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(12) United States Patent (10) Patent No.: US 8,053,479 B2 Masuda Et Al

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(12) United States Patent (10) Patent No.: US 8,053,479 B2 Masuda Et Al USO08053479B2 (12) United States Patent (10) Patent No.: US 8,053,479 B2 Masuda et al. (45) Date of Patent: Nov. 8, 2011 (54) SILICA SOL AND METHOD FOR FOREIGN PATENT DOCUMENTS PRODUCING THE SAME JP 37-996.1 8, 1962 JP 62270414 11, 1987 (75) Inventors: Norio Masuda, Kashiwa (JP); Shinsuke JP 2009708 1, 1990 Ota, Fukuchiyama (JP) JP 9100110 4f1997 JP 92O8213 8, 1997 JP 2004315300 11, 2004 (73) Assignee: Fuso Chemical Co. Ltd., Osaka (JP) JP 2004315300 A * 11, 2004 JP 2004315343 11, 2004 (*) Notice: Subject to any disclaimer, the term of this JP 2005030219 3, 2005 patent is extended or adjusted under 35 U.S.C. 154(b) by 222 days. OTHER PUBLICATIONS (21) Appl. No.: 11/993,206 PCT International Search Report for Fuso Chemical Co., Ltd., Inter national App'l No. PCT/JP2007/064607, Jul 25, 2007, Dated Oct. (22) PCT Filed: Jul. 25, 2007 30, 2007. PCT Written Opinion of the International Searching Authority, Inter (86). PCT No.: PCT/UP2007/064607 national App'l No. PCT/JP2007/064607, Jul 25, 2007, Dated Oct. S371 (c)(1), 30, 2007. (2), (4) Date: Jan. 17, 2008 * cited by examiner (87) PCT Pub. No.: WO2008/015943 PCT Pub. Date: Feb. 7, 2008 Primary Examiner — Ling Choi Assistant Examiner — Chun-Cheng Wang (65) Prior Publication Data (74) Attorney, Agent, or Firm — Law Offices of Albert US 2009/O143490 A1 Jun. 4, 2009 Wai-Kit Chan, PLLC (30) Foreign Application Priority Data (57) ABSTRACT Jul. 31, 2006 (JP) ................................. 2006-20922O This invention provides a high-purity, high-concentrated (51) Int. Cl. silica sol with long-term stability and low viscosity by pre COIB 33/4I (2006.01) venting viscosity-increase after production, and method for BOIF 3/12 (2006.01) producing the same. In one embodiment, the silica Sol pro (52) U.S. Cl. ............................................ 516/34:516786 duced by an alkoxide method comprises at least a dispersing (58) Field of Classification Search ..................... 516/34 agent and silica, wherein the concentration of said dispersing See application file for complete search history. agent is 10-3000 ppm with respect to the silica, wherein said dispersing agent may be an inorganic acid, inorganic acid salt, (56) References Cited organic acid or organic acid salt whose degradation tempera U.S. PATENT DOCUMENTS ture and boiling point are both 60° C. or higher, wherein said 2,630,410 A * 3/1953 Clapsadle et al. .............. 516.86 silica Sol has a silica concentration of 20% weight or higher. 3,012,973 A 12/1961 Atkins et al. 5,902,226 A * 5/1999 Tasaki et al. .................... 516/34 2003/0115806 A1 6, 2003 Takami et al. 14 Claims, 1 Drawing Sheet US 8,053,479 B2 1. 2 SLCA SOLAND METHOD FOR dispersing agent. Moreover, the Viscosity of the silica Sol PRODUCING THE SAME cannot be maintained at a constant level because the dispers ing agent is degraded or vaporized during long-term storage. CROSS-REFERENCE TO RELATED Thus, the Viscosity is increased and the gelation is induced APPLICATIONS with time. To solve the above problems, a silica Sol containing metals This application is the National Stage of International at a very low concentration has recently been produced. How Application No. PCT/JP2007/064607, filed Jul. 31, 2007, ever, the silica concentration is about 15 weight%. A produc which claims priority of Japanese Patent Application No. tion of the 15 weight% or lower silica sol has problems such 2006-209220 filed on Jul. 31, 2006. The entire disclosures of 10 as low production efficiency and low compounding flexibility the preceding applications are incorporated by reference of the polishing agent. It is also inappropriate with regard to herein in their entirety. transport and storage. FIELD OF THE INVENTION There is another problem regarding the production of a 15 silica sol with small silica particles. The silica sol with small This invention is related to a silica sol and a method for silica particles is likely to aggregate and induce the gelation of producing the same. Specifically, this invention is related to a Solution, compared to a silica Sol with large silica particles. In highly-concentrated, low-viscosity and high-purity silica Sol consequence, the Viscosity easily increases, which makes the with long-term stability, which is useful as a polishing mate production of the highly-concentrated silica Sol with Small rial for silicon wafers and in the CMP process of semicon silica particles difficult. ductor devices, and producing methods of the silica Sol with The silica Sol with a high concentration, low viscosity and high production efficiency by concentrating the silica Sol high purity in spite of any silica particle size differences is during the production processes. strongly desired, but no silica Sol satisfying these conditions has been produced. DESCRIPTION OF THE BACKGROUND ART 25 In view