AgI nanocomposite as an effective photocatalyst by co-precipitation method

    Simple synthesis and characterization of Ag 2 CdI4 /AgI2 nanocomposite as an effective photocatalyst by co-precipitation method Mojgan Ghanbari, Faezeh Soofivand, Masoud Salavati-Niasari PII: DOI: Reference:

S0167-7322(16)31129-1 doi: 10.1016/j.molliq.2016.07.117 MOLLIQ 6131

To appear in:

Journal of Molecular Liquids

Received date: Revised date: Accepted date:

7 May 2016 23 July 2016 25 July 2016

Please cite this article as: Mojgan Ghanbari, Faezeh Soofivand, Masoud Salavati-Niasari, Simple synthesis and characterization of Ag2 CdI4 /AgI2 nanocomposite as an effective photocatalyst by co-precipitation method, Journal of Molecular Liquids (2016), doi: 10.1016/j.molliq.2016.07.117

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ACCEPTED MANUSCRIPT Simple synthesis and characterization of Ag2CdI4/AgI2 nanocomposite as an effective photocatalyst by co-precipitation method

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Mojgan Ghanbari, Faezeh Soofivand, Masoud Salavati-Niasari *

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Iran

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Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, I. R.

* Corresponding author. Tel.: +98 31 55912383; Fax: +98 31 55913201; E-mail address:

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[email protected]

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ABSTRACT

In present study, silver cadmium tetraiodide/silver iodide (Ag2CdI4/AgI) nanocomposites have been synthesized

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successfully by simple co-precipitation method. The effect of Ag + molar ratio to Cd+2 and type of capping agent

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on morphology, size and purity of products was investigated. The obtained products were characterized by X-ray diffraction (XRD), field emission scanning and transmittance electron microscopy (FESEM, TEM), Raman and

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X-ray energy dispersive spectroscopy (EDS) analysis. The optical property of this product was studied by Ultraviolet–visible spectroscopy (UV-vis) and its band gap was estimated about 2.8 eV. Application of this product as photocatalyst through degradation of methyl orange (MO) under UV irradiation was investigated and degradation percentage of MO about 96.6 % after 100 min was calculated. Keywords: Nanocomposite; Ag2CdI4/AgI; Superionic conductors; Nanostructures; Photocatalyst. 1.

Introduction Tetraiodide compounds with general formula M2NI4 (M = Ag, Cu, Tl; N = Hg, Cd, Zn, Pb) have a wide variety

and many applications. Silver tetraiodo cadmate (Ag2CdI4) is one of these compounds that are classified in two categories: superionic compounds that are known as solid electrolytes and themochromic compounds that are sub-set of smart materials. Therefore Ag2CdI4 is a compound with binary roles: superionic [1, 2] and

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ACCEPTED MANUSCRIPT themochromism. Transition phase temperature in this compound is about 80 °C, as phase and color of it change at above this temperature [1].

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Solid electrolytes allow that the ions move without liquid media. The movement of small cations in these

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compounds causes the electrical conductivity of them [3, 4]. Superionic compounds are intermediate of crystal solids with ordered structure and liquid crystal without ordered structure that have mobile ions. These

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compounds are utilized as fuel cell, solid battery, supercapacitor, and various chemical sensors. Nowadays,

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environmental pollution has become a global crisis, so new energy sources such as solar cells and fuel cells have attracted much attention and various researchers have studied about preparation and improvement of these new

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energy sources. On the other side, synthesis and utilization of photocatalyst with high performance can be useful agent for preventing environmental concerns [5-8].

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Smart materials are designed materials that respond to environmental stimuli and they are named according to the type of stimulus and response [9]. Thermochromic materials are sub-set of this collection what can change its

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colour with changes in temperature as a stimulus, reversibly [10]. Recently, researchers have been focused on nanomaterials because of the properties of them is different from bulk materials. Synthesis engineering can be a new way for preparation of materials with desired characteristics and properties that can be done by changing of scale or preparation of new compounds such as composites. Composites are compounds that are made from two or more constituent that their characteristics are different from the individual components. Scientists and engineers have attracted much attention to nanocomposites due to their fascinating properties. Nanocomposites demonstrate good advantages over conventional materials and have many applications in various fields [11-14]. AgI is a thermochromism compound that is yellow at room temperature and its colour changes to red at above 147 °C. On the other hand, AgI is a superionic compound that its ionic conductivity is similar to liquid phase at phase transition temperature [15].

