Search results for: microwave-assisted synthesis

Authors: Shalini Arora, Sri Sivakumar

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The deep removal of high molecular weight sulphur compounds (e.g., 4,6, dimethyl dibenzothiophene) is challenging due to their steric hindrance. Hydrogenation desulfurization (HYD) pathway is the main pathway to remove these sulfur compounds, and it is mainly governed by the number of type 2 sites. The formation of type 2 sites can be enhanced by modulating the pore structure and the interaction between the active metal and support. To this end, we report the enhanced HDS catalytic activity of ultrasmall NiMo supported on amorphous alumina (A-Al₂O₃) catalysts by one pot colloidal synthesis method followed by calcination and sulfidation. The amorphous alumina (A-Al₂O₃) was chosen as the support due to its lower surface energy, better physicochemical properties, and enhanced acidic sites (due to the dominance of tetra and penta coordinated [Al] sites) than crystalline alumina phase. At 20% metal oxide composition, NiMo supported on A-Al₂O₃ catalyst showed 1.4 and 1.2 times more reaction rate constant and turn over frequency (TOF) respectively than the conventional catalyst (wet impregnated NiMo catalysts) for HDS reaction of dibenzothiophene reactant molecule. A-Al₂O₃ supported catalysts represented enhanced type 2 sites formation (because this catalystpossesses higher sulfidation degree (80%) and NiMoS sites (19.3 x 10¹⁷ sites/mg) with desired optimum stacking degree (2.5) than wet impregnated catalyst at same metal oxide composition 20%) along with higher active metal dispersion, Mo edge site fraction. The experimental observations were also supported by DFT simulations. Lower heat of adsorption (< 4.2 ev for MoS2 interaction and < 3.15 ev for Ni doped MoS2 interaction) values for A-Al₂O₃ confirmed the presence of weaker metal-support interaction in A-Al₂O₃ in contrast to crystalline ℽ-Al₂O3. The weak metal-support interaction for prepared catalysts clearly suggests the higher formation of type 2 sites which leads to higher catalytic activity for HDS reaction.

Keywords: amorphous alumina, colloidal, desulfurization, metal-support interaction

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Authors: Masoumeh Ghorbania, Falk Liebnerb, Hendrikus W.G. van Herwijnenc, Johannes Konnertha

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Phenol formaldehyde (PF) resins are widely used as wood adhesives for variety of industrial products such as plywood, laminated veneer lumber and others. Lignin as a main constituent of wood has become well-known as a potential substitute for phenol in PF adhesives because of their structural similarity. During the last decades numerous research approaches have been carried out to substitute phenol with pulping-derived lignin, whereby the lower reactivity of resins synthesized with shares of lignin seem to be one of the major challenges. This work reports about a systematic screening of different types of lignin (plant origin and pulping process) for their suitability to replace phenol in phenolic resins. Lignin from different plant sources (softwood, hardwood and grass) were used, as these should differ significantly in their reactivity towards formaldehyde of their reactive phenolic core units. Additionally a possible influence of the pulping process was addressed by using the different types of lignin from soda, kraft, and organosolv process and various lignosulfonates (sodium, ammonium, calcium, magnesium). To determine the influence of lignin on the adhesive performance beside others the rate of viscosity development, bond strength development of varying hot pressing time and other thermal properties were investigated. To evaluate the performance of the cured end product, a few selected properties were studied at the example of solid wood-adhesive bond joints, compact panels and plywood. As main results it was found that lignin significantly accelerates the viscosity development in adhesive synthesis. Bonding strength development during curing of adhesives decelerated for all lignin types, while this trend was least for pine kraft lignin and spruce sodium lignosulfonate. However, the overall performance of the products prepared with the latter adhesives was able to fulfill main standard requirements, even after exposing the products to harsh environmental conditions. Thus, a potential application can be considered for processes where reactivity is less critical but adhesive cost and product performance is essential.

Keywords: phenol formaldehyde resin, lignin phenol formaldehyde resin, ABES, DSC

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Authors: Harriet Koshie Lamptey, Richard Boateng

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Mobile learning (m-learning) is a novel approach to knowledge acquisition and dissemination and is gaining global attention. Steady progress in wireless technologies and the portability of communication devices continue to broaden the scope and use of mobiles. With the convergence of Web functionality onto mobile platforms and the affordability and availability of mobile technology, m-learning has the potential of being the next prevalent channel of education in both formal and informal settings. There is substantive literature on developed countries but the state in developing countries (DCs) however appears vague. This paper is a synthesis of extant literature on mobile learning in DCs. The research interest is based on the fact that in DCs, mobile communication and internet connectivity are popular. However, its use in education is under explored. There are some reviews on the state, conceptualizations, trends and teacher education, but to the authors’ knowledge, no study has focused on mobile learning adoption and integration issues. This study examines issues and gaps associated with its adoption and integration in DCs higher education institutions. A qualitative build-up of literature was conducted using articles pooled from electronic databases (Google Scholar and ERIC). To enable criteria for inclusion and incorporate diverse study perspectives, search terms used were m-learning, DCs, higher education institutions, challenges, benefits, impact, gaps and issues. The synthesis revealed that though mobile technology has diffused globally, its pedagogical pursuit in DCs remains quite low. The absence of a mobile Web and the difficulty of resource conversion into mobile format due to lack of funding and technical competence is a stumbling block. Again, the lack of established design and implementation rules to guide the development of m-learning platforms in DCs is a hindrance. The absence of access restrictions on devices poses security threats to institutional systems. Negative perceptions that devices are taking over faculty roles lead to resistance in some situations. Resistance to change can be a hindrance to the acceptance and success of new systems. Lack of interest for m-learning is also attributed to lower technological literacy levels of the underprivileged masses. Scholarly works on m-learning in DCs is yet to mature. Most technological innovations are handed down from developed countries, and this constantly creates a lag for DCs. Lack of theoretical grounding was also identified which reduces the objectivity of study reports. The socio-cultural terrain of DCs results in societies with different views and needs that have been identified as a hindrance to research. Institutional commitment decisions, adequate funding for the necessary infrastructural development as well as multiple stakeholder participation is important for project success. Evidence suggests that while adoption decisions are readily made, successful integration of the concept for its full benefits to be realized is often neglected. Recommendations to findings were made to provide possible remedies to identified issues.

