Journal of Science: Advanced Materials and Devices (2016) 301e310 Contents lists available at ScienceDirect Journal of Science: Advanced Materials and Devices journal homepage: www.elsevier.com/locate/jsamd Original Article Green mediated synthesis and characterization of ZnO nanoparticles using Euphorbia Jatropa latex as reducing agent M.S Geetha a, *, H Nagabhushana b, H.N Shivananjaiah c a Vijaya Composite College, Bangalore 560 011, India Prof C.N Rao Centre for Advanced Materials, Tumkur University, Tumkur 572 103, India c Government Science College, Nrupatunga Road, Bangalore 560 001, India b a r t i c l e i n f o a b s t r a c t Article history: Received April 2016 Received in revised form 17 June 2016 Accepted 17 June 2016 Available online 23 June 2016 Presently the progress of green chemistry in the synthesis of nanoparticles with the use of plants has engrossed a great attention This study reports the synthesis of ZnO using latex of Euphorbia Jatropa as reducing agent As prepared product was characterized by powder X-ray diffractometer (PXRD), Fourier transform infra-red spectroscopy (FTIR), scanning electron microscopyeenergy dispersive spectroscopy (SEMeEDS), transmission electron microscopy (TEM), X-ray photo electron spectroscopy (XPS), Rietveld refinement, UVeVisible spectroscopy and photoluminescence (PL) The concentration of plant latex plays an important role in controlling the size of the particle and its morphology PXRD graphs showed the well crystallisation of the particles The average particle size was calculated using Scherrer equation and advanced Williamson Hall (WH) plots The average particle size was around 15 nm This result was also supported by SEM and TEM analyses FTIR shows the characteristic peak of ZnO at 435 cmÀ1 SEM and TEM micrographs show that the particles were almost hexagonal in nature EDS of SEM analysis confirmed that the elements are only Zn and O EDS confirmed purity of ZnO Atomic states were confirmed by XPS results Crystal parameters were determined using Rietveld refinement From UV eVisible spectra average energy gap was calculated which is ~3.63 eV PL studies showed UV emission peak at 392 nm and broad band visible emission centred in the range 500e600 nm The Commission International de I'Eclairage and colour correlated temperature coordinates were estimated for ZnO prepared using ml, ml and ml Jatropa latex The results indicate that the phosphor may be suitable for white light emitting diode (WLED) The study fruitfully reveals simple, fast, economical and eco friendly method of synthesis of multifunctional ZnO nanoparticles (Nps) © 2016 The Authors Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/) Keywords: Nanoparticles Green mediated synthesis Rietveld refinement SEM with EDS Photoluminescence Introduction Nowadays, there has been an increasing demand for the development of nano sized semiconductors than bulk due to their significant electrical and optical properties which are highly useful in fabricating nano scaled optoelectronic and electronic devices with multi functionality [1e3] Among various semiconducting materials, zinc oxide (ZnO) is a distinctive electronic and photonic wurtzite n-type semiconductor with a wide direct band gap of 3.37 eV and a high exciton binding energy (60 meV) at * Corresponding author E-mail address: geethashivu33@gmail.com (M.S Geetha) Peer review under responsibility of Vietnam National University, Hanoi room temperature [4,5] Study of nano semiconducting ZnO doped with various impurities has resulted in several publications leading to books [1e5], reviews [6e11] and papers [12e21] But still lots of people are working on ZnO by changing the method of preparation, to extract the novel character In this regard we have synthesised ZnO using the latex of E Jatropa as reducing agent It is also well established that the decrease in crystallite size leads to changes in optical, electrical and sensing properties of nano powders In a small nano particle, large number of atoms will be situated either at or near the free surface [6,7] The materials are interesting and useful in many applications due to their size dependent