A solution combustion process for the synthesis of hollandite (BaAl2Ti6O16) powders is described. SYNROC (synthetic rock) consists of four main titanate phases: perovskite, zirconolite, hollandite and rutile. Hollandite is one of the crystalline host matrices used for the disposal of high-level radioactive wastes because it immobilizes Sr and Lns elements by forming solid solutions. The solution combustion synthesis, which is a self-sustaining oxi-reduction reaction between a nitrate and organic fuel, generates an exothermic reaction and that heat converts the precursors into their corresponding oxide products in air. The process has high energy efficiency, fast heating rates, short reaction times, and high compositional homogeneity. To confirm the combustion synthesis reaction, FT-IR analysis was conducted using glycine with a carboxyl group and an amine as fuel to observe its bonding with metal element in the nitrate. TG-DTA, X-ray diffraction analysis, SEM and EDS were performed to confirm the formed phases and morphology. Powders with an uncontrolled shape were obtained through a general oxide-route process, confirming hollandite powders with micro-sized soft agglomerates consisting of nano-sized primary particles can be prepared using these methods.

A mono-type glycerine fatty acid ester compound was chemically synthesized using medium-chain fatty acids with antibacterial activity, and the physicochemical quality and antibacterial activity of the synthesized glycerine medium-chain fatty acid ester compound were measured. At a reaction molar ratio of MCT(medium chain triglyceride) to glycerine of 1:2.5, 48.15% mono ester was produced. The physicochemical analysis of the synthesized glycerine fatty acid ester compound showed an acid content of 0.38~0.60%, which tended to increase slightly as the glycerine molar ratio increased. The saponification value decreased as the synthesized molar ratio of glycerine increased from 218 to 284. The number of bacteria was measured to confirm the degree of antibacterial activity of glycerine medium-chain fatty acid esters against food poisoning bacteria, Bacillus cereus and Salmonella typhi. The number of bacteria significantly decreased as the MCT:glycerine molar ratio increased. In particular, the antibacterial effect between the treatment groups was the highest when at an MCT:glycerine molar ratio of 1:2.5.

장대교량은 낮은 고유진동수와 감쇠비를 가지는 초유연구조물로 진동사용성 문제에 취약하다. 하지만 현재 국내 설계지침에서는 풍속이나 진폭에 대한 임계값을 기반으로 유해진동 발생 여부를 평가하고 있다. 본 연구에서는 장대교량에서 발생하는 유해진동을 보다 정교하게 식별하기 위하여 딥러닝 기반 신호분할 모델을 활용한 데이터 포인트 단위의 와류진동 식별 방법론을 제안한다. 특별 히 포락선을 가지는 사인파를 활용하여 와류진동에 해당하는 데이터를 합성함으로써 모델 구축에 필수적인 와류진동 데이터 획득 및 라벨링 과정을 대체하였다. 이후 푸리에 싱크로스퀴즈드 변환를 적용하여 시간-주파수 특징을 추출하여 신경망의 인풋 데이터로 사 용하였다. 합성데이터만을 이용하여 양방향 장단기 기억신경망(Bidirectional Long-Short-Term-Memory) 모델을 훈련하였고 이를 라 벨 정보를 포함한 실제 사장교의 계측데이터를 이용하여 학습한 모델과 비교하여 모델의 실시간 와류진동 식별 성능을 검증하였다.

3-(2-브로모에틸)인돌을 사용한 2-에티닐피리딘의 4차염화 중합을 통해 새로운 이온성 폴리아세틸렌 유도체 를 합성하였다. 3-(2-브로모에틸)인돌을 사용한 2-에티닐피리딘의 중합은 균일하게 진행되었으며 비교적 높은 수율 로 중합체를 합성할 수 있었다(78%). 3-(2-브로모에틸)인돌에 의한 2-에티닐피리딘의 4차염화 반응에 의해 형성된 N-(3-에틸인돌)-2-에티닐피리디늄 브로마이드의 활성화된 아세틸렌 삼중 결합은 별도의 개시제나 촉매 없이도 중합 반응이 잘 진행됨을 알 수 있었다. 여러 가지 분석 장비를 이용하여 중합체의 구조를 확인한 결과 설계한 인돌 치 환기를 갖는 공액구조 고분자가 생성되었음을 확인할 수 있었다. 이 중합체는 DMF, DMAc, DMSO 등과 같은 극성 유기 용매에 잘 용해하였다. 중합체는 가시광선 영역인 457 nm에서 특징적인 흡수 피크, 600 nm에서 엣지 파장 을 보였다. 중합체의 사이클릭 볼타모그램은 산화와 환원 피크 사이에서 안정한 비가역적 전기화학 거동을 나타내 었다. 스캔 속도가 증가할수록 환원 전류량이 증가하였으며 주 환원 및 산화 피크는 -1.3 V 및 1.1 V에서 관찰되었 다.

