than 1μm. Also, said layer thickness is preferably at least 0.01μm.
The present invention addresses the problem of providing active metal particles, the surface layer of which is unlikely to undergo oxidation, and a method for producing the same. This active metal particle surface modification method according to the present invention involves generating heat by moving an active metal powder in a fluid, and modifying the surface layer of the active metal particles by reacting said surface layer with an arbitrary component in the fluid by using heat. Said movement is preferably a motion which involves vibrating while moving in a substantially circular trajectory. A vibrating mill is preferably used when moving the active metal powder. As the surface layer thereof, the titanium powder or titanium alloy powder obtained by the surface modification method has a nitrogen-containing film having a thickness within the range of more than 1nm and no more than 6nm. The powder has a fluidity of 25 seconds/50g to 45 seconds/50g, inclusive.
B22F 1/00 - Metallic powderTreatment of metallic powder, e.g. to facilitate working or to improve properties
B22F 1/02 - Special treatment of metallic powder, e.g. to facilitate working, to improve properties; Metallic powders per se, e.g. mixtures of particles of different composition comprising coating of the powder
[Problem to be solved] To produce an SiO powder having a rounded spherical particulate shape and a small particle diameter; and further having a low degree of impurity contamination, efficiently and economically.
2 as an SiO gas generation raw material 9 is loaded into a crucible 2. The mixture in the crucible 2 is heated under a reduced pressure so as to generate SiO gas. The generated SiO gas is accumulated on a deposition base 5 rotating on the crucible 2. When SiO deposit 10 accumulated on the deposition base 5 is scraped off with a blade 7, a tip of the blade 7 is separated from a surface of the deposition base 5, and in a state in which a portion of the SiO deposit 10 accumulated on the deposition base 5 is left on the deposition base 5, the remaining SiO deposit 10 is scraped off by the blade 7 and collected as an SiO powder 11.
C01B 33/18 - Preparation of finely divided silica neither in sol nor in gel formAfter-treatment thereof
C23C 16/01 - Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. on substrates subsequently removed by etching
The present invention addresses the problem of providing a titanium alloy powder production method whereby the yield of titanium alloy powder is improved while allowing the environmental burden to be reduced. The titanium alloy powder production method according to the present invention comprises a first melting step, an ingot producing step, a second melting step, and a powdering step. In the first melting step, a molded body obtained by compressing a mixed powder containing a titanium powder and a powder of a metal element other than titanium is melted to prepare a first molten metal. In the ingot producing step, the first molten metal is injected into a mold, and the first molten metal solidifies to produce an ingot. In the second melting step, the ingot is melted in an inert gas atmosphere to prepare a second molten metal. In the powdering step, the second molten metal is powdered by a gas atomizing device.
B22F 1/00 - Metallic powderTreatment of metallic powder, e.g. to facilitate working or to improve properties
B22F 9/08 - Making metallic powder or suspensions thereofApparatus or devices specially adapted therefor using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
H01M 4/58 - Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFySelection of substances as active materials, active masses, active liquids of polyanionic structures, e.g. phosphates, silicates or borates
H01M 4/62 - Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
H01M 10/0525 - Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodesLithium-ion batteries
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/1391 - Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/02 - Electrodes composed of, or comprising, active material
14.
SiO POWDER PRODUCTION METHOD, AND SPHERICAL PARTICULATE SiO POWDER
22 is charged in a crucible 2. The mixture in the crucible 2 is heated under a reduced pressure to generate a SiO gas. The generated SiO gas is deposited on a deposition base 5 that is rotating on the crucible 2. In the scraping off of a SiO deposit 10 deposited on the deposition base 5 with a blade 7, the tip of the blade 7 is kept away from the surface of the deposition base 5, a portion of the SiO deposit 10 deposited on the deposition base 5 is left on the deposition base 5 and simultaneously the remainder of the SiO deposit 10 is scraped off with the blade 7 and is collected as a SiO powder 11.
H01B 1/04 - Conductors or conductive bodies characterised by the conductive materialsSelection of materials as conductors mainly consisting of carbon-silicon compounds, carbon, or silicon
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/58 - Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFySelection of substances as active materials, active masses, active liquids of polyanionic structures, e.g. phosphates, silicates or borates
17.
Lithium doped silicon oxide-based negative electrode material and method of manufacturing the same
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 10/0525 - Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodesLithium-ion batteries
H01M 4/38 - Selection of substances as active materials, active masses, active liquids of elements or alloys
H01M 10/04 - Construction or manufacture in general
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
19.
Li-containing silicon oxide powder and production method thereof
H01B 1/04 - Conductors or conductive bodies characterised by the conductive materialsSelection of materials as conductors mainly consisting of carbon-silicon compounds, carbon, or silicon
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
[Problem] To provide a silicon oxide negative electrode material capable of avoiding as quickly as possible a drop in battery performance caused by the non-uniform distribution of the Li concentration. [Solution] In this invention, a powder with the average composition represented by SiLixOy satisfies 0.05 < x < y < 1.2, and 1 μm or larger for the average particle diameter. Furthermore, when ten of the powder particles are pulled out randomly to measure in each of the particles the Li concentration L1 at a depth position of 50 nm from the outermost surface thereof, and the Li concentration L2 at a depth position of 400 nm from the outermost surface thereof, L1/L2 satisfies 0.8 < L1/L2 < 1.2 in any of the particles, and the standard deviation for L2 is 0.1 or less.
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
C01B 33/027 - Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
C01B 33/12 - SilicaHydrates thereof, e.g. lepidoic silicic acid
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/38 - Selection of substances as active materials, active masses, active liquids of elements or alloys
The present invention relates to a Li-containing SiOx powder (0.5 < x < 1.5) used in a negative electrode of a lithium secondary battery. On a powder particle cross section in a visual field of 1 μm in four directions containing a particle surface and having a definition of 50 pixels × 50 pixels or greater, EELS measurements are performed, and in so doing, the spectral intensities in the Li-K edge domain and the Si-L edge domain are determined. Among the integrated intensities over one row of a particle outermost surface in the visual field, the integrated intensity for the Li-K edge domain is ILi(s), the integrated intensity for the Si-L edge domain is ISi(s), and ILi(s)/(ILi(s) + ISi(s)) is the outermost surface Li intensity ratio R(s). Among the integrated intensities over one row of a near-surface 500 nm away inward from the particle outermost surface in the visual field, the integrated intensity for the Li-K edge domain is ILi(i), the integrated intensity for the Si-L edge domain is ISi(i), and ILi(i)/(ILi(i) + ISi(i)) is the near-surface Li intensity ratio R(i). Then, the Li-containing silicon oxide powder satisfies R(s)/R(i) < 1.
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
Provided is a method for producing a Li-containing silicon oxide powder that comprises crystallized lithium silicate, that is mostly water-insoluble Li2Si2O5, and that comprises little crystalline Si. To this end, a powdered lithium source is finely ground when mixing the powdered lithium source and a low-grade silicon oxide powder represented by the compositional formula SiOx (0.5 < x < 1.5). The median diameter D1 of the low-grade silicon oxide powder and the median diameter D2 of the powdered lithium source satisfy 0.05 ≤ D2/D1 ≤ 2. The mixed powder is fired at 300-800 °C.
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
Provided is a powder for the negative electrode of a lithium ion secondary cell, the powder including a silicon oxide powder containing Li. The average composition of the powder overall satisfies the relationships 0.5 < x < 1.5 and 0.1 < y/x < 0.8 when the molar ratio of Li, Si, and O is y:1:x. The volume median diameter of the powder for the negative electrode is within a range of 0.5 to 30 µm. When X-ray diffraction measurement of the powder is performed using CuKα rays, the relationships P2/P1 ≤ 1.0 and P3/P1 ≤ 1.0 are satisfied if P1 is the height of the peak attributed to Li2SiO3, P2 is the height of the peak attributed to crystalline Si, and P3 is the height of the peak attributed to Li4SiO4. When the powder is used in the negative electrode of a lithium ion secondary cell, the initial efficiency and capacity retention rate of a long-term cycle can be increased.
