Method for producing a shaped body and molding

Patent metadata

Field	Value
Publication number	US-10640426-B2
Application number	US-201615391238-A
Country	US
Kind code	B2
Filing date	Dec 27, 2016
Priority date	Dec 28, 2015
Publication date	May 5, 2020
Grant date	May 5, 2020

Abstract

The invention relates to a method for the production of a shaped body comprising at least the method steps of producing a blank having an open porosity by pressing and treating pourable material in a first heat treatment step comprising or consisting of a metal oxide, infiltrating the blank with an infiltration fluid containing a precursor of the metal oxide, precipitating hydroxide of the metal from the infiltration fluid by treating the blank with a basic solution, forming the metal oxide from the hydroxide by treating the blank in a second heat treatment step, wherein the blank is processed before or after the second heat treatment step to achieve a shape that corresponds to the shaped body.

First claim

The invention claimed is:

1. A method for production of a shaped body, comprising the steps of:
a) producing a blank having an open porosity through pressing and treatment of a pourable material in a first heat treatment step, the pourable material including a metal dioxide,
b) infiltrating the blank with an infiltration fluid, which includes a precursor of the metal dioxide,
c) precipitating a hydroxide of the metal dioxide from the infiltration fluid by treatment of the blank with a basic solution,
d) forming the metal dioxide from the hydroxide through treatment of the blank in a second heat treatment step, and
e) processing the blank before or after the second heat treatment step to achieve a shape corresponding to the shaped body.

2. The method according to claim 1 , wherein the second heat treatment step is carried out by sintering of the blank.

3. The method according to claim 1 , wherein the metal dioxide embedded in the blank at room temperature after the second heat treatment has a first stabilized crystal phase of at least 50%.

4. The method according to claim 3 , wherein the infiltration fluid is such that the metal dioxide formed from the hydroxide has a second crystal phase that differs from the stabilized first crystal phase.

5. The method according to claim 4 , wherein the crystals of the second crystal phase have a greater volume than the crystals of the first crystal phase.

6. The method according to claim 1 , wherein a tetragonal stabilized zirconium dioxide is used as the metal dioxide of the blank.

7. The method according to claim 1 , wherein the pourable material further includes at least one metal oxide powder being selected from the group consisting of Al 2 O 3 , TiO 2 , CeO 2 , MgO, Y 2 O 3 , and a zirconium dioxide mix crystal of the formula:
Zr 1-x Me x O 2(4n/2)x ,

wherein Me is a metal which in oxide form is present as a bivalent, trivalent or tetravalent cation (n=2, 3, 4 and 0≤x≤1) and stabilizes a tetragonal and/or cubic phase of the zirconium dioxide.

8. The method according to claim 1 , wherein the pourable material is one that includes at least one powder containing the metal dioxide as well as at least one organic binder selected from the group consisting of classes of polyvinylalcohols (PVA), polyacrylic acids (PAA), celluloses, polyethyleneglycols, thermoplasts and mixtures thereof.

9. The method according to claim 8 , wherein a binder with a percentage in the range 0.1 to 45 vol % is used.

10. The method according to claim 1 , wherein the pourable material used is one that includes a zirconium dioxide doped with yttrium oxide (Y 2 O 3 ), calcium oxide (CaO), magnesium oxide (MgO) and/or cerium oxide (CeO 2 ) and at room temperature the zirconium dioxide is stabilized in the cubic and/or tetragonal crystal form.

11. The method according to claim 1 , wherein the infiltration fluid is one in which the metal dioxide formed from the hydroxide after method step d) is monoclinic zirconium dioxide or includes monoclinic zirconium dioxide.

12. The method according to claim 1 , wherein a solution or a precursor is used as the infiltration fluid and includes deionized water and an oxychloride of zirconium.

13. The method according to claim 1 , wherein the infiltration fluid used for the step of infiltration has a dynamic viscosity η of 3.5 MPa·s≤η≤4.0 MPa·s.

14. The method according to claim 1 , wherein the blank is immersed in the infiltration fluid for a period of time t, where t>10 minutes.

15. The method according to claim 1 , wherein the blank is penetrated isotropically by the infiltration fluid.

16. The method according to claim 1 , wherein for the step of infiltration, the blank is arranged in a negative pressure atmosphere, is then immersed in the infiltration fluid at negative pressure, and is subsequently exposed to atmospheric pressure.

17. The method according to claim 1 , wherein after the step of infiltration, the blank is dried with the infiltration fluid.

18. The method according to claim 1 , wherein after the step of infiltrating, the blank is dried and then contacted with the basic solution.

19. The method according to claim 18 , wherein the basic solution is selected from the group consisting of a 45-55% NH 4 OH solution and a 15-25% NaOH solution.

20. The method according to claim 18 , wherein during the step of precipitating, the blank is contacted with the basic solution is at room temperature.

21. The method according to claim 18 , wherein during the step of precipitating, the blank is contacted with the basic solution for a period of time t where t≥10 minutes.

22. The method according to claim 18 , wherein after the step of infiltration, the blank is dried.

23. The method according to claim 22 , wherein after drying of the blank from the precipitating step, the blank is completely sintered, end-sintered or over-sintered.

24. The method according to claim 23 , wherein over-sintering is at a temperature that is 5-15% higher than a temperature at which the blank is completely sintered or end-sintered.

Assignees

• Dentsply Sirona Inc

Inventors

• Wondraczek Lothar
• Muller Lenka

Classifications

• C04B35/48

  based on zirconium or hafnium oxides, zirconates, {zircon} or hafnates · CPC title

• C04B2235/3225

  Yttrium oxide or oxide-forming salts thereof · CPC title

• C04B2235/3206

  Magnesium oxides or oxide-forming salts thereof · CPC title

• C04B35/645

  Pressure sintering · CPC title

• C04B2235/3229

  Cerium oxides or oxide-forming salts thereof · CPC title