Process for purifying metal nanowires

Patent metadata

Field	Value
Publication number	US-2017120341-A1
Application number	US-201515313038-A
Country	US
Kind code	A1
Filing date	May 19, 2015
Priority date	May 20, 2014
Publication date	May 4, 2017
Grant date	—

Abstract

Isolating metal nanowires from a reaction mixture also containing ancillary inorganic particles distinct from the nanowires, includes: providing a mixture of metal nanowires with large particles having at least two dimensions 250 nm or more, and small particles of which the largest dimension is less than 200 nm, in the form of a dispersion in a solvent medium having a viscosity at 25° C. 10 mPa·s or more; leaving the mixture to settle out under conditions conducive to the formation of a supernatent phase including the small particles and of a precipitate comprising the metal nanowires and the large particles; isolating the precipitate, and dispersing the isolated precipitate in a solvent medium having a viscosity at 25° C. less than 10 mPa·s; leaving the suspension to settle out under conditions conducive to the precipitation of said large particles; and recovering the nanowires in the form of a dispersion in the supernatent phase.

First claim

1 . A process useful for isolating metal nanowires from a reaction mixture for the synthesis thereof, the reaction mixture also containing ancillary inorganic particles distinct from the nanowires, the method comprising:
(i) providing a mixture of metal nanowires with large particles having at least two dimensions greater than or equal to 250 nm, and small particles of which the largest dimension is strictly less than 200 nm, in the form of a dispersion in a solvent medium S1 having a viscosity at 25° C. greater than or equal to 10 mPa·s; (ii) leaving said mixture to settle out under conditions conducive to the formation of a supernatent phase comprising said small particles and of a precipitate comprising the metal nanowires and said large particles; (iii) isolating the precipitate obtained at the end of the settling out (ii), and dispersing the isolated precipitate in a solvent medium S2 having a viscosity at 25° C. strictly less than 10 mPa·s; (iv) leaving the suspension formed in step (iii) to settle out under conditions conducive to the precipitation of said large particles; and (v) recovering the nanowires in the form of a dispersion in the supernatent phase obtained at the end of the settling out (iv).

2 . The process as claimed in claim 1 , wherein said metal nanowires are silver nanowires.

3 . The process as claimed in claim 1 , wherein the mixture of step (i) has a concentration of metallic material forming said nanowires, between 0.1 and 10 g/l.

4 . The process as claimed in claim 1 , wherein said solvent medium S1 has a viscosity at 25° C. between 10 and 50 mPa·s.

5 . The process as claimed in claim 1 , wherein said solvent medium S1 is formed from one or more solvents elected from the group consisting of polyols having from 2 to 6 carbon atoms, in particular diols having from 2 to 4 carbon atoms.

6 . The process as claimed in claim 1 , wherein the settling out in step (ii) is performed for a duration ranging from 6 hours to 7 days.

7 . The process as claimed in claim 1 , wherein the solvent medium S2 has a viscosity at 25° C. less than or equal to 5 mPa·s.

8 . The process as claimed in claim 1 , wherein said solvent medium S2 is formed from one or more solvents selected from the group consisting of monoalcohols having from 1 to 6 carbon atoms and water.

9 . The process as claimed in claim 1 , wherein said solvent medium S2 is formed from one or more solvents selected from the group consisting of methanol, ethanol and propanol.

10 . The process as claimed in claim 1 , wherein the suspension formed in step (iii) has a concentration of metallic material forming said nanowires between 0.1 and 10 g/l.

11 . The process as claimed in claim 1 , wherein the settling out in step (iv) is performed for a duration ranging from 1 hour to 4 days.

12 . The process as claimed in claim 1 , comprising one or more subsequent steps (vi) of washing the supernatent phase recovered in step (v) in order to remove the organic residues.

Assignees

• Commissariat Energie Atomique

Inventors

• Simonato Jean-Pierre
• Celle Caroline
• Lescouet Tristan
• Mayousse Céline

Classifications

• B22F1/0547

  Nanofibres or nanotubes · CPC title

• B22F1/0545

  Dispersions or suspensions of nanosized particles · CPC title

• B22F9/24 Primary

  starting from liquid metal compounds, e.g. solutions · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• B01D21/00

  Separation of suspended solid particles from liquids by sedimentation ({separation of ores or the like by sedimentation B03B5/48 - B03B5/60} ; differential sedimentation B03D3/00; {purification of water, waste water, sewage or sludge C02F, e.g.} devices for separating or removing fatty or oily substances or similar floating material from water, waste water or sewage C02F1/40) · CPC title