The present study examines the synthesis of Co3O4 ultra-nanosheets (Co3O4 UNSs) and Co3O4 ultra-nanosheet-Ni(OH)2 (Co3O4 UNS-Ni(OH)2) via solvothermal process and their application as non-enzymatic electrochemical sensors for glucose detection. X-ray diffraction and transmission electron microscopy results confirmed the Co3O4 UNS deposition on Ni(OH)2 surface. The presence of Co3O4 UNSs on Ni (OH) 2 surface improved the sensitivity of glucose detection, from the increase of glucose oxidation peak current at the Co3O4 UNS-Ni(OH)2/glassy carbon electrode (current density: 2000μA·cm(-2)), compared to the Co3O4 UNSs. These results confirmed that Ni(OH)2 on glassy carbon electrode is a sensitive material for glucose detection, moreover the Co3O4 UNSs can increase the interaction and detection of glucose due to their high surface area. The estimated limit of detection (S/N=3) and limit of quantification (S/N=10) of the linear segment (5-40μM) are 1.08μM and 3.60μM respectively. The reproducibility experiments confirmed the feasibility of Co3O4 UNS-Ni(OH)2 for the quantitative detection of certain concentration ranges of glucose.
In this letter, we investigate the fabrication of Silicon nanostructure patterned on lightly doped (10(15) cm(-3)) p-type silicon-on-insulator by atomic force microscope nanolithography technique. The local anodic oxidation followed by two wet etching steps, potassium hydroxide etching for silicon removal and hydrofluoric etching for oxide removal, are implemented to reach the structures. The impact of contributing parameters in oxidation such as tip materials, applying voltage on the tip, relative humidity and exposure time are studied. The effect of the etchant concentration (10% to 30% wt) of potassium hydroxide and its mixture with isopropyl alcohol (10%vol. IPA ) at different temperatures on silicon surface are expressed. For different KOH concentrations, the effect of etching with the IPA admixture and the effect of the immersing time in the etching process on the structure are investigated. The etching processes are accurately optimized by 30%wt. KOH +10%vol. IPA in appropriate time, temperature, and humidity.
Herbicides, namely 4-(2,4-dichlorophenoxy) butyrate (DPBA) and 2-(3-chlorophenoxy) propionate (CPPA), were intercalated simultaneously into the interlayers of zinc layered hydroxide (ZLH) by direct reaction of zinc oxide with both anions under aqueous environment to form a new nanohybrid containing both herbicides labeled as ZCDX. Successful intercalation of both anions simultaneously into the interlayer gallery space of ZLH was studied by PXRD, with basal spacing of 28.7 Å and supported by FTIR, TGA/DTG and UV-visible studies. Simultaneous release of both CPPA and DPBA anions into the release media was found to be governed by a pseudo second-order equation. The loading and percentage release of the DPBA is higher than the CPPA anion, which indicates that the DPBA anion was preferentially intercalated into and released from the ZLH interlayer galleries. This work shows that layered single metal hydroxide, particularly ZLH, is a suitable host for the controlled release formulation of two herbicides simultaneously.
