Method for preparing a material made from aluminosilicate and method for preparing a composite material having an aluminosilicate matrix

Patent metadata

Field	Value
Publication number	US-10717656-B2
Application number	US-201615545027-A
Country	US
Kind code	B2
Filing date	Jan 21, 2016
Priority date	Jan 23, 2015
Publication date	Jul 21, 2020
Grant date	Jul 21, 2020

Abstract

The invention relates to a method for preparing a material based on an aluminosilicate selected from barium aluminosilicate BAS, barium-strontium aluminosilicate BSAS, and strontium aluminosilicate SAS, said aluminosilicate consisting of aluminosilicate with a hexagonal structure, characterised in that it includes a single sintering step in which a mixture of powders of precursors of said aluminosilicate, including an aluminium hydroxide Al(OH) 3 powder, are sintered by a hot-sintering technique with a pulsed electric field SPS; whereby a material based on an aluminosilicate, said aluminosilicate consisting of an aluminosilicate with a hexagonal structure is obtained. The material based on an aluminosilicate prepared by said method can be used in a method for preparing a composite material consisting of an aluminosilicate matrix reinforced by reinforcements made of metalloid or metal oxide.

First claim

The invention claimed is:

1. A method for preparing a material based on an aluminosilicate selected from among barium aluminosilicate BAS, barium and strontium aluminosilicate BSAS, and strontium aluminosilicate SAS, said aluminosilicate consisting of aluminosilicate with a hexagonal structure, the method comprising a single sintering step wherein the sintering of a mixture of powders of precursors of said aluminosilicate, comprising an aluminum hydroxide powder Al(OH) 3 is carried out, by a hot sintering technique with a pulsed electric field SPS; whereby a material based on an aluminosilicate, said aluminosilicate consisting of aluminosilicate with a hexagonal structure, is obtained.

2. The method according to claim 1 , wherein the powders of precursors other than the aluminium hydroxide powder Al(OH) 3 are selected from the group consisting of powders of barium carbonate BaCO 3 , powders of silica SiO 2 , and powders of strontium carbonate.

3. The method according to claim 2 , wherein the aluminosilicate is barium aluminosilicate BAS, and the mixture of the powders of precursors comprises a mixture of a barium carbonate BaCO 3 powder, of a silica powder SiO 2 , and of an aluminium hydroxide Al(OH) 3 powder.

4. The method according to claim 3 , wherein the molar ratio of the barium carbonate BaCO 3 , of the silica powder SiO 2 , and of the aluminium hydroxide Al(OH) 3 powder in the mixture of the powders of precursors is 1 mole of BaCO 3 for 2 moles of silica SiO 2 and 2 moles of aluminium hydroxide Al(OH) 3 .

5. The method according to claim 1 , wherein the mixture of the powders of precursors is prepared by suspending the powders in a solvent, by homogenizing the suspension, and by drying the suspension.

6. The method according to claim 5 , wherein the solvent is selected from among alcohols; water; and mixtures thereof.

7. The method according to claim 6 , wherein the solvent is water at a basic pH.

8. A method according to claim 7 , wherein the water at a basic pH contains a base.

9. The method according to claim 8 , wherein the base is ammonia.

10. The method according to claim 7 , wherein the pH of the water is from 10 to 12.

11. The method according to claim 6 , wherein the solvent is water at an acid pH.

12. The method according to claim 11 , wherein the pH of the water is 4.

13. The method according to claim 6 , wherein the solvent is selected from the group consisting of aliphatic alcohols of 1 to 10 C.

14. The method according to claim 1 , wherein, during sintering, a first plateau is observed at a first temperature for removing water contained in the aluminium hydroxide Al(OH) 3 , a second optional plateau is observed at a second temperature for forming intermediate compounds, and a third plateau is observed at a third temperature for forming the aluminosilicate.

15. The method according to claim 14 , wherein:
the first plateau is carried out at a temperature from 900° C. to 1,000° C. for a duration from 1 to 5 minutes;
the second plateau is carried out at a temperature from 1,100° C. to 1,200° C. for a duration from 0 to 20 minutes;
the third plateau is carried out at a temperature from 1,200° C. to 1,700° C. for a duration from 1 to 20 minutes.

