Introduction To AgNPs-UB

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Synthesis and Optical Characterization of

Silver Nanoparticles

Course: CE2
Instructor: Dr. Uttara Basu
Email: uttarab@goa.bits-pilani.ac.in
Chamber: C220
Introduction to Nanoparticles
• Nanoparticles routinely defined as
particles with sizes between about 1 and
100 nm

• They show properties that are not found


in bulk samples of the same material

• Enormous potential for application in


electronic devices, catalysis, cosmetic
industry, healthcare, sensors

Nature Nanotechnology 4, pages634–641 (2009)

https://chembam.com/definitions/nanotechnology/
Quantum Confinement
When the length of the material is reduced to the same order as the exciton
radius, i.e., to a few nanometers, quantum confinement effect occurs.

https://www.sciencedirect.com/topics/engineering/quantum-confinement-effect
Large surface to volume ratio

https://chembam.com/definitions/nanotechnology/
Characterization techniques
Parameters Techniques
Size (structural properties) TEM, XRD, DLS
Shape/ morphology TEM, HRTEM, AFM
Elemental-chemical XRD, XPS, ICP-MS, ICP-OES
composition
Size distribution DLS
Surface charge Zeta potential
Concentration ICP-MS, UV-Vis

Nanoscale, 2018, 10, 12871-12934


Silver Nanoparticles (AgNPs)
• Silver is reduced from Ag(I) to Ag(0)
• Surfactant ligand: steric hindrance between particles
• Light-matter interaction: surface plasmon resonance
Applications:
✓Antibacterial, antimicrobial, antifungal
Places of application: hospital curtains, food containers, lunch boxes, fridges,
clothing
✓ Optoelectronic devices
Places of application: sensors, solar cells, LED
Surface Plasmon Resonance
• Surface plasmons are coherent and collective electron
oscillations confined at the dielectric–metal interface
• When electric fields of light are directed at
nanoparticles, they are excited and begin to resonate
• This creates a separation of charge and dipole
oscillation in the same direction as the electric field of
light.
• SPR allows a strong absorption and scattering of the
https://eng.libretexts.org/
incidence light
• Resonance frequency ω ∝ (Ne2/m)1/2
N is the density of carriers
m is the effective mass of carriers

npj Computational Materials volume 5, Article number: 45 (2019)


https://en.wikipedia.org/wiki/Surface_plasmon_resonance
Method 1:
a) Silver Nitrate (AgNO3): 1.2mM, 20 mL
b) Mercaptosuccinic acid (MSA): 0.3 mM, 20 mL
c) Sodium borohydride (NaBH4): 2 mM, 5 mL

Procedure: You will be given stock solutions of the reagents a-c. You have to
dilute them 10 times to prepare the reaction solutions.

E.g. A 12mM solution of AgNO3 will be given to you. You must take 2 mL from
this stock and make up the total volume up to 20 mL using distilled water in a
volumetric flask and use for the reactions.

J. Chem. Educ. 2015, 92, 339−344


Method 1 contd.
i) Take 20 mL 1.2 mM AgNO3 solution in a conical flask. Place a clean
magnetic bead in it and put it on a stirrer.
ii) To this stirring solution, gradually add the 20 mL, 0.3 mM MSA solution.
iii) To this, add the 5 mL, 2mM sodium borohydride solution, prepared freshly,
dropwise. (CAUTION: Rapid addition may cause precipitation)
iv) Note the color change happening during the reaction.
v) Let the reaction run for 30 mins.
vi) Record the UV-visible spectrum taking aliquots from the reaction mixture
when the color of the solution is a) pale yellow b) dark yellow/ brown c)
black

J. Chem. Educ. 2015, 92, 339−344


Method 2
a) Silver Nitrate (AgNO3): 2.4mM, 40 mL
b) Trisodium citrate (TSC): 40 mM, 1 mL

Procedure: You will be given the solutions a and b.


1. Take 40 mL from solution a in a round bottom flask using burette/ pipette
2. Heat it to 90 °C in a water bath.
3. To this solution, you add the TSC solution, dropwise using micropipette.
(CAUTION: Use micropipette carefully and avoid bubbles inside the tips, rapid addition may
cause precipitation)

J. Chem. Educ. 2015, 92, 339−344


Method 2 contd.
i) Note the color change happening during the reaction.
ii) Reflux the solution for ~ 45 minutes.
iii) Record the UV-visible spectrum of the reaction mixture when the color of
the solution is a) pale yellow b) dark yellow/ brown c) grey

J. Chem. Educ. 2015, 92, 339−344


J. Chem. Educ. 2015, 92, 339−344
Data Analysis
• Plot the time-dependent UV-visible spectra for the nanoparticles
synthesized by methods 1 and 2 (Make sure that the absorbance
value at the peak maxima does not exceed 1)
• Note the change in the spectra happening during the course of the
reaction
• Note the peak maxima for the NPs synthesized by methods 1 and 2
• Calculate the full width at half maxima (FWHM) from the spectra

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