US20060021468A1 - Gold nanoparticles and method of synthesizing the same - Google Patents

Gold nanoparticles and method of synthesizing the same Download PDF

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Publication number
US20060021468A1
US20060021468A1 US11/118,566 US11856605A US2006021468A1 US 20060021468 A1 US20060021468 A1 US 20060021468A1 US 11856605 A US11856605 A US 11856605A US 2006021468 A1 US2006021468 A1 US 2006021468A1
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Prior art keywords
gold
nanoplates
haucl
solution
gold nanoparticles
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US11/118,566
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Chil Ah
Wan Yun
Yong Yun
Dong Ha
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Korea Research Institute of Standards and Science KRISS
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Korea Research Institute of Standards and Science KRISS
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Assigned to KOREA RESEARCH INSTITUTE OF STANDARDS AND SCIENCE reassignment KOREA RESEARCH INSTITUTE OF STANDARDS AND SCIENCE ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: AH, CHIL SEONG, HA, DONG HAN, YUN, WAN SOO, YUN, YONG JU
Publication of US20060021468A1 publication Critical patent/US20060021468A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0551—Flake form nanoparticles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/056—Submicron particles having a size above 100 nm up to 300 nm
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/06—Metallic powder characterised by the shape of the particles
    • B22F1/068—Flake-like particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy

