IP Library Granted Patent US 7,220,454
Granted Patent B2
US 7,220,454 · App. 10/774,319 · Granted May 22, 2007

Production method of high strength polycrystalline ceramic spheres

Assignee: William Marsh Rice University
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Quick Facts
Patent No.
US 7,220,454
App. No.
10/774,319
Granted
May 22, 2007
Kind
B2
Abstract

A method for making hollow spheres of alumina or aluminate comprises: coating polymeric beads with an aqueous solution of an alumoxane, drying the beads so as to form an alumoxane coating on the beads; heating the beads to a first temperature that is sufficient to convert the alumoxane coating to an amorphous alumina or aluminate coating and is not sufficient to decompose the polymeric beads; dissolving the polymeric bead in a solvent; removing the dissolved polymer from the amorphous alumina or aluminate coating; and heating the amorphous alumina or aluminate coating to a second temperature that is sufficient to form a hollow ceramic sphere of desired porosity and strength. The hollow spheres can be used as proppants or can be incorporated in porous membranes.

Claims (16)

1. A method for making hollow spheres of alumina or aluminate comprising:

a) coating polymeric beads with an aqueous solution of an alumoxane;

b) drying the beads so as to form an alumoxane coating on the beads;

c) heating the beads to a first temperature, wherein the first temperature is sufficient to convert the alumoxane coating to an amorphous alumina or aluminate coating and is not sufficient to decompose the polymeric beads;

d) dissolving the polymeric bead in a solvent;

e) removing the dissolved polymer from the amorphous alumina or aluminate coating; and

f) heating the amorphous alumina or aluminate coating to a second temperature that is sufficient to form a hollow ceramic sphere of desired porosity and strength.

2. The method of claim 1 wherein the alumoxane comprises acetate-alumoxane.

3. The method of claim 1 wherein the average diameter of the polymeric beads is approximately 3 μm.

4. The method of claim 1 wherein the first temperature is between 180° C. and 230° C.

5. The method of claim 1 wherein the second temperature is above 600° C.

6. The method of claim 1 , further comprising:

g) covering the ceramic sphere with a solution of a metal-doped alumoxane so as to form a metal-doped alumoxane coating on the ceramic sphere; and

h) heating the coated sphere to a temperature sufficient to convert the metal-doped alumoxane coating to a mixed metal oxide phase.

7. The method of claim 6 wherein the metal-doped alumoxane comprises methoxy(ethoxyethoxy)acetic acid alumoxane.

8. The method of claim 6 wherein the metal-doped alumoxane comprises elements La, Ca, Er, Mg, Ti, or Y.

Assignments (2)
CONFIRMATORY LICENSE Recorded May 16, 2012
From: RICE UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 028216/0419 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 9, 2004
From: BARRON, ANDREW R.; DEFRIEND, KIMBERLY A.
To: WILLIAM MARSH RICE UNIVERSITY
Reel/Frame 014834/0882 →
Continuity (3)
Provisional Application 6044555100 · Feb 6, 2003
Provisional Application 6044558600 · Feb 6, 2003
Related Publication 20040224155A1 · Nov 11, 2004