of the above problems, this invention aims at pro viding a high-purity and highly-concentrated silica Sol with With a recent development of semiconductor techniques, long-term stability and low viscosity by preventing the vis there is a demand for a high-purity silica Sol containing very cosity-increase during storage after the production, and meth few metal impurities for the silicon wafer polishing and in the ods for producing the same. This invention also aims at pro CMP process of semiconductor devices because it does not 30 viding a high-purity and highly-concentrated silica Sol which contaminate materials such as silicon wafers. does not undergo the Viscosity-increase or the gelation in The production of the silica sol containing silica at a high spite of any silica particle size differences in a silica solby concentration, i.e., a highly-concentrated silica Sol, is pre adding a dispersing agent at a specific concentration to a ferred because it not only raises the production efficiency but reaction or a solvent-substitution-concentrated-solution and also increases the storage/transport efficiency. Further, it is 35 production methods thereof. preferred because it freely enables to control the compound ing of polishing agents, i.e., it increases compounding flex SUMMARY OF THE INVENTION ibility. Thus, various reports regarding the highly-concen trated silica sol have been made. In one embodiment, the inventors found that a high-purity Regarding the use of a silica Sol in the silicon wafer pol 40 and highly-concentrated silica Sol with long-term stability ishing, it is a problem that a recycled silica Sol shows a and low viscosity may be produced by using a dispersing Viscosity-increase which interferes with its efficacy as a pol agent consisting of one or more compounds with both degra ishing agent. Accordingly, a silica Sol showing long-term dation temperature and boiling point of 60° C. or higher stability and low-viscosity, even after recycling, is desired. selected from inorganic acid, inorganic acid salt, organic acid A silica Sol with Small silica particles is particularly used 45 and organic acid salt. The dispersing agent may be added to for the final polishing of 300 mm wafers, and it increases the the high-purity silica Sol prepared by the concentration and flatness without causing damage (scratch-free). This silica Sol Solvent Substitution of a reaction solution produced by an is also used as a polishing agent in the CMP process for LSI alkoxide method, in which alkoxysilane is hydrolyzed and provided with remarkably-miniaturized elements. The silica condensation-polymerized, and thereby developed this Sol with Small silica particles has high precision capable of 50 invention. polishing materials required to be scratch-free flat and micro One embodiment of the present invention is related to a structural. Thus, the highly-concentrated silica Sol with Small silica Sol produced by analkoxide method, wherein said silica silica particles is needed. Sol comprises at least a dispersing agent and silica, wherein For example, Patent application Tokukoushou No. said dispersing agent concentration is 10-3000 ppm with 37-996.1 (publication) discloses a method to prepare a 30% or 55 respect to the silica, wherein said dispersing agent consists of higher concentrated-silica Sol by adding monovalent cation one or more compounds selected from inorganic acid, inor soluble metal salts (alkali metal salt) as a dispersing agent. ganic acid salt, organic acid and organic acid salt whose This method produces the highly-concentrated silica Sol degradation temperature and boiling point are both 60° C. or while maintaining a low viscosity. According to this method, higher, wherein said silica Sol has a silica concentration of 20 the silica Sol contains alkali metal salt-derived metal impuri 60 weight% or higher. ties so that a high-purity silica Sol cannot be produced. Another embodiment of the present invention is related to Another method using ammonium salts containing lower the silica Sol, wherein said silica Sol has a metal impurity alkyl as a dispersing agent is also disclosed in the same concentration of 1 ppm or lower. document, which produces a silica Sol containing no metal Yet another embodiment of the present invention is related impurities. However, the ammonium salt is degraded in a 65 to the silica Sol, wherein said silica has a primary particle size heating process because its degradation temperature is low. of 20 nm or Smaller, wherein said dispersing agent concen This results in inadequate efficacy of ammonium salt as a tration is 10-1350 ppm with respect to the silica. US 8,053,479 B2 3 4 Yet another embodiment of the present invention is related both equal to or higher than the maximum temperature of the to a producing method of a silica Sol comprising: (1) Reaction Solution concentrated in said process (3) and/or the concen process comprising hydrolyzing and condensation-polymer trated Solution under solvent Substitution in said process (4).
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