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Fulltext The Impact of Polyvinylpyrrolidone on Properties of Cadmium Oxide Semiconductor Nanoparticles Manufactured by Heat Treatment Technique

Al-Hada NM, Saion E, Talib ZA, Shaari AH

Polymers (Basel), 2016 Apr 08;8(4).
PMID: 30979222 DOI: 10.3390/polym8040113

Cadmium oxide semiconductor nanoparticles were produced using a water based mixture, incorporating cadmium nitrates, polyvinyl pyrrolidone (PVP), and calcination temperature. An X-ray diffraction (XRD) evaluation was conducted to determine the degree of crystallization of the semiconductor nanoparticles. In addition, scanning electron microscopy (SEM) was conducted to identify the morphological features of the nanoparticles. The typical particle sizes and particle dispersal were analyzed via the use of transmission electron microscopy (TEM). The findings provided further support for the XRD outcomes. To determine the composition phase, Fourier transform infrared spectroscopy (FT-IR) was conducted, as it indicated the existence of not only metal oxide ionic band in the selection of samples, but also the efficient removal of organic compounds following calcinations. The optical characteristics were demonstrated, so as to analyze the energy band gap via the use of a UV⁻Vis spectrophotometer. A reduced particle size resulted in diminution of the intensity of photoluminescence, was demonstrated by PL spectra. Plus, the magnetic characteristics were examined using an electron spin resonance (ESR) spectroscopy, which affirmed the existence of unpaired electrons.
Fulltext Structural and Optical Properties of Ag Nanoparticles Synthesized by Thermal Treatment Method

Gharibshahi L, Saion E, Gharibshahi E, Shaari AH, Matori KA

Materials (Basel), 2017 Apr 12;10(4).
PMID: 28772762 DOI: 10.3390/ma10040402

The modified thermal treatment method via alternate oxygen and nitrogen flow was successfully employed to synthesize very narrow and pure Ag nanoparticles. The structural and optical properties of the obtained metal nanoparticles at different calcination temperatures between 400 and 800 °C were studied using various techniques. The FTIR and EDX confirmed the formation of Ag nanoparticles without a trace of impurities. The XRD spectra revealed that the amorphous sample at 30 °C had transformed into the cubic crystalline nanostructures at the calcination temperature of 400 °C and higher. The TEM images showed the formation of spherical Ag nanoparticles in which the average particle size decreased with increasing calcination temperature from 7.88 nm at 400 °C to 3.29 nm at 800 °C. The optical properties were determined by UV-vis absorption spectrophotometer, which showed an increase in the conduction band of Ag nanoparticles with increasing calcination temperature from 2.75 eV at 400 °C to 3.04 eV at 800 °C. This was due to less attraction between conduction electrons and metal ions as the particle size decreases in corresponding to fewer numbers of atoms that made up the metal nanoparticles.
Fulltext Influence of Poly(vinylpyrrolidone) concentration on properties of silver nanoparticles manufactured by modified thermal treatment method

Gharibshahi L, Saion E, Gharibshahi E, Shaari AH, Matori KA

PLoS One, 2017;12(10):e0186094.
PMID: 29045414 DOI: 10.1371/journal.pone.0186094

Very narrow and pure silver nanoparticles were synthesized by modified thermal treatment method via oxygen and nitrogen flow in succession. The structural and optical properties of the calcined silver nanoparticles at 600°C with diverse Poly(vinylpyrrolidone) concentrations varied from 2% to 4% were studied by means of different techniques. Fourier transform infrared spectroscopy was used to monitor the production of pure Ag nanoparticles at a given Poly(vinylpyrrolidone) concentration. The X-ray powder diffraction spectra are evidence for the transformation of the amorphous sample at 30°C to the cubic crystalline nanostructures at the calcination temperatures for all Poly(vinylpyrrolidone) concentrations. The transmission electron microscopy images showed the creation of spherical silver nanoparticles with the average particle size decreased by increasing Poly(vinylpyrrolidone) concentrations from 4.61 nm at 2% to 2.49 nm at 4% Poly(vinylpyrrolidone). The optical properties were investigated by means of UV-vis absorption spectrophotometer, which showed an increase in the conduction band of Ag nanoparticles with increasing Poly(vinylpyrrolidone) concentrations from 2.83 eV at 2% Poly(vinylpyrrolidone) to 2.94 eV at 4% Poly(vinylpyrrolidone) due to decreasing particle size. This was due to less attraction between conduction electrons and metal ions for smaller particle size corresponding to fewer atoms that made up the metal nanoparticles.
Fulltext Sustained release of prindopril erbumine from its chitosan-coated magnetic nanoparticles for biomedical applications

