Characterization of CaCO3 Nanoparticles Synthesized by Reverse Microemulsion Technique in Different Concentrations of Surfactants

Document Type : Research Article


1 Department of Chemical Engineering, Islamic Azad University, Yasouj Branch, Yasouj, I.R. IRAN

2 Department of Chemical Engineering, Aligarh Muslim University, Aligarh, UP, INDIA


Calcium carbonate nano-particles were synthesized by a reverse micro-emulsion method at room temperature with Tween® 80 and Span® 80 as co-surfactants. The nano-particles synthesized were surface modified by stearic acid. An important operating variable in the Span 80-Tween 80/toluene/water reverse micro-emulsion system, the ω-value (water/surfactant molar ratio) was investigated. The material was characterized by SEM, TEM, X-Ray Diffraction (XRD), FT-IR, UV-VIS and TGA/DTA techniques. The size of the nano-particles was determined by TEM as well as XRD data for various concentrations of surfactants. The results showed that the size of the nano-particles was influenced by the concentration of the surfactants in the micro-emulsion system. The XRD analysis at room temperature showed single phase formation of calcite. FT-IR confirmed the formation of calcite with characteristic absorption bands observed at 712, 881 and 1460 cm-1, corresponding to ν4, ν2, and ν3 modes of CO3-2 absorption bands of calcite. The results of the UV-VIS spectrophotometric analysis indicated that the calcite (CaCO3) is an indirect gap material [(5.60 eV (30 wt.% surfactant), 5.40 eV (36 wt.% surfactant) and 5.36 eV (42 wt.%surfactant)] at room temperature.


