Copper nanoparticle and preparation method therefor

Patent metadata

Field	Value
Publication number	US-11643568-B2
Application number	US-201816612318-A
Country	US
Kind code	B2
Filing date	Mar 7, 2018
Priority date	Mar 9, 2017
Publication date	May 9, 2023
Grant date	May 9, 2023

Abstract

The present invention relates to a low-temperature sinterable copper particle material prepared using an electride and an organic copper compound and a preparation method therefor and, more particularly, to a copper nanoparticle which can be useful as a conductive copper ink material thanks to its small size and high dispersibility, and a method for preparing the copper nanoparticle by reducing an organic copper compound with an electride as a reducing agent. The present invention provides copper nanoparticles which can be suitably used as a conductive copper nanoink material because the copper nanoparticles show the restrained oxidation of the copper, have an average particle diameter of around 5 nm to cause the depression of melting point, are of high dispersibility, and allow the removal of the electride in a simple ultrasonication process. The prepared copper nanoparticles can be useful as an oxidation preventing protector or conductive copper ink material which is small in particle size and high in dispersibility.

First claim

The invention claimed is:

1. A method of manufacturing oxidation protected copper nanoparticles, the method comprising:
reducing a two-valent copper compound with at least one electride, as a reducing agent, represented by Chemical Formulas 1 to 4 below:
M 2 C(M: Y,Gd,Tb,Dy, or Ho)  <Chemical Formula 1>;

X 2 N(X: Ca,Sr, or Ba)  <Chemical Formula 2>;

Hf 2 Z(Z: S or Se)  <Chemical Formula 3>; and

C12A7(12CaO.7Al 2 O 3 )  <Chemical Formula 4>, and

wherein the two-valent copper compound is one selected from a group consisting of Cu(CH 2 COO) 2 , Cu(NO 3 ) 2 , CuCl 2 and CuSO 4 ; and
controlling an average diameter of copper nanoparticles to within 5-10 nm by adjusting a wt % of the two-valent copper compound based on mass of the electride,
wherein the two-valent copper compound is 2.5 wt % to 10 wt % based on mass of the electride.

2. The method according to claim 1 , wherein a form of the electride is a bulk, a single crystal, or a film.

3. The method according to claim 1 , wherein the two-valent copper compound is one selected from a group consisting of Cu(CH 2 COO) 2 , Cu(NO 3 ) 2 , and CuSO 4 .

4. The method according to claim 1 , wherein the at least one electride is represented by Chemical Formula 1 or Chemical Formula 3.

5. The method according to claim 1 , wherein the obtained copper nanoparticles comprise zero-valent copper.

6. The method according to claim 1 , wherein the obtained copper nanoparticles are protected from oxidation when stored at room temperature by electrons of the at least one electride.

7. A method of manufacturing copper nanoparticles by reducing a two-valent copper compound, the method comprising:
a first step of mixing the two-valent copper compound and at least one electride represented by Chemical Formulas 1 to 4 below to obtain a mixture,
M 2 C(M: Y,Gd,Tb,Dy, or Ho)  <Chemical Formula 1>,

X 2 N(X: Ca,Sr, or Ba)  <Chemical Formula 2>,

Hf 2 Z(Z: S or Se)  <Chemical Formula 3>, and

C12A7(12CaO.7Al 2 O 3 )  <Chemical Formula 4>, and

wherein the two-valent copper compound is one selected from a group consisting of Cu(CH 2 COO) 2 , Cu(NO 3 ) 2 , CuCl 2 and CuSO 4 ; and
a second step of thermally treating the mixture to obtain copper nanoparticles,
wherein an average diameter of the copper nanoparticles is controlled to be within 5-10 nm; and
a third step of removing the electride using sonication or melting with water or an alcohol solvent after the thermal treatment to selectively separate only the copper nanoparticles from a surface of the electride.

8. The method according to claim 7 , wherein, at the first step, a nonpolar organic solvent is added to the mixture.

9. The method according to claim 8 , wherein the nonpolar organic solvent comprises a linear, branched, or cyclic alkane.

10. The method according to claim 7 , wherein, at the second step, the heat treatment is performed for 10 hours to 30 hours at a temperature of 100 to 200° C.

11. The method according to claim 7 , wherein the mixing is performed such that a wt % of the two-valent copper compound is 2.5 wt % to 10 wt % based on mass of the at least one electride.

Assignees

• Research & Business Found Sungkyunkwan Univ

Inventors

• Kim Sung-Wng
• Lee Kyu-Hyoung
• Kim Ye-Ji
• Park Jong-Ho
• Lee Seung-Yong

Classifications

• C09D11/52 Primary

  Electrically conductive inks · CPC title

• B22F1/065

  Spherical particles · CPC title

• B22F1/10

  Metallic powder containing lubricating or binding agents; Metallic powder containing organic material · CPC title

• B22F2304/054

  Particle size between 1 and 100 nm · CPC title

• B22F1/054

  Nanosized particles · CPC title