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
27.
POWDER FOR NEGATIVE ELECTRODES OF LITHIUM ION SECONDARY BATTERIES
A powder for negative electrodes of lithium ion secondary batteries, which is obtained by mixing a silicon powder coated with carbon, a silicon oxide powder doped with lithium and coated with carbon, and a graphite powder. If α (mass%) is the content ratio of the silicon powder coated with carbon, β (mass%) is the content ratio of the silicon oxide powder doped with lithium and coated with carbon, γ (mass%) is the content ratio of the graphite powder, X = (α + β)/(α + β + γ) × 100 and Y = α/β × 100, this powder satisfies all of the following relational expressions X < 50, 1 ≤ Y ≤ 10 and -9 × X + 19 ≤ Y ≤ -9/10 × X + 37. This powder for negative electrodes is able to provide good battery characteristics even if a negative electrode is produced using a slurry that contains water, an aqueous binder and a thickening agent.
This powder for negative electrode material in a lithium ion secondary cell contains a silicon oxide powder having a carbon coating, has as a whole an average composition, expressed as a molar ratio, of Si:O=1:x (0.5 ≦ x ≦ 1.5), has a volume median diameter D50 fulfilling the relation 0.5μm ≦ D50 ≦ 10μm, and has an angle of repose of 40-50°. When used as the negative electrode material in a lithium ion secondary cell, this powder can improve cycle characteristics of the cell. In this powder for a negative electrode material, the ratio of carbon in the makeup of the aforementioned carbon coating is preferably 0.5-7.0 mass%.
A lithium-containing silicon oxide powder which is used as a negative electrode material for lithium ion secondary batteries. At least some of the particles that constitute this lithium-containing silicon oxide powder are coated with carbon. This powder is characterized in that, with respect to peaks assigned to Si in the diffraction angle (2θ) range from 47.1° to 47.7° in an X-ray diffraction measurement using a CuKα ray, the peak height (P1) before the lithium-containing silicon oxide powder is mixed with water and the peak height (P2) after the lithium-containing silicon oxide powder is mixed with water and dried satisfy P2/P1 ≥ 0.42. This lithium-containing silicon oxide powder is suppressed in reactivity with water.
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
30.
LITHIUM-ION SECONDARY BATTERY NEGATIVE ELECTRODE MATERIAL POWDER, LITHIUM-ION SECONDARY BATTERY NEGATIVE ELECTRODE AND CAPACITOR ELECTRODE EMPLOYING SAME, AND LITHIUM-ION SECONDARY BATTERY AND CAPACITOR
Provided is a lithium-ion secondary battery negative electrode material powder formed from SiOx (where 0.4 ≤ x ≤ 1.2) powder with a conductive carbon film on the surface thereof, and which satisfies the formula 1.5 ≤ B/A ≤ 100. Herein, A is the specific surface area of the lithium-ion secondary battery negative electrode material powder calculated using a particle size distribution under the assumption that the particles therein are spherical bodies; B is the specific surface area of the lithium-ion secondary battery negative electrode material powder which is measured with a one-point method by the BET method; and A is represented by the following equation: A= Σ{ni*(4π(di/2)2)}/[ρ*Σ{ni*(4π(di/2)3/3)}]. Herein, di is the particle diameter of the lithium-ion secondary battery negative electrode material powder; ni is the number of particles in the particle size distribution with a particle diameter in a range of di-di+1; and ρ is the true density (2.2g/cm3) of SiO. Using this negative electrode material powder allows obtaining a lithium-ion secondary battery with large discharge capacitance, good cycling characteristics, and which is capable of withstanding use at a practical level.
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
31.
POWDER FOR LITHIUM ION SECONDARY BATTERY NEGATIVE ELECTRODE MATERIAL, LITHIUM ION SECONDARY BATTERY NEGATIVE ELECTRODE USING SAME, AND LITHIUM ION SECONDARY BATTERY
A powder for a lithium ion secondary battery negative electrode material, characterized in that: the powder comprises SiOx (0.4≤x≤1.2); and, in the spectrum measured by silicon-29 nuclear magnetic resonance, the ratio of the peak index assignable to zerovalent Si to the peak index assignable to tetravalent Si is 0.65 to 0.80, while the peak top assignable to tetravalent Si is present within a range of -110 to -105ppm. This powder for a negative electrode material makes it possible to produce a lithium ion secondary battery which has a high charge/discharge capacity and excellent cycle characteristics.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/38 - Selection of substances as active materials, active masses, active liquids of elements or alloys
32.
Negative electrode material powder for lithium ion secondary battery, negative electrode for lithium ion secondary battery, negative electrode for capacitor, lithium ion secondary battery, and capacitor
x and a value P2 of the strongest linear peak of Si (111) above the halo.
Accordingly, said powder can be used in the secondary battery with a large discharge capacity and a preferable cycle characteristics for practical use.
H01M 4/13 - Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulatorsProcesses of manufacture thereof
H01G 11/30 - Electrodes characterised by their material
H01G 9/042 - Electrodes characterised by the material
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01G 11/06 - Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
H01M 4/134 - Electrodes based on metals, Si or alloys
H01M 4/62 - Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
H01M 4/131 - Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
33.
POWDER FOR NEGATIVE-ELECTRODE MATERIAL OF LITHIUM-ION SECONDARY BATTERY, NEGATIVE-ELECTRODE OF LITHIUM-ION SECONDARY BATTERY AND NEGATIVE-ELECTRODE OF CAPACITOR USING SAME, LITHIUM-ION SECONDARY BATTERY, AND CAPACITOR
Powder for a negative-electrode material of a lithium-ion secondary battery, which has conductive carbon film formed on the surface of lower silicon-oxide powder, and which is characterized in satisfying a relationship of 0.01 ≤ Fa ≤ 0.4, wherein Fa is the average value of F of 10 particles, F is a coefficient of variation of the thickness of the carbon film and is defined as F = σ/ta, and ta is the average value and σ is the standard deviation of the thickness of the conductive carbon film measured at 24 points of a particle of the lower silicon-oxide powder. The proportion of the conductive carbon film is preferably a mass percent of 0.5% to 10%. The total content of tar constituent measured with a TPD-MS is preferably a mass ppm of 1 ppm to 3500 ppm, and the resistivity is preferably not more than 10,000 Ωcm. The maximum value (P1) of a halo due to SiOx derived by an XRD measurement, and a peak value (P2) of the strongest line of Si(111) preferably satisfy a relationship of P2/P1 < 0.01. With such a configuration, powder for a negative-electrode material to be used in a lithium-ion secondary battery that has large discharging capacity, good cycling characteristic, and that can withstand practical-level usage, is able to be provided.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01G 11/06 - Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
H01G 11/50 - Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
H01G 11/86 - Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
34.
POWDER FOR NEGATIVE POLE MATERIAL OF LITHIUM ION SECONDARY CELL, NEGATIVE POLE OF LITHIUM ION SECONDARY CELL USING SAME, AND LITHIUM ION SECONDARY CELL
Provided is a powder for a negative pole material of a lithium ion secondary cell, which is characterized by being formed from SiOx (0.4 < x < 1.2) and in that, in the spectrum determined by nuclear magnetic resonance spectroscopy with respect to the 1H that the powder inevitably contains, the peak surface area of a chemical shift of 0.2 to 0.4 ppm accounts for 5% to 40% of the peak total surface area. Preferably, in the spectrum determined by nuclear magnetic resonance spectroscopy with respect to 1H, the peak surface area of a chemical shift of 1.1 to 2.0 ppm accounts for 5% to 95% of the peak total surface area. As a result, the present invention can provide a powder for the negative pole material of a lithium ion secondary cell that is used in a lithium ion secondary cell having high discharge capacity, good initial efficiency and cycle properties.
