Hydrothermal synthesis, characterization and optical properties of 3D flower like indium sulfide nanostructures

Superlattices and Microstructures 53 (2013) 76–88

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Hydrothermal synthesis, characterization and optical properties of 3D flower like indium sulfide nanostructures Parvaneh Ghaderi Sheikhi abadi a, Masoud Salavati-Niasari a,⇑, Fatemeh Davar b a b

Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167, Islamic Republic of Iran Department of Inorganic Chemistry, Faculty of Chemistry, Razi University, Kermanshah, Islamic Republic of Iran

a r t i c l e

i n f o

Article history: Received 19 June 2012 Received in revised form 1 September 2012 Accepted 13 September 2012 Available online 12 October 2012 Keywords: Nanostructure Indium sulfide Hydrothermal Semiconductor 3D structure

a b s t r a c t High-quality and high-yield 3D flower like indium sulfide (In2S3) nanostructures with cubic structure were synthesized by a wet chemical route, without using any surfactant and organic solvents at 160 °C for 12 h, by using InCl3 and 2-aminothiophenol (2-ATP) as starting reagents. The obtained In2S3 with different morphologies and size was characterized by X-ray diffraction pattern (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and ultraviolet–visible (UV–vis) spectroscopy. The effects of reaction parameters, such as temperature, precursor concentration and reaction time on the morphology, and particle size of products were investigated. Our experimental results showed that temperature and time reaction played key roles in the final morphology of In2S3. The morphology of In2S3 structures could be changed from one-dimensional (1D) structures to three-dimensional (3D) structures by increasing reaction time to 24 h. In the present study the optical properties 3D In2S3 structures were investigated. Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction Over the past decades, there has been increasing interest in III–VI Semiconductor materials due to their novel properties and their potential applications in electronic and optoelectronic devices manufacturing. As an important semiconductor, indium sulfide (In2S3) is a promising material with optoelectronic properties [1], optical properties [2,3], electronic properties [4], photovoltaic material [5], ⇑ Corresponding author. Tel.: +98 3615912383; fax: +98 3615552930. E-mail address: [email protected] (M. Salavati-Niasari). 0749-6036/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved. http://dx.doi.org/10.1016/j.spmi.2012.09.003

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useful photoconducting material [1,2], acoustic properties and semiconductor sensitization [6]. Generally, indium sulfide has two kinds of composition forms, InS and In2S3, with band gaps of 2.44 eV [7] and 2.00–2.20 eV [8], respectively. Between these two compounds, most of the research works have been focused on In2S3. It is known to crystallize in three polymorphic forms as a function of temperature [9–11] e.g. a defective cubic structure called a-In2S3 (stable up to about 693 K), a defective spinel structure called b-In2S3 (stable up to about 1027 K) and a higher temperature layered structure, the c-form (above 1027 K). The b-phase of In2S3 is known to be an n-type semiconductor, is generally found to be stable or metastably persistent at room temperature. It is considered to be a promising photoconducting material for photovoltaic cell design. In order to improve the solar energy conversion in a ZnO/CuInS2 heterojunction indium sulfide is used as buffer layer replacing toxic CdS [12]. Besides, it has applications for preparation of green and red phosphors for the manufacture of picture tubes for color televisions [13], dry cells [3], and heterojunction for use in photovoltaic electric generators [5]. In2S3 nanoparticles can also have medical applications as bioconjugates for cancer diagnosis [14,15]. So far, various morphologies and architectures In2S3 nanostructures have been reported, such as nanoparticles [13,16,17], dendrites [18–20], dendritic patterns [18], hollow nanospheres [21], nanowires and micro- and nano-rods [22–25], films [26,27], nanosheets [28], bulk powder [5,13,27], 3D Flowerlike Structures [29], nano-flake structures [30], and urchin-like nanostructures [31]. Many efficient techniques were developed for preparing semiconductor microand nano-size In2S3, mainly including microwave route [20], Sonochemical method [32], hydrothermal and solvothermal method [13,28], precipitation [16], solvent-reduction route [17], metal-organic chemical vapor deposition approach [23], oxidization–sulfidation growth route [18], thermal decomposition [33], a direct reaction of the elements in a quartz container at a high temperature [34], the laser-induced synthesis [35] and so on. The hydrothermal technique is a wet chemical process that has been widely utilized to prepare inorganic nanomaterials at temperatures usually below 220 °C [36–45]. It not only can induce the formation of well-crystallized products at low temperatures, but also can control the shape and size of the resultant products simply through adjusting the synthesis conditions including composition of the solution, temperature and duration, etc. [36]. Herein, we present a one-step hydrothermal treatment for the formation In2S3 structures with various morphologies for example microspheres, rod-like, nanocubics, and flower-like structures which is milder, simpler, more practical, and more environmentally friendly method than other methods. The trick in hydrothermal synthesis of In2S3 structures presented here is the using of 2-aminothiophenol (2-ATP) as a sulfur source and stability agent. 2. Experimental 2.1. Materials and physical measurements All the chemicals were of analytical grade and were used and received without further purification. We chose InCl3 as indium source, 2-aminothiophenol (2-ATP) as sulfur sources. XRD pattern were recorded by a Rigaku D-max C III, X-ray diffractometer using Ni-filtered Cu Ka radiation. Scanning electron microscopy (SEM) images were obtained on philips XL-30ESEM equipped with an energy dispersive X-ray spectroscopy. Transmission electron microscopy (TEM) images were obtained on a Philips EM208 transmission electron microscopy with an accelerating voltage of 100 kV. Fourier transform infrared (FT-IR) spectra were recorded on Shimadzu Varian 4300 spectrophotometer in KBr pellets. The electronic spectra of the complexes were taken on a Shimadzu UV–vis scanning spectrometer (Model 2101 PC). 2.2. Synthesis of 3D flower-like In2S3 nanostructures In a typical experiment, 0.1 g (4.36  10 4 mol) of InCl3 was dissolved in distilled water (40 ml) under stirring. In a separate beaker, 0.14 ml (1.31  10 3 mol) 2-ATP was dissolved in 10 ml absolute ethanol and added drop wise to InCl3 solution at ambient temperature under magnetic stirring. The final yellow colloidal solution was transferred to a 60 ml Teflon-line stainless steel autoclave.

