# US 8,541,329 B2 · Process for the preparation of coloured blanks and dental shaped parts

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- Number: US 8,541,329 B2
- Document ID: US8541329B2
- Status: Granted
- Kind: B2
- Application number: 13/224,492
- Filed: 2011-09-02
- Published: 2011-12-29
- Granted: 2013-09-24
- Earliest claimed: 2006-05-23
- Assignees: Ivoclar Vivadent AG
- Applicants: Christian Ritzberger; Elke Apel; Wolfram Höland; Frank Rothbrust; Harald Kerschbaumer; Volker Rheinberger
- Inventors: Christian Ritzberger; Elke Apel; Wolfram Höland; Frank Rothbrust; Harald Kerschbaumer; Volker Rheinberger
- Web page: https://patentgrep.com/patent/US8541329B2

## CPC

- A61C 13/0022: {Blanks or green, unfinished dental restoration parts}
- A61C 5/77: Methods or devices for making crowns
- A61K 6/804: comprising manganese oxide
- A61K 6/813: comprising iron oxide
- A61K 6/818: comprising zirconium oxide
- A61K 6/822: comprising rare earth metal oxides
- A61K 6/833: Glass-ceramic composites
- C04B 35/486: Fine ceramics
- C04B 35/488: Composites
- C04B 35/6225: {Fibres based on zirconium oxide, e.g. zirconates such as PZT}
- C04B 35/62665: {Flame, plasma or melting treatment}
- C04B 35/62805: {Oxide ceramics}
- C04B 35/62815: {Rare earth metal oxides}
- C04B 35/62826: {Iron group metal oxides}
- C04B 2235/3217: Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B 2235/3224: Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B 2235/3225: Yttrium oxide or oxide-forming salts thereof
- C04B 2235/3241: Chromium oxides, chromates, or oxide-forming salts thereof
- C04B 2235/3244: Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B 2235/3246: Stabilised zirconias, e.g. YSZ or cerium stabilised zirconia
- C04B 2235/3262: Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
- C04B 2235/3265: Mn2O3
- C04B 2235/3272: Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
- C04B 2235/443: Nitrates or nitrites
- C04B 2235/444: Halide containing anions, e.g. bromide, iodate, chlorite
- C04B 2235/5409: expressed by specific surface values
- C04B 2235/6026: Computer aided shaping, e.g. rapid prototyping
- C04B 2235/604: Pressing at temperatures other than sintering temperatures
- C04B 2235/6567: Treatment time
- C04B 2235/661: Multi-step sintering
- C04B 2235/72: Products characterised by the absence or the low content of specific components, e.g. alkali metal free alumina ceramics
- C04B 2235/785: Submicron sized grains, i.e. from 0,1 to 1 micron
- C04B 2235/95: Products characterised by their size, e.g. microceramics
- C04B 2235/9653: Translucent or transparent ceramics other than alumina
- C04B 2235/9661: Colour
- A61C: DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE (non-driven toothbrushes A46B; {tongue scrapers A61B17/24;} preparations for dentistry A61K6/00; preparations for cleaning the teeth or mouth A61K8/00, A61Q11/00)
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE

## Abstract

The invention relates to compositions based on ZrO2, and single- and multi-coloured blanks made from oxide ceramics, and a process for their preparation, in which a) oxide ceramic powder is coated with a colouring substance, b) the coated powders are preferably graded and at least one coloured powder is filled into a compression mould, c) the coloured powder or powders are compressed to produce a shaped body, and d) the compressed shaped body is sintered to produce a blank, and to the use of these blanks for the preparation of dental restorations.

## Claims

### Claim 1

A composition comprising ZrO2, the composition further comprising the following components in wt.-%:
Pr, calculated as Pr2O3
0.001-0.003
Fe, calculated as Fe2O3
0.005-0.04
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0001-0.0005.

