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. 2019 Oct 11;13(9):952–956. doi: 10.1049/iet-nbt.2019.0095

Influence of surfactants on structural, morphological, optical and antibacterial properties of SnO2 nanoparticles

Sujatha Karuppiah 1,2, Seethalakshmi Thangaraj 1,✉, Sudha Arunachalam Palaniappan 2, Shanmugasundaram Olapalayam Lakshmanan 3
PMCID: PMC8676208  PMID: 31811765

Abstract

Tin oxide (SnO2) nanoparticles were synthesised using various surfactants of different charges (n‐cetyl trimethyl ammonium bromide, sodium dodecyl sulphate and TRITON X‐100) by the co‐precipitation method. The synthesised nanomaterials were characterised using different techniques to study their structural, surface morphological, optical and anti‐bacterial activities. X‐ray diffraction patterns revealed the formation of a tetragonal rutile structure in pure and surfactants‐aided SnO2 nanoparticles and the results show good agreement with JCPDS data [41‐1445]. The crystallite size of SnO2 nanoparticles was found to decrease with the addition of surfactants. Scanning electron microscopy images exhibit spherical shape morphology with an average diameter of 30–75 nm for pure and surfactants‐aided SnO2 nanoparticles. The band gap energy of the prepared materials was estimated from the UV–visible absorption spectra and a considerable increase in band gap energy was observed in surfactants‐aided SnO2 nanoparticles (3.487, 3.57, 3.50 and 3.3 eV). The antibacterial activities of the synthesised nanoparticles were studied against Escherichia coli and Staphylococcus aureus bacteria.

Inspec keywords: visible spectra, precipitation (physical chemistry), ultraviolet spectra, nanofabrication, tin compounds, X‐ray diffraction, crystallites, titanium compounds, particle size, antibacterial activity, surfactants, nanoparticles, energy gap, scanning electron microscopy, surface morphology, semiconductor materials, optical constants, semiconductor growth

Other keywords: SnO2 , co‐precipitation method, anti‐bacterial activities, X‐ray diffraction patterns, tetragonal rutile structure, spherical shape morphology, band gap energy, sodium dodecyl sulphate surfactant, surface morphology, surfactant‐aided SnO2 nanoparticles, crystallite size, scanning electron microscopy, UV–visible absorption spectra, Escherichia coli, Staphylococcus aureus bacteria, TRITON X‐100 surfactant, n‐cetyl trimethyl ammonium bromide surfactant

1 Introduction

In recent years, nanomaterials have been gaining much importance due to their unique properties. The band gap energy increased and the edges of the bands were split into discrete energy levels due to the decrease in particle size [1]. Tin oxide (SnO2) is one of the most exciting semiconducting materials which is a well‐known n‐type semiconductor with a wide band gap of 3.6 eV [2], and their unique properties are used in many applications like gas sensors, transparent conducting electrodes for solar cells, photochemical and photoconductive devices, lithium‐ion batteries etc. [3, 4, 5, 6, 7, 8, 9, 10]. SnO2 nanoparticles were prepared by many processes such as spray pyrolysis, hydrothermal methods, chemical vapour deposition, thermal evaporation of oxide powders and the sol–gel method [11, 12, 13, 14, 15, 16, 17].

