# US 2020/0392001 A1 · Hydroxyapatite based composition and film thereof comprising inorganic fullerene-like nanoparticles or inorganic nanotubes

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- Number: US 2020/0392001 A1
- Document ID: US20200392001A1
- Status: Published application
- Kind: A1
- Application number: 16/970,958
- Filed: 2019-02-21
- Published: 2020-12-17
- Earliest claimed: 2018-02-22
- Assignees: Yeda Research and Development Co. Ltd.; Holon Academic Institute of Technology
- Applicants: Yeda Research and Development Co. Ltd.; Holon Academic Institute of Technology
- Inventors: Reshef TENNE; Hila SHALOM; Lev RAPOPORT
- Web page: https://patentgrep.com/patent/US20200392001A1

## CPC

- C01B 25/32: Phosphates of magnesium, calcium, strontium, or barium
- A61L 27/04: Metals or alloys
- A61L 27/06: Titanium or titanium alloys
- A61L 27/303: {Carbon}
- A61L 27/32: Phosphorus-containing materials, e.g. apatite
- C01B 19/007: {Tellurides or selenides of metals (C01B19/002 takes precedence)}
- C01F 11/02: Oxides or hydroxides (production of lime C04B2/00)
- C01G 39/06: Sulfides
- C01G 41/00: Compounds of tungsten
- C23C 18/1204: {inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds}
- C23C 18/1254: {Sol or sol-gel processing}
- C23C 18/127: {Preformed particles}
- C25D 9/12: on light metals
- C25D 11/26: of refractory metals or alloys based thereon
- A61L 2400/10: Materials for lubricating medical devices
- A61L 2400/12: Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
- A61L 2420/04: Coatings containing a composite material such as inorganic/organic, i.e. material comprising different phases
- A61L 2430/02: for reconstruction of bones; weight-bearing implants
- A61L 2430/12: for dental implants or prostheses
- C01P 2004/13: Nanotubes
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C08K 3/30: Sulfur-, selenium- or tellurium-containing compounds
- C08K 3/32: Phosphorus-containing compounds
- C08K 2003/321: {Phosphates}
- C08K 2201/011: Nanostructured additives
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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)
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- 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)
- C25D: PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)

## Abstract

This invention is directed to compositions and films comprising hydroxyapatite with minute amounts of doped inorganic fullerene-like (IF) nanoparticles or doped inorganic nanotubes (INT); methods of preparation and uses thereof.

## Claims

### Claim 1

A composition comprising hydroxyapatite [Ca10(PO4)6(OH)2)] and inorganic fullerene-like nanoparticles or inorganic nanotubes; wherein the inorganic fullerene-like nanoparticles or inorganic nanotubes is A1−xBx-chalcogenide where A is a metal or transition metal or an alloy of one metals or transition metals including at least one of the following: Mo, W, Re, Ti, Zr, Hf, Nb, Ta, Pt, Ru, Rh, In, Ga, InS, InSe, GaS, GaSe, WMo, TiW; and B (dopant) is a metal transition metal selected from the following: Si, Nb, Ta, W, Mo, Sc, Y, La, Hf, Ir, Mn, Ru, Re, Os, V, Au, Rh, Pd, Cr, Co, Fe, Ni; x is below or equal 0.003; and the chalcogenide is selected from the S, Se, Te.

### Claim 2 (depends on 1)

The composition according to claim 1, wherein the inorganic fullerene-like nanoparticles or inorganic nanotubes are WS2, MoS2 or combination thereof.

### Claim 3 (depends on 1)

The composition according to claim 1, wherein the concentration of the dopant is below or equal to 0.3 at %.

### Claim 4 (depends on 1)

The composition according to claim 1, wherein the composition further comprises brushite, portlandite or combination thereof.

### Claim 5 (depends on 1)

The composition according to claim 1, wherein composition is deposited on a substrate forming a film.

### Claim 6 (depends on 5)

The composition according to claim 5, wherein the substrate is a biocompatible.

### Claim 7 (depends on 6)

The composition according to claim 6, wherein the substrate is a titanium, alloys of titanium, Co—Cr alloys, magnesium, stainless steel, shape memory alloys of nickel-titanium, silver, tantalum, zirconium and novel ceramics or any electrical-conductive substrate.

### Claim 8 (depends on 7)

The composition according to claim 7, wherein the titanium is porous.

### Claim 9 (depends on 1)

The composition according to claim 1, wherein the concentration of the doped inorganic fullerene-like nanoparticles is between 0.2 wt % to 5 wt % of the composition.

### Claim 10 (depends on 1)

The composition according to claim 1, wherein the composition has a positive zeta potential at pH below 6.5.

### Claim 11 (depends on 1)

The composition according to claim 1, wherein the composition further comprises a cationic surfactant.

### Claim 12 (depends on 1)

The composition according to claim 1, wherein the composition further comprises a polymeric binder.

### Claim 13 (depends on 5)

The composition according to claim 5, wherein the film has low friction coefficient of between 0.1 to 0.7.

### Claim 14 (depends on 13)

The composition according to claim 13, wherein the low friction is maintained after annealing.

### Claim 15 (depends on 1)

A method of coating a metal substrate with the composition according to claim 1, wherein the method comprises electrophoretic deposition plasma spray, ion beam coating, e-beam evaporation, thermal deposition, physical vapor deposition (PVD), aerosol deposition, vacuum deposition, sol gel deposition, or dip coating.

### Claim 16 (depends on 15)

The method according to claim 15, wherein the metal substrate is biocompatible.

### Claim 17 (depends on 16)

The method according to claim 16, wherein the metal substrate is titanium, alloys of titanium, Co—Cr alloys, magnesium, stainless steel, shape memory alloys of nickel-titanium, silver, tantalum, zirconium and novel ceramics or any electrical-conductive substrate.

### Claim 18 (depends on 15)

The method according to claim 15, wherein the metal substrate is anodized prior to the electrophoretic deposition.

### Claim 19 (depends on 15)

The method according to claim 15 wherein the electrophoretic deposition is conducted between 2 to 5 hours.

### Claim 20 (depends on 1)

A dental or orthopedic implant comprising the composition according to claim 1.

### Claim 21 (depends on 1)

A dental or orthopedic implant comprising a film on a biocompatible substrate, wherein the film comprises the composition according to claim 1.

### Claim 22 (depends on 1)

A bone regeneration therapy comprising administering an artificial bone implant comprising the composition according to claim 1.

### Claim 23 (depends on 1)

A method of osseointegration comprising contacting an artificial bone implant comprising the composition according to claim 1 in a bone needs to be improved.

### Claim 24 (depends on 23)

The method according to claim 23, wherein the artificial bone implant comprises a biocompatible substrate coated by a film, wherein the film comprises said composition.

### Claim 25 (depends on 22)

The bone regeneration therapy according to claim 22, wherein the artificial bone implant comprises a biocompatible substrate coated by a film, wherein the film comprises said composition.