# US 2021/0331202 A1 · Methods and systems for polymer deposition

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- Number: US 2021/0331202 A1
- Document ID: US20210331202A1
- Status: Published application
- Kind: A1
- Application number: 16/858,551
- Filed: 2020-04-24
- Published: 2021-10-28
- Earliest claimed: 2020-04-24
- Assignees: GVD Corporation
- Applicants: GVD Corporation
- Inventors: W. Shannan O'Shaughnessy; Andrew Grant; Kelli Byrne; Michael E. Stazinski; Hilton Pryce Lewis
- Web page: https://patentgrep.com/patent/US20210331202A1

## CPC

- B05D 1/60: {Deposition of organic layers from vapour phase (vapour phase deposition in general C23C14/00, C23C16/00)}
- B05D 5/083: {involving the use of fluoropolymers}
- C23C 14/12: Organic material
- C23C 16/4488: {by in situ generation of reactive gas by chemical or electrochemical reaction}
- C23C 16/463: {Cooling of the substrate}
- B05D 1/62: {Plasma-deposition of organic layers (plasma deposition in general C23C14/00, C23C16/00)}
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- 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

Systems having one or more features that are advantageous for depositing fluorinated polymeric coatings on substrates, and methods of employing such systems to deposit such coatings, are generally provided.

## Claims

### Claim 1

A system, comprising:
a deposition chamber comprising a reaction volume; and
a cooling element, wherein:
the reaction volume is capable of comprising hexafluoropropylene oxide vapor and being evacuated of air by a source of vacuum;
the reaction volume comprises a filament taking the form of a wire configured to increase in temperature upon the application of a voltage thereto;
the wire is configured to heat the hexafluoropropylene oxide vapor, thereby causing it to decompose;
a substrate is positioned in the reaction volume;
the cooling element is positioned around the substrate; and
the cooling element extends from a bottom of the substrate to the top of the substrate.

### Claim 2

A system, comprising:
a deposition chamber comprising a reaction volume; and
a cooling element, wherein:
the reaction volume is capable of comprising hexafluoropropylene oxide vapor and being evacuated of air by a source of vacuum;
the reaction volume comprises a filament taking the form of a wire configured to increase in temperature upon the application of a voltage thereto;
the wire is configured to heat the hexafluoropropylene oxide vapor, thereby causing it to decompose;
a substrate is positioned in the reaction volume;
the cooling element is positioned around the substrate; and
the substrate is freely-movable with respect to the cooling element.

### Claim 3

A method, comprising:
polymerizing hexafluoropropylene oxide to form a particle comprising poly(tetrafluoroethylene); and
depositing the particle comprising poly(tetrafluoroethylene) onto a surface, wherein:
the polymerization is performed in a reaction volume;
the reaction volume is positioned in a deposition chamber;
the reaction volume comprises at most 10 mTorr of air and comprises hexafluoropropylene oxide vapor;
the reaction volume comprises a filament taking the form of a resistively heated wire;
the wire heats the hexafluoropropylene oxide vapor, thereby causing it to decompose; and
when the particle forms, it is surrounded by gas.

### Claim 4

A method, comprising:
depositing a coating comprising poly(tetrafluoroethylene) on a substrate, wherein:
the substrate is positioned in a reaction volume;
the reaction volume is positioned in a deposition chamber;
the reaction volume comprises at most 10 mTorr of air and comprises hexafluoropropylene oxide vapor;
the reaction volume comprises a filament taking the form of a resistively heated wire;
the wire heats the hexafluoropropylene oxide vapor, thereby causing it to decompose;
the substrate outgasses one or more gases during the deposition of the coating; and
the one or more gases make up greater than or equal to 0.1 mol % and less than or equal to 10 mol % of the gases present in the reaction volume during the deposition of the coating.

### Claim 5

A method, comprising:
removing contaminants from a surface of a substrate by immersing the substrate in a solvent; and
within 30 minutes after the contaminants are removed, depositing a coating comprising poly(tetrafluoroethylene) onto the surface of the substrate by chemical vapor deposition, wherein, during the deposition step:
the substrate is positioned in a reaction volume;
the reaction volume is positioned in a deposition chamber;
the reaction volume comprises at most 10 mTorr of air and comprises hexafluoropropylene oxide vapor;
the reaction volume comprises a filament taking the form of a resistively heated wire; and
the wire heats the hexafluoropropylene oxide vapor, thereby causing it to decompose; and
wherein, after the deposition step, the coating has an adhesion to the substrate such that its adhesion score, as determined by the procedure described in ASTM D3359, is greater than or equal to 4.

### Claim 6 (depends on 3)

The method of claim 3, wherein a temperature of the wire is greater than or equal to 150° C. and less than or equal to 1500° C.

### Claim 7 (depends on 3)

The method of claim 3, wherein an amount of hexafluoropropylene oxide vapor in the reaction volume is greater than or equal to 1 mol % and less than or equal to 100 mol % of the gases present in the reaction volume.

### Claim 8 (depends on 3)

The method of claim 3, wherein the reaction volume further comprises a carrier gas.

### Claim 9 (depends on 8)

The method of claim 8, wherein the carrier gas is an inert gas.

### Claim 10 (depends on 3)

The method of claim 3, wherein a pressure of the reaction volume is greater than or equal to 1 mTorr and less than or equal to 100 Torr.

### Claim 11 (depends on 3)

The method of claim 3, wherein the reaction volume comprises a plurality of filaments taking the form of wires.

### Claim 12 (depends on 3)

The method of claim 3, wherein greater than or equal to 90% of the polymerization reaction results in the production of particles surrounded by gas.

### Claim 13 (depends on 1)

The system of claim 1, wherein the substrate comprises an elastomer.

### Claim 14 (depends on 1)

The system of claim 1, wherein the cooling element is cooled by the circulation of cooled fluid across and/or through the cooling element.

### Claim 15 (depends on 1)

The system of claim 1, wherein the cooling element is positioned beneath the substrate.

### Claim 16 (depends on 3)

The method of claim 3, wherein the particle has a diameter of greater than or equal to 0.5 nm and less than or equal to 50 microns.

### Claim 17 (depends on 3)

The method of claim 3, wherein the particle has a diameter of greater than or equal to 1 nm and less than or equal to 1 micron.

### Claim 18 (depends on 4)

The system of claim 4, wherein the gases outgassed by the substrate comprise water and/or air.

### Claim 19 (depends on 4)

The system of claim 4, wherein the contaminants comprise small molecules, oligomers, low molecular weight polymers, processing aids, and/or chemicals compounded with the substrate.

### Claim 20 (depends on 4)

The system of claim 4, wherein the coating is deposited prior to appreciable transport of contaminants from an interior of the substrate to a surface of the substrate.