Keywords: developing countries, higher education institutions, mobile learning, literature review

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Authors: Julie Mariam Abraham, G. J. Melendez-Torres

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Background. Maternal mortality is disproportionately higher in low- and middle- income countries (LMICs) compared to other parts of the world. At the current pace of progress, the Sustainable Development Goals for maternal mortality rate will not be achieved by 2030. A variety of factors influence the increased risk of maternal complications in LMICs. These are exacerbated by socio-economic and political factors, including poverty, illiteracy, and gender inequality. This paper aims to use realist synthesis to identify the contexts, mechanisms, and outcomes (CMOs) of maternal health interventions conducted in LMICs to inform evidence-based practice for future maternal health interventions. Methods. In May 2022, we searched four electronic databases for systematic reviews of maternal health interventions in LMICs published in the last five years. We used open and axial coding of CMOs to develop an explanatory framework for intervention effectiveness. Results. After eligibility screening and full-text analysis, 44 papers were included. The intervention strategies and measured outcomes varied within reviews. Healthcare system level contextual factors were the most frequently reported, and infrastructural capacity was the most reported context. The most prevalent mechanism was increased knowledge and awareness. Discussion. Health system infrastructure must be considered in interventions to ensure effective implementation and sustainability. Healthcare-seeking behaviours are embedded within social and cultural norms, environmental conditions, family influences, and provider attitudes. Therefore, effective engagement with communities and families is important to create new norms surrounding pregnancy and delivery. Future research should explore community mobilisation and involvement to enable tailored interventions with optimal contextual fit.

Keywords: maternal mortality, service delivery and organisation, realist synthesis, sustainable development goals, overview of reviews

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Authors: Sh. Sohrabnezhad, A. Jafarzadeh

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In this paper, MCM-41 mesoporous material nanofibers were synthesized by an electrospinning technique. The nanofibers were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray diffraction (XRD), and nitrogen adsorption–desorption measurement. Tetraethyl orthosilicate (TEOS) and polyvinyl alcohol (PVA) were used as a silica source and fiber forming source, respectively. TEM and SEM images showed synthesis of MCM-41 nanofibers with a diameter of 200 nm. The pore diameter and surface area of calcined MCM-41 nanofibers was 2.2 nm and 970 m²/g, respectively. The morphology of the MCM-41 nanofibers depended on spinning voltages.

Keywords: electrospinning, electron microscopy, fiber technology, porous materials, X-ray techniques

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Authors: Roghaye Behroozi

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The development of functionalized metal complexes and nanomaterials has gained significant attention due to their potential in catalyzing selective oxidation and coupling reactions. These catalysts play a crucial role in various industrial and pharmaceutical processes, enhancing the efficiency, selectivity, and sustainability of chemical reactions. This research aims to design and synthesize new functionalized metal complexes and nanomaterials to explore their catalytic applications in the selective oxidation of alcohols and coupling reactions, focusing on improving yield, selectivity, and catalyst reusability. The study involves the synthesis of a nickel Schiff base complex stabilized within 41-MCM as a heterogeneous catalyst. A Schiff base ligand derived from glycine was used to create a tin (IV) metal complex characterized through spectroscopic techniques and computational analysis. Additionally, iron-based magnetic nanoparticles functionalized with melamine were synthesized for catalytic evaluation. Lastly, a palladium (IV) complex was prepared, and its oxidative stability was analyzed. The nickel Schiff base catalyst showed high selectivity in converting primary and secondary alcohols to aldehydes and ketones, with yields ranging from 73% to 90%. The tin (IV) complex demonstrated accurate structural and electronic properties, with consistent results between experimental and computational data. The melamine-functionalized iron nanoparticles exhibited efficient catalytic activity in producing triazoles, with enhanced reaction speed and reusability. The palladium (IV) complex displayed remarkable stability and low reactivity towards C–C bond formation due to its symmetrical structure. The synthesized metal complexes and nanomaterials demonstrated significant potential as efficient, selective, and reusable catalysts for oxidation and coupling reactions. These findings pave the way for developing environmentally friendly and cost-effective catalytic systems for industrial applications.

Keywords: catalysts, Schiff base complexes, metal-organic frameworks, oxidation reactions, nanoparticles, reusability

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Authors: Jitlada Chumee, Drenpen Seeburin

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The cellulose was extracted from pomelo peel and an etherification reaction used for converting cellulose to carboxymethyl cellulose (CMC). The pomelo peel was refluxed with 0.5 M HCl and 1 M NaOH solution at 90°C for 1 h and 2 h, respectively. The cellulose was bleached with calcium hypochlorite and used as precursor. The precursor was soaked in mixed solution between isopropyl alcohol and 40%w/v NaOH for 12 h. After that, chloroacetic acid was added and reacted at 55°C for 6 h. The optimum condition was 5 g of cellulose: 0.25 mole of NaOH : 0.07 mole of ClCH2COOH with 78.00% of yield. Moreover, the product had 0.54 of degree of substitution (DS).