electronic, optical, chemical and magnetic properties that are comparable to or superior to their bulk [8e11] Many synthesis routes have been used to prepare metal oxides Among http://dx.doi.org/10.1016/j.jsamd.2016.06.015 2468-2179/© 2016 The Authors Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/) 302 M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 Fig Flowchart for the preparation of zinc oxide nano structure using Euphorbia Jatropa latex Fig PXRD patterns of ZnO prepared using latex of Euphorbia Jatropa as fuel (2 ml, ml and ml) these methods still simple, cost effective, nontoxic and environmentally benign is still the key issue Recently, biosynthesis or green synthesis is an alternative synthesis method to prepare nano metal oxides [12] ZnO has shown to exhibit semiconducting, pyroelectric, piezoelectric, catalysis and optoelectronic properties [13] These properties make ZnO a multifunctional material that finds applications in the field effect transistors, biosensors, light emitting diodes, diluted and ferromagnetic materials for spintronics solar cells, photo catalysis, antibacterial and antioxidants [14e16] ZnO is a well-known ntype wide band gap oxide semiconductor (3.37 eV) with high exciton binding energy (60 meV) [17] The attempts of biosynthesis of nanoparticles started as the physical and chemical processes were costly It was observed that many a times, chemical methods lead to the presence of some of the toxic chemicals absorbed on the surface of nanoparticles that may have adverse effects in medical applications [18] This problem can be overcome by synthesizing nanomaterials by green methods [19] The interaction of nanoparticles with microorganisms and bio molecules is an expanding area of research, which is still largely unexplored yet [20] The Euphorbiaceae family is one of the largest families in the plant kingdom It comprises 300 genera and about 7500 species These species are characterized by the presence of watery or milky latex [21] The different parts of the Euphorbiaceae plant are used in medicine for the treatment of painful muscular spasm, dysentery, fever, rheumatism, asthma and as an expectorant purgative etc [22e24] The latex, contains several biologically active compounds including proteins, amino acids, carbohydrates, lipids, vitamins, alkaloids resins and tannins Predominantly, milky latex contains several alkaloids of interest such as calotropin, catotoxin, calcilin etc [25] Plant extracts may act both as reducing agents and stabilizing agents in the synthesis of nanoparticles The source of the plant extract is known to influence the characteristics of the nanoparticles [26] This is because different extracts contain different concentrations and Table Crystallite size, strain, dislocation density and stress of ZnO nanoparticles prepared by various concentrations of E jatropa plant milky latex Sample ZnO (ml) Scherrer equation, D (nm) Strain, 6 11 18 5.98 3.19 2.02  10À3 Dislocation density, d ¼ 1/D2  1015 Stress, s ¼ Y  106 N mÀ2 25.4898 7.8129 3.08453 777.9 415 263 M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 303 Fig The WeH analysis (UDM, USDM, UDEDM plot) of ZnO nanoparticles using Euphorbia Jatropa as fuel Table Crystallite size, strain, stress and energy density of ZnO nanoparticles prepared by various concentrations of E jatropa plant milky latex Sample ml ml ml UDM USDM  10 D (nm) 13 21 12.44 5.81 4.63 À3 UDEDM  10 À3 D (nm) 13 21 12.4359 5.8133 4.6277 combinations of organic reducing agents [27] ZnO is potential candidate for optoelectronic applications in the short wavelength range (green, blue, UV), information storage, and sensors as it exhibits similar properties to GaN [28e30] ZnO nanoparticles are promising candidates for various applications, such as nano generators [31], gas sensors [32], biosensors [33], solar cells [34], varsities [35], photo detectors [36] and photo catalysts [37]  10À3 s (MPa) D (nm) 161.667 75.5735 60.1609 13 21 12.4358 5.8133 4.6277 s (MPa) U (kJ mÀ3) 161.6654 75.529 60.16085 10,052.34 2196.674 1392.05 Experimental The crude latex was collected from local agricultural fields, in and around Bangalore, Karnataka Latex of