# US 10,479,729 B2 · Shaded zirconia ceramic material and machinable sintered ceramic bodies made therefrom

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- Number: US 10,479,729 B2
- Document ID: US10479729B2
- Status: Granted
- Kind: B2
- Application number: 15/895,516
- Filed: 2018-02-13
- Published: 2018-08-23
- Granted: 2019-11-19
- Earliest claimed: 2017-02-22
- Assignees: James R. Glidewell Dental Ceramics, Inc.
- Applicants: James R. Glidewell Dental Ceramics, Inc.
- Inventors: Thomas C. Valenti; Kevin Michael Recor
- Web page: https://patentgrep.com/patent/US10479729B2

## CPC

- C04B 35/488: Composites
- A61C 13/0022: {Blanks or green, unfinished dental restoration parts}
- A61C 13/083: Porcelain or ceramic teeth {(A61C13/081 takes precedence; preparations A61K6/80)}
- A61K 6/818: comprising zirconium oxide
- C01F 17/276: Nitrates
- C01G 25/02: Oxides
- C01G 37/00: Compounds of chromium
- C04B 35/486: Fine ceramics
- C01P 2002/52: containing elements as dopants
- C01P 2002/54: one element only
- C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values
- C01P 2006/62: L* (lightness axis)
- C01P 2006/63: a* (red-green axis)
- C01P 2006/64: b* (yellow-blue axis)
- C01P 2006/80: Compositional purity
- 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 2235/3232: Titanium oxides or titanates, e.g. rutile or anatase
- C04B 2235/3239: Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
- C04B 2235/3241: Chromium oxides, chromates, or oxide-forming salts thereof
- C04B 2235/3262: Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
- C04B 2235/3275: Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
- C04B 2235/3279: Nickel oxides, nickalates, or oxide-forming salts thereof
- C04B 2235/3281: Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
- C04B 2235/3284: Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
- C04B 2235/40: Metallic constituents or additives not added as binding phase
- C04B 2235/443: Nitrates or nitrites
- C04B 2235/6562: Heating rate
- C04B 2235/6567: Treatment time
- C04B 2235/661: Multi-step sintering
- C04B 2235/77: Density
- C04B 2235/9661: Colour
- 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
- 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)
- C01F: COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; sulfides or polysulfides of magnesium, calcium, strontium, or barium C01B17/42; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds other than ammonia or cyanogen containing nitrogen and non-metals and optionally metals C01B21/082; amides or imides of silicon C01B21/087}; metal {imides or} amides C01B21/092, {C01B21/0923}; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanic acid C01C3/14; salts of cyanamide C01C3/16; thiocyanates C01C3/20; {double sulfates of magnesium with sodium or potassium C01D5/12; with other alkali metals C01D15/00, C01D17/00})
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Shaded, zirconia ceramic materials are disclosed that are suitable for use in dental applications. Ceramic bodies are made from a zirconia-containing ceramic material and a coloring composition comprising a terbium (Tb)-containing component and a chromium (Cr)-containing component as a coloring agent. The pre-shaded ceramic body is machinable into a dental restoration either as a bisque body or sintered body. A pre-shaded machinable sintered ceramic body may obviate the need for further processing steps, such as shading or sintering, and may be suitable for use in chair-side machining applications, such as in a dentist's office, significantly reducing the time to create a custom finished product.

## Claims

### Claim 1

A sintered ceramic body suitable for use in dental restoration applications comprising:
a. a ceramic material that comprises zirconia and
b. a coloring agent comprising 0.002 mass % to 0.65 mass % of terbium (Tb) and chromium (Cr) combined, measured as metal ions,
wherein the mass ratio of Tb to Cr, measured as metal ions, is in the range of approximately 93:7 Tb:Cr to approximately 99.5:0.5 Tb:Cr.

### Claim 2 (depends on 1)

The sintered ceramic body of claim 1, wherein the mass ratio of Tb to Cr, measured as metal ions, is in the range of approximately 94:6 Tb:Cr to approximately 99:1 Tb:Cr.

### Claim 3 (depends on 1)

The sintered ceramic body of claim 1, wherein the coloring agent further comprises at least one element selected from Er, Co, Mn, Pr, V, Ti, Ni, Cu and Zn.

