# US 12,601,050 B2 · Surface modified substrates and related methods > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 12,601,050 B2 - Document ID: US12601050B2 - Status: Granted - Kind: B2 - Application number: 18/785,339 - Filed: 2024-07-26 - Published: 2025-01-30 - Granted: 2026-04-14 - Earliest claimed: 2023-07-27 - Assignees: Entegris, Inc. - Applicants: Entegris, Inc. - Inventors: Carlo Waldfried; Surendra Maharjan; Stephen Longo - Web page: https://patentgrep.com/patent/US12601050B2 ## CPC - C23C 16/30: Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides - C23C 8/08: only one element being applied - C23C 16/52: Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)} - 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) ## Abstract Surface modified substrates and related methods are provided. A substrate having a modified surface comprises a first region and a second region. The first region is located above the second region. The first region comprises a nickel fluoride. The second region comprises a nickel alloy. A concentration of the nickel fluoride gradually decreases from the first region to the second region. ## Claims ### Claim 1 A substrate comprising: a modified surface having a first region comprising a nickel fluoride and a second region comprising a nickel alloy, wherein the first region is above the second region and wherein a concentration of the nickel fluoride decreases from the first region to the second region within the modified surface of the substrate. ### Claim 2 (depends on 1) The substrate of claim 1, wherein the substrate has an aspect ratio of 2:1 to 2000:1, wherein the aspect ratio is a ratio of two of a width, a depth, a height, a length, or a diameter. ### Claim 3 (depends on 1) The substrate of claim 1, wherein the substrate comprises: at least 50% by weight of nickel based on a total weight of the substrate. ### Claim 4 (depends on 1) The substrate of claim 1, wherein the substrate comprises: less than 10% by weight of iron based on a total weight of the substrate. ### Claim 5 (depends on 1) The substrate of claim 1 wherein the substrate does not comprise magnesium. ### Claim 6 (depends on 1) The substrate of claim 1, wherein the first region extends from a surface of the substrate to a depth of 2 nm to 5 μm. ### Claim 7 (depends on 1) The substrate of claim 1, wherein the first region has a fluorine content of up to 100% as measured by XPS. ### Claim 8 (depends on 1) The substrate of claim 1, wherein the first region has a fluorine content of 10% to 70% as measured by XPS. ### Claim 9 (depends on 1) The substrate of claim 1, wherein the first region is resistant to thermal degradation at temperature of 200° C. to 500° C. ### Claim 10 (depends on 1) The substrate of claim 1, wherein the first region is an outermost region of the substrate. ### Claim 11 A method comprising: exposing a substrate to a fluorine-containing vapor sufficient to chemically modify a surface of the substrate to form a modified surface having a first region comprising a nickel fluoride and a second region comprising a nickel alloy, wherein the first region is above the second region and wherein a concentration of the nickel fluoride decreases from the first region to the second region within the substrate. ### Claim 12 (depends on 11) The method of claim 11, wherein the substrate has an aspect ratio of 2:1 to 2000:1, wherein the aspect ratio is a ratio of two of a width, a depth, a height, a length, or a diameter. ### Claim 13 (depends on 11) The method of claim 11, wherein the substrate comprises: at least 50% by weight of nickel based on a total weight of the substrate; and less than 10% by weight of iron based on the total weight of the substrate. ### Claim 14 (depends on 11) The method of claim 11, wherein a fluorine component from the fluorine-containing vapor reacts with a nickel component of the substrate to form the first region. ### Claim 15 (depends on 11) The method of claim 11, wherein the fluorine-containing vapor comprises at least one of CF4, C2F4, C3F6, C4F8, CHF3, C2H2F2, C2F6, HF, CH3F, or any combination thereof. ### Claim 16 (depends on 11) The method of claim 11, wherein the fluorine-containing vapor comprises a vaporized fluorinated polymer. ### Claim 17 (depends on 16) The method of claim 16, wherein the vaporized fluorinated polymer is derived from at least one of polymerized perfluoroalkylethylene having a C1-C10 perfluoroalkyl group, polytetrafluoroethylene (PTFE), tetrafluoroethylene/perfluoro(alkyl vinyl ether) copolymer (PFA), tetrafluoroethylene/hexafluoropropylene copolymer (FEP), tetrafluoroethylene/perfluoro(alkyl vinyl ether)/hexafluoropropylene copolymer (EPA), polyhexafluoropropylene, ethylene/tetrafluoroethylene copolymer (ETFE), poly trifluoroethylene, polyvinylidene fluoride (PVDF), polyvinyl fluoride (PVF), polychlorotrifluoroethylene (PCTFE), ethylene/chlorotrifluoroethylene copolymer (ECTFE), or any combination thereof. ### Claim 18 (depends on 11) The method of claim 11, wherein the exposing comprises heating at least a portion of the substrate at or to a temperature of 200° C. to 600° C. ### Claim 19 (depends on 11) The method of claim 11, wherein the exposing comprises exposing the substrate to the fluorine-containing vapor for a duration of 1 millisecond to 15 hours. ### Claim 20 (depends on 11) The method of claim 11, wherein the exposing comprises exposing the substrate to the fluorine-containing vapor at about atmospheric pressure.