Search results for: intercalation.

Authors: Samir Al-Zobaidi

Abstract:

This study attempts to understand the effect of different UV irradiation methods on the intercalation of LDPE/MMT nanocomposites, and its molecular behavior at certain isothermal crystallization temperature. Three different methods of UV exposure were employed using single composition of LDPE/MMT nanocomposites. All samples were annealed for 5 hours at a crystallization temperature of 100^oC. The crystallization temperature was chosen to be at large supercooling temperature to ensure quick and complete crystallization. The raw material of LDPE consisted of two stable monoclinic and orthorhombic phases according to XRD results. The thermal behavior of both phases acted differently when UV exposure method was changed. The monoclinic phase was more dependent on the method used compared to the orthorhombic phase. The intercalation of clay, as well as, the non-isothermal crystallization temperature, has also shown a clear dependency on the type of UV exposure. A third phase that is thermally less stable was also observed. Its respond to UV irradiation was greater since it contains low molecular weight entities which make it more vulnerable to any UV exposure.

Keywords: LDPE/MMt nanocomposites, crystallization, UV irradiation, intercalation.

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Authors: A. I. Alateyah, H. N. Dhakal, Z. Y. Zhang

Abstract:

The study of the effect of the processing parameters on the level of intercalation between the layered silicate and polymer of two different methodology took place. X-ray diffraction, Scanning Electron Microscopy, Energy Dispersive X-ray Spectrometry, and Transmission Electron Microscopy were utilized in order to examine the intercalation level of nanocomposites of both methodologies. It was found that drying the clay prior to mixing with the polymer, mixing time and speed, degassing time, and the curing method had major changes to the level of distribution of the nanocomposites structure. In methodology 1, the presence of aggregation layers was observed at only 2.5 wt.% clay loading whereas in methodology 2 the presence of aggregation layers was found at higher clay loading (i.e. 5 wt.%).

Keywords: Vinyl ester, nanocomposites, layered silicate, characterisations, aggregation layers, intercalation, exfoliation.

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Authors: H. M. A. Asghar, S. N. Hussain, E. P. L. Roberts, N. W. Brown, H. Sattar

Abstract:

Intercalation imparts interesting features to the host graphite material. Two different types of intercalated compounds called (GIC-bisulphate or Nyex 1000 and GIC-nitrate or Nyex 3000) were tested for their adsorption capacity and ability to undergo electrochemical regeneration. It was found that Nyex 3000 showed comparatively slow kinetics along with reduced adsorption capacity to one half for acid violet 17 as adsorbate. Acid violet 17 was selected as model organic pollutant for evaluating comparative performance of said adsorbents. Both adsorbent materials showed 100% regeneration efficiency as achieved by passing a charge of 36 C g^-1 at a current density of 12 mA cm^-2 and a treatment time of 60 min.  

Keywords: Intercalation compound of graphite, Adsorption, electrochemical-regeneration, waste water.

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Authors: O. I. H. Dimitry, N. A. Mansour, A. L. G. Saad

Abstract:

Natural sodium montmorillonite (NaMMT), Cloisite Na⁺ and two organophilic montmorillonites (OMMTs), Cloisites 20A and 15A were used. Polycaprolactone (PCL)/MMT composites containing 1, 3, 5, and 10 wt% of Cloisite Na⁺ and PCL/OMMT nanocomposites containing 5 and 10 wt% of Cloisites 20A and 15A were prepared via solution intercalation technique to study the influence of organic modifier loading on particle dispersion of PCL/ NaMMT composites. Thermal stabilities of the obtained composites were characterized by thermal analysis using the thermogravimetric analyzer (TGA) which showed that in the presence of nitrogen flow the incorporation of 5 and 10 wt% of filler brings some decrease in PCL thermal stability in the sequence: Cloisite Na+>Cloisite 15A > Cloisite 20A, while in the presence of air flow these fillers scarcely influenced the thermoxidative stability of PCL by slightly accelerating the process. The interaction between PCL and silicate layers was studied by Fourier transform infrared (FTIR) spectroscopy which confirmed moderate interactions between nanometric silicate layers and PCL segments. The electrical conductivity (σ) which describes the ionic mobility of the systems was studied as a function of temperature and showed that σ of PCL was enhanced on increasing the modifier loading at filler content of 5 wt%, especially at higher temperatures in the sequence: Cloisite Na⁺<Cloisite 20A<Cloisite 15A, and was then decreased to some extent with a further increase to 10 wt%. The activation energy E_σ obtained from the dependency of σ on temperature using Arrhenius equation was found to be lowest for the nanocomposite containing 5 wt% of Cloisite 15A. The dispersed behavior of clay in PCL matrix was evaluated by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses which revealed partial intercalated structures in PCL/NaMMT composites and semi-intercalated/semi-exfoliated structures in PCL/OMMT nanocomposites containing 5 wt% of Cloisite 20A or Cloisite 15A.

Keywords: Polycaprolactone, organoclay, nanocomposite, montmorillonite, electrical conductivity, activation energy, exfoliation, intercalation.