Keywords: pomelo peel, carboxymethyl cellulose, bioplastic, extraction

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Authors: Flora Elvistia Firdaus

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The chemical structure of soybean oils have to be chemically modified through its tryglyceride to attain resemblance properties with petrochemicals. Sulfur acid catalyst in peracetic acid co-reagent has good performance on modified soybean oil strucutures through its unsaturated fatty acid moiety to the desired hydroxyl functional groups. A series of screening reactions have indicated that the ratio of acetic/peroxide acid 1:7.25 (mol/mol) with temperature of 600°C for soy-epoxide synthesis are prevailed for up-scaling of bodied soybean into 10 and 20 folds from initials. A two-step process was conducted for the preparation of soy-polyol in designated temperatures.

Keywords: soybean, polyol, up-scaling, polyurethane

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Authors: Evelyn Osehontue Uroro, Richard Bright, Jing Yang Quek, Krasimir Vasilev

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Bacterial infections have been a challenge both in the public and private sectors. The colonization of bacteria often occurs in medical devices such as catheters, heart valves, respirators, and orthopaedic implants. When biomedical devices are inserted into patients, the deposition of macromolecules such as fibrinogen and immunoglobin on their surfaces makes it easier for them to be prone to bacteria colonization leading to the formation of biofilms. The formation of biofilms on medical devices has led to a series of device-related infections which are usually difficult to eradicate and sometimes cause the death of patients. These infections require surgical replacements along with prolonged antibiotic therapy, which would incur additional health costs. It is, therefore, necessary to prevent device-related infections by inhibiting the formation of biofilms using intelligent technology. Antibiotic resistance of bacteria is also a major threat due to overuse. Different antimicrobial agents have been applied to microbial infections. They include conventional antibiotics like rifampicin. The use of conventional antibiotics like rifampicin has raised concerns as some have been found to have hepatic and nephrotoxic effects due to overuse. Hence, there is also a need for proper delivery of these antibiotics. Different techniques have been developed to encapsulate and slowly release antimicrobial agents, thus reducing host cytotoxicity. Examples of delivery systems are solid lipid nanoparticles, hydrogels, micelles, and polymeric nanoparticles. The different ways by which drugs are released from polymeric nanoparticles include diffusion-based release, elution-based release, and chemical/stimuli-responsive release. Polymeric nanoparticles have gained a lot of research interest as they are basically made from biodegradable polymers. An example of such a biodegradable polymer is polycaprolactone (PCL). PCL degrades slowly by hydrolysis but is often sensitive and responsive to stimuli like enzymes to release encapsulants for antimicrobial therapy. This study presents the synthesis of PCL nanoparticles loaded with rifampicin and the on-demand release of rifampicin for treating staphylococcus aureus infections.

Keywords: enzyme, Staphylococcus aureus, PCL, rifampicin

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Authors: Z. Kolacinski, L. Szymanski. G. Raniszewski, D. Koza, L. Pietrzak

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Magnetic Bio-Nano-Fluid (BNF) can be composed of a buffer fluid such as plasma and magnetic nanoparticles such as iron, nickel, cobalt and their oxides. However iron is one of the best elements for magnetization by electromagnetic radiation. It can be used as a tool for medical diagnosis and treatment. Radio frequency (RF) radiation is able to heat iron nanoparticles due to magnetic hysteresis. Electromagnetic heating of iron nanoparticles and ferro-fluids BNF can be successfully used for non-invasive thermal ablation of cancer cells. Moreover iron atoms can be carried by carbon nanotubes (CNTs) if iron is used as catalyst for CNTs synthesis. Then CNTs became the iron containers and they screen the iron content against oxidation. We will present a method of CNTs addressing to the required cells. For thermal ablation of cancer cells we use radio frequencies for which the interaction with human body should be limited to minimum. Generally, the application of RF energy fields for medical treatment is justified by deep tissue penetration. The highly iron doped CNTs as the carriers creating magnetic fluid will be presented. An excessive catalyst injection method using electrical furnace and microwave plasma reactor will be presented. This way it is possible to grow the Fe filled CNTs on a moving surface in continuous synthesis process. This also allows producing uniform carpet of the Fe filled CNTs carriers. For the experimental work targeted to cell ablation we used RF generator to measure the increase in temperature for some samples like: solution of Fe2O3 in BNF which can be plasma-like buffer, solutions of pure iron of different concentrations in plasma-like buffer and in buffer used for a cell culture, solutions of carbon nanotubes (MWCNTs) of different concentrations in plasma-like buffer and in buffer used for a cell culture. Then the targeted therapies which can be effective if the carriers are able to distinguish the difference between cancerous and healthy cell’s physiology are considered. We have developed an approach based on ligand-receptor or antibody-antigen interactions for the case of colon cancer.