C01B 15/14 - PeroxyhydratesPeroxyacids or salts thereof containing silicon
36.
POWDER FOR NEGATIVE ELECTRODE MATERIAL FOR LITHIUM ION SECONDARY BATTERY, NEGATIVE ELECTRODE OF LITHIUM ION SECONDARY BATTERY AND NEGATIVE ELECTRODE OF CAPACITOR RESPECTIVELY USING SAME, LITHIUM ION SECONDARY BATTERY AND CAPACITOR
Disclosed is a powder for negative electrode materials for lithium ion secondary batteries, which has a conductive carbon coating film on the surface of each lower silicon oxide particle, and wherein the particle size distribution of the silicon oxide particles satisfies 1 μm ≤ D50 ≤ 20 μm, with D50 and D10 satisfying 1.4 ≤ D50/D10 ≤ 2.4. It is preferable that: the thickness of the conductive carbon coating film is 1.5-7.5 nm (inclusive); the specific surface area as determined by a BET method is 0.3-7.0 m2/g (inclusive); and the ratio of the conductive coating film is 0.5-10% by mass (inclusive). It is also preferable that: the total content of tar components as determined by TPD-MS is 1-4,000 ppm by mass (inclusive); and the maximum value (P1) of an SiOx-derived halo and the strongest line peak value (P2) of Si(111) as determined by XRD satisfy P2/P1 < 0.01. Consequently, a powder for negative electrode materials to be used in lithium ion secondary batteries, which has high discharge capacity and good cycle characteristics and is capable of withstanding practical use, can be obtained.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
37.
POWDER FOR LITHIUM ION SECONDARY BATTERY NEGATIVE POLE MATERIAL, LITHIUM ION SECONDARY BATTERY NEGATIVE POLE AND CAPACITOR NEGATIVE POLE, AND LITHIUM ION SECONDARY BATTERY AND CAPACITOR
Provided is a lithium ion secondary battery negative pole material powder which comprises low-grade silicon oxide powder. A lithium ion secondary battery in which this powder is employed for the negative pole material has a charging potential of 0.45 to 1.0 V, based on Li, when initial charging is performed, and thereby has large discharging capacity and excellent cycle characteristics, making it possible to obtain a lithium ion secondary battery that can withstand practical levels of use. The significance of the fact that the charging potential at initial charging is 0.45 to 1.0 V, based on Li, is that a potential plateau produced by generation of Li silicate is observed, and that Li silicate is uniformly produced in the negative pole material. Since the negative pole material powder of the invention has a charging potential of 0.45 to 1.0 V, based on Li, at initial charging, excellent properties can be obtained in that the negative pole material can be finely crushed during charging/discharging and deterioration in the cycle characteristics can be suppressed. Preferably the powder for the negative pole material has a conductive carbon film on the surface thereof, and preferably the ratio taken up by this conductive carbon film is 0.2 to 10 mass%.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01G 11/24 - Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosityElectrodes characterised by the structural features of powders or particles used therefor
H01G 11/50 - Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
38.
Silicon oxide and negative electrode material for lithium-ion secondary battery
19 spins/g. A negative electrode material for the lithium-ion secondary battery contains not less than 20% by mass of this silicon oxide as a negative electrode active material.
H01M 4/485 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
H01M 4/134 - Electrodes based on metals, Si or alloys
H01M 10/0525 - Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodesLithium-ion batteries
39.
POWDER FOR NEGATIVE ELECTRODE MATERIAL OF LITHIUM-ION SECONDARY BATTERY, AS WELL AS NEGATIVE ELECTRODE OF LITHIUM-ION SECONDARY BATTERY, NEGATIVE ELECTRODE OF CAPACITOR, LITHIUM-ION SECONDARY BATTERY, AND CAPACITOR USING SAME
A powder for the negative electrode material of a lithium-ion secondary battery in which chlorine is added to the surface of lower silicon oxide powder, or a powder for the negative electrode material of a lithium-ion secondary battery in which a silicon-rich layer is formed on the surface of lower silicon oxide powder, and chlorine is added to the surface of the silicon-rich layer, wherein the powder for the negative electrode material of a lithium-ion secondary battery is characterized in that the concentration of surface chlorine is 0.1 mol% or greater. The powder for the negative electrode material preferably has a carbon film on the surface to which the chlorine is added. This makes it possible to provide a powder for a negative electrode material so that the powder has a large discharge capacity and good cycle characteristics, and can be used in lithium-ion secondary batteries capable of withstanding use at a practical level.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01G 11/42 - Powders or particles, e.g. composition thereof
H01G 11/50 - Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
40.
POWDER FOR NEGATIVE ELECTRODE MATERIAL OF LITHIUM ION SECONDARY BATTERY, NEGATIVE ELECTRODE FOR LITHIUM ION SECONDARY BATTERY AND NEGATIVE ELECTRODE FOR CAPACITOR USING SAME, AND LITHIUM ION SECONDARY BATTERY AND CAPACITOR
A powder for negative electrode material of a lithium ion secondary battery having a conductive carbon film on the surface of a lower order silicon oxide powder such that the total content for tar components measured by TPD-MS is 1 - 4000 ppm by mass, and in the Raman spectrum, there are peaks at 1350 cm-1 and 1580 cm-1, with the half width for the peak at 1580 cm-1 being 50 - 100 cm-1. The specific surface area measured by the BET method is preferably 0.3 - 40 m2/g, and the proportion of the conductive carbon film is preferably 0.2 - 10% by mass. The specific resistance of the lower order silicon oxide powder is preferably 40,000 Ωcm or less, and a maximum value P1 for the SiOx derived halo measured by XRD and a Si (111) maximum line peak value P2 that satisfy P2/P1 < 0.01 are preferable. Thus, a powder for a negative electrode material used in a lithium secondary battery that can withstand use at a practical level and has a large discharge capacity and excellent cycling characteristics can be provided.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01G 11/06 - Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
H01G 11/26 - Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
H01G 11/50 - Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
H01M 4/587 - Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
41.
POWDER FOR LITHIUM ION SECONDARY BATTERY NEGATIVE ELECTRODE MATERIAL, LITHIUM ION SECONDARY BATTERY NEGATIVE ELECTRODE AND CAPACITOR NEGATIVE ELECTRODE, AND LITHIUM ION SECONDARY BATTERY AND CAPACITOR
A powder for a lithium ion secondary battery negative electrode material, which comprises a lower silicon oxide powder and an electrically conductive carbon film formed on the surface of the powder, and which is characterized in that the specific surface area is more than 0.3 m2/g and not more than 40 m2/g as measured by a BET method, and no peak of SiC appears or a half width of a peak of SiC is 2° or more at 2θ = 35.6°±0.1° as measured by XRD using a CuKα ray. It is preferred that the content of the electrically conductive carbon film in the powder for a lithium ion secondary battery negative electrode material is 0.2 to 2.5 mass% inclusive. It is also preferred that the lower silicon oxide powder has a specific resistivity of 100000 Ωcm or less and the maximum value (P1) of a halo derived from SiOx as measured by XRD measurement and the strongest line peak value (P2) of Si (111) fulfill the requirement represented by the formula: P2/P1 < 0.01. In this manner, it is possible to provide a powder for a negative electrode material for use in a lithium ion secondary battery, which has large discharge capacity and good cycle properties and can be used in use applications at practical level.