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ACCEPTED MANUSCRIPT By considering above statements, both of AgI and Ag2CdI4 are undergone a phase transition at specific temperature that their color and ion-conductivity change in this temperature. So, we decided to investigate phase

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transition temperature of Ag2CdI4/AgI nanocomposite. In this work, Ag2CdI4/AgI nanocomposites have been

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synthesized by simple in-situ co-precipitation method. The effect of various parameters such as different capping agents and molar ratio of Cd to Ag on morphology and purity of products were investigated. The products were

Experimental

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2.

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characterized by XRD, SEM, TEM, EDS, UV-vis and Raman spectroscopy.

2.1. Materials and characterization

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All the chemicals reagents used in our experiments were of analytical grade and were used as received without further purification. Cetyltrimethyl ammonium bromide (CTAB), sodium dodecyl-benzene-sulfonate (SDBS),

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and poly vinyl pyrrolidone (PVP-40000) were purchased from Merck. GC-2550TG (Teif Gostar Faraz Company, Iran) were used for all chemical analyses. The XRD of products was recorded by a Rigaku D-max C

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III XRD using Ni-filtered Cu Kα radiation. SEM images were obtained on Philips XL-30ESEM equipped with an energy dispersive X-ray spectroscopy. The EDS analysis with 20 kV accelerated voltage was done. 2.2. Synthetic procedure

Ag2CdI4/AgI nanocomposites were synthesized by in-situ co-precipitation method from aqueous solutions of Cd (NO3)2.2H2O, AgNO3, and LiI. 2 H2O as starting materials. In this work, the different parameters such as: molar ratio of Ag+ to Cd+2 and type of capping agent were changed and the products were analyzed by various techniques. At the first: AgI yellow-precipitation was prepared from 0.1 g AgNO3, and 0.07 g LiI. 2H2O in 50 ml of distilled water, then the certain amount of capping agent was added to the above solution. Therefore, CdI2 whiteprecipitation was obtained from Cd (NO3)2. 2 H2O with stoichiometric amount of LiI. 2 H2O (by considering the desired molar ratio of Ag + to Cd +2 in different experiments). Finally, the solution consists of AgI was added to

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ACCEPTED MANUSCRIPT CdI2 solution and was heated in 90 °C for drying and collecting the as-prepared product. The various experiments were applied to find the optimum condition; details of experiments were illustrated in Table 1. Result and discussion

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3.

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To provide typical histogram of the particle diameters, the average particle diameters of samples 1- 3 were estimated from the SEM images by Digimizer software. As shown in Fig. 1, the particle size distribution of the

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samples no. 1- 3 is observed in the range of 0-100 nm. This histogram shows that homogeneity of sample 2 and 3

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is higher than sample 1 and the most of particles are in range of 20-40 nm. Fig. 2 (a- c) reveals SEM images of the samples synthesized by co-precipitation method and without capping

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agent. The SEM image of sample 1 shows that in addition to nanoparticles, micrometer-sized structures were produced (Fig. 2a). Fig. 2b shows SEM image of sample 2, the size of particles is less than 40 nm and

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homogeneity in this sample is high. As shown in Fig. 2c, fine particles and the agglomerated particles were obtained in this condition (SEM image of sample 3). The average size of particles in sample 3 is about 20 nm.

