Synthesis of nanomaterials

Patent metadata

Field	Value
Publication number	US-9610612-B2
Application number	US-201214357428-A
Country	US
Kind code	B2
Filing date	Nov 12, 2012
Priority date	Nov 10, 2011
Publication date	Apr 4, 2017
Grant date	Apr 4, 2017

Abstract

A method is disclosed for synthesis of nanoparticles of metal selenide, metal selenide alloys, metal chalcogenide comprising at least selenium or metal chalcogenide alloys comprising at least selenium. The method comprises obtaining a heterogeneous dispersion of powder at least selenium in a first solvent at a first temperature, the first temperature being such that the heterogeneous dispersion comprises at least a fraction of undissolved powder in the solvent. The method also comprises introducing the heterogeneous dispersion into a second solvent containing a metal cation precursor, the second solvent being at a second temperature higher than said first temperature allowing, upon introduction of the heterogeneous dispersion, dissolution of at least the fraction of the power resulting in nucleation of the nanoparticles. The method results in efficient and easy production of nanoparticles.

First claim

The invention claimed is:

1. A method for synthesis of nanoparticles of metal selenide, metal selenide alloys, metal chalcogenides comprising at least selenium or metal chalcogenide alloys comprising at least selenium, the method comprising:
obtaining a heterogeneous dispersion of powder of at least selenium in a first solvent at a first temperature, the first temperature being such that the heterogeneous dispersion comprises at least a fraction of undissolved powder in the solvent;
providing a metal cation precursor and introducing the heterogeneous dispersion into a second solvent, the second solvent being at a second temperature higher than said first temperature allowing, upon introduction of the heterogeneous dispersion, dissolution of at least the fraction of the powder resulting in nucleation of the nanoparticles.

2. A method according to claim 1 , wherein said obtaining and/or said introducing is performed under atmospheric conditions.

3. A method according to claim 1 , wherein the first and/or the second solvent is a non-coordinating solvent.

4. A method according to any of claim 1 , wherein the first and/or the second solvent is a coordinating solvent.

5. A method according to claim 1 , wherein the method further comprises selecting or tuning any or a combination of a concentration or ratio of concentrations of components in the dispersion and/or the second solvent used, the type of the first solvent and the type of the second solvent as function of a predetermined dimension of the nanoparticles to be obtained.

6. A method according to claim 1 , wherein the method further comprises adding ligands with a selected or tuned chain length for obtaining a predetermined dimension of the nanoparticles.

7. A method according to claim 1 , wherein introducing the heterogeneous dispersion into a second solvent comprises performing hot injection.

8. A method according to claim 1 , wherein the method further comprises after said obtaining a heterogeneous dispersion and after said introducing into a second solvent, the step of forming a shell around the nanoparticles already formed.

9. A method according to claim 8 , wherein the shell material comprises nanoparticles of metal selenium, metal selenide alloys, metal chalcogenide comprising at least selenium or metal chalcogenide alloys comprising at least selenium, and wherein forming the shell comprises
obtaining a second heterogeneous dispersion of powder of one or more of the group of selenium, sulfur or tellurium in a third solvent at a low temperature, the low temperature being such that the second heterogeneous dispersion comprises at least a fraction of undissolved powder in the further solvent, and
introducing the second heterogeneous dispersion into fourth solvent comprising the nanoparticles already formed and a metal cation precursor, the solvent being at a temperature allowing, upon introduction of the second heterogeneous dispersion, dissolution of the powder resulting in nucleation of shell formation around the core.

10. A method according to claim 1 , the method further comprising quenching the reaction mixture after formation of the nanoparticles.

11. A method according to claim 1 , wherein providing a metal cation precursor is performed by providing the metal cation precursor in the second solvent.

12. A method according to claim 1 , wherein providing a metal cation precursor is performed by providing the metal cation precursor in the heterogeneous dispersion.

Assignees

• Univ Gent

Inventors

• Hens Zeger
• Flamee Stijn

Classifications

• C01P2004/80

  Particles consisting of a mixture of two or more inorganic phases · CPC title

• C01P2004/52

  highly monodisperse size distribution · CPC title

• C01P2002/84

  by UV- or VIS- data · CPC title

• C01P2002/72

  by d-values or two theta-values, e.g. as X-ray diagram · CPC title

• C01P2004/04

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