Dorniani D, Hussein MZ, Kura AU, Fakurazi S, Shaari AH, Ahmad Z

Int J Mol Sci, 2013;14(12):23639-53.
PMID: 24300098 DOI: 10.3390/ijms141223639

The preparation of magnetic nanoparticles coated with chitosan-prindopril erbumine was accomplished and confirmed by X-ray diffraction, TEM, magnetic measurements, thermal analysis and infrared spectroscopic studies. X-ray diffraction and TEM results demonstrated that the magnetic nanoparticles were pure iron oxide phase, having a spherical shape with a mean diameter of 6 nm, compared to 15 nm after coating with chitosan-prindopril erbumine (FCPE). Fourier transform infrared spectroscopy study shows that the coating of iron oxide nanoparticles takes place due to the presence of some bands that were emerging after the coating process, which belong to the prindopril erbumine (PE). The thermal stability of the PE in an FCPE nanocomposite was remarkably enhanced. The release study showed that around 89% of PE could be released within about 93 hours by a phosphate buffer solution at pH 7.4, which was found to be of sustained manner governed by first order kinetic. Compared to the control (untreated), cell viability study in 3T3 cells at 72 h post exposure to both the nanoparticles and the pure drug was found to be sustained above 80% using different doses.
Fulltext SnO2/Pt thin film laser ablated gas sensor array

Shahrokh Abadi MH, Hamidon MN, Shaari AH, Abdullah N, Wagiran R

Sensors (Basel), 2011;11(8):7724-35.
PMID: 22164041 DOI: 10.3390/s110807724

A gas sensor array was developed in a 10 × 10 mm(2) space using Screen Printing and Pulse Laser Ablation Deposition (PLAD) techniques. Heater, electrode, and an insulator interlayer were printed using the screen printing method on an alumina substrate, while tin oxide and platinum films, as sensing and catalyst layers, were deposited on the electrode at room temperature using the PLAD method, respectively. To ablate SnO(2) and Pt targets, depositions were achieved by using a 1,064 nm Nd-YAG laser, with a power of 0.7 J/s, at different deposition times of 2, 5 and 10 min, in an atmosphere containing 0.04 mbar (4 kPa) of O(2). A range of spectroscopic diffraction and real space imaging techniques, SEM, EDX, XRD, and AFM were used in order to characterize the surface morphology, structure, and composition of the films. Measurement on the array shows sensitivity to some solvent and wood smoke can be achieved with short response and recovery times.
Fulltext Characterization of mixed xWO3(1-x)Y2O3 nanoparticle thick film for gas sensing application

Abadi MH, Hamidon MN, Shaari AH, Abdullah N, Misron N, Wagiran R

Sensors (Basel), 2010;10(5):5074-89.
PMID: 22399925 DOI: 10.3390/s100505074

Microstructural, topology, inner morphology, and gas-sensitivity of mixed xWO(3)(1-x)Y(2)O(3) nanoparticles (x = 1, 0.95, 0.9, 0.85, 0.8) thick-film semiconductor gas sensors were studied. The surface topography and inner morphological properties of the mixed powder and sensing film were characterized with X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Also, gas sensitivity properties of the printed films were evaluated in the presence of methane (CH(4)) and butane (C(4)H(10)) at up to 500 °C operating temperature of the sensor. The results show that the doping agent can modify some structural properties and gas sensitivity of the mixed powder.
Fulltext Preparation of Fe₃O₄ magnetic nanoparticles coated with gallic acid for drug delivery