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The phase, information on unit cell dimensions, and composition of the samples synthesized with different molar ratio of Ag +/Cd +2 were determined by XRD. The XRD patterns of sample 1- 3 were given in Fig. 3 (a- c), respectively. Fig. 3a is XRD pattern of sample 1 which molar ratio of Ag +1 to Cd +2 is 2: 1. In this pattern, three phases are shown, including Ag2CdI4 (JCPDS card No. 36-1211), CdI2 (JCPDS card No. 02-1200), and AgI (JCPDS card No. 01-0503). Fig. 3b, and c show XRD patterns of Ag2CdI4/ AgI nanocomposites prepared by molar ratio of Ag+/Cd+2 = 1 (sample 2) and 0.5 (sample 3), respectively. In both of patterns, black triangle and blue circle are indicators of Ag2CdI4 with tetragonal phase (JCPDS card No. 21-1074) and AgI with cubic phase (JCPDS card No. 01-0503), respectively. The high crystallinity of these products confirms by high intensity of the reflection peaks. The crystallite size of the samples 1-3 was calculated by Scherrer equation [16] and was estimated about 18, 13, and 11 nm, respectively.

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ACCEPTED MANUSCRIPT Fig. 4 illustrates SEM images of sample prepared in the presence of different capping agents including CTAB, SDS, Triplex, NaHSal, and PVP. The SEM images of the samples 4-8 show in Fig. 4 (a- e), respectively. Fig. 4a

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shows the SEM images of Ag2CdI4/AgI nanocomposites synthesized in presence of CTAB (sample 4), this

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nanocomposite consists of unknown microstructures with a small amount of nanoparticles. The used capping agent of sample 5 is SDS and the particle size of this sample is about 20 nm but particles are aggregated (Fig.

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4b). SEM image of sample 6 was given in Fig. 4c, as shown in this figure; 20 nm-sized agglomerated particles

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were produced. NaHSal is a ligand that is used as a capping agent, SEM image of sample synthesized by NaHSal as capping agent shows in Fig. 4d. The average particle size of this sample is about 15 nm. In Fig. 4e, the

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uniform particles with size about 10 nm are shown that related to SEM image of sample 8. PVP is a polymeric capping agent that was used for preparation of Ag2CdI4/ AgI nanocomposites in sample 8.

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The XRD patterns of samples 4- 8 are demonstrated in Fig. 5 (a- e), respectively. The peaks of Ag2CdI4, AgI, Na, and unknown phases indexed with black triangle, blue circle, green diamond, and purple square,

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respectively. The XRD pattern of sample 4 (Fig. 5a) illustrates an amorphous basis that can be related to lowcrystalliniy of this sample and the diffraction-lines that can be indexed to tetragonal phase of Ag2CdI4 (JCPDS card No. 36-1211). Fig. 5b, c and d show XRD patterns of Ag2CdI4/ AgI nanocomposites synthesized in presence of SDS, Triplex, and NaHSal as capping agents, respectively. In patterns of sample 5 (Fig. 5b), sample 6 (Fig. 5c) and sample 7 (Fig. 5d), in addition to Ag2CdI4 (47-0870, hexagonal phase for Triplex and NaHSal; 21-1073, tetragonal phase for SDS) and AgI (09-0374, hexagonal phase for SDS and NaHSal; 01-0503, cubic phase for SDS), diffraction lines of Na (JCPDS card No. 01-0850) are shown that can be related to Na ions of capping agents SDS, Triplex, and NaHSal. In Fig. 5c, besides of the diffraction lines that are related to Ag2CdI4, Na and AgI can be shown the other diffraction lines that been unknown. In XRD pattern of sample 8 that was given in Fig. 5e diffraction lines of nanocomposite components including Ag2CdI4 (JCPDS card No. 21-1074),

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ACCEPTED MANUSCRIPT AgI (JCPDS card No. 09-0374) and an amorphous basis that can be indexed to polymeric structure of PVP are shown.

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Fig. 6 (a-c) depicts TEM images of the as-prepared Ag2CdI4 nanostructures (sample no. 2) in various scale

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200, 100, and 50 nm, respectively. The average size of these nanoparticles is estimated about 30 nm. High resolution TEM imaging also helped us to identify the sample that looked like consists of more than one

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component (the area indicated by brighter lines and darker lines).

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The HRTEM images of sample 2 are shown in Fig. 7. These images indicate interplanar spacing of 0.156 nm and 0.221 nm which corresponds to the (4 0 0) plane of the cubic structure of AgI (JCPDS = 01-0503) and (2 0 4)

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plane of the tetragonal structure of Ag2CdI4 (JCPDS = 21-1074), respectively. Therefore, the HRTEM images confirm the preparation of Ag2CdI4/ AgI nanocomposite and existence both of AgI and Ag2CdI4 in this product

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(sample 2).

