High strength transparent ceramic using corundum powder and methods of manufacture

Patent metadata

Field	Value
Publication number	US-9527774-B2
Application number	US-201414470281-A
Country	US
Kind code	B2
Filing date	Aug 27, 2014
Priority date	Aug 27, 2014
Publication date	Dec 27, 2016
Grant date	Dec 27, 2016

Abstract

High strength transparent corundum ceramics using corundum powder and methods of manufacture are disclosed. The method of forming transparent corundum ceramics includes milling corundum powder in aqueous slurry with beads. The method further includes processing the slurry by a liquid shaping process to form a gelled body. The method further includes sintering the gelled body in air and pressing the gelled body by hot isostatic pressing to form a ceramic body.

First claim

What is claimed is:

1. A method of forming transparent corundum ceramics, comprising:
milling corundum powder in an aqueous slurry with beads;
processing the slurry by a liquid shaping process to form a gelled body;
sintering the gelled body in air; and
pressing the gelled body by hot isostatic pressing to form a ceramic body;
wherein the liquid shaping process comprises an ultrasonic bath, furnace with degassing process and a molding process, and wherein the gelled body is infiltrated with one or more precursors of metal ions solved in water to form colored transparent ceramics.

2. The method of claim 1 , wherein the corundum powder has a BET of 15-24 m 2 /g.

3. The method of claim 2 , wherein the corundum powder has a BET of 17-21 m 2 /g.

4. The method of claim 3 , wherein the sintering of the ceramic body in air is at a temperature between 1150° C.-1170° C. and the hot isostatic pressing is provided in Argon, Nitrogen or Oxygen at a temperature between 1100° C.-1150° C.

5. The method of claim 4 , wherein the sintering is performed at 1-10 K/min and the hot isostatic pressing is performed at between 50 and 200 MPa.

6. The method of claim 5 , wherein the sintering is performed at 5 K/min. to 950° C. and 2K/min. to final temperature.

7. The method of claim 4 , wherein the slurry is aqueous slurry comprising distilled water, stabilisator for the repulsion of the corundum particles and a sintering aid.

8. The method of claim 7 , wherein the sintering aid is MgO or MgO precursors.

9. The method of claim 4 , wherein the beads are dense sintered corundum beads with sub-μm grain size.

10. The method of claim 9 , wherein a relation of the corundum beads to powder is between 1:2 and 1:4.

11. The method of claim 9 , wherein the processing comprises adding the corundum powder to the slurry in an ultrasonic bath, then a predetermined amount of the corundum beads is added to the slurry, for about two hours milling at 1000 rpm.

12. The method of claim 1 , further comprising burning organics out of the gelled body at about 800° C.

13. A method of forming transparent corundum ceramics, comprising:
milling corundum powder in an aqueous slurry with beads;
processing the slurry by a liquid shaping process to form a gelled body;
sintering the gelled body in air; and
pressing the gelled body by hot isostatic pressing to form a ceramic body;
wherein the liquid shaping process comprises an ultrasonic bath, furnace with degassing process and a molding process, and
wherein the liquid shaping process comprises:
placing slurry molds in a vacuum furnace at about 20-25° C. with vacuuming air inside until it reaches a vacuum near the boiling point of the slurry;
inserting nitrogen gas into the vacuum furnace until it reaches atmospheric pressure;
vacuuming the nitrogen gas until it reaches a vacuum above the boiling point of the slurry;
repeated for two times the inserting nitrogen gas and vacuuming;
filling the vacuum furnace again with the nitrogen gas;
increasing the temperature to about 40° C. to 80° C. for about 4.0 hours; and
reducing the temperature to about 20-25° C.,
wherein the shaping process results in a gelled body which is dried.

14. A method comprising:
milling corundum powder with BET of 15-24 m 2 /g in an aqueous slurry with corundum beads;
processing the aqueous slurry by a liquid shaping process to form a gelled body;
sintering the gelled body in air at a temperature between 1150° C.-1170° C.; and
pressing the gelled body by hot isostatic pressing in Argon at temperatures between 1100° C.-1150° C. to form a ceramic body;
wherein the liquid shaping process comprises:
placing slurry molds in a vacuum furnace with vacuuming air inside;
inserting nitrogen gas into the vacuum furnace until it reaches a pressure higher than an initial pressure;
vacuuming the nitrogen gas;
filling the vacuum furnace again with the nitrogen gas; and
adjusting the temperature.

15. The method of claim 14 , wherein the sintering is performed at 5 K/min. to 950° C. and 2K/min. to final temperature and the hot isostatic pressing is performed at 50-200 MPa.

16. The method of claim 14 , wherein the aqueous slurry comprises distilled water organic gelling agent and HNO 3 for stabilizing the corundum powder at a pH of 4.

17. The method of claim 14 , wherein the corundum beads are dense sintered corundum beads with sub-μm grain size.

18. A method comprising:
milling corundum powder with BET of 15-24 m 2 /g in an aqueous slurry with corundum beads;
processing the aqueous slurry by a liquid shaping process to form a gelled body;
sintering the gelled body in air at a temperature between 1150° C.-1170° C.; and
pressing the gelled body by hot isostatic pressing in Argon at temperatures between 1100° C.-1150° C. to form a ceramic body;
wherein the liquid shaping process comprises an ultrasonic bath, furnace with degassing process and a molding process;
wherein the gelled body is infiltrated with one or more precursors of metal ions solved in water to form colored transparent ceramics.

Assignees

• King Abdulaziz City Sci & Tech
• Fraunhofer-Gesellschaft

Inventors

• Binhussain Mohammed A
• Alakeel Akeel Khalid
• Binmajid Majid Mohammed
• Klimke Jens

Classifications

• C04B35/62625

  Wet mixtures · CPC title

• C04B35/115 Primary

  Translucent or transparent products · CPC title

• C04B2235/616

  Liquid infiltration of green bodies or pre-forms · CPC title

• C01P2006/90

  Other properties not specified above · CPC title

• C04B2235/9661

  Colour · CPC title