WO2003059816A1 - HIGHLY PURE ULTRA-FINE SiOX POWDER AND METHOD FOR PRODUCTION THEREOF - Google Patents
HIGHLY PURE ULTRA-FINE SiOX POWDER AND METHOD FOR PRODUCTION THEREOF Download PDFInfo
- Publication number
- WO2003059816A1 WO2003059816A1 PCT/JP2003/000158 JP0300158W WO03059816A1 WO 2003059816 A1 WO2003059816 A1 WO 2003059816A1 JP 0300158 W JP0300158 W JP 0300158W WO 03059816 A1 WO03059816 A1 WO 03059816A1
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- WIPO (PCT)
- Prior art keywords
- gas
- powder
- oxidizing gas
- monosilane
- amount
- Prior art date
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- 239000000843 powder Substances 0.000 title claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 229910052814 silicon oxide Inorganic materials 0.000 title claims abstract description 5
- 239000007789 gas Substances 0.000 claims abstract description 84
- 230000001590 oxidative effect Effects 0.000 claims abstract description 37
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000001301 oxygen Substances 0.000 claims abstract description 10
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 31
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- 230000004888 barrier function Effects 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 239000012785 packaging film Substances 0.000 claims description 6
- 229920006280 packaging film Polymers 0.000 claims description 6
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 5
- 230000003287 optical effect Effects 0.000 claims description 5
- 239000004065 semiconductor Substances 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 2
- PHEXXGCUKSJMBJ-UHFFFAOYSA-N [O].[SiH4] Chemical compound [O].[SiH4] PHEXXGCUKSJMBJ-UHFFFAOYSA-N 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract 1
- 239000012535 impurity Substances 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 229910001882 dioxygen Inorganic materials 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910001120 nichrome Inorganic materials 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- 238000007740 vapor deposition Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000003082 abrasive agent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3418—Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5409—Particle size related information expressed by specific surface values
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/54—Particle size related information
- C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
- C04B2235/5454—Particle size related information expressed by the size of the particles or aggregates thereof nanometer sized, i.e. below 100 nm
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/72—Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
- C04B2235/724—Halogenide content
Definitions
- the present invention relates to a high-purity ultra-fine S i Ox powder used for an interlayer insulating film of a semiconductor, a gas barrier film, a protective film of an optical component, and the like. It relates to the manufacturing method. Background art
- S i Ox powder is used as a deposition material for forming a deposition film of a S i O x film on food packaging films and optical components.
- it is used as a raw material for forming a gas barrier film composed of a SiOx film on a food packaging film in order to prevent the permeation of water vapor and oxygen gas to prevent food deterioration.
- a mixed raw material containing silica, metallic silicon, and / or carbon is subjected to high temperature treatment in a non-nitriding atmosphere of at least 8 ⁇ 10 4 Pa or more, and the SiO 2 containing gas is treated. to produce a method for cooling it 1000 / sec in the following cooling rate (JP 2001- 158613 JP), by heating the S i 0 2 powder in incomplete combustion flame to generate S i steam, A method of sub-oxidizing it (Japanese Patent Application Laid-Open No. 5-213606) and the like are known.
- oxidizing gas monosilane gas is oxygen, air, N0 2, A process according to C_ ⁇ 2 or H 2 0 (4) or (5).
- FIG 1 Schematic diagram of the reactor used in the examples of the present invention
- the use of monosilane gas as a raw material enables a low-temperature reaction, so that the contamination of impurities from furnace materials as in the conventional method can be reduced to the utmost. As a result, high purity and ultra-fine pulverization of the resulting SiO x powder can be achieved.
- a commercially available product can be used as the monosilane (SiH 4 ) gas.
- Monosilane gas is superior to silane-based gas such as trichlorosilane in that it does not contain chlorine.
- monosilane oxidizing gas hereinafter, simply referred to as. "Oxidizing gas" as an oxygen gas, in addition to the air, for example, N 0 2 with oxidizing respect monosilane, C 0 2, H 2 0 Etc. can be used.
- These oxidizing gases preferably have impurities removed to the utmost.
- the reaction between the monosilane gas and the oxidizing gas is performed at a temperature of 500 to 100 ° C. in a non-oxidizing gas atmosphere at a pressure of 10 to 100 kPa. If the pressure is less than 10 kPa, the generated Si ⁇ x film adheres to and grows on the wall of the reaction vessel, blocking the discharge part, making long-term operation difficult. On the other hand, when the pressure exceeds 100 kPa, large-scale equipment is required to increase the pressure resistance of the reaction apparatus, and impurities tend to increase.