Rechargeable zinc-air batteries are deemed as the most feasible alternative to replace lithium-ion batteries in various applications. Among battery components, separators play a crucial role in the commercial realization of rechargeable zinc-air batteries, especially from the viewpoint of preventing zincate (Zn(OH)42-) ion crossover from the zinc anode to the air cathode. In this study, a new hydroxide exchange membrane for zinc-air batteries was synthesized using poly (2,6-dimethyl-1,4-phenylene oxide) (PPO) as the base polymer. PPO was quaternized using three tertiary amines, including trimethylamine (TMA), 1-methylpyrolidine (MPY), and 1-methylimidazole (MIM), and casted into separator films. The successful synthesis process was confirmed by proton nuclear magnetic resonance and Fourier-transform infrared spectroscopy, while their thermal stability was examined using thermogravimetric analysis. Besides, their water/electrolyte absorption capacity and dimensional change, induced by the electrolyte uptake, were studied. Ionic conductivity of PPO-TMA, PPO-MPY, and PPO-MIM was determined using electrochemical impedance spectroscopy to be 0.17, 0.16, and 0.003 mS/cm, respectively. Zincate crossover evaluation tests revealed very low zincate diffusion coefficient of 1.13 × 10-8, and 0.28 × 10-8 cm2/min for PPO-TMA, and PPO-MPY, respectively. Moreover, galvanostatic discharge performance of the primary batteries assembled using PPO-TMA and PPO-MPY as initial battery tests showed a high specific discharge capacity and specific power of ~800 mAh/gZn and 1000 mWh/gZn, respectively. Low zincate crossover and high discharge capacity of these separator membranes makes them potential materials to be used in zinc-air batteries.
Multi-walled carbon nanotubes (MWCNTs) were prepared via chemical vapor deposition (CVD) using a series of different catalysts, derived from FeCoNiAl, CoNiAl and FeNiAl layered double hydroxides (LDHs). Catalyst-active particles were obtained by calcination of LDHs at 800 °C for 5 h. Nitrogen and hexane were used as the carrier gas and carbon source respectively, for preparation of MWCNTs using CVD methods at 800 °C. MWCNTs were allowed to grow for 30 min on the catalyst spread on an alumina boat in a quartz tube. The materials were subsequently characterized through X-ray diffraction, Fourier transform infrared spectroscopy, surface area analysis, field emission scanning electron microscopy and transmission electron microscopy. It was determined that size and yield of MWCNTs varied depending on the type of LDH catalyst precursor that is used during synthesis. MWCNTs obtained using CoNiAl-LDH as the catalyst precursor showed smaller diameter and higher yield compared to FeCoNiAl and FeNiAl LDHs.
Steam explosion of oil palm frond has been carried out under different temperatures between 180 and 210°C for 4 min (severity of 2.96-3.84) after impregnation of the frond chips with water or KOH solution. The effects of impregnation and steam explosion conditions of oil palm fronds on the water soluble fraction and insoluble fraction were investigated. The maximum yield of hemicelluloses in water soluble fractions recovered was 23.49% and 25.33% for water and KOH impregnation, treated with steam explosion at temperature of 210°C (severity of 3.84) with a fractionation efficiency of 77.30% and 83.32%, respectively. Under this condition, the water insoluble fractions contained celluloses at 60.83% and 64.80% for water and KOH impregnation, respectively. The steam explosion temperature of 210°C for 4 min (logR(o) 3.84) was found to be the best condition in the extraction of hemicelluloses from OPF for both types of impregnation.
The preparation of chars and activated carbon as low-cost elemental mercury adsorbents was carried out through the carbonisation of coconut husk (pith and fibre) and the activation of chars with potassium hydroxide (KOH), respectively. The synthesised adsorbents were characterised by using scanning electron microscopy, Fourier transform infrared spectroscopy and nitrogen adsorption/desorption analysis. The elemental mercury removal performance was measured using a conventional flow type packed-bed adsorber. The physical and chemical properties of the adsorbents changed as a result of the carbonisation and activation process, hence affecting on the extent of elemental mercury adsorption. The highest elemental mercury (Hg°) adsorption capacity was obtained for the CP-CHAR (3142.57 µg g(-1)), which significantly outperformed the pristine and activated carbon adsorbents, as well as higher than some adsorbents reported in the literature.
A drug-inorganic nanostructured material involving pharmaceutically active compound lawsone intercalated Zn-Al layered double hydroxides (Law-LDHs) with Zn/AI = 4 has been assembled by co-precipitation and ion exchange methods. Powder X-ray diffraction (XRD) and Fourier transform infrared spectra (FTIR) analysis indicate a successful intercalation of lawsone between the layers of layered double hydroxides. It suggests that layered double hydroxides may have application as the basis of a drug delivery system.
