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ORIGINAL ARTICLE

ISSN No :2231-5063

International Multidisciplinary Research Journal

Golden Research Thoughts

Chief EditorDr.Tukaram Narayan Shinde

PublisherMrs.Laxmi Ashok Yakkaldevi

Associate EditorDr.Rajani Dalvi

HonoraryMr.Ashok Yakkaldevi

Vol III Issue X April 2014

Editorial Board

International Advisory Board

Welcome to GRTISSN No.2231-5063

Golden Research Thoughts Journal is a multidisciplinary research journal, published monthly in English, Hindi & Marathi Language. All research papers submitted to the journal will be double - blind peer reviewed referred by members of the editorial board.Readers will include investigator in universities, research institutes government and industry with research interest in the general subjects.

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George - Calin SERITANFaculty of Philosophy and Socio-Political Sciences Al. I. Cuza University, Iasi

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Titus PopPhD, Partium Christian University, Oradea,Romania

Golden Research ThoughtsISSN 2231-5063Volume-3 | Issue-10 | April-2014Available online at www.aygrt.isrj.net

SYNTHESIS AND CHARACTERIZATION OF COPPER CARBONATE NANOPARTICLES

Abstract:-Copper carbonate nanoparticles were synthesized via chemical co-precipitation method from copper sulphate and sodium carbonate. The formed nanoparticle is characterized by powder x-ray diffraction, scanning electron microscopy, ultra-violet spectroscopy and fourier transform infrared spectroscopy, confirmed the preferential growth of copper carbonate nanoparticles that width is 90.55nm. The SEM image shows the synthesized copper carbonate show well crystallized particles with spherical morphology. The FTIR spectrum is used to study the stretching and bending frequencies of molecular functional groups in the sample. From UV spectrum, the band gap of copper carbonate nanoparticles is found to be 3.4eV.

Keywords:XRD, SEM, FTIR, UV.

1.INTRODUCTION

A burst of research activity is witnessed in recent years in the area of synthesis and fabrication of different size and shape of metal nanoparticles. Nanometer sized particles display many interesting optical, electronic, magnetic and chemical properties yielding applications in biological nano sensors, optoelectronics, nano devices, nano electronics, information storage and catalysis [1, 2]. Amongst many metals like Au, Ag, Pd, Pt, towards which research is directed, copper and copper based compounds are the most important materials. The metallic Cu plays a significant role in modern electronics circuits due to its excellent electrical conductivity and low cost nanoparticles [1, 3]. So Cu will gain increasing importance as is expected to be an essential component in the future nano devices due to its excellent conductivity as well as good biocompatibility and its surface enhanced Raman scattering (SERS) activity [1, 4]. Metallic copper nano crystals homogeneously dispersed in silica layers have attracted great attention recently for the development of nonlinear optical devices [1, 5]. In this work, copper carbonate nanoparticles was prepared and their structural and optical properties were studied.

Basic copper carbonate is used as a pigment in paint and varnish; as a fungicide for seed treatment; as an insecticide; in pyrotechnics such as fireworks, and in pottery glazes; and in the manufacture of other copper salts. The compound is also added in small quantities to animal and poultry feed to supply nutritional copper requirements.

2. EXPERIMENTAL DETAILS

Nanoparticles of copper carbonate were prepared by chemical co-precipitation method by adding copper sulphate and sodium carbonate. Precise amounts of reagents taking into account their purity were weighed and dissolved separately in distilled water into 0.1M concentration.After obtaining a homogeneous solution, the reagents were mixed using magnetic stirring. The precipitate was separated from the reaction mixture and washed several times with distilled water and ethanol. The wet precipitate was dried and thoroughly ground using agate mortar to obtain the samples in the form of fine powder.

3. TESTS CONDUCTED

X-ray diffraction is an ideal technique for the determination of crystallite size of the powder samples. The basic principle for such a determination involves precise quantification of the broadening of the peaks. XRD line broadening method of particle size estimation was chosen in this investigation for determining the crystallite size of the powder sample. XRD

R.Hepzi Pramila Devamani and M. Sabeena SYNTHESIS AND CHARACTERIZATION OF COPPER CARBONATE NANOPARTICLES , “”, Golden Research Thoughts | Volume 3 | Issue 10 | April 2014 | Online & Print

R.Hepzi Pramila Devamani and M. Sabeena

Assistant Professor, Department of PG Physics, V.V.Vanniaperumal College for Women . M.Sc Student, Department of PG Physics, V.V.Vanniaperumal College for Women Virudhunagar.