Dorniani D, Hussein MZ, Kura AU, Fakurazi S, Shaari AH, Ahmad Z

Int J Nanomedicine, 2012;7:5745-56.
PMID: 23166439 DOI: 10.2147/IJN.S35746

Magnetic iron oxide nanoparticles were prepared using a sonochemical method under atmospheric conditions at a Fe²⁺ to Fe³⁺ molar ratio of 1:2. The iron oxide nanoparticles were subsequently coated with chitosan and gallic acid to produce a core-shell structure.
Fulltext Optimisation of the Photonic Efficiency of TiO2 Decorated on MWCNTs for Methylene Blue Photodegradation

Abdullahi N, Saion E, Shaari AH, Al-Hada NM, Keiteb A

PLoS One, 2015;10(5):e0125511.
PMID: 25993127 DOI: 10.1371/journal.pone.0125511

MWCNTs/TiO2 nanocomposite was prepared by oxidising MWCNT in H2SO4/HNO3 then decorating it with TiO2-p25 nanopowder. The composites were characterised using XRD, TEM, FT-IR PL and UV-vis spectroscopy. The TEM images have shown TiO2 nanoparticles immobilised onto the sidewalls of the MWCNTs. The UV-vis spectrum confirms that the nanocomposites can significantly absorb more light in the visible regions compared with the commercial TiO2 (P25). The catalytic activity of these nanocomposites was determined by photooxidation of MB aqueous solution in the presence of visible light. The MWCNTs/TiO2 (1:3) mass ratio showed maximum degradation efficiency. However, its activity was more favourable in alkaline and a neutral pH than an acidic medium.
Thermal Calcination-Based Production of SnO₂ Nanopowder: An Analysis of SnO₂ Nanoparticle Characteristics and Antibacterial Activities

Al-Hada NM, Kamari HM, Baqer AA, Shaari AH, Saion E

Nanomaterials (Basel), 2018 Apr 17;8(4).
PMID: 29673195 DOI: 10.3390/nano8040250

SnO₂ nanoparticle production using thermal treatment with tin(II) chloride dihydrate and polyvinylpyrrolidone capping agent precursor materials for calcination was investigated. Samples were analyzed using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), energy dispersive X-ray (EDX), transmission electron microscopy (TEM), Fourier Transform Infrared Spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), diffuse UV-vis reflectance spectra, photoluminescence (PL) spectra and the electron spin resonance (ESR). XRD analysis found tetragonal crystalline structures in the SnO₂ nanoparticles generated through calcination. EDX and FT-IR spectroscopy phase analysis verified the derivation of the Sn and O in the SnO₂ nanoparticle samples from the precursor materials. An average nanoparticle size of 4–15.5 nm was achieved by increasing calcination temperature from 500 °C to 800 °C, as confirmed through TEM. The valence state and surface composition of the resulting nanoparticle were analyzed using XPS. Diffuse UV-vis reflectance spectra were used to evaluate the optical energy gap using the Kubelka-Munk equation. Greater calcination temperature resulted in the energy band gap falling from 3.90 eV to 3.64 eV. PL spectra indicated a positive relationship between particle size and photoluminescence. Magnetic features were investigated through ESR, which revealed the presence of unpaired electrons. The magnetic field resonance decreases along with an increase of the g-factor value as the calcination temperature increased from 500 °C to 800 °C. Finally, Escherichia coli ATCC 25922 Gram (–ve) and Bacillus subtilis UPMC 1175 Gram (+ve) were used for in vitro evaluation of the tin oxide nanoparticle’s antibacterial activity. This work indicated that the zone of inhibition of 22 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.
Fulltext Preparation and characterization of 6-mercaptopurine-coated magnetite nanoparticles as a drug delivery system

