# US 10,767,257 B2 · Method for removing a metal deposit arranged on a surface in a chamber > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 10,767,257 B2 - Document ID: US10767257B2 - Status: Granted - Kind: B2 - Application number: 16/070,491 - Filed: 2017-01-16 - Published: 2019-01-31 - Granted: 2020-09-08 - Earliest claimed: 2016-01-19 - Assignees: Plasma-Therm LLC - Applicants: Kobus SAS - Inventors: Julien Vitiello; Fabien Piallat - Web page: https://patentgrep.com/patent/US10767257B2 ## CPC - C23C 14/564: {Means for minimising impurities in the coating chamber such as dust, moisture, residual gases} - C07C 45/00: Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds - C23C 16/4405: {Cleaning of reactor or parts inside the reactor by using reactive gases} - C23F 1/12: Gaseous compositions - C23G 5/00: Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents - H01J 37/32862: {In situ cleaning of vessels and/or internal parts} - C11D 2111/22: Electronic devices, e.g. PCBs or semiconductors - C23C 16/45525: {Atomic layer deposition [ALD]} - 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) - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS - C23F: NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE (working metal by laser beams B23K26/00; desurfacing by applying flames B23K7/00; working of metal by electro-erosion B23H; producing decorative effects by removing surface material, e.g. by engraving, by etching, B44C1/22; electrolytic etching or polishing C25F); INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25 - C23G: CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS - H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H) - C11D: DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL ## Abstract The invention relates to a method for removing a metal deposit (2) arranged on a surface (5) in a chamber (1), said method including repeatedly performing a sequence including: a) a first phase of injecting chemical species suitable for oxidizing said metal deposit (2); and b) a second phase of injecting chemical species suitable for volatilizing the oxidized metal deposit, said second phase b) being performed after the first phase a). ## Claims ### Claim 1 A method for removing a metal deposit arranged on a surface in a chamber, said method including repeatedly performing a sequence including the following: a) a first phase of injecting chemical species suitable for oxidizing said metal deposit, first phase said injection of chemical species suitable for oxidizing said metal deposit being done in the form of one or several pulses; b) a second phase of injecting chemical species suitable for volatilizing the oxidized metal deposit, said second phase b) being performed after an end of the first phase a), second phase said injection of chemical species suitable for volatilizing the oxidized metal deposit being done in the form of one or several pulses; and adjusting the duration of the one or several pulses in phase b) to form a barrier against a passivation on the metal deposit, so that a layer of the oxidized metal deposit is not fully volatilized. ### Claim 2 (depends on 1) The method according to claim 1, wherein during each pulse in phase b), the oxidized metal deposit is at least partially volatilized by the chemical species. ### Claim 3 (depends on 2) The method according to claim 2, wherein the duration of the injection pulses ranges from 0.02 s to 5 s, and the delay between two consecutive pulses, if any, ranges from 0.02 s to 10 s. ### Claim 4 (depends on 1) The method according to claim 1, wherein the sequence includes a phase between phase a) and phase b) during which no chemical species is injected into the chamber. ### Claim 5 (depends on 1) The method according to claim 1, wherein the sequence includes an at least partial chamber purging phase between phase a) and phase b). ### Claim 6 (depends on 1) The method according to claim 1, including, between two consecutive sequences, a step in which no chemical species is injected into the chamber and/or the chamber is at least partially purged. ### Claim 7 (depends on 1) The method according to claim 1, wherein the chamber is maintained at a temperature between 20 and 250° C. ### Claim 8 (depends on 1) The method according to claim 1, wherein phase a) includes the injection of at least one of the following oxidizing species: oxygen, ozone, and nitrous oxide. ### Claim 9 (depends on 1) The method according to claim 1, wherein the chemical species injected in phase b) include hexafluoroacetylacetone. ### Claim 10 (depends on 1) The method according to claim 1, wherein the chemical species injected in phase a) and/or in phase b) are plasma-activated. ### Claim 11 (depends on 1) A method for cleaning metal residues arranged on the inner walls of a chemical vapour deposition chamber, wherein said metal residues are removed using the method of claim 1. ### Claim 12 (depends on 1) A method for etching a metal deposit deposited in excess on a surface, wherein at least a portion of said metal deposit is removed by means of the method of claim 1. ### Claim 13 (depends on 12) The method according to claim 12, characterized in that prior to the first sequence of a) and b) phases, a mask is affixed on the metal deposit in a localized manner. ### Claim 14 (depends on 13) The method according to claim 13, characterized in that it includes the following steps: the mask is affixed to each area of the metal deposit that is to be preserved; the sequence of a) and b) phases is performed one or several times to remove the excess metal deposit in each area not covered by the mask. ### Claim 15 (depends on 1) The method according to claim 1, characterized in that the sequence of a) and b) phases is repeated as many times as necessary to remove the excess metal deposit.