Method for preparing uniform metal oxide nanoparticles with high reproducibility

Patent metadata

Field	Value
Publication number	US-9771275-B2
Application number	US-201415101002-A
Country	US
Kind code	B2
Filing date	Nov 19, 2014
Priority date	Dec 6, 2013
Publication date	Sep 26, 2017
Grant date	Sep 26, 2017

Abstract

The present invention relates to a method for preparing uniform metal oxide nanoparticles. According to the preparation method of the present invention, it is possible to maintain the temperature and pressure inside the reactor in a stable and constant manner by removing water generated in the reaction step for forming metal oxide nanoparticles. Thus, the uniformity of nanoparticles formed is increased, and the reproducibility between batches can be increased even in a repeated process and and a large-scale reaction. Therefore, the preparation method of the present invention can be used to synthesize uniform nanoparticles reproducibly in large quantities.

First claim

What is claimed is:

1. A method for preparing metal oxide nanoparticles which comprises the steps of
injecting a metal precursor compound comprising at least one metal hydroxide selected from the group consisting of iron (Fe), cobalt (Co), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), nickel (Ni), copper (Cu), yttrium (Y), zirconium (Zr), molybdenum (Mn), ruthenium (Ru), rhodium (Rh), palladium (Pd), silver (Ag), cadmium (Cd), cerium (Ce), platinum (Pt), gold (Au), barium (Ba), strontium (Sr), lead (Pb), mercury (Hg), aluminum (Al), gallium (Ga)<indium (In), tin (Sn) and germanium (Ge), a carboxylic acid, and a solvent with a boiling point of more than 200° C. into a reactor to form a mixed solution; and
reacting the mixed solution by raising the internal temperature of the reactor up to 200 to 400° C. to form a metal oxide nanoparticle, wherein water generated in the step of reacting the mixed solution is removed,
wherein the step of reacting the mixed solution to form a metal oxide nanoparticle is carried out while refluxing a vaporized material generated in the reaction step, and wherein water cooled during the refluxing process is removed by using trap, thereby preventing re-inflow of water.

2. The method for preparing metal oxide nanoparticles according to claim 1 , wherein after raising the internal temperature of the reactor, the reactor is maintained at the set temperture for more than 5 minutes.

3. The method for preparing metal oxide nanoparticles according to claim 1 , wherein after raising the internal temperature of the reactor, the internal temperature (T′) of the reactor is maintained at T−5° C.≦T′≦T+5° C. with respect to the set temperature (T).

4. The method for preparing metal oxide nanoparticles according to claim 1 , wherein the metal oxide nanoparticles have an average particle size of 2 to 50 nm.

5. The method for preparing metal oxide nanoparticles according to claim 4 , wherein a coefficient of variation (CV) of the particle size of the metal oxide nanoparticles is 10% or less.

6. The method for preparing metal oxide nanoparticles according to claim 1 , wherein the metal precursor compound is iron hydroxide (FeOOH).

7. The method for preparing metal oxide nanoparticles according to claim 1 , wherein the carboxylic acid includes one or more selected from the group consisting of oleic acid, stearic acid, lauric acid, palmitic acid, octanoic acid and decanoic acid.

8. A method for preparing iron oxide nanoparticles which comprises the steps of injecting 100 parts by weight of iron hydroxide (FeOOH), 1,000 to 1,400 parts by weight of oleic acid, and 1,200 to 1,500 parts by weight of octadecene into the reactor to form a mixed solution; and
reacting the mixed solution by raising the internal temperature of the reactor up to 310±5° C. to form an iron oxide nanoparticle, wherein water generated in the step of reacting the mixed solution is removed.

9. The method for preparing iron oxide nanoparticles according to claim 8 , wherein the iron oxide nanoparticles with a particle diameter of 10 to 15 nm account for more than 90% by weight.

Assignees

• Hanwha Chemical Corp

Inventors

• Park Ju Young
• Kim Eung Gyu
• Myeong Wan Jae
• Jeon Bong Sik
• Kwon Eun Byul

Classifications

• C01P2004/04

  obtained by TEM, STEM, STM or AFM · CPC title

• C01G45/02

  Oxides · CPC title

• C01B13/18

  by thermal decomposition of compounds, e.g. of salts or hydroxides · CPC title

• Y10S977/773

  Nanoparticle, i.e. structure having three dimensions of 100 nm or less · CPC title

• C01G39/02

  Oxides; Hydroxides · CPC title