International Journal of Scientific Research Engineering & Technology (IJSRET) Volume 2 Issue2 pp 056-059 May 2013 www.ijsret.

org ISSN 2278 - 0882

Ultrasound tailoring of industrially important nano particles

Irudayaraj Johnson *, H. Joy Prabu, S. Arulappan
Centre for Nano science and Applied Thermodynamics, Department of Physics, St. Josephs college, Trichy 620002, India

jnaadarsh@yahoo.co.in

Abstract: The behaviour of particles can be tailored effectively

to suit the industrial and medical needs of the modern society when their size has been reduced from macro or micro to nano dimension. Normally this particle size reduction has been achieved by chemical synthesis method. However non conventional techniques like ultrasound is more eco and environmental friendly one. The efficiency in size reduction is also much better when we apply the correct frequency for the desired application. The ZnSe nanoparticles have wide-ranging applications in opto elctronics and photo acoustic industries. Many researchers tried the preparation of ZnSe nano particles by chemical techniques in the past while in the present work much attention was paid on the non conventional preparation method ie., ultrasound technique to achieve efficiency in the preparation. In the present study ZnSe nanoparticles were prepared by Chemical Method and the influence of ultrasound during synthesis has been tested separately. The prepared nanostructures were characterized by using powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). The size of nano particles was estimated by Scherrers equation. It has been found that the ultrasound at high frequencies does a wonderful to achieve more finer nano particles of ZnSe and it is less hazardous and more environmental friendly.

2. EXPERIMENTAL DETAIL 2.1. Materials Zinc Selenide (ZnSe) is a transparent powder in wide spectral range from yellow (visible) to far IR. ZnSe material is a chemically inert, highly pure product that is very effective in many optical applications due to its extremely low bulk losses, high resistance to thermal shock and stability in virtually all environments. The high quality zinc and selenium powders (SIGMA ALDRICH) were used for the synthesis of ZnSe nanoparticles. Hexane, Methanol, Pyridine was used as purchased from Aldrich. All chemicals were used directly without any further purification. 2.2. Synthesis of ZnSe nanoparticles The prepared ZnSe powder (99.9%) of 1.91 gram has been taken and 25ml of Hexane is added. And this was put under a vigorous magnet stirring rotation process at the range of 200 -250 rpm for 3 hours and above at 85c temperature (2). Once the Hexane gets evaporated and the sample is taken away very carefully from the magnetic stirrer since the size of the particles are very minute and it could be easily blown away or dropped. The sample is kept in a quiet place to get settled down and to reduce its temperature. Once the temperature is reduced, the sample is filtered. 2.3. Filtering Process of ZnSe nanoparticles The filtering process starts with adding 20mL of Methanol with the sample of Zinc Selenide (ZnSe) and the solution has been filtered by using 0.2 micrometer PTFE filter paper. This is repeated for two times. A sufficient amount of Pyridine is added for further purification process and it is filtered again as we have done above. In order to get a purified powder, a small amount of acetone

Index terms: Ultrasound, High frequency, ZnSe, Nano particles, Chemical method, SEM micrograph, Powder XRD.

1. INTRODUCTION
In the present investigation we have synthesized ZnSe nanoparticles with a homogeneous crystallite size within a short time from Zn and Se elements by chemical techniques (1) while simultaneously tried with ultrasound technique. The synthesized nanoparticles were subjected to powder X-ray diffraction to check the crystalline structure, lattice parameters and to calculate the crystallite size. The scanning electron microscopy study (SEM) was used to determine the particle size and shape. It has been observed that the Ultrasound technique is having its own advantage over the conventional techniques.

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[1], d=3.2866(3), 2-theta=27.109(2)

International Journal of Scientific Research Engineering & Technology (IJSRET) Volume 2 Issue2 pp 056-059 May 2013 www.ijsret.org ISSN 2278 - 0882
[3], d=2.00836(10), 2-theta=45.107(2)

6.0e+004

[6], d=1.30189(5), 2-theta=72.552(3) [7], d=1.26901(8), 2-theta=74.747(5)

[5], d=1.41870(7), 2-theta=65.770(3)

[8], d=1.15828(5), 2-theta=83.370(4)

Intensity (cps)

4.0e+004

2.0e+004

Intensity (cps)

2.5. Scanning electron microscope The scanning electron microscope (SEM) has been used to find out the morphology and size of the synthesized nanoparticles of the ZnSe material. The ZnSe powder was dried in vacuum using rotary evaporator (5). 3. RESULTS AND DISCUSSION The Zinc Selenide (ZnSe) nanoparticle was prepared by chemical method and the powder was dried by using hot air oven (300c). The transparent yellow (ZnSe) product is obtained after the completion of reaction and characterized by various techniques in order to investigate their particle size and structural features(6).

