IP Library › Granted Patent US 12,404,184
Granted Patent B2
US 12,404,184 · App. 16/795,414 · Granted Sep 2, 2025

Method for continuous growth of water-soluble magnetic nanomaterials

Inventor: Yongfeng Zhao (Edwardsville, IL)
Assignee: Jackson State University
C01G49/08C01G49/0072H01F1/36B82Y25/00B82Y40/00C01P2002/72C01P2002/82C01P2002/88C01P2004/04C01P2004/64C01P2006/42
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Quick Facts
Patent No.
US 12,404,184
App. No.
16/795,414
Granted
Sep 2, 2025
Kind
B2
Abstract

Embodiments of a method for synthesizing water-soluble metal oxide nanoparticles are disclosed. In one embodiment, the method includes heating a first reaction mixture at a predetermined temperature for a predetermined time duration with continuous stirring to obtain a second reaction mixture that comprises water-soluble metal oxide nanoparticles of a first size. The first reaction mixture includes a reactant and a polyol. The method further includes adding a first predetermined amount of the reactant to the second reaction mixture to obtain a third reaction mixture. The method further includes heating the third reaction mixture at the predetermined temperature for the predetermined time duration with continuous stirring to obtain a fourth reaction mixture comprising water-soluble metal oxide nanoparticles of a second size. The reactant is Fe(acac) 3 and the polyol is diethylene glycol (DEG) for synthesizing water-soluble iron oxide nanoparticles.

Claims (37)

1. A method for synthesizing water-soluble metal oxide nanoparticles, the method comprising:

a. heating a first reaction mixture at a first predetermined temperature for a first predetermined time duration with continuous stirring to obtain a second reaction mixture that comprises water-soluble metal oxide nanoparticles of a first size, the first size having a standard deviation of about 10%, and the first reaction mixture comprising a reactant and a polyol, wherein the polyol is diethylene glycol (DEG);

b. adding a first predetermined amount of the reactant to the second reaction mixture to obtain a third reaction mixture; and

c. heating the third reaction mixture at a second predetermined temperature for a second predetermined time duration with continuous stirring to obtain a fourth reaction mixture comprising water-soluble metal oxide nanoparticles of a second size, wherein the second predetermined temperature is greater than the first predetermined temperature,

wherein the water-soluble metal oxide nanoparticles having a size of around 9 nm exhibit a transversal relaxivity of around 425 mMol -1 .s -1 and a longitudinal relaxivity of around 32 mMol -1 .s -1 .

2. The method as claimed in claim 1 , wherein the reactant is one of iron (II) acetate (Fe(C 2 H 3 O 2 ) 2 ) or iron (III) acetylacetonate (Fe(acac) 3 ) and wherein the water-soluble metal oxide nanoparticles correspond to water-soluble iron oxide nanoparticles.

3. The method as claimed in claim 1 further comprising heating the first reaction mixture at an initial temperature for an initial time duration prior to the heating of the first reaction mixture at the first predetermined temperature for the first predetermined time duration.

4. The method as claimed in claim 1 , wherein the first predetermined temperature is in the range of around 100° C. to 140° C. and the first predetermined time duration is in the range of around 1-3 hours.

5. The method as claimed in claim 1 further comprising:

a. separating the water-soluble metal oxide nanoparticles from the respective reaction mixtures; and

b. purifying the separated water-soluble metal oxide nanoparticles.

6. The method as claimed in claim 1 , wherein the second predetermined temperature is in the range of around 200° C. to 240° C. and the second predetermined time duration is in the range of about 1-2 hours.

7. The method as claimed in claim 1 , wherein the second size of the metal oxide nanoparticles comprised in the fourth mixture is dependent at least in part on the first predetermined amount of the reactant added to the second reaction mixture.

8. The method as claimed in claim 1 , wherein the second size is greater than the first size.

9. The method as claimed in claim 1 further comprising:

a. adding a second predetermined amount of the reactant to the fourth reaction mixture to obtain a fifth reaction mixture; and

b. heating the fifth reaction mixture at the second predetermined temperature for the second predetermined time duration with continuous stirring to obtain a sixth reaction mixture comprising water-soluble metal oxide nanoparticles of a third size, wherein the third size is greater than the second size and the first size.