Dorniani D, Hussein MZ, Kura AU, Fakurazi S, Shaari AH, Ahmad Z

Drug Des Devel Ther, 2013;7:1015-26.
PMID: 24106420 DOI: 10.2147/DDDT.S43035

BACKGROUND: Iron oxide nanoparticles are of considerable interest because of their use in magnetic recording tape, ferrofluid, magnetic resonance imaging, drug delivery, and treatment of cancer. The specific morphology of nanoparticles confers an ability to load, carry, and release different types of drugs.
METHODS AND RESULTS: We synthesized superparamagnetic nanoparticles containing pure iron oxide with a cubic inverse spinal structure. Fourier transform infrared spectra confirmed that these Fe3O4 nanoparticles could be successfully coated with active drug, and thermogravimetric and differential thermogravimetric analyses showed that the thermal stability of iron oxide nanoparticles coated with chitosan and 6-mercaptopurine (FCMP) was markedly enhanced. The synthesized Fe3O4 nanoparticles and the FCMP nanocomposite were generally spherical, with an average diameter of 9 nm and 19 nm, respectively. The release of 6-mercaptopurine from the FCMP nanocomposite was found to be sustained and governed by pseudo-second order kinetics. In order to improve drug loading and release behavior, we prepared a novel nanocomposite (FCMP-D), ie, Fe3O4 nanoparticles containing the same amounts of chitosan and 6-mercaptopurine but using a different solvent for the drug. The results for FCMP-D did not demonstrate "burst release" and the maximum percentage release of 6-mercaptopurine from the FCMP-D nanocomposite reached about 97.7% and 55.4% within approximately 2,500 and 6,300 minutes when exposed to pH 4.8 and pH 7.4 solutions, respectively. By MTT assay, the FCMP nanocomposite was shown not to be toxic to a normal mouse fibroblast cell line.
CONCLUSION: Iron oxide coated with chitosan containing 6-mercaptopurine prepared using a coprecipitation method has the potential to be used as a controlled-release formulation. These nanoparticles may serve as an alternative drug delivery system for the treatment of cancer, with the added advantage of sparing healthy surrounding cells and tissue.
Fulltext Release behavior and toxicity profiles towards leukemia (WEHI-3B) cell lines of 6-mercaptopurine-PEG-coated magnetite nanoparticles delivery system

Dorniani D, Kura AU, Hussein-Al-Ali SH, bin Hussein MZ, Fakurazi S, Shaari AH, et al.

ScientificWorldJournal, 2014;2014:972501.
PMID: 24895684 DOI: 10.1155/2014/972501

The coating of an active drug, 6-mercaptopurine, into the iron oxide nanoparticles-polyethylene glycol (FNPs-PEG) in order to form a new nanocomposite, FPEGMP-2, was accomplished using coprecipitation technique. The resulting nanosized with a narrow size distribution magnetic polymeric particles show the superparamagnetic properties with 38.6 emu/g saturation magnetization at room temperature. Fourier transform infrared spectroscopy and the thermal analysis study supported the formation of the nanocomposite and the enhancement of thermal stability in the resulting nanocomposite comparing with its counterpart in free state. The loading of 6-mercaptopurine (MP) in the FPEGMP-2 nanocomposite was estimated to be about 5.6% and the kinetic experimental data properly correlated with the pseudo-second order model. Also, the release of MP from the FPEGMP-2 nanocomposite shows the sustained release manner which is remarkably lower in phosphate buffered solution at pH 7.4 than pH 4.8, due to different release mechanism. The maximum percentage release of MP from the nanocomposite reached about 60% and 97% within about 92 and 74 hours when exposed to pH 7.4 and 4.8, respectively.
Fulltext In vitro sustained release study of gallic acid coated with magnetite-PEG and magnetite-PVA for drug delivery system

Dorniani D, Kura AU, Hussein-Al-Ali SH, Bin Hussein MZ, Fakurazi S, Shaari AH, et al.

