Lectura 1 (Effect of Size and Morphology On UV-blocking Property of Nano ZnO) PDF

International Journal of Scientific and Research Publications, Volume 3, Issue 4, April 2013 ISSN 2250-3153
Effect of size and morphology on UV-blocking property of nanoZnO in epoxy coating

Narayani Rajagopalan* & A S Khanna*
*
Metallurgical Engineering & Materials Science, Indian Institute of Technology Bombay, India
Abstract- Nano zinc oxide (ZnO) is extensively used as a UV-blocking material and finds application as a UV-blocker in cosmetics, textiles and protective coatings. However, with varying sizes and morphologies in the nano scale length, the UV-blocking behavior of nanoZnO gets varied. In the present study a DGEBA based epoxy coating on MS substrate was formulated and modified with nanoZnO with two different sizes and morphologies. Flake-like and spherical nanoZnO were synthesized by chemical routes using different precursors and characterized for their structure, size and shape. The nanoZnO modified epoxy coatings were exposed in UVB weathering conditions and the UV-blocking efficiency of the two types of nanoZnO particles were studied by evaluating the color change (dE) and yellowness index (YI) for the UVB exposed epoxy coatings with and without nanoZnO. It was observed that the flake-like nanoZnO was more efficient in lowering yellowing resistance of the epoxy coating on weathering compared to the spherical nanoZnO particles. Index Terms- Nano ZnO, UV-blocking, yellowing, epoxy
I. INTRODUCTION In recent years, zinc oxide (ZnO) ultrafine particles are well known as UV blocking materials, which make it feasible to be widely used in polymers, fabrics and cosmetic materials [1]. Zinc oxide has a band-gap at around 3.37 eV corresponding to 376 nm and thus it absorbs light that matches or exceeds this band gap energy [1-2]. UV-range of solar spectrum lies within this range and thus UV light gets absorbed by zinc oxide particles. The UV-blocking property of zinc oxide is only enhanced when it comes to nano-sized ultra-fine ZnO particles. As they are inorganic and particulate, they have added advantages of being stable and non-migratory within a matrix and thus potentially impart better effectiveness and a longer service life. With the on-going development in nano-technology, different nano-structures can be synthesized via different synthesis routes. An equally known fact is that the unique and fundamental properties of nano particles change with their size and shape [3-5]. The phase stability of nano particles depends significantly on its surface free energies and surface stress. Nanoparticles either can exist as isolated species or they can form aggregates or they can dissolve into ions in solutions. These processes result in different sizes and sizes regimes and with this variance in size, the properties also vary in nano scale length[3]. The electronic properties for semiconductor nano-particles, localized surface plasmon resonance (LSPR) of noble nanoparticles are cited to be size dependent. LSPR for Ag nanoparticles shifts across the electromagnetic spectrum as the shape of the particle changes from a sphere to cylinder to cube to prism to pyramid [3]. Similarly, the optical characteristics of zinc oxide materials have been found to depend on their micro structures, morphologies and particle size [6] . The UV-blocking property of nanoZnO also thus depends on its size and morphology i.e, nanoZnO particles with different sizes and morphologies would have varied UV-blocking properties. In the present study nanoZnO particles with two different sizes and morphologies were prepared via chemical route using different precursors. The synthesized nano particles were then incorporated in to a di-glycidylbisphenol A (DGEBA) epoxy coating based on micron-sized titanium dioxide (TiO2) and then subjected to UVB weathering conditions for two cycles and the effect of synthesized nanoZnO particles in lowering yellowing of epoxy on weathering was evaluated.It was found that the nanoZnO particles with flake-like morphology compared to the spherical nanoZnOwere more efficient in imparting yellowing resistance to the formulated epoxy coating.
