Synthesis and Characterization of Cadmium Oxide NPs using Sapindus mukorossi (Soapnut) as natural surfactant
Avnish Kumar Arora
Department of Chemistry, Vardhaman College, Bijnor
(Affiliated to M.J.P. Rohilkhand University, Bareilly (U.P.), India – 246701.
*Corresponding Author E-mail: aroradcy@gmail.com
ABSTRACT:
The synthesis of cadmium oxide nanoparticles has been carried out in the presence of Sapindus mukorossi (Soapnut) as a surfactant and the characterisation of the synthesized nanoparticles has been carried out using analytical techniques such as XRD, magnetic studies and SEM. The synthesised cadmium oxide was CdO. The structure of the CdO was face-centred cubic. Magnetic susceptibility measurements showed that there were no unpaired electrons in CdO. Hence, CdO is diamagnetic in nature. The exact size of the cadmium oxide was found using SEM. The size of the oxide was from 28 nm to 50 nm.
Nanomaterial research is of great concern today, since the properties of the materials change with size. Oxide nanoparticles are of great use as they have wide applications1-14. Cadmium oxide nanopaticles are of much concern as they have many applications in semiconductor devices, such asas catalyst, photocatalyst, nanofibre etc. Recently, some scientists have made attention towards their synthesis and applications. Khan et al.15 synthesised CdO nanoparticles using the Sol – gel method and studied their role in the photocatalytic degradation of methyl orange dye. Saravanan et al.16 synthesisedflorine-doped cadmium oxide thin films and studied their non-linear optical characterisation. Rather et al.17 synthesised cadmium sulphide and cadmium oxide nanoparticles. They studied their cytotoxic and antimicrobial role. Haider et al.18 synthesised CdO nanoparticles by green synthesis using Dalbergia sissoo leaf extract. CdO nanoparticles were utilised for their photocatalytic activity by degradation of methylene blue dye.
Fluorine-doped CdO nanoparticles were synthesized by the chemical spray pyrolysis method19. Their role in solar cell and optoelectronic devices was discussed. Nanofibre thin films of CdO were deposited at room temperature on glass and characterized by different analytical techniques20. CdO nanoparticles were developed on the CuSe surface for the making of a hybrid super capacitor by khan et al.21. Nano CdO particles have been synthesized using the sonochemical method from their coordinate precursor22 and characterised by XRD, SEM and TEM. CdO and Cs-doped CdO nanoparticles have been synthesised by Anwar et al.23. The cauliflower structure of oxide nanoparticles was developed. The spin coating method was used for their development. High-performance nanoscale polyaniline and cadmium oxide super capacitors have been developed. The antibacterial effect of nanosized cadmium oxide on Staphylococcus aureus and Pseudomonas aeruginosa bacteria was investigated by Salehi et al.24. Therefore, cadmium oxide nanoparticles are being synthesised and applied in various fields. But there are not too many references to this topic. Therefore, focus has been on their synthesis in then an orange. In this work cadmium oxide naoparticles have been synthesised using a natural surfactant. Soapnut was used as a natural surfactant. The obtained particles of Cadmium Oxide have a size ranging from 28 nm - 50nm. The synthesized NPs were characterised by X-ray diffraction, magnetic measurement, and SEM studies. This method involves a simple, inexpensive and one-step process for the synthesis of very fine Cadmium Oxide NPs as compared to other methods of synthesis like ultrasonic radiation, sol-gel approach, colloid mill, mechanical milling, etc.
2. METHODS AND MATERIALS:
2.1 Chemicals:
The chemicals used were of GR grade. CdCl2.H2O and alcohol ammonia (NH4OH) were purchased from Rankem, India. The soap was purchased from the market in natural form. Double-distilled water was used to perform the synthesis.
2.2 Cadmium oxide nanoparticles (synthesis procedure):
Cadmium chloride solution (CdCl2.H2O) in water (750mL of 0.05M solution) was taken in a beaker. In this Sapindusmukorossi (Soapnut) was added (1ml of extract in water) added. The dropwise addition of a 0.05M solution of aqueous ammonia was carried out. The solution was stirred. Liquor ammonia was added in it until the precipitation was complete. The pH was observed during the experiment and was 10.5 at the end of the reaction. The temperature of the solution was maintained at 60°C in the experiment. The precipitates were filtered. The precipitates thus obtained were washed with distilled water. Excess ammonia was removed. The precipitates were kept in an oven. Theoven temperature was set at 60oC. After twenty-four hours, the precipitates were removed. A mud furnace was used for the calcinations. The precipitates were calcined at 500°C. Calcination was carried out for six hours. The calcined oxide was ground with the help of pestle and mortar. The obtained metal oxide was sieved through 100 mesh size sieve and characterised.