Rice husk (RH), an abundant by-product of rice milling, was used for the preparation of activated carbon (RHAC) via KOH and K(2)CO(3) chemical activation. The activation process was performed at the microwave input power of 600 W for 7 min. RHACs were characterized by low temperature nitrogen adsorption/desorption, scanning electron microscopy and Fourier transform infrared spectroscopy. The adsorption behavior was examined using methylene blue as adsorbate. The K(2)CO(3)-activated sample showed higher yield and better pore structures and adsorption capacity development than the KOH-activated sample, with a BET surface area, total pore volume and monolayer adsorption capacity of 1165 m(2)/g, 0.78 cm(3)/g and 441.52 mg/g, respectively. The results revealed the feasibility of microwave heating for preparation of high surface area activated carbons from rice husks via K(2)CO(3) activation.
Fatty acid methyl ester was produced from used vegetable cooking oil using Mg(1-)(x) Zn(1+)(x)O(2) solid catalyst and the performance monitored in terms of ester content obtained. Used vegetable cooking oil was employed to reduce operation cost of biodiesel. The significant operating parameters which affect the overall yield of the process were studied. The highest ester content, 80%, was achieved with the catalyst during 4h 15 min reaction at 188°C with methanol to oil ratio of 9:1 and catalyst loading of 2.55 wt% oil. Also, transesterification of virgin oil gave higher yield with the heterogeneous catalyst and showed high selectivity towards ester production. The used vegetable cooking oil did not require any rigorous pretreatment. Catalyst stability was examined and there was no leaching of the active components, and its performance was as good at the fourth as at the first cycle.
In this study, a novel continuous reactor has been developed to produce high quality methyl esters (biodiesel) from palm oil. A microporous TiO2/Al2O3 membrane was packed with potassium hydroxide catalyst supported on palm shell activated carbon. The central composite design (CCD) of response surface methodology (RSM) was employed to investigate the effects of reaction temperature, catalyst amount and cross flow circulation velocity on the production of biodiesel in the packed bed membrane reactor. The highest conversion of palm oil to biodiesel in the reactor was obtained at 70 °C employing 157.04 g catalyst per unit volume of the reactor and 0.21 cm/s cross flow circulation velocity. The physical and chemical properties of the produced biodiesel were determined and compared with the standard specifications. High quality palm oil biodiesel was produced by combination of heterogeneous alkali transesterification and separation processes in the packed bed membrane reactor.
In this study, solidification/stabilization (S/S) of nickel hydroxide sludge using ordinary Portland cement (OPC) and oil palm ash (OPA) was carried out. The effects of increased substitution of OPA wt% in the S/S mix designs on the treated samples' physical and chemical characteristics were investigated. The physical characteristics studied were unconfined compressive strength (UCS) and changes in crystalline phases while chemical characteristics studied were leachability of nickel and leachate pH. Results indicated the optimum mix design for S/S of nickel hydroxide sludge using both OPC and OPA at B/S(d)=1 in terms of cost-effectiveness and treatment efficiency was 15 wt% OPA, 35 wt% OPC and 50 wt% sludge. The sufficient UCS and low leached nickel concentrations shown for this mix design indicate the viability of using OPA as substitute of OPC as it can significantly reduce cost normally incurred by usage of high amounts of OPC.
