# US 10,118,862 B2 · Multi-metal oxide ceramic nanomaterial

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- Number: US 10,118,862 B2
- Document ID: US10118862B2
- Status: Granted
- Kind: B2
- Application number: 15/083,885
- Filed: 2016-03-29
- Published: 2016-09-29
- Granted: 2018-11-06
- Earliest claimed: 2013-07-29
- Assignees: Research Foundation of the City University of New York
- Applicants: Research Foundation of the City University of New York
- Inventors: Stephen O'Brien; Shuangyi Liu; Limin Huang
- Web page: https://patentgrep.com/patent/US10118862B2

## CPC

- C04B 35/624: Sol-gel processing
- C01G 1/02: Oxides
- C01G 45/12: Complex oxides containing manganese and at least one other metal element
- C01G 45/1221: Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof
- C04B 35/462: based on titanates
- C04B 35/4686: {based on phases other than BaTiO3 perovskite phase}
- C04B 35/6264: {Mixing media, e.g. organic solvents}
- C04B 35/6325: {based on organo-metallic compounds}
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/85: by XPS, EDX or EDAX data
- C01P 2006/40: Electric properties
- C04B 2235/3215: Barium oxides or oxide-forming salts thereof
- C04B 2235/3267: MnO2
- C04B 2235/441: Alkoxides, e.g. methoxide, tert-butoxide
- C04B 2235/765: Tetragonal symmetry
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## 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 BaAMnBTiCOD in a controlled stoichiometry.

## Claims

### Claim 1

A method for producing a metal oxide ceramic nanomaterial, the method comprising steps of:
mixing a first metal-organic salt comprising a first metal (M1) and a second metal-organic salt comprising a second metal (M2) in an anhydrous solvent to form a first intermediate, wherein M1 is selected from the group consisting of barium, manganese, iron, nickel, copper, bismuth, cobalt, samarium, and praseodymium, and M2 is titanium;
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 M1 and M2 is integrated into the gel; and
forming a hollandiate nanomaterial from the gel.

### Claim 2 (depends on 1)

The method as recited in claim 1, wherein the anhydrous solvent is selected from the group consisting of anhydrous methanol, anhydrous ethanol and anhydrous isopropanol.

### Claim 3 (depends on 1)

The method as recited in claim 1, wherein the first metal-organic salt is a acetylacetonate salt.

### Claim 4 (depends on 1)

The method as recited in claim 1, wherein the second metal-organic salt is a isopropoxide salt.

### Claim 5 (depends on 1)

The method as recited in claim 1, wherein the nanomaterial is a mixed metal oxide of the perovskite structure type of formula M1M2O3, where M1 and M2 are different metals.

### Claim 6 (depends on 1)

The method as recited in claim 1, wherein the nanomaterial is a mixed metal oxide of the ferrite structure type of the formula M1M22O4 where M1 and M2 are different metals.

### Claim 7 (depends on 1)

The method as recited in claim 1, wherein the nanomaterial is a mixed metal oxide of the formula Mx1My2Oz wherein x is about 1 to about 3, y is about 1 to about 5, and z is about 3 to about 16.

### Claim 8

A method for producing a metal oxide ceramic nanomaterial, the method comprising steps of:
mixing a first metal-organic salt comprising a first metal (M1) and a second metal-organic salt comprising a second metal (M2) in an anhydrous solvent to form a first intermediate, wherein M1 and M2 are independently selected from the group consisting of barium, manganese, titanium, iron, nickel, copper, bismuth, cobalt, samarium, and praseodymium, wherein M1 and M2 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 M1 and M2 is integrated into the gel; and
forming a nanomaterial from the gel; wherein the first metal-organic salt is a 1,3 dicarbonyl salt.

### Claim 9

A method for producing a metal oxide ceramic nanomaterial, the method comprising steps of:
mixing a first metal-organic salt comprising a first metal (M1) and a second metal-organic salt comprising a second metal (M2) in an anhydrous solvent to form a first intermediate, wherein M1 and M2 are independently selected from the group consisting of barium, manganese, titanium, iron, nickel, copper, bismuth, cobalt, samarium, and praseodymium, wherein M1 and M2 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 M1 and M2 is integrated into the gel; and
forming a nanomaterial from the gel; wherein the first metal-organic salt is a 1,3 dicarbonyl salt and the second metal-organic salt is an alkoxide salt.
