IP Library Granted Patent US 10,518,331
Granted Patent B2
US 10,518,331 · App. 15/324,283 · Granted Dec 31, 2019

Synthesis of uniform anisotropic nanoparticles

Inventors: Chad A. Mirkin (Wilmette, IL); Matthew R. Jones (LaMesa, CA); Matthew N. O'Brien (Plymouth, MN)
Assignee: NORTHWESTERN UNIVERSITY
B22F9/24B22F1/0018B22F1/0048B22F2001/0033
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Quick Facts
Patent No.
US 10,518,331
App. No.
15/324,283
Granted
Dec 31, 2019
Kind
B2
Abstract

Methods of synthesizing various metal nanoparticle structures having high uniformity, using iterative reduction and oxidation conditions, is provided herein.

Claims (34)

1. A method of preparing gold circular disk nanoparticle comprising

(a) admixing gold triangular prisms, a stabilizing agent, and an oxidizing agent in an aqueous solution to form a first intermediate;

(b) admixing the first intermediate, a gold salt, and a reducing agent, and optionally a base and halide salt, in an aqueous solution to form a second intermediate;

(c) admixing the second intermediate, a stabilizing agent, and oxidizing agent in an aqueous solution to form the gold circular disk nanoparticle; and

(d) optionally repeating steps (b) and (c) at least once to increase the uniformity of the resulting circular disk nanoparticles;

wherein the gold circular disk nanoparticles are formed in a yield of at least 70%.

2. The method of claim 1 , wherein the gold circular disk nanoparticles are formed in a yield of at least 90%.

3. The method of claim 1 , wherein the circular disk nanoparticles having uniformity as measured by a coefficient of variation (CV) of less than 30%.

4. The method of claim 3 , wherein the circular disk nanoparticles have a CV of 10% or less.

5. The method of claim 1 , wherein the oxidizing agent of steps (a) and (c) comprises HAuCl 4 .

6. The method of claim 5 , wherein the HAuCl 4 concentration correlates to the gold triangular prism edge length: at 8 μM for an edge length of 60 nm or less; at 10 μM for an edge length of 80 nm to 120 nm; at 12 μM for an edge length of 140nm; and at 13 μM for an edge length of 180 nm.

7. The method of claim 1 , wherein the stabilizing agent is selected from the group consisting of cetyltrimethylammonium bromide (CTAB), cetyltrimethylammonium chloride (CTAC), cetylpyridinium chloride (CPC), and a mixture thereof.

8. The method of claim 1 , wherein the gold salt comprises HAuCl 4 .

9. The method of claim 1 , wherein the reducing agent comprises ascorbic acid.

10. The method of claim 1 , wherein steps (b) and (c) are repeated at least twice.

11. The method of claim 1 , wherein the gold triangular prisms are prepared by

(1) admixing a stabilizing agent, an iodide salt, a gold salt, a base, a reducing agent, and nanoparticle seeds to form gold triangular prisms; and

(2) isolating the gold triangular prisms.

12. The method of claim 11 , wherein the concentration of nanoparticle seeds is 20 to 300 pM for a selected edge length of the gold triangular prism of 30 nm to 250 nm.

13. The method of claim 1 , wherein the isolating comprises adding a halide salt to the mixture resulting from step (1) and the concentration of the halide salt is selected in view of the edge length of the gold triangular prisms: 0.4M halide salt for triangular prisms with an edge length of 30 nm to 80 nm; 0.2M halide salt for triangular prisms with an edge length of 90 nm to 120 nm; 0.1M halide salt for triangular prisms with an edge length of 130 nm to 170 nm; and 0.05M halide salt for triangular prisms with an edge length of 180 nm to 250 nm.

14. A method of preparing uniform gold spherical nanoparticles comprising

(a) admixing gold nanorods, a stabilizing agent, and an oxidizing agent in an aqueous solution to form a first intermediate;

(b) admixing the first intermediate, a gold salt, and a reducing agent, and optionally a base and halide salt, in an aqueous solution to form a second intermediate;

(c) admixing the second intermediate, a stabilizing agent, and an oxidizing agent in an aqueous solution to form the gold spherical nanoparticles; and

(d) optionally repeating steps (b) and (c) at least once to increase the uniformity of the resulting gold spherical nanoparticles, as measured by a coefficient of variation (CV); wherein

(1) the method is performed in the absence of ethylene glycol, dimethylformamide, diethylene glycol, dimethylsulfoxide, toluene, tetrahydrofuran, hexane, octane, and oleic acid;

(2) the gold spherical nanoparticles are formed in a yield of at least 90%; and

(3) the gold spherical nanoparticles have a diameter of 1 nm to 99 nm.

15. The method of claim 14 , wherein the spherical nanoparticles have a CV of 3% or less.

16. The method of claim 14 , wherein the oxidizing agent of steps (a) and (c) comprises HAuCl 4 .

17. The method of claim 14 , wherein the gold salt comprises HAuCl 4 .

18. The method of claim 14 , wherein the reducing agent comprises ascorbic acid.

19. The method of claim 14 , wherein any one of step (a), (b), and (c) is performed for 0.5 hr to 2 hr.

20. The method of claim 19 , wherein each of step (a), (b), and (c) is performed for 0.5 hr to 6 hr.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 12, 2017
From: MIRKIN, CHAD A.; JONES, MATTHEW R.; O'BRIEN, MATTHEW N.
To: NORTHWESTERN UNIVERSITY
Reel/Frame 040954/0555 →
Continuity (2)
Provisional Application 62023398 · Jul 11, 2014
Related Publication 20170203369A1 · Jul 20, 2017
Cited By (1)
US 12,497,289