IP Library Granted Patent US 9,907,865
Granted Patent B2
US 9,907,865 · App. 15/332,940 · Granted Mar 6, 2018

Room temperature ferromagnetic gadolinium silicide nanoparticles

Inventors: Magundappa Ravi L. Hadimani (Glen Allen, VA); Shalabh Gupta (Ames, IA); Shane Harstad (Rockford, MN); Vitalij Pecharsky (Ames, IA); David C. Jiles (Ames, IA)
Assignee: Iowa State University Research Foundation, Inc.
A61K49/06A61K49/1818C01B33/06C01P2004/61C01P2004/62C01P2006/42
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Quick Facts
Patent No.
US 9,907,865
App. No.
15/332,940
Granted
Mar 6, 2018
Kind
B2
Abstract

A particle usable as T 1 and T 2 contrast agents is provided. The particle is a gadolinium silicide (Gd 5 Si 4 ) particle that is ferromagnetic at temperatures up to 290 K and is less than 2 μm in diameter. An MRI contrast agent that includes a plurality of gadolinium silicide (Gd 5 Si 4 ) particles that are less than 1 μm in diameter is also provided. A method for creating gadolinium silicide (Gd 5 Si 4 ) particles is also provided. The method includes the steps of providing a Gd 5 Si 4 bulk alloy; grinding the Gd 5 Si 4 bulk alloy into a powder; and milling the Gd 5 Si 4 bulk alloy powder for a time of approximately 20 minutes or less.

Claims (28)

1. A ferromagnetic material, comprising:

a gadolinium silicide (Gd 5 Si 4 ) particle, wherein the Gd 5 Si 4 particle is ferromagnetic at temperatures up to 290 K and wherein the Gd 5 Si 4 particle is less than 2 μm in diameter.

2. The material according to claim 1 , wherein the Gd 5 Si 4 particle remains ferromagnetic at temperatures up to 310 K.

3. The material according to claim 1 , wherein the Gd 5 Si 4 particle is less than 1 μm in diameter.

4. The material according to claim 1 , wherein the Gd 5 Si 4 particle is less than 500 nm in diameter.

5. The material according to claim 1 , wherein the Gd 5 Si 4 particle includes 5 wt % or less Gd 5 Si 3 .

6. An MRI contrast agent, wherein the MRI contrast agent comprises:

a plurality of gadolinium silicide (Gd 5 Si 4 ) particles, wherein the Gd 5 Si 4 particles are less than 1 μm in diameter wherein the Gd 5 Si 4 particles are ferromagnetic at temperatures up to 290 K.

7. The MRI contrast agent according to claim 6 , wherein the Gd 5 Si 4 particles are ferromagnetic at temperatures up to 310 K.

8. A method for creating the ferromagnetic material of claim 1 comprising the steps of:

providing a Gd 5 Si 4 bulk alloy;

grinding the Gd 5 Si 4 bulk alloy into a Gd 5 Si 4 bulk alloy powder; and

milling the Gd 5 Si 4 bulk alloy powder for a time of approximately 20 minutes or less.

9. The method of claim 8 , wherein the grinding and milling steps further comprise using an inert atmosphere.

10. The method of claim 8 , wherein the using an inert atmosphere step further comprises using a noble gas atmosphere.

11. The method of claim 8 , wherein the milling step further comprises ball milling.

12. The method of claim 11 , wherein the ball milling step further comprises using a milling media with a mass ratio of milling media to Gd 5 Si 4 bulk alloy powder of between 2:1 and 10:1.

13. The method of claim 12 , wherein the using a milling media step further comprises using stainless steel balls having two different sizes.

14. The method of claim 13 , wherein the step of using stainless steel balls having two different sizes further comprises using a first size stainless steel balls with a diameter of 11.1 mm and using a second size of stainless steel balls with a diameter of 6.3 mm.

15. The method of claim 14 , further comprising the step of providing a ratio of the second size of stainless steels balls to the first size of stainless steel balls of 2:1.

16. The method of claim 8 , wherein the step of providing a Gd 5 Si 4 bulk alloy further comprises providing a pure phase alloy.

17. The method of claim 8 , wherein the providing a Gd 5 Si 4 bulk alloy step further comprises the steps of:

supplying a stoichiometric quantity of at least 99.9% purity gadolinium metal;

supplying a stoichiometric quantity of at least 99.999% purity silicon;

melting the gadolinium and silicon together in an inert atmosphere at least once; and

cooling the mixture of gadolinium and silicon at a rate fast enough to avoid neighboring phases.

18. The method of claim 17 , wherein the melting step is performed at least four times.

19. The method of claim 17 , wherein the melting step further comprises using an electric arc furnace on a water-cooled copper hearth to melt the gadolinium and silicon.

Assignments (2)
CONFIRMATORY LICENSE Recorded May 17, 2017
From: IOWA STATE UNIVERSITY
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 042522/0282 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 25, 2016
From: HADIMANI, MAGUNDAPPA RAVI L.; GUPTA, SHALABH; HARSTAD, SHANE; PECHARSKY, VITALIJ; JILES, DAVID C.
To: IOWA STATE UNIVERSITY RESEARCH FOUNDATION, INC.
Reel/Frame 040123/0213 →
Continuity (2)
Provisional Application 62250726 · Nov 4, 2015
Related Publication 20170119909A1 · May 4, 2017