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INVESTIGATION on the STRUCTURAL and OPTICAL PROPERTIES of Nio NANOFLAKES

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INVESTIGATION on the STRUCTURAL and OPTICAL PROPERTIES of Nio NANOFLAKES D. Abubakar, N. Mahmoud, Sh. Mahmud doi: 10.15407/ujpe62.11.0970 D. ABUBAKAR,1 N. MAHMOUD,2 SH. MAHMUD3 1 Physics Department, Bauchi State University Gadau (65, Itas/Gadau – Bauchi Nigeria; e-mail: [email protected]) 2 Nano-Optoelectronics Research Laboratory (NOR) – School of Physics Universiti Sains Malaysia (11800 Gelugor Pulau Pinang – Malaysia) 3 Nano-Optoelectronics Research Laboratory (NOR) – School of Physics, Universiti Sains Malaysia (11800 Gelugor Pulau Pinang – Malaysia) INVESTIGATION ON THE STRUCTURAL AND OPTICAL PROPERTIES OF NiO NANOFLAKES. PACS 68.55.-a, 78.20.-e, 81.15.Lm CHEMICAL BATH DEPOSITION OF Ni(OH)2 THIN FILMS Porous nickel oxide (NiO) nanoflakes are grown by the chemical bath deposition. The thin films are produced on an ITO/glass substrate and annealed at a variable temperature ina furnace. The structural and optical properties and the surface morphology of the thin films are studied and analyzed. FESEM results display the presence of nanoflakes with the structure of NiO/Ni(OH)2 in thin films that appear to increase in size with the annealing temperature. The sample grown at 300 ∘C is observed to have the highest surface area dimension. The EDX result reveals that the atomic ratio and weight of the treated sample has a non-stoichiometric value, which results in the p-type behavior of the NiO thin film. The result obtained by AFM indicates the highest roughness value (47.9 nm) for a sample grown at 300 ∘C. The analysis on XRD shows that the NiO nanoflakes possess a cubic structure with the orientation peaks of (111), (200), and (220). This appears with a stronger intensity at 300 ∘C. Likewise, XRD result approves the absence of the Ni(OH)2 peak at the annealing. For the optical band gap, the UV- Vis measurements give a lower value of 3.80 eV for 300 ∘C due to the highest crystallinity. The optimum temperature to synthesize high-quality NiO nanoflakes is 300 ∘C, which can be an important factor for good sensing devices. K e y w o r d s: annealing temperature, nanoflakes, thin film, chemical bath deposition, nickel oxide. 1. Introduction structure is the most commonly obtained structure Nickel oxide (NiO) thin films have attracted much [7, 8]. attention by the great chemical stability, high op- The different applications of NiO thin films are tical density, dynamic range, great electrochemi- based on their structural and morphological prop- cal effect, low-cost material device application, and erties. The porous nanostructured thin film offers a high chemical durability [1]. Nickel oxide is a semi- wide surface area that can result in a very short conductor and, generally, is considered as a model pathway for the diffusion of ions. NiO thin films with of p-type material. Due to the electronic proper- nanometric pores have been given a much attention ties of nanostructured NiO such as the wide en- because of their novel large surface area and geometry ergy band-gap of 3.6–4.0 eV with high thermal sta- of the interior. The porous nanostructure of NiO thin bility, it is qualified to be a favourable material in films has turned out to own a greater performance several applications in nanoelectronic devices such than their counterparts with compact structure, par- as electrochromic display [2], supercapacitance [3], ticularly in applications in electrochemistry [9, 10]. electrochemical charging/discharging mechanism [4], Nowadays, numerous chemical and physical tech- catalysts [5], and sensor devices [6]. NiO possesses niques such as the electro-deposition [10], thermal the cubic or rhombohedral structure, but the cubic decomposition [11], template synthesis [12], chemi- cal bath deposition (CBD) [13], sol-gel method [14], ○c D. ABUBAKAR, N. MAHMOUD, SH. MAHMUD, 2017 hydrothermal method [15], spray pyrolysis [16], pulse 970 ISSN 2071-0194. Ukr. J. Phys. 2017. Vol. 62, No. 11 Investigation on the Structural and Optical Properties NiO Nanoflakes laser deposition method (PLD) [17], and anodic elec- nickel (II)) in the solution [20]. Ni2+ ions present in trochemical deposition [18] have been employed to the solution react with Cl− ions (ligand) to forms 2− enhance the functionality of nanoporous thin films. a [NiCl4] ionic complex (tetrachloronickelate (II)) The CBD method is considered as a technique that from KCl(aq). The oxy-hydroxide presence was be- has an advantage over the other preparation tech- cause of the precursor solution of potassium chloride, niques mentioned above because of its convenience which is a complex agent resulting into the Ni(OH)2 in the large surface deposition, low cost, and low- thin film formation temperature synthesis. The CBD technique involves [Ni(OH ) ]2+ + 4Cl− [NiCl ]2− + 6H O : the substrate insertion into an aqueous solution of 2 6 (aq) (aq) 4 (aq) 2 (l) a precursor species and the heating to a certain tem- With the addition of an ammonia ligand excess perature. The required hydroxide is then precipitated aqueous solution, the mixture that contains the and deposited on the surface of the substrate, which 2− [NiCl4](aq) ions (yellowish-green tetrachloronickelate results in the production of thin films [19]. 