In this work, we investigated a modern combined processing technique for the synthesis of lightweight superhard composites based on boron–carbon. We used traditional B4C with precipitates of free graphite and Al powder as initial materials. In the first stage, the composites were fabricated by the self-propagating high-temperature synthesis (SHS) with the subsequent hot pressing of the compound. Further, by the disintegration and attrition milling, the ultrafine-grained powder was obtained. We used HCl and HNO3 acids for the chemical leaching of the powder to remove various impure compounds. At the last stage, a solid composite was obtained by the spark plasma sintering (SPS) method under nitrogen pressure. The main feature of this approach is to implement different synthesis techniques and chemical leaching to eliminate soft phases and to obtain superhard compounds from low-cost materials. The phases were studied by X-ray diffraction and scanning electron microscopy with energy-dispersive spectroscopy. The composites compacted by the SPS method contained superhard compounds such as B13C2, B11.7C3.3, and c-BN. The fabricated composite has an ultrafine-grained microstructure. Using a Berkovich indenter, the following nanohardness results were achieved: B13C2 ~ 43 GPa, c-BN ~ 65 GPa (all in Vickers scale) along with a modulus of elasticity ranging between ~ 400 GPa and ~ 450 GPa.

Lithium (Li) is a key resource driving the rapid growth of the electric vehicle industry globally, with demand and prices continually on the rise. To address the limited reserves of major lithium sources such as rock and brine, research is underway on seawater Li extraction using electrodialysis and Li-ion selective membranes. Lithium lanthanum titanate (LLTO), an oxide solid electrolyte for all-solid-state batteries, is a promising Li-ion selective membrane. An important factor in enhancing its performance is employing the powder synthesis process. In this study, the LLTO powder is prepared using two synthesis methods: sol-gel reaction (SGR) and solid-state reaction (SSR). Additionally, the powder size and uniformity are compared, which are indices related to membrane performance. X-ray diffraction and scanning electron microscopy are employed for determining characterization, with crystallite size analysis through the full width at half maximum parameter for the powders prepared using the two synthetic methods. The findings reveal that the powder SGR-synthesized powder exhibits smaller and more uniform characteristics (0.68 times smaller crystal size) than its SSR counterpart. This discovery lays the groundwork for optimizing the powder manufacturing process of LLTO membranes, making them more suitable for various applications, including manufacturing high-performance membranes or mass production of membranes.

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 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.

Selective doping of pyridinic nitrogen in carbon materials has attracted attention due to its significant properties for various applications such as catalysts and electrodes. However, selective doping of pyridinic nitrogen together with controlling skeletal structure is challenging in the absence of catalysts. In this work, four precursors including four fused aromatic rings and pyridinic nitrogen were simply carbonized in the absence of catalysts in order to attain mass synthesis at low cost and a high percentage of pyridinic nitrogen in carbon materials with controlled edges. Among four precursors, dibenzo[f,h] quinoline (DQ) showed an extremely high percentage of pyridinic nitrogen (96 and 86%) after heat treatment at 923 and 973 K, respectively. Experimental spectroscopic analyses combined with calculated spectroscopic analyses using density functional theory calculations unveiled that the C-H next to the pyridinic nitrogen in DQ generated gulf edge structures with controlled pyridinic nitrogen after carbonization. By comparing the reactivities among the four precursors, three main factors required for maintaining the pyridinic nitrogen in carbon materials with controlled edges, such as (1) high thermal stability of the pyridinic nitrogen, (2) the presence of one pyridinic nitrogen in one ring, and (3) the formation of gulf edges including pyridinic nitrogen to protect the pyridinic nitrogen by the C-H groups on the gulf edges, were revealed.

