Nanostructured multi-component and doped oxide powders and method of making same

• US 7,182,929 B1
• Filed: 08/18/2004
• Issued: 02/27/2007
• Est. Priority Date: 08/18/2003
• Status: Expired due to Fees

• Current Assignee: NEI, Inc.
• Original Assignee: NEI, Inc.
• Inventors: Singhal, Amit, Skandan, Ganesh, Jain, Mohit
• Primary Examiner(s): Vanoy; Timothy C.
• Application Number:
  US10/920,898
• Time in Patent Office: 923 Days
• Field of Search: 423/592.1, 423/593.1, 423/600, 423/594.16, 423/111, 423/155, 423/625, 423/594.14, 423/99, 423/598, 423/69, 423/335, 423/326, 423/610, 423/263, 423/21.1, 423/632, 423/633, 423/138, 423/635, 423/608, 423/618, 423/89, 423/622, 977/773, 977/775, 977/776, 977/777, 977/811
• US Class Current: 423/592.1
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 13/145 After-treatment of oxides or hydroxides, e.g. pulverising, drying, decreasing the acidity
• CPC Class Codes: C01F 7/162 Magnesium aluminates
• CPC Class Codes: C01G 23/047 Titanium dioxide
• CPC Class Codes: C01G 9/02 Oxides; Hydroxides
• CPC Class Codes: C01P 2002/32 spinel-type (AB2O4)
• CPC Class Codes: C01P 2002/54 one element only
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2004/50 Agglomerated particles
• 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 2006/12 Surface area
• CPC Class Codes: Y10S 977/773 Nanoparticle, i.e. structure having three dimensions of 100 nm or less
• CPC Class Codes: Y10S 977/775 Nanosized powder or flake, e.g. nanosized catalyst
• CPC Class Codes: Y10S 977/776 Ceramic powder or flake
• CPC Class Codes: Y10S 977/777 Metallic powder or flake
• CPC Class Codes: Y10S 977/811 Of specified metal oxide composition, e.g. conducting or semiconducting compositions such as ITO, ZnOx

Abstract

A method for producing nanostructured multi-component or doped oxide particles and the particles produced therein. The process includes the steps of (i) dissolving salts of cations, which are either dopants or components of the final oxide, in an organic solvent; (ii) adding a dispersion of nanoparticles of a single component oxide to the liquid solution; (iii) heating the liquid solution to facilitate diffusion of cations into the nanoparticles; (iv) separating the solids from the liquid solution; and (v) heat treating the solids either to form the desired crystal structure in case of multi-component oxide or to render the homogeneous distribution of dopant cation in the host oxide structure. The process produces nanocrystalline multi-component or doped oxide nanoparticles with a particle size of 5–500 nm, more preferably 20–100 nm; the collection of particles have an average secondary (or aggregate) particle size is in the range of 25–2000 nm, preferably of less than 500 nm.

Claims

1. A method of producing nanostructured multi-component or doped oxide particles, comprising the following steps:

a. proportioning the salts of cations, which are either dopants or components of the final oxide, and a dispersion of nanoparticles of a single component oxide so as to form the proportions of the desired multi-component or doped oxide particles;

b. dissolving the salts of cations, in an liquid organic solvent;

c. adding the dispersion of nanoparticles of the single component oxide to the liquid solution;

d. heating the liquid solution to facilitate diffusion of cations into the nanoparticles;

e. separating the solids from the liquid solution; and

f. heat treating the solids to form the desired crystal structure.

2. The method as claimed in claim 1, wherein the cation salt is selected from the group consisting of:

metal nitrate, metal hydroxide, metal carbonate, metal chloride, metal acetate and metal iodide.

3. The method as claimed in claim 1, wherein the organic solvent has a boiling point in the range of 150–

300°

C.

4. The method as claimed in claim 1, wherein average primary particle size of single component oxide nanoparticles is in the range of 5–

500 nm, and the average aggregate particle size is in the range of 25–

2000 nm.

5. The method as claimed in claim 1, wherein the heating step comprises refluxing.

6. The method as claimed in claim 1, wherein the heating step comprises refluxing between 5 to 40 hrs.

7. The method as claimed in claim 1, wherein the heating step is conducted at an atmospheric pressure in the range of 0.5 to 10 atmospheres.

8. The method as claimed in claim 1, wherein solid particles are separated from the liquid solution by at least one of the following methods:

filtration, evaporation and centrifuging.

9. The method as claimed in claim 1, wherein the solids are heat treated at a temperature of 250–

1000°

C.

10. The method as claimed in claim 1, wherein the solids are heat treated at a temperature of 600–

900°

C.

11. The method as claimed in claim 1, wherein the single component oxide is selected from the group consisting of:

silicon dioxide, titanium dioxide, yttrium oxide, aluminum oxide, cerium oxide, iron oxide, magnesium oxide, titanium oxide, zirconium oxide, tin oxide and zinc oxide.

12. The method as claimed in claim 1, wherein the solids are heat treated for a period of 2–

8 hrs.

13. The method as claimed in claim 1, wherein the solids are heat treated in an atmosphere containing O₂.

14. The method as claimed in claim 1, wherein the solids are heat treated in an atmosphere containing an inert atmosphere.

15. A method of producing a collection of multi-component or doped oxide nanoparticles, wherein the average primary particle size of the nanoparticles is in the range of 5–

500 nm, and the average aggregate particle size is in the range of 25–

2000 nm, the method comprising the following steps;

a. providing the salts of cations, which are either dopants or components of the final oxide;

b. providing a dispersion of nanoparticles of a single component oxide;

c. proportioning the salts of cations and the dispersion of nanoparticles so as to form the proportions of the desired multi-component or doped oxide particles;

d. dissolving the salts of cations in an liquid organic solvent;

e. adding the dispersion of nanoparticles of the single component oxide to the liquid solvent solution;

f. heating the liquid solution to facilitate diffusion of the cations into the nanoparticles;

g. separating the solids from the liquid solution; and

h. heat treating the solids to form the desired crystal structure of the final oxide.

16. The method as claimed in claim 15 wherein the multi-component nanoparticles have a first and second component, at least one of the first and second components being a metal.

17. The method as claimed in claim 15, wherein each of the nanoparticles has a particle size of 20–

100 nm;

the collection of particles having an aggregate particle size of less than 500 nm.

18. The method as claimed in claim 15, wherein the amount of cations is proportioned such that it acts as a dopant.

19. The method as claimed in claim 15, wherein the single component oxide is selected from the group consisting of:

silicon dioxide, titanium dioxide, yttrium oxide, aluminum oxide, cerium oxide, iron oxide, magnesium oxide, titanium oxide, zirconium oxide, tin oxide and zinc oxide.

20. The method as claimed in claim 15, wherein the first component comprises γ

-aluminum oxide and the second component comprises magnesium.

21. The method as claimed in claim 15, wherein the first component comprises titanium dioxide and the second component comprises a rare earth metal proportioned such that it acts as a dopant.

22. The method as claimed in claim 15, wherein the first component comprises zinc oxide and the second component comprises aluminum proportioned such that it acts as a dopant.