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
H01G 11/06 - Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
H01G 11/30 - Electrodes characterised by their material
H01M 4/36 - Selection of substances as active materials, active masses, active liquids
42.
POWDER FOR LITHIUM ION SECONDARY BATTERY NEGATIVE ELECTRODE MATERIAL, LITHIUM ION SECONDARY BATTERY NEGATIVE ELECTRODE, CAPACITOR NEGATIVE ELECTRODE, LITHIUM ION SECONDARY BATTERY, AND CAPACITOR
Disclosed is a powder for a negative electrode material which can be used for a lithium ion secondary battery having high discharge capacity and good cycle properties, and capable of application at a practical level. Specifically disclosed is a powder for a lithium ion secondary battery negative electrode material, which comprises a lower silicon oxide powder and an electrically conductive carbon coating film formed on the surface of the powder, and which is characterized in that the content of Si (that is contained in SiC) is 15.1 wt% or less, or that A3 is 15.1 or less (A3 ≤ 15.1) (wherein A1 (wt%) represents the Si content as measured by an acid dissolution method; A2 (wt%) represents the Si content as measured by an alkali dissolution method; and A3 = A2-A1) and the specific resistance is 30000 Ωcm or less. It is preferred that the lower silicon oxide powder fulfills the requirement represented by the formula: P2/P1 < 0.01 (wherein P1 represents the maximum value of a SiOx-derived halo that appears at 2θ=10°-30° and P2 represents the value of a strongest intensity peak of Si(111) that appears at 2θ = 28.4 ± 0.3° as measured by XRD using CuKα beam). It is also preferred that the content of a tar component is 1 to 4000 ppm inclusive.
Disclosed are a powder for the negative electrode material of a lithium-ion rechargeable battery having a silicon-rich layer on the surface of a low-grade silicon oxide powder, and a powder for the negative electrode material of a lithium-ion rechargeable battery comprising a silicon oxide powder. The powder for the negative electrode material of a lithium-ion rechargeable battery is characterized in that c/d <1, where c is the value of the molar ratio of oxygen to silicon on the surface of the silicon oxide powder, and d is the value of the molar ratio of the total oxygen to silicon. Preferably, c < 1 and/or 0.8 < d < 1.0. In addition, preferably: the surface of the powder does not contain crystalline silicon; the inside of the powder is amorphous; and there is a conductive carbon film on the surface. The surface of the powder for the negative electrode material of a lithium-ion rechargeable battery is coated with silicon using disproportionation of SiClx (X <4). A powder for the negative electrode material of a lithium-ion rechargeable battery, which can be used in a lithium-ion rechargeable battery having a large reversible capacity and a small irreversible capacity, and a method of producing a powder for the negative electrode material of a lithium-ion rechargeable battery can thus be provided.
Disclosed is a negative electrode active material for a lithium ion secondary battery, which is characterized by comprising an SiOx having an A1/A2 ratio of 0.1 or less wherein A1 represents the intensity of a peak A1 that is derived from a silanol group and appears around 3400 to 3800 cm-1 and A2 represents the intensity of a peak A2 that is derived from a siloxane bond and appears around 1000 to 1200 cm-1 in spectra measured by means of a Fourier transform infrared spectrometer after a vacuum pumping treatment of the SiOx at 200˚C. Preferably, the variable x in the SiOx is smaller than 1, a peak A3 derived from an Si-H bond and appearing around 2100 cm-1 in the spectra measured by means of a laser raman spectrometer does not exist, and the Y/X ratio is 0.98 or less wherein X represents the molar ratio of O to Si in the SiOx and Y represents the molar ratio of O to Si in an area located adjacent to the surface of the SiOx. When the active material is used, a lithium ion secondary battery having high initial efficiency and a high charge-discharge capacity can be produced.
Disclosed is an SiOx which generates an H2O gas in an amount of 680 ppm or less as detected in a temperature range from 200 to 800°C in a thermally evolved gas analysis. In the SiOx, it is preferred that the amount of the H2O gas generated be 420 ppm or less. It is also preferred that the peak intensity (P1) which is a peak intensity at an Si peak point appearing around 2θ = 28° and the base intensity (P2) which is an intensity appearing at a peak point that is assumed based on an average gradient as determined in a backward and a forward of the aforementioned peak point in a graph produced by X-ray diffraction meet the requirement represented by the following formula: (P1-P2)/P2 ≤ 0.2. When the SiOx is used as a deposition material, a deposited film that does not undergo the occurrence of splashing during the formation of the film and has excellent gas barrier performance can be produced. When the SiOx is used as a negative electrode active material for a lithium ion secondary battery, the initial efficiency of the lithium ion secondary battery can be maintained at a high level.
B65D 81/24 - Adaptations for preventing deterioration or decay of contentsApplications to the container or packaging material of food preservatives, fungicides, pesticides or animal repellants
H01M 4/48 - Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
46.
SILICON OXIDE, AND NEGATIVE ELECTRODE MATERIAL FOR LITHIUM ION SECONDARY BATTERY
Disclosed is a powdery silicon oxide which can be used as a negative electrode active material for a lithium ion secondary battery and is represented by the following chemical formula: SiOx. In the powdery silicon oxide, the particle diameter (D90) at a 90% cumulative frequency in a particle size cumulative distribution curve is 31 μm or smaller and the content of a micropowder having a particle diameter of 1 μm or smaller is 5 mass% or less. The powdery silicon oxide can be used as a negative electrode active material for a lithium ion secondary battery having excellent initial efficiency and cycle properties. In the powdery silicon oxide, it is preferred to adjust the value x so as to fall within the range of 0.7 < x < 1.3 and adjust the molar ratio of oxygen to silicon (i.e., O/Si) on the particle surfaces to 0.6 to 1.8. It is more preferred that the ratio of D90 and D10 (i.e., D90/D10) is 6 or less, wherein each of D90 and D10 is a particle diameter at a X% cumulative frequency in a particle size cumulative distribution curve of the silicon oxide.
Disclosed is a powder silicon oxide used in the active anode material of a lithium ion secondary cell and represented by SiOx, that is characterized in that when the silicon oxide is measured using an X-ray diffraction device equipped with an enclosed light source as the light source and a high-speed detector as the detector, a halo is detected at 20° ≦ 2θ ≦ 40°, a peak is detected at the maximum line position of quartz, and the height of the aforementioned halo (P1) and the height of the aforementioned quart maximum line position peak (P2) fulfill P2/P1 ≦ 0.05. By using the silicon oxide as the active anode material, a lithium ion secondary cell provided with stable initial efficiency and cycle characteristics can be obtained. The x in the aforementioned SiOx is preferably 0.7 < x < 1.5. Additionally, the anode material for the lithium ion secondary cell comprises at least 20 mass% of the silicon oxide as the active anode material.
Provided is a silicon oxide used in a negative-electrode active material for a lithium-ion secondary battery. Said silicon oxide is characterized by a g-value of at least 2.0020 and no more than 2.0050, measured by an ESR spectrometer, and is further characterized in that A/B is at least 0.5 and C/B is no more than 2, where A, B, and C are the integrated intensities of peaks near 420 cm−1, 490 cm−1, and 520 cm−1 respectively, in a Raman spectrum measured by a Raman spectrometer. Using this silicon oxide as a negative-electrode active material allows a high-capacity lithium-ion secondary battery having excellent cycle characteristics and initial efficiency. The silicon oxide preferably has a spin density of at least 1 × 1017 spins/g and no more than 5 × 1019 spins/g. Also provided is a negative-electrode material for a lithium-ion secondary battery, said negative-electrode material containing at least 20% by mass of the silicon oxide as a negative-electrode active material.