2.3 Characterization of nanoparticles:
The characterization of the nanoparticles was carried out using an X-ray diffractometer (Bruker, D – 8). The scanning electron microscope LEO 435 VP was used to measure the exact size of the particles. The magnetic behaviour was measured using the PAR 155 model.
Outcome and Deliberations:
3.1. X-ray results:
The obtained XRD of the zirconium oxide is given in Fig. 1. In X-ray diffraction, the obtained spectra were compared with the standard with their d - values (1.21A0 to 2.70A0) [JCPDS file No. JCP 2.2 CA-00-001-1049]. On the basis of x-ray diffraction, this was concluded that the synthesised oxide is pure CdO and exists in face-centre cubic form. (Table 1). All peaks correspond only to cadmium oxide. No peak due to any impurity shows that synthesised exists in its pure form. The peaks of the obtained spectra were sharp. Hence, it shows good crystal growth of nanoparticles of oxide. The size of the particles was calculated using Scherer’s formula and it was observed form 34.88nm to 54.34nm (Table 2).
Figure 1: XRD spectra of Cadmium oxide NPs
(JCPDS file of standard Cadmium Oxide)
Table1: X-RAY Diffraction Data for Cadmium Oxide NPs
S. N. |
d-spacing value [Ao] (Observed) |
d-spacing value [Ao] (Reported) |
I/I×100% (Observed) |
I/I×100% (Reported) |
1. |
2.70912 |
2.7000 |
100 |
100 |
2. |
2.34140 |
2.3400 |
79.32 |
100 |
3. |
1.65849 |
1.6598 |
42.54 |
100 |
4. |
1.63045 |
1.6304 |
18.69 |
20 |
5. |
1.41490 |
1.4158 |
24.87 |
75 |
6. |
1.35521 |
1.3552 |
10.69 |
30 |
Table 2: Observation for the Thickness of Crystal Size for CdO NPs
S. N. |
2 (observed) |
Ɵ |
B (radians) |
t (nm) |
1. |
31.42 |
15.71 |
0.028 |
50.98 |
2. |
21 |
10.5 |
0.039 |
35.86 |
3. |
19 |
9.5 |
0.026 |
54.34 |
4. |
37 |
18.5 |
0.031 |
47.03 |
5. |
52 |
26 |
0.043 |
34.88 |
6. |
58 |
29 |
0.042 |
37.51 |
3.2 Magnetic studies:
Magnetic studies showed the diamagnetic behaviour of the cadmium oxide nanoparticles. The value of the magnetic moment obtained was 0.320 B.M at 250C. This value of the magnetic moment is in close agreement with that of pure CdO as it is diamagnetic in nature and has a real value of 0.0 B.M. Therefore, all electrons are paired and therefore the oxide is diamagnetic [Table 3].
Table 3: Magnetic susceptibility data of CAD NPs
Metal Oxide |
meff (cal) (B.M.) |
meff (obs) (B.M.) |
Cadmium oxide |
0.0 |
0.320 |
3.5 SEM studies of cadet oxide oxide NPs:
The exact particle size of the synthesised NPs was measured with the help of SEM. Scanning electron microscopy showed the nano range of the particles. The size ranged from 28nm to 50nm (Fig.2). Scanning electron microscopy revealed that oxide nanoparticles are glossy in nature.
Fig. 2: SEM studies of Cadmium oxide NPs
4. CONCLUSIONS:
Synthesised nanoparticles are face-centred cubic. The purity of the oxides is reflected in the XRD studies, as no other peak as a result of any impurity was there. In the presence of Soapnut as a surfactant, the nanoparticles obtained were in a limited range of 28nm - 50nm. The diamagnetic behaviour of the synthesized oxide was observed with the help of magnetic measurement studies.
Cadmium oxide NPs having face-centred cubic structure have been synthesised successfully by the aqueous precipitation method using ammonia as the precipitating agent and soapnutas the surfactant. X-ray diffraction (XRD) studies show that cadmium oxide was formed as pure CdO. From SEM study, it is observed that they are of size ranging from 28nm to 50nm. Magnetic measurements studies show diamagnetic behaviour of Cadmium oxide NPs.
5. ACKNOWLEDGEMENT:
The authors acknowledge Punjab University Chandigarh and CBRI, Roorkee for carrying out XRD, Magnetic studies, and SEM, respectively.
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Received on 03.08.2023 Modified on 14.10.2023
Accepted on 28.12.2023 ©AJRC All right reserved
Asian J. Research Chem. 2024; 17(1):41-44.