ScientificWorldJournal, 2014;2014:416354.
PMID: 24737969 DOI: 10.1155/2014/416354

The efficacy of two nanocarriers polyethylene glycol and polyvinyl alcohol magnetic nanoparticles coated with gallic acid (GA) was accomplished via X-ray diffraction, infrared spectroscopy, magnetic measurements, thermal analysis, and TEM. X-ray diffraction and TEM results showed that Fe3O4 nanoparticles were pure iron oxide having spherical shape with the average diameter of 9 nm, compared with 31 nm and 35 nm after coating with polyethylene glycol-GA (FPEGG) and polyvinyl alcohol-GA (FPVAG), respectively. Thermogravimetric analyses proved that after coating the thermal stability was markedly enhanced. Magnetic measurements and Fourier transform infrared (FTIR) revealed that superparamagnetic iron oxide nanoparticles could be successfully coated with two polymers (PEG and PVA) and gallic acid as an active drug. Release behavior of gallic acid from two nanocomposites showed that FPEGG and FPVAG nanocomposites were found to be sustained and governed by pseudo-second-order kinetics. Anticancer activity of the two nanocomposites shows that the FPEGG demonstrated higher anticancer effect on the breast cancer cell lines in almost all concentrations tested compared to FPVAG.
Fulltext Effect of Ratio in Ammonium Nitrate on the Structural, Microstructural, Magnetic, and AC Conductivity Properties of BaFe12O19

Azis RS, Che Muda NN, Hassan J, Shaari AH, Ibrahim IR, Mustaffa MS, et al.

Materials (Basel), 2018 Nov 06;11(11).
PMID: 30404131 DOI: 10.3390/ma11112190

This paper investigates the effect of the ratio of ammonium nitrate (AN) on the structural, microstructural, magnetic, and alternating current (AC) conductivity properties of barium hexaferrite (BaFe12O19). The BaFe12O19 were prepared by using the salt melt method. The samples were synthesized using different powder-to-salt weight ratio variations (1:3, 1:4, 1:5, 1:6 and 1:7) of BaCO₃ + Fe₂O₃ and ammonium nitrate salt. The NH₄NO₃ was melted on a hot plate at 170 °C. A mixture of BaCO₃ and Fe₂O₃ were added into the NH₄NO₃ melt solution and stirred for several hours using a magnetic stirrer under a controlled temperature of 170 °C. The heating temperature was then increased up to 260 °C for 24 hr to produce an ash powder. The x-ray diffraction (XRD) results show the intense peak of BaFe12O19 for all the samples and the presence of a small amount of the impurity Fe₂O₃ in the samples, at a ratio of 1:5 and 1:6. From the Fourier transform infra-red (FTIR) spectra, the band appears at 542.71 cm - 1 and 432.48 cm - 1 , which corresponding to metal⁻oxygen bending and the vibration of the octahedral sites of BaFe12O19. The field emission scanning electron microscope (FESEM) images show that the grains of the samples appear to stick each other and agglomerate at different masses throughout the image with the grain size 5.26, 5.88, 6.14, 6.22, and 6.18 µm for the ratios 1:3, 1:4, 1:5, 1:6, and 1:7 respectively. From the vibrating sample magnetometer (VSM) analysis, the magnetic properties of the sample ratio at 1:3 show the highest value of coercivity Hc of 1317 Oe, a saturation magnetization Ms of 91 emu/g, and a remnant Mr of 44 emu/g, respectively. As the temperature rises, the AC conductivity is increases with an increase in frequency.
Fulltext Down-top nanofabrication of binary (CdO)x (ZnO)1-x nanoparticles and their antibacterial activity

Al-Hada NM, Mohamed Kamari H, Abdullah CAC, Saion E, Shaari AH, Talib ZA, et al.