Definitions

  • the present invention relates to gold nanoparticles and a synthesis method thereof, and more particularly to gold nanoparticles which can be produced at low costs, high yields and large amounts by a liquid phase synthesis and has a planar shape with a controlled size, as well as a synthesis method thereof.
  • gold nanoparticles are widely used in various fields, such as catalysts, chemical sensors, biosensors, optoelectronic devices, optical devices, nano-devices, and surface enhanced Raman scattering (SERS).
  • SERS surface enhanced Raman scattering
  • Such gold nanoparticles show various optical properties depending on their shape. For example, spherical gold nanoparticles have a strong absorbance peak at 500-600 nm, whereas nanorods and nanoboxes show absorbance peaks at 500-1,500 nm. Such optical properties are very important variables in various application fields of the gold nanoparticles, particularly in applications to biosensors or optical devices.
  • the shape of the gold nanoparticles determines their physical and chemical properties. Gold nanoparticles with a certain shape have the properties according to their shape. Therefore the shape control of the gold nanoparticles means the control of their properties.
  • an object of the present invention is to provide gold nanoparticles consisting of gold nanoplates, which can be produced at low cost with high yields in large amounts by a liquid-phase synthesis and whose size can be controlled, as well as a synthesis method thereof.
  • Another object of the present invention is to provide gold nanoparticles consisting of gold nanoplates, which are highly crystalline and have the size controlled in the nanometer range.
  • the present invention provides gold nanoparticles consisting of gold nanoplates, which have a polygonal or circular plate structure.
  • the edge length or diameter of the gold nanoplates is preferably 10 nm-2,000 nm, and the thickness of the gold nanoplates is preferably 1 nm-100 nm.
  • the present invention provides a method for preparing gold nanoplates, which comprises the steps of stirring and heating an aqueous solution of HAuCl 4 .3H 2 O; adding a dispersion stabilizer to the HAuCl 4 .3H 2 O solution; adding a reducing agent to the HAuCl 4 .3H 2 O solution to which the dispersion stabilizer had been added; and heating and cooling the resulting mixture so as to form gold nanoplates.
  • the inventive method may further comprise the step of inducing the precipitation of the aqueous solution having the gold nanoplates formed therein, and then treating the upper layer with a filter.
  • the concentration of the HAuCl 4 .3H 2 O solution is preferably 0.1 mM to 10 mM.
  • the dispersion stabilizer is preferably any one selected from the group consisting of citric acid, polyacrylic acid (PVA), polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP). If polyvinylpyrrolidone is used as the dispersion stabilizer, the molar ratio between the gold ions of the HAuCl 4 .3H 2 O solution and the polyvinylpyrrolidone is preferably 1:0.05 to 1:15, and more preferably 1:0.1 to 1:10.
  • the reducing agent is preferably sodium citrate.
  • the molar ratio between the gold ions of the HAuCl 4 .3H 2 O solution and sodium citrate is preferably 1:0.1 to 1:10, and more preferably 1:0.1 to 1:1.
  • FIG. 1 is a flow chart for illustrating a method for synthesizing gold nanoparticles according to one embodiment of the present invention
  • FIG. 2 shows the shape of gold nanoparticles according to an embodiment of the present invention, which was measured by a scanning electron microscope;
  • FIG. 3 a shows the shape and crystallinity of gold nanoplates according to an embodiment of the present invention, which were measured by a scanning electron microscope, a transmission electron microscope, and X-ray diffraction (XRD) analysis;
  • FIG. 3 b illustrates that the size of gold nanoplates can be controlled by controlling synthetic conditions
  • FIG. 4 a shows the results of energy dispersive spectrometry for the nanoplates according to an embodiment of the present invention.
  • FIG. 4 b shows the UV-Vis NIR spectra of gold nanoplates according to the size of the nanoplates.
  • the present invention provides gold nanoparticles consisting of gold nanoplates, which are highly crystalline and have the size controlled in the nanometer range.
  • the present invention provides gold nanoparticles consisting of gold nanoplates which can be produced at low cost with high yields in large amounts by a liquid phase synthesis method.
  • FIG. 1 is a flow chart for illustrating a method for synthesizing gold nanoparticles according to one embodiment of the present invention.
  • the inventive method for synthesizing gold nanoparticles comprises the steps of: (S1) stirring and heating an aqueous solution of HAuCl 4 .3H 2 O; (S2) adding a dispersion stabilizer to the HAuCl 4 .3H 2 O solution; (S3) adding a reducing agent to the HAuCl 4 .3H 2 O solution to which the dispersion stabilizer had been added; and (S4) heating and cooling the resulting mixture so as to form gold nanoplates.
  • the inventive preparation method may further comprise the step (S5) of inducing the precipitation of the aqueous solution having the gold nanoplates formed therein, at room temperature, and then treating the upper layer with a filter, thus obtaining gold nanoparticles consisting of high-purity gold nanoplates.
  • an aqueous solution of HAuCl 4 .3H 2 O is prepared from HAuCl 4 .3H 2 O with a purity of more than 99.9%, and heated in a reflux system with vigorous stirring.
  • the concentration of the HAuCl 4 .3H 2 O solution is preferably 0.1 mM to 10 mM, and most preferably 1 mM.
  • the dispersion stabilizer such as citric acid, polyacrylic acid (PPA), polyethylene glycol (PEG) or polyvinylpyrrolidone (PVP), is added to the HAuCl 4 .3H 2 O solution being stirred and heated.
  • PPA polyacrylic acid
  • PEG polyethylene glycol
  • PVP polyvinylpyrrolidone
  • polyvinylpyrrolidone is used as the dispersion stabilizer.
  • the polyvinylpyrrolidone is a kind of polymer with a molecular weight of about 50,000 and has a characteristic in that it is easily dissolved in water.