- the preferred pressure is between 50 and 300 kPa.
- reaction temperatures are from 550 to 950, particularly preferably from 650 to 850C.
- the reaction time is preferably from 0.2 to 1 second.
- the reaction between the monosilane gas and the oxidizing gas is performed in the presence of a non-oxidizing gas.
- a non-oxidizing gas an inert gas such as argon or helium is optimal, but H 2 , N 2 , NH 3 , CO, etc. may be used as long as the reaction is not hindered.
- air the air contains a N 2 and 0 2, will be used both oxidizing gas and non-oxidizing gas.
- the amount of the non-oxidizing gas is preferably larger than the total amount of the monosilane gas and the amount of oxygen that contributes to the oxidation reaction of the oxidizing gas, and the molar ratio is 2 times or more, especially 10 times or more. It is preferred that Here, the amount of oxygen participates in the oxidation reaction of the oxidizing gas was example if it the air is the amount of oxygen contained therein, N0 2 and in the case of C0 2, its oxygen atom liberated from this an oxygen amount of one minute, in the case of H 2 0 Further, it is the oxygen content of the oxygen atoms fraction to configure.
- reaction vessel made of a high-purity material such as quartz glass.
- the shape may be a cup shape with a bottom, but a tubular shape is preferred, and the orientation may be either vertical installation or horizontal installation.
- heating method of the reaction vessel means such as a resistance heating heating element, high frequency heating, infrared radiation heating and the like can be used.
- the SiO x powder generated in the reaction vessel is discharged out of the system together with the non-oxidizing gas and by-product gas, and is recovered from a powder recovery device such as a bag filter.
- Siox powders having different X values in Siox are produced. If the X value of the SiO x powder of the present invention is out of the range of 0.6 to 1.8, the deposition rate is lowered, and it is necessary to increase the deposition temperature, which is not desirable. Preferred X values are 0.9 to 1.6.
- the X value is obtained by measuring the molar amount of Si in the SiO 2 powder in accordance with JIS-R 6124 (chemical analysis of silicon carbide abrasives), and measuring the molar amount of oxygen with an OZN simultaneous analyzer (for example, LECO "TC-136")) and can be calculated from their molar ratios.
- the specific surface area of the high-purity ultra-fine S i Ox powder of the present invention is 10 m 2 Zg or more. If the specific surface area is less than 10 m 2 Zg, the deposition start temperature will be low.
- the preferred specific surface area is at least 50 m 2 Zg, particularly preferably 55 to: L 00 m 2 / g.
- the total content of Na, Fe, A 1 and C 1 in the S i OX powder is 10 ppm or less. If the total content of Na, Fe, A1 and C1 exceeds 10 ppm, it causes insulation failure and corrosion when used as an interlayer insulating film or a negative electrode active material of a lithium ion battery.
- the total content is preferably 5 ppm or less, particularly preferably 3 ppm or less. These impurities can be measured by an emission spectrometry such as ICP.
- the Siox powder preferably has a weight average particle size of preferably 1 to 300 nm, particularly preferably 1 to 50 nm.
- the high-purity ultra-fine powder S i Ox powder of the present invention is used for interlayer insulating films of semiconductor devices, These are vapor deposition materials for forming gas barrier films for batteries, gas barrier films for food packaging films, and protective films for optical components.
- the reaction vessel 1 is heated so as to maintain a predetermined reaction temperature (see Table 1) by energizing a nichrome wire heater 2 having its outer periphery wound.
- the temperature was adjusted by measuring the temperature with a thermocouple installed at the center of the center of the reaction vessel and controlling the power of the nichrome wire heater.
- the pressure in the reaction vessel was set at 100 ⁇ 10 kPa, which was almost equal to that under the atmospheric pressure.
- the pressure reduction below the atmospheric pressure in the reaction vessel was performed by adjusting the opening of the valve while reducing the pressure with a vacuum pump provided on the discharge side.
- Pressurization exceeding atmospheric pressure was performed in a double structure by covering a stainless steel container on the outside of the reaction container. At this time, a fibrous heat insulating material is embedded between the nichrome wire heater and the stainless steel, and argon gas is introduced between the reaction vessel and the stainless steel vessel so that the pressure inside the reaction vessel becomes equal to that of the reaction vessel.
- the gas pressure inside and outside was balanced.
- the generated SiO x powder was discharged from the discharge pipe 5 together with the by-product gas and the argon gas, and recovered by a bag filter provided on the way.
- the X value, specific surface area, and impurities of the SiO x powder were measured. Table 1 shows the results.
