# US 10,441,941 B2 · Preparation method of alumina supported cerium oxide powder material

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- Number: US 10,441,941 B2
- Document ID: US10441941B2
- Status: Granted
- Kind: B2
- Application number: 15/735,247
- Filed: 2016-05-06
- Published: 2018-06-21
- Granted: 2019-10-15
- Earliest claimed: 2015-07-03
- Assignees: Hohai University
- Applicants: Hohai University
- Inventors: Jianfeng Zhang; Gaiye Li; Huiyang Cao; Xin Zhang; Wenmin Guo; Yuping Wu
- Web page: https://patentgrep.com/patent/US10441941B2

## CPC

- B01J 23/10: of rare earths
- B01J 35/19: {Catalysts containing parts with different compositions}
- B01J 37/0238: {via the gaseous phase-sublimation}
- B01J 21/04: Alumina
- B01J 35/40: characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77)
- B01J 35/45: Nanoparticles
- B01J 37/0223: {by rotation}
- B01J 2235/15: X-ray diffraction
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

The present invention discloses a preparation method of an alumina supported cerium oxide powder material. A cerium organometallic precursor is effectively decomposed into CeO2 nanoparticles at 500-700° C. in an oxygen atmosphere condition by using a chemical vapor deposition method, and the CeO2 nanoparticles are evenly dispersed on an Al2O3 support. The decomposition of the CeO2 precursor is accelerated by changing experimental parameters of reaction between organic materials and oxygen, so as to control the size and microstructure of powder, thereby achieving the preparation and even dispersion of cerium oxide nanoparticles, and avoiding the problem of generation of toxic waste liquor during reaction. The method of the present invention is simple, has a short preparation period, and the cerium oxide nanoparticles prepared are evenly dispersed, can be used as catalytic materials and functional materials, and have a broad application prospect in multiple fields.

## Claims

### Claim 1

A method of preparing an alumina supported cerium oxide powder material, comprising:
(1) providing a cerium organometallic precursor as a CeO2 material, and heating the cerium organometallic precursor in a feed vaporizer to vaporize, wherein a heating temperature range is 100 to 300° C.;
(2) pretreating Al2O3 powder by drying and sieving, and then placing the pretreated Al2O3 powder into a chemical vapor deposition reaction chamber, vacuumizing to 5 to 20 Pa, and preheating, wherein a preheating temperature is 500 to 800° C.;
(3) feeding a mixed gas of oxygen and argon gas, and vaporized CeO2 material into a rotating reactor, and conducting rotary chemical vapor deposition under a high temperature to make the cerium organometallic precursor be decomposed into CeO2 and deposited on the Al2O3 powder;
(4) after completing the reaction, stopping the rotation of the reaction chamber, closing a valve, cooling to a room temperature, and removing the coated powder; and
(5) grinding and sieving the powder obtained by step (4).

### Claim 2 (depends on 1)

The method according to claim 1, wherein in step (1), the cerium organometallic precursor is any one of Ce(DPM)4, cerium isooctanoate, Ce(C5H5)3, or cerium acetate.

### Claim 3 (depends on 1)

The method according to claim 1, wherein in step (2), the average particle size of the Al2O3 powder is 0.1 to 100 μm, and the purity of the Al2O3 powder is no less than 95%.

### Claim 4 (depends on 1)

The method according to claim 1, wherein in step (2), the temperature rise rate of the preheating process is 2 to 10° C./min.

### Claim 5 (depends on 1)

The method according to claim 1, wherein in step (3), the condition of the rotary chemical vapor deposition is: a reaction temperature is 600 to 800° C., the rotating speed of the chemical vapor deposition reaction chamber is 20 to 60 rpm, and a thermal insulation reaction is conducted for 0.5 to 4 h, wherein the gas flow of argon gas is 80 to 100 sccm, and the gas flow of oxygen is 10 to 100 sccm.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the total pressure of the fed mixed gas of oxygen and argon gas is 200 to 1000 Pa, and the partial pressure of oxygen is 50 to 200 Pa.

### Claim 7 (depends on 1)

The method according to claim 1, wherein in step (2), the temperature of pretreating the Al2O3 powder for drying is 80 to 100° C., the size of a sieve pore for sieving the Al2O3 powder is 50 to 200 meshes, and the Al2O3 powder is sieved three times.

### Claim 8 (depends on 1)

The according to claim 1, wherein in step (5), the size of a sieve pore for sieving the powder is 50 to 200 meshes, and the powder is sieved three times.

### Claim 9 (depends on 1)

An alumina supported cerium oxide powder material prepared by the preparation method according to claim 1, comprising CeO2 nanoparticles on a surface of the Al2O3 powder; wherein:
the average particle size of the Al2O3 powder is 0.1 to 100 μm, and the purity of the Al2O3 powder is no less than 95%;
the CeO2 nanoparticles have an average particle size of 6-13 nm;
the CeO2 nanoparticles are evenly distributed on the surface of the Al2O3 powder; and
the CeO2 nanoparticles are included at 0.5-5.2 wt % of the alumina supported cerium oxide powder material.