Multi-layered zirconia dental mill blank and process of production

Patent metadata

Field	Value
Publication number	US-10898302-B2
Application number	US-201716095433-A
Country	US
Kind code	B2
Filing date	Oct 21, 2017
Priority date	Apr 25, 2016
Publication date	Jan 26, 2021
Grant date	Jan 26, 2021

Abstract

The invention relates to a porous multi-layered coloured zirconia dental mill blank comprising a bottom layer B having the composition COMP-B which comprises ceramic components CER-COMP-B, colouring components COL-COMP-B and stabilizing components STAB-COMP-B, a top layer E having the composition COMP-E which comprises ceramic components CER-COMP-E, colouring components COL-COMP-E stabilizing components STAB-COMP-E, at least one intermediate layer Ex having the composition COMP-E of top layer E, at least one intermediate layer Bx having the composition COMP-B of bottom layer B, x being an integer and indicating the number of intermediate layers, wherein the layers with compositions COMP-B and COMP-E are arranged in alternating order, and wherein the thickness of the individual layers B, Bx is decreasing from bottom to top and the thickness of the individual layers E, Ex is decreasing from top to bottom. The dental mill blank can be used for producing dental articles.

First claim

The invention claimed is:

1. A porous multi-layered coloured zirconia dental mill blank, comprising:
a bottom layer B comprising:
a composition COMP-B comprising:
ceramic components CER-COMP-B,
colouring components COL-COMP-B, and
stabilizing components STAB-COMP-B;

a top layer E comprising:
a composition COMP-E comprising:
ceramic components CER-COMP-E,
colouring components COL-COMP-E, and
stabilizing components STAB-COMP-E,

wherein one or more of CER-COMP-B and CER-COMP-E comprises zirconia;

at least one intermediate layer E x comprising the composition COMP-E; and
at least one intermediate layer B x comprising the composition COMP-B;
wherein the layers with compositions COMP-B and COMP-E are arranged top to bottom in an alternating order, and
wherein each of the layers B and B x have a thickness, wherein the thickness increases from top to bottom, and
wherein each of the layers E and E x have a thickness, wherein the thickness decreases from top to bottom.

2. The mill blank of claim 1 not comprising layers having a composition other than COMP-B or COMP-E.

3. The mill blank of claim 1 , the difference in colour intensity expressed as colour space value ΔE E,B for composition COMP-B and COMP-E being below 10.

4. The mill blank of claim 1 , the thickness of the layers being as follows:
bottom layer B: from 7 to 24 mm;
top layer E: from 5 to 10 mm;
intermediate layer E x : from 0.6 to 4 mm; and
intermediate layer B x : from 0.6 to 4 mm.

5. The mill blank of claim 1 , being characterized by at least one or more of the following features:
raw breaking resistance: 20 to 70 MPa determined according to ISO 6872:2015 applying the punch on 3 balls test adapted to measurement in porous state;
porosity: 30 to 70%;
average connected pore diameter: 0.010 to 0.190 μm;
density: from 2 to 4 g/cm 3 .

6. The mill blank of claim 1 , at least one of the compositions COMP-B or COMP-E comprising a fluorescing agent.

7. The mill blank of claim 1 , both compositions COMP-B and COMP-E comprising a fluorescing agent, the concentration of the fluorescing agent in composition COMP-B being preferably higher than the concentration of the fluorescing agent in composition COMP-E.

8. The mill blank of claim 1 , the ceramic components being present in an amount from 80 to 95 wt. % with respect to the weight of the mill blank.

9. The mill blank of claim 1 , the colouring components being present in an amount from 0.01 to 1 wt. % with respect to the weight of the mill blank.

10. The mill blank of claim 1 , the stabilizing components being present in an amount from 3 to 12 wt. % with respect to the weight of the mill blank.

11. The mill blank of claim 1 , comprising
a bottom layer B having the composition COMP-B which comprises ceramic components CER-COMP-B, colouring components COL-COMP-B and stabilizing components STAB-COMP-B;
a top layer E having the composition COMP-E which comprises ceramic components CER-COMP-E, colouring components COL-COMP-E stabilizing components STAB-COMP-E;
at least one intermediate layer E x having the composition of top layer E;
at least one intermediate layer B x having the composition of bottom layer B,
the layers with compositions COMP-B and COMP-E being arranged in alternating order,
the thickness of the individual layers B, B x decreasing from bottom to top,
the thickness of the individual layers E, E x decreasing from top to bottom;
the ceramic components of CER-COMP-E and CER-COMP-B being selected from oxides of Zr, Hf, Al and mixtures thereof;
the stabilizing components of STAB-COMP-B and STAB-COMP-E being selected from oxides of Y, Mg, Ca, Ce and mixtures thereof;
the colouring components of COL-COMP-B and COL-COMP-E being selected from the oxides of Mn, Er, Tb and mixtures thereof;
at least one of the chemical compositions COMP-B or COMP-E comprising a fluorescing agent; and
the ceramic components, stabilizing components and optionally the colouring components contained in all the layers being the same.

12. A process of producing a mill blank as described in claim 1 , the process comprising:
layering compositions COMP-B and COMP-E in alternating order one above the other;
applying pressure; and
conducting a heat treatment step.

13. A process for producing a dental article, the process:
providing a mill blank as described in claim 1 ;
machining an item out of the mill blank, the item having the shape of a dental article; and
conducting a sintering step to obtain a sintered dental article.

14. A dental article obtained by a process as described in claim 13 .

Assignees

• 3M Innovative Properties Co

Inventors

• Dittmann Rainer K
• Schnagl Hans R
• Kindler Grit
• Theelke Björn
• Sogl Michael
• Urban Michaela

Classifications

• C04B2237/348

  Zirconia, hafnia, zirconates or hafnates · CPC title

• C04B2235/9661

  Colour · CPC title

• C04B2235/668

  Pressureless sintering · CPC title

• C04B2235/608

  Green bodies or pre-forms with well-defined density · CPC title

• C04B2235/604

  Pressing at temperatures other than sintering temperatures · CPC title