# US 7,608,461 B1 · Surface engineered nanoparticles for improved surface enhanced Raman scattering applications and method for preparing same

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- Number: US 7,608,461 B1
- Document ID: US7608461B1
- Status: Granted
- Kind: B1
- Application number: 11/228,934
- Filed: 2005-09-16
- Granted: 2009-10-27
- Earliest claimed: 2005-09-16
- Assignees: Sandia Corporation
- Inventors: Blake A. Simmons; Albert Alec Talin
- Web page: https://patentgrep.com/patent/US7608461B1

## CPC

- B22F 9/24: starting from liquid metal compounds, e.g. solutions
- B22F 1/054: Nanosized particles
- B22F 1/0553: {Complex form nanoparticles, e.g. prism, pyramid, octahedron}
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B22F 2999/00: Aspects linked to processes or compositions used in powder metallurgy
- Y10S 977/777: Metallic powder or flake
- B22F: WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER (making alloys by powder metallurgy C22C); APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- Y10S: TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS

## Abstract

A method for producing metal nanoparticles that when associated with an analyte material will generate an amplified SERS spectrum when the analyte material is illuminated by a light source and a spectrum is recorded. The method for preparing the metal nanoparticles comprises the steps of (i) forming a water-in-oil microemulsion comprising a bulk oil phase, a dilute water phase, and one or more surfactants, wherein the water phase comprises a transition metal ion; (ii) adding an aqueous solution comprising a mild reducing agent to the water-in-oil microemulsion; (iii) stirring the water-in-oil microemulsion and aqueous solution to initiate a reduction reaction resulting in the formation of a fine precipitate dispersed in the water-in-oil microemulsion; and (iv) separating the precipitate from the water-in-oil microemulsion.

## Claims

### Claim 1

A method for preparing SERS gold nanoparticles, the method comprising the steps of:
(a) forming a first emulsion comprising:
(i) forming a first oil phase mixture comprising a bulk oil phase and a surfactant mixture comprising sodium bis(2-ethylhexyl) sulfosuccinate (AOT) and phosphatidylcholine (PTC);
(ii) forming a first dilute aqueous solution consisting essentially of water and a gold salt;
(iii) adding the first dilute aqueous solution into the first oil phase mixture; and
(iv) agitating the first oil phase mixture to provide the first emulsion;
(b) forming a second emulsion comprising:
(i) forming a second oil phase mixture comprising a bulk oil phase and a surfactant mixture comprising AOT and PTC;
(ii) forming a second dilute aqueous solution comprising a reducing agent selected from the group consisting of reducing agent selected from the group of ascorbic acid, urea, dimethylamine borane (DMAB), sulfur dioxide or β-mercaptoethanol;
(iii) adding the second dilute aqueous solution into the second oil phase mixture; and
(iv) agitating the second oil phase mixture to provide the second emulsion;
(c) adding the second emulsion to the first emulsion to provide an emulsion mixture;
(d) stirring the emulsion mixture to initiate a reduction reaction between the reducing agent and the gold salt solution to provide a precipitate dispersed in the emulsion mixture; and
(e) separating the precipitate from the emulsion mixture, thereby providing a plurality of gold nanoparticles, wherein the gold nanoparticles comprise a nanometer scale roughened surface structure.

### Claim 2 (depends on 1)

The method of claim 1, wherein the step of forming the first oil phase mixture further comprises the steps of adding and mixing the AOT before adding and mixing the PTC.

### Claim 3 (depends on 1)

The method of claim 1, wherein the step of forming the second oil phase mixture further comprises the steps of adding and mixing the AOT before adding and mixing the PTC.

### Claim 4 (depends on 1)

The method of claim 1, wherein the step of adding the second emulsion to the first emulsion further comprises the step of dispensing the second emulsion drop-wise into the first emulsion while stirring the first emulsion.

### Claim 5 (depends on 1)

The method of claim 1, wherein the step of separating the precipitate from the emulsion mixture further comprises the steps of:
(a) pouring the emulsion into one or more containers;
(b) spinning the containers in a centrifuge for a period of time sufficient to concentrate the precipitate in one end of each of the one or more containers;
(c) decanting the supernate liquid; and
(d) washing the concentrated precipitate by re-suspending the precipitate in a quantity of solvent media;
(e) repeating steps (b) through (d) at least twice; and
(f) re-suspending the washed precipitate in a final quantity of solvent media.

### Claim 6 (depends on 1)

Metal nanoparticles made by the process of claim 1, wherein the roughened surface structures of the metal nanoparticles comprise a plurality of protruding knobs distributed roughly uniformly across a generally spheroidal body.