In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H2SO4/SiO2 as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO2 was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 °C. SiO2 with a 200-mesh size was impregnated with 98 % H2SO4 by mixing for 1 h. The resulting 33 % (w/w) H2SO4/SiO2 catalyst was separated by centrifugation, dried, and calcined at 600 °C. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 °C for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H2SO4/SiO2 could generate an average benzene conversion of 40.33 %.
In this study, based on the saturation magnetic flux density experimental values (Bs) of 622 Fe-based bulk metallic glasses (BMGs), regression models were applied to predict Bs using artificial neural networks (ANN), and prediction performance was evaluated. Model performance evaluation was investigated by using the F1 score together with the coefficient of determination (R2 score), which is mainly used in regression models. The coefficient of determination can be used as a performance indicator, since it shows the predicted results of the saturation magnetic flux density of full material datasets in a balanced way. However, the BMG alloy contains iron and requires a high saturation magnetic flux density to have excellent applicability as a soft magnetic material, and in this study F1 score was used as a performance indicator to better predict Bs above the threshold value of Bs (1.4 T). After obtaining two ANN models optimized for the R2 and F1 score conditions, respectively, their prediction performance was compared for the test data. As a case study to evaluate the prediction performance, new Fe-based BMG datasets that were not included in the training and test datasets were predicted using the two ANN models. The results showed that the model with an excellent F1 score achieved a more accurate prediction for a material with a high saturation magnetic flux density.
One-dimensional MgO nanostructures with various morphologies were synthesized by a thermal evaporation method. The synthesis process was carried out in air at atmospheric pressure, which made the process very simple. A mixed powder of magnesium and active carbon was used as the source powder. The morphologies of the MgO nanostructures were changed by varying the growth temperature. When the growth temperature was 700 °C, untapered nanowires with smooth surfaces were grown. As the temperature increased to 850 °C, 1,000 °C and 1,100 °C, tapered nanobelts, tapered nanowires and then knotted nanowires were sequentially observed. X-ray diffraction analysis revealed that the MgO nanostructures had a cubic crystallographic structure. Energy dispersive X-ray analysis showed that the nanostructures were composed of Mg and O elements, indicating high purity MgO nanostructures. Fourier transform infrared spectra peaks showed the characteristic absorption of MgO. No catalyst particles were observed at the tips of the one-dimensional nanostructures, which suggested that the one-dimensional nanostructures were grown in a vapor-solid growth mechanism.
Porous ceramics are used in various industrial applications based on their physical properties, including isolation, storage, and thermal barrier properties. However, traditional manufacturing environments require additional steps to control artificial pores and limit deformities, because they rely on limited molding methods. To overcome this drawback, many studies have recently focused on fabricating porous structures using additive manufacturing techniques. In particular, the binder jet technology enables high porosity and various types of designs, and avoids the limitations of existing manufacturing processes. In this study, we investigated process optimization for manufacturing porous ceramic filters using the binder jet technology. In binder jet technology, the flowability of the powder used as the base material is an important factor, as well as compatibility with the binder in the process and for the final print. Flow agents and secondary binders were used to optimize the flowability and compatibility of the powders. In addition, the effects of the amount of added glass frit, and changes in sintering temperature on the microstructure, porosity and mechanical properties of the final printed product were investigated.
Thermoelectric (TE) energy harvesting, which converts available thermal resources into electrical energy, is attracting significant attention, as it facilitates wireless and self-powered electronics. Recently, as demand for portable/wearable electronic devices and sensors increases, organic-inorganic TE films with polymeric matrix are being studied to realize flexible thermoelectric energy harvesters (f-TEHs). Here, we developed flexible organic-inorganic TE films with p-type Bi0.5Sb1.5Te3 powder and polymeric matrices such as poly(3,4-eethylenedioxythiophene):poly(styrene sulfonate) (PEDOT:PSS) and poly (vinylidene fluoride) (PVDF). The fabricated TE films with a PEDOT:PSS matrix and 1 wt% of multi-walled carbon nanotube (MWCNT) exhibited a power factor value of 3.96 μW ‧ m-1 ‧ K-2 which is about 2.8 times higher than that of PVDF-based TE film. We also fabricated f-TEHs using both types of TE films and investigated the TE output performance. The f-TEH made of PEDOT:PSS-based TE films harvested the maximum load voltage of 3.4 mV, with a load current of 17.4 μA, and output power of 15.7 nW at a temperature difference of 25 K, whereas the f-TEH with PVDF-based TE films generated values of 0.6 mV, 3.3 μA, and 0.54 nW. This study will broaden the fields of the research on methods to improve TE efficiency and the development of flexible organic-inorganic TE films and f-TEH.