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Authors: Benalia Kouini, Aicha Serier

Abstract:

Nanocomposites based on polypropylene/polyamide 66 (PP/PA66) nanoblends containing organophilic montmorillonite (OMMT) and maleic anhydride grafted polypropylene (PP-g-MAH) were prepared by melt compounding method followed by injection molding. Two different types of nanoclays were used in this work. DELLITE LVF is the untreated nanoclay and DELLITE 67G is the treated one. The morphology of the nanocomposites was studied using the XR diffraction (XRD). The results indicate that the incorporation of treated nanoclay has a significant effect on the impact strength of PP/PA66 nanocomposites. Furthermore, it was found that XRD results revealed the intercalation, exfoliation of nanaclays of nanocomposites.

Keywords: Nanoclay, nanocomposites, polypropylene, polyamide, melt processing, mechanical properties.

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Authors: H. M. A. Asghar, S. N. Hussain, E. P. L. Roberts, N. W. Brown, H. Sattar

Abstract:

A unique combination of adsorption and electrochemical regeneration with a proprietary adsorbent material called Nyex 100 was introduced at the University of Manchester for waste water treatment applications. Nyex 100 is based on graphite intercalation compound. It is non porous and electrically conducing adsorbent material. This material exhibited very small BET surface area i.e. 2.75 m2g-1, in consequence, small adsorptive capacities for the adsorption of various organic pollutants were obtained. This work aims to develop composite adsorbent material essentially capable of electrochemical regeneration coupled with improved adsorption characteristics. An organic dye, acid violet 17 was used as standard organic pollutant. The developed composite material was successfully electrochemically regenerated using a DC current of 1 A for 60 minutes. Regeneration efficiency was maintained at around 100% for five adsorption-regeneration cycles.

Keywords: Adsorption, electrically conducting adsorbent material, electrochemical regeneration, waste water.

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Authors: Mala Nath, Nagamani Kompelli, Partha Roy, Snehasish Das

Abstract:

Two new metal-based anticancer chemotherapeutic agents, [(Ph2Sn)2(HGuO)2(phen)Cl2] 1 and [(Ph3Sn)(HGuO)(phen)]- Cl.CH3OH.H2O 2, were designed, prepared and characterized by analytical and spectral (IR, ESI-Mass, 1H, 13C and 119Sn NMR) techniques. The proposed geometry of Sn(IV) in 1 and 2 is distorted octahedral and distorted trigonal-bipyramidal, respectively. Both 1 and 2 exhibit potential cytotoxicity in vitro against MCF-7, HepG-2 and DU-145 cell lines. The intrinsic binding constant (Kb) values of 1 (2.33 × 105 M-1) and 2 (2.46 × 105 M-1) evaluated from UV-Visible absorption studies suggest non-classical electrostatic mode of interaction via phosphate backbone of DNA double helix. The Stern- Volmer quenching constant (Ksv) of 1 (9.74 × 105 M-1) and 2 (2.9 × 106 M-1) determined by fluorescence studies suggests the groove binding and intercalation mode for 1 and 2, respectively. Effective cleavage of pBR322 DNA is induced by 1.Their interaction with DNA of cancer cells may account for potency.

Keywords: Anticancer agents, DNA binding studies, NMR spectroscopy, organotin.

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Authors: A. I. Alateyah, H. N. Dhakal, Z. Y. Zhang

Abstract:

Contact angle measurement was utilized in order to study the subject of the wettability and surface chemistry of the nanocomposites materials. Water and glycerol droplets were used in this study. The incorporation of layered silicate into the vinyl ester matrix helped to improve the wettability and reduced the θ values of both liquids used. The addition of 2 wt.% clay loading reduced the θ values of water and glycerol by up to 21% and 6% respectively. Likewise, the incorporation of 4 wt.% clay loading reduced the water and glycerol θ values by 49% and 38% respectively. Also this study confirms the findings in the literature regarding the relationship between the intercalation nanocomposites level and the wettability. Wide Angle X-ray Diffraction, Scanning Electron Microscopy and Transmission Electron Microscopy were utilised in order to characterise the interlamellar structure of nanocomposites.

Keywords: Vinyl ester, nanocomposites, layered silicate, characterisations, contact angle measurement, wettability.

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Authors: M. D. Stelescu, E. Manaila, G. Pelin, M. Georgescu, M. Sonmez

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This paper presents studies on the development and characterization of nanocomposites based on ethylene-propylene terpolymer rubber (EPDM), chlorobutyl rubber (IIR-Cl) and organically modified montmorillonite (OMMT). Mixtures were made containing 0, 3 and 6 phr (parts per 100 parts rubber) OMMT, respectively. They were obtained by melt intercalation in an internal mixer - Plasti-Corder Brabender, in suitable blending parameters, at high temperature for 11 minutes. Curing agents were embedded on a laboratory roller at 70-100 ºC, friction 1:1.1, processing time 5 minutes. Rubber specimens were obtained by compression, using a hydraulic press at 165 ºC and a pressing force of 300 kN. Curing time, determined using the Monsanto rheometer, decreases with the increased amount of OMMT in the mixtures. At the same time, it was noticed that mixtures containing OMMT show improvement in physical-mechanical properties. These types of nanocomposites may be used to obtain rubber seals for the space application or for other areas of application.