- Comparative Example 3 In Comparative Example 3 in which the pressure in the reaction vessel was 5 kPa, only a small amount of the product could be recovered, and most of the product adhered to the outlet of the reaction vessel. Further, the color tone of the recovered product was white compared to the light brown or brown color obtained in the examples. On the other hand, in Comparative Example 4 in which the pressure in the reaction vessel was increased to 1200 kPa, the desired specific surface area and purity could not be obtained.
- Non-oxidizing gas ratio (argon gas amount) / (monosilane gas amount + oxygen gas amount)
- the high-purity ultra-fine Siox powder of the present invention can be used as a vapor deposition material for producing interlayer insulating films for semiconductors, plastic liquid crystal panels, gas barrier films for amorphous solar cells, gas barrier films for food packaging films, and the like. It can be used as a negative electrode active material of an ion battery. According to the production method of the present invention, the high-purity ultra-fine S i Ox powder can be easily produced.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Structural Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Silicon Compounds (AREA)
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU2003201860A AU2003201860A1 (en) | 2002-01-10 | 2003-01-10 | HIGHLY PURE ULTRA-FINE SiOX POWDER AND METHOD FOR PRODUCTION THEREOF |
EP03700523.8A EP1464621A4 (en) | 2002-01-10 | 2003-01-10 | ULTRA-FINE SB X / SB HIGH PURITY SIO POWDER AND PROCESS FOR PRODUCING THE SAME |
US10/500,737 US7585480B2 (en) | 2002-01-10 | 2003-01-10 | Highly pure ultra-fine SiOx powder and method for production thereof |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2002-3226 | 2002-01-10 | ||
JP2002003226A JP4044762B2 (ja) | 2002-01-10 | 2002-01-10 | 高純度・超微粉SiOx粉及びその製造方法 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2003059816A1 true WO2003059816A1 (en) | 2003-07-24 |
Family
ID=19190855
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2003/000158 WO2003059816A1 (en) | 2002-01-10 | 2003-01-10 | HIGHLY PURE ULTRA-FINE SiOX POWDER AND METHOD FOR PRODUCTION THEREOF |
Country Status (6)
Country | Link |
---|---|
US (1) | US7585480B2 (ja) |
EP (1) | EP1464621A4 (ja) |
JP (1) | JP4044762B2 (ja) |
CN (1) | CN1280190C (ja) |
AU (1) | AU2003201860A1 (ja) |
WO (1) | WO2003059816A1 (ja) |
Families Citing this family (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4044762B2 (ja) | 2002-01-10 | 2008-02-06 | 電気化学工業株式会社 | 高純度・超微粉SiOx粉及びその製造方法 |
JP5036161B2 (ja) * | 2005-10-14 | 2012-09-26 | パナソニック株式会社 | リチウムイオン二次電池用負極活物質、その製造方法、およびそれを用いたリチウムイオン二次電池 |
JP5221075B2 (ja) * | 2007-08-09 | 2013-06-26 | 国立大学法人電気通信大学 | 酸化膜形成方法、MOSデバイス製造方法、MOSトランジスタ製造方法、SiOx粉末、及びSiOx粉末製造方法 |
JP5374705B2 (ja) * | 2009-09-02 | 2013-12-25 | 株式会社大阪チタニウムテクノロジーズ | SiOxの製造方法 |
JP5618113B2 (ja) * | 2010-06-29 | 2014-11-05 | ユミコア | 低酸素含量のサブミクロンサイズのシリコン粉末 |
WO2012109028A1 (en) * | 2011-02-10 | 2012-08-16 | Temple University - Of The Commonwealth System Of Higher Education | Plastic-based cementitious materials |
CN103732536B (zh) * | 2011-07-29 | 2016-08-24 | 电气化学工业株式会社 | 球形硅石微粉末以及使用球形硅石微粉末的静电图像显影用调色剂外部添加剂 |
US10285874B2 (en) | 2014-03-06 | 2019-05-14 | The Procter & Gamble Company | Multi-component topsheets |
WO2015134371A1 (en) | 2014-03-06 | 2015-09-11 | The Procter & Gamble Company | Multi-component topsheets |
EP3113741B1 (en) | 2014-03-06 | 2020-04-22 | The Procter and Gamble Company | Three-dimensional substrates |