A process for producing a titanium or titanium alloy ingot through consumable-electrode vacuum remelting. The process eliminates the uneven distribution of raw materials among compacts and in the individual compacts, to be used as a consumable electrode in the process, and thereby gives an ingot free from inhomogeneity. Titanium sponge particles and other particulate raw materials are charged, in respective amounts corresponding to one compact, into a mixing vessel (10) from hoppers (21a to 25a) via weighing devices (21b to 25b). The mixing vessel (10) into which the raw-material particles have been charged in an amount corresponding to one compact is biaxially rotated in a mixing part (30) with a mixer. The raw-material particles in the mixing vessel (10) are forcibly stirred efficiently to give a raw material mixture reduced in the uneven distribution of the raw materials.
Disclosed is a metal manufacturing method whereby the metal powder component is separated from a mixture of metal salt and metal powder, wherein the metal manufacturing method is capable of reducing the amount of energy required for manufacturing. A mixture (1) of metal salt and metal powder is supplied to the starting material input region (12) of a first hearth (10) which is partitioned by means of a skimmer (11). A plasma (19a) is used to perform heating to a temperature equal to or greater than the melting point of the metal salt and lower than the melting point of the metal powder, and this temperature is maintained, producing an upper layer (a molten salt (2) of molten metal salt) and a second, lower layer (a highly concentrated solid-liquid mixture (3) with an increased concentration of metal powder). Next, the upper layer, the molten salt (2), is discharged from a discharge port at the top of the first hearth while the lower layer, the highly concentrated solid-liquid mixture (3), is discharged from a lower layer discharge port (14). Next, the highly concentrated solid-liquid mixture (3) is heated to a temperature equal to or greater than the melting point of the metal powder and the temperature is maintained, and the metal powder within the highly concentrated solid-liquid mixture (3) is melted to produce molten metal, which forms an upper layer (molten salt (4)) and a lower layer (molten metal (5)). The molten metal (5) is separated from the molten salt (4), and the molten metal (5) is solidified into an ingot (6).
Provided are a fusing method in which metal powder is fused and separated from a mixture of metal salt and metal powder, and fusion apparatus which employs this method, wherein it is possible to use moving plasma having excellent energy efficiency. A lining part (15) comprising a second metal is inserted in such a way as to cover the side walls and upper edges of the side walls of a bath (10) comprising a first metal. Then the mixture (1) comprising metal salt and metal powder is introduced into a mixture introduction region (16) of the bath (10) which is partitioned by a skimmer (13) and, maintaining a state where the whole of the mixture (1) has been fused using the plasma (19a), two layers, namely an upper layer (fused salt (6)) where the metal salt has been fused) and a lower layer (fused metal (7)) are formed as a result of the difference in specific gravities. The formation of a fused salt layer which is an insulator by the solidification of the fused salt (6) on the inner surface of the bath (10) is prevented by maintaining the temperature of the portion of the lining part (15) in contact with the fused salt (6) above the melting point of the fused salt (6).
Disclosed is an SiO sintering and vapor depositing material that can significantly suppress the occurrence of splash and particles and can realize high strength and low cost. Also disclosed is a process for producing the same. To this end, a starting material powder of precipitated SiO is molded into a shape as a vapor depositing material. The molded product of SiO is sintered at a low temperature in an oxygen-containing atmosphere. The low-temperature sintered compact is sintered at a high temperature in a nonoxidizing atmosphere. Upon the low temperature sintering in an oxygen-containing atmosphere, the quantitative value for oxygen (O1) [= 100/(1 + 1/A1)] determined from a corrected value (A1) (= 1/K쮏A) for an O/Si ratio obtained by correcting a measured value (A) of the O/Si ratio as measured by EPMA with a correction coefficient (K), which is a ratio of an O/Si ratio (a) obtained by quantitatively analyzing a standard sample of SiO2 by EPMA to a theoretical value a0(nearly equal to 1.14), i.e., a/a0, is 44 to 49% of the value before the low temperature sintering. Raising the sintering temperature becomes possible by suppressing the adverse effect of the precipitated Si at the high temperature sintering, and, in this case, the compression breaking strength is increased to not less than 15 MPa and even to not less than 30 MPa.
C04B 35/14 - Shaped ceramic products characterised by their compositionCeramic compositionsProcessing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxides based on silica
Disclosed are a method and an apparatus for concentrating a Ti powder in a CaCl2-containing molten material, particularly in a CaCl2-containing molten material which contains a Ti granule (powder) produced by the Ca reduction of TiCl4. The Ti concentration in a CaCl2-containing molten material which has a Ti powder dispersed therein is increased by liquid cyclone. This method can be suitably applied to the concentration of a Ti powder in a CaCl2-containing molten material which contains a Ti powder produced by the Ca reduction of TiCl4. The liquid cyclone may be one having a trunk part (9) with a diameter (Dc) of 40 to 300 mm and a length (L) of 0.5 to 8 times the diameter. By using this type of liquid cyclone, the Ti concentration in a molten salt can be increased at a good collection rate. This concentration method can be achieved readily by using the concentration apparatus according to the invention.
A rotary wing type pump capable of handling high-temperature molten metals, especially, a rotary wing type pump capable of being used for transferring molten CaCl2 when metal Ti is produced by Ca reduction. The rotary wing pump is provided in the pump body with a plurality of molten metal discharging ports (9), and can handle high-temperature molten metal (12) at 650-1000 °C. Discharging pipes respectively connected with the plurality of discharging ports may be merged inside or outside a container (13) containing the above molten metal. When a mechanism, for maintaining air-tightness in the container while releasing stress due to thermal expansion force difference acting on discharging pipes in the container containing the above molten metal, is provided at a portion where the discharging pipes (11) penetrate through the flange (7) of the pump, thermal deformation of and damages to the discharging pipes can be effectively prevented. When this pump is used for transferring molten CaCl2 when metal Ti is produced by Ca reduction, Ti can be produced continuously and smoothly.
F04D 7/06 - Pumps adapted for handling specific fluids, e.g. by selection of specific materials for pumps or pump parts of centrifugal type the fluids being hot or corrosive, e.g. liquid metal
55.
PROCESS FOR PRODUCING METAL AND APPARATUS FOR PRODUCING METAL
This invention provides a process for producing a metal by an electrolytic process for alkali metals, alkaline earth metals or rare earth metals(particularly metallic Ca), and an apparatus for producing a metal which is used in practicing the process. Electrolysis is carried out while circulating an electrolytic bath on a cathode (11) side within an electrolysis tank (10). The metal can be taken out while continuing the electrolysis by introducing the electrolytic bath on the cathode side into a regulation tank (15) for regulating the concentration of the metal in the bath, taking out a metal (18) having a necessary concentration from the regulation tank (15), and then returning the electrolytic bath (20) to the electrolysis tank (10). Preferably, a flow-type electrolysis tank, which can conduct electrolysis while allowing the electrolytic bath to flow in a single direction near the surface of a cathode, is used. This process can be carried out by an electrolysis tank, a circulation passage (13) for circulating the electrolytic bath on the cathode side, and an apparatus for producing a metal according to this invention provided with a regulation tank.
In a powder-sintered-type SiO sintered body used for forming an evaporated film of silicon monoxide, evaporated residue is reduced, material strength durable for use is ensured, and the occurrence of splash is prevented. To achieve these objects, a mixed powder of small grain size powder and large grain size powder manufactured from separated SiO is used as a sintered material powder of the SiO sintered body. The mixed ratio of the small grain size powder to the material powder is set to 10 to 30 wt%. The sintering temperature is set to as low as 700 to 1,000 ˚C.