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II. EXPERIMENTAL Synthesis of nanoZnO particles 1. Flake-like nanoZnO Materials Zinc sulfate heptahydrate (ZnSO47H2O), ammonia solution (NH4OH), ammonium bicarbonate (NH4HCO3), anhydrous alcohol and deionized water
Methodology The first stage involved synthesis of the precursor, zinc carbonate hydroxide (ZCH) using a 1:10:1 (ratio by volume) of aqueous ammonia (7 mol/L): ZnSO47H2O solution (0.5 mol/L): NH4HCO3 (3 mol/L). Aqueous ammonia followed by NH4HCO3 solution, both, were drop-wise added to a continuously stirred solution of ZnSO47H2O at room temperature. The reaction mixture was then heated up to 600C and stirred at this temperature for 30 minutes. The ZCH precipitate was then filtered and washed with deionized water to ensure complete removal of sulphate ions (SO42-). The ZCH precursor was air dried and calcined at 4000C for two hours to obtain nano sized zinc oxide particles.
2. Spherical nanoZnO Materials Zinc acetate dihydrate, methanol, KOH Methodology The following two solutions of appropriate concentrations were prepared which were mixed at room temperature with continuous stirring: Solution A - Zinc acetate dehydrate in methanol Solution B - KOH in methanol A bulky white precipitate arose immediately which became translucent after stirring for approximately 70 minutes. The solution was then heated to boiling point, after which the heat source was switched off. The solution was then allowed to stand over-night. The sediment thus obtained was stirred and centrifuged off. The white gel like product obtained was washed with de-ionized water and then dried to obtain the nano-sized zinc oxide particles. The synthesized nano-powders were investigated by Transmission Electron Microscopy (TEM, Philips CM200 electron microscope), Scanning Electron Microscopy (SEM, Model no.S3400, Hitachi) and X-ray diffraction (XRD, XPert Pro Philip) for its shape, size and crystallinity. FTIR (JASCO FTIR 6100) studies of nano-powders were carried out to study the structure of the oxides. Preparation of epoxy coated samples Materials Di-glycidyl ether of bis-phenol A epoxy (EEW=185), Diethylene-tetramine (DETA), xylene, titanium dioxide (TiO2), BYK additives The mild steel (MS) samples to be coated were de-greased, cleaned and then roughened mechanically with abrasive paper (emery paper grade no.: 100). A TiO2 based white coating was formulated with 35% pigment concentration, 50% epoxy resin concentration, ssssDETA as hardener and rest with the appropriate concentrations of additives and xylene as solvent. The nanoZnO modified epoxy coatings were prepared by addition of firstly the micron sized TiO 2 pigment along with the required amount of nanoZnO at different loading levels, maintaining the 35% pigment concentration in the coating followed by the additives. Nano zinc oxide was added to the epoxy resin using ultra-sonnication at 1%, 2% and 5% (by weight) of the total coating formulation. The only purpose to take TiO2 as the pigment was to formulate a white coating
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and hence evaluate discoloration/ yellowness of the coating on weathering. The pigment concentration was always maintained at 35% with and without nanoZnO while formulating the coatings. The coating formulation for different loading of nanoZnO in the coating is as tabulated as follows:
Table.1. Epoxy coating formulation with and without nanoZnO

