# US 11,077,496 B2 · Microwave-assisted carbon template method for preparing supported nano metal materials

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- Number: US 11,077,496 B2
- Document ID: US11077496B2
- Status: Granted
- Kind: B2
- Application number: 16/279,926
- Filed: 2019-02-19
- Published: 2019-06-13
- Granted: 2021-08-03
- Earliest claimed: 2016-10-08
- Assignees: Wuhan Institute of Technology; Changzhou University
- Applicants: Wuhan Institute of Technology; Changzhou University
- Inventors: Xingmao Jiang; Jingyuan Cao; Xue Tong; Zhongnan Zhang; Jian Feng
- Web page: https://patentgrep.com/patent/US11077496B2

## CPC

- B22F 9/22: using gaseous reductors
- B22F 1/054: Nanosized particles
- B22F 9/24: starting from liquid metal compounds, e.g. solutions
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C04B 35/6267: {Pyrolysis, carbonisation or auto-combustion reactions}
- C04B 35/62805: {Oxide ceramics}
- C04B 35/6286: {Carbides}
- C08L 1/28: Alkyl ethers
- B22F 2201/01: Reducing atmosphere
- B22F 2202/11: Use of irradiation
- B22F 2301/15: Nickel or cobalt
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- C04B 2235/3227: Lanthanum oxide or oxide-forming salts thereof
- C04B 2235/3229: Cerium oxides or oxide-forming salts thereof
- C04B 2235/3418: Silicon oxide, silicic acids or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
- C08L 1/08: Cellulose derivatives
- C08L 3/02: Starch; Degradation products thereof, e.g. dextrin
- C08L 5/00: Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- 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
- C08L: COMPOSITIONS OF MACROMOLECULAR COMPOUNDS (compositions based on polymerisable monomers C08F, C08G; artificial filaments or fibres D01F; textile treating compositions D06)

## Abstract

The present disclosure provides a microwave-assisted carbon template method for preparing supported nano metal-oxides or nano metals. The method includes mixing a carbohydrate, urea, and a precursor of an oxide support with a metal salt in a container, adding a certain amount of water, and completely dissolving the solid chemicals through ultrasonic stirring to form a homogeneous solution. The method also includes performing microwave treatment on the obtained solution for approximately 0.1 minute to 60 minutes with a microwave heating power in a range of approximately 100 W to 50 kW to dehydrate and carbonize the carbohydrate and thus form a dark brown solid. The method further includes performing heat treatment on the dark brown solid at a temperature in a range of approximately 200° C. to 1100° C. in an air atmosphere for approximately 0.5 hour to 24 hours to obtain a metal-oxide supported by a porous oxide support.

## Claims

### Claim 1

A microwave-assisted carbon template method for preparing supported nano metal-oxides or nano metals, comprising:
a) mixing a carbohydrate, urea, and a precursor of an oxide support together with a metal salt in a container, adding a certain amount of water, and completely dissolving solid chemicals in water through ultrasonic stirring to form a homogeneous solution;
b) performing microwave treatment on the solution obtained in a) for approximately 0.1 minute to 60 minutes with a microwave heating power in a range of approximately 100 W to 50 kW, such that the carbohydrate is dehydrated and carbonized and a solid is formed; and
c) performing heat treatment on the solid obtained in b) at a temperature in a range of approximately 200° C. to 1100° C. in an air atmosphere for approximately 0.5 hour to 24 hours to obtain a metal-oxide supported by a porous oxide support.

### Claim 2 (depends on 1)

The method according to claim 1, after performing heat treatment on the solid to obtain the porous oxide supported metal-oxide, further including:
d) heat treating the metal-oxide supported by the porous oxide support obtained in c) at a temperature in a range of approximately 200° C. to 1100° C. in a reducing atmosphere for approximately 0.5 hour to 24 hours to obtain a nano metal supported by a porous oxide support.

### Claim 3 (depends on 2)

The method according to claim 2, wherein:
a reducing gas used in d) is a mixed gas containing hydrogen or carbon monoxide in a volume fraction of approximately 5% to 10%, and nitrogen or argon as an equilibrium gas.

### Claim 4 (depends on 2)

The method according to claim 2, wherein:
the porous oxide support obtained in d) is a single element oxide or a composite oxide, wherein:
the single element oxide is an oxide of Si, Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os; and
the composite oxide includes oxides of two or more different elements of Si, Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La and Os.

### Claim 5 (depends on 2)

The method according to claim 2, wherein:
the nano metal supported by the porous oxide support obtained in d) is an elementary metal of Mg, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pt, Pd, Ru, Os, Rh, Ir, Au, Ag, Pb, In, Sn, Sb, Zr, Nb, La, Ce, Ta, Mo W, or Re; or an alloy or an intermetallic compound of two or more different metal elements of Mg, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Pt, Pd, Ru, Os, Rh, Ir, Au, Ag, Pb, In, Sn, Sb, Zr, Nb, La, Ce, Ta, Mo, W, and Re.

### Claim 6 (depends on 1)

The method according to claim 1, wherein:
the precursor of the oxide support used in a) includes a common silicon source, a common aluminum source, or other common metal salt, wherein:
the common silicon source includes at least one of silica sol, sodium silicate, and tetraethyl orthosilicate;
the common aluminum source includes at least one of aluminum sol, aluminum sulfate, aluminum chloride, aluminum nitrate, and aluminum isopropoxide; and
the other common metal salt is a nitrate, halide, hypochlorite, acetate, oxalate, phosphate, or sulfate of a metal element, or includes more than one salt of different metal elements, wherein:
the metal elements include Mg, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La, and Os.

### Claim 7 (depends on 1)

The method according to claim 1, wherein:
the metal salt used in a) is a nitrate, halide, hypochlorite, acetate, oxalate, phosphate, or sulfate of a metal element, or includes more than one salt of different metal elements, wherein:
the metal elements include Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La, and Os.

### Claim 8 (depends on 1)

The method according to claim 1, wherein:
the carbohydrate used in a) is one of glucose, fructose, sucrose, maltose, lactose, starch, methylcellulose, and dextrin.

### Claim 9 (depends on 1)

The method according to claim 1, wherein:
a mass ratio of the carbohydrate to urea in a) is approximately 20:1 to 1:60;
a mass ratio of the carbohydrate to the metal salt in a) is approximately 100:1 to 1:10;
a mass ratio of the carbohydrate to the precursor of the oxide support in a) is approximately 100:1 to 1:50; and
a mass ratio of the carbohydrate to water in a) is approximately 50:1 to 1:100.

### Claim 10 (depends on 1)

The method according to claim 1, wherein:
the porous oxide support obtained in c) is a single element oxide or a composite oxide, wherein
the single element oxide is an oxide of Si, Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La, or Os; and
the composite oxide includes oxides of two or more different elements of Si, Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La, and Os.

### Claim 11 (depends on 1)

The method according to claim 1, wherein:
the metal-oxide supported by the porous oxide support obtained in c) is a single metal element oxide or a composite metal-oxide, wherein:
the single metal-oxide is an oxide of Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La or Os; and
the composite metal-oxide includes oxides of two or more different metal elements of Mg, Al, Pb, In, Sn, Sb, Zr, Nb, Ce, Ta, Mo, W, Re, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Pt, Pd, Ir, Ru, Rh, Y, Ba, Sr, La and Os.