1

GRT

https://www.facebook.com/ashok.yakkaldevi.3

http://en.wikipedia.org/wiki/Orthogonal

.

study of the powder samples was carried out at Alagappa University, Karaikudi. The morphology of the powder samples was studied by the scanning electron microscope (SEM) analysis taken at STIC Cochin. The infra red spectroscopic (IR) studies of copper carbonate nanoparticles were made by using 'SHIMADZU' FTIR 8400S model spectrometer through KBr method. The UV spectrum was taken in the absorbance mode in the wavelength range from 200 to 800 nm.

4. RESULTS AND DISCUSSION

4.1. XRD studies

4.1.1 XRD – Particle Size Calculation

The XRD patterns of the prepared samples of copper carbonate are shown in figure.1. XRD studies reveal that the samples are nano sized and crystalline. The fine particle nature of the samples is reflected in the X-ray line broadening. The size of the synthesized copper carbonate nanoparticles are calculated using Scherrer equation .

where ë represents wavelength of X rays, ß represents half width at full maximum and ? is the diffraction angle. The average grain size of the particles is found to be 90.55 nm.

Figure.1 XRD pattern of copper carbonate nanoparticles

A good agreement between the experimental diffraction angle [2è] and standard diffraction angle [2è] of specimen is confirming standard of the specimen. The peaks at 2è values of copper carbonate is observed and tabulated in table-1 and compared with the standard powder diffraction card of Joint Committee on Powder Diffraction Standards (JCPDS), copper carbonate file No70-2053. The d-spacing values of experimental is also confirming to the standard values.

Synthesis And Characterization Of Copper Carbonate Nanoparticles

2Golden Research Thoughts | Volume 3 | Issue 10 | April 2014

D = 0.9 ë / â cosè (1)

Position [°2Theta] (Copper (Cu))

20 30 40 50 60 70

Counts

0

200

400

600

800 Copper Carbonate

.

Table.1. Experimental and standard diffraction angles of copper carbonate specimen.

4.2. XRD - Expected 2è Positions

The value of d (the interplanar spacing between the atoms) is calculated using

Bragg’s Law: 2d sin ? = n ?

Wavelength ë = 1.5418 Å for Cu Ka

The expected 2? positions of all the peaks in the diffraction pattern and the interplanar spacing d for each peak is calculated using following formula and the details are shown in table-2.

Bragg's Law is used to determine the 2è value: The expected 2è and d values are close with the experimental 2è and d values.

Table 2. The Lattice plane and the lattice spacing from d from XRD of copper carbonate nanoparticles.


Experimental Standard – JCPDS 70-2053

Diffraction angle

(2è in degrees)

D spacing (Å) Diffraction angle

(2è in degrees)

D spacing (Å)

24.12 3.68711 24.766 3.5905

25.701 3.46346 25.831 3.4463

33.30 2.6886 33.828 2.6476

35.670 2.51507 35.671 2.5149

38.67 2.32631 38.245 2.3514

52.64 1.7372 52.414 1.7442

54.77 1.67473 54.744 1.6754

60.04 1.53976 60.886 1.5202

61.52 1.50619 61.711 1.5019

Hkl 2è(deg) D((Å)

Experiment Expected Experiment Expected

110 24.12 24.56 3.68 3.59

001 25.70 25.62 3.46 3.44

-111 33.30 33.31 2.68 2.64

-201 35.67 35.07 2.52 2.51

111 38.67 37.52 2.32 2.35

-311 52.64 50.57 1.73 1.74

-221 54.77 52.65 1.674 1.675

221 60.04 58.02 1.53 1.52

311 61.52 58.74 1.506 1.502


.

