Method and apparatus for producing inorganic fullerene-like nanoparticles

• US 7,018,606 B2
• Filed: 10/25/2001
• Issued: 03/28/2006
• Est. Priority Date: 10/25/2000
• Status: Expired due to Term

• Current Assignee: Yeta Research and Development Co., Ltd.
• Original Assignee: Yeda Research and Development Co. Ltd. (Weizmann Institute of Science)
• Inventors: Tenne, Reshef, Feldman, Yishay, Rosentsveig, Rita, Zak, Alla
• Primary Examiner(s): Silverman, Stanley S.
• Assistant Examiner(s): Hertzog, Ardith E
• Application Number:
  US10/415,089
• Publication Number:
  US 20040018306A1
• Time in Patent Office: 1,615 Days
• Field of Search: 423/509, 423/561.1, 427/255.28, 118/724, 118/723.VE, 977/DIG.1
• US Class Current: 423/561.1
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 17/20 Methods for preparing sulfides or polysulfides, in general ammonium sulfides or polysulfides C01C; sulfides or polysulfides of metals, other than alkali metals, magnesium, calcium, strontium and barium, see the relevant groups of subclasses C01F or C01G, according to the metal
• CPC Class Codes: C01B 19/007 Tellurides or selenides of metals C01B19/002 takes precedence
• CPC Class Codes: C01G 39/06 Sulfides
• CPC Class Codes: C01P 2004/04 obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/52 highly monodisperse size distribution
• CPC Class Codes: C01P 2004/62 Submicrometer sized, i.e. from 0.1-1 micrometer
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2004/86 Thin layer coatings, i.e. the coating thickness being less than 0.1 time the particle radius
• CPC Class Codes: Y10S 977/843 Gas phase catalytic growth, i.e. chemical vapor deposition

Abstract

A process and apparatus are presented for obtaining inorganic fullerene-like nanostructures. A metal oxide is evaporated at predetermined temperature conditions, and is swept towards a reacting zone, to which first and second gas phase reacting agents are concurrently swept. The evaporated metal oxide thus interacts with the first reacting agent and is converted into metal suboxide nanoparticles in the gas phase. The condensing metal suboxide nanoparticles interact with the second reacting agent in the gas phase resulting in substantially pure phase of the inorganic fullerene-like nanoparticles.

Claims

1. A method for obtaining inorganic fullerene-like nanostructures, the method comprising evaporation of a metal oxide at predetermined temperature conditions, wherein the metal oxide is MoO₃ or WO₃, reduction of the evaporated metal oxide by a first reacting agent being hydrogen gas to obtain a suboxide of said metal, and interaction of the suboxide with at least one second reacting agent being a volatile sulfur or selenium compound or mixtures thereof, and being characterized in that:

said evaporation occurs prior to the metal oxide arrival to a reacting zone, where the reduction and the interaction occur, and a flow of the evaporated metal oxide is driven from its initial location inside a reactor towards the reacting zone by means of an inert carrier;

a flow of the first reacting agent and the at least one second reacting agent in the gas phase is supplied into the reacting zone, such that the agents'"'"' flow meets the evaporated metal oxide flow while in an opposite upward/downward direction with respect to the reacting zone, thereby causing the first reacting agent interaction with the evaporated metal oxide prior to that of the at least one second reacting agent, the interaction between the evaporated metal oxide and the first reacting agent causing reduction of the evaporated metal oxide into metal suboxide nanoparticles in the gas phase resulting in condensation of the suboxide nanoparticles, and the interaction between said at least one second reacting agent and the condensing metal suboxide nanoparticles causing formation of substantially pure phase of inorganic fullerene-like nanostructures.

2. The method according to claim 1, wherein the first and second reacting agents are supplied into different subsequent sub-zones of the reacting zone with respect to the direction of flow of the evaporated metal oxide.

3. The method according to claim 2, wherein said reduction occurs within the first sub-zone with respect to the direction of the evaporated metal oxide flow.

4. The method according to claim 3, wherein said interaction between the condensing metal suboxide nanoparticles and the second reacting agent occurs within the subsequent sub- zone.

5. The method according to claim 1, wherein an additional second reacting agent is used, the two reacting agents forming a mixture of volatile sulfur and selenium compounds.

6. The method according to claim 5, wherein the second reacting agent is H₂S, the interaction between the second reacting agent and the condensing metal suboxide nanoparticles thereby causing sulfidization of the metal suboxide nanoparticles, thereby producing the inorganic fullerene-like nanostructures formed by metal sulfide nanoparticles.

7. The method according to claim 6, wherein the reaction product of the interaction between condensing metal suboxide nanoparticles and said second reacting agent contains particles each formed by a core of a nanosize cluster of MoO₃₋

x and coatings of MoS₂.

8. The method according to claim 1, wherein the inert carrier is N₂.

9. The method according to claim 1, wherein the supply of the first and second reacting agents is carried out by said inert carrier.

10. The method according to claim 1, wherein said driving of the flow of the evaporated metal oxide comprises controlling the rate of flow of the inert carrier.

11. The method according to claim 1, wherein the provision of the first and second reacting agents in the reacting zone comprises controlling the rate of flow of the first and second reacting agents so as to define the diffusion length for each of the reacting agents.

12. The method according to claim 1, wherein the temperature gradient within the reacting zone is in the range of 650°

C.–

950°

C.

13. The method according to claim 1 further comprising annealing of the produced nanoparticles so as to remove oxygen therefrom.