IP Library Granted Patent US 9,359,259
Granted Patent B2
US 9,359,259 · App. 14/445,760 · Granted Jun 7, 2016

Multi-metal oxide ceramic nanomaterial

Inventors: Stephen O'Brien (Jersey City, NJ); Shuangyi Liu (New York, NY); Limin Huang (Newark, NJ)
Assignee: Research Foundation of the City University of New York
C04B35/462C01G1/02C01G45/1221C04B35/624C04B35/6264C04B35/6325C01P2002/72C01P2002/85C01P2006/40C04B2235/3215C04B2235/3267C04B2235/441C04B2235/765
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Quick Facts
Patent No.
US 9,359,259
App. No.
14/445,760
Granted
Jun 7, 2016
Kind
B2
Abstract

A convenient and versatile method for preparing complex metal oxides is disclosed. The method uses a low temperature, environmentally friendly gel-collection method to form a single phase nanomaterial. In one embodiment, the nanomaterial consists of Ba A Mn B Ti C O D in a controlled stoichiometry.

Claims (29)

1. A method for producing a multi-metal oxide ceramic nanomaterial, the method comprising steps of:

mixing a first metal-organic salt comprising a first metal (M 1 ), a second metal-organic salt comprising a second metal (M 2 ) and a third metal-organic salt comprising a third metal (M 3 ) in an anhydrous solvent to form a first intermediate, wherein M 1 , M 2 and M 3 are independently selected from the group consisting of barium, manganese, titanium, iron, nickel, copper, bismuth, cobalt, samarium, and praseodymium, wherein M 1 , M 2 and M 3 are different;

adding deionized water to the anhydrous solvent to hydrolyze the first intermediate to produce a precursor solution;

permitting the precursor solution to form a gel wherein, after gel formation, at least 90% of M 1 , M 2 and M 3 is integrated into the gel;

sintering the gel for a predetermined time at a predetermined temperature to form a nanomaterial, wherein the predetermined temperature is less than 180° C.

2. The method as recited in claim 1 , wherein M 1 , M 2 and M 3 are independently selected from the group consisting of barium, titanium and a third metal selected from the group consisting of manganese, iron, nickel, copper, bismuth, cobalt, samarium, and praseodymium.

3. A method for producing a multi-metal oxide ceramic nanomaterial, the method comprising steps of:

mixing a first metal-organic salt comprising a first metal (M 1 ), a second metal-organic salt comprising a second metal (M 2 ) and a third metal-organic salt comprising a third metal (M 3 ) in an anhydrous solvent to form a first intermediate, wherein M 1 , M 2 and M 3 are independently selected from the group consisting of barium, titanium and manganese, wherein M 1 , M 2 and M 3 are different, such that the nanomaterial has a formula Ba A Mn B Ti C O D , where A is 1 to 2, B is 2 to 4, C is 3 to 5 and D is 12 to 18;

adding water to the anhydrous solvent to hydrolyze the first intermediate to produce a precursor solution;

permitting the precursor solution to form a gel wherein, after gel formation, at least 90% of M 1 , M 2 and M 3 is integrated into the gel;

sintering the gel for a predetermined time at a predetermined temperature to form a nanomaterial, wherein the predetermined temperature is less than 180°.

4. A method for producing a multi-metal oxide ceramic nanomaterial, the method comprising steps of:

mixing a first metal-organic salt comprising a first metal (M 1 ), a second metal-organic salt comprising a second metal (M 2 ) and a third metal-organic salt comprising a third metal (M 3 ) in an anhydrous solvent to form a first intermediate, wherein M 1 , M 2 and M 3 are selected from the group consisting of barium, titanium and manganese, wherein M 1 , M 2 and M 3 are different, such that the nanomaterial has a formula Ba A Mn 3 Ti 4 O D , where A is 1 to 1.12 and D is 14.25 to 16;

adding water to the anhydrous solvent to hydrolyze the first intermediate to produce a precursor solution;

permitting the precursor solution to form a gel wherein, after gel formation, at least 90% of M 1 , M 2 and M 3 is integrated into the gel;

sintering the gel for a predetermined time at a predetermined temperature to form a nanomaterial, wherein the predetermined temperature is less than 180°.

5. The method as recited in claim 4 , wherein D is about 16.

6. The method as recited in claim 4 , wherein D is about 14.

7. A method for producing a multi-metal oxide ceramic nanomaterial, the method comprising steps of:

mixing a first metal-organic salt comprising a first metal (M 1 ), a second metal-organic salt comprising a second metal (M 2 ) and a third metal-organic salt comprising a third metal (M 3 ) in an anhydrous solvent to form a first intermediate, wherein M 1 , M 2 and M 3 are independently selected from the group consisting of barium, manganese, titanium, iron, nickel, copper, bismuth, cobalt, samarium, and praseodymium, wherein M 1 , M 2 and M 3 are different;

adding water to the anhydrous solvent to hydrolyze the first intermediate to produce a precursor solution;

permitting the precursor solution to form a gel wherein, after gel formation, at least 90% of M 1 , M 2 and M 3 is integrated into the gel;

sintering the gel for a predetermined time at a predetermined temperature to form a nanomaterial, wherein the predetermined temperature is less than 180° C., wherein the nanomaterial is a mixed metal oxide of the Hollandite supergroup structure type of the formula M 1 M 2 M 3 O z where z is 12 to 18.

8. The method as recited in claim 7 , wherein M 1 is Ba, M 2 is Mn, M 3 is Ti such that the formula is Ba A Mn B Ti C O z , where A is 1 to 2, B is 2 to 4, C is 3 to 5 and Z is 12 to 18.

9. The method as recited in claim 8 , wherein A is 1 to 1.12, B is about 3, C is about 4 and Z is about 14 to 16.

10. The method as recited in claim 8 , wherein A is 1 to 1.5, Z is 14 to 16.

11. The method as recited in claim 8 , wherein the nanomaterial has a dielectric constant of greater than 10 4 at 1 kHz and greater than 200 at 100 MHz.

12. The method as recited in claim 1 , wherein the deionized water has a conductivity of less than 0.10 μS per cm.

13. The method as recited in claim 1 , wherein the deionized water has been purged of bicarbonate ions, carbon dioxide and oxygen.

Assignments (2)
CONFIRMATORY LICENSE Recorded Sep 1, 2017
From: RESEARCH FOUNDATION OF THE CITY UNIVERSITY OF NEW YORK
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 043468/0928 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 11, 2015
From: O'BRIEN, STEPHEN; LIU, SHUANGYI; HUANG, LIMIN
To: RESEARCH FOUNDATION OF THE CITY UNIVERSITY OF NEW YORK
Reel/Frame 035887/0868 →
Continuity (2)
Provisional Application 61859447 · Jul 29, 2013
Related Publication 20150094199A1 · Apr 2, 2015