Process for the preparation of nanoparticles

Patent metadata

Field	Value
Publication number	US-11377366-B2
Application number	US-201716319657-A
Country	US
Kind code	B2
Filing date	Jul 26, 2017
Priority date	Jul 27, 2016
Publication date	Jul 5, 2022
Grant date	Jul 5, 2022

Abstract

The present invention relates to a “safety-by-design” method for the preparation of nanoparticles, to a method for the preparation of a nanocomposite material, and to the use of a direct liquid injection device so as to prepare nanoparticles or nanocomposite materials in a “safety-by-design” process.

First claim

The invention claimed is:

1. A method for the preparation of nanoparticles selected from the group consisting of metal nanoparticles, metal oxide nanoparticles and semiconductor nanoparticles,
wherein said method is implemented in a device comprising:
at least one reacting chamber including at least one first inlet for admission of said liquid phase in said reacting chamber, at least one second inlet for admission of said gas phase in said reacting chamber, and an outlet for expulsion of said nanoparticles from said reacting chamber,
a liquid injector arranged upstream of the first inlet for injecting or spraying said liquid phase into said reacting chamber,
an injector of nanoparticles arranged downstream of the outlet for injecting or spraying said nanoparticles through an outlet of said nanoparticles injector, and
control means for controlling the injection or the spray of said liquid phase and/or said nanoparticles, and wherein said method comprises:
a step 1) of injecting a liquid phase comprising at least one nanoparticles precursor selected from the group consisting of precursors of metals, precursors of metal oxides and precursors of semiconductors in said reacting chamber through said liquid injector,
a step 2) of contacting said liquid phase with a gas phase comprising at least one carrier gas and at least one reacting gas, said step 2) being carried out in said reacting chamber,
a step 3) of reacting the nanoparticles precursor with the reacting gas so as to form nanoparticles, and
a step 4) of expulsion of the nanoparticles produced in step 3) from the reacting chamber through the nanoparticles injector, said nanoparticles being under the form of an aerosol at the outlet of the nanoparticles injector.

2. The method according to claim 1 , wherein the nanoparticles precursor used in step 1) is either liquid at ambient temperature or dissolved in a solvent so as to form a liquid phase at ambient temperature.

3. The method according to claim 1 , wherein the liquid phase further comprises at least one stabilizing agent.

4. The method according to claim 1 , wherein the device further comprises a tank T 1 for containing the liquid phase, said tank T 1 being connected by a conduit or a supply line to the first inlet of the reacting chamber.

5. The method according to claim 4 , wherein the tank T 1 is connected to a tank T 2 of pressurized gas, so as to enable the introduction of the pressurized gas through the upper portion of the tank T 1 .

6. The method according to claim 5 , wherein the pressure P 2 in the tank T 2 is at least 1.5 bar above the atmospheric pressure.

7. The method according to claim 4 , wherein said method comprises prior to step 1), a step i) of preparing the liquid phase in the tank T 1 .

8. The method according to claim 1 , wherein the control means control the flow rate of the liquid injector and during step 1) the duration of the opening of the liquid injector ranges from 1 ms to 20 ms.

9. The method according to claim 1 , wherein during step 1), the frequency of the injection of the liquid injector can range from 1 Hz to 50 Hz.

10. The method according to claim 1 , wherein the device further comprises a tank T 3 for containing the gas phase and possibly a reacting liquid, said tank T 3 being connected by a conduit or a supply line to the second inlet of the reacting chamber.

11. The method according to claim 10 , wherein the tank T 3 is connected to a tank T 4 for containing the carrier gas.

12. The method according to claim 11 , wherein the pressure in the tank T 4 is at least equal to a pressure P 4 =Pressure in the tank T 2 -0.5 bar.

13. The method according to claim 10 , wherein said method comprises prior to step 2), a step i′) of preparing the gas phase in the tank T 3 and a step ii′) of introducing the gas phase in the reacting chamber through the second inlet.

14. The method according to claim 1 , wherein during step 4) the duration of the opening of the nanoparticles injector ranges from 1 ms to 20 ms.

15. The method according to claim 1 , wherein during step 4), the frequency of the injection of the nanoparticles injector ranges from 1 Hz to 50 Hz.

16. The method according to claim 1 , wherein step 3) is a chemical reaction involving the reaction of an organometallic compound with water.

17. A method for the preparation of a nanocomposite material comprising nanoparticles and at least one matrix material, wherein the method comprises at least the following steps:
A) a step of preparing nanoparticles according to the method as defined in claim 1 ,
B) a step of dispersing said nanoparticles with a matrix material or a precursor of a matrix material, and
C) a step of producing the nanocomposite material, and wherein step B) is carried out either in the reacting chamber of the device or in a process chamber which is connected to the outlet of the nanoparticles injector of the device.

18. The method according to claim 17 , wherein step C) is chosen from a polymerization step, a deposition step, a sol-gel process, any conventional plastic forming step and a mixture thereof.

19. A device comprising:
at least one reacting chamber including at least one first inlet for admission of a liquid phase comprising at least one nanoparticles precursor selected from the group consisting of precursors of metals, precursors of metal oxides and precursors of semiconductors in said reacting chamber,
at least one second inlet for admission of a gas phase comprising at least one carrier gas and at least one reacting gas in said reacting chamber, and
an outlet for expulsion of nanoparticles selected from the group consisting of metal nanoparticles, metal oxide nanoparticles and semiconductor nanoparticles from said reacting chamber, wherein
a liquid injector is arranged upstream of the first inlet for injecting or spraying said liquid phase into said reacting chamber,
a nanoparticles injector is arranged downstream of the outlet for injecting or spraying said nanoparticles through an outlet of said nanoparticles injector, and
a control means is configured to control the injection or the spray of said liquid phase and/or said nanoparticles, for the preparation of said nanoparticles or of a nanocomposite material, by contacting in the reacting chamber of the device the liquid phase comprising the at least one nanoparticles precursor with the gas phase comprising the at least one carrier gas and the at least one reacting gas.

Assignees

• Centre Nat Rech Scient
• Inst Nat Polytechnique Toulouse
• Univ Toulouse Iii—Paul Sabatier

Inventors

• Kahn Myrtil
• Champouret Yohan
• Clergereaux Richard
• Vahlas Constantin
• Mingotaud Anne-Francoise
• Carnide Guillaume

Classifications

• C01P2004/04

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

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C01G9/02

  Oxides; Hydroxides · CPC title

• C01G19/02

  Oxides · CPC title

• B01J4/002

  Nozzle-type elements (nozzle-type reactors B01J19/26) · CPC title