16. The method according to claim 1 , wherein the material based on an aluminosilicate is dense, homogeneous, and non-cracked.

17. The method according to claim 1 , which further comprises a step during which the material based on an aluminosilicate, consisting of aluminosilicate with a hexagonal structure, is heat-treated for transforming the aluminosilicate with a hexagonal structure into an aluminosilicate with an orthorhombic structure, or to an aluminosilicate with a monoclinic structure.

18. A method for preparing a composite material, consisting of a matrix made of at least one aluminosilicate, reinforced with reinforcements made of at least a metal oxide or metalloid oxide for which the thermal expansion coefficient is within 10% of the thermal expansion coefficient of said at least one aluminosilicate, wherein the following successive steps are carried out:
a) a material based on an aluminosilicate is prepared by the method according to claim 1 , and a powder of said material based on an aluminosilicate is prepared;
b) the powder of the material based on an aluminosilicate is put into contact with reinforcements made of least one metal oxide or metalloid oxide, for which the thermal expansion coefficient is within 10% of the thermal expansion coefficient of the at least one aluminosilicate;
c) sintering of the powder of the material based on an aluminosilicate and of the reinforcements made of at least one metal oxide or metalloid oxide is achieved by a hot sintering method with a pulsed electric field;
d) the sintered powder and reinforcements are cooled;
e) the composite material is recovered.

19. The method according to claim 18 , wherein the aluminosilicate is barium aluminosilicate BAS.

20. The method according to claim 18 wherein the reinforcements are made of alumina.

21. The method according to claim 18 , wherein the reinforcements made of at least one metal oxide or metalloid oxide appear in one or several form(s) selected from among particles; and fiber fabrics.

22. The method according to claim 21 , wherein during step b) a mixture of the powder of the material based on the aluminosilicate and of particles made of at least one metal oxide or metalloid oxide is prepared.

23. The method according to claim 21 , wherein during step b) a fiber fabric made of the at least one metal oxide or metalloid oxide is impregnated with a slurry of the powder of the material based on the aluminosilicate.

24. A method for preparing a composite material, consisting of a matrix made of at least one aluminosilicate, reinforced with reinforcements made of at least a metal oxide or metalloid oxide for which the thermal expansion coefficient is within 10% of the thermal expansion coefficient of said at least one aluminosilicate, wherein the following successive steps are carried out:
a) a material based on an aluminosilicate is prepared by the method according to claim 17 , and a powder of said material based on an aluminosilicate is prepared;
b) the powder of the material based on an aluminosilicate is put into contact with reinforcements made of least one metal oxide or metalloid oxide, for which the thermal expansion coefficient is within 10% of the thermal expansion coefficient of the at least one aluminosilicate;
c) sintering of the powder of the material based on an aluminosilicate and of the reinforcements made of at least one metal oxide or metalloid oxide is achieved by a hot sintering method with a pulsed electric field;
d) the sintered powder and reinforcements are cooled;
e) the composite material is recovered.

25. The method according to claim 24 , wherein the aluminosilicate is barium aluminosilicate BAS.

26. The method according to claim 24 , wherein the aluminosilicate consists of an aluminosilicate of monoclinic structure and wherein the reinforcements are made of silica and/or mullite.

27. The method according to claim 24 , wherein the reinforcements made of at least one metal oxide or metalloid oxide appear in one or several form(s) selected from among particles; and fiber fabrics.

28. The method according to claim 27 , wherein during step b) a mixture of the powder of th

Assignees

• Commissariat Energie Atomique
• Centre Nat Rech Scient
• Commissariat Alenergie Atomique Et Aux Energies Alternatives

Inventors

• Allemand Alexandre
• Belleville Philippe
• Le Petitcorps Yann
• Billard Romain
• Dolle Mickael

Classifications

• C04B35/80

  Fibres, filaments, whiskers, platelets, or the like · CPC title

• C04B2235/6562

  Heating rate · CPC title

• C04B2235/76

  Crystal structural characteristics, e.g. symmetry · CPC title

• C04B2235/6565

  Cooling rate · CPC title

• C04B35/62625

  Wet mixtures · CPC title