[IEEE 2012 IEEE 12th International Conference on Nanotechnology (IEEE-NANO) - Birmingham, United Kingdom (2012.08.20-2012.08.23)] 2012 12th IEEE International Conference on Nanotechnology (IEEE-NANO) - Fabrications of highly attractive nanoscale nickel structures and their catalytic applications

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  • 2012 12th IEEE International Conference on Nanotechnology (IEEE-NANO)

    The International Conference Centre Birmingham

    20-23 August 20112, Birmingham, United Kingdom

    Fabrications of Highly Attractive Nanoscale Nickel Structures and Their Catalytic Applications

    Nazar Hussain\ Sirajuddin1, Keith Richrad Hallam2 and Tom Bligh Scott2 INational Centre of Excellence in Analytical Chemistry, University of Sind, Jamshoro 76080, Pakistan 2

    Interface Analysis Centre, University of Bristol, Bristol BS2 8BS, UK Email: nazarkalwar@gmail.com.drsiraj03@yahoo.com.K.R.Hallam@bristol.ac.uk and T.B.Scott@bristol.ac.uk

    Abstract - Present study describes synthesis of highly active and ordered nanoscale structures of nickel catalysts. The

    study reveals efficient catalytic activity for the degradation of

    toxic and lethal organic dye Eosin-B (EB). The stable colloidal

    dispersions of ordered nickel nanostructures (Ni NSs) arrays

    were prepared via modified hydrazine reduction route with

    unique morphologies in a lyotropic liquid crystalline medium

    using Triton x-tOO. The characterization studies like

    optimization of various parameters for preparation of

    nanoscale nickel structures, surface binding interactions, size

    and morphologies of Ni NSs were carried out by IN-Visible

    Spectroscopy, Scanning Electron Microscopy (SEM) and XRay Diffraction (XRD) Analysis.

    Index Terms - Nickel Nanostructures, TX-IOO, Eosin B


    Dyes have gotten tremendous importance on industrial scale because variety of organic dyes have extensively been used as veterinary medicine, biological stain, preservative to poultry feed to restrain the proliferation of harmful bacteria, dermatological agents as well as for commercial textile [1]. On the other hand, dyes also cause a number of toxic effects to the mammalian cells, reports have also shown that dyes are mutagen and mitotic poison; these are also basis for coloration of waters which troubles to aquatic life, at the same time harmful effects of dyes are left onto the environment [2, 3]. The UV-induced degradation of industrially important dyes have been studied by many workers such as reduction of methyl orange and methyl red have been carried out in water using the substrate immobilized ZnO nanocrystal capped with surfactant [4].

    We report the synthesis of nickel nanostructures by a simple and inexpensive route and their use as highly efficient nanocatalysts for degradation of Eosin B dye. Course of reduction/degradation examined for Eosin B was apparent from disappearance of the relative color during the experiments; optimization studies and extent of degradation have been monitored by UV -Vis absorption spectroscopy.


    A. Procedure of Synthesis

    A typical experiment was performed by mixing, NiCb.6H20 (0.5ml, 0.033M), NaOH (0.3ml, O.lM), N2H4.H20 (l.Oml, 0.2M), and Triton X-I 00 (0.5ml, 0.5M) at room temperature, the solution was finally diluted to 10ml with deionized water. On addition of desired quantities of

    reducing agent light blue colour was appeared, a stable colour was chosen to carry out further experiments.

    B. Characterizations

    Shimadzu UV -160 digital spectrophotometer (Kyoto, Japan) was used to record UV-Visible spectra. ASEM of Jeol, Japan, model, JSM 6380A was used to image the nanostructures. XRD patterns of Ni NSs were examined by Model D-8 of Bruker between 2 theta wavelength ranges of 20-80.

    C. Catalytic Test

    Eosin-B (EB) was selected as target compound to check the efficiency of catalyst deposited on glass cover slip. All experiments were performed in an aqueous medium using 20 /lM concentration of dye, 0.1 M NaBH4 (reducing agent) and 0.1 mg quantity ofNi NSs (catalyst).


    Formations of mixed Ni NSs have been described using a nonionic surfactant (Triton X-lOO) as stabilizing agent in an aqueous solution. The nanosized Ni Ss have been prepared by using hydrazine as reducing agent, mechanism for reduction is similar as cited in literature [5-7].

    A. UV- Visible Spectroscopy

    The nanometer size regime of newly synthesized Ni NSs was spectrophotometrically monitored which exhibited a characteristic absorption profile in the range 350-400 nm as shown in Figure 1, this is in the fine agreement with already reported work [5].


