WELCOME

Janeetta J.V
Physical science
Csi college of education
parassala

STRUCTURAL CHARACTERIZATION AND

THE
PHOtoCATALYTIC ACTIVITY OF PURE AND
COPPER DOPED CADMIUM OXIDE
NANOPARTICLES

NANO MATERIALS

Nanotechnology
the most promising technology that can be applied
almost all spheres of life
Nanomaterials
Dimension less than 100 nm
Classified into nanocrystalline materials and nanoparticles.
Nanoparticles have a much greater surface area per unit mass
compared with larger particles.
Metal Oxide Nanomaterials
Exhibit unique physical and chemical properties due to their
limited size and a high density of corner or edge surface sites.
Applications of Nanomaterials
water filters, medical, textiles, cosmetics and drug delivery.

METHODS FOR THE SYNTHESIS OF NANOMATERIALS

Several synthesis methods have been developed to
enhance the performance of nanomaterials like better control
over particle size distribution, morphology, purity, quantity
and quality
Gas Condensation
Vacuum Deposition and Vaporization
Chemical Vapour Deposition (CVD)
Chemical Vapour Condensation (CVC)
Sol-Gel Technique
Co-precipitation
Among the available methods chemically controlled co-precipitation
method is a simple and low cost method that yield pure materials in
nanoscale size.

PURE AND Cu2+ DOPED CdO NANOPARTICLES AS

PHOTOCATALYSTS
Photo catalytic procedure is an effective and applicable
method to eliminate the organic dye pollutants from aqueous
solutions.
Pure and Cu2+ doped CdO not only has unique optical
and optoelectrical characteristics suitable for use in the
photodegradation of toxic organic compounds, dyes,
pigments and other environmental pollutants.
The present study deals with the photo catalytic activity of
pure and Cu2+ doped CdO in the degradation of methylene blue dye
in aqueous solution

CdO
n-type degenerate semiconducting metal oxide with a wide
band gap that varies from 2.2-2.8 eV, high conductivity, large linear
refractive index (n0 = 2.49), high transparency in the visible range of
solar spectrum, one of the semiconducting oxides with high carrier
mobility, and has great potential for using in optoelectronic devices.
Methylene blue

Methylene blue is a heterocyclic aromatic chemical

compound with the molecular formula C16H18N3SCl which act as an
organic pollutant.

EXPERIMENTAL PROCEDURES AND CHARACTERIZATIOTOOLS

In the present study pure and Cu2+ doped CdO have been
synthesized using chemical co-precipitation method and its structural
characterization was done using x-ray diffraction spectra recorded in
PANalyticalXpert-pro instrumentation. The photocatalytic activity of
the prepared samples in aqueous dye solutions were characterized
from the UV-Visible spectrum recorded using Varian Cary-5000
spectrophotometer.

Synthesis of pure and Cu2+ doped CdO nanoparticles

using co-precipitation method
Ammonium hydroxide was added drop-wise to 0.5M cadmium
acetate the pH value of the solution attains 8. The resultant solution
was kept undisturbed for 18 to 20 hours .Resulted precipitate was
then filtered and washed repeatedly.The hydroxide thus formed was
calcined at different temperatures 400C for 2h to produce
nanocrystalline powders.
(CH3COO)2CdH2O + 2NH4OH
Cd(OH)2 +2H2O + 2CH3COONH4
Cd(OH)2
CdO + H2O
For doped samples the Cu source, 0.5M copper chloride was
dissolved in required amounts along with the 0.5M cadmium acetate.

RESULTS AND DISCUSSION

XRD analysis
The observed d spacings and the respective prominent
peaks for the calcinedCdO nanoparticles correspond to
reflections of (111), (200), (220), (311) and (222) planes and are
in good agreement with the standard data (JCPDS card no.: 750593).

Observed and standard lattice d-spacing value

Samples

d spacing []

hkl

Observed

Standard

CdO400

2.70892
2.34637
1.65961
1.41542
1.35537

2.7111
2.3479
1.6602
1.4158
1.3555

1
2
2
3
2

1
0
2
1
2

1
0
0
1
2

0.5CuCdO400

2.71227
2.34939
1.66064
1.41617
1.35631

2.7111
2.3479
1.6602
1.4158
1.3555

1
2
2
3
2

1
0
2
1
2

1
0
0
1
2

Lattice parameter, Volume, Density

The lattice structure of CdO is cubic and therefore the unit
cell parameters are determined using the relation connecting
inter-planner distance (d) and miller indices (h k l) given by
1/d2= (h2 +k2 +l2)/a2 ......................(1)
Unit cell volume is
V=a3 .......................................(2)
The change in lattice constants after doping may be due
to the substitution of smaller Cu2+ ions in the interstitial sites.
The volume of unit cell of host CdO crystalline structure
slightly increased with Cu doping due to the disorder effect
caused by the substitution.