Euphorbiaceae Jatropa was collected in the early morning, as production of latex is highest at that time Crude latex obtained by cutting the green stem of Euphorbiaceae Jatropa plant was stored in freezer maintained at À4 C until use In a typical synthesis ml, ml and ml of crude 304 M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 D ẳ kl=b cos qị (1) where D is the particle size in nm, l is the wavelength of the radiation (1.54056 Å for CuKa radiation), k is a constant equal to 0.9, b is the peak width at half-maximum intensity and q is the peak position Micro strain is calculated using the equation ¼ b cos q=4 (2) Dislocation density is calculated using the equation d ¼ D2 (3) and stress is calculated using the equation s ¼ 3Y Fig FTIR of ZnO with latex of Euphorbia Jatropa as fuel latex was dissolved in 10 ml of double distilled water To each g of Zinc Nitrate was added and mixed well using magnetic stirrer for approximately 5e10 and then placed in a preheated muffle furnace maintained at 450 ± 10 C The reaction mixture boils froths and thermally dehydrates forming foam The entire process was completed in less than 30 Further, the final white powder was kept for calcination at a temperature of 750 C for h in the muffle furnace A typical flowchart for ZnO synthesis using combustion method is shown in Fig The PXRD profiles were recorded using Shimadzu (XRD-7000) with CuKa radiation in the range of 20e80 UVeVis spectra were recorded using Lambda-35 (PerkinElmer) spectrophotometer in the wavelength range 200e800 nm PL studies were carried out using Flurolog-3 spectro fluorimeter (JobinYvon USA) at RT The phosphor was excited at 394 nm and emission spectra were recorded in the range 450e800 nm with the help of grated PMT detector Morphology and crystallite size were examined by scanning electron microscope (SEM, Hitachi-3000) and transmission electron microscope (TEM, TECNAI F-30) respectively Results and discussion Fig shows the powder PXRD pattern of ZnO and the observed pattern was in well agreement with the standard JCPDS file (811551) No diffraction peaks corresponding to other impurities were observed Well defined peaks in PXRD shows that the particles were well crystallised The prominent peaks correspond to (hkl) values of (010), (002), (011), (012), (110), (103) The crystallite size was estimated for the powder from the full width half maximum of the diffraction peaks using DebyeeScherrer's method and Williamson Hall modified form of uniform deformation model (UDM), uniform stress deformation model (USDM), uniform deformation energy-density model (UDEDM) 3.1 Crystallite method by Scherrer method Crystallite size and lattice strain due to dislocation can be calculated from peak broadening of PXRD X-ray line broadening method was used to determine the particle size of the ZnO nanoparticles using Scherrer equation (4) The readings are tabulated in Table The crystallite size was found to be 6e18 nm The particle size found to increase with decrease in fuel concentration The decrease in crystallite size with increase in fuel/oxidant molar ratio may be due to number of moles of gaseous products liberated As more gases are liberated with increase in fuel to oxidant molar ratio, the agglomerates disintegrate and additional heat is carried away from the system thereby hindering the particle growth, which in turn produces nanoparticles of smaller size with high specific area The micro strain decreases with increase in particle size The average dislocation density was found to be 25  1015 to  1015 The small dislocation density for ZnO NPs indicates higher crystallisation of the sample Thus ml shows high level of surface defects and deteriorates crystal quality But ml and ml of ZnO show low level of surface defects 3.2 Crystallite size by WH plot Depending on different q positions the separation of size and strain broadening analysis is done using Williamson and Hall The following results are the addition of the Scherrer equation and z bs/tan q Therefore bhkl ẳ kl=D cos qị ỵ 43 tan q (5) Rearranging Equation (5) we get the equation b cos q ẳ kl=Dị ỵ 43 sin q (6) Equation (6) stands for Uniform Deformation Model (UDM) where it is assumed that strain is uniform in all crystallographic directions From the lattice parameters calculations it was observed that this strain might be due to the lattice shrinkage Fig shows WeH plot (UDM) of ZnO nanoparticles using E-jatropa latex as fuel Using the intercept and slope particle size and micro strain were calculated UDM analysis is shown in Table From the Hooke's Law maintaining linear proportionality between stress and strain, s ¼ Y3, where s is the stress and Y is the Young's modulus Equation (6) becomes b cos q ẳ kl=D ỵ 4s sin q=Y (7) USDM was a plot of b cos q versus 4sin q/Y (where Y ¼ 130  109 N mÀ2) The USDM plot is shown in Fig From the intercept and slope, the particle size and stress were calculated The values are tabulated in Table Energy density u and strain are related by u ¼ Y3 2/2 Thus equation (6) becomes M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 Fig SEM images (a) with EDS graph (b) and histogram (c) of ZnO nanoparticles 305 306 M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 Fig TEM images (a) and (b), SAED pattern (c), histogram (d) of ZnO nanoparticles b cos q ¼ kl=D þ 4ð2u=YÞ1=2 sin q (8) The graph of b cos q versus 4sin q/(Y/2)1/2 (where Y ¼ 130  109 N mÀ2) was plotted The plot obtained is shown in Fig Using the intercept and slope particle size and energy density were calculated Micro strain ¼ (2u/Y)1/2 and stress s ¼ Y were also calculated UDEDM analysis results are shown in Table The average crystallite size obtained Scherrer method is almost same as that from WH plot From Table we can conclude that as the latex concentration increases, particle size decreases, stress increases, strain increases and energy density also increases histogram for the SEM image The particle size was taken using ImageJ software From the histogram, most particles were having size of the order of 500 nm There is difference in the average particle size obtained by PXRD (18 nm) and SEM result (500 nm) This is because SEM image was taken for very small portion of the sample Probably, the part of the sample for which SEM image taken was large in size EDS micrograph showed purity of the ZnO compound No other elements other than Zn and O were found in the sample According to EDS report the weight percentage and atomicity of Zn and O were found to be 77.47, 22.53 and 54.3,45.7 respectively which is close to bulk ZnO weight percentage (80 for Zn and 20 for O) 3.3 Fourier transform infrared spectroscopy (FTIR) Fig shows the FTIR spectra of ZnO NPs taken in the range (400e4500 cmÀ1) The FTIR broad peak at 3436 cmÀ1 represented OeH group stretching of OeH, H-bonded single bridge 2106 cmÀ1 peak may be due to the absorption of atmospheric carbon di oxide by metallic cations The peak at 540 cmÀ1 corresponds to ZnO bonding which confirms the presence of ZnO particles 3.4 Scanning electron microscopy (SEM)eEDS Fig shows SEM images with EDS graph and histogram of ZnO nanoparticles From the SEM images it was observed that the particles were well shaped Most of the particles were hexagonal in shape The average crystallite size was obtained by drawing 3.5 Transmission electron microscopy The TEM images of ZnO are shown in Fig The TEM study was carried out to understand the crystalline characteristics and size of the nanoparticles The TEM images of ZnO confirm that the particles are almost hexagonal with slight variation in thickness, which supports SEM results The average particle size by histogram was found to be 50e200 nm This image reveals that most of the ZnO NPs are hexagonal in shape with average particles of the size of 100 nm The SAED pattern revealed that the diffraction rings of the synthesized ZnO exhibited DebyeeScherrer rings assigned (010), (002), (011), (012), (110), (103) respectively The particle size determined from TEM analysis is close to that of the XRD analysis M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 307 Fig (a) Wide spectra XPS of (b) Zn, (c) O and (d) C 3.6 X-ray photo electron spectroscopy Fig shows the XPS spectrum of ZnO The XPS technique is used to investigate the chemicals at the surface of a sample Photons of specific energy are used to