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Journal of NanoScience, NanoEngineering & Applications
Contents
1. A Study on the Synthesis and Characterization of Silver Metal Nanoparticles with Acrylic Acid-Acrylamide (AA) Copolymer as Mediating Agent B. Sanjeeva Rao, K. Rajendra Prasad, S. Kalahasti, Ch. Srinivas, B. Suresh Babu
1
2. Characterization of Mn Dopped SrAlO Nano-Phosphors Prepared via Sol-Gel Method V.T. Jisha
5
3. Effect of Annealing on Structural and Surface Properties of Nanostructured ZnO Thin Films T. Shiyani, U.D. Khachar, R. Mansuriya, P. Solanki, R. Doshi, P. Vachhani, J.H. Markna, D.G. Kuberkar
11
4. Influence of Dip Cycles on the Structural, Optical and Morphological Properties of CdS-SILAR Deposited Thin Films Kester O. Ighodalo, Tochukwu M. Emeakaroha, Blessing N. Ezealigo, Kenneth Iloure
19
5. Growth and Description of Cu Nanostructure via a Chemical Reducing Process S.C. Barman, D.K. Saha, H. Mamur, M.R.A. Bhuiyan
27
Journal of Nanoscience, Nanoengineering & Applications ISSN: 2231-1777(online), ISSN: 2321-5194(print) Volume 6, Issue 3 www.stmjournals.com
A Study on the Synthesis and Characterization of Silver Metal Nanoparticles with Acrylic Acid-Acrylamide (AA) Copolymer as Mediating Agent B. Sanjeeva Rao1, K. Rajendra Prasad2, S. Kalahasti3, Ch. Srinivas4, B. Suresh Babu5 1
Department of Physics, Government Degree College, Mulugu, Warangal, West Bengal, India 2 Department of Physics, Kakatiya Institute of Technology and Science, Warangal, West Bengal, India 3 Department of Physics, Kakatiya University, Warangal, West Bengal, India 4 Department of Physics, SR Degree College, Hanamkonda, West Bengal, India 5 Department of Physics, Kakatiya Government College, Hanamkonda, West Bengal, India
Abstract
Silver metal nano-particles (MNP) have been synthesized by chemical methods with acrylic acid- acryl amide (AA) copolymer as mediating agent. Formation and interaction of silver metal nano- particles with AA copolymer has been confirmed by ultraviolet–visible (UV-VIS), Fourier Transform Infrared (FTIR) techniques. Thermal and morphological properties of the composite have been studied by Differential Scanning Calorimetry (DSC) and Scanning Electron Microscope (SEM) techniques. Change in intensity together with shift of FTIR absorption bands in the regions of 3500–3150 cm-1 and 1700 cm-1 position in an evidence for interaction of silver metal particles with amide (CONH2) and carboxylic acid functional (COOH) groups of the copolymer. Presence of 280 nm, 350 nm and 450 nm optical absorption bands indicate the formation and existence of silver nano metal particles in copolymer matrix. DSC thermogram indicates that the thermal stability of the complex is more than the copolymer. The silver nano metal particles are found to lie on the surface of copolymer matrix. Keywords: Copolymer matrix, nanoparticles, optical absorption, silver metal
INTRODUCTION
The metal nanoparticles (MNPs) have attracted the attention of various researches due to their attractive electrical, optical and catalytic properties. The MNPs can be produced by both chemical and physical methods. As the generated MNPs have a tendency to agglomerate, surface passive elements, surfactant molecules like polymers are used to prevent this. In this context, Choo et al. [1], Shin et al. [2] have used poly (vinyl pyrrolidone) (PVP) and Kumar et al. [3], Luo et al. [4] have used poly (ethylene glycol) (PEG) as mediator for the synthesis of silver nanoparticles and to prevent the agglomerates. Comparing to the conventional reducing agents like hydrazine, sodium boroxide and dimethylformamide, ethylene glycol (EG) or polyethylene glycol (PEG) is reported to be environmentally benign. Various types of
reducing agents are reported in the literature [5], to produce nanoparticles. In this context, the authors have used poly (acrylic acid) as mediating agent to synthesize the silver MNPs [6]. In the present studies, authors were attempted to generate silver MNPs with acrylic acid-acryl amide (AA) copolymer as reducing or mediating agent. The spectroscopic, thermal and morphological properties are investigated.