Fig. 8 indicates the EDS spectrum of the Ag2CdI4/ AgI nanocomposite obtained from the sample 2. In this

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spectrum, the peaks of Ag, Cd, and I elements were detected. The other peaks were not detected in this spectrum, so purity of the as-prepared product was confirmed. In order to make a complete vibrational assignment of the modes of Ag2Cdl4, Raman spectrum at the room temperature of sample 2 was given in Fig. 9. In this spectrum, six bands at 25.58, 33.47, 38.4, 87.18, 105.93, and 137.9 cm-l are shown. The vibrational modes can be assigned by considering Ag2CdI4 as consisting of the vibrational modes of AgI and (CdI4)-2. The intense band at 137.9 cm-1 is assigned to the “A” symmetric stretch of the (HgI4)-2 species [17]. Raman shift values of Ag2CdI4 nanostructures synthesized in this work compared to Raman shift values of Ag2CdI4 prepared in former works [1] have blue-shift that can be related to a phonon confinement effect and the strain caused by decreasing size of nanoscale materials [18]. The 80-110 cm-1 region consists of two bands at the positions 87.18 cm-1 and 105.93 cm-1 at room temperature. It is known from the

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ACCEPTED MANUSCRIPT Raman spectra of silver ion conductors that this region consists of mostly Agl [19] stretching modes. Hence, in Ag2Cdl4 also the bands in this region can be assigned to symmetric stretching modes of AgI.

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Fig. 10a shows the UV-vis absorption spectrum of the as-prepared Ag2CdI4 nanostructures (sample 2). In this spectrum an absorption peak around 328 nm can be observed. Optical band gap (Eg) may be evaluated base on

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the optical absorption spectrum using the following equation [20]: (Ahυ)n = B(hυ-Eg); Where hυ is the photon

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energy, A is absorbent, B is a material constant and n is 2 or 1/2 for direct and indirect transitions, respectively.

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The optical band gap for the absorption peak is obtained by extrapolating the linear portion of the (Ahυ) n curve versus hυ to zero. No linear relation was found for n = 1/2, suggesting that the prepared Ag2CdI4 nanostructures

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are semiconductor with direct transition at this energy. The band gap of as-prepared Ag2CdI4 nanostructures was calculated about 2.8 eV (Fig. 10b). The calculated band gap confirms that this compound can be used as an

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effective photocatalyst.

The various samples with different size and components were studied by DRS spectroscopy and their band gap

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was estimated by Tauc plot and the results are shown in Fig. 11. As shown, band gap depends on size and components of materials. Band gap of Ag2CdI4/AgI nanocomposites with Na (samples 5 and 7); Ag2CdI4 nanostructures (sample 4) and Ag2CdI4/AgI/CdI2 nanocomposite (sample 1) were calculated about 3.4, 3.9 and 2.9 respectively. Hence can be said that band gap of materials can be affected by their components. The photocatalytic activity of Ag2CdI4 nanoparticles was investigated by monitoring the degradation of methyl orange solution (MO) dye under UV light irradiation (Fig. 12). The photocatalytic degradation reaction was performed out in a quartz photocatalytic reactor and carried out with a 10 ppm MO solution containing 0.05 g of photocatalyst (Ag2CdI4 nanoparticles, sample 2). This mixture was aerated for 30 min to reach adsorption equilibrium. Then, the mixture was placed inside the photoreactor in which the vessel was 40 cm away from the UV of 400 W Osram lamp. The quartz vessel and light sources were placed inside a black box equipped with a

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ACCEPTED MANUSCRIPT fan to prevent UV leakage. The experiments were performed at room temperature and pH of the MO solution was adjusted 3– 4. The MO degradation percentage was calculated by Eq. (1) as follows: (1)

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D.P. (t) = (A0-At)/A0 ×100

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where A0 and At are the absorbance value of MO solution at 0 and t min, respectively [21-26]. According to photocatalytic calculations by Eq. (1), the MO degradation percentage was about 96.6% after 100

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min irradiation of UV light in presence Ag2CdI4 nanoparticles as photocatalyst.