Int J Nanomedicine, 2017;12:8309-8323.
PMID: 29200844 DOI: 10.2147/IJN.S150405

In the present study, binary oxide (cadmium oxide [CdO])x (zinc oxide [ZnO])1-x nanoparticles (NPs) at different concentrations of precursor in calcination temperature were prepared using thermal treatment technique. Cadmium and zinc nitrates (source of cadmium and zinc) with polyvinylpyrrolidone (capping agent) have been used to prepare (CdO)x (ZnO)1-x NPs samples. The sample was characterized by X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. XRD patterns analysis revealed that NPs were formed after calcination, which showed a cubic and hexagonal crystalline structure of (CdO)x (ZnO)1-x NPs. The phase analysis using EDX spectroscopy and FTIR spectroscopy confirmed the presence of Cd and Zn as the original compounds of prepared (CdO)x (ZnO)1-x NP samples. The average particle size of the samples increased from 14 to 33 nm as the concentration of precursor increased from x=0.20 to x=0.80, as observed by TEM results. The surface composition and valance state of the prepared product NPs were determined by X-ray photoelectron spectroscopy (XPS) analyses. Diffuse UV-visible reflectance spectra were used to determine the optical band gap through the Kubelka-Munk equation; the energy band gap was found to decrease for CdO from 2.92 to 2.82 eV and for ZnO from 3.22 to 3.11 eV with increasing x value. Additionally, photoluminescence (PL) spectra revealed that the intensity in PL increased with an increase in particle size. In addition, the antibacterial activity of binary oxide NP was carried out in vitro against Escherichia coli ATCC 25922 Gram (-ve), Salmonella choleraesuis ATCC 10708, and Bacillus subtilis UPMC 1175 Gram (+ve). This study indicated that the zone of inhibition of 21 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.
Fulltext A facile thermal-treatment route to synthesize ZnO nanosheets and effect of calcination temperature

Al-Hada NM, Saion EB, Shaari AH, Kamarudin MA, Flaifel MH, Ahmad SH, et al.

PLoS One, 2014;9(8):e103134.
PMID: 25093752 DOI: 10.1371/journal.pone.0103134

A facile thermal-treatment route was successfully used to synthesize ZnO nanosheets. Morphological, structural, and optical properties of obtained nanoparticles at different calcination temperatures were studied using various techniques. The FTIR, XRD, EDX, SEM and TEM images confirmed the formation of ZnO nanosheets through calcination in the temperature between 500 to 650 °C. The SEM images showed a morphological structure of ZnO nanosheets, which inclined to crumble at higher calcination temperatures. The XRD and FTIR spectra revealed that the samples were amorphous at 30 °C but transformed into a crystalline structure during calcination process. The average particle size and degree of crystallinity increased with increasing calcination temperature. The estimated average particle sizes from TEM images were about 23 and 38 nm for the lowest and highest calcination temperature i.e. 500 and 650 °C, respectively. The optical properties were determined by UV-Vis reflection spectrophotometer and showed a decrease in the band gap with increasing calcination temperature.
Fulltext Superconducting Properties of YBa2Cu3O7-δ with a Multiferroic Addition Synthesized by a Capping Agent-Aided Thermal Treatment Method

Dzul-Kifli NAC, Kechik MMA, Baqiah H, Shaari AH, Lim KP, Chen SK, et al.

Nanomaterials (Basel), 2022 Nov 10;12(22).
PMID: 36432245 DOI: 10.3390/nano12223958

A bulk YBa2Cu3O7-δ (Y-123) superconductor synthesized by a thermal treatment method was added with different weight percentages (x = 0.0, 0.2, 1.0, 1.5, and 2.0 wt.%) of BiFeO3 (BFO) nanoparticle. X-ray diffraction (XRD), alternating current susceptibility (ACS), and field emission scanning electron microscopy (FESEM) were used to determine the properties of the samples. From the XRD results, all samples showed an orthorhombic crystal structure with a Pmmm space group. The sample x = 1.0 wt.% gave the highest value of Y-123. The high amounts of BFO degraded the crystallite size of the sample, showing that the addition did not promote the grain growth of Y-123. From ACS results, the Tc-onset value was shown to be enhanced by the addition of the BFO nanoparticle, where x = 1.5 wt.% gave the highest Tc value (91.91 K). The sample with 1.5 wt.% showed a high value of Tp (89.15 K). The FESEM analysis showed that the average grain size of the samples decreased as BFO was introduced. However, the small grain size was expected to fill in the boundary, which would help in enhancing the grain connectivity. Overall, the addition of the BFO nanoparticles in Y-123 helped to improve the superconducting properties, mainly for x = 1.5 wt.%.

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