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Electrical and optical properties of nanostructured zinc oxide thin films influenced by annealing temperature

Shariffudin SS, Mamat MH, Rusop M

J Nanosci Nanotechnol, 2012 Oct;12(10):8165-8.
PMID: 23421195

Transparent nanostructured ZnO thin films were successfully deposited using sol-gel spin coating method on a quartz substrate. The 0.4 M ZnO solution gel was prepared using zinc acetate dihydrate (Zn(CH3COO)22H2O) as the precursor, 2-methoxyethanol as the solvent and monoethanolamine (MEA) as the stabilizer. The electrical and optical properties dependencies on the annealing temperature of the nanostructured ZnO thin films were investigated. It was found that as the annealing temperature increased, the particle size, conductivity and the peak of the UV emission also increased.
Aging effects on physical and electrical properties of nano-structured MgZnO thin films for carbon nanotube applications

Ahmad R, Salina M, Mamat MH, Teh AA, Kara M, Rusop M, et al.

J Nanosci Nanotechnol, 2012 Oct;12(10):8153-7.
PMID: 23421193

This paper addresses the growth of nano-structured MgZnO thin films by sol-gel spin coating method which will be used as a template layer to grow carbon nanotubes. The nano-structured MgZnO films were deposited on platinized (100) silicon substrates. In this work, we focused on the effect of aging and Mg content on the film structure and resistivity. Sols with Mg content of 10, 30 and 50 at.% were subjected to aging times of between 3 to 240 hours. Results from scanning (SEM) and field emission scanning electron (FESEM) microscopes and surface profiler (SP) showed that the sol aging increased the thickness, grain size and surface roughness for aging up to 240 hours. The energy dispersive analysis by X-ray (EDAX) confirmed the element of Mg in the ZnO films. The electrical resistivity also increased with aging time as confirmed by four point probe method. The results suggest that appropriate aging of the sol is important for improving physical quality and electrical performance of MgZnO thin films derived from sol-gel technique.
Electrochemical analysis of asymmetric supercapacitors based on BiCoO3@g-C3N4 nanocomposites

Varatharajan P, Shameem Banu IB, Mamat MH, Vasimalai N

Dalton Trans, 2023 Oct 03;52(38):13704-13715.
PMID: 37706529 DOI: 10.1039/d3dt01758c

Supercapacitors are gaining popularity these days because of their good cycle stability, superior specific capacitance, high power density, and energy density. Herein, we report the synthesis of bismuth cobalt oxide (BiCoO3) combined with graphitic carbon nitride (g-C3N4) by the hydrothermal method. The BiCoO3@g-C3N4 nanocomposite was well characterized using XRD, FE-SEM, FT-IR, and DRS-UV techniques. The supercapacitor properties of the BiCoO3@g-C3N4 nanocomposite were then studied using cyclic voltammetry, galvanic charging-discharging, and impedance spectroscopy techniques. Due to the synergistic effect, BiCoO3@g-C3N4 showed a high specific capacitance value of 341 F g-1 at a current density of 1 A g-1 and excellent retention of specific capacitance (98.82%) after 1000 cycles and a high power density of 1125 W kg-1. Using the impedance spectroscopy technique, the charge transfer resistance of BiCoO3, g-C3N4, and BiCoO3@g-C3N4 was measured. BiCoO3@g-C3N4 showed a low charge transfer resistance compared with BiCoO3 and g-C3N4. The asymmetric supercapacitor (ASC) device was prepared using activated carbon (negative side) and BiCoO3@g-C3N4 (positive side) electrodes. It showed a specific capacitance of 129 F g-1 at 1 A g-1, power density 2800 W kg-1 and energy density 35 W h kg-1. Finally, we conclude that, due to the high specific capacitance, good cycle retention, fast redox activity, and low charge transfer resistance BiCoO3@g-C3N4 is a good electrode material for energy storage applications.
Fulltext High-performance dye-sensitized solar cells based on morphology-controllable synthesis of ZnO-ZnS heterostructure nanocone photoanodes