From the research studies, it can be noted that the microstructure of the nanoparticles can be changed with the addition of surfactants. This research investigates the effect of surfactants on the surfaces of SnO2 nanoparticles. Organic surfactants can be easily separated from the structure of synthesised material by calcinations or washing through alcohols. In the preparation of nanocrystalline metal oxide, surfactants are used to control their growth and to provide solubility [18]. Surfactants used to arrange the small oxide crystallites into a suitably ordered structure to produce regular pores and low‐angle Bragg reflection [19]. Kiran Jain et al. [20] observed that the gas sensitivity of surfactants‐aided nanopowders was increased for liquefied petroleum gas (LPG) and compressed natural gas (CNG) due to a low degree of agglomeration. Muhammad Akhyar Farrukh et al. [21] reported that the particle size of tin oxide nanoparticles was decreased with the addition of non‐ionic surfactant (oleyl amine). Amininezhad et al. [22] stated that SnO2 nanoparticles have the strongest antibacterial activity against Escherichia coli bacteria and moderate activity against Staphylococcus aureus. Even though fewer reports are available on the synthesis of surfactants‐aided SnO2 nanoparticles, to the best of our information no earlier report has been found that examines the effect of surfactants with different charges on the structural, surface morphological, optical and anti‐bacterial activity of the SnO2 nanoparticles obtained by the co‐precipitation method. The aim of this work is to synthesis SnO2 nanoparticles by the co‐precipitation method and to study the influence of cationic, anionic and nonionic surfactants [n‐cetyl trimethyl ammonium bromide (CTAB), sodium dodecyl sulphate (SDS) and TRITON X‐100] on the properties of SnO2 nanoparticles. Furthermore, the co‐precipitation method is simple, less time‐consuming, cost‐effective and does not require any sophisticated instruments compared to the other methods.

2 Experimental procedure

2.1 Materials

The chemicals used for the synthesis of pure and surfactants‐aided tin oxide nanoparticles were stannous chloride (SnCl2 ·2H2 O), CTAB, SDS, TRITON X‐100, ammonium hydroxide (NH4 OH) and double distilled water. Double distilled water was used as a solvent to prepare the solution of chemical mixtures. All chemicals are of analytical grade and used as received without any further purification.

2.2 Synthesis of pure SnO2 nanoparticles

The pure SnO2 nanoparticles were synthesised by the chemical precipitation method. About 1 M (4.5 g) of SnCl2 ·2H2 O was dissolved in 20 ml distilled water with constant stirring for15 min. The pH of the solution was adjusted to 8 with the dropwise addition of ammonium hydroxide solution under vigorous magnetic stirring. At the end of the reaction, a white colour solution was obtained and the solution was aged for 96 h at room temperature. The resultant solution was washed with deionised water several times to remove chlorine ions and further washed with ethanol to remove NH4+ ions. The final solution was filtered using Whatman filter paper and the obtained precipitate was dried for 1 h at 80°C using an oven. The dried sample was calcinated at 350°C for 1 h using a muffle furnace to improve crystallinity. Finally, the powder was ground using a mortar and pestle to get pure tin oxide nanoparticles.

2.3 Synthesis of surfactants‐aided SnO2 nanoparticles

The authors followed the same procedure (synthesis of pure tin oxide nanoparticles) for the synthesis of surfactants‐aided SnO2 nanoparticles. The aqueous solutions of 20 ml of CTAB (0.01 M), SDS (0.01 M) and TRITON X‐100 (5 ml) were stirred continuously for 15 min and added to the final solution and the same process was repeated for ageing, drying and calcination to get the final surfactants‐aided SnO2 nanoparticles.

3 Characterisation techniques

The pure and surfactants‐aided nanoparticles were characterised using different characterisation techniques. X‐ray diffraction (XRD) patterns were obtained using a LABX XRD 6000‐X RAY diffractometer with Cu Kα (λ  = 1.5406 Å) and the data were recorded in the 2Ɵ range of 10–90°. A scanning electron microscopy (SEM) image was obtained using a JEOL‐SEM (JSM‐6390 LV). The optical properties were analysed using an UV–VIS–NIR spectrophotometer (JASCO) in the wavelength range 200–800 nm. The antibacterial activities of the samples were tested against S. aureus (ATCC 29213) and E. coli (ATCC 25922) according to agar diffusion method.

