# US 11,898,241 B2 · Method for a treatment to deposit a barrier coating

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- Number: US 11,898,241 B2
- Document ID: US11898241B2
- Status: Granted
- Kind: B2
- Application number: 17/423,788
- Filed: 2019-06-17
- Published: 2022-04-14
- Granted: 2024-02-13
- Earliest claimed: 2019-01-17
- Assignees: Innovative Systems Et Technologies (Isytech)
- Applicants: Innovative Systems Et Technologies (Isytech)
- Inventors: Nasser Beldi; Fabrice Oge; Patrick Chollet; Mikaël Jaouen
- Web page: https://patentgrep.com/patent/US11898241B2

## CPC

- C23C 16/045: {Coating cavities or hollow spaces, e.g. interior of tubes; Infiltration of porous substrates}
- B05D 1/62: {Plasma-deposition of organic layers (plasma deposition in general C23C14/00, C23C16/00)}
- B05D 7/02: to macromolecular substances, e.g. rubber (treatment or coating of shaped articles made of macromolecular substances C08J7/00)
- B05D 7/227: {of containers, cans or the like}
- C23C 16/4409: {characterised by sealing means}
- C23C 16/4412: {Details relating to the exhausts, e.g. pumps, filters, scrubbers, particle traps}
- C23C 16/511: using microwave discharges
- C23C 16/517: using a combination of discharges covered by two or more of groups C23C16/503 - C23C16/515
- H01J 37/32192: {Microwave generated discharge (H01J37/32357, H01J37/32366, H01J37/32394, H01J37/32403 take precedence)}
- H01J 37/32229: {Waveguides}
- H01J 37/32394: {Treating interior parts of workpieces}
- H05H 1/46: using applied electromagnetic fields, e.g. high frequency or microwave energy (H05H1/26 takes precedence)
- H05H 1/461: {Microwave discharges}
- H05H 1/4645: {Radiofrequency discharges}
- B05D 5/083: {involving the use of fluoropolymers}
- H05H 2245/40: Surface treatments
- 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)
- B05D: PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL (conveying articles or workpieces through baths of liquid B65G, e.g. B65G49/02)
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- H05H: PLASMA TECHNIQUE (apparatus or processes specially adapted for producing X-rays H05G2/00); PRODUCTION OF ACCELERATED ELECTRICALLY-CHARGED PARTICLES OR OF NEUTRONS; PRODUCTION OR ACCELERATION OF NEUTRAL MOLECULAR OR ATOMIC BEAMS

## Abstract

Method for treating in an enclosure an inner surface of a container made from polymer material, in order to deposit a barrier coating there on, comprises: inserting the container into the enclosure; introducing a precursor gas into the container intended, once transformed into the plasma state, to be deposited at least partially on the inner surface of the container in order to constitute the coating; wherein the method further comprises: transforming the precursor gas into the plasma state by a combination of excitations comprising a main excitation by means of electromagnetic waves comprising microwaves, and a secondary excitation by means of an electrical discharge of alternating voltage having a frequency between 1 kHz and 15 MHz.

## Claims

### Claim 1

Method for treating in an enclosure an inner surface of a container made from polymer material in order to deposit a barrier coating there on, comprising:
inserting the container into the enclosure,
introducing a precursor gas into the container, wherein the precursor gas is intended, once transformed into the plasma state, to be deposited at least partially on the inner surface of the container in order to constitute the coating, the method being characterized in that it furthermore comprises:
transforming the precursor gas into the plasma state by a combination of excitations comprising a main excitation by means of electromagnetic waves comprising microwaves, and a secondary excitation by means of an electrical discharge of alternating voltage having a frequency of between 1 kHz and 15 MHz, wherein the secondary excitation stabilizes the plasma state generated by the main excitation, wherein the excitation by means of electromagnetic waves comprising microwaves and the excitation by means of an electrical discharge of alternating voltage are carried out simultaneously during a treatment phase known as a plasma phase, and wherein a power of the main excitation is greater than a power of the secondary excitation.

### Claim 2 (depends on 1)

Treating method according to claim 1 characterized in that the plasma phase duration is between one second and 10 minutes.

### Claim 3 (depends on 1)

Treating method according to claim 1, characterized in that the effective value of the voltage of the electrical discharge is between 100 V and 1000 V.

### Claim 4 (depends on 1)

Treating method according as claimed in claim 1, characterized in that the precursor gas is a gas of 1,1,1,2-tetrafluoroethane, pentafluoroethane, difluoromethane, acetylene, or a combination of some of them or a mixture of some of them with a rare gas.

### Claim 5 (depends on 1)

Treating method as claimed in claim 1, characterized in that the power of the electrical discharge is between 1 W and 2000 W.

### Claim 6 (depends on 1)

Treating method as claimed in claim 1, characterized in that the gas is introduced into the enclosure with a controlled flow rate so as to maintain the enclosure at a pressure of between 0.002 mbar and 10 mbar.

### Claim 7 (depends on 1)

The method of claim 1, wherein the main excitation provides the energy to transform the precursor gas into the plasma, and wherein the secondary excitation stabilizes the plasma transformed by the main excitation.

### Claim 8 (depends on 1)

The method of claim 1, wherein the main excitation is introduced into the enclosure through at least one waveguide opening, and wherein the secondary excitation is generated by at least one electrode placed within the container.