Synthesis and Photocatalytic Performance of Cu Doped TiO2-CNT Nanocomposite Powder

Synthesis and photocatalytic performance of Cu doped TiO₂-CNT nanocomposite powder

Abstract: The nanocomposite TiO₂-CNT doped with Cu were synthesized by sol-gel method. The CNT content was fixed 10 wt.% with respect to the expected mass of TiO₂ and the amount of Cu in the sample was fixed and is equal to 1 atomic present. The samples were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM/EDS), differential thermal analysis (DTA), diffuse reflectance spectroscopy (DRS) and UV–visible absorption. DTA results showed calcination temperature was 400°C and at this temperature the structure was anatase with non-combustion of CNT in the nanopowder. XRD results showed the amorphous structure before calcination, Also presence of only crystalline TiO₂ anatase phase and CNTs after calcination. From the FESEM results indicate the synthesized sample a homogenous morphology with individual CNTs covered with TiO₂ and diameter of coated CNTs by TiO₂ can reach to about 50 nm. DRS results showed band gap in this sample compare to TiO₂ decreases from 3.2eV to 2.85eV. Finally, compared to pure TiO₂ nanoparticles, nanocomposite TiO₂-10 wt.% CNT and nanocomposite 1 at. % Cu doped TiO₂-10wt.% CNT exhibit higher catalytic activities in degradation of methylene blue (MB) under visible light. Degradation of 5 ppm of methylene blue solution by 1 at. % Cu doped TiO₂-10wt.% CNT with 0.4 g/L photocatalyst dose of substance and pH=7 can reach to 82 % after 60 min irradiation of visible light.

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Keyword: TiO₂-CNT-Cu,Synthesis, nanocomposite, sol-gel, photocatalytic, Methylene Blue.

1. Introduction

Water pollution is one of the main issues of environmental concerns. Large amount of industrial wastewaters are produced containing a wide variety of harmful organic contaminants such as synthetic dyes. Removal of dyes from wastewater is an important environmental issue [1]. Many methods including biodegradation, adsorption, and membrane process have been used to remove pollutants from wastewater [2]. In general, the conventional methods may not be very efficient, because the pollution transfer from one phase to another. However, advanced oxidation process by semiconductor photocatalytic process has shown a great potential as a low-cost, environmental friendly and sustainable treatment technology to oxidize harmful organic species to harmless water and carbon dioxide [3]. The main advantages are the possibility of complete destruction of pollution, recovery of photocatalysts, degradation of pollutants at mild conditions of temperature and pressure, using natural sunlight as irradiation source and hence low operating cost [4].

Different types of semiconductors such as metal oxides and sulfides have been examined as photocatalysts. The most commonly studied semiconductors include TiO₂, ZnO, WO₃, Fe₂O₃, ZnS and FeS [5,6]. Titanium oxide (TiO₂), with a wide bandgap of 3.2 eV, has received considerable attention due to its availability, nontoxicity, low-cost, physical and chemical stability and unique electronic and optical properties [7,8]. TiO₂ has three different crystalline structures of anatase (tetragonal), rutile (tetragonal) and brookite (orthorombic). Thermodynamically, rutile is the most stable phase in atmospheric pressure, and other phases are semi-stable [9]. However, TiO₂ suffers greatly in fast electron-hole pair recombination and light absorption only in the ultraviolet (UV) region [10]. In recent years, there has been considerable progress to overcome these challenges by several methods such as optimization of powders morphology, doping of TiO₂ with metals and preparation of TiO₂ composites [11]. It is reported in literature that doping of TiO₂ with metals can suppress the recombination of charge carriers, thus improve its photocatalytic activity. In addition, the modification of TiO₂ by doping transition metals likes Cr, Zn, Ag and Cu can extend the absorption threshold towards the visible region [12-14]. Among these metals, Cu has drawn considerable attention, because of better effects on the improvement of photocatalytic performance of TiO₂ [15]. Previous studies have shown that 1%.at Cu doped in TiO₂ has best photocatalytic performance [16,17]. Cu doping to TiO₂ can reduce the band gap energy of this material and hence improve photocatalytic properties. On the other hand, carbon-related materials have been extensively studied for the catalytic applications either by serving as a supporting matrix to tailor the electronic or photonic properties of catalysts, or as catalyst by itself [18]. Particularly, CNT has been successfully used as a catalyst supporting due to their outstanding physical, chemical and electerical properties. In comparison with pure TiO₂, TiO₂-CNT composites (generally with 10-30wt.% CNT content) showed an enhanced photocatalytic effect on degradation of some organic compounds [10,19-20]. This is related to the extended visible light absorption, enhanced electron and hole pairs and boosted reactant adsorbability giving high reaction possibility [21]. TiO₂ has been prepared by various methods such as sol-gel [21], hydrothermal [22] and mechanical alloying [23]. Most of the literature states that pure TiO₂, Cu-doped TiO₂ and TiO₂-CNT composite nano powder can be prepared by sol-gel method [14,16,20]. The sol-gel method seems to be the most promising one as it offers different advantages. Materials with distinct properties being obtained by varying the synthesis conditions.

