Facile synthesis of calcium silicate hydrate using sodium dodecyl sulfate as a surfactant assisted by ultrasonic irradiation

doi:10.1016/j.ultsonch.2013.08.012

Ultrasonics Sonochemistry

Volume 21, Issue 2, March 2014, Pages 735-742

https://doi.org/10.1016/j.ultsonch.2013.08.012 Get rights and content

Highlights

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By sonication method calcium silicate hydrate was synthesized in high yields and short times.
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The effects of various time and SDS on morphology, crystallite sizes and yield were investigated.
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The CSH Nanosheets with high yield were obtained in ultra short period of 10 min with 0.2 g SDS in solvent.

Abstract

Calcium silicate hydrate (CSH) consisting of nanosheets has been successfully synthesized assisted by a tip ultrasonic irradiation (UI) method using calcium nitrate (Ca(NO₃)·4H₂O), sodium silicate (Na₂SiO₃·9H₂O) and sodium dodecyl sulfate (SDS) in water. Systematic studies found that reaction time of ultrasonic irradiation and concentrations of surfactant (SDS) in the system were important factors to control the crystallite size and morphologies. The products were characterized by X-ray power diffraction (XRD), field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectrometry (FTIR). The size–strain plot (SSP) method was used to study the individual contributions of crystallite sizes and lattice strain on the peak broadening of the CSH. These characterization techniques revealed the successful formation of a crystalline phase with an average crystallite size of about 13 nm and nanosheet morphology at a reaction time of 10 min UI with 0.2 g SDS in solvent which were found to be optimum time and concentrations of SDS for the synthesis of CSH powders.

Introduction

Calcium silicate (CaSiO₃) has gained significant attention due to its wide range of applications. It is well known that CaSiO₃ has excellent bioactivity, degradability, biocompatibility, and thus can be used as a substitute material for damaged teeth or bones and drug delivery [1], [2], [3]. Some studies have shown that calcium silicate hydrate (CSH) can induce formation of a bone-like apatite layer on their surface after soaking in simulated body fluid (SBF) [4]. The biocompatibility, stability, heat-insulating ability, low dielectric loss at high frequency and mechanical properties of calcium silicates are determined by their morphology, crystal size, composition and structure. Hence, the control over the morphology of calcium silicate and CSH is of great importance for biomedical and industrial applications [5], [6], [7], [8]. Many efforts have been made to synthesize CaSiO₃ and CSH of different morphologies such as nanowires, nanobelts and hollow microspheres with varying diameters [2], [6], [7], [9], [10]. Many methods have been also used for synthesizing CaSiO₃ including solid-state reaction, sol–gel, hydrothermal, precipitation methods, mechanochemical and microwave-assisted methods [6], [10], [11], [12]. The chemical precipitation method is the most often reported for preparing CaSiO₃ materials [2]. This method is low cost, simple and appropriate for industrial production but the product morphology is poor and large size crystalline particles are obtained. Recent investigations reveal that the reactivity of chemical species in solution being involved in a synthesis method can be stimulated by ultrasonic irradiation of the reaction mixture [13]. Sonochemistry shows potential for the synthesis of nanomaterials due to the ultrasonic cavitation process in an aqueous medium including formation, growth and collapse of micro bubbles. The sonochemical method has been used to produce unusual morphologies such as flower-like of monetite [14], nanorods of ZnO [15], nanosheets of SnO [16] and nanospheres of MnO₂ [17]. Recently, Zhang and Chang [7] synthesized CSH microspheres in an ultrasonic cleaning bath but other morphologies have not been well investigated. Meanwhile, the efficiency and duration of the synthesis process depend on the type of used ultrasonic device. Some literature indicate that a tip ultrasonic homogenizer is more efficient than an ultrasonic bath [13].

In the present study, we intend to synthesize calcium silicate hydrate powders by employing a tip ultrasonic irradiation in water solvent. Initially, the effect of UI time on morphology, crystallite sizes and lattice strain of the obtained powders was analyzed. The anionic surfactant SDS was then used in order to investigate the influence on the assembly of the nanosheets and crystallite sizes.

Section snippets

Chemicals and apparatus

All chemicals were procured from Sigma–Aldrich Ltd. and used as received. The ultrasound apparatus was a Sonic Vibra Cell Ks-1220 model (20 kHz, 1200 W) using a direct immersion titanium horn.

Synthesis of calcium silicate hydrate by sonication at different times

The calcium silicate hydrate for the present study were synthesized by the reaction of calcium nitrate (Ca (NO₃)₂·4H₂O) and sodium silicate (Na₂SiO₃·9H₂O). 15 ml of 0.1 ml Ca (NO₃)₂·4H₂O with a pH of 11.5, and 15 ml of 0.1 ml Na₂SiO₃·9H₂O were mixed and the solution was stirred at room temperature for 10 min.

Results and discussion

As shown in Table 1, it was found that the yield of CSH increased when the sonication time was extended from 5 to 15 min at the same UI condition. The UI wave is not enough to blend the solution and precipitant uniformly within a short period of time, therefore the yield of CSH powders increased at longer times of insonation.

Fig. 1 shows the X-ray Diffraction (XRD) patterns of G1-Group obtained at different sonication time and in non-sonicated sample, which coincided with the calcium silicate

Conclusion

The main contribution of this study is that the synthesis of calcium silicate hydrate with appropriate quality and different morphologies is successfully performed via ultrasonic irradiation method. The following conclusions are drawn: (і) The output data from XRD and FESEM indicated that needle like morphology with average crystallite size of 9 nm have been successfully obtained by using calcium nitrate (Ca (NO₃)·4H₂O) and sodium silicate (Na₂SiO₃·9H₂O) in distilled water via UI. Moreover, the

Acknowledgments

Valuable discussions with Dr M.R. Mahmoudian and A.R. Akhiani are appreciated. This study was funded by Ministry of Higher Education (MOHE) of Malaysia, Grant number UM.C/HIR/MOHE/ENG/10 D000010-16001 and Institute of Research Management and Consultancy (IPPP), University of Malaya No. (PV008/2012A). The authors are grateful for the grants.

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View full text

Facile synthesis of calcium silicate hydrate using sodium dodecyl sulfate as a surfactant assisted by ultrasonic irradiation

Highlights

Abstract

Introduction

Section snippets

Chemicals and apparatus

Synthesis of calcium silicate hydrate by sonication at different times

Results and discussion

Conclusion

Acknowledgments

J. Endod.

Mater. Lett.

Mater. Lett.

Acta Biomater.

Mater. Charact.

Mater. Lett.

Ultrason. Sonochem.

Ceram. Int.

Ultrason. Sonochem.

Electrochem. Commun.

Solid State Sci.

Nucl. Instrum. Methods Phys. Res. Sect. B

Ultrason. Sonochem.

Ultrason. Sonochem.

Chem. Phys. Lett.