Keywords: cancer treatment, carbon nano tubes, drag delivery, hyperthermia, iron

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Authors: Mehmet Doğan, Mahir Alkan, Yasemin Turhan, Zürriye Gündüz, Pinar Beyli, Serap Doğan

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Advances and new discoveries in the field of the material science on the basis of technological developments have played an important role. Today, material science is branched the lower branches such as metals, nonmetals, chemicals, polymers. The polymeric nano composites have found a wide application field as one of the most important among these groups. Many polymers used in the different fields of the industry have been desired to improve the thermal stability. One of the ways to improve this property of the polymers is to form the nano composite products of them using different fillers. There are many using area of boron compounds and is increasing day by day. In order to the further increasing of the variety of using area of boron compounds and industrial importance, it is necessary to synthesis of nano-products and to find yourself new application areas of these products. In this study, PMMA/boronoxide nano composites were synthesized using solution intercalation, polymerization and melting methods; and PAA/boronoxide nano composites using solution intercalation method. Furthermore, rheological properties of nano composites synthesed according to melting method were also studied. Nano composites were characterized by XRD, FTIR-ATR, DTA/TG, BET, SEM, and TEM instruments. The effects of filler material amount, solvent types and mediating reagent on the thermal stability of polymers were investigated. In addition, the rheological properties of PMMA/boronoxide nano composites synthesized by melting method were investigated using High Pressure Capillary Rheometer. XRD analysis showed that boronoxide was dispersed in polymer matrix; FTIR-ATR that there were interactions with boronoxide between PAA and PMMA; and TEM that boronoxide particles had spherical structure, and dispersed in nano sized dimension in polymer matrix; the thermal stability of polymers was increased with the adding of boronoxide in polymer matrix; the decomposition mechanism of PAA was changed. From rheological measurements, it was found that PMMA and PMMA/boronoxide nano composites exhibited non-Newtonian, pseudo-plastic, shear thinning behavior under all experimental conditions.

Keywords: boronoxide, polymer, nanocomposite, rheology, characterization

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Authors: Héctor González Espinosa, Ricardo Ivan Cordova Chávez, Alejandra Contreras Ramos, Itzia Irene Padilla Martínez, José Guadalupe Trujillo Ferrara, Marvin Antonio Soriano Ursúa

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Boronic acids are able to create diester bonds with carbohydrates because of their hydroxyl groups; in nature, there are some organoborates with these characteristics, such as the calcium fructoborate, formed by the union of two fructose molecules and a boron atom, synthesized by plants. In addition, it has been observed that, in animal cells only the compounds with cis-diol functional groups are capable of linking to boric or boronic acids. The formation of these organoboron compounds could impair the physical and chemical properties of the precursors, even their acute toxicity. In this project, two carbohydrate-derived boron-containing compounds from D-fructose and D-arabinose and phenylboronic acid are analyzed by different spectroscopy techniques such as Raman, Infrared with Fourier Transform Infrared (FT-IR), Nuclear Magnetic Resonance (NMR) and X-ray diffraction crystallography to describe their chemical characteristics. Also, an acute toxicity test was performed to determine their LD50 using the Lorke’s method. It was confirmed by multiple spectra the formation of the adducts by the generation of the diester bonds with a β-D-pyranose of fructose and arabinose. The most prominent findings were the presence of signals corresponding to the formation of new bonds, like the stretching of B-O bonds, or the absence of signals of functional groups like the hydroxyls presented in the reagents used for the synthesis of the adducts. The NMR spectra yielded information about the stereoselectivity in the synthesis reaction, observed by the interaction of the protons and their vicinal atoms in the anomeric and second position carbons; but also, the absence of a racemic mix by the finding of just one signal in the range for the anomeric carbon in the 13C NMR spectra of both adducts. The acute toxicity tests by the Lorke’s method showed that the LD50 value for both compounds is 1265 mg/kg. Those results let us to propose these adducts as highly safe agents for further biological evaluation with medical purposes.

Keywords: acute toxicity, adduct, boron, carbohydrate, diester bond

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Authors: Vadim V. Zefirov, Victor E. Sizov, Marina A. Pigaleva, Igor V. Elmanovich, Mikhail S. Kondratenko, Marat O. Gallyamov

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This work presents a novel method for treating porous hydrophobic polyolefin membranes using supercritical carbon dioxide that allows usage of the modified membrane in redox flow batteries with an aqueous electrolyte. Polyolefin membranes are well known and widely used, however, they cannot be used as separators in redox flow batteries with an aqueous electrolyte since they have insufficient wettability, and therefore do not provide sufficient proton conductivity. The main aim of the presented work was the development of hydrophilic composites based on cheap membranes and precursors. Supercritical fluid was used as a medium for the deposition of the hydrophilic phase on the hydrophobic surface of the membrane. Due to the absence of negative capillary effects in a supercritical medium, a homogeneous composite is obtained as a result of synthesis. The in-situ synthesized silicon oxide nanoparticles and the chitosan polymer layer act as the hydrophilic phase and not only increase the affinity of the membrane towards the electrolyte, but also reduce the pore size of the polymer matrix, which positively affects the ion selectivity of the membrane. The composite material obtained as a result of synthesis has enhanced hydrophilic properties and is capable of providing proton conductivity in redox flow batteries. The morphology of the obtained composites was characterized by electron microscopy. To analyze the phase composition, infrared spectroscopy was used. The hydrophilic properties were studied by water contact angle measurements. In addition, the proton conductivity and ion selectivity of the obtained samples were studied, and tests in real redox flow batteries were performed. As a result, modified membrane was characterised in detail and moreover it was shown that modified cheap polyolefin membranes have pronounced proton conductivity and high ion selectivity, so their performance in a real redox flow battery approaches expensive commercial analogues, reaching 70% of energy efficiency.