0.0e+000 20 1.0e+004 5.0e+003 0.0e+000 -5.0e+003 -1.0e+004 20 40 40

[2], d=2.2265(8), 2-theta=40.482(16)

60

80

60

80

2-theta (deg)

Figure 1. X-ray diffraction pattern of ZnSe

The values of the lattice parameter determined from the Xray diffractogram using powder X software which clearly matches with the reported values of lattice parameter of ZnSe. The presence of a relatively sharp peak on a background of a wider peak suggests that both large and small grains are collected together. Scherrers formula is used for calculating the nanoparticle size of the sample (7). The surface morphology of Zinc Selenide (ZnSe) was studied by SEM technique that shows that these materials are polycrystalline in nature. Particle sizes are found have a range of 10 to 15 nm.

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[9], d=1.09183(4), 2-theta=89.741(4)

2.4. X-ray powder diffraction The synthesized nanoparticles were subjected to powder X-ray diffraction to know the crystalline phase presents in the synthesized compound using PW3710 based Philips Analytical powder X-ray diffractometer with nickel filtered (3,4). The specimen was scanned for the angular range 560 of 2-theta with the scan rate of 0.001/s.

[4], d=1.71207(7), 2-theta=53.477(2)

is added and then filtered again and again many times. At last the powder is collected in Petri dish.

International Journal of Scientific Research Engineering & Technology (IJSRET) Volume 2 Issue2 pp 056-059 May 2013 www.ijsret.org ISSN 2278 - 0882

10 nm
Figure4. SEM micrograph for ZnSe nanoparticles (after Ultrasound irradiation -final). Figure 2 SEM micrograph for ZnSe original powder (Immediately after chemical synthesis) The crystallinity of the derived particles was probed by Xray diffraction. Typical XRD patterns of the prepared ZnSe nanoparticle were showed in Fig. 1. The three distinct diffraction peaks were observed and it was matched with JCPDS No. 050522). Broad nature of the XRD peaks could be attributed to the nano-crystalline nature of ZnSe particles. With the reaction temperature higher, the intensity of the XRD peaks increased, which may indicate that the reaction temperature have important influence on the crystallinity of ZnSe nanocrystals. The Scanning electron microscopy (SEM) images of the ZnSe nanoparticles at different stages have been reported in Figs. 2 and 3. But however it is important to note that a grerater reduction and finer particle size is made possible only after subjection of ZnSe to ultrasonic irradiation of frequency 12 MHz. for nearly one week time duration. It has been observed that successive reduction synthesis and ultrasonic irradiation process yields good result in reducing the particle size than exclusive chemical synthesis techniques. These figures show that the product particles are spherical in shape and agglomeration is also observed. This agglomeration is caused because we did not use any capping agent for synthesis of ZnSe nanoparticles. 4. CONCLUSIONS In the present investigation we have observed a greater reduction in the size of ZnSe nano particles by Ultrasound method than chemical synthesis method. Powder X-ray diffractogram shows that ZnSe

Figure 3. SEM micrograph for ZnSe nanoparticles after 2 rounds of reduction by chemical synthesis techniques.

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International Journal of Scientific Research Engineering & Technology (IJSRET) Volume 2 Issue2 pp 056-059 May 2013 www.ijsret.org ISSN 2278 - 0882

nanocrystallites are polycrystalline in nature. The calculated crystallite size was found ~ 6.33 nm while the particle size obtained by SEM was ~4.45 nm. The SEM image shows that the ZnSe nanoparticles are spherical in shape with agglomeration. Acknowledgements The authors are thankful to CSIR, New Delhi for its financial assistance in the form of Major research project. REFERENCES 1. M.P. Deshpande, S.H. Chaki, N.H. Patel, S.V. Bhatt, B.H. Soni J. Nano- Electron. Phys. 3 (2011) No1, P.193-202. 2. B.O. Dabbousi, (CdSe) ZnS Core shell quantum dots . Synthesis and characterization of a size series of highly luminescent nano crystallites, J. Phys. Chem. B 1997, 101, 9463-9475 3. F. Mollaamin,Synthesis of various nano and micro ZnSe morphologies by using hydrothermal method,2011,International Journal of the Physical Sciences Vol. 6(6), pp. 1496-1500. 4. Gon H, Huang H, Wang M, Liu K (2007). Characterization and growth mechanism of ZnSe microspheres prepared by hydrothermal synthesis. Ceram. Inl., 33:1381-1384. 5. Mohd. Shakir,Characterization of ZnSe nanoparticles synthesized by microwave heating process,Solid State Communications 149 (2009) 2047-2049. 6. Hyun-Chul Ko,New approach to the fabrication of CdSe/ZnSe quantum dots using a cleaved-edge overgrowth technique Journal of Crystal Growth ,1998, 283-287. 7. Pradeep Verma,Optical Identification of Cu Doped ZnSe Nanoparticles ,J. Pure Appl. & Ind. Phys. 2011,Vol.1 (4), 212-220 .

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