Rouhi J, Mamat MH, Ooi CH, Mahmud S, Mahmood MR

PLoS One, 2015;10(4):e0123433.
PMID: 25875377 DOI: 10.1371/journal.pone.0123433

High-density and well-aligned ZnO-ZnS core-shell nanocone arrays were synthesized on fluorine-doped tin oxide glass substrate using a facile and cost-effective two-step approach. In this synthetic process, the ZnO nanocones act as the template and provide Zn2+ ions for the ZnS shell formation. The photoluminescence spectrum indicates remarkably enhanced luminescence intensity and a small redshift in the UV region, which can be associated with the strain caused by the lattice mismatch between ZnO and ZnS. The obtained diffuse reflectance spectra show that the nanocone-based heterostructure reduces the light reflection in a broad spectral range and is much more effective than the bare ZnO nanocone and nanorod structures. Dye-sensitized solar cells based on the heterostructure ZnO-ZnS nanocones are assembled, and high conversion efficiency (η) of approximately 4.07% is obtained. The η improvement can be attributed primarily to the morphology effect of ZnO nanocones on light-trapping and effectively passivating the interface surface recombination sites of ZnO nanocones by coating with a ZnS shell layer.
Photocatalytic performance improvement by utilizing GO_MWCNTs hybrid solution on sand/ZnO/TiO2-based photocatalysts to degrade methylene blue dye

Idris NJ, Bakar SA, Mohamed A, Muqoyyanah M, Othman MHD, Mamat MH, et al.

Environ Sci Pollut Res Int, 2021 Feb;28(6):6966-6979.
PMID: 33025441 DOI: 10.1007/s11356-020-10904-y

In this work, sand/zinc oxide (ZnO)/titanium dioxide (TiO2)-based photocatalysts were hybridized with graphene oxide (GO) and GO_multi-walled carbon nanotubes (MWCNTs) hybrid solution. The novel hybrid was then used in photocatalysis to degrade dye contamination. The nanocomposite photocatalyst was initially fabricated by growing ZnO nanorods (NRs) via sol-gel immersion followed by synthesizing TiO2 NRs for different times (5 and 20 h) using a hydrothermal method on sand as a substrate. Prior to the hybridization, the initial GO was synthesized using electrochemical exfoliation and further mixed with 1 wt% MWCNTs to form GO_MWCNTs hybrid solution. The synthesized GO and GO_MWCNTs hybrid solution were then incorporated onto sand/ZnO/TiO2 nanocomposite-based photocatalysts through immersion. Various sand/ZnO/TiO2-based photocatalysts were then tested for methylene blue (MB) dye degradation within 3 days. On the basis of UV-Vis measurement, the highest MB degradation was achieved by using sand/ZnO NRs/TiO2 NRs (5 h)/GO_MWCNTs (92.60%). The high surface area and high electrical conductivity of GO_MWCNTs prolonged the lifetime of electron/hole separation and thus enhanced the photocatalytic performance.
Incorporation of graphene oxide/titanium dioxide with different polymer materials and its effects on methylene blue dye rejection and antifouling ability

Mohamat R, Bakar SA, Mohamed A, Muqoyyanah M, Othman MHD, Mamat MH, et al.

Environ Sci Pollut Res Int, 2023 Jun;30(28):72446-72462.
PMID: 37170051 DOI: 10.1007/s11356-023-27207-7

