Method for producing a porous monolithic material

Patent metadata

Field	Value
Publication number	US-10500313-B2
Application number	US-201615743492-A
Country	US
Kind code	B2
Filing date	Jul 15, 2016
Priority date	Jul 17, 2015
Publication date	Dec 10, 2019
Grant date	Dec 10, 2019

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.

First claim

The invention claimed is:

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.

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

3. 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.

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

5. 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.

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

7. 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).

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

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

10. 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.

11. 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.

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

13. 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.

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

15. 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.

16. 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.

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

Assignees

• Centre Nat Rech Scient
• Univ Bordeaux

Inventors

• Largeteau Alain
• Prakasam Mythili

Classifications

• C04B30/00

  Compositions for artificial stone, not containing binders · CPC title

• C04B2111/00844

  for electronic applications · CPC title

• C04B2111/00836

  for medical or dental applications · CPC title

• C04B2111/0081

  as catalysts or catalyst carriers · CPC title

• C01G25/006

  Compounds containing zirconium, with or without oxygen or hydrogen, and containing two or more other elements · CPC title