Keywords: Chlorobutyl rubber, ethylene-propylene-diene terpolymers, montmorillonite, rubber seals, space application.

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Authors: Fitria Rahmawati, Nuryani, Liviana Wijayanti

Abstract:

This research study the application of the immobilized TiO2 layer and Cu-TiO2 layer on graphite substrate as a negative electrode or anode for Li-ion battery. The titania layer was produced through chemical bath deposition method, meanwhile Cu particles were deposited electrochemically. A material can be used as an electrode as it has capability to intercalates Li ions into its crystal structure. The Li intercalation into TiO2/Graphite and Cu- TiO2/Graphite were analyzed from the changes of its XRD pattern after it was used as electrode during discharging process. The XRD patterns were refined by Le Bail method in order to determine the crystal structure of the prepared materials. A specific capacity and the cycle ability measurement were carried out to study the performance of the prepared materials as negative electrode of the Li-ion battery. The specific capacity was measured during discharging process from fully charged until the cut off voltage. A 300 was used as a load. The result shows that the specific capacity of Li-ion battery with TiO2/Graphite as negative electrode is 230.87 ± 1.70mAh.g-1 which is higher than the specific capacity of Li-ion battery with pure graphite as negative electrode, i.e 140.75 ±0.46mAh.g-1. Meanwhile deposition of Cu onto TiO2 layer does not increase the specific capacity, and the value even lower than the battery with TiO2/Graphite as electrode. The cycle ability of the prepared battery is only two cycles, due to the Li ribbon which was used as cathode became fragile and easily broken.

Keywords: Cu-TiO2, electrode, graphite substrate, Li-ion battery, TiO2 layer.

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Authors: H. M. Mohammad, A. Martin, N. Brown, N. Hodson, P. Hill, E. Roberts

Abstract:

Graphite intercalation compound (GIC) has been demonstrated to be a useful, low capacity and rapid adsorbent for the removal of organic micropollutants from water. The high electrical conductivity and low capacity of the material lends itself to electrochemical regeneration. Following electrochemical regeneration, equilibrium loading under similar conditions is reported to exceed that achieved by the fresh adsorbent. This behavior is reported in terms of the regeneration efficiency being greater than 100%. In this work, surface analysis techniques are employed to investigate the material in three states: ‘Fresh’, ‘Loaded’ and ‘Regenerated’. ‘Fresh’ GIC is shown to exhibit a hydrogen and oxygen rich surface layer approximately 150 nm thick. ‘Loaded’ GIC shows a similar but slightly thicker surface layer (approximately 370 nm thick) and significant enhancement in the hydrogen and oxygen abundance extending beyond 600 nm from the surface. 'Regenerated’ GIC shows an oxygen rich layer, slightly thicker than the fresh case at approximately 220 nm while showing a very much lower hydrogen enrichment at the surface. Results demonstrate that while the electrochemical regeneration effectively removes the phenol model pollutant, it also oxidizes the exposed carbon surface. These results may have a significant impact on the estimation of adsorbent life.

Keywords: Graphite, adsorbent, electrochemical, regeneration, phenol.

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Authors: PoiSim Khiew, MuiYen Ho, ThianKhoonTan, WeeSiong Chiu, Roslinda Shamsudin, Muhammad Azmi Abd-Hamid, ChinHua Chia

Abstract:

In the present work, we have developed a symmetric electrochemical capacitor based on the nanostructured iron oxide (Fe3O4)-activated carbon (AC) nanocomposite materials. The physical properties of the nanocomposites were characterized by Scanning Electron Microscopy (SEM) and Brunauer-Emmett-Teller (BET) analysis. The electrochemical performances of the composite electrode in 1.0 M Na2SO3 and 1.0 M Na2SO4 aqueous solutions were evaluated using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The composite electrode with 4 wt% of iron oxide nanomaterials exhibits the highest capacitance of 86 F/g. The experimental results clearly indicate that the incorporation of iron oxide nanomaterials at low concentration to the composite can improve the capacitive performance, mainly attributed to the contribution of the pseudocapacitance charge storage mechanism and the enhancement on the effective surface area of the electrode. Nevertheless, there is an optimum threshold on the amount of iron oxide that needs to be incorporated into the composite system. When this optimum threshold is exceeded, the capacitive performance of the electrode starts to deteriorate, as a result of the undesired particle aggregation, which is clearly indicated in the SEM analysis. The electrochemical performance of the composite electrode is found to be superior when Na2SO3 is used as the electrolyte, if compared to the Na2SO4 solution. It is believed that Fe3O4 nanoparticles can provide favourable surface adsorption sites for sulphite (SO3 2-) anions which act as catalysts for subsequent redox and intercalation reactions.

Keywords: Metal oxide nanomaterials, Electrochemical Capacitor, Double Layer Capacitance, Pseduocapacitance

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