Exposure of synthetic dye, such as methylene blue (MB), in water bodies led to a serious threat to living things because they are toxic and non-degradable. Amongst the introduced dye removal methods, membrane separation process can be considered a powerful technique for treating dye contamination. However, this method commonly suffered from drawbacks, such as short membrane lifetime, low permeability and selectivity. To overcome these issues, graphene oxide (GO) and titanium dioxide (TiO2) were used as additives to fabricate polyethersulfone (PES)- and polyvinylidene fluoride (PVDF)-based hybrid membranes via non-solvent-induced phase separation method. Prior to membrane fabrication, GO was synthesised via electrochemical exfoliation method assisted by customised triple-tail surfactant. The potential of PES- and PVDF-based hybrid membranes for wastewater treatment has been discussed widely. However, direct comparison between these two polymeric membranes is not critically discussed for MB dye separation application yet. Therefore, this study is aimed at evaluating the performance of different types of polymers (e.g. PES and PVDF) in terms of membrane morphology, properties, dye rejection and antifouling ability. Results showed that the incorporation of GO and TiO2 alters the morphology of the fabricated membranes and affects dye rejection further, as well as their antifouling performance. In contrast with pristine membrane, PES-GO/TiO2 and PVDF-GO/TiO2 possessed high hydrophilicity, as indicated by their low contact angle (67.38° and 62.12°, respectively). Based on this study, PVDF-GO/TiO2 showed higher porosity value (94.88%), permeability (87.32 L/m2hMPa) and MB rejection rate (92.63%), as well as flux recovery ratio value of > 100% as compared with others. Overall, the incorporation of GO and TiO2 with PVDF polymer are proven to be effective hybrid materials of membrane fabrication for dye rejection application in the near future. The polymer material's intrinsic properties can affect the attributes of the fabricated membrane.
Fabrication and application of composite adsorbents made by one-pot electrochemical exfoliation of graphite in surfactant ionic liquid/nanocellulose mixtures

Jamaluddin NA, Mohamed A, Bakar SA, Ardyani T, Sagisaka M, Saito H, et al.

Phys Chem Chem Phys, 2021 Sep 15;23(35):19313-19328.
PMID: 34524298 DOI: 10.1039/d1cp02206g

Previously, surfactant-assisted exfoliated graphene oxide (sEGO) formed with the triple-chain surfactant TC14 (sodium 1,4-bis(neopentyloxy)-3-(neopentylcarbonyl)-1,4-dioxobutane-2-sulfonate) was applied in wastewater treatment. The extent of dye-removal and the adsorption capacity of the sEGO formed with this triple-chain surfactant outperformed those of two other systems, namely, the di-chain version of TC14 (AOT14; sodium 1,2-bis-(2,2-dimethyl-propoxycarbonyl)-ethanesulfonate) and the single-chain surfactant sodium n-dodecylsulfate. In the present study, to further optimise the surfactant chemical structure, the sodium ion of TC14 was substituted with 1-butyl-3-methyl-imidazolium (BMIM) generating surfactant ionic liquids (SAILs; 1-butyl-3-imidazolium 1,4-bis(neopentyloxy)-3-(neopentyloxycarbonyl)-1,4-dioxobutane-2-sulfonate), hereafter denoted as BMIM-TC14. This SAIL, together with nanofibrillated kenaf cellulose (NFC), was used to electrochemically exfoliate graphite, yielding BMIM-TC14 sEGO/NFC composites. These highly hydrophobic polymer composites were then used for the removal of methylene blue (MB) from aqueous solution. 1H NMR spectroscopy was used to elucidate the structure of the synthesised SAILs. The morphologies of the resulting nanocomposites were investigated using Raman spectroscopy, field-emission scanning electron microscopy, and high-resolution transmission electron microscopy. Analysis using small-angle neutron scattering was performed to examine the aggregation behaviour of sEGO and custom-made SAILs. Zeta potential, surface tension, and dynamic light-scattering measurements were used to study the aqueous properties and colloidal stability of the suspension. Amongst the surfactants tested, BMIM-TC14 sEGO/NFC exhibited the highest MB adsorption ability, achieving 99% dye removal under optimum conditions. These results highlight the importance of modifying the hydrophilic moieties of amphiphilic compounds to improve the performance of sEGO/NFC composites as effective adsorbents for wastewater treatment.
Preparation of conductive cellulose paper through electrochemical exfoliation of graphite: The role of anionic surfactant ionic liquids as exfoliating and stabilizing agents

Mohamed A, Ardyani T, Bakar SA, Sagisaka M, Umetsu Y, Hussin MRM, et al.