### Claim 2

A composition comprising ZrO2, the composition further comprising the following components in wt.-%:
Pr, calculated as Pr2O3
0.002-0.004
Fe, calculated as Fe2O3
0.04-0.15
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0003-0.002.

### Claim 3

A composition comprising ZrO2, the composition further comprising the following components in wt.-%:
Pr, calculated as Pr2O3
0.003-0.006
Fe, calculated as Fe2O3
0.04-0.15
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0005-0.002.

### Claim 4

A composition comprising ZrO2, the composition further comprising the following components in wt.-%:
Pr, calculated as Pr2O3
0.003-0.006
Fe, calculated as Fe2O3
0.04-0.25
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.001-0.007.

### Claim 5

A multi-colored shaped body comprising a composition comprising ZrO2 and further comprising the following components:
Pr, calculated as Pr2O3,
Fe, calculated as Fe2O3,
Tb, calculated as Tb2O3, and
Mn, calculated as Mn2O3,
in a total quantity of 0.0001 to 0.75 wt.-%,
wherein the multi-coloration is produced by differently colored layers.

### Claim 6 (depends on 5)

The shaped body according to claim 5, wherein said composition comprises
Tb, calculated as Tb2O3, in a quantity of 0.0001 to 0.075 wt.-% and.

### Claim 7 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises the components in a total quantity of 0.0001 to 0.6 wt.-%.

### Claim 8 (depends on 7)

The shaped body according to claim 7, wherein said composition comprises the components in a total quantity of 0.0004 to 0.37 wt.-%.

### Claim 9 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises the components in the following quantities, in wt.-%:
Pr, calculated as Pr2O3
0.0001-0.01
Fe, calculated as Fe2O3
0.005-0.5
Tb, calculated as Tb2O3
0.0001-0.1
Mn, calculated as Mn2O3
0.0001-0.1.

### Claim 10 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises Pr, calculated as Pr2O3, in a quantity of 0.0005 to 0.01 wt.-%.

### Claim 11 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises Fe, calculated as Fe2O3, in a quantity of 0.0005 to 0.4 wt.-%.

### Claim 12 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises Fe, calculated as Mn2O3, in a quantity of 0.0001 to 0.075 wt.-%.

### Claim 13 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises 4 to 8 wt.-% Y2O3.

### Claim 14 (depends on 6)

The shaped body according to claim 6, wherein said composition comprises up to 1 wt.-% Al2O3.

### Claim 15 (depends on 6)

The shaped body according to claim 6, wherein said composition is a powder composition and comprises 98.0 to 99.9999 wt.-% of nanoscale ZrO2 powder.

### Claim 16 (depends on 15)

The shaped body according to claim 15, wherein the nanoscale ZrO2 powder has a specific surface area of ≧100 m2*g-1.

### Claim 17 (depends on 15)

The shaped body according to claim 15, wherein the nanoscale ZrO2 powder has a primary particle size between 5 and 50 nm.

### Claim 18 (depends on 6)

The shaped body according to claim 6, wherein said composition is obtainable by a process in which a powder based on ZrO2 is coated with compounds of Pr, Tb, Fe and/or Mn.

### Claim 19 (depends on 18)

The shaped body according to claim 18, wherein the powder is coated by means of fluidized bed coating.

### Claim 20 (depends on 6)

The shaped body according to claim 6, wherein the shaped body is in the form of a blank, dental shaped part or dental restoration.

### Claim 21 (depends on 6)

The shaped body according to claim 6, wherein the shaped body comprises at least 2 differently colored layers.

### Claim 22 (depends on 21)

The shaped body according to claim 21, wherein the shaped body comprises up to 8 differently colored layers.

### Claim 23 (depends on 1, 21)

The shaped body according to claim 21, wherein at least one layer has the composition according to claim 1.

### Claim 24 (depends on 21)

The shaped body according to claim 21, wherein at least one layer has a composition comprising ZrO2, the composition further comprising the following components in wt.-%:
Pr, calculated as Pr2O3
0.001-0.003
Fe, calculated as Fe2O3
0.005-0.04
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0001-0.0005.