4.1.3. XRD – Dislocation Density

The dislocation density is defined as the length of dislocation lines per unit volume of the crystal. In materials science, a dislocation is a crystallographic defect, or irregularity, within a crystal structure. The presence of dislocations strongly influences many of the properties of materials. The movement of a dislocation is impeded by other dislocations present in the sample. Thus, a larger dislocation density implies a larger hardness. The X-ray line profile analysis has been used to determine the dislocation density. The dislocation density (ä) in the sample has been determined using expression.

Where ä is dislocation density, ß is broadening of diffraction line measured at half of its maximum intensity (in radian), ? is Bragg’s diffraction angle (in degree), a is lattice constant (in nm) and D is particle size (in nm). The dislocation density can also be calculated from

Where ä is dislocation density and D is the crystallite size. Results of the dislocation density calculated from both the formulas are given in table-3. The number of unit cell is calculated from

Where D is the crystallite size and V is the cell volume of the sample [6].

Table-3. Dislocation Density and Number of Unit Cell from XRD.

It is observed from these tabulated details, and from figures.2, 3 & 4, dislocation density is indirectly proportional to particle size and number of unit cell. Dislocation density increases while both particle size and number of unit cell decreases.


(2)

(3)

(4)

2è (deg) Particle Size

D (nm)

Dislocation Density (m2) Number of

Unit Cell ä = 15âcosè /4aD ä = 1 / D2

24.12 15.045 3.769x1015 4.418x1015 0.1888x105

25.701 90.548 1.041x1014 1.219x1014 4.1173x105

33.30 23.035 1.607x1015 1.884x1015 0.6778x105

35.670 27.843 1.100 x1015 1.289 x1015 1.1970x105

38.67 10.529 7.695 x1015 9.019x1014 0.0647 x105

52.64 44.339 4.339 x1014 5.086x1014 4.8349 x105

54.77 29.828 9.588 x1014 1.123 X1014 1.4721 x105

60.04 22.943 1.6208x1015 1.899 x1014 0.6698 x105

61.52 11.558 6.3866 x1015 7.4858 x1014 0.0856 x105


.

Figure.2 Dislocation density Vs Particle size for copper carbonate nanoparticles

Figure.3 Number of Unit cells Vs Dislocation density for copper carbonate nanoparticles

Figure.4 Number of unit cells Vs particle size for copper carbonate nanoparticles.


Particle Size Vs Dislocation density

0.00E+00

1.00E+15

2.00E+15

3.00E+15

4.00E+15

5.00E+15

6.00E+15

7.00E+15

8.00E+15

0 20 40 60 80 100

Particle Size(nm)

Dis

locati

on

Den

sit

y(m

2)

Number of Unitcells Vs Dislocation Density

0.00E+00

1.00E+15

2.00E+15

3.00E+15

4.00E+15

5.00E+15

6.00E+15

7.00E+15

8.00E+15

0.00E+00 1.00E+06 2.00E+06 3.00E+06 4.00E+06 5.00E+06

Number of Unitcells

Dis

locati

on

Den

sit

y(m

2)

Num be r of Unitce lsl Vs Pa rticle S ize

0

10

20

30

40

50

60

70

80

90

100

0 0 .1 0 .2 0 .3 0 .4 0 .5

Nu m b e r o f Un it ce l ls

Par

ticl

eS

ize(

nm

)


.

4.1.4. XRD – Morphology Index

A XRD morphology index (MI) is calculated from FWHM of XRD data using the relation

Where M.I. is morphology index, FWHMh is highest FWHM value obtained from peaks and FWHMp is value of particular peak’s FWHM for which M.I. is to be calculated. The relation between morphology index and particle size is shown in table-4.

Table 4. Relation between Morphology Index and Particle size for copper carbonate nanoparticles

Figure.5 Morphology Index of copper carbonate nanoparticles.

It is observed that MI has direct relationship with particle size and the results are shown in Figure.5.


(5)

FWHM (â) radians Particle Size(D) nm Morphology Index

(unitless)

0.00942 15.045 0.12477

0.00157 90.548 0.46103

0.00628 23.035 0.17617

0.00523 27.843 0.20432

0.00139 10.529 0.0878

0.00348 44.339 0.2781

0.00523 29.828 0.2042

0.00697 22.943 0.16141

0.00139 11.558 0.0878

0

0.05

0.1

0.15

0.2

0.25

0.3

0.35

0.4

0.45

0.5

0 20 40 60 80 100

Particle Size(nm )

Mo

rph

olo

gy

Ind

ex


.