Activated carbon was prepared from coconut husk using physicochemical activation method which consisted of potassium hydroxide (KOH) treatment and carbon dioxide (CO(2)) gasification. The effects of three preparation variables (CO(2) activation temperature, CO(2) activation time and KOH:char impregnation ratio) on the 2,4,6-trichlorophenol (2,4,6-TCP) uptake and activated carbon yield were investigated. Based on the central composite design, two quadratic models were developed to correlate the preparation variables to the two responses. From the analysis of variance (ANOVA), the most influential factor on each experimental design response was identified. The activated carbon preparation conditions were optimized by maximizing both the 2,4,6-TCP uptake and activated carbon yield. The predicted 2,4,6-TCP uptake and carbon yield from the models agreed satisfactorily with the experimental values. The optimum conditions for preparing activated carbon from coconut husk for adsorption of 2,4,6-TCP were found as follow: CO(2) activation temperature of 750 degrees C, CO(2) activation time of 2.29 h and KOH:char impregnation ratio of 2.91, which resulted in 191.73 mg/g of 2,4,6-TCP uptake and 20.16 % of activated carbon yield.
In this work, preparation of granular activated carbon from oil palm biodiesel solid residue, oil palm shell (PSAC) by microwave assisted KOH activation has been attempted. The physical and chemical properties of PSAC were characterized using scanning electron microscopy, volumetric adsorption analyzer and elemental analysis. The adsorption behavior was examined by performing batch adsorption experiments using methylene blue as dye model compound. Equilibrium data were simulated using the Langmuir, Freundlich and Temkin isotherm models. Kinetic modeling was fitted to the pseudo-first-order, pseudo-second-order and Elovich kinetic models, while the adsorption mechanism was determined using the intraparticle diffusion and Boyd equations. The result was satisfactory fitted to the Langmuir isotherm model with a monolayer adsorption capacity of 343.94mg/g at 30°C. The findings support the potential of oil palm shell for preparation of high surface area activated carbon by microwave assisted KOH activation.
Layered double hydroxide of Mg-Al-carbonate system (MACH) was prepared and its heat-treated product (MACHT) was obtained by calcination at 500 degrees C. The resulting materials were used as an adsorbent for removal of color from synthetic textile wastewater (STW) and textile wastewater (TWW). Batch kinetic study showed that these materials are an efficient adsorbent for textile dye. The maximum adsorption capacities between 16 to 32 mg of dyes per g of adsorbent was obtained by fitting the adsorption data to the Langmuir adsorption Isotherm. It was found that the adsorption capacity of MACHT is higher than MACH.
Hybridization of beneficial organic guest with inorganic host affords scientists an opportunity to synthesize various combinations of new organic-inorganic nanohybrids with various potential applications, especially for controlled delivery of beneficial agent and storage. A new layered organic-inorganic nanohybrid material containing an agrochemical, 4-(2,4-dichlorophenoxy)butyrate (DPBA) in Zn-Al-layered double hydroxide inorganic interlayer was synthesised by direct and indirect methods. Both methods yielded mesoporous-type, phase pure, well-ordered layered nanohybrids with similar basal spacing of 28.5-28.7 angstroms and organic loading of around 54.3%. Compared to the material prepared by direct method, the ion exchanged product inherited more of the host's properties especially the pore structure and the organic moiety is also more easily released. This shows that the method of preparation plays an important role in determining the resulting physicochemical properties, in particular the release property and therefore can be used as a means to tune up the release property of the beneficial agent.
Metanilate-layered double hydroxide nanohybrid compound was synthesized for controlled release purposes through co-precipitation method of the metal cations and organic anion. The effect of various divalent metal cations (M2+), namely Zn2+, Mg2+ and Ca2+ on the formation of metanilate-LDH nanohybrids, in which metanilate anion was intercalated into three different layered double hydroxide (LDH) systems; Zn-Al, Mg-Al and Ca-Al were investigated. The syntheses were carried out with M2+ to Al3+ initial molar ratio, R of 4. The pH of the mother liquor was maintained at pH 7.5 and 10 during the synthesis, and the resulting mixture was aged at around 70 degrees C for about 18 h. The intercalation of metanilate anion into the host was found to be strongly influenced by the M2+ that formed the inorganic metal hydroxide layers. Under our experimental condition, the formation of the nanohybrid materials was found to be more feasible for the Zn-Al than for the other two systems, in which the former showed well-ordered layered organic-inorganic nanohybrid structure with good crystallinity. Intercalation is confirmed by the expansion of the interlayer spacing to about 15-17 A when metanilate was introduced into the interlamellae of Zn-Al LDHs. In addition, CHNS and FTIR analyses also support that metanilate anion has been successfully intercalated into the interlamellae of the inorganic LDH. Apart from M2+, this study also shows that the initial pH of the mother liquor plays an important role in determining the physicochemical properties of the resulting nanohybrids, especially the mole fraction of the Zn2+ substituted by the Al3+ ion in the LDH inorganic sheets which in turn controlled the loading percentage of the organic anion, surface properties and the true density. Preliminary study shows that LDH can be used to host beneficial guests, active agent with controlled release capability of the guests. Generally the overall process is governed by pseudo second order kinetic but for the first 180 min, the release process can be slightly better described by parabolic diffusion than the other models.
