IP Library Granted Patent US 12,558,203
Granted Patent B2
US 12,558,203 · App. 17/753,195 · Granted Feb 24, 2026

Dental mill blank of a porous zirconia material containing oxides of Tb, Er and Cr, process of producing and use thereof

Inventors: Michael Jahns (Gilching, DE); Gallus Schechner (Herrsching, DE)
Assignee: Solventum Intellectual Properties Company
A61C13/0022A61C5/77A61K6/78A61K6/818A61K6/822C04B35/486C04B2111/00836C04B2235/3244C04B2235/6562C04B2235/6567C04B2235/9653
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Quick Facts
Patent No.
US 12,558,203
App. No.
17/753,195
Granted
Feb 24, 2026
Kind
B2
Abstract

The present invention relates to a dental zirconia mill blank comprising a porous zirconia material, the porous zirconia material comprising Zr oxide, Y oxide, optionally Al oxide, Bi oxide, Tb oxide, Er oxide, Cr oxide, the porous zirconia material not comprising Fe oxide calculated as Fe 2 O 3 of more than 0.01 wt. %, Mn oxide calculated as MnO 2 of more than 0.005 wt. %, Co oxide calculated as Co 2 O 3 of more than 0.005 wt. %, wt. % with respect to the weight of the porous zirconia material. The invention also relates to a process of producing such a dental zirconia mill blank and a dental restoration which can be machined from the dental zirconia mill blank. Further, the invention relates to a kit of parts comprising such a dental zirconia mill blank and a dental cement.

Claims (80)

1 . A process of producing a dental mill blank comprising a porous zirconia material,

the porous zirconia material comprising Zr oxide, and Y oxide calculated as Y 2 O 3 : 13 to 15 wt. %,

the porous zirconia material not comprising

Fe oxide calculated as Fe 2 O 3 of more than 0.01 wt. %,

Mn oxide calculated as MnO 2 of more than 0.005 wt. %, or

Co oxide calculated as Co 2 O 3 of more than 0.005 wt. %,

the wt. % is calculated with respect to the weight of the porous zirconia material,

wherein the porous zirconia material is further characterized by a biaxial flexural strength of greater than 40 MPa to 80 MPa,

the process comprising the steps of

providing a first zirconia powder comprising Tb oxide,

providing a second zirconia powder comprising Er oxide in an amount of 0.5 to 12.0 wt. %,

mixing and layering a plurality of zirconia powders including the first zirconia powder and the second zirconia powder,

compacting the layered and mixed zirconia powders to provide a compacted zirconia mixture, and

sintering the compacted zirconia mixture to produce the dental mill blank.

2 . The process of claim 1 , wherein the porous zirconia material does not comprise at least one of the following components:

oxide(s) selected from Dy, Sm, Nd, Eu, Cu, V, Mo, Ni, each in an amount above 0.01 wt. %,

glass in an amount above 1 wt. %,

glass ceramic in an amount above 1 wt. %,

lithium (di) silicate ceramic in an amount above 1 wt. %, or

combinations thereof,

the wt. % is calculated with respect to the weight of the porous zirconia material.

3 . The process of claim 1 , wherein the porous zirconia material is characterized by the following features alone or in combination:

(a) average grain size: less than 100 nm;

(b) average connected pore diameter: 10 to 100 nm;

(c) BET surface: 2 to 20 m 2 /g; or

(d) Vickers hardness: 25 (HV 0.5) to 150 (HV 1).

4 . The process of claim 1 , wherein the porous zirconia material further comprises the respective oxides in the following amounts:

Zr oxide calculated as ZrO 2 : 80 to 96 wt. %,

Y oxide calculated as Y 2 O 3 : 14 to 15 wt. %,

Al oxide calculated as Al 2 O 3 : 0 to 0.15 wt. %,

Bi oxide calculated as Bi 2 O 3 : 0.01 to 0.2 wt. %,

Tb oxide calculated as Tb 4 O 7 : 0.01 to 0.8 wt. %,

Er oxide calculated as Er 2 O 3 : 0.01 to 3.0 wt. %, and

Cr oxide calculated as Cr 2 O 3 : 0.0001 to 0.1 wt. %,

the wt. % is calculated with respect to the weight of the porous zirconia material.

