Synthesis of nanoparticles with a closed structure of metal chalcogens having a lamellar crystalographic structure
View Patent ↗The invention relates to a spray pyrolysis method characterized in that it is used in the synthesis of nanoparticles with a closed structure of metal chalcogens having a lamellar crystalographic structure of general formula M a X b , wherein M represents a metal and X represents a chalcogen, a and b represent the respective proportions of metal and chalcogen, and in that it comprises pyrolysis of a liquid aerosol obtained from a solution of at least one metal precursor (M) and a chalcogen (X), or at least one precursor of said metal (M) and at least one precursor of said chalcogen (X) dissolved in a solvent, said solution being atomized into fine droplets in a suspension in a vector gas.
1. A spray pyrolysis method for the synthesis of closed-structure nanoparticles of metal chalcogenides having a lamellar crystallographic structure, of the general formula (I) M a X b , said method comprising the steps of:
(a) providing a solution of at least one precursor having the formula (II) (A) c M(X) d dissolved in a solvent,
(b) providing a liquid aerosol by atomizing the solution obtained in step a) into fine droplets in suspension in an inert carrier gas, and
(c) pyrolyzing the liquid aerosol obtained in step c); wherein, in formulas (I) and (II):
A represents a cation,
M represents a transition metal or a metal from group III, IV or V of the periodic table of the elements,
X represents a chalcogen selected from oxygen, sulfur, selenium and tellurium, a and b each represents the proportion of metal and of chalcogen, respectively, in formula (I),
c and d each represents the proportion of cations and of chalcogens, respectively, in formula (II),
M and X represent a metal and a chalcogen, respectively, of a metal chalcogenide M a X b having a lamellar crystallographic structure.
2. The method as claimed in claim 1 , said method comprising the following steps:
forming said solution of said at least one precursor having the formula (II) in a solvent,
atomizing said solution in liquid aerosol form by a nebulizer, through which the carrier gas is flowing,
injecting the aerosol into a heated furnace to evaporate the solvent and to react and/or break down said at least one precursor having the formula (II) so as to form the nanoparticles,
transporting the nanoparticles to the furnace outlet using the carrier gas, and
recovering the nanoparticles at the furnace outlet.
3. The method as claimed in claim 1 , wherein A is K + , Na + or NH4 + .
4. The method as claimed in claim 1 , wherein M is a transition metal selected from among Ti, Zr, Hf, V, Nb, Ta, Mo, W, Re, Co, Ni, Pt, Pd, Cr and Ru.
5. The method as claimed in claim 1 , wherein M is Ga or In.
6. The method as claimed in claim 1 , wherein M is Sn, Pb or Ge.
7. The method as claimed in claim 1 , wherein M is Bi.
8. The method as claimed in claim 3 , wherein said at least one precursor of formula (II) is a tetrathiometallate or a tetraselenometallate.
9. The method as claimed in claim 8 , wherein M is molybdenum or tungsten.
10. The method as claimed in claim 1 , wherein said carrier gas is an inert gas selected from nitrogen and argon and/or hydrogen.
11. The method as claimed in claim 1 , wherein said solvent is a polar solvent.
12. The method as claimed in claim 1 , wherein said nanoparticles are nanotubes, fullerenes and/or nanoboxes.
13. The method as claimed in claim 2 , wherein the nebulizer is a pneumatic or ultrasonic type nebulizer.
14. the method as claimed in claim 11 , wherein the solvent is water, ethanol, or a mixture thereof.