Sample
Details

Lattice
Paramet
er (a)

CdO 400

4.6937

0.5CuCdO
400
Determination

4.6978

Standard
Lattice Parameter
(a)

4.69582

Volum
e
3

Standard
Volume
3

103.4
0

103.55
103.6
7
parameter
(a) using

of precise value of lattice

Bradley-Jay and Nelson Riley Extrapolation Methods

The precise lattice parameters of pure and Cu2+ doped CdO

were calculated by the Bradley-Jay and Nelson-Riley extrapolation
method that minimizes the influence of systematic errors.
Bradley-Jay plot is drawn with cos2 along the X-axis and
the lattice parameter a for all the obtained peaks along the Y-axis.
Nelson-Riley plot is drawn with {cos2/sin}+{cos2/} along
the X-axis and the lattice parameter a for all the obtained peaks
along the Y-axis.

Fig. 5.2 Bradley-Jay Plot

Fig. 5.3 Nelson-Riley Plot

Preciselattice parameter values from B-J and N-R plot

Sample
Detail
s
CdO 400
CuCdO
400

Lattice Parameter (a) ()

Obs.

B-J
plo
t

N-R
plo
t

4.702
78

4.696
47

4.697 4.695
8
86

4.697
07

4.693
7

Standa
rd

4.6958
2

Crystallite size
The average size D of the samples was calculated using
the Debye Scherer formula
D=0.94/( cos)..................................(3)

Crystallite size of the prepared samples for the

prominent peaks
Sample
Details

2[2Th]

FWHM[2Th] D(nm)

CdO 400

33.041

0.2

44.6924

38.331

0.22

41.1001

55.31

0.22

43.7239

65.943

0.21

48.4911

69.27

0.22

47.0701

33.0269

0.00175

99.44132

38.3122

0.00262

62.0669

55.2726

0.00249

70.1572

65.9033

0.0032

56.0326

69.2127

0.0032

57.1254

CuCdO 400

Average D
39.32

73.83

Photocatalytic Activity of pure and copper doped CdO nanoparticles

in the degradation of methylene blue dye
The prepared samples were employed to destruct the organic dye,
methylene blue.
Pure and doped CdO
was able to effectively catalyse the
degradation of these pollutants. Cu2+ doped CdO nanoparticles are active
than pure CdO.
The photocatalytic degradation of pure and Cu2+ doped CdO
nanoparticles are 62 and 64% respectively, in 4 hour.
It was found that Cu2+ doped CdO sample showed the maximum
photocatalytic activity.
The rate of degradation was found to obey (pseudo) first order kinetics
and hence the rate constant for degradation, k, was obtained from the firstorder plot of kinetic analysis according to equation
[MB]=[MB]0ekt
As can be seen, the [MB] vs. time has an exponential decay which is
the characteristic of the first order reaction.

Fig.5.5. MB absorption spectra at different times of irradiation (Cu doped

CdO)

% Degradation for pure CdO

Time

Absorption

% Degradation

0.58

0.45

22

0.37

36

0.32

44

0.22

62

0.16

72

% Degradation for Cu doped CdO

Time

Absorption

% Degradation

0.5

0.38

24

0.31

38

0.24

52

0.18

64

[MB] normalized as a function

of time (pure CdO)

[MB] normalized as a function

of time (Cu doped CdO)

The kinetics of disappearance

of MB with time (pure CdO)

The kinetics of disappearance of

MB with time (Cu doped CdO)

CONCLUSION
Nano-sized pure and Cu2+ doped cadmium oxide powder
was successfully synthesized using the chemical coprecipitation method.
The pure and Cu2+ doped CdO particles were in cubic
(fcc) structure.
Precise determination of lattice parameter of pure and
Cu2+ doped CdO nanoparticles was done by Bradley-Jay and
Nelson-Riley extrapolation methods.
The crystallite sizes for pure and Cu-doped CdO were
calculated using Scherrer formula.
Crystallinity increased on Cu doping, which was
observed by the increase of intensity of the reflections.
The degradation rate of methylene blue followed the
pseudo-first order kinetics.

THANK YOU