Keywords: carbon dioxide, chitosan, polymer membrane, redox flow batteries, silica nanoparticles, supercritical fluid

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Authors: Nastaran Hazrati, Ali Akbar Miran Beigi, Majid Abdouss, Amir Vahid

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Hydrogen sulfide is the most toxic gas of crude oil. Adsorption is an energy-efficient process used to remove undesirable compounds such as H2S in gas or liquid streams by passing the stream through a media bed composed of an adsorbent. In this study, H2S of Iran crude oil was separated via cold stripping then zinc incorporated MCM-41 was synthesized via an in-situ method. ZnO functionalized mesoporous silica samples were characterized by XRD, N2 adsorption and TEM. The obtained results of adsorption of H2S showed superior ability of all the materials and with an increase in ZnO amount adsorption was increased.

Keywords: MCM-41, ZnO, H2S removal, adsorption

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Authors: Seungmin Shin, Jin-Baek Kim

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Hematite (α-Fe2O3) has very good semiconducting properties with a band gap of 2.1 eV and is antiferromagnetic. Due to its electrochemical stability, low toxicity, wide abundance, and low-cost, hematite, it is a particularly attractive material for photoelectrochemical cells. Additionally, hematite has also found applications in gas sensing, field emission, heterogeneous catalysis, and lithium-ion battery electrodes. Here, we discovered a new universal top-down method for the synthesis of one-dimensional hematite nanowire arrays. Various shapes and lengths of hematite nanowire have been easily fabricated over large areas by sequential processes. The obtained hematite nanowire arrays are promising candidates as photoanodes in photoelectrochemical solar cells.

Keywords: hematite, lithography, nanowire, top-down process

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Authors: S. Varnagiris, M. Urbonavicius, S. Tuckute, M. Lelis, K. Bockute

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Amongst many water purification techniques, TiO₂ photocatalysis is recognized as one of the most promising sustainable methods. It is known that for photocatalytical applications anatase is the most suitable TiO₂ phase, however heterojunction of anatase/rutile phases could improve the photocatalytical activity of TiO₂ even further. Despite the relative simplicity of TiO₂ different synthesis methods lead to the highly dispersed crystal phases and photocatalytic activity of the corresponding samples. Accordingly, suggestions and investigations of various innovative methods of TiO₂ synthesis are still needed. In this work structural and photocatalytical properties of TiO₂ films deposited by the unconventional method of simultaneous co-sputtering from two magnetrons powered by pulsed-Direct Current (pDC) and Radio Frequency (RF) power sources with negative bias voltage have been studied. More specifically, TiO₂ film thickness, microstructure, surface roughness, crystal structure, optical transmittance and photocatalytical properties were investigated by profilometer, scanning electron microscope, atomic force microscope, X-ray diffractometer and UV-Vis spectrophotometer respectively. The proposed unconventional two magnetron co-sputtering based TiO₂ film formation method showed very promising results for crystalline TiO₂ film formation while keeping process temperatures below 100 °C. XRD analysis revealed that by using proper combination of power source type and bias voltage various TiO₂ phases (amorphous, anatase, rutile or their mixture) can be synthesized selectively. Moreover, strong dependency between power source type and surface roughness, as well as between the bias voltage and band gap value of TiO₂ films was observed. Interestingly, TiO₂ films deposited by two magnetron co-sputtering without bias voltage had one of the highest band gap values between the investigated films but its photocatalytic activity was superior compared to all other samples. It is suggested that this is due to the dominating nanocrystalline anatase phase with various exposed surfaces including photocatalytically the most active {001}.

Keywords: films, magnetron co-sputtering, photocatalysis, TiO₂

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Authors: M. Obaid, Nasser A. M. Barakat, Fadali O.A

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Low stability in oil media and the hydrophobicity problems of the ploysulfone electrospun membranes could be overcome in the present study. Synthesis of super-hydrophilic and highly stable in oil polysulfone electrospun nanofiber membrane was achieved by electrospinning of polysulfone solution containing NaOH salt followed by activation of the dried electrospun membrane by deposition of polyamide layer on the surface using m-phenylenediamine and 1,3,5-benzenetricarbonyl chloride. The introduced membrane has super-hydrophilicity characteristic (contact angle=3o), excellent stability in oil media and distinct performance in oil-water separation process.

Keywords: electrospinning, oil-degradability, membrane, nanofibers

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Authors: Hanan. Al Chaghouri, Mohammad Azad Malik, P. John Thomas, Paul O’Brien

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The process of assembling metal nanoparticles at the interface of two liquids has received a great interest over the past few years due to a wide range of important applications and their unusual properties compared to bulk materials. We present a low cost, simple and cheap synthesis of metal nanoparticles, core/shell structures and semiconductors followed by assembly of these particles between immiscible liquids. The aim of this talk is divided to three parts: firstly, to describe the achievement of a closed loop recycling for producing cadmium sulphide as powders and/or nanostructured thin films for solar cells or other optoelectronic devices applications by using a different chain length of commercially available secondary amines of dithiocarbamato complexes. The approach can be extended to other metal sulphides such as those of Zn, Pb, Cu, or Fe and many transition metals and oxides. Secondly, to synthesis significantly cheaper magnetic particles suited for the mass market. Ni/NiO nanoparticles with ferromagnetic properties at room temperature were among the smallest and strongest magnets (5 nm) were made in solution. The applications of this work can be applied to produce viable storage devices and the other possibility is to disperse these nanocrystals in solution and use it to make ferro-fluids which have a number of mature applications. The third part is about preparing and assembling of submicron silver, cobalt and nickel particles by using polyol methods and liquid/liquid interface, respectively. Noble metal like gold, copper and silver are suitable for plasmonic thin film solar cells because of their low resistivity and strong interactions with visible light waves. Silver is the best choice for solar cell application since it has low absorption losses and high radiative efficiency compared to gold and copper. Assembled cobalt and nickel as films are promising for spintronic, magnetic and magneto-electronic and biomedics.

