# US 10,119,189 B2 · Biocompatible multilayer-thin-film-type coating as a surface treatment for biomedical substrates, and method for the production thereof

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- Number: US 10,119,189 B2
- Document ID: US10119189B2
- Status: Granted
- Kind: B2
- Application number: 14/896,384
- Filed: 2013-10-04
- Published: 2016-05-05
- Granted: 2018-11-06
- Earliest claimed: 2013-06-07
- Assignees: Universidad Del Valle
- Applicants: Universidad Del Valle
- Inventors: Federico Sequeda Osorio; Jose Oscar Gutierrez Montes; Alexander Ruden Muñoz
- Web page: https://patentgrep.com/patent/US10119189B2

## CPC

- C23C 14/3464: {using more than one target (C23C14/56 takes precedence)}
- A61F 2/0077: {Special surfaces of prostheses, e.g. for improving ingrowth (A61F2/30767 takes precedence)}
- A61L 27/30: Inorganic materials
- A61L 31/082: {Inorganic materials}
- C23C 14/0641: {Nitrides (C23C14/0617 takes precedence)}
- C23C 14/14: Metallic material, boron or silicon
- C23C 14/165: {by cathodic sputtering}
- C23C 14/34: Sputtering
- C23C 14/35: by application of a magnetic field, e.g. magnetron sputtering {(C23C14/3457 takes precedence)}
- C23C 28/321: {with at least one metal alloy layer}
- C23C 28/34: {including at least one inorganic non-metallic material layer, e.g. metal carbide, nitride, boride, silicide layer and their mixtures, enamels, phosphates and sulphates}
- A61L 2420/08: Coatings comprising two or more layers
- 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)
- A61F: FILTERS IMPLANTABLE INTO BLOOD VESSELS; PROSTHESES; DEVICES PROVIDING PATENCY TO, OR PREVENTING COLLAPSING OF, TUBULAR STRUCTURES OF THE BODY, e.g. STENTS; ORTHOPAEDIC, NURSING OR CONTRACEPTIVE DEVICES; FOMENTATION; TREATMENT OR PROTECTION OF EYES OR EARS; BANDAGES, DRESSINGS OR ABSORBENT PADS; FIRST-AID KITS (dental prosthetics A61C)
- 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)

## Abstract

The present invention discloses a process for the manufacture of a thin-film multilayered coating used in treating biomedical substrates and a coating in multilayered thin-film form (S/TiN/Ti/TiZr) to treat biomedical substrates used in surgical implants.

## Claims

### Claim 1

A process to manufacture a thin-film multilayered coating for the treatment of biomedical substrates, comprising:
polishing the substrate surface to a granulometry of between 700 and 2500 to generate a mirror surface finish;
washing the substrate with acetone in ultrasound for 10 to 20 min;
submerging the substrate in a PVD-DC magnetron sputtering reactor at a temperature of between 20 and 25° C., vacuum of 5.1×10-6 torr, and 50 to 60% relative humidity;
depositing a TiN coating layer with thickness of between 550 and 590 nm from a Ti precursor target (99.99%) at a pressure of 2 to 4 mtorr, argon flow between 8 and 12 sccm, nitrogen flow between 0.1 and 0.2 sccm, precursor target potential between 80 and 120 W, polarization voltage from −50 to −120 V, and interelectrode distance between 8 and 12 cm;
depositing the Ti coating layer with thickness between 550 and 590 nm from a Ti precursor target (99.99%) at a pressure from 2 to 4 mtorr, argon flow between 8 and 12 sccm, precursor target potential between 80 and 120 W, polarization voltage from −50 to −120 V, and interelectrode distance between 8 and 12 cm; and
depositing the TiZr coating layer with thickness between 550 and 590 rim from a TiZr precursor target (30-70%) at a pressure from 2 ; to 4 mtorr, argon flow between 8 and 12 sccm, precursor target potential between 60 and 100 W, polarization voltage from −50 to −120 V, and interelectrode distance between 8 and 12 cm.

### Claim 2

A coated biomedical substrate, comprising:
a multilayered thin-film coat comprising a TiN coating layer having a thickness of between 550 and 590 nm over the substrate; an intermediate layer of Ti having a thickness of between 550 and 590 nm; and
an external TiZr layer having a thickness between 550 and 590 nm.

### Claim 3 (depends on 2)

A surgical implant comprising the coated biomedical substrate of claim 2, wherein the substrate is selected from the group consisting of 316L stainless steel, Co—Cr alloy, and Ti alloy.