4 Results and discussion

4.1 XRD analysis

The crystalline nature of the synthesised samples was examined using the XRD system. Fig. 1 shows the powder XRD pattern of pure and surfactants‐aided (CTAB, SDS and TRITON X‐100) SnO2 nanoparticles. From the pattern, it can be clearly seen that all diffraction peaks were well indexed to the tetragonal structure of SnO2 nanoparticles [23]. The XRD peaks pointed at 2θ  = 26.647°, 34.0°, 51.872°, corresponding to the (110), (101) and (211) reflection planes were in good agreement with the standard values (JCPDS 41‐1445). Related XRD results were also observed in the reported literature for the SnO2 nanoparticles [24, 25]. It was observed that the XRD peaks were well defined which indicated that the samples were crystallised. Interestingly, no extra diffraction peaks were observed in the result which shows no impurities were found, which further demonstrated that the prepared nanoparticles were pure SnO2.

Fig. 1.

Fig. 1

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XRD patterns of pure and surfactants‐aided SnO2 nanoparticles: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 : TRITON

Fig. 2 shows the variation in the intensity of the primary peak of surfactants‐aided nanoparticles with pure SnO2 (A1). A close investigation reveals that there was some increase or decrease in the intensity of the primary peak of SnO2 nanoparticles due to the influence of surfactants. Furthermore, the intensity of the primary peak of pure and TRITON X‐100‐aided SnO2 nanoparticles were increased [26]. However, a decrease in the intensity peak was observed in CTAB (A2)‐ and SDS (A3)‐aided SnO2 nanoparticles [27, 28].

Fig. 2.

Fig. 2

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Primary peak shift of surfactants‐aided SnO2 nanoparticles: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

Changes in the peak width and peak shift of the primary diffraction peak (110) were observed for all surfactants‐aided SnO2 nanoparticles. The changes in the peak width of surfactants‐aided SnO2 nanoparticles occur as a result of the changes in strain which exposes that the addition of surfactants concentrates at the SnO2 lattice [29]. The calculated average crystallite size values (Table 1) were found to be decreasing for CTAB and SDS surfactants‐aided SnO2 nanoparticles [30] whereas the values were increased in TRITON‐aided SnO2 nanoparticles. The crystallite size of pure and surfactants‐aided (CTAB, SDS and TRITON) SnO2 nanoparticles were found to be 10.39, 8.436, 8.73 and 13.49 nm, respectively.

Table 1.

Structural parameters of pure and surfactants‐aided SnO2 nanoparticles

S. No. Samples Crystallite size D, nm Dislocation density (δ) ( × 1015 lines/m2) Microstrain (ɛ) (10−3) Lattice parameter, Å Unit cell volume (V), Å3 Distortion ratio (a /c)
a c
1 A1 10.39 9.2633 3.3333 4.7271 3.1732 70.9081 1.489725051
2 A2 8.436 14.0516 4.1064 4.6879 3.1598 69.4419 1.483607683
3 A3 8.73 13.1211 3.9673 4.7153 3.1655 70.3821 1.489612221
4 A4 13.49 5.4992 2.5689 4.7492 3.1899 71.9476 1.488841981
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It was observed that the value of the microstrain for all the samples indicated the line shifting in the d spacing deviation. The calculated microstrain using (3) is positive due to the presence of tensile stress on the surface of the particles [31]. Lattice distortion is proportional to the microstrain:

1d2=h2+k2a2+l2c2 (1)
V=a2c (2)
ε=βcosθ4 (3)

Lattice parameters a and c, cell volume of the samples were calculated using (1) and (2) and well matched with the reported value. Lattice parameters and cell volume were decreased for the addition of surfactants (CTAB, SDS) to the SnO2 nanoparticles. The tetragonal distortion (a /c) ratio of samples A1, A2, A3 and A4 were 1.4897, 1.483, 1.4896 and 1.488, respectively.

4.2 SEM analysis

The surface morphology of the nanoparticles was investigated using a SEM. Fig. 3 shows the usual SEM images of synthesised pure and surfactants‐aided SnO2 nanoparticles.

Fig. 3.