Keywords: assembling nanoparticles, liquid/liquid interface, thin film, core/shell, solar cells, recording media

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Authors: A. Guemache, M. Omari

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Oxides with formula Ca1-xSrx MnO3(0≤x≤0.2) were synthesized using co precipitation method. The identification of the obtained phase was carried out using infrared spectroscopy and x-ray diffraction. Thermogravimetric and differential analysis was permitted to characterize different transformations of precursors which take place during one heating cycle. The study of electrochemical behavior was carried out by cyclic voltammetry and impedance spectroscopy. The obtained results show that apparent catalytic activity improved when increasing the concentration of strontium. Anodic current densities varies from 1.3 to 5.9 mA/cm2 at the rate scan of 20 mV.s-1 and a potential 0.8 V for oxides with composition x=0 to 0.2.

Keywords: oxide, co-precipitation, thermal analysis, electrochemical properties

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Authors: Dong-Gi Lee, Suyeon Cha, Yong-Sun Bahn

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Sterol lipid is essential for cell membrane structure in eukaryotic cells. In mammalian cells, sterol regulatory element binding proteins (SREBPs) act as principal regulators of cellular cholesterol which is essential for proper cell membrane fluidity and structure. SREBP and sterol regulation are related to levels of cellular oxygen because it is a major substrate for sterol synthesis. Upon cellular sterol and oxygen levels are depleted, SREBP is translocated to the Golgi where it undergoes proteolytic cleavage of N terminus, then it travels to the nucleus to play a role as transcription factor. In yeast cells, synthesis of ergosterol is also highly oxygen consumptive, and Sre1 is a transcription factor known to play a central role in adaptation to growth under low oxygen condition and sterol homeostasis in Cryptococcus neoformans. In this study, we observed phenotypes in other strains of Cryptococcus species by constructing hob1Δ and sre1Δ mutants to confirm whether the functions of both genes are conserved in most serotypes. As a result, hob1Δ showed no noticeable phenotype under treatment of antifungal drugs and most environmental stresses in R265 (C. gattii) and XL280 (C. neoformans), suggesting that Hob1 is related to sterol regulation only in H99 (serotype A). On the other hand, the function of Sre1 was found to be conserved in most serotypes. Furthermore, mating experiment of hob1Δ or sre1Δ showed dramatic defects in serotype A (H99) and D (XL280). It revealed that Hob1 and Sre1 related to mating ability in Cryptococcus species, especially cell fusion efficiency. In conclusion, HOB1 and SRE1 play crucial role in regulating sterol-homeostasis and differentiation in C. neoformans, moreover, Hob1 is specific gene in Cryptococcus neoformans. It suggests that Hob1 is considered as potent factor-targeted new safety antifungal drug.

Keywords: cryptococcus neoformans, Hob1, Sre1, sterol regulatory element binding proteins

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

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Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

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Authors: J. E. Mendes, T. T. de Barros, O. B. G. de Assis, J. D. C. Pessoa

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Chitosan, a natural polysaccharide of β-1,4-linked glucosamine residues, is a biopolymer obtained primarily from the exoskeletons of crustaceans. Interest in polymeric materials increases year by year. Chitosan is one of the most plentiful biomaterials, with a wide range of pharmaceutical, biomedical, industrial and agricultural applications. Chitosan nanoparticles were synthesized via the ionotropic gelation of chitosan with sodium tripolyphosphate (TPP). Two concentrations of chitosan microparticles (0.1 and 0.2%) were synthesized. In this study, it was possible to synthesize and characterize microparticles of chitosan biomaterial and this will be used for future applications in cell anchorage for 3D bioprinting.

Keywords: chitosan microparticles, biomaterial, scaffold, bioprinting

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Authors: Elodie Niemiec, Philippe Champagne, Jean-Francois Blach, Philippe Moreau, Anthony Thuault, Arnaud Tricoteaux

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Hygiene of equipment in contact with users is an important issue in the railroad industry. The numerous cleanings to eliminate bacteria and dirt cost a lot. Besides, mechanical solicitations on contact parts are observed daily. It should be interesting to elaborate on a self-cleaning and antibacterial coating with sufficient adhesion and good resistance against mechanical and chemical solicitations. Thus, a Hauts-de-France and Maubeuge Val-de-Sambre conurbation authority co-financed Ph.D. thesis has been set up since October 2017 based on anterior studies carried by the Laboratory of Ceramic Materials and Processing. To accomplish this task, a soft chemical route has been implemented to bring a lotus effect on metallic substrates. It involves nanometric liquid zinc oxide synthesis under 100°C. The originality here consists in a variation of surface texturing by modification of the synthesis time of the species in solution. This helps to adjust wettability. Nanostructured zinc oxide has been chosen because of the inherent photocatalytic effect, which can activate organic substance degradation. Two methods of heating have been compared: conventional and microwave assistance. Tested subtracts are made of stainless steel to conform to transport uses. Substrate preparation was the first step of this protocol: a meticulous cleaning of the samples is applied. The main goal of the elaboration protocol is to fix enough zinc-based seeds to make them grow during the next step as desired (nanorod shaped). To improve this adhesion, a silica gel has been formulated and optimized to ensure chemical bonding between substrate and zinc seeds. The last step consists of deposing a wide carbonated organosilane to improve the superhydrophobic property of the coating. The quasi-proportionality between the reaction time and the nanorod length will be demonstrated. Water Contact (superior to 150°) and Roll-off Angle at different steps of the process will be presented. The antibacterial effect has been proved with Escherichia Coli, Staphylococcus Aureus, and Bacillus Subtilis. The mortality rate is found to be four times superior to a non-treated substrate. Photocatalytic experiences were carried out from different dyed solutions in contact with treated samples under UV irradiation. Spectroscopic measurements allow to determinate times of degradation according to the zinc quantity available on the surface. The final coating obtained is, therefore, not a monolayer but rather a set of amorphous/crystalline/amorphous layers that have been characterized by spectroscopic ellipsometry. We will show that the thickness of the nanostructured oxide layer depends essentially on the synthesis time set in the hydrothermal growth step. A green, easy-to-process and control coating with self-cleaning and antibacterial properties has been synthesized with a satisfying surface structuration.