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    - 3




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    0.10 5

  • B. Scanning Electron Microscopy (SEM)

    The SEM images show that Ni NSs were formed with mixed morphologies containing highly ordered assembly of 2D nanosheets/foils with absolutely smooth surface having thickness in the range of 24-240 nm, while the average thickness is 72 nm, the diameter of these nanosheets is found in 0.9-7.0 11m with an average diameter of 3.1 11m, and size of spherical nickel nanoparticles ranges 8-300 nm, with the observed average size of 45 nm subsequent data is shown in Figure 2.

    Fig. 2 SEM images ofTX-IOO stabilized Ni NSs

    These Ni NSs were used as heterogeneous catalysts for the reduction/degradation of Eosin B.

    C. X-Ray Diffractometery (XRD)

    The phase composition of crystal structures of these products were also analyzed by X-ray diffraction technique. Figure 3, shows the XRD pattern of powdered Ni NSs which correspond to the formation of nanosheets/foils.


    111 ITX-l00- Ni Nssl 1200

    1000 100

    $ 800 c:

    111 "

    0 010 u 600



    w 40 W W ro w

    2 theta (degrees)

    Fig. 3 XRD pattern ofTX-1 00 stabilized Ni NSs

    More over the characteristic peaks (111) and (200) of products are in strong co-relation with formed nanoscale Ni structures, already reported [8-9]. We obtained mixed crystal structures with typical diffraction pattern indicating the formation of fcc phased Ni NPs with additional peaks for Ni based nanosheets/foils as appeared elsewhere [8], which are confirmed by surface morphology illustrations via SEM images.

    D. Degradation of Dyes

    Experiments for degradation/reduction of Eosin B with NaBH4 in presence and absence ofNi NSs were performed. The study revealed that EB dye was completely reduced in 30 seconds in presence of catalyst, as shown in Figure 4.


    Eosin B

    (I) -fresh CJ 1.0 I: -10sec ro

    -20 sec .c ...

    0 -30 sec I/)

    .c 0.5 -40 sec


    Wavelength (nm)

    Fig. 4 UV Visible spectra recorded for Eosin B degradation in presence of TX-1 00 stabilized Ni NSs.

    Eosin B was chosen because it produces different color shades in degraded and un-degraded forms.


    We present a modified hydrazine reduction route for fabrication of stable colloidal dispersions of nickel nanostructures using Triton X-I00 a nonionic surfactant. The extended complexity and functionality of the nanoscale systems are predictable from efficient linkages employed by OR group of TX-I00 molecules and Ni particles in a lyotropic liquid crystalline medium. These NSs were used for the reduction of an organic dye and found highly active catalysts.


    Financial assistance by Higher Education Commission, Islamabad, Pakistan and the facilities provided by National Centre of Excellence in Analytical Chemistry, University of Sindh, Iamshoro 76080, Pakistan and Interface Analysis Centre, University of Bristol, Bristol BS2 8BS, UK during this project are highly thanked and gratefully acknowledged.


    [I] H. He, S. Yang, K. Yu, Y. .Iu, C. Sun, L. Wang . .I. Hazard. Mater. 1 73 (20 1 0) 393-400.

    [2] S M. Thomas, D. G. MacPhee. Mutat. Res. Lett 1 40 ( 1 984) 165- 167. [3] M. M. Nassar, Y H. Magdy. Chern. Eng. J. 66 ( 1 997) 223-226. [4] R. Comparelli, E, Fanizza, M.L. Curri, P.D, Cozzoli, G, Mascolo, A.

    Agostiano. Applied Catalysis B Environmental 60 (2005) I-II. [5] N. H. Kalwar, Sirajuddin, S T. H. Sherazi, M, 1. Abro, Z. A. Tagar, S.

    S, Hassan, Y .Iunejo, M, 1. Khattak, Appl. Catal., AAOO (201 1 ) 2 1 5-220,

    [6] M. S Hussain, K. M. A. Haque. J. Sci. Res. 2 (201 0) 3 13-321 . [7] L Bai, F. Yuan, Q. Tang, Mater. Lett 62 (2008) 2267-2270. [8] B, Zhang, X, Ye, W. Dai, W, Hou, y, Xie, Chem, Eur. .I. 12 (2006)

    2337 - 2342, [9] H. Wang, X Kou, J. Zhang, J. Li. BulL Mater. Sci. 31 (2008) 97-1 00.

    978-1-4673-2200-3/12/$31.00 2012 IEEE


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