Synthesis and Characterization of Zirconium Oxide Nanoparticles using Sapindus mukorossi (Soapnut) as natural surfactant, A green synthetic approach

 

Avnish Kumar Arora¹*, Lalit Chauhan², Pankaj Kumar³

¹Department of Chemistry, Vardhaman College, Bijnor

(Affiliated to MJPRU Bareilly, (U.P.), India – 246701.

²Department of Physics, Vardhaman College, Bijnor

(Affiliated to MJPRU Bareilly, (U.P.), India – 246701.

³Department of Chemistry, COES University of Petroleum and Energy Studies,

Bidholi, Dehradun (U.K.), India – 248006.

*Corresponding Author E-mail: aroradcy@gmail.com

 

 

1. INTRODUCTION:

Nanomaterial research is of great concern now a day as the properties of the materials changes with the size. Oxide nanoparticles are of much use as they have wide applications. Zirconium oxide is has applications in medicinal chemistry. It is highly resistant to heat so it has application in ceramics. Besides it is used in jewelry also. Zirconium oxide has been synthesized and their applications in different fields are under view. Zirconium oxide have been synthesized using thermal treatment method by Keitab et al.¹ synthesized zirconia nanoparticles and studied their structural and optical properties. Hu et al.² used zirconium nano size particles in dentistry. Hazmi et al.³ synthesized and characterized zirconium oxide nanoparticles for their various applications. Zirconium oxide nanoparticles have been fabricated ant studied their applications as antioxidant and anticancer agent by Balaji and coworkers⁴. Copper oxide – dopped zirconium oxide microfibers have been synthesized by Liu and co workers⁵.

 

Non – enzymatic MP sensors have been made by using them for their applications. Zirconium oxide nanopaeticles have been synthesized by using bael fruit extract and further studied for their antimicrobial activities⁶. Nagaraju et al. synthesized⁷ synthesisd Tantalum-zirconium oxide (TZ). Synthesisd catalyst have been used for biodiesel production. One pot synthesis of Tetrahydropyridines using Polyaniline – zirconium oxide as catalyst have been done by Ajeet and cowokers⁸. Zirconium oxide based sorbents have been synthesized and further used for removal of fluoride from water⁹. Non imprinting lithograpy method have been used to develop self-aligned crystals on zirconium oxide¹⁰. Different research publication show the application of zirconium oxide in various fields. Hence synthesis of zirconium oxide nanoparticles is of much importance. As the size and properties depends upon the method of synthesis, so methods are being developed for synthesis. This research work is on the synthesis of zirconium oxide nanoparticles using a natural surfactant. Soapnut was used as surfactant. The obtained particles of zirconium Oxide have size ranging from 13nm -26 nm. The synthesized nanoparticles were characterized by using X–Ray Diffraction method, Magnetic Measurement and TEM studies.

 

 

2. MATERIALS AND METHODS:

2.1 Chemicals:

Chemicals used were of GR grade. ZrOCl₂ and Liquor Ammonia (NH₄OH) were purchased from Rankem, India. Soapnut was purchased from market in natural form. Double distilled water was used to perform the synthesis.

2.2 Zirconium Oxide Nanoparticles (Procedure of Synthesis):

Zirconium oxy Chloride (ZrOCl₂) solution in water (750mL of 0.05M solution) was taken in a beaker. In this Sapindus mukorossi (Soapnut) was (1 mL extract in water) added. Dropwise addition of 0.05M solution of aqueous ammonia was carried out. Solution was stirred. Liquor ammonia was added in it till complete precipitation. pH was noted during the experiment and it was 10.5 at the end of the reaction. Temperature of the solution was maintained at 60°C in the experiment. Precipitates were filtered. The precipitates thus obtained were washed with distilled water. Excess of ammonia was removed. Precipitates had been kept in an oven. Temperature of the oven was fixed at 60°C. After twenty four hours precipitates were taken out. Muffle furnace was used for calcinations. Precipitates were calcined at 500°C. Calcination was carried out for six hours. Calcined oxide was grinded. 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:

Characterization of nanoparticles was carried out using X- Ray diffractometer (Bruker, D – 8). FEI Tecnai G² 20 S-Twin TEM was used for measuring the exact size of particles.. The magnetic behavior was measured out by using Model PAR 155.

 

Figure 1 : XRD spectra of Zirconium  oxide nanoparticles

 

3. OUTCOME AND DELIBERATIONS:

3.1. X-ray results:

Obtained XRD of the zirconium oxide is  given in Fig 1. In X-ray diffraction, obtained spectra was compared with the standard with their d - values (1.22A⁰ to 2.96A⁰) [JCPDS file No.JCP 2.2 CA-00-006-0395]. Om the basis of x-Ray diffraction, this was concluded that the synthesised oxide is pure ZrO₂ and exist in monoclinic form. (Table 1).  All peaks correspond to zirconium oxide only. No peak due to any impurity shows that synthesised exists in its pure form.

3.2 Magnetic Studies:

Magnetic studies showed diamagnetic behavior of the zirconium oxide nanoparticles. The value of the magnetic moment obtained was 0.140 B.M at 25⁰C. This value of magnetic moment is in close agreement of the pure ZrO₂ as it is diamagnetic in nature and has real value of 0.0 B.M. So all electrons are paired and hence the oxide is diamagnetic [Table 2].

 

Table1: XRD values of Zirconium Oxide 

 

Table 2 Magnetic susceptibility data of zirconium oxide Nanoparticles

 

Fig.  3. TEM studies of Zirconium oxide Nanoparticles

 

 

3.3 Transmission Electron microscopic measurement:

Exact particle size of the synthesized NPs was measured with the help of TEM. Transmission Electron microscopic measurement showed the nano range of the particles.   Size was from 13nm to 26nm (Fig 2.)

4. CONCLUSION:

Synthesized nanoparticles are monoclinic.  Purity of the oxides is reflected with the XRD studies as no other peak due to any impurity was there. In the presence of the Soapnut as surfactant, nanoparticles obtained were in a limited range from 13nm – 26nm. Diamagnetic behavior of the synthesized oxide was observed with the help of magnetic measurement studies

 

5. ACKNOWLEDGEMENT:

Acknowledgements are to Punjab University Chandigarh for carrying out for carrying out XRD  and TEM and IITR for magnetic  studies.

 

6. REFERENCES:

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Received on 22.10.2022                    Modified on 20.11.2022

Accepted on 07.12.2022                   ©AJRC All right reserved