# US 10,117,966 B2 · Method for producing nanosurfaces with nano, micron, and/or submicron structures on a polymer

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- Number: US 10,117,966 B2
- Document ID: US10117966B2
- Status: Granted
- Kind: B2
- Application number: 15/066,747
- Filed: 2016-03-10
- Published: 2016-11-10
- Granted: 2018-11-06
- Earliest claimed: 2010-06-25
- Assignees: Nanovis, LLC
- Applicants: Nanovis, Inc.
- Inventors: Matthew Hedrick; Ganesan Balasundaram; Chang Yao
- Web page: https://patentgrep.com/patent/US10117966B2

## CPC

- A61L 27/18: obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- A61B 17/0401: {Suture anchors, buttons or pledgets, i.e. means for attaching sutures to bone, cartilage or soft tissue; Instruments for applying or removing suture anchors (A61B17/0642 takes precedence; fixation devices for tendons or ligaments A61F2/0811)}
- A61B 17/06166: {Sutures (suture materials A61L17/00; manufacture of artificial threads D01D; treatment of threads D06M)}
- A61C 8/00: Means to be fixed to the jaw-bone for consolidating natural teeth or for fixing dental prostheses thereon; Dental implants; Implanting tools (fastening of peg-teeth in the mouth A61C13/30)
- A61F 2/0063: {Implantable repair or support meshes, e.g. hernia meshes}
- A61L 17/04: Non-resorbable materials
- A61L 17/14: Post-treatment to improve physical properties
- A61L 27/10: Ceramics or glasses
- A61L 27/50: Materials characterised by their function or physical properties {, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials}
- A61L 31/048: {obtained by reactions only involving carbon-to-carbon unsaturated bonds (A61L31/041 takes precedence)}
- A61L 31/06: obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds {(A61L31/041 takes precedence)}
- A61L 31/14: Materials characterised by their function or physical properties {, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials}
- B29C 59/022: {characterised by the disposition or the configuration, e.g. dimensions, of the embossments or the shaping tools therefor}
- C08F 110/06: Propene
- C08G 63/88: Post-polymerisation treatment
- C08G 65/4012: {Other compound (II) containing a ketone group, e.g. X-Ar-C(=O)-Ar-X for polyetherketones}
- C08G 65/46: Post-polymerisation treatment, e.g. recovery, purification, drying
- C08L 23/10: Homopolymers or copolymers of propene
- C08L 71/00: Compositions of polyethers obtained by reactions forming an ether link in the main chain (of polyacetals C08L59/00; of epoxy resins C08L63/00; of polythioether-ethers C08L81/02; of polyether-sulfones C08L81/06); Compositions of derivatives of such polymers
- A61L 2400/12: Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
- A61L 2400/18: Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
- B29C 41/24: for making articles of indefinite length
- B29K 2071/00: Use of polyethers {, e.g. PEEK, i.e. polyether-etherketone or PEK, i.e. polyetherketone or derivatives thereof}, as moulding material
- B29L 2031/7532: {Artificial members, protheses}
- C08G 2650/40: containing ketone groups, e.g. polyarylethylketones, PEEK or PEK
- Y10T 428/24355: Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
- Y10T 428/2978: Surface characteristic
- Y10T 428/2982: Particulate matter [e.g., sphere, flake, etc.]
- 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)
- A61B: DIAGNOSIS; SURGERY; IDENTIFICATION (usefulness limited to only animals A61D)
- A61C: DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE (non-driven toothbrushes A46B; {tongue scrapers A61B17/24;} preparations for dentistry A61K6/00; preparations for cleaning the teeth or mouth A61K8/00, A61Q11/00)
- 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)
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- B29K: INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR {MOULDS, } REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29L: INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

The present invention relates to a modified polymeric material. The modified polymeric material includes a polymer having a modified surface, where the modified surface includes nano, micron, and/or submicron scale features. The present invention also relates to an implant comprising the modified polymeric material. The present invention further relates to processes for making the modified polymeric material and the implant.