Carbohydr Polym, 2018 Dec 01;201:48-59.
PMID: 30241844 DOI: 10.1016/j.carbpol.2018.08.040

A facile electrochemical exfoliation method was established to efficiently prepare conductive paper containing reduced graphene oxide (RGO) with the help of single chain anionic surfactant ionic liquids (SAILs). The surfactant ionic liquids are synthesized from conventional organic surfactant anions and a 1-butyl-3-methyl-imidazolium cation. For the first time the combination of SAILs and cellulose was used to directly exfoliate graphite. The ionic liquid 1-butyl-3-methyl-imidazolium dodecylbenzenesulfonate (BMIM-DBS) was shown to have notable affinity for graphene, demonstrating improved electrical properties of the conductive cellulose paper. The presence of BMIM-DBS in the system promotes five orders of magnitude enhancement of the paper electrical conductivity (2.71 × 10-5 S cm-1) compared to the native cellulose (1.97 × 10-10 S cm-1). A thorough investigation using electron microscopy and Raman spectroscopy highlights the presence of uniform graphene incorporated inside the matrices. Studies into aqueous aggregation behavior using small-angle neutron scattering (SANS) point to the ability of this compound to act as a bridge between graphene and cellulose, and is responsible for the enhanced exfoliation level and stabilization of the resulting dispersion. The simple and feasible process for producing conductive paper described here is attractive for the possibility of scaling-up this technique for mass production of conductive composites containing graphene or other layered materials.
Surfactants with aromatic headgroups for optimizing properties of graphene/natural rubber latex composites (NRL): Surfactants with aromatic amine polar heads

Ardyani T, Mohamed A, Bakar SA, Sagisaka M, Umetsu Y, Mamat MH, et al.

J Colloid Interface Sci, 2019 Jun 01;545:184-194.
PMID: 30878784 DOI: 10.1016/j.jcis.2019.03.012

HYPOTHESIS: The compatibility of surfactants and graphene surfaces can be improved by increasing the number of aromatic groups in the surfactants. Including aniline in the structure may improve the compatibility between surfactant and graphene further still. Surfactants can be modified by incorporating aromatic groups in the hydrophobic chains or hydrophilic headgroups. Therefore, it is of interest to investigate the effects of employing anilinium based surfactants to disperse graphene nanoplatelets (GNPs) in natural rubber latex (NRL) for the fabrication of electrically conductive nanocomposites.
EXPERIMENTS: New graphene-philic surfactants carrying aromatic moieties in the hydrophilic headgroups and hydrophobic tails were synthesized by swapping the traditional sodium counterion with anilinium. 1H NMR spectroscopy was used to characterize the surfactants. These custom-made surfactants were used to assist the dispersion of GNPs in natural rubber latex matrices for the preparation of conductive nanocomposites. The properties of nanocomposites with the new anilinium surfactants were compared with commercial sodium surfactant sodium dodecylsulfate (SDS), sodium dodecylbenzenesulfonate (SDBS), and the previously synthesized aromatic tri-chain sodium surfactant TC3Ph3 (sodium 1,5-dioxo-1,5-bis(3-phenylpropoxy)-3-((3phenylpropoxy)carbonyl) pentane-2-sulfonate). Structural properties of the nanocomposites were studied using Raman spectroscopy, field emission scanning electron microscopy (FESEM), and high-resolution transmission electron microscopy (HRTEM). Electrical conductivity measurements and Zeta potential measurements were used to assess the relationships between total number of aromatic groups in the surfactant molecular structure and nanocomposite properties. The self-assembly structure of surfactants in aqueous systems and GNP dispersions was assessed using small-angle neutron scattering (SANS).
FINDINGS: Among these different surfactants, the anilinium version of TC3Ph3 namely TC3Ph3-AN (anilinium 1,5-dioxo-1,5-bis(3-phenylpropoxy)-3-((3phenylpropoxy)carbonyl) pentane-2-sulfonate) was shown to be highly efficient for dispersing GNPs in the NRL matrices, increasing electrical conductivity eleven orders of magnitude higher than the neat rubber latex. Comparisons between the sodium and anilinium surfactants show significant differences in the final properties of the nanocomposites. In general, the strategy of increasing the number of surfactant-borne aromatic groups by incorporating anilinium ions in surfactant headgroups appears to be effective.
Rational design of aromatic surfactants for graphene/natural rubber latex nanocomposites with enhanced electrical conductivity

Mohamed A, Ardyani T, Abu Bakar S, Sagisaka M, Umetsu Y, Hamon JJ, et al.