Fig. 3

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SEM images of pure and surfactants‐aided SnO2 nanoparticles: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

The structural changes were observed in pure and surfactants‐aided SnO2 nanoparticles. The SEM image of SnO2 nanoparticles (A1) revealed that the obtained nanostructure was spherical in shape with various particle sizes ranging from 35 to 55 nm. Fig. 3 (A2–A4) shows the effect of (CTAB, SDS and TRITON X‐100) surfactants‐aided SnO2 nanoparticles on their particle sizes. It has been found that CTAB‐aided SnO2 nanoparticles possess high affinity of agglomeration due to van der Waals force of attraction between molecules.

The size of CTAB‐ and SDS‐aided SnO2 nanoparticles was decreased (30–50 nm) which means that both these surfactants suppress the growth of SnO2 nanoparticles. However, the size was increased (45–75 nm) by the addition of TRITON X‐100 surfactant [32].

4.3 EDAX analysis

Energy dispersive X‐ray spectra (EDAX) was performed to analyse the elemental composition of samples. The EDAX pattern of pure and surfactants‐aided (CTAB, SDS and TRITON X‐100) SnO2 nanoparticles (Fig. 4) confirms the presence of constituent elements (Sn and O) by the appearance of their respective signals.

Fig. 4.

Fig. 4

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EDAX spectra of pure and surfactants‐aided SnO2 nanoparticles: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

The percentage of elemental composition is given in Table 2.

Table 2.

EDAX analysis of pure and surfactants‐aided SnO2 nanoparticles

Sample Weight, % Total
Sn L O K
SnO2 (A1) 57.13 42.87 100
SnO2 :CTAB (A2) 57.97 42.03 100
SnO2 :SDS (A3) 58.81 41.19 100
SnO2 :TRITON (A4) 65.08 34.92 100
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4.4 UV‐SPECTRA analysis

The transmittance spectra of pure and surfactants‐aided SnO2 nanoparticles can be seen in Fig. 5. All samples showed transmission from 50 to 70% in the visible region and a strong decrease in transmittance below 440 nm was observed which is interrelated to the optical band gap. In all cases, blue shifts were observed which were attributed to the smaller size of pure and surfactants‐aided (CTAB, SDS and TRITON X‐100) SnO2 nanoparticles [33, 34].

Fig. 5.

Fig. 5

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Transmittance spectra of pure and surfactants‐aided SnO2 nanoparticles: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

In semiconducting materials, the optical transitions took place by direct and indirect transitions. The absorption coefficient α of the material was expressed by the following relation [35]:

αhν=Ahν−Eg2

where A is an energy‐independent constant, E g is the optical band gap, for indirect allowed transition, n  = 2; for direct allowed transition, n  = 1/2. The (αhν)2 is plotted as a function of hν as shown in Fig. 6 which has a linear portion and the intercept of this linear portion on the energy axis gives the band gap. The calculated band gap energies for CTAB‐ and SDS‐aided surfactant SnO2 nanoparticles were larger than that of pure SnO2 nanoparticles [36] Table 3 which show a decrease in crystallite size [37, 38] as observed from the XRD analysis. However, the band gap energy was decreased with the addition of the TRITON X‐100 surfactant. The growth of surfactants‐aided SnO2 nanoparticles was restricted due to the effect of quantum confinement.

Fig. 6.

Fig. 6

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Plot of (αhν)2 vs. hν of pure and surfactants‐aided SnO2 nanoparticles: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

Table 3.

Band gap energy of pure and surfactants‐aided SnO2 nanoparticles

S. No. Sample Band gap energy, eV
1 SnO2 (A1) 3.487
2 SnO2 :CTAB (A2) 3.5774
3 SnO2 :SDS (A3) 3.507
4 SnO2 :TRITON (A4) 3.304
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4.5 Antibacterial activity

The pure and surfactants‐aided (CTAB, SDS and TRITON) SnO2 nanoparticles were tested for antibacterial activity against S. aureus (ATCC 29213) and E. coli (ATCC 25922) according to the agar diffusion method [39]. Sodium hydroxide was used for the uniform dispersion of the sample during the test. About 50 and 25 µl sample from pure and surfactants‐aided (CTAB, SDS and TRITON) SnO2 nanoparticles were taken for an antibacterial study: (i) 50 µl of samples, (ii) 25 µl of samples, (iii) 20 µl of NAOH and (iv) ampicillin disc.