### Claim 4 (depends on 1)

The sintered ceramic body of claim 1, wherein at least one coloring agent further comprises at least one element selected from Er, Co, Mn, and Pr.

### Claim 5 (depends on 1)

The sintered ceramic body of claim 1, comprising between 0.01 mass % and 0.1 mass % Fe.

### Claim 6 (depends on 1)

The sintered ceramic body of claim 1, comprising between 0 mass % and 0.002 mass % Fe ions.

### Claim 7 (depends on 1)

The sintered body of claim 1, having a center cross-sectional geometry that is at least 6 mm.

### Claim 8 (depends on 7)

The sintered body of claim 7, having a CIE L*a*b* ΔE of less than 5 between a cross-sectional center and a perimeter of the sintered ceramic body.

### Claim 9 (depends on 7)

The sintered body of claim 7, having a CIE L*a*b* ΔE of less than 3 between a cross-sectional center and a perimeter of the sintered ceramic body.

### Claim 10 (depends on 1)

The sintered ceramic body of claim 1, wherein the coloring agent comprises
a. 0.002 mass % to 0.3 mass % Tb, measured as Tb ions,
b. 0.000006 mass % to 0.01 mass % Cr, measured as Cr ions,
c. 0.02 mass % to 1.5 mass % Er, measured as Er ions, and
d. 0 mass % to 0.009 mass % Co, measured as Co ions.

### Claim 11 (depends on 1)

The sintered ceramic body of claim 1 wherein zirconia comprises between 85 wt % to approximately 100 wt % of the ceramic material.

### Claim 12 (depends on 1)

The sintered ceramic body of claim 1, wherein the ceramic material comprises yttria-stabilized zirconia comprising from 2 mol % to 7 mol % yttria, and 0 mol % to 1 mol % alumina.

### Claim 13

A ceramic powder suitable for use in dental restoration applications that comprises
a. a ceramic material comprising an yttria-stabilized zirconia that comprises from 2 mol % to 7 mol % yttria, and
b. a coloring agent comprising 0.002 mass % to 0.65 mass % Tb and Cr combined, measured as metal ions,
wherein a mass ratio of Tb ions to Cr ions is in a range of approximately 93:7 Tb:Cr to 99.5:0.5 Tb:Cr, and
c. optionally, a binder.

### Claim 14 (depends on 13)

The ceramic powder of claim 13, comprising 0.002 mass % to 0.3 mass % Tb and Cr combined, measured as metal ions.

### Claim 15 (depends on 13)

The ceramic powder of claim 13, wherein the mass ratio of Tb to Cr, measured as metal ions, is in the range of approximately 94:6 Tb:Cr to approximately 99:1 Tb:Cr.

### Claim 16 (depends on 13)

The ceramic powder of claim 13, wherein the coloring agent further comprises at least one element selected from Er, Co, Mn, Pr, V, Ti, Ni, Cu and Zn.

### Claim 17

A millable, pre-sintered ceramic body for use in making dental restorations comprising:
a. a ceramic material comprising an yttria-stabilized zirconia having from 2 mol % to 7 mol % yttria,
b. optionally comprising alumina, which if present comprises between 0 mol % and 1 mol %, and
c. a coloring agent comprising 0.03 mass % to 2 mass % of metal-containing components measured as metal ions,
wherein the coloring agent comprises terbium (Tb) and chromium (Cr) which are present in a mass ratio in a range of 93:7 Tb:Cr to 99.5:0.5 Tb:Cr, and
wherein Tb comprises 0.002 mass % to 0.65 mass %.

### Claim 18 (depends on 17)

The millable, pre-sintered ceramic body of claim 17, wherein the coloring agent further comprises at least one metal-containing component having an element selected from Er, Co, Mn, Pr, V, Ti, Ni, Cu and Zn.

### Claim 19 (depends on 17)

The millable, pre-sintered ceramic body of claim 17, wherein the coloring agent comprises terbium (Tb) and chromium (Cr) which are present in a mass ratio in a range of 94:6 Tb:Cr to 99:1 Tb:Cr.

### Claim 20 (depends on 17)

The millable, pre-sintered ceramic body of claim 17, wherein Tb comprises 0.002 mass % to 0.3 mass %.