# US 11,306,389 B2 · Ultraviolet activated antimicrobial surfaces

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- Number: US 11,306,389 B2
- Document ID: US11306389B2
- Status: Granted
- Kind: B2
- Application number: 16/399,214
- Filed: 2019-04-30
- Published: 2019-08-22
- Granted: 2022-04-19
- Earliest claimed: 2006-02-25
- Assignees: Metascape LLC
- Applicants: Metascape, LLC
- Inventors: Terrence S. Mcgrath; Deidre Sewell; Daniel M. Storey
- Web page: https://patentgrep.com/patent/US11306389B2

## CPC

- C23C 14/221: {Ion beam deposition (C23C14/46, C23C14/48 take precedence)}
- A61L 29/042: {Rubbers}
- A61L 29/085: {Macromolecular materials}
- A61L 29/106: {Inorganic materials other than carbon}
- A61L 29/16: Biologically active materials, e.g. therapeutic substances {(A61L29/048 takes precedence)}
- C02F 1/32: with ultraviolet light
- C23C 4/10: Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
- C23C 14/0688: {Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides}
- C23C 14/18: on other inorganic substrates
- C23C 14/205: {by cathodic sputtering}
- C23C 14/30: by electron bombardment
- C23C 14/325: {Electric arc evaporation}
- C23C 14/34: Sputtering
- C23C 14/54: Controlling or regulating the coating process
- A61L 2300/102: Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
- A61L 2300/104: Silver, e.g. silver sulfadiazine
- A61L 2300/404: Biocides, antimicrobial agents, antiseptic agents
- A61L 2300/606: Coatings
- 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)
- A61L: METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES (preservation of bodies or disinfecting characterised by the agents employed A01N; preserving, e.g. sterilising, food or foodstuffs A23; preparations for medical, dental or toiletry purposes A61K)
- C02F: TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE (separation in general B01D; special arrangements on waterborne vessels of installations for treating water, waste water or sewage, e.g. for producing fresh water, B63J; adding materials to water to prevent corrosion C23F; treating radioactively-contaminated liquids G21F9/04; regeneration of reactants for recirculation into processes, see the relevant places for the processes)

## Abstract

The invention is directed to an ion plasma deposition (IPD) method adapted to coat polymer surfaces with highly adherent antimicrobial films. A controlled ion plasma deposition (IPD) process is used to coat a metal or polymer with a selected metal/metal oxide. Exposing the coated surface to ultraviolet light significantly improves the antimicrobial properties of the deposited coatings.

## Claims

### Claim 1

An antibacterial coated medical implant device, comprising:
a metal and metal oxide ion plasma deposited nanoparticulate first layer from a target onto a medical device surface, said first layer consisting of metal and metal oxide nanoparticulates substantially free of macroparticulates formed by the process of:
(a) using ion plasma to deposit the first layer onto the substrate; and
(b) exposing the metal and metal oxide nanoparticulates to ultraviolet (UV) light irradiation during step (a), thereby activating ground state oxygen in the metal oxide to form a reactive oxygen species to provide an antimicrobially active coating on the medical device.

### Claim 2 (depends on 1)

The coated medical implant device of claim 1 wherein step (b) is performed in the presence of a gas selected from the group consisting of Ar/O; O2; N2; and Ar.

### Claim 3 (depends on 2)

The coated medical implant device of claim 2 wherein the gas is at about 40 mTorr pressure.

### Claim 4 (depends on 1)

The coated medical implant device of claim 1 wherein step (b) is performed at about 20 degrees Celsius.

### Claim 5 (depends on 1)

The coated medical implant device of claim 1, further comprising the step of:
(c) using ion plasma to deposit a second layer onto the substrate, the second layer being formed of macroparticulates; and
(d) exposing the macroparticulates to ultraviolet (UV) light irradiation during step (c), thereby activating ground state oxygen in the second layer to a reactive oxygen species to provide an antimicrobially active coating on the medical device.

