# US 7,638,167 B2 · Controlled deposition of silicon-containing coatings adhered by an oxide layer > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 7,638,167 B2 - Document ID: US7638167B2 - Status: Granted - Kind: B2 - Application number: 10/862,047 - Filed: 2004-06-04 - Published: 2005-12-08 - Granted: 2009-12-29 - Earliest claimed: 2004-06-04 - Assignees: Applied Microstructures, Inc. - Inventors: Boris Kobrin; Romuald Nowak; Richard C. Yi; Jeffrey D. Chinn - Web page: https://patentgrep.com/patent/US7638167B2 ## CPC - C23C 16/402: {Silicon dioxide} - B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites - C23C 16/0227: {by cleaning or etching} - C23C: COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL (making metal-coated products by extrusion B21C23/22; covering with metal by connecting pre-existing layers to articles, see the relevant places, e.g. B21D39/00, B23K; metallising of glass C03C; metallising mortars, concrete, artificial stone, ceramics or natural stone C04B41/00; enamelling of, or applying a vitreous layer to, metals C23D; treating metal surfaces or coating of metals by electrolysis or electrophoresis C25D; single-crystal film growth C30B; by metallising textiles D06M11/83; decorating textiles by locally metallising D06Q1/04) - B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES ## Abstract We have developed an improved vapor-phase deposition method and apparatus for the application of films/coatings on substrates. The method provides for the addition of a precise amount of each of the reactants to be consumed in a single reaction step of the coating formation process. In addition to the control over the amount of reactants added to the process chamber, the present invention requires precise control over the total pressure (which is less than atmospheric pressure) in the process chamber, the partial vapor pressure of each vaporous component present in the process chamber, the substrate temperature, and typically the temperature of a major processing surface within said process chamber. Control over this combination of variables determines a number of the characteristics of a film/coating or multi-layered film/coating formed using the method. By varying these process parameters, the roughness and the thickness of the films/coatings produced can be controlled. ## Claims ### Claim 1 A method of controlling the hydrophobicity of a substrate surface by depositing an oxide upon said substrate surface, where said oxide is formed from at least one precursor in a manner which provides control over a density of hydroxyl groups on said oxide surface during deposition of said oxide onto the substrate surface, wherein said oxide is formed on said substrate surface in a process chamber operated at a pressure within the range of about 0.5 Torr to about 30 Torr, wherein said substrate surface temperature during deposition of said oxide ranges from about 15° C. and about 80° C., wherein a precise, specific quantity of each precursor material is charged to said process chamber in a batch-like manner by adding each precursor material into the process chamber in controlled aliquots, and wherein said oxide is formed by reacting a chlorosilane vaporous precursor having at least two chlorine atoms with a water precursor. ### Claim 2 (depends on 1) A method in accordance with claim 1, wherein said water precursor is in the form of water vapor. ### Claim 3 (depends on 1, 2) A method in accordance with claim 1 or claim 2, wherein said precursors react essentially on said substrate surface. ### Claim 4 (depends on 1) A method in accordance with claim 1, wherein a combination of a partial pressure of said chlorosilane vaporous precursor and a partial pressure of said water precursor is used to control said reaction between said chlorosilane precursor and said water precursor. ### Claim 5 (depends on 4) A method in accordance with claim 4, wherein said chlorosilane is selected from the group consisting of tetrachlorosilane, hexachlorosilane, hexachlorosiloxane and combinations thereof. ### Claim 6 (depends on 1) A method in accordance with claim 1, wherein a partial pressure of said chlorosilane vaporous precursor ranges from about 1 Torr to about 15 Torr. ### Claim 7 (depends on 1) A method in accordance with claim 1, wherein a temperature of a major processing surface inside said processing chamber ranges from about 20° C. to about 100° C. ### Claim 8 (depends on 2) A method in accordance with claim 2, wherein a partial pressure of said water vapor precursor ranges from about 0.5 Torr to about 20 Torr. ### Claim 9 (depends on 1) A method in accordance with claim 1, wherein, subsequent to the deposition of said oxide and the creation of hydroxyl groups on said oxide surface, a vaporous organo-chlorosilane which includes a specific functional group is reacted with said hydroxyl groups to impart specific functional characteristics to said coating. ### Claim 10 (depends on 9) A method in accordance with claim 9, wherein a partial pressure of said organo-chlorosilane vaporous precursor is used to control said reaction between said organo-chlorosilane precursor and said hydroxyl groups so that said reaction occurs substantially on said substrate surface. ### Claim 11 (depends on 10) A method in accordance with claim 10, wherein said reaction occurs essentially on said substrate surface. ### Claim 12 (depends on 9) A method in accordance with claim 9 wherein said organo-silane vaporous precursor includes a functional moiety selected from the group consisting of an alkyl group, an alkoxyl group, an alkyl substituted group containing fluorine, an alkoxyl substituted group containing fluorine, a vinyl group, an ethynyl group, an epoxy group, a glycoxy group, an acrylo group, a substituted group containing a silicon atom or an oxygen atom, and combinations thereof. ### Claim 13 (depends on 12) A method in accordance with claim 12, wherein a partial pressure of said organo-chlorosilane vaporous precursor ranges from about 0.1 Torr to about 10 Torr. ### Claim 14 (depends on 13) A method in accordance with claim 13, wherein said temperature of said major process surface ranges from about 20° C. to about 100° C.