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Table 1 Products obtained under different hydrothermal conditions. Sample no.

Temperature (°C)

Reaction time (h)

Molar ratio In:S

In2S3 (mol)

I

160

12

1:1

4.36  10

4

4.37  10

4

Nanocubic

II

160

12

1:3

4.36  10

4

1.31  10

3

Microspheres + nanoflakes

III

160

12

1:5

4.36  10

4

2.18  10

3

Microspheres

IV

110

12

1:3

4.36  10

4

1.31  10

3

Amorphous

V

140

12

1:3

4.36  10

4

1.31  10

3

Microspheres + nanoflakes

VI

180

12

1:3

4.36  10

4

1.31  10

3

Nanoflower

VII

160

4

1:3

4.36  10

4

1.31  10

3

Spheric + rod-like

VIII

160

18

1:3

4.36  10

4

1.31  10

3

Amorphous

IX

160

24

1:3

4.36  10

4

1.31  10

3

Nanoflower

2-ATP (mol)

Morphologies of the products

SEM images

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The autoclave was sealed and maintained at 160 °C for 12 h in a digital temperature-controlled oven. After thermal treatment, the autoclave was cooled to room temperature and the resulting reddish orange precipitate was collected, filtered, and washed with distilled water and absolute ethanol for several times to remove impurities and the unreacted chemicals, and finally dried in vacuum oven at 60 °C for 5 h. A series of further experiments were carried out to investigate the reaction conditions. Detailed reaction conditions and the corresponding results are summarized in Table 1. 3. Results and discussion Our study demonstrates that 3D flower-like In2S3 structure can be synthesized by addition of 2-ATP into InCl3 solution at ambient temperature and by this facile one-pot hydrothermal treatment. The influence of the experimental conditions such as temperature, reaction time, and 2-ATP concentration on the morphology were investigated. Scheme 1 shows the influence of hydrothermal treatment. 3.1. Phase and structure of the products By XRD analysis the phase, crystalline change, and purity of the as-obtained products were characterized. Fig. 1 shows the typical XRD pattern of the sample prepared at 160 °C for 12 h. The XRD pattern exhibits multiple intense peaks that are clearly distinguishable. All the reflection peaks can be

Scheme 1. The influence of hydrothermal treatment.

Fig. 1. XRD pattern of as-prepared Cubic b-In2S3 at 160 °C for 12 h (sample II).

