Photocatalytic degradation of methyl orange

dye using Mn doped CdS nanoparticles.

PRESENTED BY: VIVEK NIRALA

BIT PATNA

08-08-2022 Birla Institute of Technology Mesra Patna Campus 1

 Introduction

• Enormous growth of nanoparticles in the field of tumour destruction, petrochemical industries, environmental
remediation, agriculture, biological, biochemical application, purification/ water distillation, electronics,
electrochemical industries, photocatalysis, energy storage and sensors etc. [1-4]

• Cadmium Sulphide (CdS) nanoparticle is one of the most prominent nanoparticle that have wide range of areas
including biosensing, bio imaging techniques, photovoltaic cells, nanomedicines, molecular pathology, drug
delivery, biomolecular detection, in medical fields due to their wide band gap, high photosensitivity,
photoconductivity [5-8]

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 OBJECTIVE
• Synthesis of undoped and Mn doped CdS nanoparticles by microwave method.

• To study the structural properties of synthesized Mn doped and pure CdS nanoparticles by XRD .

• To study the different functional and vibrational groups present in the as synthesized sample of Mn
doped CdS nanoparticles by the FTIR .

• To find the kinetics and rate of dye-degradation in presence of sunlight.

• UV-visible spectroscopic study of doped CdS nanoparticles with dye.

The aim of this work is :

To study the photo catalytic degradation of Methyl Orange because it’s generally used in most of the dye
or textiles industries.

To study the rate of degradation of dye in the presence of CdS nanoparticle as photo catalyst at different
time interval of radiation in the visible range.
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 SYNTHESIS OF CdS NANOPARTICLE
Microwave method:
1)225 ml of 0.2M solution of cadmium acetate was mixed with 450 ml of 0.1M solution
of sodium sulfide.

2)Stirring process-the above mixture was stirred at 700rpm for 50 minutes at the
temperature of 60degree c.

3)After the stirring process, the sample was covered with aluminum foil .(40 minutes)
fig No.1 Stirring process
4)Microwave process-the sample undergoes microwave process, in which the sample was
microwaved for 20 seconds and then relaxed for the next 60 seconds which constitute one
complete cycle with 25% duty cycle. About 17 to 18 cycles took place for the formation
of nanoparticles.

5)The sample was cooled at room temperature for 20-30 minutes.

6)The sample (filtered residue) was washed thoroughly using double distilled water and
again filtered.

7)The residue obtained after filtration is dried in an oven at 80degree C for 24hours. fig No.2 Microwave Process
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 SYNTHESIS OF Mn DOPPED CdS
1) 225 ML of cadmium acetate (0.2M) is mixed with 100 ml of .

2) The above mixture is stirred on a magnetic stirrer at 700 rpm for 15 minutes at room
temperature.

3) 450 ml of solution (0.1M) is slowly added to the above mixture solution drop by drop.

4) Stirring process: the above mixture of sample is kept on a magnetic stirrer for 15 minutes at
700rpm. Observation: the solution turned yellowish brown when S solution was added.

5) Microwave irradiation process: The sample goes through the microwave irradiation process after stirring. Eight
complete cycles took for the formation of the nanoparticle, which look like jelly particle.

6)Filtration process :After microwave process , the sample is first cool down in temperature for 20-30 minutes after that ,it
is filtered by the use of filter paper. The obtain residue is washed thoroughly with distilled water and again filtered.

7)The obtained residue is kept in an oven at 80 degree c for 24 hours.

8)Conclusion :Mn dopped CdS nanoparticle obtained.

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 1.X-RAY DIFFRACTION (XRD) STUDIES OF Mn DOPED
CdS:

 The structural properties of as synthesized Mn doped CdS

nanoparticles have been studied by XRD analysis. It is a
primarily used technique used for phase identification and
can also provide a unit cells dimension.