EXPERIMENTAL SETUP
Silver nanoparticles are synthesized by chemical method with AA copolymer as reduction agent. The AA copolymer is dissolved in 100ml of water and aqueous solution of 0.1 AgNO3 is added to it by drop by drop with constant stirring for several hours at 80°C.The resultant solution is annealed to get the powder of complex. Optical absorption
JoNSNEA (2016) 1-4 © STM Journals 2016. All Rights Reserved
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Journal of Nanoscience, Nanoengineering & Applications ISSN: 2231-1777(online), ISSN: 2321-5194(print) Volume 6, Issue 3 www.stmjournals.com
Characterization of Mn Dopped SrAlO Nano-Phosphors Prepared via Sol-Gel Method V.T. Jisha* Research Centre, S.T. Hindu College, Nagercoil, Tamil Nadu, India Abstract
Strontium aluminate with Mn dopped phosphor was synthesized by Sol-Gel method using Strontium Acetate, Aluminium Acetate as raw material and 2-methoxyethanol as complexing agent. The transparent sol was preheated at 100 C for 2 h and then the precursor was finally annealed at 950C for 2 h. The phosphor emits luminescence with peak wavelength at 395 nm and 520 nm under near-ultraviolet excitation at 360 nm. The morphology, composition and structure of the synthesized phosphors were characterized by scanning electron microscope (SEM), energy dispersive X-ray (EDX) and X-ray diffraction (XRD) respectively. Keywords: Strontium aluminate, stoichiometry, nanocrystals, aluminium acetate, sol-gel method
INTRODUCTION
For the synthesis of aluminum-based oxide phosphors, this method has been widely accepted nowadays. Several reports are available on the synthesis of different strontium aluminate family hosts, such as Sr3Al2O6, Sr4Al14O25, SrAl2O4, and SrAl12O19 using low temperature combustion technique [1–4]. Sol-gel synthesis possesses some benefits, namely, relatively low preparation temperature, easy control of the stoichiometry, high levels of product homogeneity, and no need for the use of expensive equipment. Luminescent semiconductor nano-crystals, especially II-VI semiconductors, have attracted great deal of attention in the past few decades due to their unique properties and potential applications [5–10]. The most extensively investigated doped semiconductors are Mn, Dy and Eu doped BaAIO, CaAlO and SrAlO nano-crystals. The doping ion act as recombination centers for the excited electron-hole pairs and result in strong and characteristic luminescence. In doped compound semiconductors, in contrast to the undoped semiconductors, the impurity states can play a special role in affecting the electronic energy structures and transition probabilities. Phosphors based on oxide matrices are attractive host materials for the development of advanced phosphors due to their ease of synthesis and
stability. We have developed a phosphors of SrA1O:Mn and studied its photoluminescence properties [11, 12].
EXPERIMENT
The procedure of synthesizing nanoparticles is thoroughly described as follows: 98 wt% of 2 M Strontium acetate [(CH3.COO)2 Sr.2H2O was dissolved in 25 ml of 2-methoxyethanol with vigorous stirring. 1 wt% of 2M Manganese nitrate [(CH3.COO)2 Mn.2H2O] was dissolved in 25 ml of 2-methoxyethanol with vigorous stirring. Simultaneously, 1 wt% of 2M Aluminum acetate [C4H6AlO4.4H2O] was dissolved in 25 ml of 2-methoxyethanol with vigorous stirring and subsequently, it was added to the first solution to reach 50 ml in total. Then it was stirred for 30 min at room temperature for the second time. Ammonia was slowly added to this solution with a constant stirring until a pH of 10.5 was achieved. After the stirring of the solution for 30 min, acetic acid and ethylene glycol in the ratio 1:1 was added to the solution. The sol was heated at 80°C while being mechanically stirred with a magnetic stirrer. As the evaporation proceeded, the sol turned into a viscous gel. The gel was aged for 2 h and then dried at 100°C for about 5 h. The resulting materials were well grinded and annealed at 950°C for 5 h to obtain Mn doped SrAl4O7 nanopowders. For the
JoNSNEA (2016) 5-10 © STM Journals 2016. All Rights Reserved
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Journal of Nanoscience, Nanoengineering & Applications ISSN: 2231-1777(online), ISSN: 2321-5194(print) Volume 6, Issue 3 www.stmjournals.com
Effect of Annealing on Structural and Surface Properties of Nanostructured ZnO Thin Films T. Shiyani1,2,*, U.D. Khachar1, R. Mansuriya1, P. Solanki1, R. Doshi1, P. Vachhani1, J.H. Markna1,2, D.G. Kuberkar1 1
Department of Physics, Saurashtra University, Rajkot, Gujarat, India Department of Nanotechnology, VVP Engineering College, Gujarat Technological University, Rajkot, Gujarat, India
2
Abstract