10. The method as claimed in claim 1 , wherein the first size and the second size of the metal oxide nanoparticles lie in the range of about 4 nm to about 13 nm.

11. A method of continuous synthesis of water-soluble metal oxide nanoparticles of varying sizes, the method comprising:

a. performing a first heating operation on a reaction mixture at an initial temperature of about 100° C. to about 140° C. for an initial time duration of about 1 hour to about 3 hours, the reaction mixture comprising a first predetermined amount of a reactant and a polyol, wherein the polyol is diethylene glycol (DEG);

b. performing a second heating operation, on the reaction mixture obtained from the first heating operation, at a predetermined temperature for a predetermined time duration to obtain water-soluble metal oxide nanoparticles of a selected first size, wherein the first predetermined amount of the reactant added during the first heating operation is determined by the selected first size, wherein the predetermined temperature is greater than the initial temperature;

c. adding a second predetermined amount of the reactant to the reaction mixture obtained from the second heating operation; and

d. performing a third heating operation, on the reaction mixture obtained from adding the second predetermined amount of the reactant, at the predetermined temperature for the predetermined time duration to obtain water-soluble metal oxide nanoparticles of a selected second size, wherein the second predetermined amount of the reactant added is determined by the selected second size,

wherein the water-soluble metal oxide nanoparticles having a size of around 9 nm exhibit a transversal relaxivity of around 425 mMol -1 .s -1 and a longitudinal relaxivity of around 32 mMol -1 .s -1 .

12. The method as claimed in claim 11 , wherein the reactant is Fe(acac) 3 .

13. The method as claimed in claim 11 , wherein the predetermined temperature is in the range of around 200° C. to 240° C. and the predetermined time duration is in the range of about 1-2 hours.

14. The method as claimed in claim 11 , wherein the second size of the metal oxide nanoparticles is dependent at least in part on the second predetermined amount of the reactant added to the reaction mixture.

15. A method of synthesizing water-soluble metal oxide nanoparticles having incremental particle sizes, the method comprising:

a. performing a preliminary heating operation on a reaction mixture at an initial temperature in a range of about 100° C. to about 140° C. for an initial time duration prior to performing any heating operation, wherein the initial temperature is less than a predetermined temperature;

b. performing a heating operation on the reaction mixture at the predetermined temperature in a range of about 200° C. to about 240° C. for a predetermined time duration to obtain water-soluble metal oxide nanoparticles of a first size, the reaction mixture comprising a reactant and a polyol, wherein the polyol is diethylene glycol (DEG); and

c. performing recursively an addition operation of a predetermined amount of the reactant to the reaction mixture obtained from a previous heating operation and a heating operation on the reaction mixture, obtained from the addition operation, at the predetermined temperature for the predetermined time duration to obtain water-soluble metal oxide nanoparticles,

wherein the particle size of water-soluble metal oxide nanoparticles obtained from every heating operation is greater than the particle size of water-soluble metal oxide nanoparticles obtained from a previous heating operation and wherein the water-soluble metal oxide nanoparticles having a size of around 9 nm exhibit a transversal relaxivity of around 425 mMol -1 .s -1 and a longitudinal relaxivity of around 32 mMol -1 .s -1 .

16. The method as claimed in claim 15 , wherein the recursive addition operation and heating operation are performed up to 6 times or less to obtain water-soluble metal oxide nanoparticles having particle sizes in the range of about 4 nm to about 13 nm.

17. The method as claimed in claim 15 , wherein the decomposition temperature of the reactant is lower than the boiling point of the polyol.

18. The method as claimed in claim 15 , wherein the reactant is Fe(acac) 3 .

19. The method as claimed in claim 18 , wherein the water-soluble metal oxide nanoparticles correspond to water-soluble iron oxide nanoparticles.

20. The method as claimed in claim 15 , wherein the reactant is selected from a group consisting of Mn(acac) 2 , Ni(acac) 2 , Co(acac) 2 and Fe(C 2 H 3 O 2 ) 2 .

Assignments (1)
CONFIRMATORY LICENSE Recorded Apr 23, 2025
From: JACKSON STATE UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 071017/0138 →
Continuity (2)
Provisional Application 62807407 · Feb 19, 2019
Related Publication 20200262715A1 · Aug 20, 2020
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