Keywords: antibacterial, biomimetism, soft-chemistry, zinc oxide

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Authors: Parya Nasehi, Mohammad Kazem Mohammadi

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3,4-dihydropyrimidin-2(1H)-thiones were synthesized in the presence of Ag nanoparticle/melamine sulfonic acid (MSA) supported on alumina. The reaction was carried out at 110 oC for 20 min under solvent free conditions. This method have some advantages such as good yield, mild reaction conditions, ease of operation and work up, short reaction time and high product purity.

Keywords: nanoparticle melamine sulfonic acid, Al2O3, Biginelli reaction, 3, 4-dihydropyrimidin-2(1H, solvent free

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Authors: Ji Hoi Heo, Jun Seong Park, Hyo Kim

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Geopolymer is an inorganic material synthesized by alkali activation of source materials rich in soluble SiO₂ and Al₂O₃. Many researches have studied the effect of aluminum species on the synthesis of geopolymer. However, it is still unclear about the influence of Al additives on the properties of geopolymer. The current study identified the role of the Al additive on the thermal performance of fly ash based geopolymer and observing the microstructure development of the composite. NaOH pellets were dissolved in water for 14 M (14 moles/L) sodium hydroxide solution which was used as an alkali activator. The weight ratio of alkali activator to fly ash was 0.40. Sodium aluminate powder was employed as an Al additive and added in amounts of 0.5 wt.% to 2 wt.% by the weight of fly ash. The mixture of alkali activator and fly ash was cured in a 75°C dry oven for 24 hours. Then, the hardened geopolymer samples were exposed to 300°C, 600°C and 900°C for 2 hours, respectively. The initial compressive strength after oven curing increased with increasing sodium aluminate content. It was also observed in SEM results that more amounts of geopolymer composite were synthesized as sodium aluminate was added. The compressive strength increased with increasing heating temperature from 300°C to 600°C regardless of sodium aluminate addition. It was consistent with the ATR-FTIR results that the peak position related to asymmetric stretching vibrations of Si-O-T (T: Si or Al) shifted to higher wavenumber as the heating temperature increased, indicating the further geopolymer reaction. In addition, geopolymer sample with higher content of sodium aluminate showed better compressive strength. It was also reflected on the IR results by more shift of the peak position assigned to Si-O-T toward the higher wavenumber. However, the compressive strength decreased after being exposed to 900°C in all samples. The degree of reduction in compressive strength was decreased with increasing sodium aluminate content. The deterioration in compressive strength was most severe in the geopolymer sample without sodium aluminate additive, while the samples with sodium aluminate addition showed better thermal durability at 900°C. This is related to the phase transformation with the occurrence of nepheline phase at 900°C, which was most predominant in the sample without sodium aluminate. In this work, it was concluded that sodium aluminate could be a good additive in the geopolymer synthesis by showing the improved compressive strength at elevated temperatures.

Keywords: compressive strength, fly ash based geopolymer, microstructure development, Na-aluminate

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Authors: N. K. Fuloria, S. Fuloria, R. Gupta

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Esterification of p-bromo-m-cresol offered 2-(4-bromo-3-methyl phenoxy)acetate (1), which was hydrazinated to yield 2-(4-bromo-3-methyl phenoxy)aceto hydrazide (2). Compound (2) was reacted with different aromatic aldehydes to yield N-(substituted benzylidiene)-2-(4-bromo-3-methyl phenoxy)acetamide(3a-c). Cyclization of compound (3a-c) with thioglycolic acid yielded 2-(4-bromo-3-methylphenoxy)-N-(4-oxo-2-arylthiazolidin-3-yl) acetamide (4a-c). The newly synthesized compounds were characterized on the basis of spectral studies and evaluated for antibacterial and antifungal activities.

Keywords: imines, thiazolidinone, schiff base, antimicrobial

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Authors: V. Mani Rathnam, Giridhar Madras