Main Subjects

[1] Clifford Y.T., Chih-kuang C., Particle Morphology, Habit, and Size Control of CaCO3 Using Reverse Micro-Emulsion Technique, Chemical Engineering Science, 63, p. 3632 (2008).
[2] Sonawane S.H., Gumfekar S.P., Meshram S., Deosarkar M.P.,  Mahajan C.M., Khanna P., Combined Effect of Surfactant and Ultrasound on Nano Calcium Carbonate Synthesized by crystallization process, International Journal of Chemical Reactor Engpneering, 7, p. 1 (2009).
[3] Pai R.K., Pillai S., Nanoparticles of Amorphous Calcium Carbonate by Miniemulsion: Synthesis and Mechanism, Cryst. Eng. Comm., 10, P. 865 (2008).
[4] Liu, S.T., “Stabilized Vaterite”, USP 2005/0106110, (2005).
[5] Qiu S., Dong J., Chen G., Wear and Friction Behavior of CaCO3 Nano-Particles Used as Additives in Lubricating Oils, Lubrication Science, 12, p. 205 (2000).
[6] Chen J.F., Wang Y.H., Guo F., Wang X.M., Zheng C., Synthesis of Nanoparticles with Novel Technology: High-Gravity Reactive Precipitation, Industrial & Engineering Chemistry Research, 39, p. 948 (2000).
[7] Kelsall R., Hamley I., Geoghegan M., “Nanoscale Science and Technology”, John Wiley Sons, Weinheim, (2005).
[8] Wong T.S., Brough B., Ho C.M., Creation of Functional Micro/Nano Systems through Top-down and Bottom-up Approaches, MCB, 6, p. 1 (2009).
[9] Chowdhury A., Bould J., Nano-powders of Na0.5K0.5NbO3 Made by a Sol-Gel Method, J Nanopart Res, 12, p. 209 (2010).
[10] Weller H., Synthesis and Self-Assembly of Colloidal Nano-Particles, Phil.Trans. R. Soc. Lond. A, 361, p. 229 (2003).
[11] Sau T.K., Rogach A.L., Nonspherical Noble Metal Nanoparticles: Colloid-Chemical Synthesis and Morphology Control, Adv. Mater., 22, p. 1781 (2010).
[12] Wang Y.G., Sakurai M., Aono M., Mass Production of ZnO Nano-Tetrapods by a Flowing Gas Phase Reaction Method, Nanotechnology, 19, p. 245 (2008).
[13] Dutta J., Hofmann H., “Nano-materials”, SFIT, p. 4, (2003).
[14] Yu D., Chu Y., Dong L.H., Zhuo Y.J., Controllable Synthesis of CaCO3 Micro/Nanocrystals with Different Morphologies in Microemulsion, Chem. Research Chinese Universities, 26, p. 678 (2010).
[15] Sadowski Z., Polowczyk I., Frąckowiak A., Koźlecki T., Chibowski S., Bioinspired Synthesis of Calcium Carbonate Colloid Particles, Physicochem. Probl. Miner. Process, 44, p. 205 (2010).
[16] Alves L., Simoes H.W., Carvalho E.A., Bell M.J.V., Dos Anjos V.C., “Structural, Electronic and Vibrational Properties of the Calcite Phase of CaCO3: An Experimental and Theoretical Study”,, accessed September 05, (2011).
[17] Porras M., Solans C., Gonzalez C., Martınez A., Guinart A., Gutierrez J.M., Studies of formation of W/O Nano-Emulsions, Colloids and Surfaces A: Physicochem. Eng. Aspects, 249, p. 115 (2004).
[18] Deshmukh G.S., Pathak S.U., Peshwe D.R., Ekhe J.D., Effect of Uncoated Calcium Carbonate and Stearic Acid Coated Calcium Carbonate on Mechanical, Thermal and Structural Properties of Poly (Butylene Terephthalate) (PBT)/Calcium Carbonate Composites, Bull. Mater. Sci., 33, p. 277 (2010).
[19] Samsudin M.S.F., Mohd Ishak Z.A., Jikan S.S., Ariff Z.M., Ariffin A., Effect of Filler Treatments on Rheological Behavior of Calcium Carbonate and Talc-Filled Polypropylene Hybrid Composites, J. Appl. Polym. Sci., 102, p. 5421 (2006).
[20] Ottewill R.H., Tiffany J.M., The Adsorption of Long Chain Acids onto Rutile From n-Heptane, Journal of the Oil Colour Chemists Association, 50, p. 844 (1976).
[21] Roeges N.A, “Guide to the Complete Interpretation of Infrared Spectra of Organic Structures”, John Wiley & Sons, Chichester, (1994).
[22] Fanili G., Fermani S., Gazzano M., Oriented Crystallization of Vaterite in Collagenous Matrices, Chemistry, 4, p. 1048 (1998).
[23] Klugg H.P., Alexander L.E., “X-Ray Diffraction Procedures”, John Wiley & Sons, New York, (1974).
[24] Kumar T.S., “Preparation and Characterization of Novel Span-80: Tween-80 Based Organogels for Food and Pharmaceutical Industries”, A Thesis Submitted in Partial Fulfilment of the Requirements for the Degree of Master of Technology In Biomedical Engineering, National Institute of Technology Rourkela, p. 1 (2011).
[25] Sugih A.K., Shukla D., Heeres H.J., Mehra A., CaCO3 Nanoparticle Synthesis by Carbonation of Lime Solution in Microemulsion Systems, Nanotechnology, 18, p. 1 (2007).
[26] Blessie A.B., Marian E.G.P., Archilles A.V.C., Michael O.D.P., Persia A.D.Y., Study on the Functionality of Nano-Precipitated Calcium Carbonate as Filler in Thermoplastics, Journal of Solid Mechanics and Materials Engineering, 1, p. 564 (2007).
[27] Viravaidya C., Li M., Mann S., Microemulsion-Based Synthesis of Stacked Calcium Carbonate (Calcite) Superstructures, Chemical Communications, p. 2182 (2004).
[28] Wan W., Yu D., Xie Y., Guo X., Zhou W., Cao J., Effects of Nanoparticle Treatment and Mechanical Properties of Polypropylene/Calcium Carbonate Nano-Composites, Journal of Applied Polymer Science, 102, p. 3480 (2006).
[29] Tjong S.C., Structural and Mechanical Properties of Polymer Nanocomposites, Materials Science and Engineering R., 53, p. 73 (2006).
[30] Al-Ani S.K.J., Zihlif A.M., Optical Properties of Epoxy-Glass Microballoons Composite, Optical Materials, 59, p. 69 (1996).
[31] Zhao L.N., Feng J.D., Wang Z.C., In Situ Synthesis and Modification of Calcium Carbonate Nanoparticles via a Bobbling method, Sci. China Ser B-Chem., 52, p. 924 (2009).
[32] Chi-Ming C., Jingshen W., Jian-Xiong L., Ying-Kit C., Polypropylene/Calcium Carbonate Nano-Composites, Polymer, 43, p. 2981 (2002).