IP Library Granted Patent US 8,900,537
Granted Patent B2
US 8,900,537 · App. 13/105,102 · Granted Dec 2, 2014

Synthesis of pyrochlore nanostructures and uses thereof

Inventors: Vaidyanathan Subramanian (Sparks, NV); Sankaran Murugesan (Austin, TX)
Assignee: Board of Regents of the Nevada System of Higher Education, on behalf of the University of Nevada, Reno
C01G29/00C01P2004/04C01P2004/03C01P2004/16B82Y40/00C01P2002/36B82Y30/00C01P2002/84C01P2002/72
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Quick Facts
Patent No.
US 8,900,537
App. No.
13/105,102
Granted
Dec 2, 2014
Kind
B2
Abstract

A template-free reverse micelle (RM) based method is used to synthesize pyrochlore nanostructures having photocatalytic activity. In one embodiment, the method includes separately mixing together a first acid stabilized aqueous solution including pyrochlore precursor A and a second acid stabilized aqueous solution including pyrochlore precursor B with an organic solution including a surfactant to form an oil-in-water emulsion. Next, equimolar solutions of the first and second acid stabilized oil-in-water emulsions are mixed together. Then, the mixture of the first and second acid stabilized oil-in-water emulsion is treated with a base to produce a precipitate including pyrochlore precursors A and B. After which, the precipitate is dried to remove volatiles. The precipitate is then calcined in the presence of oxygen to form a pyrochlore nanostructure, such as a bismuth titanate (Bi 2 Ti 2 O 7 ) pyrochlore nanorod. The method of synthesizing the pyrochlore nanorod is template-free.

Claims (17)

1. A method of synthesizing a pyrochlore nanostructure having the general formula A 2 B 2 O 7 , where A and B are rare-earth or transition metal species and O is oxygen, the method comprising:

separately mixing together a first acid stabilized aqueous solution including a pyrochlore precursor A and a second acid stabilized aqueous solution including a pyrochlore precursor B with an organic solvent mixture comprising a surfactant and an organic solvent to form a first acid stabilized oil-in-water emulsion of precursor A and a second acid stabilized oil-in-water emulsion of precursor B;

mixing together equimolar portions of the first and second acid stabilized oil-in-water emulsions to form a mixed acid stabilized oil-in-water emulsion comprising the pyrochlore precursor A and the pyrochlore precursor B;

treating the mixed acid stabilized oil-in-water emulsion with a base to increase the pH from acidic to alkaline to produce a precipitate including the pyrochlore precursors A and B;

isolating the precipitate; and

calcining the precipitate in the presence of oxygen to form the pyrochlore nanostructure, wherein the method of synthesizing the pyrochlore nanostructure is template-free.

2. The method of claim 1 , wherein B of the pyrochlore precursor B is titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), iron (Fe), nickel (Ni), zirconium (Zr), tin (Sn), hafnium (Hf), tantalum (Ta), tungsten (W), or combinations thereof.

3. The method of claim 1 , wherein A of the pyrochlore precursor A is bismuth (Bi), calcium (Ca), strontium (Sr), yttrium (Y), barium (Ba), lanthanum (La), or combinations thereof.

4. The method of claim 1 , wherein the first and second acid stabilized solutions each include an acid independently selected from hydrochloric acid (HCl), nitric acid (HNO 3 ), acetic acid (CH 3 CO 2 H), sulfurous acid (H 2 SO 3 ), formic acid (HCO 2 H), perchloric acid (HClO 4 ), or combinations thereof.

5. The method of claim 1 , wherein the surfactant is selected from an anionic surfactant comprising a sulfate, a sulfonate, a phosphinate, or a carboxylate moiety; a cationic surfactant comprising an ammonium moiety; or a nonionic surfactant.

6. The method of claim 1 , wherein the organic solvent is selected from an alkane, an alkanol, an alkanone, or combinations thereof.

7. The method of claim 1 , wherein calcining is performed at a temperature greater than 350° C. and less than 900° C.

8. The method of claim 7 , wherein calcining is performed at a temperature greater than 500° C.

9. The method of claim 1 wherein the pyrochlore nanostructure is a pyrochlore nanorod.

10. The method of claim 9 wherein the pyrochlore nanorod is a bismuth titanate (Bi 2 Ti 2 O 7 ) pyrochlore nanorod.

11. The method of claim 1 wherein the pyrochlore nanostructure has photocatalytic activity.

12. The method of claim 1 wherein a ratio of water to organic solvent mixture of the first and second acid stabilized aqueous solutions is from 4 to 40 v/v.

Assignments (2)
CONFIRMATORY LICENSE Recorded Feb 25, 2025
From: UNIVERSITY OF NEVADA RENO
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 070314/0580 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 8, 2014
From: SUBRAMANIAN, VAIDYANATHAN; MURUGESAN, SANKARAN
To: BOARD OF REGENTS OF THE NEVADA SYSTEM OF HIGHER EDUCATION, ON BEHALF OF THE UNIVERSITY OF NEVADA, RENO
Reel/Frame 033499/0471 →
Continuity (2)
Provisional Application 61333463 · May 11, 2010
Related Publication 20110281111A1 · Nov 17, 2011