C04B 35/622 - Forming processesProcessing powders of inorganic compounds preparatory to the manufacturing of ceramic products
C04B 35/01 - Shaped ceramic products characterised by their compositionCeramic compositionsProcessing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxides
C23C 14/30 - Vacuum evaporation by wave energy or particle radiation by electron bombardment
01 - Chemical and biological materials for industrial, scientific and agricultural use
02 - Paints, varnishes, lacquers
06 - Common metals and ores; objects made of metal
07 - Machines and machine tools
09 - Scientific and electric apparatus and instruments
10 - Medical apparatus and instruments
11 - Environmental control apparatus
40 - Treatment of materials; recycling, air and water treatment,
42 - Scientific, technological and industrial services, research and design
Goods & Services
Industrial chemicals; metallic oxides for formation of
deposited films; metallic oxides for vapor deposition;
metallic oxides for sputtering target; silicon; silicon
oxides; silicon oxide powder; polycrystalline silicon;
polycrystalline silicon powder; polycrystalline silicon
rods; polycrystalline silicon chunks; titanium oxide;
titanium dioxide; titanium dioxide powder; photocatalysts;
photocatalyst solution; titanium-oxide-based coating
materials; titanium tetrachlorides; diluted titanium
tetrachloride; silicon tetrachloride; silicon monoxide;
trichlorosilane; magnesium chloride; sputtering target. Titanium-oxide-based paints; paints, varnishes, lacquers. Common metals and their alloys; irons and steels; nonferrous
metals and their alloys; titanium and its alloys; titanium
ores; titanium ingots; titanium alloy ingots; titanium
sponges; titanium powders; porous titanium; titanium alloy
powders; titanium hydride; hydrided titanium sponges;
titanium hydride powders; ferroalloy containing titanium;
ferroalloy powders containing titanium. Filters as parts of filtering machines and apparatus;
suction pads for use as parts of vacuum
gripping/clamping/handling systems; semiconductor
manufacturing machines and systems, and their parts and
fittings; loading-unloading machines and apparatus, and
their parts and fittings; plastic processing machines and
apparatus, and their parts and fittings. Electrodes, not for medical purposes; electrolysis
electrodes; fuel-cell electrodes. Medical apparatus and instruments; filters for medical
purposes; filters for hemofiltration; electrodes for medical
purposes. Filters for air conditioning and/or purifying apparatus and
installations; air-conditioning apparatus and installations;
air cooling and/or heating apparatus and installations; air
purifying apparatus and installations for industrial
purposes; filters for water purifying apparatus and devices;
water purifying apparatus and devices; household tap-water
filters; parts and fitting for all the aforementioned goods,
all included in this class. Processing of titanium and its alloys; melting of titanium
and its alloys; powder manufacturing process of titanium and
its alloys. Analysis of titanium and its alloys.
01 - Chemical and biological materials for industrial, scientific and agricultural use
02 - Paints, varnishes, lacquers
06 - Common metals and ores; objects made of metal
07 - Machines and machine tools
09 - Scientific and electric apparatus and instruments
10 - Medical apparatus and instruments
11 - Environmental control apparatus
40 - Treatment of materials; recycling, air and water treatment,
42 - Scientific, technological and industrial services, research and design
Goods & Services
Industrial chemicals; metallic oxides for formation of
deposited films; metallic oxides for vapor deposition;
metallic oxides for sputtering target; silicon; silicon
oxides; silicon oxide powder; polycrystalline silicon;
polycrystalline silicon powder; polycrystalline silicon
rods; polycrystalline silicon chunks; titanium oxide;
titanium dioxide; titanium dioxide powder; photocatalysts;
photocatalyst solution; titanium-oxide-based coating
materials; titanium tetrachlorides; diluted titanium
tetrachloride; silicon tetrachloride; silicon monoxide;
trichlorosilane; magnesium chloride; sputtering target. Titanium-oxide-based paints; paints, varnishes, lacquers. Common metals and their alloys; irons and steels; nonferrous
metals and their alloys; titanium and its alloys; titanium
ores; titanium ingots; titanium alloy ingots; titanium
sponges; titanium powders; porous titanium; titanium alloy
powders; titanium hydride; hydrided titanium sponges;
titanium hydride powders; ferroalloy containing titanium;
ferroalloy powders containing titanium. Filters as parts of filtering machines and apparatus;
suction pads for use as parts of vacuum
gripping/clamping/handling systems; semiconductor
manufacturing machines and systems, and their parts and
fittings; loading-unloading machines and apparatus, and
their parts and fittings; plastic processing machines and
apparatus, and their parts and fittings. Electrodes, not for medical purposes; electrolysis
electrodes; fuel-cell electrodes. Medical apparatus and instruments; filters for medical
purposes; filters for hemofiltration; electrodes for medical
purposes. Filters for air conditioning and/or purifying apparatus and
installations; air-conditioning apparatus and installations;
air cooling and/or heating apparatus and installations; air
purifying apparatus and installations for industrial
purposes; filters for water purifying apparatus and devices;
water purifying apparatus and devices; household tap-water
filters; parts and fitting for all the aforementioned goods,
all included in this class. Processing of titanium and its alloys; melting of titanium
and its alloys; powder manufacturing process of titanium and
its alloys. Analysis of titanium and its alloys.
59.
METHOD FOR PRODUCTION OF Ti GRANULE OR Ti ALLOY GRANULE, METHOD FOR PRODUCTION OF METAL Ti OR Ti ALLOY, AND PRODUCTION APPARATUS
Disclosed is a method for producing a Ti granule or a Ti alloy granule, which comprises the step of contacting Ti particles or Ti alloy particles produced by the reduction in a molten salt with one another to produce the Ti granule or Ti alloy granule. The method may further comprise the step of condensing the Ti granule or the Ti alloy granule in the molten salt that contains the Ti granule or the Ti alloy granule produced by the method. The method for producing a Ti granule or a Ti alloy granule in a molten salt may be applied to a step for separating the produced Ti granule or the Ti alloy granule from the molten salt in the process forthe production of metal Ti or a Ti alloy by Ca reduction. In this case, the productivity rate can be improved and it becomes possible to produce metal Ti or a Ti alloy at low cost.
B22F 9/20 - Making metallic powder or suspensions thereofApparatus or devices specially adapted therefor using chemical processes with reduction of metal compounds starting from solid metal compounds
C22B 5/04 - Dry processes by aluminium, other metals, or silicon
C22B 9/10 - General processes of refining or remelting of metalsApparatus for electroslag or arc remelting of metals with refining or fluxing agentsUse of materials therefor
A lighting equipment comprising a lamp capable of emitting full-spectrum light; and, disposed so as to surround the lamp, a translucent substratum provided with a photocatalyst reaction layer carrying a photocatalyst of titanium dioxide thin-film, or a translucent substratum provided with a photocatalyst reaction layer carrying a photocatalyst of titanium dioxide thin-film, this translucent substratum having an infrared ray absorbing capability, wherein between the lamp and the translucent substratum, there is provided a space allowing circulation of air, so that the air purification function by ultraviolet rays, lighting function by visible rays and heating function by infrared rays, namely, effective utilization according to the respective characteristics thereof can be attained to thereby reduce the wasting of photoenergy emitted from the lamp. Moreover, by not only heating by photoenergy emitted from the lamp but also the effect of heating by infrared rays emitted from the lamp, there is produced, in the air circulation space, forced convection leading to satisfactory air ventilation, thus promoting the action of air purification.
Disclosed is a method for producing a titanium porous sintered plate having high porosity and large area with high productivity. Specifically, a titanium secondary particle wherein titanium primary particles aggregate into a spherical shape is produced. Then, the spherical titanium secondary particles are mixed with a binder to form a slurry, and the slurry is processed into a plate-like molded body. The molded body is dried, then heated for removing the binder, and then sintered at high temperature.
