METHODS FOR MAKING METAL-CONTAINING NANOPARTICLES OF CONTROLLED SIZE AND SHAPE

• US 20080164141A1
• Filed: 01/08/2007
• Published: 07/10/2008
• Est. Priority Date: 01/08/2007
• Status: Abandoned Application

• Current Assignee: Afton Chemical Corporation (Newmarket Corporation), Virginia Commonwealth University
• Original Assignee: Afton Chemical Corporation (Newmarket Corporation), Virginia Commonwealth University
• Inventors: Panda, Asit Baran, El-Shall, Mohamed Samy Sayed, Aradi, Allen A., Jao, Tze-Chi
• Application Number:
  US11/620,773
• Publication Number:
  US 20080164141A1
• Time in Patent Office: Days
• US Class Current: 204/157.21
• CPC Class Codes: B82Y 30/00 Nanotechnology for materials or surface science, e.g. nanocomposites
• CPC Class Codes: C01B 13/18 by thermal decomposition of compounds, e.g. of salts or hydroxides
• 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 19/002 Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions
• CPC Class Codes: C01B 19/007 Tellurides or selenides of metals C01B19/002 takes precedence
• CPC Class Codes: C01F 17/235 Cerium oxides or hydroxides
• CPC Class Codes: C01G 1/00 Methods of preparing compounds of metals not covered by subclasses C01B, C01C, C01D, or C01F, in general electrolytic production of inorganic compounds C25B1/00
• CPC Class Codes: C01G 1/02 Oxides
• CPC Class Codes: C01G 1/12 Sulfides
• CPC Class Codes: C01G 45/00 Compounds of manganese
• CPC Class Codes: C01G 45/1221 Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
• CPC Class Codes: C01G 49/0018 Mixed oxides or hydroxides, C01G49/0009 takes precedence
• CPC Class Codes: C01G 51/00 Compounds of cobalt
• CPC Class Codes: C01G 9/00 Compounds of zinc
• CPC Class Codes: C01P 2002/32 spinel-type (AB2O4)
• CPC Class Codes: C01P 2002/50 Solid solutions
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2002/84 by UV- or VIS- data
• CPC Class Codes: C01P 2004/04 obtained by TEM, STEM, STM or AFM
• CPC Class Codes: C01P 2004/10 extending in one dimension, e.g. needle-like
• CPC Class Codes: C01P 2004/16 : Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
• CPC Class Codes: C01P 2004/20 : extending in two dimensions, e.g. plate-like
• CPC Class Codes: C01P 2004/32 : Spheres
• CPC Class Codes: C01P 2004/38 : cube-like
• CPC Class Codes: C01P 2004/64 : Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2004/82 : two phases having the same anion, e.g. both oxidic phases

Abstract

A method for producing metal-containing nanoparticles. The method includes combining a metal organic compound selected from metal acetates, metal acetyl acetonates, and metal xanthates with an amine to provide a solution of metal organic compound in the amine. The solution is then irradiated with a high frequency radiation source to provide metal nanoparticles having the formula (A_a)_m(B_b)_nX_x, wherein each of A and B is selected from a metal, X is selected from the group consisting of oxygen, sulfur, selenium, phosphorus, halogen, and hydroxide, subscripts a, b, and x represent compositional stoichiometry, and each of m and n is greater than or equal to zero, with the proviso that at least one of m and n is greater than zero.

Claims

1. A method for producing metal-containing nanoparticles comprising:

combining a metal organic compound selected from the group consisting of metal acetates, metal acetyl acetonates, and metal xanthates with an amine to provide a solution of metal organic compound in the amine; and

irradiating the solution with a high frequency radiation source to provide metal nanoparticles having the formula (A_a)_m(B_b)_nX_x, wherein each of A and B is selected from a metal, X is selected from the group consisting of oxygen, sulfur, selenium, phosphorus, halogen, and hydroxide, subscripts a, b, and x represent compositional stoichiometry, and each of m and n is greater than or equal to zero, with the proviso that at least one of m and n is greater than zero.