 X-ray is also used for the identification of the unknown

crystalline materials. The major peaks in the spectrum of
Mn doped CdS nanoparticles as shown in fig4 have been
observed at 2θ equals 26.5°, 43.8° and 51.7°.

fig No.4 XRD for Mn doped CdS

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The average crystallite size has been calculated at the full width half maximum (FWHM) of the diffraction
peaks using Debye-Scherrer equation:
D = 𝑘λ /𝛽 cos𝜃 (1)
 
Where,
𝑘 =particle shape factor (taken 0.9)
λ=X-Ray wavelength (1.5418 Å)
𝛽= FWHM value
𝜃=angle of diffraction
 
 The inter planer spacing d can be calculated using Bragg’s law:
 
nλ = 2dsin𝜃 (2)
Where,
λ=X- Ray wavelength (1.5418 Å)
d=the inter planer spacing
𝜃 = the angle of diffraction
 

The average crystal size was found to be around 3 nm and the interplanar spacing was calculated to be
0.2393nm.
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 2.FTIR STUDIES

 The different functional and vibrational groups present in the as

synthesized sample of Mn doped CdS nanoparticles has been
identified by the FTIR Spectra (SHIMADZU-IR-Prestige21) recorded
in the range 400 to 4000 cm-1 at room temperature.

 The FTIR Spectra of Mn+2 ion doped (3%) CdS nanoparticles is

shown in fig 5. Weak absorption band around 3400-3600 cm-1 is
assigned to the presence of OH stretching vibration of water
molecules and moisture present in the prepared sample.

 The absorption peak around 2800-2900cm-1 is assigned to C-H

stretching. The small and weak peak around 1600cm-1 is due to
the presence of H-O-H bending vibration of water molecules. The
small peaks in the range of 1000-1150cm-1 are possibly due to
stretching vibration of sulphate group. The sharp peak around
615-625 cm-1 corresponds to Cd-S and Mn+2 ion doped CdS
stretching. fig No.5 FTIR of 3% Mn doped CdS

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 3.UV-Visible-Spectroscopy

 The optical properties have been explored by UV-Visible

spectroscopy (RAYLEIGH-UV2601), in which the absorption
spectra of the methyl orange mixed with Mn doped CdS
nanoparticles is recorded in the range 200-800 nm at room
temperature.

 The absorption graph is as shown in fig 6 and variation in

absorption wavelength with time interval is as given in table-1.
The graph show that the there a blue slight shift in peak as time
increases.

 As per the Beer–Lambert law, the concentration of MO is

proportional to absorbance of it and hence, the degradation
efficiency of MO can be obtained from the equation

fig No.6 Absorption spectra of Mn doped

CdS nanoparticles
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 Time (in minutes) Wavelength(nm) Absorbance(a.u) %Degradation

Pure Methyl Orange 472 0.013

Methyl Orange with CdS:Mn after 30 mins 471 0.010 23.07

Methyl Orange with CdS:Mn after 60 mins 469 0.006 53.84

Methyl Orange with CdS:Mn after 90 mins 469 0.005 61.51

Methyl Orange with CdS:Mn after 120 mins 467 0.004 69.23

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 CONCLUSION

 The synthesis of Mn+2 ion doped CdS nanoparticles were carried out by microwave method using cadmium
acetate, manganese chloride and sodium sulfide in aqueous medium. The structural analysis reveals the cubic
structure of the synthesized nanoparticles. The average crystallite size was calculated by Scherrer equation and
it was found to be around 3 nm and the interplanar spacing was calculated to be 0.2393nm.

 The various functional and vibrational groups present in the sample were characterized by FTIR analysis. A
calculated amount of nanoparticles of Mn doped CdS was mixed in the aqueous solution of an organic dye
(Methyl Orange) and the solution was irradiated in presence of intense sunlight. Weak absorption band is
assigned to the presence of OH stretching The absorption peak is assigned to C-H stretching. The small and
weak peak is due to the presence of H-O-H bending. The small peaks are possibly due to stretching vibration of
sulphate group. The sharp peak around corresponds to Cd-S and Mn +2 ion doped CdS stretching.

 The UV-Visible Spectra of irradiated sample at a specific time-intervals reveals the fact that absorption peak
shifts towards lower wavelength side. The absorbance spectra also show that there is a decrease in
absorbance peak with the increasing time interval of exposure of sunlight, which results in degradation of dye
as irradiation time increases, at 120 min degradation goes upto 69.23%.

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 CONFERENCE PAPPER

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 Thank you

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