Component TiO2 pigment Nano ZnO Resin BYK 530 BYK 333 BYK 9076 BYK 320 Xylene Neat Epoxy (%) 35.0 0 50.0 2.0 1.0 1.5 0.5 10 1% nanoZnO + Epoxy (%) 34 1 50.0 2.0 1.0 1.5 0.5 10 2% nanoZnO + Epoxy (%) 5% nanoZnO + Epoxy (%) 33 2 50.0 2.0 1.0 1.5 0.5 10 30 5 50.0 2.0 1.0 1.5 0.5 10
As mentioned in the table above, the resin content was kept constant throughout in the coatings, with different nanoZnO concentrations. The resulting blend was ultrasonnicated for 20 minutes and the shear time via ultrasonication was kept constant for all loadings of nanoZnO. After mixing TiO2 pigment, nanoZnO and additives, at the end, hardener and solvent were mixed to obtain the nanoZnO modified epoxy coatings. The formulated coating was applied using brush on the surface treated MS panels so as to achieve uniformly coated panels with good finish and then allowed to hard cure. Weathering Test The coated MS panels were subjected to accelerated weathering in a UV weatherometer (QUV Weatherometer, Q-Lab Products & Services) equipped with UVB-313 nm lamps. The test cycle in UVB-weatherometer comprised of 4 hours UVB simulation at 600C followed by 4 h of condensation (UVB-lights off during condensation) at 500C as per accordance of ASTM G-154. The epoxy coated MS panels were exposed to two test cycles, i.e, 16 hours in the weatherometer. The coatings exposed in UVB weatherometer were characterized for color change (dE) and yellowness index (YI) using a spectrometer (BYK-Gardener Spectrometer) equipped with Color-Lab Quality Control software. The data were reported on L, a, b scales and overall color difference was given in the following equation: dE = [L2+ a2+ b2] where; L = L2 - L1, a = a2 - a1, and b = b2 - b1 Respective numbers 1 and 2 are denoted to samples before and after the exposure test. The yellowness index was measured as per ASTM D 1925, formulated as: YI = 100 (1.28 XCIE 1.06 ZCIE) / YCIE As per ASTM D 1925, the conditions for measurement are as follows: Illuminant: C, Standard Observer function: 2 0, denoted as C/20. X, Y and Z are the tristimulus values and 1.28 and 1.06 are the coefficients as per C/20 conditions. The surface morphology of the coatings was studied using SEM microscopy (SEM, Model no.S3400, Hitachi) to look for the distribution of nano zinc oxide at different loading levels in the coatings.
III. RESULTS& DISCUSSION
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Characterization of nanoZnO 1. Flake-like nanoZnO The synthesis methodology involving zinc sulfate heptahydrate (ZnSO47H2O), ammonia solution (NH4OH) and ammonium bicarbonate (NH4HCO3) as starting materials, resulted in formation of zinc carbonated hydroxide (ZCH) which on calcination gave nanoZnO. The purity of nanoZnO was checked by FTIR and XRD analysis and their shape and size were established by SEM, TEM and HRTEM analysis. Zinc oxide shows typical characteristic Zn-O peak at around 470 and 480 cm-1[7-9]. This was confirmed by FTIR analysis as seen in figure.1 which showed Zn-O peaks at 468 and 480 cm-1.
Figure.1. FTIR spectrum of flake-like nano zinc oxide
Figure.2 shows the XRD spectra of the synthesized nano zinc oxide. The XRD analysis identified well indexed diffraction peaks, in good agreement with those of a wurtzite hexagonal structure of ZnO (ICSD Reference code 01-075-0576) [10-12]. The flake-like nanoZnO particles showed the characteristic peaks at 320, 340 and 36 resulting from the 100, 002 and 101 planes respectively.
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Figure.2. XRD spectrum of flake-likenanoZnO The SEM micrograph (figure.3), showed the nanoZnO particles to have flake-like morphology.
Figure.3. SEM micrograph of flake-like nanoZnO
The flake-like morphology was confirmed by TEM.As shown in figure.4, the flake-like morphology of ZnO composed of small spherical particles with diameter ranging from 7 to 20 nm.
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Figure.4. TEM image of flake-like nanoZnO
The lattice fringes of synthesized zinc oxide were clearly identified in the HR-TEM image as shown in figure.5. The interplanar spacing i.e. d-spacing was obtained as 0.29 nm which closely matched to the d-spacing of 100 plane (0.281nm) of zinc oxide [13-15].
Figure.5. HR-TEM image of flake-like nano-ZnO
2. Spherical nanoZnO Nano ZnO was found to have spherical particle shape when prepared by chemical route using zinc acetate dehydrate and methanol as starting materials. The FTI spectrum with characteristic Zn-O peaks at 468 cm-1 and 476 cm-1 is as shown in figure.4.6. iThe XRD spectrum of the nanoZnO particles is shown in figure.7. The XRD pattern observed was assigned to the pure phase of zinc oxide (Joint Committee on Powder Diffraction Standards (JCPDS card number: 01-079-0205) which confirmed a wurtzite hexagonal structure.