## Claims

### Claim 1

A process for preparing a modified polymeric material, said process comprising:
providing a polymer, wherein the polymer is polyetheretherketone (PEEK); and
subjecting the polymer to a high vacuum treatment regimen under conditions effective to modify a surface of the polymer by introducing to the surface of the polymer features selected from the group consisting of nanoscale features, micron scale features, and submicron scale features,
wherein said high vacuum treatment regimen comprises simultaneously heating the polymer at a temperature of between 275° C. and 400° C. and incubating the polymer in a vacuum chamber under high vacuum conditions in a range of 10−2 Torr to 10−6 Torr effective to modify the surface of the polymer,
wherein said subjecting comprises:
(a) loading the polymer at a first temperature;
(b) increasing the temperature during a ramp-up period to a second temperature of 275° C. to 400° C.;
(c) maintaining the polymer at the second temperature;
(d) then, decreasing the temperature by 125° C. to 250° C. during a ramp-down period to a third temperature; and
(e) after the ramp-down period, extracting the polymer.

### Claim 2 (depends on 1)

The process according to claim 1, wherein the first temperature is about 150° C.

### Claim 3 (depends on 1)

The process according to claim 1, wherein the second temperature is about 275° C. to about 350° C.

### Claim 4 (depends on 1)

The process according to claim 1, wherein the third temperature is about 150° C.

### Claim 5 (depends on 1)

The process according to claim 1, wherein the ramp-up period is performed over the course of about 1 hour.

### Claim 6 (depends on 1)

The process according to claim 1, wherein the polymer is maintained at the second temperature for about 1 hour.

### Claim 7 (depends on 1)

The process according to claim 1, wherein the ramp-down period is performed over the course of about 1 hour.

### Claim 8 (depends on 1)

The process according to claim 1, wherein said incubating is carried out for at least 5 hours.

### Claim 9 (depends on 1)

The process according to claim 1, further comprising storing the extracted polymer under high vacuum conditions in a range of 10−2 Torr to 10−6 Torr for about 8 hours.

### Claim 10 (depends on 1)

The process according to claim 1, further comprising at least one of:
applying an acid etching procedure either before or after the polymer is modified; and
integrating or coating the modified polymeric material with another material to yield a two layer or integration of the modified polymeric material and the other material.

### Claim 11 (depends on 10)

The process according to claim 10, wherein the other material comprises hydroxyapatite, titanium, or calcium.

### Claim 12 (depends on 1)

The process according to claim 1, wherein the polymer is in the form of a polymeric film, fiber, sphere, ovoid, rod, filament, monofilament, or scaffold, plug, or matrix.

### Claim 13 (depends on 1)

The process according to claim 1, wherein said modified polymeric material is effective to modify a biological response, fixation, or a therapeutic attachment/delivery compared to a corresponding non-modified polymeric material.

### Claim 14 (depends on 13)

The process according to claim 13, wherein said modified polymeric material is effective to modify the biological response, and the biological response is selected from the group consisting of protein or antibody adsorption, cell attachment, cell function, and tissue growth.

### Claim 15 (depends on 13)

The process according to claim 13, wherein said modified polymeric material is effective to modify the therapeutic attachment/delivery, and the therapeutic is selected from the group consisting of a peptide, protein, growth factor, antibody, drug, metal, antimicrobial metal, antibiotic metal, biologic tissue, biologic agent, chemical agent, stem cell, and modified cell.

### Claim 16 (depends on 1)

The process according to claim 1, wherein the modified polymeric material further comprises at least one of:
a functional attachment effective to increase biological response or therapeutic attachment/delivery; and
a ceramic, metal, or another polymer integrated into the modified polymeric material or coated onto the surface of the modified polymeric material.

### Claim 17 (depends on 16)

The process according to claim 16, wherein the functional attachment is selected from the group consisting of a peptide, protein, growth factor, antibody, drug, metal, antimicrobial metal, antibiotic metal, biologic tissue, biologic agent, chemical agent, stem cell, and modified cell.

### Claim 18 (depends on 1)

A process for making an implant, said process comprising preparing a modified polymeric material according to claim 1, and forming an implant comprising the modified polymeric material.

### Claim 19 (depends on 18)

The process according to claim 18, wherein the implant is a spine cage, vertebral body replacement, suture anchor, dental implant, or maxillofacial implant.