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indexed to the cubic b-In2S3, with calculated lattice parameters of a = 10.74 Å, which agree well with the reported values for b-In2S3 (JCPDS Card No. 65-0459) [21,46–48]. No peaks attributable to InS, In2O3, and InCl3 were observed. The strong and sharp reflection peaks suggest that the as-synthesized products are well crystallized. 3.2. Morphology and composition of the products Controlling the shape, size, and structure of inorganic nanomaterials is of fundamental importance, because of the strong correlation between these parameters and physical/chemical properties [49– 51]. The external and internal morphologies and size of the obtained products under different conditions were characterized by SEM and TEM. The mainly SEM and TEM images in my work indicate that the obtained products are mainly composed of 3D structures. Series of reaction parameters were investigated for a better understanding of the crystal growth mechanism. The SEM and TEM images (Fig. 2a–h) show that the morphology of products obtained at 160 °C for 12 h. When the values of 2-ATP was 4.37  10 4 mol, nanocubics In2S3 were appeared with an approximate size of 200–600 nm in diameters (Fig. 2a). With increase in values 2-ATP to 1.31  10 3 mol the microspheres In2S3 nanoflakes were appeared with good monodispersity (Fig. 2b–d). If the values of 2-ATP was high (2.18  10 3 mol) microspheres with coarse surfaces obtained (Fig. 2f–h). The morphologies and microstructures of the as-prepared cubic b-In2S3 were further investigated using TEM. Fig. 2e displays TEM images of the as-prepared cubic b-In2S3 via the hydrothermal process (sample II). The TEM image demonstrates expressly that the obtained products have microstructures of flower like. The flower petals exhibited a thickness of about 15–20 nm. Briefly, if the dosage of 2-ATP was increased, there would be not appropriate in the solution to growth the microspheres In2S3 nanoflakes. Thus the growth of the flowery nanostructures was inhibited and spherical particles with coarse surfaces came into being in a broad size range. When the raw materials react at 110 °C for 12 h, no there are any flower like patterns (Fig. 3a). If the reaction proceeds at 140 °C and 160 °C, more microspheres with the porous surfaces in narrow size range and connected each other (Figs. 3b–d and 2b–d). When heating up to 180 °C 3D flower like nanostructures were observed (Fig. 3e and f). When the raw materials react for 4 h it seems that several nanorods grow out of the surface of the spherical nanocore (Fig. 4a and b). as reaction time proceeds to 12 h the small nanorods disappear and microspheres In2S3 nanoflakes are obtained (Fig. 2b–d). As time proceeds to 18 h microspheres disappear (Fig. 4c) and in the 24 h composite is composed of 3D microstructures and some leaf-like nanopatches growing on the 3D microstructures (Fig. 4d and e). The microspheres nanoflakes structures were presumed to be the intermediate states of spherical rod-like to flower patterns. The flowers formed through the crystallization of the aggregates that fused gradually into one crystal. The different morphology under various experimental conditions the as-prepared cubic b-In2S3 via the hydrothermal process was shown in Scheme 2. 3.3. FT-IR analysis To investigate whether the surface of the nanoparticles was capped with organic surface the FT-IR of the as-synthesized samples were performed. The FT-IR spectrum of the pure 2-ATP [52], the mother solution, and synthesized products at room temperature shows in Fig. 5a–c, respectively. For pure 2-ATP (Fig. 5a), the band at 2524 cm 1 corresponds to the SAH stretch vibration, and 1306 and 1088 cm 1 is related to the CAN and CAS stretching respectively. The peaks at 1610 and 1480 cm 1 are C@C stretching vibrations. The peak at 3359 and 3448 cm 1 are symmetrical stretching vibration of NAH. However, FTIR spectrum of the mother solution (Fig. 5b) does not show any obvious evidence in the SAH vibration mode range, which proves that the 2-ATP are bound to the InCl3 through sulfide group, (the disappears of SAH peaks and the presence of C@C, NAH, CAN and CAS in Fig. 5b can prove the explanation above). The Fig. 5c was shown FT-IR spectrum of the microspheres In2S3 nanoflakes (sample II). Since the curve under this conditions has no absorption peaks in the range of 4000– 500 cm 1, so pure In2S3 sample was synthesized without any impurities.

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Fig. 2. SEM and TEM images of In2S3 prepared at 160 °C for 12 h with molar ratio of In:S; (a) 1:1, (b–e) 1:3, and (f–h) 1:5.

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Fig. 3. SEM images of prepared In2S3 with molar ratio (In:S; 1:3) for 12 h in: (a) 110 °C, (b–d) 140 °C and (e and f) 180 °C.

3.4. Optical properties We carried out UV–vis absorption spectra to investigate the optical properties of the cubic b-In2S3 structures. Dispersed ethanol solutions of In2S3 had a slight yellow color. Fig. 6 shows UV–vis absorption spectra of microspheres In2S3 nanoflakes (sample II). There is a strong and broad absorption peak centered at about 255 nm, those of the microspheres In2S3 nanoflakes was blue-shifted compared with the reported data of 620.6 nm for In2S3 bulk materials [1,2], which could be attributed to the quantum confinement of the excitonic transition for microspheres In2S3 nanoflakes structures, which allowed to be utilized as promising materials for quantum electronic.

