International Journal of Physics JOURNAL Issue 1, January- June(IJP) INTERNATIONAL (IJP), Volume 1, OF PHYSICS 2012 ISSN 0976 66xx

x (Print) ISSN 0976 64xx(Online) Volume 1, Issue 1, January- June (2012), pp. 32-40 IAEME: www.iaeme.com/ijitmis.html Journal Impact Factor (2011): 1.910 (Calculated by GISI) www.jifactor.com

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SYNTHESIS OF NANO YTRRIUM OXIDE PHOSPHORS BY SIMPLE METHODS AND THEIR MORPHOLOGICAL STUDIES
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G. Bhavani1, S. Ganesan2 Department of Physics, Jansons Institute of Technology, Coimbatore, TN, India-641659 21 Department of Physics, Government College of Technology, Coimbatore, TN, India- 641 013
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Email: bhavaneeg@gmail,com

ABSTRACT Among the family of rare earth compounds, yttrium oxide is a widely used material. Due to its chemical and physical properties, it is well known that yttrium oxide is a common luminescent host material. In many of the applications, reduction of the yttrium oxide crystallite size into the nanometer regime would result in improved performance compared to coarse grained yttrium oxide. This is particularly evident in phosphor application, where the phosphor efficiency varies inversely as the square of the particle size due to quantum confinement effect In this paper, synthesis and characterization of yttrium oxide by various methods are analyzed. Many research works is done on synthesis of Yttrium oxide and their characterization. Yttrium oxide samples are prepared by methods like Wet chemical, solvothermal process, and Sol-gel method. Then the samples are analyzed by XRD, SEM, EDAX and UV-Vis absorption studies. By optimizing various synthesis conditions, nanophosphors with high quantum efficiency and wide structural tenability can be prepared for their use in future display applications. Keywords: Phosphor, precipitation, calcinations

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1. INTRODUCTION Yttrium oxide finds many high technology applications due to its excellent high temperature stability, high affinity for oxygen, sulfur and well defined crystal structures whose properties can be tailored by incorporating different types of ions into the structure [1,2]. Inorganic nanomaterials are attracting a great deal of attention due to their many potential applications in the fabrication of electronic devices, sensors, biochips and energy storage media [3-14]. In many of the applications, reduction of the yttrium oxide crystallite size into the nanometer regime would result in improved performance compared to coarse grained yttrium oxide. This is particularly evident in phosphor application, where the phosphor efficiency varies inversely as the square of the particle size due to quantum confinement effect [15]. Phosphor films play an important role in high resolution display devices such as cathode ray tubes (CRTs) used in medical imaging, graphics, helmet mounted display, thin film electroluminescence panels, gas sensors and thermomechanic devices. In addition to high resolution, displays with thin film phosphors have higher contrast, ruggedness, exhibit a high degree of uniformity and better adhesion. [16]. Among the family of rare earth compounds, yttrium oxide is a widely used material due to its chemical and physical properties; it is well known that yttrium oxide is a common luminescent host material [10]. In this paper, synthesis and characterization of yttrium oxide by various methods are analysed. By optimizing various synthesis conditions, nanophosphors with high quantum efficiency and wide structural tenability can be prepared for their use in future display applications. 2. EXPERIMENTAL 2.1 Sol- gel method In this method, the nanocrystalline yttrium oxide powders wereprepared by taking the precursor,Yttrium nitrate hexahydrate (Y(NO3)3.6H2O). 1gram of Yttrium nitratehexadydrate was dissolved in 10 ml of distilled water. The solution was stirred with magnetic stirrer for the salt to dissolve completely, till clear solution was obtained. 30 ml of ammonium hydroxide diluted with 20 ml of water was added till precipitation is complete. The precipitate was left for 15

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International Journal of Physics (IJP), Volume 1, Issue 1, January- June 2012

hours to settle. Then the precipitate was washed with distilled water and dried in an oven at 373K for 3 hours. After drying, the powder was obtained as agglomeration, which was ground. The yttrium hydroxide powder thus obtained were converted into yttrium oxide through calcination by heating the sample at 623K for 15 hours and cooled to room temperature [17]. 2.2 Solvothermal Method In this method, Yttrium oxide was prepared by dissolving 0.01M Y(NO3)3.6H2O in 40ml of absolute ethanol under stirringby Magnetic stirrer. Once the yttrium nitrate dissolved completely, 0.04M of sodium hydroxide was dropped into it followed by 30 minutes vigorousstirring. After that the sample was heated at 433K for 3 hours and cooled to room temperature. The white powder formed at the bottom was washed ethanol and distilled water several times to remove any possible remnants. Finally the product was dried at 353K for 2 hours [18]. 2.3 Wet chemical Method The preparation involves a precipitation reaction between the yttrium nitrate (Y(NO3)3.6H2O) and oxalic acid as precipitant agent. Yttrium nitrate solution (0.3M) was added with diluted oxalic acid (0.45M) The precipitated white powder was filtered and dried at 423K for 3 hours[19]. 3. CHARACTERISATION The samples were characterized by XRD on a Bruker AXS D8 Advance X-ray diffractometer equipped with Si(Li) PSD detector monochromatised Cu, Wavelength 1.5406 A. The morphological investigation of the samples of Y2O3 nanoparticles was performed in JEOL Model JSM - 6390LV Scanning Electron Microscope. The absorption spectrum of the samples was recorded using a Varian, Cary 5000 spectrophotometer. Elemental analysis of the samples is done by EDAX EOL Model JED 2300 make to determine the presence and percentage of yttrium and oxygen ions.

