# US 2014/0193499 A1 · Bioactive glass composition, its applications and respective preparation methods

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- Number: US 2014/0193499 A1
- Document ID: US20140193499A1
- Status: Published application
- Kind: A1
- Application number: 14/110,407
- Filed: 2012-04-05
- Published: 2014-07-10
- Earliest claimed: 2011-04-05
- Assignees: Reg4Life Regeneration Technology, S.A.
- Inventors: José Maria Da Fonte Ferreira; Ashutosh Goel
- Web page: https://patentgrep.com/patent/US20140193499A1

## CPC

- A61K 33/08: Oxides; Hydroxides
- A61K 9/0024: {Solid, semi-solid or solidifying implants, which are implanted or injected in body tissue (compositions for intravenous administration, normal injectable solutions or dispersions for, e.g. subcutaneous administration A61K9/0019; brain implants A61K9/0085; (coated) prostheses, catheters or stents A61L)}
- A61K 33/00: Medicinal preparations containing inorganic active ingredients
- A61K 33/16: Fluorine compounds
- A61K 33/42: Phosphorus; Compounds thereof
- A61L 27/10: Ceramics or glasses
- A61L 27/306: {Other specific inorganic materials not covered by A61L27/303 - A61L27/32}
- A61L 27/32: Phosphorus-containing materials, e.g. apatite
- A61L 27/58: Materials at least partially resorbable by the body
- C03C 3/064: containing boron
- C03C 3/112: containing fluorine
- C03C 3/115: containing boron
- C03C 4/0007: {for biologically-compatible glass}
- C03C 10/00: Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- A61L 2400/06: Flowable or injectable implant compositions
- A61L 2430/02: for reconstruction of bones; weight-bearing implants
- A61L 2430/12: for dental implants or prostheses
- A61L 2430/38: for reconstruction of the spine, vertebrae or intervertebral discs
- 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)
- 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)
- 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

## Abstract

The present invention relates to development of bioactive glass/glass-ceramic composition that are able to promote a fast deposition layer of carbonated hydroxyapatite upon immersion in simulated body fluid (SBF) for time periods as short as one hour. Such composition might include fluorides, and a variety of oxides (or their precursor compounds), such as Na2O—Ag2O—SrO—CaO—MgO—ZnO—P2O5—SiO2—Bi2O3—B2O3—CaF2, be prepared by the melt route or by the sol-gel process, with the specific composition and the preparation route selected according to the intended functionalities, which can present controlled biodegradation rate and bactericidal activity. The powders derived from glass melts purred in cold water (frits) may completely densify by sintering at temperatures up to 800° C. without devitrification, resulting in bioglass compacts with high flexural strength (˜85 MPa). The bioactive glass powders prepared by sol-gel densify at lower temperatures due to their higher specific surface area and reactivity.

## Claims

### Claim 1

A bioactive glass composition comprising the following components:
(a) calcium oxide (CaO), between 20-60%;
(b) magnesium oxide (MgO), between 0-30%;
(c) phosphorous pentoxide (P2O5), between 0-10%;
(d) silica (SiO2) between 29-60%; and
(e) calcium fluoride in the form of CaF2, between 0-5%;
wherein all the percentages are molar percentages.

### Claim 2 (depends on 1)

The composition according to claim 1, further comprising alkali metals in a concentration less than 5%.

### Claim 3 (depends on 1)

The composition according to claim 1, which is alkali-free.

### Claim 4 (depends on 1)

The composition according to claim 1, wherein the phosphorous pentoxide and the silica are glass network formers.

### Claim 5 (depends on 1)

The composition according to claim 1, comprising the following components:
(a) calcium oxide (CaO), between 25-53%;
(b) magnesium oxide (MgO), between 2-24%;
(c) phosphorous pentoxide (P2O5), between 1.7-8%;
(d) silica (SiO2) between 29-50%; and
(e) calcium fluoride in the form of CaF2, between 0-3%;
wherein all the percentages are molar percentages.

### Claim 6 (depends on 1)

The composition according to claim 1, wherein the source of calcium is selected from at least one of the following: calcium oxide, calcium hydroxide, calcium carbonate, calcium nitrate, calcium sulphate, and calcium silicates.

### Claim 7 (depends on 1)

The composition according to claim 1, wherein the source of magnesium is selected from at least one of the following: magnesium oxide, magnesium hydroxide, magnesium carbonate, magnesium nitrate, magnesium sulphate, and magnesium silicates.

### Claim 8 (depends on 1)

The composition according to claim 1, wherein the source of phosphorous is selected from at least one of the following: phosphorous pentoxide, ammonium dihydrogen phosphate, trimethyl phosphafate, triethyl phosphate, phosphoric acid, and any other source of phosphorous pentoxide.

### Claim 9 (depends on 1)

The composition according to claim 1, wherein the source of fluorine is selected from at least one of the following: calcium fluoride, magnesium fluoride, trifluoroacetic acid, hexafluorophosphate acid, and ammonium hexafluorophosphate.

