# US 10,117,964 B2 · Monolithic bodies of sintered chemically bonded ceramic (CBC) biomaterial prepared ex vivo for implantation, preparation and use thereof

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- Number: US 10,117,964 B2
- Document ID: US10117964B2
- Status: Granted
- Kind: B2
- Application number: 15/309,848
- Filed: 2015-05-12
- Published: 2017-09-21
- Granted: 2018-11-06
- Earliest claimed: 2014-05-14
- Assignees: Doxa AB
- Applicants: Doxa Aktiebolag
- Inventors: Leif Hermansson; Jesper Lööf; Emil Abrahamsson
- Web page: https://patentgrep.com/patent/US10117964B2

## CPC

- A61L 27/105: {containing Al2O3}
- A61K 6/71: Fillers
- A61K 6/74: comprising phosphorus-containing compounds
- A61K 6/76: comprising silicon-containing compounds
- A61K 6/802: comprising ceramics
- A61K 6/86: Al-cements
- A61K 6/864: Phosphate cements (apatite A61K6/838)
- A61K 6/871: Quartz; SiO2
- A61K 6/876: Calcium oxide
- A61L 27/12: Phosphorus-containing materials, e.g. apatite
- C01F 7/164: Calcium aluminates
- C03C 3/091: containing aluminium
- C04B 7/32: Aluminous cements
- C04B 28/06: Aluminous cements (monolithic refractories or refractory mortars C04B35/66)
- C04B 28/18: containing mixtures of the silica-lime type
- C04B 35/111: Fine ceramics
- C04B 35/14: based on silica
- C04B 35/195: Alkaline earth aluminosilicates, e.g. cordierite {or anorthite}
- C04B 35/48: based on zirconium or hafnium oxides, zirconates, {zircon} or hafnates
- C04B 35/488: Composites
- C04B 35/624: Sol-gel processing
- C04B 35/62665: {Flame, plasma or melting treatment}
- A61L 2400/18: Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
- A61L 2430/02: for reconstruction of bones; weight-bearing implants
- A61L 2430/12: for dental implants or prostheses
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C04B 2111/00836: {for medical or dental applications}
- C04B 2235/3222: Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
- 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)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- 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})
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present invention generally relates to the use of pre-formed bodies of Chemically Bonded Ceramics (CBCs) biomaterial for implantation purposes wherein the bodies are prepared ex vivo allowing process parameters to be optimized for desired long term properties of the resulting CBC biomaterial. More particularly, the pre-formed CBC material bodies of the present invention are sintered. The pre-formed body of CBC material is machined to the desired geometry and then implanted using a CBC cementation paste for fixation of the body to tissue. The invention also relates to a method of preparing pre-formed bodies of CBC biomaterial for implantation purposes, methods of preparing an implant thereof having desired geometry, and a method of implantation of the implant, as well as a kit for use in the method of implantation.

## Claims

### Claim 1

A method of preparing ex vivo a monolithic sintered, hardened raw body of CBC biomaterial for implantation purposes comprising the following steps:
A providing a CA-system CBC powder or a CAS-system CBC powder additionally containing phases of calcium phosphate;
B compacting the CBC powder into a green body;
S sintering ex vivo the green body, so as to obtain a sintered body; and
D hydrating ex vivo the sintered body obtained in step S using an aqueous hydration liquid, so as to obtain a raw hardened, sintered body of CBC biomaterial.

### Claim 2 (depends on 1)

The method of claim 1, wherein the CBC powder is a CAS-system CBC powder additionally containing phases of calcium phosphate.

### Claim 3 (depends on 1)

The method of claim 1, wherein the CBC powder is a CA-system CBC powder.

### Claim 4 (depends on 1)

The method of claim 1, wherein the predominant Ca-aluminate phase is C3A.

### Claim 5

A method of preparing ex vivo a sintered, monolithic CBC biomaterial implant comprising the following steps:
A providing a CA-system CBC powder or a CAS-system CBC powder additionally containing phases of calcium phosphate;
B compacting the powder into a green body;
S sintering ex vivo the green body, so as to obtain a sintered body;
D hydrating ex vivo the sintered body obtained in step S using an aqueous hydration liquid, so as to obtain a hardened, sintered body of CBC biomaterial;
E establishing a desired geometry of a desired implant;
F machining to the desired geometry established in step E either:
a) the compacted dry powder green body obtained in step B;
b) the partly or fully hydrated body in step D; or
c) the sintered body obtained in step S, so as to obtain a monolithic CBC biomaterial implant.

### Claim 6 (depends on 5)

The method of claim 5, wherein the CBC powder is a CAS-system CBC powder additionally containing phases of calcium phosphate.

### Claim 7 (depends on 5)

The method of claim 5, wherein the CBC powder is a CA-system CBC powder.

### Claim 8 (depends on 5)

The method of claim 5, wherein the predominant Ca-aluminate phase is C3A.

### Claim 9 (depends on 1)

A method of preparing ex vivo a monolithic, sintered CBC biomaterial implant, especially suited for chairside applications, comprising the steps of:
AA-D providing a pre-formed hardened, sintered raw monolithic CBC material body for implantation purposes, obtained by the method of claim 1;
E establishing a desired geometry of a desired implant; and,
F machining the pre-formed hardened, sintered raw monolithic CBC material body to the desired geometry established in step E so as to obtain a monolithic CBC biomaterial implant.

### Claim 10 (depends on 5)

The method of claim 5, wherein machining step (F) is accomplished using CAD/CAM.

### Claim 11 (depends on 9)

The method of claim 9, wherein machining step (F) is accomplished using CAD/CAM.

### Claim 12 (depends on 5)

A method of implanting a hardened, sintered, monolithic CBC biomaterial implant prepared ex vivo comprising the steps of:
AA-F providing a machined monolithic, sintered, hardened CBC biomaterial implant, obtained by the method of claim 5;
G providing a CA-, CS- or CAS-system CBC powder;
I mixing the CBC powder with an aqueous hydration liquid so as to obtain a cementation paste;
J applying the paste obtained in step Ito the implant;
K inserting the implant with the paste applied thereupon obtained in step J into a site of implantation; and
L allowing the cementation paste to harden at the site of implantation in vivo for fixation of the implant to the surrounding endogenous hard tissue.