5 . The process of claim 1 , wherein the dental mill blank is characterized by the following features alone or in combination:

shape: cubic, cuboid, cylindric, disc-shaped;

size:

for cubic or cuboid shaped blanks: more than 19 mm in 2 dimensions, more than 12 mm in a particular dimension; or

for cylindric or disc shaped blanks: more than 19 mm in diameter, more than 12 mm in height; or

comprising means for attaching the dental mill blank to a machining device.

6 . The process of claim 1 , wherein the dental mill blank is characterized as follows:

having a shape of a cube, rectangular prism, cylinder or disc, and

comprising means for attaching the dental mill blank to a machining device,

the porous zirconia material being characterized as follows:

BET surface: 2 to 20 m 2 /g;

biaxial flexural strength: 8 to 80 MPa;

x, y dimension: at least 19 mm;

z dimension: at least 12 mm; or

Density: 30 to 95% of theoretical density;

the porous zirconia material comprising:

Zr oxide calculated as ZrO 2 : 80 to 96 wt. %,

Al oxide calculated as Al 2 O 3 : 0 to 0.15 wt. %,

Y oxide calculated as Y 2 O 3 : 14 to 15 wt. %,

Bi oxide calculated as Bi 2 O 3 : 0.01 to 0.2 wt. %,

Tb oxide calculated as Tb 4 O 7 : 0.01 to 0.8 wt. %,

Er oxide calculated as Er 2 O 3 : 0.2 to 1.2 wt. %, and

Cr oxide calculated as Cr 2 O 3 : 0.0005 to 0.006 wt. %,

the porous zirconia material not comprising:

Fe oxide calculated as Fe 2 O 3 in an amount of more than 0.01 wt. %,

Mn oxide calculated as MnO 2 in an amount of more than 0.005 wt. %,

Co oxide calculated as Co 2 O 3 in an amount of more than 0.005 wt. %, or

a glass, glass ceramic or lithium disilicate material above 1 wt. %,

the wt. % is calculated with respect to the weight of the porous zirconia material.

7 . A process of producing a dental restoration, the process comprising the steps of:

providing a dental mill blank obtained by the process of claim 1 ,

machining the dental restoration out of the porous zirconia material of the dental mill blank, and

sintering the dental restoration.

8 . The process of producing a dental restoration according to claim 7 , the sintering being done by applying either of the following heat-treatment steps:

sintering step comprising a heating rate of 1 to 60° C./min; and

sintering step comprising a heating rate of 1.5 to 7° C./sec.

9 . The process of producing a dental restoration according to claim 7 , the sintering of the dental restoration being done by applying the following conditions:

heating rate in a range of 2 to 7° C./sec;

sintering temperature of at least 1,500° C.; and

duration of less than 60 min.

10 . The process of claim 1 , wherein none of the zirconia powders or the dental mill blank comprise:

Fe oxide calculated as Fe 2 O 3 in an amount of more than 0.01 wt. %,

Mn oxide calculated as MnO 2 in an amount of more than 0.005 wt. %, or

Co oxide calculated as Co 2 O 3 in an amount of more than 0.005 wt. %.

11 . The process of claim 1 , wherein the porous zirconia material comprises an average grain size of less than 100 nm.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 1, 2024
From: 3M INNOVATIVE PROPERTIES COMPANY
To: SOLVENTUM INTELLECTUAL PROPERTIES COMPANY
Reel/Frame 066430/0149 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 23, 2022
From: JAHNS, MICHAEL; SCHECHNER, GALLUS
To: 3M INNOVATIVE PROPERTIES COMPANY
Reel/Frame 059078/0527 →
Continuity (1)
Related Publication 20220273404A1 · Sep 1, 2022
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