4.1.5. XRD – Unit Cell Parameters

Unit cell parameters values calculated from XRD are enumerated in table-5.

Table.5. XRD parameters of copper carbonate nanoparticles.

4.2. SEM studies

Scanning electron microscopy was used to analyze the morphology and size of the synthesized copper carbonate nanoparticles. Figure.6 and Figure.7 show the SEM images of the copper carbonate nanoparticles at various magnifications. The SEM images of copper carbonate nano particles show well crystallized particles with spherical morphology. In this case the particles sizes are slightly increased and is also observed that the particles are distributed with agglomeration.

Figure.6 SEM image at 1500 magnifications


Parameters Values

Structure

Space group

Symmetry of lattice

Particle size

Bond Angle

Lattice parameters

Vol.unit cell(V)

Density ( ñ )

Dislocation Density

Mass

End- centered

Cm(8)

Monoclinic

90.55 nm

â = 101.34

a = 6.092;b = 4.493;c = 3.515

94.33

4.350

1.219x1014

123.56amu


.

Figure.7 SEM image at 5000 magnifications

4.3. FTIR Studies

The FTIR spectrum of the copper carbonate sample is shown in the figure.8.The FTIR spectrum for copper carbonate -1show peaks at 3585.42, 3384.84, 3315.41, 3222.83, 3184.26 and 3164.97cm corresponding to the free O-H group [1] and the

-1peak at 1650.95cm is bending mode of hydroxyl group [1]. The peak at 817.76 cm-1 is due to carbonate ions and the peak at -1603.68 cm-1 is due to Cu-O stretching bond. The peak at 426.24 cm represents Cu-O bond in the vibrational mode. The peak at

-1511.1 cm represents the absorption peak of Cu nanoparticles and copper nanoparticles display a broad absorption from 550 to 700nm [7].

Figure.8 FTIR spectra of copper carbonate nanoparticles

4.4. UV Studies

The band gap of the prepared sample copper carbonate was determined by using UV visible studies. From the UV spectrum the optical band gap of copper carbonate is 3.4eV. Figure.9 and figure.10 show the absorbance curve for copper carbonate nanoparticles and graph to find the band gap of copper carbonate nanoparticles.



.

Figure.9 The absorbance curve for copper carbonate nanoparticles

Figure.10 Graph to find the band gap of copper carbonate nanoparticles.

CONCLUSIONS

The copper carbonate nanoparticles have been prepared by chemical co-precipitation method. XRD analysis suggests that the average particle size is in the nano range (90.55nm). The SEM picture reveals the well crystallized particles with spherical morphology. From the FTIR spectrum, the stretching and bending frequencies of the molecular functional groups in the sample are studied. From the UV spectra, the band gap was found.

5. REFERENCES

1.M.Samim, N.K.Kaushik and A.Maitra, Bull. Mater. Sci., 30(5), 535–540 (2007). 2.D.L.Feldheim and C.A Foss, “Metal Nanoparticles: Synthesis, characterization and applications (2002).


Bandgap for copper carbonate

0

5E-37

1E-36

1.5E-36

2E-36

2.5E-36

3E-36

0 1 2 3 4 5 6 7

E in eV

(Ah

u)(

Ah

u)


.

3.A.K.Schaper, H.Hou, A.Greiner, R.Schneider and F.Philips, Appl.Phys.A Mater.Sci.Process., 78, 73 (2004).4.B.Pergolese, M.Muniz Miranda and A.Bigotto, J.Phys.Chem. B110, 9241 (2006).5.C.J.Flytzanis, Physics B, At. Mol. Opt. Phys. 38, S661 (2005).6.T.Theivasanthi, M.Alagar, Nano.Biomed.Eng. 5(1), 11-19 (2013).7.A.Nasirian, Int.J.Nano.Dim. 2(3), 159-164 (2012).



R.Hepzi Pramila Devamani Assistant Professor, Department of PG Physics, V.V.Vanniaperumal College for Women .

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