Nanoparticles

• US 7,867,557 B2
• Filed: 08/14/2006
• Issued: 01/11/2011
• Est. Priority Date: 08/12/2005
• Status: Active Grant

• Current Assignee: Nanoco Technologies Limited (Nanoco Group Plc)
• Original Assignee: Nanoco Technologies Limited (Nanoco Group Plc)
• Inventors: Daniels, Steven, O'Brien, Paul, Pickett, Nigel
• Primary Examiner(s): Cleveland; Michael
• Assistant Examiner(s): Jiang; Lisha
• Application Number:
  US11/997,973
• Publication Number:
  US 20080220593A1
• Time in Patent Office: 1,611 Days
• Field of Search: 257/14, 427/212, 427/214, 427/215, 428/403, 428/404, 428/405
• US Class Current: 427/214
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 19/007 Tellurides or selenides of metals C01B19/002 takes precedence
• CPC Class Codes: C01G 9/08 Sulfides
• CPC Class Codes: C01P 2002/84 by UV- or VIS- data
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2004/84 one phase coated with the other
• CPC Class Codes: C09K 11/02 Use of particular materials as binders, particle coatings or suspension media therefor
• CPC Class Codes: C09K 11/025 non-luminescent particle coatings or suspension media
• CPC Class Codes: C09K 11/565 with zinc cadmium
• CPC Class Codes: C09K 11/883 with zinc or cadmium
• CPC Class Codes: C30B 29/605 Products containing multiple oriented crystallites, e.g. columnar crystallites
• CPC Class Codes: C30B 7/00 Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions from molten solvents C30B9/00; by normal or gradient freezing C30B11/00; under a protective fluid C30B27/00
• CPC Class Codes: C30B 7/005 Epitaxial layer growth
• CPC Class Codes: H01L 31/0296 including, apart from doping material or other impurities, only AIIBVI compounds, e.g. CdS, ZnS, HgCdTe
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]
• CPC Class Codes: Y10T 428/2991 Coated
• CPC Class Codes: Y10T 428/2993 Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
• CPC Class Codes: Y10T 428/2995 Silane, siloxane or silicone coating
• CPC Class Codes: Y10T 428/2996 Glass particles or spheres

Abstract

Method for producing a nanoparticle comprised of core, first shell and second shell semiconductor materials. Effecting conversion of a core precursor composition comprising separate first and second precursor species to the core material and then depositing said first and second shells. The conversion is effected in the presence of a molecular cluster compound under conditions permitting seeding and growth of the nanoparticle core. Core/multishell nanoparticles in which at least two of the core, first shell and second shell materials incorporate ions from groups 12 and 15, 14 and 16, or 11, 13 and 16 of the periodic table. Core/multishell nanoparticles in which the second shell material incorporates at least two different group 12 ions and group 16 ions. Core/multishell nanoparticles in which at least one of the core, first and second semiconductor materials incorporates group 11, 13 and 16 ions and the other semiconductor material does not incorporate group 11, 13 and 16 ions.

Claims

1. A method for producing a nanoparticle comprised of a core comprising a core semiconductor material, a first layer comprising a first semiconductor material provided on said core and a second layer comprising a second semiconductor material provided on said first layer, said core semiconductor material being different to said first semiconductor material and said first semiconductor material being different to said second semiconductor material, the method comprising:

effecting conversion of a nanoparticle core precursor composition to the material of the nanoparticle core;

depositing said first layer on said core; and

depositing said second layer on said first layer, said core precursor composition comprising a first precursor species containing a first ion to be incorporated into the growing nanoparticle core and a separate second precursor species containing a second ion to be incorporated into the growing nanoparticle core,

said conversion being effected in the presence of a molecular cluster compound different from the nanoparticle core precursor composition.

2. The method of claim 1, wherein a ratio of the number of moles of cluster compound compared to a total number of moles of the first and second precursor species lies in the range 0.0001-0.1:

1.

3. The method of claim 1, wherein a molar ratio of the first precursor species to the second precursor species lies in the range 100-1:

1.

4. The method of claim 1, wherein the molecular cluster compound and the core precursor composition are dispersed in a dispersing medium at a first temperature and a temperature of the dispersing medium containing the cluster compound and the core precursor composition is then increased to a second temperature greater than the first temperature.

5. The method of claim 4, wherein the first temperature is in the range 50°

C. to 100°

C.

6. The method of claim 4, wherein the second temperature is in the range 120°

C. to 280°

C.

7. The method of claim 1, the method comprising:

a. dispersing the molecular cluster compound and an initial portion of the nanoparticle core precursor composition which is less than a total amount of the core precursor composition to be used to produce said nanoparticle cores in a suitable dispersing medium at a first temperature;

b. increasing a temperature of the dispersing medium containing the cluster compound and the core precursor composition to a second temperature greater than the first temperature; and

c. thereafter, adding one or more further portions of the core precursor composition to the dispersing medium containing the growing nanoparticle cores,

wherein the temperature of the dispersing medium containing the growing nanoparticle cores is further increased above the second temperature at least one of before, during, or after the addition of the initial portion or each further portion of the nanoparticle core precursor composition.

8. The method of claim 7, wherein the temperature of the dispersing medium containing the growing nanoparticle cores is increased to the second temperature at a rate in the range 0.05°

C./min to 1°

C./min.

9. The method of claim 7, wherein said first temperature is in the range 15°

C. to 60°

C.

10. The method of claim 7, wherein said second temperature is in the range 90°

C. to 150°

C.

11. The method of claim 7, wherein the initial portion or each further portion of the nanoparticle core precursor composition is added dropwise to the dispersing medium containing the growing nanoparticle cores.

12. The method of claim 7, wherein said initial portion of the nanoparticle core precursor composition is less than or equal to approximately 90% of the total amount of the nanoparticle core precursor composition to be used to produce said nanoparticle cores.

13. The method of claim 7, wherein one further portion of the nanoparticle core precursor composition is added to the dispersing medium containing the growing nanoparticle cores and said one further portion is less than or equal to approximately 90% of the total amount of the nanoparticle core precursor composition to be used to produce said nanoparticle cores.

14. The method of claim 7, wherein a plurality of further portions of the nanoparticle core precursor composition is added to the dispersing medium containing the growing nanoparticle cores and each of said further portions is less than or equal to approximately 45% of the total amount of the nanoparticle core precursor composition to be used to produce said nanoparticle cores.

15. The method of claim 7, wherein formation of said molecular cluster compound is effected in situ in said dispersing medium prior to dispersing the molecular cluster compound and the initial portion of the nanoparticle core precursor composition in said dispersing medium.

16. The method of claim 1, wherein conversion of the core precursor composition to the nanoparticle core is effected in a reaction medium and said nanoparticle core is isolated from said reaction medium prior to deposition of the first layer.

17. The method of claim 1, wherein:

a) at least two of the core, first shell and second shell materials incorporate ions from groups 12 and 15 of the periodic table, groups 14 and 16 of the periodic table, or groups 11, 13 and 16 of the periodic table;

or

b) the second shell material incorporates ions of at least two different elements from group 12 of the periodic table and ions from group 16 of the periodic table;

or

c) at least one of the core, first and second semiconductor materials incorporates ions from groups 11, 13 and 16 of the periodic table and at least one other of the core, first and second semiconductor materials is a semiconductor material not incorporating ions from groups 11, 13 and 16 of the periodic table.