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4. RESULTS AND DISCUSSION 4.1 XRD

Figure 1. Powder X ray diffraction pattern of nanocrystalline cubic Yttrium Oxide prepared by (a)Sol-Gel method, (b) Solvothermal method and (c) Wet chemical method Figure 1(a), (b) and (c) shows the XRD patterns of the samples of nanocrystalline yttrium oxide prepared using Ammonium hydroxide, sodium hydroxide and oxalic acid as a precipitating agent. The increased width of the diffraction peak shows that the samples are nano crystalline. In addition to the yttrium oxide peaks a few number of yttrium hydroxide peaks are in as prepared nano crystalline sample B which is shown in the XRD pattern. The average crystallite size is estimated for all the samples from Scherrers equation [20]. The estimated crystallite sizes of the samples are found as given in the table along with their structure.

Sample Precipitating agent A

Ammonium BCC Hydroxide B Sodium Hydroxide 1.526 Monoclinic, primitive C Oxalic acid 4.621 Hexagonal, primitive Table. 1. The estimated particle sizes of the sample from XRD pattern.

Particle size in nm 1.223

Structure from JCPDS

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4.2 EDAX
From the EDAX spectrum of figure 2 (a), (b), and (c) the presence of the characteristic and distinct line of yttrium (L) and Oxygen (K) has been identified. Theoretical atomic weight to percentage of yttrium o t oxide is 60% oxygen and 40% yttrium[21]. In the sample A, prepared by sol gel technique, the percentage of oxygen sol-gel is found to be 24% and that of yttrium is 76%. Similarly the sample B prepared by solvothermal method, percentage of oxygen is 56% and that of yttrium is 44%. In the sample C, prepared by wet chemical method, the oxygen content is found to be 40% and yttrium is 60%. Hence the yttrium oxide sample produced by solvothermalmethod has oxygen and yttrium percentage near to the theoretically predicted atomic weight percentage.

(a)

(b)

(d) (c)

Fig. 2 EDAX spectrum of elemental analysis of the Yttrium Oxide prepared by (a) Sol-Gel method, (b) Solvothermal method , (c) Wet chemical method and (d) Gel comparison of their atomic weight percentage.

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International Journal of Physics (IJP), Volume 1, Issue 1, January- June 2012

4.3 UV- Vis ABSORPTION SPECTRUM The UV-Vis absorption spectrum of yttrium oxide nanopowders prepared by using different precipitating agents are shown in figures 3 and 4 (a), (b), and (c). The samples prepared show peaks around 200 nm which is due to the absorption of yttrium oxide[22].

Fig.3 Absorption spectrum of the Yttrium Oxide prepared by (a)Sol-Gel method, (b) Solvothermal method and (c) Wet chemical method

Fig.4 Reflectivity of the Yttrium Oxide prepared by (a)Sol-Gel method, (b) Solvothermal method and (c) Wet chemical method

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4.4 SEM The precipitating reagents could also influence the precursor and phosphor morphology and particle size as illustrated by the SEM images. All the SEM images of the samples of yttrium oxide prepared using ammonium hydroxide, sodium hydroxide, and oxalic acid as the precipitating agent. All the SEMimages of the samples A and B show the cumulative nature of secondary particles which are made up of agglomeration of many primary particles. Depending upon the precipitating agent used in the synthesis, the morphology of the sample varies. This may be due to the difference in ionic strength of the solution [23]. The obtained particles donot have a uniform shape and size as obtained from SEM micrographs. Figure 7 show the SEM images of the as prepared yttrium oxide sample by wet chemical method. A typical SEM image shows that the yttrium oxide is composed of 3D flower like microstructures with diameter in the range of 500600 nm. Regarding the formation of 3D flower like yttrium oxide nanopowders, the discussion is proposed as follows. It is well known that the shape control of the nanocrystals can be achieved by manipulating the growth kinetics [24-26]. In the present case, the high concentration of yttrium ions led to the burst of the initial homogeneous nucleation and then the super saturated yttrium oxide nuclei tended to aggregate together to decrease the surface energy. As the reaction proceeded the concentration of the yttrium oxide monomer became lower and some active sites on the surface of the initially formed yttrium oxide aggregations would grow along the oriented direction. The preferential growth along the oriented directions resulted in yttrium oxide nanoflakes on the surface of the initially formed yttrium oxide aggregation[27]. As a result, 3 D flower like yttrium oxide nanoflakes was prepared in the present reaction system.

Fig. 5.(a), (b), (c) SEM images of yttrium oxide prepared by sol-gel technique

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International Journal of Physics (IJP), Volume 1, Issue 1, January- June 2012

Fig. 6(a), (b), (c) SEM images of Yttrium oxide prepared by Solvothermal technique

Fig. 7(a), (b), (c) SEM images of Yttrium oxide prepared by Wet chemical method.
5. CONCLUSION

In conclusion, we have synthesized the Y2O3 nanoparticles using simple sol-gel, solvothermal and wet chemical technique. Using XRD, SEM, UV-Vis and EDAX characterization techniques, we have extensively analyzed the morphology and absorption of Y2O3 nanoparticles. Wet chemical method resulted in the formation of nanoflakes, Solvothermal had somewhat uniform distribution in size but needs annealing to avoid the presence of Yttrium Hydroxide and sol- gel method needs more annealing process to overcome agglomeration of particles.
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