# US 2016/0355671 A1 · Nanoparticle, method for producing nanoparticle, addition curing silicone resin composition, and semiconductor apparatus > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2016/0355671 A1 - Document ID: US20160355671A1 - Status: Published application - Kind: A1 - Application number: 15/146,102 - Filed: 2016-05-04 - Published: 2016-12-08 - Earliest claimed: 2015-06-05 - Assignees: Shin-Etsu Chemical Co., Ltd. - Applicants: Shin-Etsu Chemical Co., Ltd. - Inventors: Tomoyuki MIZUNASHI; Takayuki KUSUNOKI; Yuusuke TAKAMIZAWA - Web page: https://patentgrep.com/patent/US20160355671A1 ## CPC - C08K 9/06: with silicon-containing compounds - C08G 77/08: characterised by the catalysts used - C08G 77/70: {Siloxanes defined by use of the MDTQ nomenclature} - C08G 77/80: {Siloxanes having aromatic substituents, e.g. phenyl side groups} - C08K 3/36: Silica - C08L 83/04: Polysiloxanes - C09D 183/04: Polysiloxanes - H10H 20/854: characterised by their material, e.g. epoxy or silicone resins - H10W 74/473: {containing a filler} - H10W 74/476: {Organic materials comprising silicon} - C08G 77/12: containing silicon bound to hydrogen - C08G 77/20: containing silicon bound to unsaturated aliphatic groups - C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09) - C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS - C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06) - C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D) - H10H: INORGANIC LIGHT-EMITTING SEMICONDUCTOR DEVICES HAVING POTENTIAL BARRIERS - H10W: GENERIC PACKAGES, INTERCONNECTIONS, CONNECTORS OR OTHER CONSTRUCTIONAL DETAILS OF DEVICES COVERED BY CLASS H10 ## Abstract The present invention provides a nanoparticle of an inorganic oxide particle being surface-treated, wherein: a primary particle size of the nanoparticle measured by a dynamic light scattering method is 8 nm or more and 30 nm or less, and the inorganic oxide particle is surface-treated in such a way that alkoxy groups having 1 to 10 carbon atoms are contained in a range of 0.001 to 0.5 mol/100 g. The inventive nanoparticle, being added to a silicone resin composition, enables the cured product thereof to possess excellent mechanical properties, transparency, crack resistance, heat resistance, and gas barrier properties, and enables the composition to have low viscosity and good workability even after the addition of the nanoparticle. ## Claims ### Claim 1 A nanoparticle of an inorganic oxide particle being surface-treated, wherein: a primary particle size of the nanoparticle measured by a dynamic light scattering method is 8 nm or more and 30 nm or less, and the inorganic oxide particle is surface-treated in such a way that alkoxy groups having 1 to 10 carbon atoms are contained in a range of 0.001 to 0.5 mol/100 g. ### Claim 2 (depends on 1) The nanoparticle according to claim 1, wherein the inorganic oxide particle is any of silicon dioxide particle, zirconium oxide particle, titanium oxide particle, aluminum oxide particle, and zinc oxide particle. ### Claim 3 (depends on 1) The nanoparticle according to claim 1, wherein the nanoparticle contains a silicon atom-bonded hydrogen atom and/or at least one functional group selected from an alkyl group having 1 to 10 carbon atoms, a fluoroalkyl group having 1 to 10 carbon atoms in which at least one hydrogen atom of an alkyl group is substituted with a fluorine atom, an alkoxy group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms, an alkenyl group having 2 to 10 carbon atoms, a hydroxyl group, an epoxy group, and a (meth)acryl group. ### Claim 4 (depends on 2) The nanoparticle according to claim 2, wherein the nanoparticle contains a silicon atom-bonded hydrogen atom and/or at least one functional group selected from an alkyl group having 1 to 10 carbon atoms, a fluoroalkyl group having 1 to 10 carbon atoms in which at least one hydrogen atom of an alkyl group is substituted with a fluorine atom, an alkoxy group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms, an alkenyl group having 2 to 10 carbon atoms, a hydroxyl group, an epoxy group, and a (meth)acryl group. ### Claim 5 (depends on 1) An addition curing silicone resin composition, comprising organopolysiloxane having a silicon atom-bonded alkenyl group, an organosilicon compound having a silicon atom-bonded hydrogen atom, and an addition reaction catalyst, further comprising: the nanoparticle according to claim 1. ### Claim 6 (depends on 2) An addition curing silicone resin composition, comprising organopolysiloxane having a silicon atom-bonded alkenyl group, an organosilicon compound having a silicon atom-bonded hydrogen atom, and an addition reaction catalyst, further comprising: the nanoparticle according to