The influence of specimen geometry and notch on the hydrogen embrittlement of an SA372 steel for pressure vessels was investigated in this study. A slow strain-rate tensile (SSRT) test after the electrochemical hydrogen charging method was conducted on four types of tensile specimens with different directions, shapes (plate, round), and notches. The plate-type specimen showed a significant decrease in hydrogen embrittlement resistance owing to its large surface-to-volume ratio, compared to the round-type specimen. It is well established that most of the hydrogen distributes over the specimen surface when it is electrochemically charged. For the round-type specimens, the notched specimen showed increased hydrogen susceptibility compared with the unnotched one. A notch causes stress concentration and thus generates lots of dislocations in the locally deformed regions during the SSRT test. The solute hydrogen weakens the interactions between these dislocations by promoting the shielding effect of stress fields, which is called hydrogen-enhanced localized plasticity mechanisms. These results provide crucial insights into the relationship between specimen geometry and hydrogen embrittlement resistance.
This study aimed to address the limitations of traditional plasma nitriding methods by implementing a short-term plasma oxy-nitriding treatment on the surface of AISI 420 martensitic stainless steel. This treatment involved the sequential formation of nitride and oxide layers, to enhance surface hardness and corrosion resistance, respectively. The process resulted in the formation of a 20 μm-thick nitride layer and a 3 μm-thick oxide layer on the steel surface. Initially, the hardness increased by 2.2 times after nitriding, followed by a subsequent decrease of approximately 31 % after oxidation. While the nitriding process reduced corrosion resistance, the subsequent oxidation process led to the formation of a passive oxide film, effectively resolving this issue. The pitting corrosion of the oxide passive film started at 82.6 mVssc, providing better corrosion resistance characteristics than the nitride layer. Consequently, the trade-off between surface hardness and corrosion resistance in plasma oxy-nitrided AISI 420 martensitic stainless steel is anticipated to be recognized as an innovative and comprehensive surface treatment process for biomedical components.
In the present work, we address the new route for the green synthesis of manganese dioxide (MnO2) by an innovative method named the solution plasma process (SPP). The reaction mechanism of both colloidal and nanostructured MnO2 was investigated. Firstly, colloidal MnO2 was synthesized by plasma discharging in KMnO4 aqueous solution without any additives such as reducing agents, acids, or base chemicals. As a function of the discharge time, the purple color solution of MnO4 - (oxidation state +7) was changed to the brown color of MnO2 (oxidation state +4) and then light yellow of Mn2+ (oxidation state +2). Based on the UV-vis analysis we found the optimal discharging time for the synthesis of stable colloidal MnO2 and also reaction mechanism was verified by optical emission spectroscopy (OES) analysis. Secondly, MnO2 nanoparticles were synthesized by SPP with a small amount of reducing sugar. The precipitation of brown color was observed after 8 min of plasma discharge and then completely separated into colorless solution and precipitation. It was confirmed layered type of nanoporous birnessite- MnO2 by X-ray powder diffraction (XRD), fourier-transform infrared spectroscopy (FT-IR), and electron microscopes. The most important merits of this approach are environmentally friendly process within a short time compared to the conventional method. Moreover, the morphology and the microstructure could be controllable by discharge conditions for the appropriate potential applications, such as secondary batteries, supercapacitors, adsorbents, and catalysts.