Method for coating metal nanoparticles on oxide ceramic powder surface

Patent metadata

Field	Value
Publication number	US-10112874-B2
Application number	US-201515328094-A
Country	US
Kind code	B2
Filing date	Jun 30, 2015
Priority date	Aug 11, 2014
Publication date	Oct 30, 2018
Grant date	Oct 30, 2018

Abstract

The present invention discloses a method for uniformly coating metal nanoparticles without a carbon impurity on an oxide ceramic powder surface, which includes the steps of putting grinded and mixed a metal organic material and oxide ceramic powder into a rotational reaction chamber, then bubbling oxidizing gas under a rotational and heating condition to oxidize the metal organic material into a metal oxide, and finally bubbling reducing gas to reduce the metal oxide into nanoparticles in a metallic state, so as to implement the uniform coating of the nanoparticles in the metallic state, and avoid coarsening and growing problems of nanoparticles led by a long-term coating reaction under a high temperature. The present invention has a simple method and a short preparation period, and the metal nanoparticles prepared are uniformly dispersed and have wide application prospects in multiple fields like catalytic materials and conductive ceramics.

First claim

The invention claimed is:

1. A method for coating metal nanoparticles on an oxide ceramic surface, comprising the following steps of:
(1) blending oxide ceramic powder and a metal organic material according to a weight ratio of (1:1)-(10:1), obtaining blended powders through grinding and mixing the materials for 1-3 h, putting the grinded and blended powder into a rotational reactor, and starting up the rotational reactor to make the rotational reactor rotate, wherein the metal organic material is a stable organometallic compound formed by bonding an alkyl group or an alkyl of an aryl with a metal atom;
(2) bubbling mixed gas of oxygen and argon into the rotational reactor, keeping the temperature for 0.5-2 h after warming up to 400-500° C. at a rate of 5-10° C./min to oxidize the metal organic material into a metal oxide, and then closing a gas inlet valve for oxygen and argon; and
(3) bubbling reducing gas into the rotational reactor to reduce the metal oxide in step (2) into nanoparticles in a metallic state, cooling at a rate of 5-10° C./min, closing a gas inlet valve for reducing gas after cooling the temperature to room temperature, stopping the rotation of the rotational reactor, opening the reactor, taking the powder out, sieving and collecting the powder.

2. The method according to claim 1 , wherein the oxide ceramic powder is any one of Al 2 O 3 , ZrO 2 , SiO 2 , MgO and TiO 2 , with a particle size ranging from 100 nm to 100 μm, and a purity greater than 95%.

3. The method according to claim 1 , wherein the metal organic material is any one of nickelocene, tetracarbonyl nickel and nickel acetate.

4. The method according to claim 1 , wherein the metal organic material is copper dipivaloylmethanate.

5. The method according to claim 1 , wherein the metal organic material is cobaltocene or hydroxyl cobalt.

6. The method according to claim 1 , wherein the metal organic material is ferrocene.

7. The method according to claim 1 , wherein a total pressure of the mixed gas of oxygen and argon bubbled in step (2) ranges from 200 to 1000 Pa, a partial pressure of the oxygen ranges from 50 to 200 Pa, and a rotation rate of the rotational reactor ranges from 15 to 60 r/min.

8. The method according to claim 1 , wherein the reducing gas in step (3) is any one of hydrogen, carbonic oxide and methane, and a partial pressure of the reducing gas ranges from 100 to 400 Pa.

9. The method according to claim 1 , wherein the powder in step (3) is sieved for three times through a 50-200 mesh sieve.

Assignees

• Univ Hohai

Inventors

• Zhang Jianfeng
• Wu Yuping
• Hong Sheng
• Li Gaiye
• Guo Wenmin

Classifications

• C04B35/486

  Fine ceramics · CPC title

• C04B2235/6582

  Hydrogen containing atmosphere · CPC title

• C04B35/46

  based on titanium oxides or titanates (containing also zirconium or hafnium oxides, zirconates or hafnates C04B35/49) · CPC title

• C04B35/04

  based on magnesium oxide · CPC title

• C04B35/111

  Fine ceramics · CPC title