J Colloid Interface Sci, 2018 Apr 15;516:34-47.
PMID: 29360058 DOI: 10.1016/j.jcis.2018.01.041

HYPOTHESIS: Graphene nanoplatelets (GNPs) can be dispersed in natural rubber matrices using surfactants. The stability and properties of these composites can be optimized by the choice of surfactants employed as stabilizers. Surfactants can be designed and synthesized to have enhanced compatibility with GNPs as compared to commercially available common surfactants. Including aromatic groups in the hydrophobic chain termini improves graphene compatibility of surfactants, which is expected to increase with the number of aromatic moieties per surfactant molecule. Hence, it is of interest to study the relationship between molecular structure, dispersion stability and electrical conductivity enhancement for single-, double-, and triple-chain anionic graphene-compatible surfactants.
EXPERIMENTS: Graphene-philic surfactants, bearing two and three chains phenylated at their chain termini, were synthesized and characterized by proton nuclear magnetic resonance (1H NMR) spectroscopy. These were used to formulate and stabilize dispersion of GNPs in natural rubber latex matrices, and the properties of systems comprising the new phenyl-surfactants were compared with commercially available surfactants, sodium dodecylsulfate (SDS) and sodium dodecylbenzenesulfonate (SDBS). Raman spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM), and high-resolution transmission electron microscopy (HRTEM) were used to study structural properties of the materials. Electrical conductivity measurements and Zeta potential measurements were used to assess the relationships between surfactant architecture and nanocomposite properties. Small-angle neutron scattering (SANS) was used to study self-assembly structure of surfactants.
FINDINGS: Of these different surfactants, the tri-chain aromatic surfactant TC3Ph3 (sodium 1,5-dioxo-1,5-bis(3-phenylpropoxy)-3-((3phenylpropoxy)carbonyl) pentane-2-sulfonate) was shown to be highly graphene-compatible (nanocomposite electrical conductivity = 2.22 × 10-5 S cm-1), demonstrating enhanced electrical conductivity over nine orders of magnitude higher than neat natural rubber-latex matrix (1.51 × 10-14 S cm-1). Varying the number of aromatic moieties in the surfactants appears to cause significant differences to the final properties of the nanocomposites.
Carbon nanotubes from waste cooking palm oil as adsorbent materials for the adsorption of heavy metal ions

Abu Bakar S, Jusoh N, Mohamed A, Muqoyyanah M, Othman MHD, Mamat MH, et al.

Environ Sci Pollut Res Int, 2021 Dec;28(46):65171-65187.
PMID: 34231144 DOI: 10.1007/s11356-021-14918-y

In this work, waste cooking palm oil (WCPO)-based carbon nanotubes (CNTs) with encapsulated iron (Fe) nanoparticles have been successfully produced via modified thermal chemical vapor deposition method. Based on several characterizations, the dense WCPO-based CNT was produced with high purity of 89% and high crystallinity proven by low ID/IG ratio (0.43). Moreover, the ferromagnetic response of CNTs showed that the average coercivity and magnetization saturation were found to be 551.5 Oe and 13.4 emu/g, respectively. These produced WCPO-based CNTs were further used as heavy metal ions adsorbent for wastewater treatment application. Some optimizations, such as the effect of different adsorbent dosage, varied initial pH solution, and various heavy metal ions, were investigated. The adsorption studies showed that the optimum adsorbent dosage was 1.8 g/L when it was applied to 100 mg/L Cu (II) solution at neutral pH (pH 7). Further measurement then showed that high Cu (II) ion removal percentage (~80%) was achieved when it was applied at very acidic solution (pH 2). Last measurement confirmed that the produced WCPO-based CNTs successfully removed different heavy metal ions in the following order: Fe (II) > Zn (II) ≈ Cu (II) with the removal percentage in the range of 99.2 to 99.9%. The adsorption isotherm for Cu (II) was better fitted by Langmuir model with a correlation coefficient of 0.82751. WCPO-based CNTs can be a potential material to be applied as adsorbent in heavy metal ion removal.

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