How to effectively deal with the polluted water by the pollutant of organic dyes is the world problem. It is of great significance if the organic dyes in the polluted water can be directly turned into the useful materials through a facile approach. Herein, the water which contains the common organic dye, Reactive red 2 (RR2), has been chosen to be the model to synthesize graphene quantum dots (GQDs) by a facile route. The comprehensive characterizations, including TEM (HRTEM), XPS, Raman, PL and UV–Vis. spectra, have been performed to confirm the structures and explore the properties of the synthesized GQDs. Meanwhile, the excellent PL properties and low biotoxicity of the GQDs confer them with the potential applications in the biological fields. When the GQDs are excited by the wavelength of 360 nm, the maximum emission is achieved at 428 nm. It is well demonstrated that the synthesized GQDs are able to detect the Al3+ which causes multiple diseases, such as Parkinson, Alzheimer, kidney disease, and even cancer. The detection range is from 90 to 800 μM, which is different from the reported kinds of the literature. Therefore, this work not only provides an economical and environmental route on solving the universal problem from organic dyes, but also facilitates to advancing the synthesis and application of GQDs.

In this work, subabul wood biomass was used to prepare carbon adsorbents by physical and chemical activation methods at various carbonization temperatures. The properties of the carbon adsorbents were estimated through characterization techniques such as X-ray diffraction, Fourier transform infrared spectroscopy, X–ray photo electron spectroscopy, laser Raman spectroscopy, scanning electron microscopy, CHNS-elemental analysis and N2 adsorption studies. Subabul-derived carbon adsorbents were used for CO2 capture in the temperature range of 25–70 °C. A detailed adsorption kinetic study was also carried out. The characterization results indicated that these carbons contain high surface area with microporosity. Surface properties were depended on treatment method and carbonization temperature. Among the carbons, the carbon prepared after treatment of H3PO4 and carbonization at 800 °C exhibited high adsorption capacity of 4.52 m.mol/g at 25 °C. The reason for high adsorption capacity of the adsorbents was explained based on their physicochemical characteristics. The adsorbents showed easy desorption and recyclability up to ten cycle with consistent activity.

Medicinal plant-derived carbon dots are eco-friendly and possess therapeutic properties. Among the medicinal plants studied throughout the world, Centella asiatica (L.) Urb. is known for its medicinal values, especially its neuroceutical and cogniceutical properties. This work discusses the green synthesis of carbon dots (CDs) using C. asiatica leaves as the carbon source via fast and cost-effective microwave-assisted method, and its physico-chemical characterization via UV–visible, fluorescence and FTIR spectrometry, XRD, SEM, AFM, TEM, SAED, EDX and zeta potential analyses. The study revealed quasi-spherical CDs having size ~ 3–6 nm, polycrystalline nature, and presence of various functional groups like –COOH, –H, =CH2 and C–O–C with UV absorption peaks at 213 and 322 nm. Interestingly, the C. asiatica-derived CDs exhibited blue fluorescence under UV with maximum emission wavelength of 460 nm when excited at 400 nm. Further, these CDs were evaluated for their biological applications, which uncovered their potential in therapeutics such as antimicrobial properties against both Gram-positive and Gram-negative bacteria at a dose of 10 μg, strong antioxidant activity with IC50 values of 165.28 and 128.48 μg mL− 1 in DPPH and H2O2 assays, respectively, and profound anti-inflammatory activity with IC50 value of 106.20 μg mL− 1 in protein denaturation assay. The CDs were also assessed for cytotoxicity using whole blood cells and were found to be safe for in vitro administration. Thus, the C. asiatica-derived CDs can be exploited for their potent biomedicinal properties. Fluorescent carbon dots (CDs) were prepared by microwave-assisted pyrolysis of Centella asiatica leaf extract and purification. The as synthesized CDs were subjected to various physico-chemical characterization and biomedical assays to understand its properties.

Ammonium (NH4 +) serves as a nitrogen source, but its elevated levels can hinder plant growth and production. Excess NH4 + with α-ketoglutarate is assimilated into glutamate, a precursor of proline and glutathione (GSH). This study aimed to investigate the effects of excessive NH4 + on the regulation of proline and GSH synthesis. Detached leaves from oilseed rape (Brassica napus L.) were fed with 0, 50, 100, 500, and 1000 mM NH4Cl for 16 h. As the NH4 + concentrations increased, the leaves exhibited progressive wilting and yellowing. Furthermore, total carotenoid and chlorophyll concentrations declined in response to all NH4 + treatments, with the lowest levels observed in 1000 mM NH4 + treatment. Hydrogen peroxide (H2O2) concentration showed a minor increase at low NH4 + concentration (50 and 100 mM) treatments but a significant increase at high NH4 + (500 and 1000 mM), which was consistent with the localization of H2O2. Amino acid concentrations increased with increasing in NH4 + concentration, while the protein concentration displayed the opposite trend. Proline and cysteine concentrations exhibited a gradual increase in response to increasing NH4 + concentrations. However, GSH concentrations rose only in the 50 mM NH4 + treatment and decreased in the 500 and 1000 mM NH4 + treatments. These results indicate that excessive NH4 + is primarily assimilated into proline, while GSH synthesis is adversely affected.

