Ph.

D PROGRESS REPORT - 02 On SYNTHESIS AND CHARACTERIZATION OF RARE EARTH DOPED

NANO CRYSTALLINE OXIDES AND THEIR LUMINESCENCE PROPERTIES

Submitted To

Visvesvaraya Technological University, Jnana Sangama, Belgaum -590 018, Karnataka, India.

By D PRAKASH (USN 1PI12PGN01)

Under the guidance of Dr. K R Nagabhushana Department of Physics P.E.S. Institute of Technology, Bangalore

PHYSICS RESEARCH CENTRE DEPARTMENT OF PHYSICS

PES INSTITUTE OF TECHNOLOGY

BANGALORE 560 085 Ph.D. PROGRESS REPORT - 02 Name of the Candidate Course : : D. PRAKASH Ph.D

Year of Registration

Nov 2012

Research Topic

Synthesis and characterization of rare earth doped nanocrystalline oxides and their luminescence properties 1PI12PGN01

U.S.N Research work carried out

: :

Following work has been carried out from July 2013 to Dec 2013 Analysis of X-Ray diffraction , Fourier transform Infra red spectroscopy and Photoluminescence spectra

Details of the Research work

Annexure -I

Candidate (D Prakash)

Guide (Dr. K R Nagabhushana)

Principal (Dr.K.N.B.Murthy)

ANNEXURE-I

Details of Research Work

Calculation of crystalline size from X-ray diffraction: The phase analysis and crystal structure of CaO was studied by X-ray diffraction (XRD) technique. The XRD patterns of calcium oxide (CaO) heat treated at 900C was shown in figure 1. Crystallite size of material often helps to correlate many physical properties of a system undergoing transformation [1]. X-ray line broadening analysis provides a method of finding bulk average size of coherently diffracting domains and strain. The average crystallite size (D) from X-ray line broadening has been calculated using the Debye-Scherrer equation [2,3]. D= Where is the wavelength of the X-ray beam, D is average crystallite size in angstroms, is the full width at the half- maximum intensity, and is the Bragg angle.

250

900 C

200

(101) (001)

intensity (a.u.)

150

100

(100)

(110) (102)

50

0 10 20 30 40 50 60 70

2 (degree)

figure 1. XRD patterns for 9000C heat treated CaO. The XRD patterns of the CaO shows diffraction peaks at 18.1, 28.80, 34.20, 47.20 and 50.10 and these diffraction peaks are assigned to (0 0 1), (1 0 0 ), (1 0 1 ), (1 0 2 ), (1 1 0 ), respectively. These reflections are attributed to a Calcium hydroxide phase. The sample matched well with the standard data base of Expertise core (00-001-0095).

Unit cell parameters were obtained by the XRD data. XRD data revealed that the product was hexagonal calcium hydroxide with P-3M1 space group having nanosized particles [4]. The characteristics peaks were higher in intensity and narrower spectral width indicates that the products were of good crystallinity. The average crystallite size calculated using Scherer relation is found to be 15 nm. Fourier Transform Infrared spectroscopy (FTIR): To verify chemical purity, CaO powders were analyzed by FTIR the bands due to ionic, hydroxyl and carbonate are distinctly displayed in the spectrum [5]. Figure 2 shows 600C heat treated CaO of IR spectra, The spectra displays band at 3643 cm-1 corresponds to the O-H bonds from the remaining hydroxide band at 1460 cm-1 and 875 cm-1 corresponds to the C-O bond and Figure 3 Shows 900C heat treated of IR spectra, The spectra displays band at 3643 cm-1 corresponds to the O-H bonds from the remaining hydroxide band at 1415 cm-1 and 873 cm-1 corresponds to the C-O bond [1, 6]. It is also evidenced from the characteristics absorption of C=O between 2000 cm-1 and 1500 cm-1.

600 C
20

25

900 C

20

15

Transmitance (%)

Transmitence (%)

15

10

10

5
0 4000 3500 3000 2500 2000
-1

1500

1000

500

wave number (cm )

4000 3500 3000 2500 2000
-1

1500

1000

500

wave number (cm )

Fig 2. FTIR spectra of CaO nanoparticles

Fig 3. FTIR spectra of CaO nanoparticles

Photoluminescence (PL): Figure 4 shows PL spectra of combustion synthesized heat treated CaO. A broad PL emission with peak at 393 nm in 500oC heat treated samples and 900oC heat treated CaO shows a broad PL emissions spectra with peak at 424nm when excited of with 288 nm. The PL intensity decreases with increasing calcination temperature [7].

8000 7000 6000

393 nm Emission Spectra ex = 288 nm (a) 500 C o (b) 900 C

o

424 nm

Intensity (a.u)

5000 4000 3000 2000 1000 0 300

(a) (b)

400

500

600

700

800

Wavelength (nm)

(Figure-4): Photoluminesence (PL) spectra of caO Conclusions: The XRD pattern of nanocrystalline structure of CaO shows calcium hydraoxide phase, the average crystallite size found to be 15 nm. Lattice parameters are found to be a=3.5899 A o, b=3.5899 Ao and c=4.9160 Ao. FTIR analysis revealed the formation CaO structure. Photoluminescence intensity decreases with increasing calcination temperature. REFERENCES(1).Arup Roy and et al , volume 10 ,No.3(2011)413-418. (2).Songkla-na Karin. J. sci : technol. 32(6),627-634 ,2010. (3).Reac KinetMech cat (2010) 99 :235-241.. (4)Expertise core File 00-001-0095 Grant in Aid(1992, Winchell.A , Winchell H, Microscopic character of Artificial Inorg. Solid sub,69(1964) (5).R.A.Naquist and R.O. Rangeli , Handbook of infrared and Raman Spectra of inorganic compound and organic salts.,vol.4 (infrared spectra of inorganic compounds 3800-4500cm-1)(Acadmic,San Diego, , 1997),pp.207. (6).Bull . Chem . soc . Ethiop . 2011 , 25(1) ,37-42 (7)M.D.Jones.etal,App phys 15561,british journal, Jan 1964.

Candidate

Guide

(D Prakash)

(Dr. K R Nagabhushana)