excite the electronic states of atoms below the surface of the sample Then the intensity for a defined energy is recorded by a detector The XPS spectrum confirmed Zn and O elements in the sample A trace of carbon was resulted due to the hydrocarbon from XPS itself Fig 7(a) shows wide range of spectrum of XPS Fig 7(b)e(d) shows the high resolution XPS spectra of the elements of Zn, O and C respectively In Fig 7(b) the peaks located at 288 eV and 870 eV were associated to Zn 2P3/2 and Zn 2P1/2 respectively Fig 7(c) shows high intensity peak at 533 eV which corresponds to O 1S [42] 3.7 Rietveld refinement The lattice parameters of ZnO NPs at ml, ml and ml latex of Euphorbia Jatropa were calculated using Rietveld refinement analysis which is shown in Fig The analysis was performed with the FULLPROF software PseudoeVoigt function was used in order to fit the several parameters to the data point Two factors (scale, overall B-factor), six cell parameters (a, b, c, a, b and g), four FWHM parameters (U, V, W and IG), two shape parameters (Etr-0, and X), six background polynomials (a0ea5), four Instrumental parameters (Zero, displacement, transparency and wavelength) were used for refinement The Rietveld refinement confirmed that the crystal system of ZnO is hexagonal with Laue class 6/m, point group and Bravis lattice P The refined parameters such as occupancy, atomic functional positions for ZnO NPs at ml, ml and ml latex of Euphorbia Jatropa are summarized in Table A good agreement was obtained between the experimental relative intensity (observed XRD intensities) and simulated intensity (calculated XRD intensities) In last two figures of Fig 8, two extra peaks before and after the intense peaks were observed This may be due to incomplete reaction during combustion The refined lattice parameters (a and c) and cell volume confirm that ZnO NPs have a hexagonal crystal structure The lattice parameters a and c were found to be 3.2 Å and 5.2 Å respectively Direct cell volume was found to be 48 (Å)3 Rp, Rwp, Rexp were found to be ~5.6, ~7.1 and ~5.8 respectively The GOF (goodness of fit) was found to be ~1.3 which decreases with increase in latex of Jatropa concentration which confirms good fitting between experimental and theoretical plots 3.8 Packing diagram The packing diagram was drawn using VESTA software as shown in Fig System of particles was taken to be hexagonal with space group P 63 Lattice parameters a ¼ b and c were chosen to be Å and Å respectively The lattice positions of Zn were (0,0,0) and (1/ 3,2/3,1/2) Lattice positions of O were (0,0,u) and (1/3,2/3,1/2 ỵ u) where u ~ 0.378 From the packing diagram, the bond length between the neighbouring Zinc atoms was found to be Å and that between Zinc and Oxygen was found to be 1.84136 Å 308 M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 Fig Rietveld refinement of ZnO NPs with Euphorbia Jatropa latex ml (a), ml (b) and ml (c) as fuel 3.9 UVevisible spectroscopy Fig 10 shows the room temperature UVeVisible spectra of the ZnO nanoparticles prepared with various concentrations of the Euphorbia Jatropa latex The maximum absorbance was observed at 365 nm, 360 nm and 310 nm for Jatropa ml, ml and ml respectively The corresponding band gap was calculated using the formula Eg ¼ 1240/l The corresponding band gap energy was 3.4 eV, 3.45 eV and 4.00 eV So as the particle size decreases energy gap increases due to Quantum size effects on electronic energy bands of semiconductors It becomes more prominent when the size of the nano crystallites is less than the bulk excitation Bohr radius Columbic interactions between holes and electrons play a crucial role in nano sized solids The quantum confinement of charge carriers modifies valence and conduction bands of semiconductors corresponding to the near band gap excitonic emission [40], the other broad band is located at around 520 nm attributed to the presence of singly ionized oxygen vacancies [41] and the third band is around 651 nm which may be a second order feature of UV emission [43] The emission is caused by the recombination of a photo generated hole with an electron occupying the oxygen vacancy Further, the spectrum