Preparation of Nano particles in details Characterizatio by different techniques #SEM #FT-IR #XRD #ION-TOF MS

2. Presented by:
Kashif AliKashifdude035@gmail.com
Roll no. 29
Semester 1st
Class M. Phil Chemistry
Section A
Department Of Chemistry
Minhaj University Lahore

3. Topic:
“Preparation and characterization of
ZnO nanoparticles coated paper "
activity study”
Presented to:
Ma’am Shamaila

4. Introduction
Preparation
characterization
Main Outlines of Presentation

5. Introduction:
• What is Nano-particle?
Nanoparticle is a microscopic particle whose size is measured in
nanometers.
 Size of Nanoparticles is 1nm up to 100 nm.
 Nano = 10-9 (Extremely small) particle = small piece of matter
Nanochemistry
It is branch of science deals mainly with synthesis characterization
and applications of nanoparticles.
Note:
Nanoparticles nanorods, nanocrystals, nanotubes, nanopowders, nanorings
are the different forms of Nano materials.

6. “Preparation and characterization of
ZnO nanoparticles coated paper and
its antibacterial activity study”
• Authors:
 Kalyani Ghule
 Anil Vithal Ghule
 Bo-Jung Chen
 Yong-Chien Ling
Publication:
• Received 20th April 2006, Accepted 31st August 2006
• First published as an Advance Article on the web 15th September
2006
• DOI: 10.1039/b605623g
Article title

7. Importance of ZnO NPs:
ZnO NPs are considered as workhorse of technological development
exhibiting excellent electrical, optical, and chemical properties with
broad range of applications as
Semiconductors
In optical devises
Piezoelectric devises
Sensors
Transparent electrodes
Solar cells
Antibacterial activity
UV inks
Security papers
e-print
portable energy

8. Earlier work on ZnO NPs coatings
• In the past following methods were used to produce ZnO NPs
Coatings.
• Solid supports used such as
• Metal , Metal oxides , Glass and Thermally stable substrates
• Coatings of ZnO nanoparticles on thermo labile surfaces are
scarce
• Coating on paper is yet to be reported.
• Coatings with biomolecules, oil, pigments (calcium carbonate,
clay, talc, silicates, TiO2, etc.), polymers, plastics etc. has been
reported with the help of suitable binders and co-binders.
Chemical Thermal Spin coating Spray pyrolysis
Pulsed laser
deposition

9.  On the other hand, choice of paper coating technique is
an important consideration.
• Coating techniques (off-machine and machine) like
Dip Brush Mechanical blade Bench coater
Rolling Air brush Curtain
Spin coating Spray Print
Cast Strip coaters
have been used for coating the paper surfaces since decades.
 Some coating techniques are not proffered like contact mechanical
techniques. These causes problems*
*Cause web break,
*Surface defects,
*Variable layer
*Consume more material by filling fiber interstices
*Need excess solvent (water), energy
*Affect surface properties like gloss and brightness

10. Preparation:
• ZnO NPs coating paper was obtained by “Sonochemical”
method.
Basic Principle:
 The chemical effects of ultrasound arise from
acoustic cavitation phenomena, that is, the formation,
growth, and implosive collapse of bubbles in a liquid
medium. These unusual chemical and physical
environments are generally utilized in sonochemical
processing.
 Although, sonochemistry has been used in
industries and in fabrication of nanomaterials.
Note:
• This technique is a simple, green, and cost-effective

11. Process:
1) ZnO nanoparticles (average diameter y20 nm) were
obtained from Echo Chemicals, Taiwan. NPs were heated to
450 uC to remove organic contaminants prior to their use in
experiment.
2) Further, the ZnO nanoparticles were characterized using
TEM (transmission electron microscope) (Philips, Tecnai 20,
200 kV) with inbuilt energy dispersive X-ray analysis (EDS).
3) For ZnO NPs coating 2 g of ZnO nanoparticles were dispersed
200 mL of deionized (DI) water using a fixed power sonicator
(L&R Ultrasonics, Quantrex 140, 150 W, 45 kHz) for 10 min.
4) Then added drop wise NH4OH till a pH of 8 was achieved 10
min before experiments. Use of NH3 is also acceptable.
5) The paper surface to be coated (white paper, YFY Papers,
Taiwan) was attached face down to the substrate, and the
position was set such that the paper surface just touched
dispersed solution.

12. 6) The sonication time (5, 10, 15, 20, 25, and 30 min) was
varied in each experiment.
7) In the last step coated paper was detached and dried at 80
uC.

13. Characterization:
• Scanning Electron MicroscopySEM
• Energy Dispersive spectroscopyEDS
• Thermal Gravimetric AnalysisTGA
• X-rays DiffractionXRD
• Attenuated Total Reflectane FTIRATR-FTIR
• Time of flight Secondary Ion MSTOF-SIMS
 Characterization refers to the study of material features
such as its composition, structure and various features like
Physical, Electrical, Magnetic.

14. SEM:
Purpose: Surface morphology and elemental composition was characterized
by SEM.
Model: SEM (Hitachi-S4700) with inbuilt EDS.
Note: Images indicated the coating of ZnO NPs on paper.
Scanning Electron Microscopy device ZnO NPs coated paper

15. EDS:
Purpose: EDS analysis showed the presence of Zn, Ca, Mg, C, and O
confirming the deposition of ZnO nanoparticles.
Model: SEM (Hitachi-S4700) with inbuilt EDS.
Note: EDS provided a lot of hidden info about NPs on ZnO coated paper.
Energy Dispersive Spectrometer

16. TGA:
Purpose: Thermal stability , mass loss over time and amount of ZnO
loading on the paper surface was estimated using TGA. ZnO NPs coating
increased as time of sonication is enhanced was also investigated by TGA.
Model: TGA analyzer (Perkin Elmer TGA6
Note: 73.1% weight losses recorded by TGA of ZnO NPs coated paper.
Thermal Gravimetric Analyzer Thermo- gram by TGA

17. XRD:
Purpose: Surface information and Crystallinity of nanoparticles on ZnO NPs
coated paper determined by XRD.
Model: Not mentioned
Note: XRD patterns were obtained using Material Analysis and Characterization
(MAC) advanced powder X-ray diffract-meter (using Cu Ka = 1.54056 A° radiation).
X-ray Diffract meter XRD Spectra

18. ATR-FTIR:
Purpose: Mechanism of ZnO NPs coating paper was investigated by ATR-
FTIR.
Model: Perkin Elmer (System 2000 FTIR).
Note: Basic info about functional groups,
(M–O) 732 cm-1 (C–O) 900–1300 cm-1 C–H 1300–1500 cm-1
(M–N) bond 460-560 cm-1 N–H bond 1486-1630 cm-1
Attenuated Total Reflectane FTIR
ATR-FTIR spectra

19. TOF-SIMS:
Purpose: Nature of binding and also the distribution of the ZnO NPs
on the coated paper surface was investigated by TOF-SIMS.
Model: Positive TOF-SIMS (ION-TOF; Munich, Germany)
Note: Positive ion detection mode used for blank paper and ZnO NPs coated
paper.
Time of flight secondary ion
Mass spectrometer
TOF-SIMS spectrogram

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