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Figure.6. FTIR spectrum of spherical nanoZnO
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Figure.7. XRD spectrum of spherical nanoZnO
The SEM micrograph of the nano-ZnO particles showed single phase primary particles with spherical shape. TEM monograph showed that the product consisted of particles with diameter ranging from 20-25 nm.
Figure.8. SEM micrograph of spherical nanoZnO
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Figure.9. TEM micrograph of spherical nanoZnO Weathering Study of nanoZnO modified Epoxy Coatings The effect of nano-ZnO addition to epoxy was studied by formulating epoxy coating with different concentrations of nanoZnO. A TiO2 based coating with DGEBA epoxy resin and DETA hardener, as mentioned in the previous chapter, was formulated with different concentrations of nanoZnO particles to optimize the concentration of nano-ZnO in the coating. Nano ZnO, both flake-like and spherical shaped, was added at 1%, 2% and 5% by weight of total coating formulation. The pigment concentration was maintained as 35% during the loading of nanoZnO particles in the coating. Evaluation of color change and yellowing of weathered nanoZnO modified epoxy coatings The neat epoxy and both flake-like and spherical shaped nanoZnO modified epoxy coatings formulated as per the above tabulated values were exposed to accelerated UVB exposure for two cycles (16 hours). The color change (dE) and yellowness index (YI) values obtained by spectrophotometric analysis are as shown in figure.10-11
Figure.10. dE and YI plot for flake-like nanoZnO + epoxy coating
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Figure.11. dE and YI plot for spherical nanoZnO + epoxy coating The epoxy coatings formulated with and without nano-ZnO, were applied on 0.7 mm thick MS panels by brush. The coating thickness was determined using a thickness measuring gauge (Elcometer DFT Gauge) and the coating thickness for the coating systems were found to be in the range of 85-100 microns. The color change (dE) and yellowness index (YI) results were evaluated after 16 hours of UVB exposure. i.e, two cycles of UV (B) weathering were each cycle of 8 hours comprises of 4 hour UVB light followed by 4 hour condensation.The discoloration observed in epoxies on weathering is attributed to the formation of a quinone- methide structure and has been confirmed in many cited studies by both infrared and UV-Vis analysis[16]. As observed from the dE and YI plots, both flake-like and spherical shaped nanoZnO exhibited lower dE and YI values at all loading levels compared to the neat epoxy coating system. The optimized loading concentration of both flake-like and spherical nanoZnO was observed to be 2 wt% of the total coating formulation. Flake-like nanoZnO lowered yellowing and color change by 12 and 8 units respectively while the spherical nanoZnO lowered the same by only 5 and 3 units respectively. The increase in dE and YI values for both flake-like and spherical nanoZnO beyond the optimized 2 wt% loading is attributed to the agglomeration of nano particles in the coating matrix. Agglomeration of nano-particles is undesirable as it makes nano-particles lose their high surface area and thus the desired functional properties [17]. The result of agglomeration is that the nanoZnO would not be evenly distributed and so there will be regions in the coating that would be starved of zinc oxide and not protected, by zinc oxide in the coating. The extent of weathering resistance, offered by the nanoZnO modified epoxy coating systems were determined by evaluating the percentage reductions in color change (dE) and yellowing (YI) during the exposure. The percentage reduction values were calculated as follows: Suppose after a test cycle, Neat Epoxy = A Modified Epoxy = B A and B are dE/YI values after the weathering cycle, then; % Reduction = [(A-B) / A] x 100 The percentage reduction values in dE and YI, thus calculated for the nanoZnO modified epoxy coatings are as shown in figure.12 13.
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Figure.12. % Reduction in dE and YI plot for flake-like nanoZnO + epoxy coating
Figure.4.13. % Reduction in dE and YI plot for spherical nanoZnO + epoxy