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To the best of our knowledge, there is one work has been reported on the production of a novel functional TiO₂ material by combining two different species of CNT and Cu [24]. In this work, a two-step process was used. Firstly the mesoporous TiO₂, synthesized by a sol-gel method from titanium isopropoxide precursor. Then it was combined with the CNT-Cu nanocomposites which was produced separately. Actually, the TiO₂ lattice has not been doped with Cu ion. To our knowledge, preparation of TiO₂-10 wt.% CNT doped with 1at.% Cu nanopowder by a one-step modified sol-gel simple method has not been reported yet. The aim of present work is to study the effect of combined effect of CNT and Cu doping on TiO₂ photocatalyst. A detailed understanding of the preparation process and of subsequent heat treatments is crucial in order to control the morphology and structure of the catalyst powder for the desired photocatalytic applications. Structure, morphology, optical and photocatalytic properties of Cu-doped TiO₂-10 wt.% CNT nanocomposite powder were investigated.

2. Experimental procedure

The materials used in this work are Tetrabutyl-orthotitanate (TBOT, Merck KGaA) as a titanium precursor, ethanol (EtOH, Merck KGaA) as a solvent, deionized water for hydrolysis, benzyl alcohol (BA, KOSDAQ Korea) as a surfactant, multi walled carbon nanotubes (MWCNTs, US Research Nanomaterials, inc., US) with the diameter of 20-30 nm and purity of >95% and Cu(NO₃)₂.3H₂O (Merck KGaA) as a Cu precursor. Three samples of pure TiO₂ powder (here after called TP sample), TiO₂-10wt.% CNT nano-composite powder (here after called TC sample) and 1 at. % Cu doped TiO₂-10wt.% CNT nano-composite powder (here after called TCC sample) were prepared by sol-gel method. A general flow chart for the preparation of TiO₂-based photocatalyst by sol-gel process is shown in Fig. 1. First, the hydrolysis solution was prepared by mixing distilled water with BA at 0 ˚C. Also, TBOT was dissolved into anhydrous ethanol. Then, this solution was added drop by drop to the hydrolysis solution under vigorous stirring and additionally stirred for one hour. The reaction was carried out using TBOT:BA:EtOH:H₂O molar ratio of 1:5:100:5. In this way, the pure TiO₂ sol was obtained. For the TiO₂-10 wt.%CNT nano-composite synthesis, the CNTs were firstly dispersed in EtOH with the assistance of ultrasonication for 10 minutes. This mixture was added first separately to the hydrolysis solution during the sol-gel reaction, as presented in the Fig. 1. In order to study the effect of Cu doping in the preparation of TiO₂-10 wt.% CNT nano-composite powder, an additional solution of Cu(NO₃)₂.3H₂O was dissolved in EtOH. This solution were added first separately to the hydrolysis solution during the sol-gel reaction, as presented in the Fig. 1. In this way, TiO₂ sol doped with 1 at.% Cu. After one hour of stirring to achieve hydrolysis and condensation, the precipitates were centrifuged for 5 minute at 5000 rpm. Finally, the resulting precipitate dried in air at room temperature for 24 hour and heat treated at 400 °C for 1 hour.

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Fig. 1. Flow chart for the preparation of TiO₂-based photocatalysts by sol-gel method.

X-ray Diffraction (XRD), Philips PW3040/60 X-ray diffractometer with Cu-K_α radiation, was used for the structural characterization. The average crystallite size of the samples was calculated by the Scherrer equation [25]:

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