# US 10,479,900 B2 · VO2 and V2O5 nano- and micro-materials and processes of making and uses of same

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- Number: US 10,479,900 B2
- Document ID: US10479900B2
- Status: Granted
- Kind: B2
- Application number: 15/506,422
- Filed: 2015-08-26
- Published: 2017-08-24
- Granted: 2019-11-19
- Earliest claimed: 2014-08-26
- Assignees: The Research Foundation for The State University of New York
- Applicants: The Research Foundation for The State University of New York
- Inventors: Sarbajit Banerjee; Gregory Horrocks
- Web page: https://patentgrep.com/patent/US10479900B2

## CPC

- C09D 7/61: inorganic
- C01G 31/02: Oxides
- C08K 3/00: Use of inorganic substances as compounding ingredients
- C08L 101/00: Compositions of unspecified macromolecular compounds
- C09D 5/24: Electrically-conducting paints {(conductive materials H01B1/00)}
- C09D 5/26: Thermosensitive paints
- C09D 7/70: {characterised by shape, e.g. fibres, flakes or microspheres}
- C01P 2002/52: containing elements as dopants
- C01P 2002/54: one element only
- C01P 2002/72: by d-values or two theta-values, e.g. as X-ray diagram
- C01P 2002/76: by a space-group or by other symmetry indications
- C01P 2002/77: by unit-cell parameters, atom positions or structure diagrams
- C01P 2002/82: by IR- or Raman-data
- C01P 2002/88: by thermal analysis data, e.g. TGA, DTA, DSC
- C01P 2004/03: obtained by SEM
- C01P 2004/04: obtained by TEM, STEM, STM or AFM
- C01P 2004/16: Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
- C01P 2004/61: Micrometer sized, i.e. from 1-100 micrometer
- C01P 2004/62: Submicrometer sized, i.e. from 0.1-1 micrometer
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2004/84: one phase coated with the other
- C01P 2006/32: Thermal properties
- C01P 2006/33: Phase transition temperatures
- C01P 2006/60: Optical properties, e.g. expressed in CIELAB-values
- C08K 3/22: of metals
- C08K 7/08: Oxygen-containing compounds
- C08K 2003/221: {of rare earth metal}
- C08K 2201/005: Additives being defined by their particle size in general
- C08K 2201/011: Nanostructured additives
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- 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)
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

VO2 and V2O5 nano- or micro-materials. The VO2 nano-materials and micro-materials have an M1 phase structure and oxygen stoichiometry that deviates 2% or less from theoretical stoichiometry. The VO2 nano-materials and micro-materials may doped with cation dopants and/or anion dopants. The VO2 and V2O5 nano- or micro-materials can be made by hydrothermal methods starting with V3O7.H2O nano- or micro-material. The VO2 and V2O5 nano- or micro-materials can be used as, for example, thermochromic window coatings.

## Claims

### Claim 1

A method for making VO2 nano-material or micro-material having an M1 phase structure and oxygen stoichiometry that deviates 2% or less from theoretical stoichiometry,
wherein the VO2 nano-material or micro-material exhibits a metal-insulator transition and 80% or more of the total change in resistivity resulting from the metal-insulator transition occurs over a range of 5° C. or less, comprising:
a) providing a solid V3O7.H2O nano-material or micro-material and hydrothermally reducing the solid V3O7.H2O nano-material or micro-material with water and, optionally, one or more agents selected from the group consisting of:
i) a C1-C8 linear or branched, substituted or unsubstituted, mono- or di-alcohol;
ii) a C1-C8 linear or branched, substituted or unsubstituted mono- or di-carboxylic acid; and
iii) a C1-C4 linear or branched, substituted or unsubstituted dialkyl-CO to produce a mixture of VO2 (A) and VO2 (B) nano- or micro-material;
b) filtering and washing the product from a) to isolate the mixture of VO2 (A) and VO2 (B) nano-material or micro-material;
c) annealing the isolated mixture of VO2 (A) and VO2 (B) nano-material or micro-material under an inert atmosphere at a temperature of at least 450° C.; and
d) cooling the product of c) to produce VO2 nano-material or micro-material in the M1 phase.

### Claim 2 (depends on 1)

The method for making VO2 nano-material or micro-material of claim 1, wherein the ratio (v/v) of agent to water in a) is 1:20 to 1:1.

### Claim 3 (depends on 1)

The method for making VO2 nano-material or micro-material of claim 1, wherein the cooling in d) occurs by the cessation of heating.

### Claim 4 (depends on 1)

The method for making VO2 nano-material or micro-material of claim 1, wherein a cation dopant source is present in a) and the cation dopant source comprises a metal and the cation dopant source is a nitrate salt of the metal, acetate salt of the metal, oxalate salt of the metal, oxide of the metal, or a combination thereof.

### Claim 5 (depends on 4)

The method for making VO2 nano-material or micro-material of claim 4, wherein the cation dopant source is tungstic acid, chromic acid, molybdic acid, lead acetate, tungsten oxide, molybdenum oxide, niobium oxide, chromium oxide, aluminum oxide, iron oxide, titanium oxide, zirconium oxide, tantalum oxide, scandium oxide, or gallium oxide.

### Claim 6 (depends on 1)

The method for making VO2 nano-material or micro-material of claim 1, wherein an anion dopant source is present in a).

### Claim 7 (depends on 6)

The method for making VO2 nano-material or micro-material of claim 6, wherein the anion dopant source comprises a semi-metal or main group element.

### Claim 8 (depends on 1)

The method for making VO2 nano-material or micro-material of claim 1, further comprising obtaining V3O7.H2O nano-material or micro-material by:
e) hydrothermally exfoliating and reducing bulk vanadium pentoxide (V2O5) with water and a reducing agent; and
f) isolating the V3O7.H2O nano-material or micro-material from the product from e).

### Claim 9 (depends on 8)

The method for making VO2 nano-material or micro-material of claim 8, wherein the isolating the V3O7.H2O nano-material or micro-material is carried out by filtering and washing the product from e).