also reveals the nano metre distribution of nanoparticles in the powder as the luminescence peak fullwidth half-maximum (FWHM) is only in few nm Commission International de I'Eclairage (CIE) 1931 xey chromaticity diagram of ZnO nano phosphors is presented in Fig 12 excited under 350 nm As shown in the figure the CIE coordinates were located in the white region To identify technical applicability of this white emission, CCT (Correlated Color Temperature) was estimated from CIE coordinates Fig 12 shows the CCT diagram of ZnO nano phosphors excited under 350 nm In the present study, the average CCT value of ZnO nano phosphor was found to be ~6687 K 3.10 Photoluminescence Because of “Quantum size effect”, the physical properties of semiconducting materials undergo changes when their dimensions get down to nano metre scale For example, quantum confinement increases the band gap energy of ZnO, which has been observed from photoluminescence The photoluminescence originates from the recombination of surface states The strong PL implies that the surface states remain very shallow, as it is reported that quantum yields of band edge will decrease exponentially with increasing depth of surface state energy levels [38,39] Fig 11 shows the photoluminescence spectrum of ZnO nanopowder with excitation wavelength 394 nm at room temperature The spectrum exhibits two emission peaks, one is located at around 434 nm (UV region) Conclusions For the first time pure, multifunctional Zinc oxide nanoparticles were synthesized by a sustainable, inexpensive, bio-inspired, eco friendly combustion route using Euphorbia Jatropa latex as reducing agent Structure and morphology of the samples were investigated using PXRD, UVeVis, SEM and TEM measurements PXRD measurements showed that the particle size is between nm and 21 nm which is supported by SEM and TEM analyses Rietveld refinement showed the hexagonal crystal system with point group UVevisible spectrum showed that as the particle size decreases energy gap increases PL showed prominent peaks at 392 nm, M.S Geetha et al / Journal of Science: Advanced Materials and Devices (2016) 301e310 309 Table Crystal parameters by Rietveld refinement of ZnO prepared using ml, ml and ml E jatropa plant latex Jatropa ml Jatropa ml Jatropa ml Crystal system Laue class Point group Bravis lattice Lattice symbol Hexagonal 6/m P hP Hexagonal 6/m P hP Hexagonal 6/m P hP Cell parameters a¼b c a¼b g a/c 3.263067 5.224156 90 120 0.6246 3.261789 5.223933 90 120 0.62439 3.261789 5.232172 90 120 0.6234101 Direct cell volume (Å)3 48.1724 48.1327 48.2086 Atomic coordinates Zn x y z B Occupancy 0.3333 0.6666 0.03495 8.05209 0.81625 0.3333 0.6666 0.03495 4.84811 0.88619 0.3333 0.6666 0.03891 1.14091 1.63398 0.3333 0.6666 0.41154 28.57724 2.50358 0.3333 0.6666 0.41456 26.46827 2.4314 0.3333 0.6666 0.42321 9.60219 2.48647 5.4 6.64 5.3 1.57 1.3 7.891 5.78 7.4 5.87 1.59 1.3 7.54 5.66 7.13 6.14 1.35 1.2 6.181 O x y z B Occupancy Rp Rwp Rexp c2 GOF index Density of compound (g/cc) Fig 10 UVevisible spectrum of ZnO NPs using Euphorbia Jatropa as fuel conventional semiconductor These semiconductors allowing more powerful electrical mechanism to built which are cheaper and more energy efficient Thus this can be used in high power application with high breakdown voltage, white LED, transducers and high electron mobility transistor (HEMT) 520 nm and 651 nm The energy gap of synthesised ZnO was around eV Thus ZnO can be used as wide band gap semiconductor These wide band gap 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... equation s ¼ 3Y Fig FTIR of ZnO with latex of Euphorbia Jatropa as fuel latex was dissolved in 10 ml of double distilled water To each g of Zinc Nitrate was added and mixed well using magnetic stirrer... The crude latex was collected from local agricultural fields, in and around Bangalore, Karnataka Latex of Euphorbiaceae Jatropa was collected in the early morning, as production of latex is highest... parameters of ZnO NPs at ml, ml and ml latex of Euphorbia Jatropa were calculated using Rietveld refinement analysis which is shown in Fig The analysis was performed with the FULLPROF software PseudoeVoigt