IP Library Granted Patent US 9,212,294
Granted Patent B2
US 9,212,294 · App. 14/681,379 · Granted Dec 15, 2015

Silver nanoplate compositions and methods

Inventors: Steven J. Oldenburg (Encinitas, CA); Martin Miranda (San Diego, CA); David S. Sebba (Cary, NC); Todd J. Harris (Carlsbad, CA)
Assignees: nanoComposix, Inc.; Sienna Labs, Inc.
C09D139/06A61K9/5115A61K9/5123A61K9/5138A61K33/38A61L27/00B22F1/0081C09D125/06C09D129/04A61L2300/104B22F1/0022B22F1/0055B22F1/02
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Quick Facts
Patent No.
US 9,212,294
App. No.
14/681,379
Granted
Dec 15, 2015
Kind
B2
Abstract

Embodiments of the present invention relate to methods for preparing high optical density solutions of nanoparticle, such as nanoplates, silver nanoplates or silver platelet nanoparticles, and to the solutions and substrates prepared by the methods. The process can include the addition of stabilizing agents (e.g., chemical or biological agents bound or otherwise linked to the nanoparticle surface) that stabilize the nanoparticle before, during, and/or after concentration, thereby allowing for the production of a stable, high optical density solution of silver nanoplates. The process can also include increasing the concentration of silver nanoplates within the solution, and thus increasing the solution optical density.

Claims (55)

1. A process for making concentrated silver nanoplates that preserve shape post-concentration while increasing optical density, the process comprising:

adding a stabilizing agent to a pre-concentrated solution,

wherein the pre-concentrated solution comprises silver nanoplates,

wherein each of the silver nanoplates has a plate shape,

wherein the pre-concentrated solution has a peak optical density at a first wavelength;

wherein the stabilizing agent comprises a polyvinyl based polymer and a borate; and

increasing a concentration of the silver nanoplates in the pre-concentrated solution to generate a concentrated solution,

wherein the concentrated solution has a peak optical density at a second wavelength,

wherein the first wavelength is substantially the same as the second wavelength,

wherein the peak optical density of the concentrated solution is greater than the peak optical density of the pre-concentrated solution, and

wherein at least a portion of the silver nanoplates in the pre-concentrated solution retain the plate shape in the concentrated solution.

2. The process of claim 1 ,

wherein increasing the concentration is performed using tangential flow filtration,

wherein the peak optical density of the concentrated solution is at least ten times higher than the peak optical density of the pre-concentrated solution,

wherein the peak optical density of the concentrated solution is at least 100 cm −1 ,

wherein the polyvinyl based polymer comprises at least one of the group consisting of: a polyvinyl pyrrolidone (PVP) and a polyvinyl alcohol (PVA),

wherein the borate comprises sodium borate,

wherein the second wavelength of the concentrated solution is in a range between 300 nm and 1500 nm, and

wherein at least one optical property of the concentrated solution is substantially the same as the pre-concentrated solution in that the peak optical density of the pre-concentrated solution and the peak optical density of the concentrated solution occurs at substantially the same wavelength, and

wherein the portion of the silver nanoplates that retain the plate shape is greater than 90% in the concentrated solution.

3. The process of claim 1 ,

wherein the silver nanoplates are prepared via a seed mediated growth mechanism,

wherein the seed mediated growth mechanism comprises:

combining citrate, polystyrene sodium sulfonate (PSSS), and sodium borohydride in a first solution,

adding silver nitrate to the first solution to form a seed solution,

adding a portion of the seed solution to a second solution, wherein the second solution comprises ascorbic acid, and

adding silver nitrate to the second solution to form the pre-concentrated solution.

4. The process of claim 1 ,

wherein increasing the concentration is performed using tangential flow filtration,

wherein the tangential flow filtration utilizes a filter membrane with pores with a molecular weight cutoff in a range between 10 kDa and 0.05 micron,

wherein the peak optical density of the concentrated solution is at least ten times higher than the peak optical density of the pre-concentrated solution,

wherein the peak optical density of the concentrated solution is at least 100 cm −1 .

5. The process of claim 1 , further comprising coating the silver nanoplates with silica, wherein coating the silver nanoplates with silica comprises:

adding ethanol to the pre-concentrated solution,

adding a base to the pre-concentrated solution, and

adding a silane to the pre-concentrated solution.

6. The process of claim 1 , wherein the stabilizing agent comprises at least one of the group consisting of: a polyvinyl pyrrolidone (PVP), a polyvinyl alcohol (PVA), and a polyethylene glycol (PEG).