A process for producing a spherical titanium alloy powder by gas atomization while economically diminishing differences in alloy composition among product particles differing in diameter. Sponge titanium particles are mixed with additive metallic-element particles with a mixer having a pulverizing function, such as a ball mill. The resultant particulate mixture is molded by compression into a rod-form raw material for melting. The molded rod-form raw material for melting is powdered by the gas atomization method. In the mixing step, the additive metallic-element particles are pulverized and, depending on the kind of the particles, are ground down. These metallic-element particles tenaciously adhere to the surface of the sponge titanium particles. Thus, uniform mixing is possible.
B22F 9/08 - Making metallic powder or suspensions thereofApparatus or devices specially adapted therefor using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
VISIBLE LIGHT RESPONSE-TYPE TITANIUM OXIDE PHOTOCATALYST, METHOD FOR MANUFACTURING THE VISIBLE LIGHT RESPONSE-TYPE TITANIUM OXIDE PHOTOCATALYST, AND USE OF THE VISIBLE LIGHT RESPONSE-TYPE TITANIUM OXIDE PHOTOCATALYST
This invention provides a visible light response-type titanium oxide photocatalyst that can develop high photocatalytic activity upon exposure to visible light. The visible light response-type titanium oxide photocatalyst is manufactured by heat treating titanium oxide and/or titanium hydroxide, produced by neutralizing an acidic titanium compound with a nitrogen-containing base, in an atmosphere containing a hydrolyzable metal compound (for example, titanium halide), and further conducting heat treatment in a gas having a water content of 0.5 to 4.0 vol% at a temperature of 350°C or above. In a mass fragment spectrum at an m/e value of 28 by a thermal desorption analysis, wherein m represents mass number and e represents ion charge number, the photocatalyst of the nitrogen-containing titanium oxide does not substantially have any peak at 600°C or above, and the peak having the smallest half-value width is in the range of 400 to 600°C. Further, for the photocatalyst, the nitrogen content calculated from a peak, which appears at 400 eV 됙 1.0 eV in an N1s shell bond energy spectrum by an XPS measurement, is at least 20 times larger than the nitrogen content determined by a chemical analysis.
A process for the production of Ti powder which comprises the step (a) of charging a mixture of a Ti material and a CaCl2-containing molten salt into a heater and melting the mixture by heating in an inert gas atmosphere, the step (b) of cooling the molten salt constituting the upper layer of the two-layer melt formed in the step (a), and the step (c) separating and recovering Ti powder contained in the cooled salt and which brings about a fine Ti powder of uniform size. Ti powder can be relatively easily recovered by conducting the step (b) by cooling the molten salt to the melting pointing of the salt or below and conducting the step (c) by dissolving the cooled salt in a solvent such as water or alcohol and collecting Ti powder. The separation and recovery of Ti powder can be carried out by any of centrifugal separation, filtration and sedimentation. When the process is applied to the separation and recovery of Ti from a Ti-containing molten salt which is formed by Ca reduction of TiCl4 and contains CaCl2, high-quality Ti powder can be efficiently obtained with small energy consumption.
B22F 9/06 - Making metallic powder or suspensions thereofApparatus or devices specially adapted therefor using physical processes starting from liquid material
65.
METHOD OF REMOVING/CONCENTRATING METAL-FOG-FORMING METAL PRESENT IN MOLTEN SALT, APPARATUS THEREFOR, AND PROCESS AND APPARATUS FOR PRODUCING Ti OR Ti ALLOY WITH THESE
A method by which a metal-fog-forming metal dissolved in a molten salt comprising a molten salt containing the metal-fog-forming metal can be removed and transferred to another molten salt to heighten the concentration thereof. The method can hence be utilized as a means of treating molten salts in various fields of the mining and manufacturing industries where molten salts containing a metal-fog-forming metal such as calcium or sodium are handled. In particular, when the method is utilized in producing titanium through calcium reduction, the calcium dissolved in a molten salt to be sent to an electrolytic cell can be rapidly removed (recovered) and the efficiency of calcium generation during the electrolysis of the molten salt can be heightened. Consequently, calcium generation and TiCl4 reduction in the electrolysis of a molten salt can be efficiently conducted and a stable operation on an industrial scale is possible. Thus, the method can be effectively utilized in producing titanium or a titanium alloy through calcium reduction.
01 - Chemical and biological materials for industrial, scientific and agricultural use
06 - Common metals and ores; objects made of metal
40 - Treatment of materials; recycling, air and water treatment,
Goods & Services
(1) Chemicals for use in the metallurgical industry; chemicals for use in the metal-working industry; chemicals for use in the electronics industry; metallic oxide plating compositions, namely, metallic oxides for formation of deposited films, metallic oxides for vapor deposition, metallic oxides for sputter deposition; silicon oxide granules; silicon oxide tablets; silicon oxide blocks; silicon oxide powder; polycrystalline silicon powder; polycrystalline silicon rods; polycrystalline silicon chunks; titanium oxide; titanium dioxide; titanium dioxide powder; photocatalysts, namely, catalysts that accelerate chemical reactions caused by exposure to light; photocatalyst solution, namely, catalyst solutions that accelerate chemical reactions caused by exposure to light; titanium-oxide-based photocatalytic coating materials; titanium tetrachlorides; diluted titanium tetrachloride; silicon tetrachloride; silicon monoxide; trichlorosilane; magnesium chloride; sputtering target; common metals and their alloys; iron and steels; nonferrous metals and their alloys; titanium and its alloys; titanium ores; titanium ingots; titanium alloy ingots; titanium sponges; titanium powders; porous titanium; titanium alloy powders; titanium hydride; hydrided titanium sponges; titanium hydride powders; ferroalloy containing titanium; ferroalloy powders containing titanium. (1) Processing of titanium and its alloys; melting of titanium and its alloys; powder manufacturing process of titanium and its alloys.
01 - Chemical and biological materials for industrial, scientific and agricultural use
06 - Common metals and ores; objects made of metal
40 - Treatment of materials; recycling, air and water treatment,
Goods & Services
(1) Chemicals for use in the metallurgical industry; chemicals for use in the metal-working industry; chemicals for use in the electronics industry; metallic oxide plating compositions, namely, metallic oxides for formation of deposited films, metallic oxides for vapor deposition, metallic oxides for sputter deposition; silicon oxide granules; silicon oxide tablets; silicon oxide blocks; silicon oxide powder; polycrystalline silicon powder; polycrystalline silicon rods; polycrystalline silicon chunks; titanium oxide; titanium dioxide; titanium dioxide powder; photocatalysts, namely, catalysts that accelerate chemical reactions caused by exposure to light; photocatalyst solution, namely, catalyst solutions that accelerate chemical reactions caused by exposure to light; titanium-oxide-based photocatalytic coating materials; titanium tetrachlorides; diluted titanium tetrachloride; silicon tetrachloride; silicon monoxide; trichlorosilane; magnesium chloride; sputtering target; common metals and their alloys; iron and steels; nonferrous metals and their alloys; titanium and its alloys; titanium ores; titanium ingots; titanium alloy ingots; titanium sponges; titanium powders; porous titanium; titanium alloy powders; titanium hydride; hydrided titanium sponges; titanium hydride powders; ferroalloy containing titanium; ferroalloy powders containing titanium. (1) Processing of titanium and its alloys; melting of titanium and its alloys; powder manufacturing process of titanium and its alloys.