claim 2. ### Claim 7 (depends on 3) An addition curing silicone resin composition, comprising organopolysiloxane having a silicon atom-bonded alkenyl group, an organosilicon compound having a silicon atom-bonded hydrogen atom, and an addition reaction catalyst, further comprising: the nanoparticle according to claim 3. ### Claim 8 (depends on 4) An addition curing silicone resin composition, comprising organopolysiloxane having a silicon atom-bonded alkenyl group, an organosilicon compound having a silicon atom-bonded hydrogen atom, and an addition reaction catalyst, further comprising: the nanoparticle according to claim 4. ### Claim 9 (depends on 5) The addition curing silicone resin composition according to claim 5, wherein the addition curing silicone resin composition contains: (A) a linear organopolysiloxane having two or more alkenyl groups in one molecule with a viscosity of 10 to 1,000,000 mPa·s at 25° C. measured by the method described in JIS K 7117-1:1999; (B) a branched organopolysiloxane comprising either or both of an SiO4/2 unit and an RSiO3/2 unit (“R” independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms), having two or more silicon atom-bonded alkenyl groups in one molecule, and having at least one group selected from a silicon atom-bonded alkoxy group having 1 to 10 carbon atoms and a silanol group in one molecule, and the total amount of the silicon atom-bonded alkoxy groups having 1 to 10 carbon atoms and the silanol groups in the component (B) is 0.01 to 0.6 mol/100 g, wherein the amount of the component (B) is 1 to 99% by mass relative to the total amount of the component (A) and the component (B); (C) an organosilicon compound having two or more silicon atom-bonded hydrogen atoms and at least one silicon atom-bonded aryl group in one molecule, wherein the amount is such that an amount of the silicon atom-bonded hydrogen atoms in the component (C) is 0.1 to 4.0 mol relative to 1 mol of the total amount of the alkenyl groups in the component (A) and the component (B); (D) a platinum group metal based catalyst, wherein the amount is a catalytic amount; and (E) the nanoparticle, wherein the amount is 1 to 99% by mass relative to the total amount of the composition. ### Claim 10 (depends on 6) The addition curing silicone resin composition according to claim 6, wherein the addition curing silicone resin composition contains: (A) a linear organopolysiloxane having two or more alkenyl groups in one molecule with a viscosity of 10 to 1,000,000 mPa·s at 25° C. measured by the method described in JIS K 7117-1:1999; (B) a branched organopolysiloxane comprising either or both of an SiO4/2 unit and an RSiO3/2 unit (“R” independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms), having two or more silicon atom-bonded alkenyl groups in one molecule, and having at least one group selected from a silicon atom-bonded alkoxy group having 1 to 10 carbon atoms and a silanol group in one molecule, and the total amount of the silicon atom-bonded alkoxy groups having 1 to 10 carbon atoms and the silanol groups in the component (B) is 0.01 to 0.6 mol/100 g, wherein the amount of the component (B) is 1 to 99% by mass relative to the total amount of the component (A) and the component (B); (C) an organosilicon compound having two or more silicon atom-bonded hydrogen atoms and at least one silicon atom-bonded aryl group in one molecule, wherein the amount is such that an amount of the silicon atom-bonded hydrogen atoms in the component (C) is 0.1 to 4.0 mol relative to 1 mol of the total amount of the alkenyl groups in the component (A) and the component (B); (D) a platinum group metal based catalyst, wherein the amount is a catalytic amount; and (E) the nanoparticle, wherein the amount is 1 to 99% by mass relative to the total amount of the composition. ### Claim 11 (depends on 7) The addition curing silicone resin composition according to claim 7, wherein the addition curing silicone resin composition contains: (A) a linear organopolysiloxane having two or more alkenyl groups in one molecule with a viscosity of 10 to 1,000,000 mPa·s at 25° C. measured by the method described in JIS K 7117-1:1999; (B) a branched organopolysiloxane comprising either or both of an SiO4/2 unit and an RSiO3/2 unit (“R” independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms), having two or more silicon atom-bonded alkenyl groups in one molecule, and having at least one group selected from a silicon atom-bonded alkoxy group having 1 to 10 carbon atoms and a silanol group in one molecule, and the total amount of the silicon atom-bonded alkoxy groups having 1 to 10 carbon atoms and the silanol groups in the component (B) is 0.01 to 0.6 mol/100 g, wherein the amount of the component (B) is 1 to 99% by mass relative to the total amount of the component (A) and the component (B); (C) an organosilicon compound having two or more silicon atom-bonded hydrogen atoms and at least one silicon atom-bonded aryl group in one molecule, wherein the amount is such that an amount of the silicon atom-bonded hydrogen atoms in the component (C) is 0.1 to 4.0 mol relative to 1 mol of the total amount of the alkenyl groups in the component (A) and the component (B); (D) a platinum group metal based catalyst, wherein the amount is a catalytic amount; and (E) the nanoparticle, wherein the amount is 1 to 99% by mass relative to the total amount of the composition. ### Claim 12 (depends on 8) The addition curing silicone resin composition according to claim 8, wherein the addition curing silicone resin composition contains: (A) a linear organopolysiloxane having two or more alkenyl groups in one molecule with a viscosity of 10 to 1,000,000 mPa·s at 25° C. measured by the method described in JIS K 7117-1:1999; (B) a branched organopolysiloxane comprising either or both of an SiO4/2 unit and an RSiO3/2 unit (“R” independently represents a monovalent hydrocarbon group having 1 to 10 carbon atoms), having two or more silicon atom-bonded alkenyl groups in one molecule, and having at least one group selected from a silicon atom-bonded alkoxy group having 1 to 10 carbon atoms and a silanol group in one molecule, and the total amount of the silicon atom-bonded alkoxy groups having 1 to 10 carbon atoms and the silanol groups in the component (B) is 0.01 to 0.6 mol/100 g, wherein the amount of the component (B) is 1 to 99% by mass relative to the total amount of the component (A) and the component (B); (C) an organosilicon compound having two or more silicon atom-bonded hydrogen atoms and at least one silicon atom-bonded aryl group in one molecule, wherein the amount is such that an amount of the silicon atom-bonded hydrogen atoms in the component (C) is 0.1 to 4.0 mol relative to 1 mol of the total amount of the alkenyl groups in the component (A) and the component (B); (D) a platinum group metal based catalyst, wherein the amount is a catalytic amount; and (E) the nanoparticle, wherein the amount is 1 to 99% by mass relative to the total amount of the composition. ### Claim 13 (depends on 9) The addition curing silicone resin composition according to claim 9, wherein 10 to 80% of the silicon atom-bonded groups contained in the addition curing silicone resin composition is an aryl group. ### Claim 14 (depends on 9) The addition curing silicone resin composition according to claim 9, wherein the addition curing silicone resin composition has a viscosity of 10 to 1,000,000 mPa·s at 25° C. measured by the method described in JIS K 7117-1:1999 when the component (E) is contained in an amount of 10% by mass relative to the total amount of the composition; and a viscosity ratio (x/y) is in a range of 0.5 to 3.0, where “x” is a viscosity of a composition X consisting of the components (A) to (E) at 25° C. measured by the method described in JIS K 7117-1:1999, “y” is a viscosity of a composition Y consisting of the components (A) to (D) contained in the composition X at 25° C. measured by the method described in JIS K 7117-1:1999. ### Claim 15 (depends on 5) The addition curing silicone resin composition according to claim 5, wherein the addition curing silicone resin composition further comprises (F) a fluorescent substance. ### Claim 16 (depends on 5) The addition curing silicone resin composition according to claim 5, wherein the addition curing silicone resin composition gives a cured product with a direct light transmittance of 70% or more at a wavelength of 450 nm when cured by heating to a thickness of 1 mm. ### Claim 17 (depends on 5) The addition curing silicone resin composition according to claim 5, wherein the addition curing silicone resin composition gives a cured product with a refractive index of 1.37 to 1.57 when cured by heating. ### Claim 18 (depends on 5) A semiconductor apparatus, wherein a semiconductor device is encapsulated by a cured product of the addition curing silicone resin composition according to claim 5. ### Claim 19 A method for producing a nanoparticle by surface-treatment of an inorganic oxide particle, wherein: reacting an inorganic oxide particle having a primary particle size of 3 nm or more and 30 nm or less measured by a dynamic light scattering method with a surface-treatment agent containing an alkoxy group having 1 to 10 carbon atoms at 20 to 150° C. for 1 to 72 hours to perform a surface-treatment of the inorganic oxide particle in such a way that the alkoxy groups having 1 to 10 carbon atoms are contained in a range of 0.001 to 0.5 mol/100 g.