Alumina-based opaque ceramic

Patent metadata

Field	Value
Publication number	US-8993466-B2
Application number	US-201113637846-A
Country	US
Kind code	B2
Filing date	Apr 1, 2011
Priority date	Apr 1, 2010
Publication date	Mar 31, 2015
Grant date	Mar 31, 2015

Abstract

The invention relates to an alumina-based opaque ceramic, similar to ruby and having a high toughness. This ceramic comprises, by weight: 0.4% to 5% of at least from one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron; 0.00080 to 0.5% of magnesium oxide; and 0.05 to 6% of at least one oxide of an element of the group of rare earths. The ceramic is applicable in particular in jewelry, fine jewelry and watch making. The invention also relates to methods of preparing such a ceramic.

First claim

The invention claimed is:

1. An alumina-based opaque ceramic comprising, by weight:
from 0.4% to 5% of at least one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron;
from 0.00080% to 0.5% of magnesium oxide; and
from 0.05% to 6% of at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide.

2. The alumina-based opaque ceramic as claimed in claim 1 , comprising, by weight:
more than 2% of at least one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron;
from 0.00083% to 0.5% of magnesium oxide; and
from 0.1% to 5% of at least one oxide of an element from the group of rare earths.

3. An alumina-based opaque ceramic as claimed in claim 1 , which is obtained by a process wherein:
a) a mixture is prepared comprising, in percentages by weight:
from 0.4% to 5% of at least one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron;
from 0.00080% to 0.5% of magnesium oxide;
from 0.05% to 6% of at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide; and
the balance to 100% of alumina;
to which are added organic additives enabling the forming and at least one liquid;

b) the mixture obtained in step a) is milled;
c) the mixture obtained in step b) is spray-dried;
d) the spray-dried mixture obtained in step c) is then formed;
e) the product obtained in step d) is subjected to one or more heat treatments;
and wherein the heat treatment or, where appropriate, the last heat treatment is carried out under a pressure of less than 10 bar.

4. The alumina-based opaque ceramic as claimed in claim 3 , the heat treatment or, where appropriate, the last heat treatment being carried out in an atmosphere of an oxygen-containing gas.

5. An alumina-based opaque ceramic as claimed in claim 1 , which is obtained by a process wherein:
a) a mixture is prepared comprising, in percentages by weight:
from 0.4% to 5% of at least one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron;
from 0.00080% to 0.5% of magnesium oxide; and
from 0.05% to 6% of at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide; and
the balance to 100% of alumina;
to which are added organic additives enabling the forming and at least one liquid;

b) the mixture obtained in step a) is milled;
c) the mixture obtained in step b) is spray-dried;
d) the spray-dried mixture obtained in step c) is then formed; and
e) the product obtained in step d) is subjected to at least one heat treatment under a pressure of less than 10 bar,
and wherein the product obtained in step e) is left to cool in order to obtain the alumina-based opaque ceramic.

6. The alumina-based opaque ceramic as claimed in claim 3 , wherein, in step a) of said process, the mixture comprises, in percentages by weight:
more than 2% of at least one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron;
from 0.00083% to 0.5% of magnesium oxide;
from 0.1% to 5% of at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide; and
the balance to 100% of alumina.

7. The alumina-based opaque ceramic as claimed in claim 3 , wherein, in step a) of the process, the oxide of the element from the group of rare earths is heated in the presence of concentrated nitric acid until the oxide is completely dissolved to form a solution and the solution is left to cool before adding it to said mixture.

8. The alumina-based opaque ceramic as claimed in claim 3 , wherein, in step (e) of the process, the heat treatment takes place at a temperature between 1640 and 1690° C.

9. The alumina-based opaque ceramic as claimed in claim 8 , wherein the temperature of the heat treatment is between 1645 and 1680° C.

10. The alumina-based opaque ceramic as claimed in claim 9 , wherein the temperature of the heat treatment is between 1650 and 1675° C.

11. The alumina-based opaque ceramic as claimed in claim 1 , comprising between 0.5% and 2.5% by weight of at least one oxide of an element from the rare earths.

12. The alumina-based opaque ceramic as claimed in claim 1 , comprising two oxides of elements from the rare earths, one of which is erbium oxide, and another of which is an yttrium oxide wherein said yttrium oxide is present in a proportion of from 0.012% to 0.26% by weight.

13. The alumina-based opaque ceramic as claimed in claim 1 , wherein the alumina-based opaque ceramic is free of silicon.

14. A process for preparing a ceramic as claimed in claim 1 , comprising a step during which at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide, is added to a mixture of alumina, magnesium oxide and at least one oxide of at least one metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron, so as to obtain the ceramic as claimed in claim 1 .

15. The process as claimed in claim 14 , wherein the oxide of the element from the group of rare earths is heated in the presence of concentrated nitric acid until the oxide is completely dissolved to form a solution and the solution is left to cool before adding it to said mixture.

16. The process as claimed in claim 15 , comprising, in addition, a step of sintering between 1640 and 1690° C.

17. The process as claimed in claim 16 , wherein the sintering temperature is between 1645 and 1680° C.

18. The process as claimed in claim 17 , wherein the sintering temperature is between 1650 and 1675° C.

19. The process as claimed in claim 16 , wherein the sintering is carried out under a pressure of less than 10 bar of an oxygen-containing gas.

20. The ceramic as claimed in claim 3 , wherein, in step a) of the process, the mixture is prepared from:
at least one compound capable of being converted by heating into an amount of from 0.4% to 5% of at least one oxide of a metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron;
at least one compound capable of being converted by heating into an amount of from 0.00080% to 0.5% of magnesium oxide;
at least one compound capable of being converted by heating into an amount of from 0.05% to 6% of at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide; and
the balance to 100% of alumina;
and also organic additives enabling the forming and at least one liquid.

21. A process for preparing a ceramic as claimed in claim 11 , comprising a step during which at least one oxide of an element from the group of rare earths, wherein the at least one oxide of the element from the group of the rare earths is an erbium oxide, is added to a mixture of alumina, magnesium oxide and at least one oxide of at least one metal chosen from chromium, cobalt, nickel, manganese, vanadium, titanium and iron, so as to obtain the ceramic.

22. The ceramic as claimed in claim 5 , wherein, in step a) of the process, the mixture is prepared f

Assignees

• Pujol Ollivier
• Rigot Isabelle
• Rolex Sa

Inventors

• Pujol Ollivier
• Rigot Isabelle

Classifications

• C04B2235/3279

  Nickel oxides, nickalates, or oxide-forming salts thereof · CPC title

• C04B2235/3225

  Yttrium oxide or oxide-forming salts thereof · CPC title

• C04B2235/6582

  Hydrogen containing atmosphere · CPC title

• C04B2235/3272

  Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite · CPC title

• C04B35/111 Primary

  Fine ceramics · CPC title