To develop a high capacity lithium secondary battery, a new approach to anode material synthesis is required, capable of producing an anode that exceeds the energy density limit of a carbon-based anode. This research synthesized carbon nano silicon composites as an anode material for a secondary battery using the RF thermal plasma method, which is an ecofriendly dry synthesis method. Prior to material synthesis, a silicon raw material was mixed at 10, 20, 30, 40, and 50 wt% based on the carbon raw material in a powder form, and the temperature change inside the reaction field depending on the applied plasma power was calculated. Information about the materials in the synthesized carbon nano silicon composites were confirmed through XRD analysis, showing carbon (86.7~52.6 %), silicon (7.2~36.2 %), and silicon carbide (6.1~11.2 %). Through FE-SEM analysis, it was confirmed that the silicon bonded to carbon was distributed at sizes of 100 nm or less. The bonding shape of the silicon nano particles bonded to carbon was observed through TEM analysis. The initial electrochemical charging/ discharging test for the 40 wt% silicon mixture showed excellent electrical characteristics of 1,517 mAh/g (91.9 %) and an irreversible capacity of 133 mAh/g (8.1 %).

In this study, we evaluated the effects of acid leaching on the properties of Cr powder synthesized using self-propagating high-temperature synthesis (SHS). Cr powder was synthesized from a mixture of Cr2O3 and magnesium (Mg) powders using the SHS Process, and the byproducts after the reaction were removed using acid leaching. The properties of the recovered Cr powder were analyzed via X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), particle size analysis (PSA), and oxygen content analysis. The results show that perfect selective leaching of Cr is challenging because of various factors such as incomplete reaction, reaction kinetics, the presence of impurities, and incompatibility between the acid and metal mixture. Therefore, this study provides essential information on the properties under acidic conditions during the production of high-quality Cr powder using a self-propagating high-temperature synthesis method.

본 연구에서는 현탁중합을 통해 이온교환입자를 합성하였다. 또한 음이온 교환막을 제조하기 위해 brominated poly(phenylene oxide) (Br-PPO)로 교환막 합성을 진행하였으며, 합성한 이온교환입자를 Br-PPO에 첨가하여 음이온 교환막 에 성능을 향상시키고자 하였고, 이를 적용하여 음이온 교환막 연료전지 시스템의 성능 평가를 진행했다. 이온교환입자는 FT-IR, TGA 및 UTM을 통해 구조 분석, 열적 기계적 특성을 평가하였다. Br-PPO는 NMR을 통해 화학적 구조 분석 및 합성 여부를 확인하였고, 음이온 교환막 연료 전지 셀 테스트를 진행하기 전 이온전도도와 이온교환용량, 팽윤도 및 수분함수율을 측정해 연구되고 있는 다른 음이온 교환막들과 비교를 통해 성능을 평가했다. 최종적으로 가장 성능이 우수했던 이온교환입 자를 0.7 wt%를 첨가한 Br-PPO-TMA- SDV 음이온 교환막을 연료전지 시스템에 도입하여 상용 막인 FAA-3-50과 성능을 비 교했다.

Mass production of high-quality carbon nanotubes (CNTs) remains a challenge, requiring the development of new wetimpregnated catalyst suitable for the catalytic chemical vapor deposition (CCVD) of CNTs in a fluidized bed reactor. For the successful development of a new catalyst, a highly robust system to synthesize CNTs must be established. Here, we systematically investigated the robustness of CNT synthesis by CCVD using a wet-impregnated catalyst. We statistically tested four factors that could potentially affect the robustness of CNT synthesis system, focusing on carbon yield and IG/ID. First, we tested the effect of vacuum baking before CNT growth. F test and CV equality test concluded that vacuum baking recipe did not significantly reduce the variability of the CNT synthesis. Second, we tested the batch-to-batch variation of catalysts. The results of t test and one-way analysis of variance indicate that there is significant difference in carbon yield and IG/ID among catalysts from different batches. Third, we confirmed that there is spatial non-uniformity of wet-impregnated catalysts within a batch when they are produced in large scale. Finally, we developed a multi-step heating recipe to mitigate the temperature overshooting during the CNT synthesis. The multi-step recipe increased the mean of carbon yield, but did not influence the variability of CNT synthesis. We believe that our research can contribute to the establishment of a robust CNT synthesis system and development of new wet-impregnated catalysts.