  • the molar ratio between the gold ions of the HAuCl 4 .3H 2 O solution and the polyvinylpyrrolidone is preferably 1:0.05 to 1:15, more preferably 1:0.1 to 1:10, and most preferably 1:10 to 1:7.
  • the step (S3) is the step where the reducing agent is added to the HAuCl 4 .3H 2 O solution to which the dispersion stabilizer had been added.
  • sodium citrate (C 6 H 5 Na 3 O 7 ) is preferably used as the reducing agent.
  • the molar ratio between the gold ions of the HAuCl 4 .3H 2 O solution and the sodium citrate is preferably 1:0.1 to 1:10, more preferably 1:0.1 to 1:1, and most preferably 1:0.5.
  • the sodium citrate has the following formula 1:
  • step (S4) of heating and cooling the HAuCl 4 .3H 2 O solution to which the reducing agent had been added the solution is heated with vigorous stirring, and then cooled with stirring at room temperature, so as to form gold nanoparticles consisting of gold nanoplates.
  • the gold nanoplates are formed via the following reaction scheme:
  • Au 3+ is reduced into Au 0 by the sodium citrate so as to induce the nucleation of gold nanoplates, and the anisotropic growth of the nuclei leads to form gold nanoparticles consisting of gold nanoplates.
  • the HAuCl 4 .3H 2 O solution in which the gold nanoparticles consisting of gold nanoplates had been formed is kept at room temperature to induce the precipitation, and then the upper layer portion in which the gold nanoplates are suspended are collected and filtered.
  • the upper layer solution in which the gold nanoplates are suspended is filtered several times using deionized water as a cleaning solvent. This is because the gold nanoplates with high purity are suspended in the upper layer portion of the solution.
  • FIG. 2 shows the shape of gold nanoparticles according to an embodiment of the present invention, which was measured with a field emission scanning electron microscope (FS-SEM).
  • FS-SEM field emission scanning electron microscope
  • the gold nanoparticles according to an embodiment of the present invention consist of nanoplates with a thickness of 10-50 nm and a side length of 50-1,000 nm. Namely, it can be found that the gold nanoparticles according to the embodiment of the present invention consist of gold nanoplates.
  • FIG. 3 a shows the shape and crystallinity of gold nanoplates according to an embodiment of the present invention, which were measured by a scanning electron microscope, a transmission electron microscope, and X-ray diffraction (XRD) analysis.
  • FIG. 3 b illustrates that the size of gold nanoplates can be controlled by controlling synthesis conditions.
  • FIG. 3 a (a) and (b) are a low-magnification and a high-magnification SEM photograph, respectively.
  • the gold nanoplates according to the embodiment of the present invention have an edge length of 50-1,000 nm.
  • (c) is a TEM photograph.
  • the inset in (c) is a diffraction pattern taken along a direction perpendicular to the surface of the gold nanoplate, and shows ⁇ 220 ⁇ and ⁇ 422 ⁇ Bragg diffraction peaks corresponding to lattice constants 1.44 ⁇ and 0.83 ⁇ , respectively, relative to [111] axis.
  • (d) shows the diffraction pattern of the gold nanoplates according to the embodiment of the present invention. The comparison of (d) with the JCPDS card shows that the inventive nanoparticles have the crystalline structure of pure gold.
  • FIG. 3 b (a), (b), (c), and (d) are electron microscope photographs of gold nanoplates formed when the molar ratios between HAuCl 4 .3H 2 O and polyvinylpyrrolidone are 1:9, 1:5, 1:2, and 1:0.1, respectively.
  • the size of the gold nanoparticles consisting of gold nanoplates can be slightly controlled depending on the kind of a filter used in the filtering step, the size of the gold nanoplates is strongly dependent upon the ratio of polyvinylpyrrolidone, a dispersion stabilizer, to HAuCl 4 .3H 2 O. More specifically, it is found that an increase in the ratio of polyvinylpyrrolidone to HAuCl 4 .3H 2 O leads to an increase in the size of the gold nanoplates formed.
  • FIG. 4 a shows the results of analysis using an energy dispersive spectrometer for the nanoplates according to the inventive embodiment
  • FIG. 4 b shows the UV-Vis NIR spectra of the gold nanoplates according to the size of the nanoplates.
  • the nanoplates according to the embodiment of the present invention show peaks at the characteristic wavelength of gold. Namely, the nanoplates according to the embodiment of the present invention are made of gold.
  • the spectra 1 to 4 in FIG. 4 b represent the spectra of the gold nanoparticles composed of the gold nanoplates shown in (a) to (d) of FIG. 3 b, respectively.
  • the gold nanoplates according to the embodiment of the present invention have two characteristic and strong absorbance peaks at visible and near infrared region (wavelength region of 500-2,000 nm), indicating that they have thin and planar shapes.
  • the above-described method for synthesizing the gold nanoplates allows the provision of gold nanoparticles of various sizes and shapes, as well as the provision of gold nanoparticles having various physical and chemical properties.
  • the above-described gold nanoparticles consisting of gold nanoplates can be widely applied for the development of new materials, catalysts, photosensors, optical and electronic devices, nanomechanical parts, etc.
  • the present invention will provide a synthesis method which allows the gold nanoplates to be produced at low costs, with high yields and in large amounts.
  • the present invention can provide the gold nanoparticles consisting of the gold nanoplates which can be produced at low costs, high yields and large amounts by the liquid phase synthesis method, as well as the synthesis method thereof.
  • the present invention can provide the gold nanoparticles consisting of the gold nanoplates with a single-crystalline structure and a size controlled in the nanometer range.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
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  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Crystallography & Structural Chemistry (AREA)
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US11/118,566 2004-07-26 2005-04-29 Gold nanoparticles and method of synthesizing the same Abandoned US20060021468A1 (en)

