# US 10,500,313 B2 · Method for producing a porous monolithic material

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- Number: US 10,500,313 B2
- Document ID: US10500313B2
- Status: Granted
- Kind: B2
- Application number: 15/743,492
- Filed: 2016-07-15
- Published: 2018-07-19
- Granted: 2019-12-10
- Earliest claimed: 2015-07-17
- Assignees: Centre National De La Recherche Scientifiqu; Universite De Bordeaux
- Applicants: Centre National De La Recherche Scientifique; Universite De Bordeaux
- Inventors: Alain Largeteau; Mythili Prakasam
- Web page: https://patentgrep.com/patent/US10500313B2

## CPC

- A61L 27/56: Porous materials, {e.g. foams or sponges}
- A61L 27/025: {Other specific inorganic materials not covered by A61L27/04 - A61L27/12}
- A61L 27/12: Phosphorus-containing materials, e.g. apatite
- A61L 27/222: {Gelatin}
- A61L 27/24: Collagen
- C01B 25/327: {After-treatment}
- C01F 7/021: After-treatment of oxides or hydroxides
- C01G 23/08: Drying; Calcining {; After treatment of titanium oxide}
- C01G 25/006: {Compounds containing zirconium, with or without oxygen or hydrogen, and containing two or more other elements}
- C01G 25/02: Oxides
- C04B 30/00: Compositions for artificial stone, not containing binders
- C04B 38/0605: {by sublimating}
- F26B 5/06: the process involving freezing
- A61L 2430/02: for reconstruction of bones; weight-bearing implants
- C04B 2111/0081: {as catalysts or catalyst carriers}
- C04B 2111/00836: {for medical or dental applications}
- C04B 2111/00844: {for electronic applications}
- 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)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- 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)
- 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
- F26B: DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM (drying devices for combines A01D41/133; racks for drying fruit or vegetables A01F25/12; drying foodstuffs A23; drying hair A45D20/00; body-drying implements A47K10/00; drying household articles A47L; drying gases or vapours B01D; chemical or physical processes for dewatering or like separating liquids from solids B01D43/00; centrifugal apparatus B04; drying ceramics C04B33/30; drying yarns or fabrics in association with some other form of treatment D06C; drying frames for laundry without heating or positive air circulation, domestic laundry-or spin-driers, wringing or hot pressing laundry D06F; furnaces, kilns, ovens F27)

## Abstract

Disclosed is a method for producing a porous monolithic material from at least one powder, preferably mineral, the method including at least one step of low-temperature compression of a mixture based on powder and at least one solvent, preferably water. The materials produced by the method have improved mechanical properties compared to the prior art materials. The materials for medical application, such as hydroxyapatite, also have improved biocompatibility compared to the prior art materials. Also disclosed are materials produced by the method.

## Claims

### Claim 1

Method for producing a porous monolithic material (5), this method comprising at least the following steps:
(a) Supplying at least one mineral or organic powder (S),
(b) Preparing a mixture (1) comprising at least the powder of step (a) and at least one solvent,
(c) Packing the mixture of step (b) in sealed packaging (2) made from an elastically deformable material in order to form a sample (3),
(d) Applying to the sample (3) of step (c) a pressure (P) greater than or equal to 50 MPa at a temperature at which the solvent is in solid form,
(e) Returning to atmospheric pressure,
(f) Opening the packaging and recovering the material,
(g) Removing the solvent at a temperature at which the solvent is in solid form.

### Claim 2 (depends on 1)

Method according to claim 1, in which the powder (S) is selected from mineral or inorganic powders.

### Claim 3 (depends on 2)

The method of claim 2, wherein the powder (S) is selected from: metals, their salts and derivatives, chosen from oxides, hydroxides, phosphate salts, carbonate salts, borides, carbides, and nitrides; ceramics; and composite materials.

### Claim 4 (depends on 2)

Method according to claim 2, in which the mixture (1) of step (b) comprises at least one organic component.

### Claim 5 (depends on 2)

Method according to claim 2, in which the mixture (1) comprises 50 to 95% by weight of powder (S) with respect to the total weight of the mixture.

### Claim 6 (depends on 3)

The method of claim 3, wherein the powder (S) is selected from alkali and alkaline earth metals and transition metals.

### Claim 7 (depends on 1)

Method according to claim 1 in which the powder (S) is mineral or inorganic and is selected from: hydroxyapatite, alumina, titanium dioxide, zirconia, Yttria-Stabilized Zirconia (YSZ) and Magnesia Partially Stabilized Zirconia (PSZ).

### Claim 8 (depends on 7)

Method according to claim 7, in which the mixture (1) of step (b) comprises at least one organic component.

### Claim 9 (depends on 1)

Method according to claim 1, in which the mixture (1) of step (b) comprises at least one organic component.

### Claim 10 (depends on 9)

The method of claim 9, wherein the at least one organic component is selected from a group consisting of: a therapeutic active ingredient; peptides; proteins; coagulants; markers; growth factors; natural or synthetic polymers; dopants for electronics; electrically conductive polymers; chemical sensors; a cross-linking agent; and a water-miscible solvent.

### Claim 11 (depends on 1)

Method according to claim 1, in which the mixture (1) comprises 50 to 95% by weight of powder (S) with respect to the total weight of the mixture.

### Claim 12 (depends on 11)

The method of claim 11, wherein the powder (S) is mineral or inorganic powder.

### Claim 13 (depends on 1)

Method according to claim 1, in which step (d) comprises at least the following sub-steps:
(d1) Conditioning the sample at atmospheric pressure and at a temperature selected so that the solvent is in solid form,
(d2) Applying a pressure greater than or equal to 50 MPa at a temperature selected so that the solvent is in solid form.

### Claim 14 (depends on 13)

The method of claim 13, wherein the solvent is water.

### Claim 15 (depends on 1)

Method according to claim 1, in which step (d) comprises at least conditioning at a temperature of between −5° C. and −60° C. and at a pressure of between 50 MPa and 700 MPa.

### Claim 16 (depends on 1)

Method according to claim 1, in which the solvent is water and the removal of the water in step (g) is carried out by lyophilisation.

### Claim 17 (depends on 1)

The method of claim 1, wherein the at least one solvent is water.