ze ss te ch nik. Recycling. Introduction. General synthetic routes for gold nanoparticles. Gold nanoparticle ... 0,27 0,54 0,82 1,09 1,36 1,63 1,9 2,18 2,45 2,72.
NANOCON2015, Brno
Synthesis of Gold Nanoparticles via Chemical Reduction Method ZHAO Jingyue, FRIEDRICH Bernd IME Institute of Process Metallurgy and Metal Recycling RWTH Aachen University, Aachen, Germany
IME Process Metallurgy and Metal Recycling, RWTH Aachen University Prof. Dr.-Ing. Dr. h.c. Bernd Friedrich
Introduction Potential market share of applications for gold nanoparticles
Electronic Manufacturing
Medical and Healthcare
Au
chn ik ss te Pro ze
Metallurgie
Photovoltaic
Recycling
Catalyst
Introduction General synthetic routes for gold nanoparticles
Gold nanoparticle synthetic routes
Chemical method
Physicochemical method
Turkevich method Brust Method
chn ik ss te Pro ze
Metallurgie
The Faraday method
Recycling
Physical method
UV irradation Ultrasonic spray
Laser ablation Plasma synthesis
Motivation Production of gold nanoparticles: • lab scale (e.g. 100ml) • expensive (€ 272 per 100ml, • hazardous aspects
)
The main aim is to develop a complete process chain for the production of gold nanoparticles.
Material efficient Robust
Straight forward method
chn ik ss te Pro ze
Metallurgie
“green” process Recycling
To optimize the experimental paramenter
Less toxic and organic agents involved
Experiments 1. The citrate reduction method
75oC
100oC
2. The NaBH4 reduction method
150oC
20oC
0oC
Teflon coated magnetic bar Sealing clamp for dialysis membrane tube dialysis
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Metallurgie
24h Recycling
48h
Gold nanoparticle sampe in dialysis tube
96h
120h
144h
168h
3. The purification process
Results and Discussion: 1.The citrate reduction method Average particle diameter changes for gold nanoparticles with different Na3C6H5O7/Au molar ratios evaluated by Nanotrac wave600 analyser
Particle Diameter (nm)
500 400 300 200 100 0 0,27 0,54 0,82 1,09 1,36 1,63
1,9
2,18 2,45 2,72
chn ik ss te Pro ze
Metallurgie
Na3C6H5O7/ HAuCl4 molar ratios Recycling
Results and Discussion: 1.The citrate reduction method
50nm
chn ik ss te Pro ze
Metallurgie
20nm
Recycling
20nm
TEM images of the synthesized gold nanoparticles with different Na3C6H5O7/Au molar ratios: A, 0.82 B, 1.63 C, 2.45
Results and Discussion: 1.The citrate reduction method Gold nanoparticles with different Au concentrations up: Size distribution evaluated by Nanotrac wave analyser down: TEM images of the synthesized gold nanoparticles
chn ik ss te Pro ze
Metallurgie
20nm
Recycling
20nm
50nm
50nm
Results and Discussion: 2.The NaBH4 reduction method
TEM images of gold nanoparticles morphologies Sample 1: with high reaction rate, Sample 2: with modified reaction rate, Sample 3: with controlled low reaction rate. Sample 2
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Metallurgie
Sample 1
Recycling
Sample 3
200nm
200nm
100nm
100nm
100nm
50nm
100nm
1µm
10nm
Results and Discussion: 3. Investigation of purification
ICP results for gold nanoparticles samples with different particle size purified by dialysis through time (mg/L) Mean particle size(nm)
0h
24h
48h
96h
144h
168h
Au Na Cl Au Na Cl Au Na Cl Au Na Cl Au Na Cl Au Na Cl 117
90
95
94
1
16
100
53
90,6
94
7
0,94
113 296 10,8
81
6
0,04
118 38,8 77,8 53.3 2,77 3,1 41,1 0,65 0,4 44,8 0,15 0,3
chn ik ss te Pro ze
Metallurgie
23,9 37,7 9,6 37,7
Recycling
31,4 0,1
0,3
Results and Discussion: 3. Investigation of purification
72h
A1) via citrate reduction
A2) After dialysis
24h 48h 144h
168h
B1) via NaBH4 reduction
chn ik ss te Pro ze
Metallurgie
24h
Recycling
48h
72h
B2) After dialysis
Conclusions •
Spherical gold nanoparticles around 10nm were successfully fabricated via the Citrate reduction method and the NaBH4 reduction method in liter scale.
•
Stable and robust production routes are offered with optimised parameters.
chn ik ss te Pro ze
Metallurgie
• 48h dialysis can decrease impurities by large portion, and provide an improved particle quality of the citrate stabilized gold nanoparticles
Recycling
NANOCON2015, Brno
Thank you very much for your attention!
IME Process Metallurgy and Metal Recycling, RWTH Aachen University Prof. Dr.-Ing. Dr. h.c. Bernd Friedrich