# US 12,179,383 B2 · Process and slip for the production of ceramic shaped bodies made of zirconium oxide by 3D inkjet printing

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- Number: US 12,179,383 B2
- Document ID: US12179383B2
- Status: Granted
- Kind: B2
- Application number: 18/346,536
- Filed: 2023-07-03
- Published: 2023-11-02
- Granted: 2024-12-31
- Earliest claimed: 2018-11-29
- Assignees: Ivoclar Vivadent AG
- Applicants: Ivoclar Vivadent AG
- Inventors: Christian Ritzberger; Johannes Renner
- Web page: https://patentgrep.com/patent/US12179383B2

## CPC

- B28B 1/001: {Rapid manufacturing of 3D objects by additive depositing, agglomerating or laminating of material (selective deposition modelling of metallic powder B22F10/00; rapid manufacturing of 3D objects in general and in particular of plastics B29C64/00)}
- A61C 8/005: {Connecting devices for joining an upper structure with an implant member, e.g. spacers}
- A61C 13/0013: {using stereolithographic techniques}
- A61C 13/082: {Cosmetic aspects, e.g. inlays; Determination of the colour (A61C19/10 takes precedence)}
- A61C 13/083: Porcelain or ceramic teeth {(A61C13/081 takes precedence; preparations A61K6/80)}
- A61K 6/818: comprising zirconium oxide
- B28B 11/243: {Setting, e.g. drying, dehydrating or firing ceramic articles (B28B11/242 takes precedence)}
- C04B 35/119: with zirconium oxide
- C04B 35/488: Composites
- B33Y 10/00: Processes of additive manufacturing
- B33Y 70/00: Materials specially adapted for additive manufacturing
- B33Y 80/00: Products made by additive manufacturing
- C04B 35/48: based on zirconium or hafnium oxides, zirconates, {zircon} or hafnates
- C04B 35/6263: {characterised by their solids loadings, i.e. the percentage of solids}
- C04B 35/6264: {Mixing media, e.g. organic solvents}
- C04B 35/632: Organic additives
- C04B 2235/3206: Magnesium oxides or oxide-forming salts thereof
- C04B 2235/3208: Calcium oxide or oxide-forming salts thereof, e.g. lime
- C04B 2235/3225: Yttrium oxide or oxide-forming salts thereof
- C04B 2235/3227: Lanthanum oxide or oxide-forming salts thereof
- C04B 2235/3229: Cerium oxides 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 2235/5427: millimeter or submillimeter sized, i.e. larger than 0,1 mm
- C04B 2235/5454: nanometer sized, i.e. below 100 nm
- C04B 2235/6026: Computer aided shaping, e.g. rapid prototyping
- C04B 2235/606: Drying
- C04B 2235/608: Green bodies or pre-forms with well-defined density
- C04B 2235/6562: Heating rate
- C04B 2235/6565: Cooling rate
- C04B 2235/6567: Treatment time
- C04B 2235/6581: Total pressure below 1 atmosphere, e.g. vacuum
- C04B 2235/6583: Oxygen containing atmosphere, e.g. with changing oxygen pressures
- C04B 2235/665: Local sintering, e.g. laser sintering
- C04B 2235/77: Density
- C04B 2235/96: Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B 2235/9646: Optical properties
- B28B: SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER (foundry moulding B22C; working stone or stone-like material B28D; shaping of substances in a plastic state, in general B29C; making layered products not composed wholly of these substances B32B)
- 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
- B33Y: ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING

## Abstract

Process and slip for the production of ceramic shaped parts made of zirconium oxide ceramic by a 3D inkjet printing process. The slip contains zirconium oxide which is suspended in a liquid medium, wherein the slip has a zirconium oxide content of from 68 to 88 wt.-% and contains not more than 5 wt.-% organic components. The process for the production of ceramic components comprises the layered shaping and subsequent sintering of the desired component from the slip.

## Claims

### Claim 1

A slip for use in an inkjet printing process comprising
zirconium oxide with a particle size of from 50 to 250 nm, measured as the d50 value and relative to the volume of the particles, which comprises one or more coloring elements and is suspended in a liquid medium,
wherein the slip has a zirconium oxide content of from 68 to 88 wt.-%, and not more than 3 wt.-% organic components, relative to the total mass of the slip, and
wherein the slip has a viscosity of from 5 to 100 mPas, measured at a shear rate of from 0.1 to 1000 s−1 and a temperature of 25° C.

### Claim 2 (depends on 1)

The slip according to claim 1 comprising
70 to 86 wt.-% zirconium oxide and
not more than 3 wt.-% organic components.

### Claim 3 (depends on 1)

The slip according to claim 1,
wherein the zirconium oxide comprises one or more coloring elements selected from Fe, Mn, Cr, Ni, Co, Pr, Ce, Eu, Gd, Nd, Yb, Tb, Er and Bi.

### Claim 4 (depends on 1)

The slip according to claim 1,
wherein the zirconium oxide in the slip has a primary particle size of from 30 to 100 nm.

### Claim 5 (depends on 1)

The slip according to claim 1,
wherein the zirconium oxide is stabilized with 2 to 14 mol.-% Y2O3, La2O3, CeO2, MgO and/or Cao, relative to the zirconium oxide content.

### Claim 6 (depends on 1)

The slip according to claim 1,
wherein the liquid medium comprises water.

### Claim 7 (depends on 1)

The slip according to claim 1 comprising
the organic components in a quantity of from 0.05 to 3 wt.-%, relative to the total mass of the slip.

### Claim 8 (depends on 1)

The slip according to claim 1,
wherein the liquid medium contains at least one compound selected from amino alcohol, glycol, carboxylic acid and carboxylic acid salt and at least one compound selected from ethanolamine, ethylene glycol, dipropylene glycol, citric acid and citric acid salt.

### Claim 9 (depends on 1)

The slip according to claim 1 comprising
a mixture of zirconium oxide powders with different compositions and with a different coloring and/or translucence.

### Claim 10 (depends on 1)

The slip according to claim 1 comprising
70 to 86 wt.-% zirconium oxide and
not more than 2 wt.-% organic components.

### Claim 11 (depends on 1)

The slip according to claim 1 comprising
70 to 86 wt.-% zirconium oxide and
not more than 1 wt.-% organic components.

### Claim 12 (depends on 1)

The slip according to claim 1 comprising
75 to 85 wt.-% zirconium oxide and
not more than 3 wt.-% organic components.

### Claim 13 (depends on 1)

The slip according to claim 1 comprising
75 to 85 wt.-% zirconium oxide and
not more than 2 wt.-% organic components.

### Claim 14 (depends on 1)

The slip according to claim 1 comprising
75 to 85 wt.-% zirconium oxide and
not more than 1 wt.-% organic components.