Table.2. dE, YI, % Reduction in dE and YI for nanoZnO modified epoxy coatings Systems dE 0% nanoZnO +Epoxy 1% nanoZnO + Epoxy 14.07 23.51 18.25 Flake-like nanoZnO + Epoxy YI 29.99 % Reduction dE 23 % Reduction YI 22 15.86 25.75 dE 18.25 Spherical nanoZnO + Epoxy YI 29.99 % Reduction dE 13 % Reduction YI 14
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2% nanoZnO + Epoxy 5% nanoZnO + Epoxy
10.74
18.24
41
40
15.2
24.69
17
18
11.75
19.33
36
35
16.69
27.7
8.5
High percentage reduction values in dE and YI indicates more resistance to color change and yellowing. The highest percentage reduction values were observed at 2% loading level respectively for flake-like and spherical nanoZnO modified epoxy coatings compared to 1% and 5%. Flake-like nanoZnO reduced color change and yellowing by 40% while spherical nanoZnO reduced the same by 17%, at 2% loading in the coating formulation. The enhanced weathering resistance for the nano-ZnO incorporated epoxy coatings is due to UV-absorption property of ZnO owing to its large band gap energy. Zinc oxide has a band-gap at around 3.37 eV corresponding to 376 nm and thus it absorbs light that matches or exceeds this band gap energy[1, 2]. UV-range of solar spectrum lies within this range and thus UV light gets absorbed by zinc oxide particles. The UV-blocking property of zinc oxide is only enhanced when it comes to nano-sized ultra-fine ZnO particles. Though, both flake-like and spherical nanoZnO offered resistance to color change and yellowing in the nanoZnO modified epoxy coatings, the flake-like nanoZnO outperformed spherical nanoZnO. Nano ZnO with flake-like morphology acted as a better UV-blocker than the spherical nano-ZnO and hence imparted more efficient weathering resistance when incorporated in the epoxy coatings. It was thus inferred that nanoZnO with different shape and size performed differently when incorporated in epoxy coatings and subjected to UVB exposures. The better performance of the flake-like nano-ZnO is attributed to its morphology and size. Nano particles possess unique properties owing to their nano size dimensions however these properties change with their shape and size and the causes are different for different materials [3, 4]. RoshidahRusdi et al. (2011) have reported in their work that ZnOnano-tubes have a wider band gap compared to that of spherical nanoZnO particles and have explained this by the characteristics of materials at nano dimensions[6]. At nano scale, increase in pressure results in strong forces in the interiors of crystallites and hence the lattice spacing of ZnO nanotube decreases. It was proposed then, that due to the strong internal forces, the electrons taking part in transition from the valence band to the conduction band need greater energy, accounting for the observed wider band gap [3, 4]. All these changes eventually change the properties of the nano particles. It was also seen that the absorption profile for nanoZnO with nanotube and nano rod structures were a little different from that of the spherical particles. Also, from thermodynamic considerations, the total free energy is a sum of free energy of the bulk and the surface of nano particle. G nanoparticle= G bulk + G surface For nanoparticles, G surface is no longer a minor component and hence all fundamental properties of nanoparticles are size dependent as well as shape dependent [5]. The flake like nanoZnO particles diameter ranged from 7 20 nm while the spherical shaped nano particles had diameter size of 20 25 nm.The different behavior of flake-like and spherical nanoZnO in imparting weathering resistance to epoxy coating can be thusexplained on the basis of size and morphology difference of the nanoZnO particles. As the nano size decreases, the space in which charge carriers move decreases and additional quantum confinement is imposed on their motion. This leads to increase in the band gap energy, electron-hole kinetic energy and the density of the charge carriers within and at the nanoparticle surface.The enhanced reduction in color change and yellowing for the flake-like nanoZnO compared to spherical nanoZnO in the epoxy coating at all loadings in the epoxy coating is thus attributed to the difference in their size, shape and morphology.
IV. CONCLUSION Nano zinc oxide (ZnO) particles were synthesized with two different morphologies namely, flake-like and spherical with different sizes. Flake-like nanoZnO had diameter ranging from 7-20nm while spherical nanoZnO had diameter in the