Biomass-derived porous carbon is an excellent scientific and technologically interesting material for supercapacitor applications. In this study, we developed biomass-derived nitrogen-doped porous carbon nanosheets (BDPCNS) from cedar cone biomass using a simple KOH activation and pyrolysis method. The BDPCNS was effectively modified at different temperatures of 600 °C, 700 °C, and 800 ℃ under similar conditions. The as-prepared BDPCNS-700 electrode exhibited a high BET surface area of 2883 m2 g− 1 and a total pore volume of 1.26 cm3 g− 1. Additionally, BDPCNS-700 had the highest electrical conductivity (11.03 cm− 1) and highest N-doped content among the different electrode materials. The BDPCNS-700 electrode attained a specific capacitance of 290 F g− 1 at a current density of 1 A g− 1 in a 3 M KOH electrolyte and an excellent longterm electrochemical cycling stability of 93.4% over 1000 cycles. Moreover, the BDPCNS-700 electrode had an excellent energy density (40.27 Wh kg− 1) vs power density (208.19 W kg− 1). These findings indicate that BDPCNS with large surface areas are promising electrode materials for supercapacitors and energy storage systems.

In this study platform, electrocatalytic detection of the antibiotic chloramphenicol (CAP) in phosphate buffer (pH 7) was easily achieved using a carbon paste electrode modified with NiO nanoparticles (note NiO-CPE). The peak reduction potential of chloramphenicol on the modified electrode is at (− 0.60 V/NiO-CPE vs. Ag/AgCl), its electrochemical behavior is completely irreversible, and controlled by adsorption phenomena. An excellent electrocatalytic activity has been demonstrated by the modified elaborated electrode towards the NO2 attracting group on the side chain of chloramphenicol. The structure and chemical composition of the NiO-CPE sensor were analyzed by SEM, and the X-ray diffraction results indicated that nickel oxide microcrystals were formed on the carbon sheets. The electrochemical characteristics of the NiO-CPE sensor were examined by cyclic voltammetry and electrochemical impedance spectroscopy in comparison with the unmodified carbon. Since the DPV technique allows plotting the linearity curve between the electrocatalytic current intensity of the Chloramphenicol peak and their concentration, the proposed sensor showed a remarkable detection limit of 1.08 × 10– 8 mol/L M (S/N = 3) and a wide determination range from 100 to 0.1 μM for Chloramphenicol. The developed sensor was successfully applied in the detection of Chloramphenicol in real samples.

Graphene oxide/Iron III oxide (GO: Fe2O3) nanocomposites (NCs) have been topical in recent times owing to the enhanced properties they exhibit. GO acting as a graphene derivative has demonstrated superior features as obtainable in a graphene sheet. Furthermore, the attachment of oxygen functional groups at its basal and edge planes of graphene has allowed for easy metal/oxide functionalization for improved properties harvesting. Fe2O3 nanoparticles (NPs) on the other hand have polymorphic property enabling the degeneracy of Fe2O3 in different phases, thereby resulting in different physical and crystalline properties when used to functionalize GO. The properties of GO: Fe2O3 have been applied to supercapacitor energy harvesting, Li-ion batteries, and biomedicine. The enhanced properties are attributed to the adsorption and electronic structure properties of Fe atoms. In this review, the various synthesis used in the preparation of reduced/graphene oxide: Fe2O3 is discussed. As indicated in the considered literature, the XPS analysis suggests electronic bond interactions between C–C, C–O, C–Fe and Fe–C. The available report on UPS measurements further suggests the formation of mixed states emanating from  and  bonds. The discussed reports further suggest that the various applications based on the harvesting of electronic, electrical, and magnetic properties are due to the ionic and exchange interactions between the different orbital states of carbon, oxygen and iron. The challenges and future prospects of the synthesis and application of GO/Fe2O3 are examined. Graphical abstract showing the process of exfoliation, reduction and functionalization of graphite to produce reduced graphene oxide (rGO).