### Claim 10 (depends on 1)

The composition according to claim 1, further comprising as a doping agent at least one of the following elements: Na, K, Li, Ru, Cs, Fr, Sr, Bi, Zn, Ag, B, Cu, Mn, Fe, and Ti or an oxide thereof in a molar percentage between 0-10%.

### Claim 11 (depends on 1)

The composition according to claim 1, wherein the individual molar percentage of the doping oxide varies between 0-5%.

### Claim 12 (depends on 1)

The composition according to claim 1, comprising the following:
(a) an oxide, such as Na2O, K2O, SiO2, CaO, MgO, P2O5, Ru2O, Cs2O, Fr2O, SrO, Bi2O3, ZnO, Ag2O, B2O3, Cu2O, MnO2, Fe2O3, or TiO2;
(b) an alkoxide, such as traethyl orthosilicate, Si(OC2H5)4, (TEOS) or tetramethyl orthosilicate, Si(OCH3)4, (TMOS), or titanium isopropoxide, C12H28O4Ti;
(c) a hydroxide, such as NaOH, Ca(OH)2, Mg(OH)2, or Fe(OH)3;
(d) a carbonate, such as Na2CO3, K2CO3, CaCO3, MgCO3, or SrCO3;
(e) a nitrate, such as NaNO3, Ag(NO3), Mg(NO3)2, Ca(NO3)2, Ca(NO3)2.4H2O, Ag2(NO3)2, Fe(NO3)3, or Fe(NO3)3.9H2O;
(f) a sulphate, such as Na2SO4, K2SO4, or CaSO4;
(g) a phosphate, or phosphorus precursor, such as ammonium dihydrogen phosphate (NH4H2PO4), trimethyl phosphate, (CH3O)3PO (TMP), triethyl phosphate, (C2H5O)3PO (TEP), phosphoric acid, disodium hydrogen phosphate, Na2HPO4, monosodium phosphate, NaH2PO4, sodium tripolyphosphate, Na5O10P3, or sodium hexametaphosphate, (NaPO3)6;
(h) a fluoride, or fluorine precursor, such as calcium fluoride, CaF2, magnesium fluoride (MgF2), trifluoroacetic acid, CF3COOH (TFA), hexafluorophosphoric acid, (HPF6), ammonium hexafluorophosphate (NH4PF6), etc.), or a chloride (ex.: CaCl2, MgCl2, FeCl3); and
(i) a borate, such as sodium borate decahydrate, Na2B4O7.10H2O.

### Claim 13 (depends on 1)

The composition according to claim 1, further comprising a polymeric resin.

### Claim 14 (depends on 1)

The composition according to claim 1, in powder form.

### Claim 15 (depends on 1)

The composition according to claim 1, in the form of particles with sizes less than 500 mm.

### Claim 16 (depends on 1)

The composition according to claim 1, further comprising injectable cements based on calcium phosphates or on polymethylmethacrylate.

### Claim 17

(canceled)

### Claim 18 (depends on 1)

The composition according to claim 1, in the form of a prosthesis, implant, tooth paste, dental cement, or bone filler.

### Claim 19 (depends on 1)

The composition according to claim 1, for use in the synthesis in vitro of bone tissue.

### Claim 20 (depends on 18)

The composition according to claim 18, in the form of a coating on an implant, namely, an orthopaedic or dental prosthesis.

### Claim 21 (depends on 20)

The composition according to claim 20, wherein the prostheses is made of a chromium cobalt alloy, stainless steel, a titanium alloy such as Ti6Al4V, a polymeric material, a ceramic material or mixture of two or more of the foregoing,

### Claim 22 (depends on 1)

Frits comprising the bioglass compositions according to claim 1.

### Claim 23 (depends on 1)

Fibres, nets, meshes or discs comprising the composition according to claim 1.

### Claim 24 (depends on 1)

A method of preparation of the bioactive glass composition, according to claim 1, comprising the following steps:
(a) melting of the batches composed of mixtures of components, preferentially, oxides carbonates, nitrates, sulphates, fluorides, at temperatures in the range of 1050-1600° C. and time intervals between 1-2 h; and
(b) pouring the melts into moulds, preferentially, metallic or graphite moulds, to obtain bulk glasses.

### Claim 25

(canceled)

### Claim 26 (depends on 1)

A method for obtaining the bioactive glass composition according to claim 1, comprising the following steps:
(a) dissolution of compounds that include: alkoxides, phosphates, fluorides, nitrates, chlorides, sulphates, oxides, acids in absolute ethanol;
(b) addition of water and catalysts;
(c) formation of a colloidal suspension;
(d) polymerization;
(e) production of inorganic colloidal materials dispersed in a solvent, through the growth of oxo-metal polymers forming a porous three-dimensional structure;
(f) aging and formation of the rigid gel; and
(g) thermal treatment.

### Claim at position 27

27-29. (canceled)