7. The process of claim 1 , further comprising forming a metal oxide shell on the surface of the silver nanoplate.

8. The process of claim 7 , wherein the metal oxide shell is any of the group consisting of: a silica shell and a titanium dioxide shell, wherein the metal oxide shell has a thickness in a range between 1 nm to 100 nm.

9. The process of claim 1 , wherein the stabilizing agent further comprises a thiol chemical group.

10. The process of claim 9 , wherein the thiol chemical group comprises at least one of the group consisting of: a lipoic acid, a mercaptohexadecanoic acid, a mercaptoundecanoic acid, and a dihydrolipoic acid.

11. The process of claim 1 , wherein the second wavelength is within 10% of the first wavelength.

12. The process of claim 1 , wherein the portion of the concentrated silver nanoplates that retain the plate shape after increasing the concentration is greater than 80%.

13. The process of claim 1 , wherein the pre-concentrated solution is centrifuged after increasing the concentration using tangential flow filtration.

14. The process of claim 1 , where the pre-concentrated solution is incubated with a substrate, wherein the substrate comprises a fiber.

15. A composition comprising:

a plurality of silver nanoplates in a solution comprising an optical density,

wherein the silver nanoplates comprise a coating on a surface of the silver nanoplates,

wherein the optical density is greater than 100 cm −1 , and

wherein the coating comprises a borate and at least one agent selected from the group consisting of: a polyvinyl based polymer and a thiol-containing molecule.

16. The composition of claim 15 , wherein the borate comprises at least one of the group consisting of: a sodium borate and a potassium tetraborate.

17. The composition of claim 15 , wherein the coating comprises said polyvinyl based polymer, wherein the polyvinyl based polymer is selected from the group consisting of: a polyvinyl pyrrolidone (PVP) and a polyvinyl alcohol (PVA).

18. The composition of claim 15 , wherein the coating comprises said thiol-containing molecule, wherein the thiol-containing molecule comprises at least one of the group consisting of: a lipoic acid, a mercaptohexadecanoic acid, a mercaptoundecanoic acid, and a dihydrolipoic acid.

19. The composition of claim 15 , wherein the coating further comprises a metal oxide shell.

20. The composition of claim 19 , wherein the metal oxide shell is any of the group consisting of: a silica shell and a titanium dioxide shell, wherein the metal oxide shell has a thickness in a range between 1 nm to 100 nm.

Assignments (11)
SECURITY INTEREST Recorded Aug 14, 2026
From: NANOCOMPOSIX, LLC
To: ANTARES CAPITAL LP, AS COLLATERAL AGENT
Reel/Frame 075659/0460 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 28, 2022
From: HERCULES TECHNOLOGY MANAGEMENT CO IV, LLC
To: CORONADO AESTHETICS, LLC
Reel/Frame 059763/0794 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 27, 2022
From: SEBACIA, INC.
To: HERCULES TECHNOLOGY MANAGEMENT CO IV, LLC
Reel/Frame 059750/0939 →
CHANGE OF NAME Recorded Sep 28, 2021
From: NANOCOMPOSIX, INC.
To: NANOCOMPOSIX, LLC
Reel/Frame 057624/0016 →
SECURITY INTEREST Recorded Sep 17, 2021
From: NANOCOMPOSIX, LLC
To: ANTARES CAPITAL LP, AS COLLATERAL AGENT
Reel/Frame 057518/0226 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 17, 2020
From: SIENNA BIOPHARMACEUTICALS, INC.
To: SEBACIA, INC.
Reel/Frame 052138/0380 →
ASSIGNEE CHANGE OF ADDRESS Recorded Feb 17, 2017
From: SIENNA BIOPHARMACEUTICALS, INC.
To: SIENNA BIOPHARMACEUTICALS, INC.
Reel/Frame 041746/0955 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 21, 2016
From: HARRIS, TODD J.
To: SIENNA LABS, INC.
Reel/Frame 038346/0493 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 21, 2016
From: OLDENBURG, STEVEN J.; MIRANDA, MARTIN G.; SEBBA, DAVID S.
To: NANOCOMPOSIX, INC.
Reel/Frame 038346/0455 →
CHANGE OF NAME Recorded Mar 2, 2016
From: SIENNA LABS, INC.
To: SIENNA BIOPHARMACEUTICALS, INC.
Reel/Frame 037977/0634 →
ASSIGNEE CHANGE OF ADDRESS Recorded Oct 8, 2015
From: SIENNA LABS, INC.
To: SIENNA LABS, INC.
Reel/Frame 036819/0344 →
Continuity (3)
Continuation PCTUS2013063920 · Oct 8, 2013
Provisional Application 61795149 · Oct 11, 2012
Related Publication 20150225599A1 · Aug 13, 2015