A label-free chemical bonding strategy mediated by reduced graphene oxide (rGO) basal plane functional groups has been developed for cardiac Troponin I (cTnI) detection. Four different chemical strategies on respective electrode sensing surface were precedingly examined using electrochemical impedance spectroscopy. The impedimetric assessment was carried out by sweeping frequency at the range 0.1-500 kHz perturbated at a small amplitude of AC voltage (25 mV). The chemical strategy-4 denoted as S-4 shows a significant analytical performance on cTnI detection in spiked buffer and human serum, whereby the pre-mixture of rGO and (3-Aminopropyl)triethoxysilane (APTES) creates a large number of amine sites (-NH2), which significantly enhanced the antibody immobilization without excessive functionalization. The as-fabricated immunosensor exhibited an ultra-low limit of detection of 6.3 ag mL-1 and the lowest antigen concentration measured was at 10 ag mL-1. The immunosensor showed a linear and wide range of cTnI detection (10 ag mL-1-100 ng mL-1) in human serum with a regression coefficient of 0.9716, rapid detection (5 min of binding time), and stable and highly reproducible bioelectrode response with RSD
To develop a novel granular adsorbent to remove arsenic and antimony from water, calcined Mg/Al-layered double-hydroxide (CLDH)-incorporated polyethersulfone (PES) granular adsorbents (PES-LDH) were prepared using a core-shell method having 25% PES in an N,N-dimethylformamide solution. The PES-LDH displayed a spherical hollow shape having a rough surface and the average particle size of 1-2 mm. On the PES-LDH surface, nanosized CLDH (100-150 nm) was successfully immobilized by consolidation between PES and CLDH. The adsorption of Sb(V) by PES-LDH was found to be more favorable than for As(V), with the maximum adsorption capacity of As(V) and Sb(V) being 7.44 and 22.8 mg/g, respectively. The regeneration results indicated that a 0.5 M NaOH and 5 M NaCl mixed solution achieved an 80% regeneration efficiency in As(V) adsorption and desorption. However, the regeneration efficiency of Sb(V) gradually decreased due to its strong binding affinity, even though the PES-LDH showed much higher Sb(V) adsorption efficiency than As(V). This study suggested that PES-LDH could be a promising granular adsorbent for the remediation of As(V) and Sb(V) contained in wastewater.
The potential of solar cells have not been fully tapped due to the lack of energy conversion efficiency. There are three important mechanisms in producing high efficiency cells to harvest solar energy; reduction of light reflectance, enhancement of light trapping in the cell and increment of light absorption. The current work represent studies conducted in surface modification of single-crystalline silicon solar cells using wet chemical etching techniques. Two etching types are applied; alkaline etching (KOH:IPA:DI) and acidic etching (HF:HNO3:DI). The alkaline solution resulted in anisotropic profile that leads to the formation of inverted pyramids. While acidic solution formed circular craters along the front surface of silicon wafer. This surface modification will leads to the reduction of light reflectance via texturizing the surface and thereby increases the short circuit current and conversion rate of the solar cells.