JP2015170542A (ja) * | 2014-03-10 | 2015-09-28 | 三洋電機株式会社 | 非水電解質二次電池 |
EP3340954B1 (en) | 2015-08-26 | 2020-03-25 | The Procter and Gamble Company | Absorbent articles having three-dimensional substrates and indicia |
EP3349278B1 (en) | 2015-09-10 | 2022-09-07 | Shin-Etsu Chemical Co., Ltd. | Method for producing negative electrode active material for nonaqueous electrolyte secondary batteries, method for manufacturing nonaqueous electrolyte secondary battery, method for producing negative electrode for nonaqueous electrolyte secondary batteries, and nonaqueous electrolyte secondary battery |
JP6759369B2 (ja) | 2016-07-01 | 2020-09-23 | ザ プロクター アンド ギャンブル カンパニーThe Procter & Gamble Company | 改善されたトップシート乾燥度を有する吸収性物品 |
CN111072038B (zh) | 2019-12-27 | 2021-01-01 | 江西壹金新能源科技有限公司 | 一种用于锂离子电池负极的改性一氧化硅材料及其制备方法 |
GB2605379A (en) * | 2021-03-29 | 2022-10-05 | Barton Blakeley Tech Limited | Reaction vessel |
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JP2001089125A (ja) * | 1999-09-28 | 2001-04-03 | Shinetsu Quartz Prod Co Ltd | 多孔質シリカ顆粒、その製造方法及び該多孔質シリカ顆粒を用いた合成石英ガラス粉の製造方法 |
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JP2868039B2 (ja) | 1992-01-31 | 1999-03-10 | 日亜化学工業株式会社 | 低級金属酸化物の製造方法 |
US6726990B1 (en) * | 1998-05-27 | 2004-04-27 | Nanogram Corporation | Silicon oxide particles |
JP4087029B2 (ja) | 1999-12-02 | 2008-05-14 | 電気化学工業株式会社 | 低級酸化ケイ素粉末及びその製造方法 |
JP3952118B2 (ja) * | 2000-02-04 | 2007-08-01 | 信越化学工業株式会社 | 活性なケイ素を含むケイ素酸化物及びその評価方法 |
WO2001086707A1 (fr) | 2000-05-08 | 2001-11-15 | Denki Kagaku Kogyo Kabushiki Kaisha | Film siox de faible permittivite relative, procede de production, dispositif semi-conducteur contenant ledit film |
JP2001348656A (ja) * | 2000-06-07 | 2001-12-18 | Denki Kagaku Kogyo Kk | SiOx多孔質成形体 |
JP2002260651A (ja) * | 2001-02-28 | 2002-09-13 | Shin Etsu Chem Co Ltd | 酸化珪素粉末及びその製造方法 |
US6896968B2 (en) * | 2001-04-06 | 2005-05-24 | Honeywell International Inc. | Coatings and method for protecting carbon-containing components from oxidation |
JP4044762B2 (ja) | 2002-01-10 | 2008-02-06 | 電気化学工業株式会社 | 高純度・超微粉SiOx粉及びその製造方法 |
-
2002
- 2002-01-10 JP JP2002003226A patent/JP4044762B2/ja not_active Expired - Fee Related
-
2003
- 2003-01-10 EP EP03700523.8A patent/EP1464621A4/en not_active Withdrawn
- 2003-01-10 US US10/500,737 patent/US7585480B2/en not_active Expired - Fee Related
- 2003-01-10 AU AU2003201860A patent/AU2003201860A1/en not_active Abandoned
- 2003-01-10 CN CNB038021099A patent/CN1280190C/zh not_active Expired - Fee Related
- 2003-01-10 WO PCT/JP2003/000158 patent/WO2003059816A1/ja active Application Filing
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2001089125A (ja) * | 1999-09-28 | 2001-04-03 | Shinetsu Quartz Prod Co Ltd | 多孔質シリカ顆粒、その製造方法及び該多孔質シリカ顆粒を用いた合成石英ガラス粉の製造方法 |
JP2001199716A (ja) * | 2000-01-11 | 2001-07-24 | Denki Kagaku Kogyo Kk | 低級酸化ケイ素粉末の製造方法 |
JP2001226112A (ja) * | 2000-02-15 | 2001-08-21 | Shin Etsu Chem Co Ltd | 高活性な酸化珪素粉末及び製造方法 |
Non-Patent Citations (1)
Title |
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See also references of EP1464621A4 * |
Also Published As
Publication number | Publication date |
---|---|
JP2003206126A (ja) | 2003-07-22 |
EP1464621A1 (en) | 2004-10-06 |
US20050084439A1 (en) | 2005-04-21 |
CN1615271A (zh) | 2005-05-11 |
AU2003201860A1 (en) | 2003-07-30 |
EP1464621A4 (en) | 2015-04-08 |
JP4044762B2 (ja) | 2008-02-06 |
US7585480B2 (en) | 2009-09-08 |
CN1280190C (zh) | 2006-10-18 |
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