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AT (1) ATE440690T1 (ko)
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US20130107254A1 (en) * 2011-09-26 2013-05-02 University Of Maryland, College Park Porous SERS Analytical Devices and Methods of Detecting a Target Analyte
CN103217416A (zh) * 2013-03-20 2013-07-24 中国科学院宁波材料技术与工程研究所 检测二价汞离子的检测组合物、方法与试剂盒
WO2013143017A1 (es) 2012-03-30 2013-10-03 Universidad De Santiago De Chile Uso de botrytis cinerea para la obtención de nanopartículas de oro
US9823246B2 (en) 2011-12-28 2017-11-21 The Board Of Trustees Of The Leland Stanford Junior University Fluorescence enhancing plasmonic nanoscopic gold films and assays based thereon
CN112387980A (zh) * 2019-08-19 2021-02-23 近镒生技股份有限公司 纳米金粒子、包含其的药物载体、其制备方法及其用途
CN113668029A (zh) * 2021-08-27 2021-11-19 安徽大学 粗糙金纳米颗粒构成的薄膜及其制备方法和用途
WO2023073685A1 (en) * 2021-10-28 2023-05-04 Rise Nano Optics Ltd. Diffusion of nanoparticles into transparent plastic

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20130107254A1 (en) * 2011-09-26 2013-05-02 University Of Maryland, College Park Porous SERS Analytical Devices and Methods of Detecting a Target Analyte
US9255843B2 (en) * 2011-09-26 2016-02-09 University Of Maryland, College Park Porous SERS analytical devices and methods of detecting a target analyte
US9823246B2 (en) 2011-12-28 2017-11-21 The Board Of Trustees Of The Leland Stanford Junior University Fluorescence enhancing plasmonic nanoscopic gold films and assays based thereon
US10088478B2 (en) 2011-12-28 2018-10-02 The Board Of Trustees Of The Leland Stanford Junior University Fluorescence enhancing plasmonic nanoscopic gold films and assays based thereon
WO2013143017A1 (es) 2012-03-30 2013-10-03 Universidad De Santiago De Chile Uso de botrytis cinerea para la obtención de nanopartículas de oro
CN103217416A (zh) * 2013-03-20 2013-07-24 中国科学院宁波材料技术与工程研究所 检测二价汞离子的检测组合物、方法与试剂盒
CN112387980A (zh) * 2019-08-19 2021-02-23 近镒生技股份有限公司 纳米金粒子、包含其的药物载体、其制备方法及其用途
CN113668029A (zh) * 2021-08-27 2021-11-19 安徽大学 粗糙金纳米颗粒构成的薄膜及其制备方法和用途
WO2023073685A1 (en) * 2021-10-28 2023-05-04 Rise Nano Optics Ltd. Diffusion of nanoparticles into transparent plastic
US11994755B2 (en) 2021-10-28 2024-05-28 Rise Nano Optics Ltd. Diffusion of nanoparticles into transparent plastic

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JP2006037221A (ja) 2006-02-09
EP1623781A3 (en) 2006-06-07
EP1623781A2 (en) 2006-02-08
DE602005016193D1 (de) 2009-10-08
ATE440690T1 (de) 2009-09-15
EP1623781B1 (en) 2009-08-26
KR20060009735A (ko) 2006-02-01
KR100600938B1 (ko) 2006-07-13

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