Nano-porous corundum ceramics and methods of manufacture

Patent metadata

Field	Value
Publication number	US-9776930-B2
Application number	US-201414470243-A
Country	US
Kind code	B2
Filing date	Aug 27, 2014
Priority date	Aug 27, 2014
Publication date	Oct 3, 2017
Grant date	Oct 3, 2017

Abstract

Nano-porous corundum ceramics and methods of manufacture are disclosed. The method of forming nano-porous 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 between 600° C. to 1000° C.

First claim

What is claimed is:

1. A method of forming nano-porous 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; and
sintering the gelled body between 600° C. to 1000° C.,
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 a pressure higher than an initial pressure is reached;
vacuuming the nitrogen gas;
filling the vacuum furnace again with the nitrogen gas; and
adjusting the temperature.

2. The method of claim 1 , wherein the corundum powder has a BET of 14-24 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 1 , wherein the beads are sintered corundum beads with sub-μm grain size.

5. The method of claim 1 , wherein the beads are one of corundum beads and ZrO 2 beads with 3 mol % Y 2 O 3 .

6. The method of claim 5 , wherein the slurry is aqueous slurry comprising distilled water and a stabilizing agent for corundum powder particles.

7. The method of claim 6 , further comprising adding a gelling agent after milling.

8. The method of claim 1 , wherein the sintering has a final temperature of about 800° C. for a hold time between about 0 hours and 8 hours.

9. The method of claim 8 , wherein the sintering of the gelled body is in air, oxygen or mixtures of inert gasses with oxygen.

10. The method of claim 8 , wherein the corundum powder has a purity of >99.9% and the beads are corundum milling beads with purity >99.9%.

11. The method of claim 10 , wherein the corundum powder has a purity of 99.995% and the beads are corundum milling beads with purity >99.95%.

12. A method of forming nano-porous corundum ceramics, comprising:
milling corundum powder in an aqueous slurry with beads;
processing the slurry by a liquid shaping process to form a celled body; and
sintering the gelled body between 600° C. to 1000° C.,
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 a pressure higher than an initial pressure is reached; and
vacuuming the nitrogen gas,

wherein the liquid shaping process further comprises using an ultrasonic bath,
wherein the placing the slurry molds in the vacuum furnace comprises placing the slurry molds in the vacuum furnace at about 20-25° C. with the vacuuming air inside until a vacuum at least 50 mbar above a boiling point of the slurry is reached,
wherein the inserting the nitrogen gas comprises inserting the nitrogen gas into the vacuum furnace until the vacuum furnace reaches atmospheric pressure,
wherein the vacuuming the nitrogen gas comprises vacuuming the nitrogen gas until a vacuum at least 50 mbar above the boiling point of the slurry is reached,
wherein the inserting the nitrogen gas and the vacuuming the nitrogen gas is repeated, and
wherein the liquid shaping process further comprises:
filling the vacuum furnace again with the nitrogen gas;
increasing the temperature to about 40° C. to 80° C. for 0-8 hours; and
reducing the temperature to about 20-25° C.

13. A method comprising:
milling corundum powder with BET of 17-21 m 2 /g in an aqueous slurry with beads, the aqueous slurry being distilled water and HNO 3 for stabilizing a pH of the corundum powder between 3.5 and 4.5;
processing the aqueous slurry by a liquid shaping process to form a gelled body; and
sintering the gelled body in air at a temperature between 800° C. to 900° C.,
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.

14. The method of claim 13 , wherein the beads are sintered corundum beads with sub-μm grain size.

15. The method of claim 13 , wherein the beads are ZrO 2 beads with 3 mol % Y 2 O 3 .

16. The method of claim 13 , wherein a sintering aid of MgO or a MgO precursor comprising <0.05 wt % MgO is added to the slurry.

17. The method of claim 13 , wherein the corundum powder has a purity of >99.9% and the beads are corundum milling beads with purity >99.9%.

18. The method of claim 13 , wherein a final temperature of the sintering is about 800° C. with a hold time of about 2 hours.

Assignees

• King Abdulaziz City Sci & Tech
• Fraunhofer-Gesellschaft

Inventors

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

Classifications

• C04B2235/6562

  Heating rate · CPC title

• C04B2235/6585

  at an oxygen percentage above that of air · CPC title

• C04B2235/6027

  Slip casting · CPC title

• C04B38/0054

  the pores being microsized or nanosized · CPC title

• C04B38/0074

  expressed as porosity percentage · CPC title