Deposition of ZnSO4 · 3Zn(OH)2 · 4H2O films by SILAR method and their study by XRD, SEM and µ-Raman

Main Article Content

F N Jiménez García
H H Ortiz Alvarez
H Reyes Pineda

Keywords

ZnSO4 · 3Zn(OH)2 · 4H2O, ZnO, SILAR, XRD, SEM, Raman, corrosion.

Abstract

ZnSO4 · 3Zn(OH)2 · 4H2O(Zinc Sulfate Hidroxide Hidrate) films were obtained on glass substrates by SILAR method. It was employed a precursor
solution of ZnSO4 and MnSO4 and water near boiling point complexed with 1 ml of NH4OH as a second solution. Films were treated on air at 300oC by 1 hour. Both films ZnSO4·3Zn(OH)2·4H2O as ZnO are important protective against zinc corrosion because they are passive films that give a longer duration to material, it is therefore relevant to study their response to temperature changes. For those reasons films were analyzed before and after thermal treatment to study the structural and morphological changes by X ray diffraction (XRD), Scanning electron microscopy (SEM) and Raman Microscopy techniques. It was found before thermal treatment by XRD the
presence of ZnSO4 · 3Zn(OH)2 · 4H2O triclinic phase and after such treatment the ZnO hexagonal phase was evidenced. The morphology identified by SEM before thermal treatment was sheets formed by platelet like structure of micrometric size which changes after thermal treatment to a combination of
those sheets with flowers like structure characteristic of ZnO hexagonal. By µ-Raman the hexagonal ZnO phase before thermal treatment as the triclinic
ZnSO4 · 3Zn(OH)2 · 4H2O phase after thermal treatment were confirmed.
One objective of this study was to obtain this protective corrosion material in a controlled manner by techiniques of low cost and high simplicity as Silar
method. Which, even under temperture increases continue being protective corrosion although suffers phase changes because new phases have protective
corrosive characteristics too.

PACS: 81.65.Rv, 81.05.-t

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References

[1] TE. Graedel. Gildes model studies of aqueous chemistry. I. Formulation andpotential applications of the multi regime model. Corros. Sci, ISSN 0010-938X,38(12), 2153–2180 (1996).
[2] V. Ligier, M. Wery, JY. Hihn, J. Faucheu, M. Tachez. Formation of the mainatmospheric zinc and products: N aZn4Cl(OH)6SO4• 6H2O, Zn4SO4(OH)6•nH2O, Zn4Cl2(OH)4SO4• 5H2O in [Cl−1][SO2−4][HCO−3][H2O2] electrolytes.Corros. Sci, ISSN 0010-938X, 41(6), 1139–1164 (1999). Referenciado en 34
[3] SC. Chung, AS. Lin, JR. Chang, HC. Shih. EXAFS study of atmosphericcorrosion products on zinc at the initial stage. Corros. Sci, ISSN 0010-938X,42(9), 1599–1610 (1999).[4] N. Sato. Ion-selective diffusion layer and passivation of metal anodes.Electrochim. Acta, ISSN 0013-4686, 41(9), 1525–1532 (1996).

[5] UR. Evans. Corrosion and Oxidation of Metals. ISBN 9780713125368. Arnold,London, 1960.

[6] XD. Gao, XM. Li, WD. Yu, L. Li, F. Peng, CY. Zhang.Microstructure analysis and formation mechanism of ZnO nanoporous film viathe ultrasonic irradiation mediated SILAR method. Journal of Crystal Growth,ISSN 0022-0248, 291(1), 175–178 (2006).
[7] VR. Shinde, CD. Lokhande, RS. Mane, SH. Han. Hydrophobic andtextured ZnO films deposited by chemical bath deposition: annealing effectApplied Surface Science, ISSN 0169-4332, 245(1), 407–413 (2005).

[8] VR. Shinde, TP. Gujar, CD. Lokhande. Studies on growth of ZnO thin films by anovel chemical method. Solar Energy Materials Solar Cells, ISSN 0927-0248,91(12), 1055–1061 (2007).

[9] C. Yan, D. Xue. Solution growth of nano- to microscopic ZnO on Zn.Applied Surface Science, ISSN 0022-0248, 310(7), 1836–1840 (2008).

[10] KS. Choi, HC. Lichtenegger, GD. Stucky, EW. McFarland. ElectrochemicalSynthesis of Nanostructured ZnO Films Utilizing Self-Assemblyof Surfactant Molecules at Solid-Liquid Interface. J. Am. Chem. Soc,ISSN 00002-7836, 124(42), 12402–12403 (2002).

[11] H. Usui. The effect of surfactants on the morphology and optical properties ofprecipitated wurtzite ZnO. Mater. Lett, ISSN 0167-577X, 63(17), 1489-1492(2009).

[12] R. Tena-Zaera, J. Elias, C. Levy-Clement, C. Bekeny, T. Voss, I. Mora-Sero,J. Bisquert. Influence of the Potassium Chloride Concentration on the PhysicalProperties of Electrodeposited ZnO Nanowire Arrays. J. Phys. Chem. C, ISSN1932-7447, 112 (42), 16318–16323 (2008).

13] R. Yi, H. Zhou, N. Zhang, G. Qiu, X. Liu. Effects of specific salts on themorphologies of ZnO microstructures. J. Alloys Compd., ISSN 0925-8388,479(1), L50–L53 (2009).
[14] L. Wang, G. Liu, L. Zou, D. Xue. Phase evolution from rod-like ZnO to plate likezinc hydroxysulfate during electrochemical deposition. Journal of Alloys andcompounds, ISSN 0925-8388, 493(2), 471-475 (2010).

[15] G. Hodes. Chemical Solution Deposition of semiconductor films. ISBN 978-0824708511. Marcel Dekker, INC. New York, 2003.

[16] JW Mellor. A Comprenhensive Treatise on Inorganic and Theoretical Chemistry.ISBN 0582462770. Longman, NY, 1953.

[17] RS. Jayasree, VPM. Pillai, VU. Nayar, I. Odnevall, G. Keresztury.Raman and infrared spectra analysis of corrosion products on zincN aZn4Cl(OH)6SO4,6H2O and Zn4Cl2(OH)64SO4 • 5H2O.Mater. Chem. Phys., ISSN 0254-0584, 99(2), 474–478 (2006).

[18] SPS. Porto, B. Tell, TC. Damen. Near-Forward Raman Scattering in Zinc Oxide.Phys. Rev. Lett., ISSN 0031-9007, 16(11), 450–452 (1966).

[19] VR. Shinde, CD. Lokhande, RS. Mane, SH. Han. Hydrophobic and textured ZnOfilms deposited by chemical bath deposition:annealing effect.Applied Surface Science, ISSN 0169-4332, 245(1), 407–413 (2005).

[20] P. Suresh Kumar, A. Dhayal Raj, D. Mangalaraj, D. Nataraj.Growth and charac-terization of ZnO nanostructured thin films by a two stepchemical method. Applied Surface Science, ISSN 0169-4332, 255(5), 2382–2387(2008).

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