The test was carried out to determine the zone of inhibition by pure tin oxide and surfactants‐aided (CTAB, SDS and TRITON) SnO2 nanoparticles. The zone of inhibition of pure tin oxide and surfactants‐aided (CTAB, SDS and TRITON) SnO2 nanoparticles against the S. aureus and E. coli is shown in Table 4 and Figs. 7 and 8. Pure tin oxide, tin oxide +CTAB and tin oxide +TRITON show good antibacterial activity against E. coli and the zone inhibition was greater than 0.2 cm in the 50 µl sample and no zone formation was observed in the 25 µl sample and a similar trend was observed in a S. aureus organism. All samples possess moderate antibacterial activity against S. aureus organism and zone of inhibition between 6.1 and 6.4 mm, respectively. The control sample (ampicillin disc) indicated positive antibacterial activity against E. coli bacteria.

Table 4.

Zone of inhibition of pure and surfactants‐aided SnO2 nanoparticles

Name of the sample E. coli, mm S. aureus, mm Ampicillin DISC, mm Control for NaOH (20 µl), cm
50 µl 25 µl 50 µl 25 µl E.coli S.aureus
SnO2 (A1) 6.0 — 3.0 — 3.00 — —
SnO2 :CTAB (A2) 6.1 0.2 3.0 0.1 — — —
SnO2 :SDS (A3) 6.4 — 4.0 — 7.00 — —
SnO2 :TRITON(A4) 6.2 — 3.0 — 3.05 — —
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Fig. 7.

Fig. 7

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Antibacterial activity of pure and surfactants‐aided SnO2 nanoparticles against E. coli: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

Fig. 8.

Fig. 8

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Antibacterial activity of pure and surfactants‐aided SnO2 nanoparticles against S. aureus: (A1) SnO2, (A2) SnO2 :CTAB, (A3) SnO2 :SDS, (A4) SnO2 :TRITON

Qamar et al. [40] demonstrated the antibacterial activity of cobalt‐doped tin oxide against E. coli (Gram‐negative) and Bacillus subtil is (Gram‐positive) organisms and zone of inhibition was greater than 16 mm against bacterial strains. Kumar and their team members [41] obtained high antibacterial activity in tin oxide nanoparticles against Pseudomonas aureginosa and S. aureus bacteria under the agar diffusion test method. Silver‐doped tin oxide nanoparticles indicated a positive antibacterial efficacy against S. aureus, Aeronomous hydrophila, Shigella flexineri and E. coli bacteria and a moderate activity was observed in pure tin oxide by John et al. [42].

5 Conclusion

The pure and surfactants‐aided (CTAB, SDS and TRITON X‐100) tin oxide nanoparticles were effectively synthesised using the co‐precipitation method. The XRD pattern confirmed the formation of the tetragonal rutile structure in pure and surfactants‐aided SnO2 nanoparticles. The crystallite size of SnO2 nanoparticles was found to decrease with the addition of the surfactants. The surfactant‐influenced particle growth and the size of nanoparticles were distributed in the range from 30 to 75 nm. Moreover, the size of SnO2 nanoparticles was decreased by the addition of the surfactants (CTAB and SDS). However, the size was increased in SnO2 nanoparticles aided by TRITON X‐100. An increase in band gap energy was observed in surfactants‐aided (CTAB and SDS) SnO2 nanoparticles (3.487, 3.57, 3.50 and 3.3 eV). The surfactants‐aided SnO2 nanoparticles showed positive antibacterial activities than that of pure SnO2 nanoparticles against S. aureus and E. coli bacteria.

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