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range of 20-25nm. Both flake-like and spherical nanoZnO when incorporated in a DGEBA based epoxy coating lowered yellowing of the epoxy coating on weathering. The optimized loading concentration was 2 wt% of the total coating formulation. The efficiency of the nanoZnO particles were found to be size and morphology dependent as the flake-like nanoZnO lowered yellowing and color change by 40% while the spherical nanoZnO particles lowered the same by 18%.
REFERNCES [1]Cao, Z., et al., Synthesis and UV shielding properties of zinc oxide ultrafine particles modified with silica and trimethylsiloxane. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2009. 340(13): p. 161-167. [2]GeunjaeKwak, et. Al.,Multifunctional transparent ZnOnanorod films.Journal of Nanotechnology, 2011.22. [3]ClememsBurda., et al.,Chemistry and Properties of Nanocrystals of Different Shapes.Chemical Review, 2005. 105: p. 1025 - 1102. [4] El-Sayed, M.A., Some Interesting Properties of Metals Confined in Time and Nanometer Space of Different Shapes Accounts of Chemical Research, 2001.34(4): p. 257-264. [5]Grassian, V.H., When Size Really Matters: Size-Dependent Properties and Surface Chemistry of Metal and Metal Oxide Nanoparticles in Gas and Liquid Phase Environments.Journal of Physical Chemistry C, 2008.112(47): p. 18303 18313 [6] R. Rusdi, et al., Preparation and band gap energies of ZnO nanotubes, nanorods and spherical nanostructures. Journal of Powder Technology, 2011, 210 (1), 18-22 [7] Cao, Z., et al., Synthesis and UV shielding properties of zinc oxide ultrafine particles modified with silica and trimethylsiloxane. Colloids and Surfaces A: Physicochemical and Engineering Aspects, 2009. 340(13): p. 161 167. [8] Geunjae Kwak, S.J.a.K.Y., Multifunctional transparent ZnO nanorod lms. NANOTECHNOLOGY, 2011. 22. [9] Xiong, M., et al., Preparation and characterization of poly(styrene butylacrylate) latex/nano-ZnO nanocomposites. Journal ofApplied Polymer Science, 2003. 90(7): p. 1923-1931. [10] Allen, N.S., et al., Behaviour of nanoparticle (ultrafine) titanium dioxide pigments and stabilisers on the photooxidative stability of water based acrylic and isocyanate based acrylic coatings. Polymer Degradation and Stability, 2002. 78(3): p. 467 - 478. [11] Amirudin, A. and D. Thieny, Application of electrochemical impedance spectroscopy to study the degradation of polymercoated metals. Progress in Organic Coatings, 1995. 26(1): p. 1-28. [12] Ariosa, D., et al., Texture vs morphology in ZnO nano-rods: On the x-ray diffraction characterization of electrochemicallygrown samples. Journal of Applied Physics, 2011. 110(12): p. 124901. [13] Armstrong, R.D., A.T.A. Jenkins, and B.W. Johnson, An investigation into the uv breakdown of thermoset polyester coatingsusing impedance spectroscopy. Corrosion Science, 1995. 37(10): p. 1615-1625. [14] Xu, X., et al., Size Dependence of Defect-Induced Room Temperature Ferromagnetism in Undoped ZnO Nanoparticles. TheJournal of Physical Chemistry C, 2012. 116(15): p. 8813-8818. [15] R. Sreej., et al., Linear and nonlinear optical properties of luminescent ZnOnanoparticles embedded in PMMA matrix Optics Communications, 2010. 283: p. 29082913. [16] Down, J.L., The Yellowing of Epoxy Resin Adhesives: Report on High-Intensity Light Aging. Studies in Conservation, 1986.31(4): p. 159-170. [17] Raymond, H.F., Nanocomposite and Nanostructured Coatings: Recent Advancements, in Nanotechnology Applications in Coatings2009, American Chemical Society. p. 2-21.
AUTHORS First Author NarayaniRajagopalan, Research Scholar, IIT Bombay, narayani@iitb.ac.in Second Author Anand S Khanna, PhD, IIT Bombay, kkhanna@iitb.ac.in Correspondence Author NarayaniRajagopalan,narayani@iitb.ac.in , indu03raj@gmail.com Contact number - 9833357520
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International Journal of Scientific and Research Publications, Volume 3, Issue 4, April 2013 ISSN 2250-3153

Effect of size and morphology on UV-blocking property of nanoZnO in epoxy coating

Table.1. Epoxy coating formulation with and without nanoZnO

III. RESULTS& DISCUSSION

Figure.1. FTIR spectrum of flake-like nano zinc oxide

Figure.3. SEM micrograph of flake-like nanoZnO

Figure.4. TEM image of flake-like nanoZnO

Figure.5. HR-TEM image of flake-like nano-ZnO

Figure.6. FTIR spectrum of spherical nanoZnO

Figure.7. XRD spectrum of spherical nanoZnO

Figure.8. SEM micrograph of spherical nanoZnO

Figure.10. dE and YI plot for flake-like nanoZnO + epoxy coating

Figure.12. % Reduction in dE and YI plot for flake-like nanoZnO + epoxy coating

Figure.4.13. % Reduction in dE and YI plot for spherical nanoZnO + epoxy

2% nanoZnO + Epoxy 5% nanoZnO + Epoxy

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