ZnO thin films with different grain size were grown on amorphous quartz substrate using spin coating method. We have reported the effect of annealing temperatures on the structural and surface properties of ZnO thin films. The surface properties were characterized by AFM. From XRD analysis, it can be seen that, the FWHM decreases with an increase in annealing temperature from 500 to 575ºC which is reflected in the increase in the particle size with annealing temperature. The grains are well developed in nature with the size ranging between 100 and 200 nm and the height of the grains range between 25 and 55 nm. The absorption spectrum in the UV-visible range of ZnO film was taken to confirm the diameter of nanoparticle. The value of the average diameter (D) of ZnO particle in the CSD grown film is estimated to be ~10 nm, which is in the range of the particle size obtain from XRD. Keywords: ZnO, thin film, microstructure, annealing
INTRODUCTION
Nanotechnology is the technology of materials usually in the range of 1 to 100 nm. When at least one of the dimensions of any type of material is reduced below ~100 nm, its mechanical, thermal, optical, magnetic and other properties change at some size characteristic of that material [1, 2]. Thus within the same material one can get range of properties. There are two fundamental approaches to fabricating nanomaterials. First, bottom-up approach corresponds to construction of nanomaterials from fundamental building blocks such as molecules or atoms. Second, top-down approach corresponds to create a nanostructure from a bulk material [3]. There are large numbers of physical, chemical, biological and hybrid techniques available to synthesize different type of nanomaterials in the form of colloids, clusters, powders, tubes, rods, wires, thin films, etc. A bulk material should have constant mechanical properties regardless of its size, but at the nanoscale this is often not the case. The properties of materials change
dramatically as their size reaches to the nanoscale. Mechanical properties such as hardness, mechanical strength, ductility, toughness, etc. are affected at nanoscale. The enhanced diffusivity observed in the grain boundary structure of nanostructured materials is the mechanism thought to be responsible for the changes in thermal properties. In metals, thermal conductivity and melting point have been observed to decrease while thermal expansion coefficients have been observed to increase. An increased chemical activity can be obtained by the large number of atoms on the surface of nano-crystallites providing active sites for reactions. The size of dispersion materials in a composite can alter the wavelength of light that is absorbed by the particulates. Altering the size of a particle can change the associated energy and wavelength of light absorbed. In semiconducting materials, the band gap between the valance band and conduction band increases as the size of the particle decreases. The resistivity of nanomaterials is higher because of the electron scattering at grain boundaries [2–6]. ZnO is a semiconductor with direct bandgap energy of 3.37 eV at room temperature. It is soluble in
JoNSNEA (2016) 11-18 © STM Journals 2016. All Rights Reserved
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Journal of NanoScience, NanoEngineering & Applications ISSN: 2231-1777(online), ISSN: 2321-5194(print) Volume 6, Issue 3 www.stmjournals.com
Influence of Dip Cycles on the Structural, Optical and Morphological Properties of CdS-SILAR Deposited Thin Films Kester O. Ighodalo*, Tochukwu M. Emeakaroha, Blessing N. Ezealigo, Kenneth Iloure Crystal Growth and Characterization Laboratory, Department of Physics and Astronomy, University of Nigeria, Nsukka, Nigeria
Abstract
Cadmium sulphide (CdS) thin films were deposited on a glass substrate by a relatively simple and cost effective successive ionic layer adsorption and reaction (SILAR) method at temperature 80ºC at different deposition cycles. For a fine nanocrystalline thin film growth, the parameters include concentrations of cationic and ionic precursors, number of immersion cycles, and the immersion time. A study was made to know how dip cycles affects the structural, surface morphological and optical properties of the film using X-ray diffraction (XRD), EDAX, scanning electron microscopy (SEM) and UV-VIS (ultraviolet visible) spectrophotometer. The deposited CdS thin films were found to be greenockite αCdS film with a strong preferred orientation along the (002) plane exhibit hexagonal phase with optical band gaps between 2.38 and 2.70eV. The band gap with a value to a certain extent larger than the distinctive value of the bulk CdS (2.42 eV), can be ascribed to quantum confinement effects due to the nanometer crystallite size of the CdS thin films. Keyword: Thin films, SILAR, SEM, XRD, UV-VIS
INTRODUCTION
