IP Library Granted Patent US 11,167,350
Granted Patent B2
US 11,167,350 · App. 16/390,439 · Granted Nov 9, 2021

Droplet-based microreactors for nanoparticles

Inventors: Joshua S. Santana (Bloomington, IN); Sara E. Skrabalak (Bloomington, IN)
Assignee: The Trustees of Indiana University
B22F9/24B01J19/0093B01J2219/0086B01J2219/00813B01J2219/00826B01J2219/00833B01J2219/00862B01J2219/00873B01J2219/00894B22F2301/255B22F2304/05
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Quick Facts
Patent No.
US 11,167,350
App. No.
16/390,439
Granted
Nov 9, 2021
Kind
B2
Abstract

Different Au—Pd nanoparticles, ranging from sharp-branched octopods to core@shell octahedra, can be achieved by inline manipulation of reagent flowrates in a microreactor for seeded growth. Significantly, these structures represent different kinetic products, demonstrating an inline control strategy toward kinetic nanoparticle products that should be generally applicable.

Claims (36)

1. A microreactor comprising:

a plurality of syringes, each syringe placed on a syringe pump;

tubing connected to each syringe;

capillaries connected to the tubing, an end of the capillaries meeting at an injector site of a respective syringe; and

a heating element, the tubing positioned in the heating element to heat the tubing, wherein droplets from the tubing are collected in a centrifuge vial after exiting the tubing.

2. The microreactor of claim 1 , wherein the plurality of syringes includes four syringes.

3. The microreactor of claim 2 , wherein three of the four syringes contain reagents and one of the syringes contains silicone oil.

4. The microreactor of claim 3 , wherein a flowrate of a reagent through the tubing is 1.8 mL per hour.

5. The microreactor of claim 3 , wherein a first reagent includes H2PdCl4.

6. The microreactor of claim 5 , wherein a second reagent includes Au nanocubes.

7. The microreactor of claim 6 , wherein a third reagent includes L-aa.

8. The microreactor of claim 1 , wherein:

the tubing includes polytetrafluoroethylene; and

the capillaries include silica capillaries.

9. The microreactor of claim 1 , wherein the tubing has an inner diameter of approximately 1.58 millimeters.

10. The microreactor of claim 1 , wherein the capillaries have an inner diameter of approximately 0.250 millimeters.

11. The microreactor of claim 1 , wherein the heating element has a temperature of approximately 55° C.

12. A method for nanoparticle synthesis comprising:

placing a plurality of syringes on a syringe pump;

connecting tubing to each syringe;

connecting capillaries to the tubing so that ends of the capillaries meet at an injector site of a respective syringe;

positioning the tubing in a heating element to heat the tubing;

controlling a flowrate of a reagent through the tubing; and

collecting droplets from the tubing in a centrifuge vial after exiting the tubing.

13. The method of claim 12 , wherein placing a plurality of syringes on a syringe pump includes placing four syringes on the syringe pump.

14. The method of claim 13 , further comprising:

filling three of the four syringes with reagents; and

filling one of the syringes with silicone oil.

15. The method of claim 14 , wherein controlling the flowrate of a reagent through the tubing further comprises adjusting the flowrate of the reagent through the tubing to 1.8 mL per hour.

16. The method of claim 14 , wherein filling three of the four syringes with reagents further comprises filling a first syringe with a reagent that includes H2PdCl4.

17. The method of claim 16 , wherein filling three of the four syringes with reagents further comprises filling a second syringe with a reagent that includes Au nanocubes.

18. The method of claim 17 , wherein filling three of the four syringes with reagents further comprises filling a third syringe with a reagent that includes L-aa.

19. The method of claim 12 , wherein:

connecting tubing to each syringe further comprises connecting polytetrafluoroethylene tubing to each syringe; and

connecting capillaries to the tubing further comprises connecting silica capillaries to the tubing.

20. The method of claim 12 , further comprising heating the heating element to a temperature of approximately 55° C.

Assignments (3)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 2, 2019
From: SANTANA, JOSHUA S.; SKRABALAK, SARA E.
To: THE TRUSTEES OF INDIANA UNIVERSITY
Reel/Frame 049940/0544 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 5, 2019
From: SANTANA, JOSHUA S.; SKRABALAK, SARA E.
To: THE TRUSTEES OF INDIANA UNIVERSITY
Reel/Frame 049377/0385 →
CONFIRMATORY LICENSE Recorded May 1, 2019
From: INDIANA UNIVERSITY
To: NATIONAL SCIENCE FOUNDATION
Reel/Frame 050176/0239 →
Continuity (2)
Provisional Application 62661135 · Apr 23, 2018
Related Publication 20190321895A1 · Oct 24, 2019