01 - Chemical and biological materials for industrial, scientific and agricultural use
06 - Common metals and ores; objects made of metal
40 - Treatment of materials; recycling, air and water treatment,
Goods & Services
(1) Chemicals for use in the metallurgical industry; chemicals for use in the metal-working industry; chemicals for use in the electronics industry; metallic oxide plating compositions, namely, metallic oxides for formation of deposited films, metallic oxides for vapor deposition, metallic oxides for sputter deposition; silicon oxide granules; silicon oxide tablets; silicon oxide blocks; silicon oxide powder; polycrystalline silicon powder; polycrystalline silicon rods; polycrystalline silicon chunks; titanium oxide; titanium dioxide; titanium dioxide powder; photocatalysts, namely, catalysts that accelerate chemical reactions caused by exposure to light; photocatalyst solution, namely, catalyst solutions that accelerate chemical reactions caused by exposure to light; titanium-oxide-based photocatalytic coating materials; titanium tetrachlorides; diluted titanium tetrachloride; silicon tetrachloride; silicon monoxide; trichlorosilane; magnesium chloride; sputtering target; common metals and their alloys; iron and steels; nonferrous metals and their alloys; titanium and its alloys; titanium ores; titanium ingots; titanium alloy ingots; titanium sponges; titanium powders; porous titanium; titanium alloy powders; titanium hydride; hydrided titanium sponges; titanium hydride powders; ferroalloy containing titanium; ferroalloy powders containing titanium. (1) Processing of titanium and its alloys; melting of titanium and its alloys; powder manufacturing process of titanium and its alloys.
Generation of algae is prevented under underwater light receiving environment in the cooling tower, water purification tank, filter, and the like, of an air conditioner. In order to achieve the purpose, an antifouling object (2) immersed in the water (1) and receiving light on the surface serves as a first conductive member. A photocatalyst layer (3) is provided on the surface, i.e. the antifouling object surface. A second conductive member connected electrically with the conductive antifouling object (2) through an external circuit (4) is combined as a counter pole (5) and placed in the water (1). Algae prevention effect by the photocatalyst layer (3) is reinforced with no power supply through the use of the counter pole (5).
Hypochlorous acid is economically produced without supply of external electrical energy. Specifically, a photocell composed of a titanium oxide electrode (1) and a counter electrode (2) is placed in an electrolyte solution (3) containing a metal chloride. The titanium oxide electrode (1) is irradiated with light under a circumstance where oxygen can be supplied to the counter electrode (2) of the photocell in the electrolyte solution (3).
Disclosed is a method for economically forming a uniform titanium oxide film on the surface of a base. Specifically, an aqueous titanium tetrachloride solution having a Ti content of 0.1-17% by weight is applied over the surface of a heat-resistant base in a film form. The aqueous titanium tetrachloride solution in the liquid film form is then heated to a temperature not less than 300˚C, thereby volatilizing H2O and HCl in the liquid film and forming a titanium oxide film. In case where the base is composed of a material such as aluminum that is poor in acid resistance, an acid-resistant coating film such as an oxide film is formed in advance on the surface of the metal base.
A combination of primary warm forging by prismatic cogging with flat dies and secondary forging by cylindrical cogging with round dies is employed in order to produce a titanium material for sputtering which has a clean macro structure, a fine micro structure, less surface imperfection, and excellent upset forgeability by the use of a molten ingot as the starting material. In the primary forging, a satisfactory reduction is attained in the early stage of the warm forging, whereby the cast structure remaining in the surface layer of the sectional macro structure is destroyed, while in the secondary forging, the accumulation of work strain and the working into a shape similar to the final one are attained and working force is uniformly and regularly transmitted to the central part of a workpiece to make the crystal grains finer and uniform, which imparts regularity to the crystal orientation distribution and enables the material to exert excellent upset forgeability. By virtue of these characteristics, the titanium material is widely useful as a sputtering target.
A process for producing Ti, comprising the reduction step of providing a molten salt containing CaCl2 and having Ca dissolved therein and reacting TiCl4 with the Ca to thereby form Ti particles, the separation step of separating the Ti particles formed in the molten salt from the molten salt and the electrolysis step of electrolyzing the molten salt so as to increase the concentration of Ca, wherein the molten salt having the concentration of Ca increased in the electrolysis step is introduced in a regulation vessel to thereby render the Ca concentration of the molten salt constant and thereafter is used in the reduction ofTiCl4 in the reduction step. In this process, not only can any fluctuation of Ca concentration of molten salt charged in a reduction vessel be suppressed but also a high concentration thereof can be maintained. Further, continuous processing of a large volume of molten salt becomes feasible. Therefore, the reduction reaction of TiCl4 can be efficiently performed, and as a process for realization of Ti production on an industrial scale, the process can be effectively utilized in the production of Ti by Ca reduction.
This invention provides a method for the electrolysis of a molten salt that can enhance metal fog formation metal concentration of the molten salt. In the method, electrolysis is carried out in such a state that a molten metal containing a chloride of a metal fog forming metal is supplied from one end of an electrolytic cell to a part between an anode and a cathode in a continuous or intermittent manner to provide a flow rate in one direction to the molten salt in its part near the surface of the cathode and thus to allow the molten salt to flow in one direction at the part near the surface of the cathode. In the method, while high current efficiency is maintained, only a molten salt enriched with a metal fog forming metal such as Ca can be effectively taken out. Further, this method can easily be carried out by the electrolytic cell according to the present invention. Furthermore, the application of the method for the electrolysis of a molten salt to the production of Ti by Ca reduction can realize the production of metal Ti with high efficiency. Thus, the method for the electrolysis of a molten salt, the electrolytic cell, and the process for producing Ti can be effectively utilized by the production of Ti by Ca reduction.
International Manufacturing & Engineering Services Co., Ltd (Japan)
Inventor
Kido, Jyunji
Natsume, Yoshitake
Ogasawara, Tadashi
Azuma, Kazuomi
Mori, Koichi
Abstract
Disclosed is a sputtering target which enables to provide a sputtering film with high moisture barrier properties and high flexibility. This sputtering target also secures high film-forming rate while reducing damages to an object on which the film is formed during the sputtering. In order to realize such a sputtering target, a powder mixture containing, in a weight ratio, 20-80% of an SiO powder and the balance of TiO2 powder and/or a Ti powder is subjected to pressure sintering. The sintered body has a composition expressed as Si&agr;Ti&bgr;O (wherein &agr;, &bgr; and represent respective molar ratios of Si, Ti and O), and &agr;/&bgr; satisfies 0.45-7.25 while /(&agr; + &bgr;) satisfies 0.80-1.70.
H01L 51/50 - Solid state devices using organic materials as the active part, or using a combination of organic materials with other materials as the active part; Processes or apparatus specially adapted for the manufacture or treatment of such devices, or of parts thereof specially adapted for light emission, e.g. organic light emitting diodes (OLED) or polymer light emitting devices (PLED)
A silicon monoxide vapor deposition material resulting from powder sintering that is used in the production of silicon monoxide vapor-deposited film, which material is capable of inhibiting splashing. Further, the vapor deposition material ensures a strength capable of enduring uses. For realizing these, the vapor deposition material is prepared by sintering a raw material powder of deposited SiO at 700° to 1000°C. Si deposition during the sintering process is suppressed, and, in the measurement according to XRD, peak intensity P1 at Si peak point occurring around 2θ=28° and base intensity P2 at peak point assumed from an average intensity gradient in the vicinity of the peak point satisfy the relationship P1/P2≤3. Through screened employment of deposited SiO produced by a vacuum aggregation apparatus, the compression failure strength of the vapor deposition material after sintering is enhanced to 5 MPa or higher.
G09F 9/30 - Indicating arrangements for variable information in which the information is built-up on a support by selection or combination of individual elements in which the desired character or characters are formed by combining individual elements