### Claim 25 (depends on 21)

A dental restoration comprising the shaped body according to claim 21.

### Claim 26 (depends on 25)

The dental restoration according to claim 25, wherein the dental restoration is in the form of a crown or a bridge.

### Claim 27

A single- or multi-colored body made from colored oxide ceramic powder having a ratio of oxide ceramic component to mixtures of coloring oxides, of 100: 0.0001 to 2.0 parts by weight, wherein Pr2O3, Fe2O3, Tb2O3 and Cr2O3 are used as coloring oxides and wherein Tb2O3is used in a quantity of 0.0001 to 0.075 wt. %.

### Claim 28 (depends on 27)

The single- or multi-colored body according to claim 27, wherein the coloring oxides are selected from the oxides of the d- and f-elements of the periodic table.

### Claim 29 (depends on 28)

The single- or multi-colored body according to claim 28, wherein oxides of V, Ti, Nd, Eu, Dy, Er and/or Yb are used as further coloring oxides.

### Claim 30 (depends on 21)

A dental restoration part comprising the shaped body according to claim 21.

### Claim 31

A single- or multi-colored body made from colored oxide ceramic powder having a ratio of oxide ceramic component to mixtures of coloring oxides, of 100: 0.0001 to 2.0 parts by weight, wherein Pr2O3, Fe2O3, Tb2O3 and Mn2O3 are used as coloring oxides, wherein the coloring oxides are used in the following quantities, in wt.-%:
Pr, calculated as Pr2O3
0.001-0.003
Fe, calculated as Fe2O3
0.005-0.04
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0001-0.0005.

### Claim 32

A single- or multi-colored body made from colored oxide ceramic powder having a ratio of oxide ceramic component to mixtures of coloring oxides, of 100: 0.0001 to 2.0 parts by weight, wherein Pr2O3, Fe2O3, Tb2O3 and Mn2O3 are used as coloring oxides, wherein the coloring oxides are used in the following quantities, in wt.-%:
Pr, calculated as Pr2O3
0.002-0.004
Fe, calculated as Fe2O3
0.04-0.15
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0003-0.002.

### Claim 33

A single- or multi-colored body made from colored oxide ceramic powder having a ratio of oxide ceramic component to mixtures of coloring oxides, of 100: 0.0001 to 2.0 parts by weight, wherein Pr2O3, Fe2O3, Tb2O3 and Mn2O3 are used as coloring oxides, wherein the coloring oxides are used in the following quantities, in wt.-%:
Pr, calculated as Pr2O3
0.003-0.006
Fe, calculated as Fe2O3
0.04-0.15
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.0005-0.002.

### Claim 34

A single- or multi-colored body made from colored oxide ceramic powder having a ratio of oxide ceramic component to mixtures of coloring oxides, of 100: 0.0001 to 2.0 parts by weight, wherein Pr2O3, Fe2O3, Tb2O3 and Mn2O3 are used as coloring oxides, wherein the coloring oxides are used in the following quantities, in wt.-%:
Pr, calculated as Pr2O3
0.003-0.006
Fe, calculated as Fe2O3
0.04-0.25
Tb, calculated as Tb2O3
0.0005-0.004
Mn, calculated as Mn2O3
0.001-0.007.

### Claim 35 (depends on 5)

The shaped body according to claim 5, wherein the shaped body is in the form of a blank, dental shaped part or dental restoration.

### Claim 36 (depends on 5)

The shaped body according to claim 5, wherein the shaped body comprises at least 2 differently colored layers.

### Claim 37 (depends on 36)

The shaped body according to claim 36, wherein the shaped body comprises up to 8 differently colored layers.

### Claim 38 (depends on 5)

A dental restoration comprising the shaped body according to claim 5.

### Claim 39 (depends on 38)

The dental restoration according to claim 38, wherein the dental restoration is in the form of a crown or a bridge.