Granted Patent B2

US 12,601,050 · App. 18/785,339 · Granted Apr 14, 2026

Inventors: Carlo Waldfried (Middleton, MA); Surendra Maharjan (Lowell, MA); Stephen Longo (Westford, MA)

Assignee: ENTEGRIS, INC.

C23C16/30C23C16/52

Abstract

Claims (33)

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.

2 . 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.

3 . The substrate of claim 1 , wherein the substrate comprises:

at least 50% by weight of nickel based on a total weight of the substrate.

4 . The substrate of claim 1 , wherein the substrate comprises:

less than 10% by weight of iron based on a total weight of the substrate.

5 . The substrate of claim 1 wherein the substrate does not comprise magnesium.

6 . 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.

7 . The substrate of claim 1 , wherein the first region has a fluorine content of up to 100% as measured by XPS.

8 . The substrate of claim 1 , wherein the first region has a fluorine content of 10% to 70% as measured by XPS.

9 . The substrate of claim 1 , wherein the first region is resistant to thermal degradation at temperature of 200° C. to 500° C.

10 . The substrate of claim 1 , wherein the first region is an outermost region of the substrate.

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.

12 . 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.

13 . 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.

14 . 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.

15 . The method of claim 11 , wherein the fluorine-containing vapor comprises at least one of CF 4 , C 2 F 4 , C 3 F 6 , C 4 F 8 , CHF 3 , C 2 H 2 F 2 , C 2 F 6 , HF, CH 3 F, or any combination thereof.

16 . The method of claim 11 , wherein the fluorine-containing vapor comprises a vaporized fluorinated polymer.

17 . The method of claim 16 , wherein the vaporized fluorinated polymer is derived from at least one of polymerized perfluoroalkylethylene having a C 1 -C 10 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.

18 . 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.

19 . 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.

20 . The method of claim 11 , wherein the exposing comprises exposing the substrate to the fluorine-containing vapor at about atmospheric pressure.

Assignments (1)

Continuity (2)

References Cited (62)