2+ (II)) and [Ni(H2O)6](aq) (ion pale-green stable hex- 2+ 2. Experimental aaqua nickel(II)) reacts to form the ([Ni(NH3)6](aq) 2.1. Sample preparation ion complex (hexammine blue-violet solution), which is a substitution reaction of typical ligand [21] The thin layer of nanostructured NiO was de- 2− 2+ − posited,by using the CBD technique. The chemicals [NiCl4](aq) + 6NH3(aq) [Ni(NH3)6](aq) + 4Cl(aq); used were reagents of analytical grade and were em- 2+ 2+ [Ni(OH2)6] +6NH3(aq) [Ni(NH3)6] +6H2O(l): ployed with no more purification. Deionized water (aq) (aq) was utilized in this deposition. The precursor solu- The precipitation of blue-violet was observed at the tion for NiO nanoporous thin films was obtained, by interface due to the hydroxide ion and nickel (II) ion using 2.24 g of potassium chloride (KCl) and 2.63 g reaction from the ammonia hydrolysis with a basic of nickel sulphate hexahydrate (NiSO4 · 6H2O) aque- solution ous solutions. Furthermore, 40 ml of a 35% aqueous Ni2+ + 2OH− Ni(OH) ; solution of ammonia was further introduced as a com- (aq) (aq) 2(s) + − plex agent. The complete solution volume was made NH3(aq) + H2O(l) NH4(aq) + OH(aq): to 100 ml by topping with 20 ml of de-ionized wa- 2+ 2− ter into a beaker 100 ml in volume. The mixture was The [Ni(NH3)6] and [NiCl4] complexes are − stirred at 300 rpm for 30 min in order to have solution then hydrolyzed because of the high OH concen- homogeneity. The layers of the substrates were ultra- tration, which reduces the Ni(OH)2(s) insoluble pale ∘ sonically and chemically cleaned in ethanol, as well green solid precipitate formation at the 90 C heating as in acetone, each for 15 min, at a 40 ∘C heating temperature. This substance is known as an ampho- − temperature. Then, finally, the substrate was rinsed teric substance, since it can be formed by the OH with deionized water and dried in a nitrogen gas. The ion (hydroxide) addition that results in the forma- 2+ substrates were then vertically inserted into the solu- tion of a soluble salt of Ni ion. Finally, a Ni(OH)2 tion and heated inside a laboratory oven at a fixed thin-film layer is deposited on the substrate as shown temperature of 90 ∘C. Then they were annealed at a below: variable temperature of 200, 300 and 400 ∘C inside 2+ − [Ni(NH3)6] + OH Ni(OH)2(s) + NH3(aq); a furnace to obtain the desired NiO nanoflakes thin (aq) 2− − − film. [NiCl4] + OH(aq) Ni(OH)2(s) + 4Cl : The substrate was then washed with deionized wa- 2.2. Mechanisms ter after the thin film deposition in order to de- The chemical reactions of ions involved in the growth tached Ni(OH)2 particles, which are weakly bonded, of Ni(OH)2 nanoflakes can be seen as follows. Inthe and dried with a nitrogen gas flow. The thin films aqueous solution of hydrated nickel (II) sulphate, appear pale-green, which indicates a solid thin de- the stable solution was obtained with green as a re- posited layer of Ni(OH)2. The thickness of the as- 2+ sult of the presence of [Ni(OH2)6](aq) ions (hexaaqua grown Ni(OH)2 deposited thin film was measured to ISSN 2071-0194. Ukr. J. Phys. 2017. Vol. 62, No. 11 971 D. Abubakar, N. Mahmoud, Sh. Mahmud Fig. 1. XRD peaks for the as-grown Ni(OH)2 sample of NiO and samples annealed at different temperatures be about 1013 nm. The synthesis procedure for NiO equipped with CuK훼 (1.5406 A)˚ radiation. To study was based on the Ni(OH)2 thermal decomposition to the surface physical morphology and roughness, an produce a nanostructured NiO thin film, as shown in Atomic Force Microscope (AFM) Veeco NanoScope the reaction below: Analysis version 1.2 (Model: Dimension EDGE, Ni(OH) NiO + H O: BRUKER) Atomic force microscopy (AFM) was 2 2 used; a field-emission scanning electron microscope To find the optimum temperature of the synthesis (FESEM Model: FEI Nova NanoSEM 450) was em- of NiO thin films from the as-grown Ni(OH)2, three ployed to analyze the nanostructure of thin films; and samples were annealed at 200, 300 and 400 ∘C in a a UV-VIS-NIR spectrometer (Jobin Yvon HR 800 furnace for 90 min for the growth of desired NiO thin UV) was used to investigate the optical properties films. of the obtained thin film layer.
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