Process for making surfactant capped metal oxide nanocrystals, and products produced by the process
View Patent ↗Disclosed is a process for making surfactant capped nanocrystals of metal oxides which are dispersable in organic solvents. The process comprises decomposing a metal cupferron complex of the formula M X Cup X , wherein M is a metal, and Cup is a N-substituted N-Nitroso hydroxylamine, in the presence of a coordinating surfactant, the reaction being conducted at a temperature ranging from about 150 to about 400° C., for a period of time sufficient to complete the reaction. Also disclosed are compounds made by the process.
1. A process for making dispersable surfactant capped nanocrystals of metal oxides which comprises: (a) mixing a solution of a metal cupferron precursor complex of the formula M X Cup X , wherein M X is a metal ion in the oxidation state X selected from the group consisting of elements in Group 2, Group 3-12 of the 4 th period, Group 3-6 of the 5 th and 6 th period, Group 10-12 of the 5 th period, Group 12 of the 6 th . Groups 13 to 15, and the Lanthanide and Actinide series of the periodic table, and X is a number between 1 and 4, and Cup is a N-substituted N-nitroso hydroxylamine, with a coordinating surfactant, and (b) heating the mixture at a temperature and for a sufficient period of time to cause thermal decomposition of the M X Cup X precursor and formation of the nanocrystals.
2. The process of claim 1 wherein the process is conducted in an inert atmosphere.
3. The process of claim 2 wherein said inert atmosphere is argon or nitrogen gas.
4. The process of claim 1 wherein said process is conducted in the absence of water, air or oxygen.
5. The process of claim 1 wherein the mixture is heated to or maintained at a temperature ranging from about 150° C. to about 400° C.
6. The process of claim 1 wherein M is Fe.
7. The process of claim 1 wherein M is Mn.
8. The process of claim 1 wherein M is Cu.
9. The process of claim 1 wherein said coordinating surfactant is an organic molecule consisting of a polar headgroup and an apolar group providing stabilization against coagulation and precipitation of particles.
10. The process of claim 9 wherein said coordinating surfactant is hexadecylamine or trioctyl amine.
11. The process of claim 1 wherein said N-substituted N-nitroso hydroxylamine is N-nitroso-N-phenyl hydroxylamine.
12. The process of claim 1 wherein M is Fe, Cup is N-nitroso-N-phenyl hydroxylamine, and the coordinating surfactant is hexadecylamine.
13. A process for making dispersable surfactant capped nanocrystals of metal oxides with non-hydroxylated particle surfaces which comprises -mixing a solution of a metal cupferron complex of the formula M X Cup X , wherein M X is a metal ion in the oxidation state X selected from the group consisting of elements in Group 2, Group 3-12 of the 4 th period, Group 3-6 of the 5 th and 6 th period, Group 10-12 of the 5 th per Group 12 of the 6 th period, Groups 13 to 15, and the Lanthanide and Actinide series of the periodic table, and X is a number between 1 and 4, and Cup is cupferron, into an amine based coordinating surfactant, at a temperature ranging from about 250° C. to about 300° C., and allowing the reaction to proceed for a period of time sufficient to cause thermal decomposition of said M X Cup X , and formation of the nanocrystals.
14. A surfactant capped nanocrystal made in accordance with the process of claim 1 .
15. A process for making soluble surfactant capped nanocrystals of transition metal oxides with non-hydroxylated particle surfaces which comprises injecting a solution of a metal cupferron complex of the formula M X Cup X , where x is a number between 1 and 4, wherein M is selected from the group consisting of Fe, Mn, and Cu, and Cup is N-nitroso-N-phenyl hydroxylamine, into a coordinating surfactant, the injection being conducted at a temperature ranging from about 220° C. to about 350° C., for a period of time sufficient to complete the process.
16. A process for making surfactant capped nanocrystals of transition metal oxides which comprises injecting a solution of a metal cupferron complex of the formula M X Cup X , where x is a number between 1 and 4, andwherein M is selected from the group consisting of Fe, Mn , andCu, and Cup is N-nitroso-N-phenyl hydroxylamine, into an amine based coordinating surfactant, the injection being conducted at a temperature ranging from about 150° C. to about 400° C., for a period of time sufficient to complete the eaetion process.
17. The process of claim 1 wherein the numerical value of X is 1.
18. The process of claim 1 wherein the numerical value of X is 2.
19. The process of claim 1 wherein the numerical value of X is 3.
20. The process of claim 1 wherein the numerical value of X is 4.