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NanotechnologyinChemicalEngineering

(CHN425)

LL16AnalysisTechniquesIII
16 Analysis Techniques III
(BET/XRD/UVvis/FTIR/Raman)
(Surfacearea/crystalsizesofsamples)

byDr.T.Das

Date:17/10/2016
DepartmentofChemicalEngineering
IndianInstituteofTechnologyRoorkee,India

Content
Analysis Techniques

Microscopes
Mi
SEM/TEM/ SPM/STM/AFM/SNOM
Diffraction Techniques
q
XRD
Spectroscopies
UV Vis NIR/FTIR/Raman/XPS
UVVisNIR/FTIR/Raman/XPS
Physical methods
BET

BET
Multilayer adsorption theory:

Langmuir equation is valid for adsorption less than monolayer coverage


Brunauer, Emmette and Teller derived an relationship between the volume of gas
physically adsorbed and the partial pressure of the adsorbate which is valid for
multilayer
ltil
adsorption
d
ti

BET
BETequation:

v0 =v, is volume of gas adsorbed per unit area of adsorbent surface and
vm is the volume of gas adsorbed when the entire adsorbent surface is covered with a
complete unimoleculer layer
p0 : saturation pressure of gas ( infinite no of layers can build up on the surface)
c: constant

BET
Isothermsmostcommonlyusedincatalysis
y
y

Type

Langmuir

Freundlich

Temkin

Brunauer Emmet Teller


BrunauerEmmetTeller

Isotherm equations

Type of adsorption
Chemisorption
Physisorption
Chemisorption
and
physisorption at low coverage
Ch i
Chemisorption
i

Multilayer
u t aye p
physical
ys ca adso
adsorption
pt o

BET
The equilibrium adsorption of N2 on an oxide sample at 77.4K, b.pt of N2

X RayDiffraction(XRD)
XRayDiffraction(XRD)
(crystalstructureofpolycrystallinesamples,thinfilmsandnanoparticles)

XRayDiffraction(XRD)
X
tt d by
b atoms
t
bl us to
t understand
d t d about
b t arrangementt off atoms
t
i solids
lid
X-rays
scattered
enable
in
X-rays are scattered by atoms i.e that they are scattered by electrons of atoms
The scattered intensity at point P is given as (by JJ Thomson)

Ie:IntensityofXraysatpointP
e:chargeofanelectron
I:IntensityoftheXraybeamatorigin
y
y
g
r:distanceofpointPfromtheorigin
n:numberofelectron
m:massofanelectron
:anglebetweenincidentandscattered
beam
c:velocityoflight

XRayDiffraction(XRD)
X
diff t
t
X-ray
diffractometer

For crystal structure analysis


Used for nanomaterials analysis
Commonly used diffractometer is known as Powder Diffractometer or DebyeScherrer Diffractometer

XRayDiffraction(XRD)
A monochromatic source of X-rays
A Cu (copper) target or anode giving CuK (=0.154nm)
(=0 154nm)
A sample holder
An X-ray detector(Geiger Muller tube)

Both sample and detector move around an axis passing through sample center
and normal plane of the paper
Diffracted rays make an angle 2 at the detector
A plot
l t off intensity
i t it (counts)
(
t ) as a function
f ti off angle
l 2
2 (usually
(
ll 20 to
t 160 o) is
i a
diffraction pattern ready for analysis

XRayDiffraction(XRD)
B
Law
L off diffraction
diff ti
Braggs

A beam of X-rays fall on crystal planes at some grazing incidence,


B
Beam
off parallel
ll l rays is
i assumedd
Parallel rays of AO and BP are incident on atoms O and P and making an angle
Rays are scattered as OA and PB.
Distance between O and P is d
is the path difference between rays AOA and BPB

XRayDiffraction(XRD)
Diff ti from
f
diff
t types
t
l
Diffraction
different
off samples
Dont have infinite
ordered of arrangement
of atoms and have few
atoms and few planes
Scattering
without
diffraction peaks

Diffraction peaks are


sharp and broadened,
since nano particles and
i planes
its
l
are small
ll
Dont have infinite
arrangement of atoms

XRayDiffraction(XRD)
Diff ti from
f
ti l and
d Scherrer
S h
ti
Diffraction
nanoparticles
equation

FWHM

Nanoparticles are similar to single crystals and diffraction peaks are broadened
Particle sizes (T) decreases with increasing width of peak

XRayDiffraction(XRD)
Spacing between atomic planes of a crystal:
The plane spacing of cubic crystal is related to the lattice parameter (a) by the
following equation

XRayDiffraction(XRD)
ZnS nanoparticles: Diffraction peak at 30 degree is due to ZnS nanoparticles

UVvisNIRspectrometer

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