2. The method of claim 1, wherein the solution is heated prior to the irradiating step.

3. The method of claim 2, wherein the solution is heated for a period of time ranging from about 1 minute to about 50 minutes.

4. The method of claim 2, wherein the solution is heated to a temperature ranging from about 50°

to about 150°

C.

5. The method of claim 1, wherein the high frequency radiation source comprises a microwave radiation source having a frequency in the range of from about 0.4 to about 40 GHz.

6. The method of claim 1, wherein the high frequency radiation source comprises a microwave radiation source having a frequency in the range of from about 0.7 to about 24 GHz.

7. The method of claim 6, wherein the solution is irradiated for a period of time ranging from about 10 seconds to about 50 minutes to provide the substantially stabilized dispersion of metal nanoparticles.

8. The method of claim 1, further comprising, washing the substantially stabilized dispersion of metal nanoparticles with an alcohol subsequent the irradiation step.

9. The method of claim 8, wherein the alcohol comprises a C₁ to C₄ alcohol.

10. The method of claim 1, further comprising drying the metal nanoparticles.

11. The method of claim 1, wherein the solution of metal organic compound and amine further comprises an unsaturated fatty acid containing from about 10 to about 26 carbon atoms.

12. The method of claim 10, wherein the organic acid comprises oleic acid.

13. The method of claim 1, wherein the amine comprises a hydrocarbyl amine containing from about 3 to about 24 carbon atoms.

14. The method of claim 13, wherein the amine comprises oleylamine.

15. The method of claim 11, wherein a mole ratio of amine to organic acid in the solution ranges from about 1:

1 to about 3;

1.

16. The method of claim 15, wherein a mole ratio of amine to metal organic compound in the solution ranges from about 5:

1 to about 10;

1.

17. The method of claim 1, wherein the organic metal compound further comprises a first metal organic compound and a second metal organic compound, wherein the first and second metal organic compounds are selected from the group consisting of metal acetates, metal acetyl acetonates, and metal xanthates.

18. The method of claim 17, wherein each metal of the first and second metal organic compounds is selected from the group consisting of metals from Groups 1A, 2A, 3A, 4A, 5A, and 6A of the Periodic Table, transition metals, lanthanides, actinides, and mixtures thereof.

19. The method of claim 1, wherein the metal of the metal organic compound is selected from the group consisting of metals from Groups 1A, 2A, 3A, 4A, 5A, and 6A of the Periodic Table, transition metals, lanthanides, actinides, and mixtures thereof.

20. A method for producing oil dispersible nanoparticles comprising:

combining cerium acetate with a hydrocarbyl component to provide a cerium acetate solution; and

irradiating the solution with a high frequency radiation source to provide substantially stabilized dispersion of cerium oxide nanoparticles.

21. The method of claim 20, wherein the solution is heated prior to the irradiating step to remove any crystalline water from the cerium acetate.

22. The method of claim 21, wherein the solution is heated for a period of time ranging from about 1 minute to about 50 minutes.

23. The method of claim 21, wherein the solution is heated to a temperature ranging from about 100°

to about 120°

C.

24. The method of claim 20, wherein the high frequency radiation source comprises a microwave radiation source having a frequency in the range of from about 0.4 to about 40 GHz.

25. The method of claim 20, wherein the high frequency radiation source comprises a microwave radiation source having a frequency in the range of from about 0.7 to about 24 GHz.

26. The method of claim 25, wherein the solution is irradiated for a period of time ranging from about 10 seconds to about 50 minutes to provide the substantially stabilized dispersion of cerium oxide nanoparticles.

27. The method of claim 20, further comprising, washing the substantially stabilized dispersion of cerium oxide nanoparticles with an alcohol subsequent the irradiation step.

28. The method of claim 27, wherein the alcohol comprises a C₁ to C₄ alcohol.

29. The method of claim 20, further comprising drying the cerium oxide nanoparticles.

30. The method of claim 20, wherein the hydrocarbyl component contains from about 10 to about 26 carbon atoms.