SILAR deposition technique is known to be a simple and inexpensive large-scale deposition technique. It has been used in the deposition of semiconductor thin films for many years. This technique does not require high quality target or substrate and it does not need high vacuum to work. Also we can easily control the thickness and deposition rate of the films in wide variation by changing the duration of rinsing, changing the number of cycles and so on. Nanometer-sized semiconductors exhibit structural, electronic, optical, luminescence, and photo conducting properties [1, 2]. Nanocrystalline cadmium sulphide (CdS) is a wide band gap material, which belongs to IIVI group compound materials in the periodic table. Its band gap varies between 2.1 and 2.4 eV, depending upon chemical composition and many other factors. This CdS thin films have been vastly used in the world due to its applications in piezoelectric transducers, photoconductors, transistors, photo-resistors, laser materials and photovoltaic cells, also it
can be used as a window material together with several semiconductors such as CdTe, Cu2S and CuInSe2 [3, 4]. In CdS/CdTe heterojunction solar cells, where CdS acts as the n-type semiconductor for the window layer. A thicker CdS layer is believed to yield a includes a cadmium salt, a complexing agent, and thiourea as sulphur source. CdS films have lower transmittance. In addition, as CdS films become thinner, the probability of a short circuit between the CdTe and the front contact increases. The SILAR process for the preparation of CdS thin films been prepared by many techniques, some of the techniques including electrochemical method, chemical bath deposition method, thermal evaporation method, chemical vapor deposition method, vapor–liquid–solid growth method, pulsed laser deposition method, spray pyrolysis method, chemical bath technique under rotation method [5–13]. Thus, the deposition rate can be improved by changing the chemical reagents concentrations, changing the bath temperature and deposition
JoNSNEA (2016) 19-26 © STM Journals 2016. All Rights Reserved
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Journal of NanoScience, NanoEngineering & Applications ISSN: 2231-1777(online), ISSN: 2321-5194(print) Volume 6, Issue 3 www.stmjournals.com
Growth and Description of Cu Nanostructure via a Chemical Reducing Process 1
S.C. Barman1, D.K. Saha2, H. Mamur3, M.R.A. Bhuiyan3,*
Department of Applied Physics, Electronics and Communication Engineering, Islamic University, Kushtia 7003, Bangladesh 2 Materials Science Division, Atomic Energy Centre, Dhaka, Bangladesh 3 Department of Electrical and Electronic Engineering, Cankiri Karatekin University, Cankiri 18100, Turkey
Abstract
Chemical reduction process has been employed to produce copper (Cu) nanostructure by using L-ascorbic acid. The use of L-ascorbic acid makes this process cost effective. In this process, copper chloride (CuCl2.2H2O) has been used as a precursor to produce the Cu nanostructure. They were characterized through UV-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The experimental findings revealed that the molar concentrations of L-ascorbic acid played an important influence over the particles size. The result observed was the average particle size ~50 nm. Keywords: Cu nanostructure, ascorbic acid, particle size, X-ray diffraction (XRD), scanning electron microscopy (SEM)
INTRODUCTION
Copper (Cu) is more conductive, economical and cost-effective element than gold (Au) and silver (Ag). For this reason, Cu is the best alternative material instead of Au and Ag. Nowadays, the easiest and most useful processes are employed for the growth of Cu nanostructure in the chemical reduction process. In the process, a copper salt (CuCl2.2H2O) has been decreased by a reducing agent such as L-ascorbic acid. To avoid oxidation, the process has been normally activated in a non-aqueous solution at very low concentration and under nitrogen gas atmosphere conditions. Looking at the application areas of Cu nanostructure such as magnetic, electronic, optical and catalytic properties [1–5], its technological and commercial importance has been introduced by using several areas such as storage information [6], magnetic biosensors [7], drug delivery, and hard strong materials [8]. Recently, a number of processes such as chemical reduction, laser ablation, polyol synthesis and thermal decomposition have been also developed to produce Cu nanostructure [1, 9–11]. The chemical reduction process among them is normally employed to produce nanosized materials because of its easier handling, minimum-cost and more efficiency [12].
During the process, the growth and morphology could be controlled by an optimizing molar concentration. Moreover, it could improve a crystalline dimension to control the optimization of experimental measurement tools.
Fig. 1: Growth of CU-NPs. On the other hand, the growth rate of nanosized particles depends on so many factors— one of them is the concentration of metal ions. The flexibility of enormous number of nuclei
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