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It is well known that photocataltic activity has close relation with composition of nanocomposites. Hence, should evaluate photocatalytic activity of different samples prepared in different conditions was evaluated. By

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considering XRD patterns of samples can be seen that two nanocomposites Ag2CdI4/ AgI and Ag2CdI4/CdI2/AgI were synthesized, so performance of these composites was investigated. On the other hand, the photocatalytic

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activity of samples with different morphology and size was studied, because of these parameters can be influenced on activity of nanostructures. The curve of MO degradation versus time were given in Fig. 13 and the

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results show that the photocatalytic activity of sample 5 is more than the others and the photocatalytic activity of sample 1 is lower than the others. Hence, can be said that photocatalytic performance of Ag2CdI4/AgI nanocomposite is higher than Ag2CdI4 nanostructures and the photocatalytic performance of Ag2CdI4 nanostructures is higher than Ag2CdI4/CdI2 nanocomposite. 4.

Conclusions

Ag2CdI4/ AgI nanocomposites have been successfully synthesized by simple, eco-friendly, inexpensive and low temperature method in presence of different salts as starting materials. The reaction conditions in this method are very easy to control. The molar ratio of Ag+/Cd+2 and type of capping agent can be influenced on components, purity and size of nanocomposites. Therefore, the various experiments were done and the optimum condition was found. The properties of products were characterized by FESEM, XRD, TEM, EDS, and Raman spectroscopy. The optical property of this product was studied by UV-vis and its band gap was calculated about

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ACCEPTED MANUSCRIPT 2.8 eV. The calculated band gap confirms that of Ag2CdI4 nanoparticles can be used as an effective photocatalyst. To investigate the photocatalytic properties of this product, photo-oxidation of methyl orange

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(MO) was performed. The photocatalytic test shows that the methyl orange degradation was about 96.6 % after

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100 min irradiation of UV light. Acknowledgements

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Authors are grateful to the council of Iran National Science Foundation and University of Kashan for supporting

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this work by Grant No (159271/354).

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ACCEPTED MANUSCRIPT References [1] R. Sudharsanan, T. K. K. Srinivasan, S. Radhakrishna, Solid State Ionics 13 (1984) 277.

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[2] I. Karbovnyk, S. Piskunov, I. Bolesta, S. Bellucci, M. Cestelli Guidi, M. Piccinini, E. Spohr, A. I. Popov,

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Eur. Phys. J. B 70 (2009) 443. [3] S. Hull Superionics, Rep. Prog. Phys. 67 (2004) 1233.

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[4] N. Saba, A. Ahmad, Anal. Bioanal. Electrochem. 3 (2011) 521.

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[5] N. Zhang, M. Q. Yang, S. Liu, Y. Sun, Y. J. Xu, Chem. Rev. 115 (2015) 10307. [6] S. Liu, Z. R. Tang, Y. Sun, J. C. Colmenares, Y. J. Xu, Chem.Soc.Rev. 44 (2015) 5053.

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[7] C. Han, M. Q. Yang, B. Weng, Y. J. Xu, Physical Chemistry Chemical Physics 16 (2014) 16891. [8] F. Motahari, M. R. Mozdianfard, F. Soofivand, M. Salavati-Niasari, RSC Advances 4 (2014), 27654.

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[9] P. Bamfield, G. Hutchings Michael, Chromic Phenomena; technological applications of colour chemistry. Royal Society of Chemistry, Cambridge, 2010. ISBN 978-1-84755-868-8.