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Fig. 4. SEM images of prepared In2S3 in 160 °C with molar ratio (In:S; 1:3) for: (a and b) 4 h, (c) 18 h, and (d and e) 24 h.

Fig. 7 shows the UV–vis absorption spectra of In2S3 nanostructures with difference morphologies recorded [53,54,29]. Fig. 7a consists of the UV–vis spectra for In2S3 dandelion flowers, that these were blue-shifted. The blue shift in absorption edge for organic mediated sample (Fig. 7a1) in comparison with water mediated sample (Fig. 7a2) may be due to the small petal size and different particle morphology [53]. Fig. 7b indicates of the UV–vis spectra for hollow In2S3 nanospheres and In2S3 nanospheres. A much more intense absorption band between 318 and 512 nm (Fig. 7b2) is observed in hollow In2S3 nanospheres while it is not seen in In2S3 nanospheres (Fig. 7b1), which can be contributed to the narrow size distribution and good crystal quality of hollow In2S3 nanospheres [54]. Fig. 7c shows two representative UV–vis absorption spectra of before (Fig. 7c1) and after (Fig. 7c2) heat treatment In2S3 samples, whose peaks are located at 395 nm (3.14 eV) and 440 nm (2.82 eV), respectively. Interestingly, there was a difference between the UV–vis spectra of before and after heat

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Scheme 2. The different morphology under various experimental conditions.

treatment In2S3 flowerlike architectures, which was due to the different size and crystallinity of particles between the two products [29]. Therewith, the morphology effect on the optical properties Sb2S3, CdS, and HgS nanostructure were observed [39,42,55]. It is reported that In2S3 nanostructures have prepared previously by Patra et al., Liu et al. and Cao and co-workers using microwave, hydrothermal and refluxed + hydrothermal synthesize in two steps reactions with longer times, respectively [20,21,56]. The synthesizes of reaction time and the number and type of precursors and solvents were not suitable. On the other hand, it is reported that In2S3 nanostructures have prepared previously by Datta and co-workers and Cao and co-workers using hydrothermal synthesize in presence two sources of sulfur [19,21], and it is reported that In2S3

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Fig. 5. FT-IR spectrum of (a) the pure 2-ATP, (b) the mother solution, and (c) as-synthesized products with 1.31  10 ATP for 12 h at 160 °C.

Fig. 6. UV–vis spectra of the cubic b-In2S3 (sample name II).

3

mol 2-

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Fig. 7. UV–vis absorption spectra of In2S3 nanostructures with difference morphologies [53,54,29].

nanostructures have prepared previously by Datta and co-workers, Fu et al. and Gao et al. using at ambient temperature synthesize and hydrothermal synthesize in longer time (7 days, 60 and 48 h, respectively) [19,30,57] and Datta et al. using hydrothermal synthesize in longer temperature (200 °C) [58]. Furthermore, previous researches have been mostly focused on the inorganic sulfides as sulfur sources. To the best of our knowledge, there is no report on the fabrication of In2S3 with 2-aminothiophenol (2-ATP). In this paper, we developed a hydrothermal method to synthesize In2S3 without any surfactant and toxicity solvent in 160 °C for only 12 h with difference morphologies (nanocubic, rod-like structures, microsphere and flower-like structures). 4. Conclusion In summary, we report a simple convenient and efficient method for the morphology control of In2S3 by a hydrothermal method at temperatures in the range of 110–180 °C by using indium chloride

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(InCl3) and 2-aminothiophenol (2-ATP) as starting reagents. XRD results reveal that the microspheres In2S3 nanoflakes are synthesized through hydrothermal method and the growth of the 3D structures does not need the participation of any templates and surfactant additives. The obtained products were characterized by XRD, FT-IR, SEM and TEM. Compared with the absorption peak of bulk In2S3 materials the as-prepared microspheres In2S3 nanoflakes were blue-shifted, which could be attributed to the quantum confinement of the excitonic transition for 3D structures. Acknowledgment Authors are grateful to the council of Iran National Science Foundation and University of Kashan for supporting this work by Grant No. (159271/33). References [1] [2] [3] [4] [5] [6] [7] [8] [9] [10] [11] [12] [13] [14] [15] [16] [17] [18] [19] [20] [21] [22] [23] [24] [25] [26] [27] [28] [29] [30] [31] [32] [33] [34] [35] [36] [37] [38] [39] [40] [41] [42] [43] [44] [45] [46] [47] [48] [49] [50]

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