### Claim 6 (depends on 5)

The coated medical implant device of claim 5, wherein the second layer consists of mixed sizes of metal and metal oxide macroparticulates ranging from 100 nm up to about 1 micron.

### Claim 7

An antibacterial bilayer coated medical implant device, comprising:
a metal and metal oxide ion plasma deposited nanoparticulate first layer from a target onto a medical device surface, said first layer consisting of metal and metal oxide nanoparticulates substantially free of macroparticulates; a metal and metal oxide deposited second layer over the first layer, said second layer consisting of mixed sizes of metal and metal oxide macroparticulates ranging from 100 nm up to about 1 micron; formed by the process of:
(a) using ion plasma to deposit the first layer and the second layer onto the substrate; and
(b) exposing the metal and metal oxide nanoparticulates and the macroparticulates to ultraviolet (UV) light irradiation during step (a), thereby activating ground state oxygen in the metal oxide to a reactive oxygen species to provide an enhanced antimicrobially active coating on the medical device.

### Claim 8 (depends on 7)

The coated medical implant device of claim 7 wherein step (b) is performed in the presence of a gas selected from the group consisting of Ar/O; O2; N2; and Ar.

### Claim 9 (depends on 8)

The coated medical implant device of claim 8 wherein the gas is at about 40 mTorr pressure.

### Claim 10 (depends on 7)

The coated medical implant device of claim 7 wherein step (b) is performed at about 20 degrees Celsius.

### Claim 11 (depends on 7)

The coated medical implant device of claim 7 wherein the bilayer thickness is about 100 nm.

### Claim 12 (depends on 7)

The coated medical implant device of claim 7 wherein the first, second, or first and second layers consist of mixed metal and metal oxide macroparticles selected from groups consisting of: (i) silver (Ag) and silver oxides (AgO and Ag2O); (ii) copper (Cu) and copper oxides (CuO and Cu2O); and (iii) titanium (Ti) and titanium oxides (TiO and TiO2).

### Claim 13 (depends on 12)

The coated medical implant device of claim 12 wherein the first and second layers consist of mixed silver metal and silver metal oxides AgO and Ag2O.

### Claim 14 (depends on 13)

The coated medical implant device of claim 13 wherein said layers consist of the silver metal oxides AgO and Ag2O.

### Claim 15

An antibacterial bilayer coated medical implant device, comprising:
a metal and metal oxide ion plasma deposited nanoparticulate first layer from a target onto a medical device surface, said first layer consisting of metal and metal oxide nanoparticulates substantially free of macroparticulates; a metal and metal oxide deposited second layer over the first layer, said second layer consisting of mixed sizes of metal and metal oxide macroparticulates ranging from 100 nm up to about 1 micron; formed by the process of:
(a) placing the substrate in a vacuum chamber at about 20 degrees Celsius;
(b) using ion plasma to deposit the first layer and the second layer onto the substrate; and
(c) exposing the metal and metal oxide nanoparticulates and the macroparticulates to ultraviolet (UV) light irradiation in the vacuum chamber during step (b), thereby activating ground state oxygen in the metal oxide to a reactive oxygen species to provide an enhanced antimicrobially active coating on the medical device.

### Claim 16 (depends on 15)

The antibacterial bilayer coated medical implant device of claim 15 wherein the vacuum chamber is at about 40 mTorr pressure.

### Claim 17 (depends on 16)

The antibacterial coated medical implant device according to claim 16, wherein step (a) further comprises including diatomic oxygen in the chamber.

### Claim 18 (depends on 16)

The antibacterial coated medical implant device according to claim 16, wherein step (a) further comprises including ozone in the chamber.

### Claim 19 (depends on 15)

The antibacterial bilayer coated medical implant device of claim 15 wherein step (a) comprises varying a distance between the target and the substrate.

### Claim 20 (depends on 15)

The antibacterial bilayer coated medical implant device of claim 15, wherein step (a) comprises varying a relative speed of movement between the target and the substrate.