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[10] P. Kiri, G. Hyett, R. Binions, Adv. Mat. Lett. 1 (2010) 86. [11] M. Masjedi-Arani, M. Salavati-Niasari, J. Mater. Sci.: Mater. Electron. 26 (2015) 2316. [12] M. Mousavi-Kamazani, M. Salavati-Niasari, Composites: Part B 56 (2014) 490. [13] F. Soofivand, M. Salavati-Niasari, RSC advances 5 (2015) 64346. [14] K. Siraj, R. Rafiuddin, International Journal of Chemistry 3 (2011) 174. [15] E. A. Secco, M. G. Usha, Solid State Ion. 68 (1994) 213. [16] R. Jenkins, R. L. Snyder, Introduction to X-ray Powder Diffractometry. John Wiley & Sons Inc., 1996. [17] J. E. D. Davies, D. A. Long, J. Chem. Soc. A (1968) 2564. [18] C. Y. Xu, P. X. Zhang, L. Yan, J. Raman Spectrosc. 32 (2001) 862. [19] G. L. Bottger, A. L. Geddes, J. Chem. Soc. A (1968) 2054. [20] J. Tauc, Materials Research Bulletin 3 (1968) 37.

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ACCEPTED MANUSCRIPT [21] F. Soofivand, F. Mohandes, M. Salavati-Niasari, Materials research bulletin 48 (2013) 2084. [22] D. Ghanbari, M. Salavati-Niasari, S. Karimzadeh, S. Gholamrezaei, Journal of NanoStructures 4, 227

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(2014).

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[23] G. Nabiyouni; S. Sharifi; D. Ghanbari; M. Salavati-Niasari, Journal of NanoStructures 4, 317 (2014).

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[24] M. Panahi-Kalamuei, M. Mousavi-Kamazani, M. Salavati-Niasari, Journal of NanoStructures 4, 459

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(2014).

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[25] F. Beshkar; M. Salavati-Niasari, Journal of NanoStructures 5, 17 (2015) [26] L. Nejati-Moghadam; A. Esmaeili Bafghi-Karimabad; M. Salavati-Niasari; H. Safardoust, Journal of

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NanoStructures 5, 47 (2015).

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ACCEPTED MANUSCRIPT Figure caption: Fig. 1. Particle size distribution Histogram of sample no. 1, 2, 3.

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Fig. 2. SEM image of sample no. (a) 1, (b) 2, and (c) 3.

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Fig. 3. XRD pattern of sample no. (a) 1, (b) 2, and (c) 3. Fig. 4. SEM image of sample no. (a) 4, (b) 5, (c) 6, (d) 7, and (e) 8.

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Fig. 5. XRD pattern of sample no. (a) 4, (b) 5, (c) 6, (d) 7, and (e) 8.

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Fig. 6. TEM images at scale 200 (a), 100 (b), and 50 (c) nm of sample no. 2. Fig. 7. HRTEM images of sample no. 2 at scale 2 nm.

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Fig. 8. EDS spectrum of samples no. 2. Fig. 9. Raman spectrum of sample no. 2

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Fig. 10. (a) UV–vis spectrum, (b) curve (Ahυ)n versus hυ of sample no. 2.

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Fig. 11. (a) UV–vis spectrum, (b) curve (Ahυ)n versus hυ of samples 4, 7, 5 and 1.

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Fig. 12. Degradiation of MO under UV irradiation in presence sample no. 2 as photocatalyst. Fig. 13. Degradiation of MO under UV irradiation in presence samples 4, 7, 5 and 1 as photocatalyst. Table 1. The preparation conditions of sample no. 1-8.

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Fig. 1.

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Fig. 12.

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99.33%

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sample 7

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sample 4 sample 5

34.50%

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Degradation Percent (%)

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SCHEME 1

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Table 1. Ag+: Cd+2 molar ratio

Type of capping agent

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1

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0.5

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1

CTAB

Ag2CdI4 (low crystallinity)

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1

SDS

Ag2CdI4, AgI, Na

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Sample no.

Produced product Ag2CdI4, CdI2, AgI Ag2CdI4, AgI Ag2CdI4, AgI

Ag2CdI4, AgI, Na, Unknown phases

NaHSal

Ag2CdI4, AgI, Na

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Ag2CdI4 (low crystallinity)

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Triplex

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Highlights Herein, for the first time Ag2CdI4/AgI nanocomposites were synthesized by co-precipitation.

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The effects of Ag+/Cd+2 molar ratio, and type of capping agent, size and purity were investigated.

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Various analysis results show that Ag2CdI4/AgI nanocomposites were synthesized successfully.

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Application of Ag2CdI4/AgI nanocomposites as a photocatalyst was investigated through degradation.

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