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Fossil fuels are depleting rapidly as the demand for energy, and its allied chemicals are continuously increasing in the modern world. Therefore, sustainable renewable energy sources based on non-edible oils are being explored as a viable option as they do not compete with the food commodities. Oils such as castor oil are rich in fatty acids and thus can be used for the synthesis of biodiesel, bio-lubricants, and many other fine industrial chemicals. There are several processes available for the synthesis of different chemicals obtained from the castor oil. One such process is the transesterification of castor oil, which results in a mixture of fatty acid methyl esters. The main products in the above reaction are methyl ricinoleate and methyl 10-undecenoate. To separate these compounds, supercritical carbon dioxide (SCCO₂) was used as a green solvent. SCCO₂ was chosen as a solvent due to its easy availability, non-toxic, non-flammable, and low cost. In order to design any separation process, the preliminary requirement is the solubility or phase equilibrium data. Therefore, the solubility of a mixture of methyl ricinoleate with methyl 10-undecenoate in SCCO₂ was determined in the present study. The temperature and pressure range selected for the investigation were T = 313 K to 333 K and P = 10 MPa to 18 MPa. It was observed that the solubility (mol·mol⁻¹) of methyl 10-undecenoate varied from 2.44 x 10⁻³ to 8.42 x 10⁻³ whereas it varied from 0.203 x 10⁻³ to 6.28 x 10⁻³ for methyl ricinoleate within the chosen operating conditions. These solubilities followed a retrograde behavior (characterized by the decrease in the solubility values with the increase in temperature) throughout the range of investigated operating conditions. An association theory model, coupled with regular solution theory for activity coefficients, was developed in the present study. The deviation from the experimental data using this model can be quantified using the average absolute relative deviation (AARD). The AARD% for the present compounds is 4.69 and 8.08 for methyl 10-undecenoate and methyl ricinoleate, respectively in a mixture of methyl ricinoleate and methyl 10-undecenoate. The maximum solubility enhancement of 32% was observed for the methyl ricinoleate in a mixture of methyl ricinoleate and methyl 10-undecenoate. The highest selectivity of SCCO₂ was observed to be 12 for methyl 10-undecenoate in a mixture of methyl ricinoleate and methyl 10-undecenoate.

Keywords: association theory, liquid mixtures, solubilities, supercritical carbon dioxide

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Authors: A. Abbasi Moshaii, M. Soltan Rezaee, M. Mohammadi Moghaddam

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Control of some mechanisms is hard because of their complex dynamic equations. If part of the complexity is resulting from uncertainties, an efficient way for solving that is robust control. By this way, the control procedure could be simple and fast and finally, a simple controller can be designed. One kind of these mechanisms is 3-RRR which is a parallel mechanism and has three revolute joints. This paper aims to robust control a 3-RRR planner mechanism and it presents that this could be used for other mechanisms. So, a significant problem in mechanisms control could be solved. The relevant diagrams are drawn and they show the correctness of control process.

Keywords: 3-RRR, dynamic equations, mechanisms control, structural uncertainty

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Authors: Tulika Malviya, Ritesh Chandra Shukla, Praveen Kumar Tandon

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Traditional methods of synthesis are hazardous for the environment and need nature friendly processes for the treatment of industrial effluents and contaminated water. Use of plant parts for the synthesis provides an efficient alternative method. In this paper, we report an ecofriendly and nonhazardous biobased method to prepare zerovalent iron nanoparticles (ZVINPs) using the liquor of commercially available tea. Tea liquor as the reducing agent has many advantages over other polymers. Unlike other polymers, the polyphenols present in tea extract are nontoxic and water soluble at room temperature. In addition, polyphenols can form complexes with metal ions and thereafter reduce the metals. Third, tea extract contains molecules bearing alcoholic functional groups that can be exploited for reduction as well as stabilization of the nanoparticles. Briefly, iron nanoparticles were prepared by adding 2.0 g of montmorillonite K10 (MMT K10) to 5.0 mL of 0.10 M solution of Fe(NO3)3 to which an equal volume of tea liquor was then added drop wise over 20 min with constant stirring. The color of the mixture changed from whitish yellow to black, indicating the formation of iron nanoparticles. The nanoparticles were adsorbed on montmorillonite K10, which is safe and aids in the separation of hazardous arsenic species simply by filtration. Particle sizes ranging from 59.08±7.81 nm were obtained which is confirmed by using different instrumental analyses like IR, XRD, SEM, and surface area studies. Removal of arsenic was done via batch adsorption method. Solutions of As(III) of different concentrations were prepared by diluting the stock solution of NaAsO2 with doubly distilled water. The required amount of in situ prepared ZVINPs supported on MMT K10 was added to a solution of desired strength of As (III). After the solution had been stirred for the preselected time, the solid mass was filtered. The amount of arsenic [in the form of As (V)] remaining in the filtrate was measured using ion chromatograph. Stirring of contaminated water with zerovalent iron nanoparticles supported on montmorillonite K10 for 30 min resulted in up to 99% removal of arsenic as As (III) from its solution at both high and low pH (2.75 and 11.1). It was also observed that, under similar conditions, montmorillonite K10 alone provided only <10% removal of As(III) from water. Adsorption at low pH with precipitation at higher pH has been proposed for As(III) removal.

Keywords: arsenic removal, montmorillonite K10, tea liquor, zerovalent iron nanoparticles

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Authors: Tom Nakotte, Hongmei Luo

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Lead chalcogenide-based (PbS, PbSe, and PbTe) quantum dots (QDs) were synthesized for the purpose of implementing them in radiation detectors. Pb based materials have long been of interest for gamma and x-ray detection due to its high absorption cross section and Z number. The emphasis of the studies was on exploring how to control charge carrier transport within thin films containing the QDs. The properties of QDs itself can be altered by changing the size, shape, composition, and surface chemistry of the dots, while the properties of carrier transport within QD films are affected by post-deposition treatment of the films. The QDs were synthesized using colloidal synthesis methods and films were grown using multiple film coating techniques, such as spin coating and doctor blading. Current QD radiation detectors are based on the QD acting as fluorophores in a scintillation detector. Here the viability of using QDs in solid-state radiation detectors, for which the incident detectable radiation causes a direct electronic response within the QD film is explored. Achieving high sensitivity and accurate energy quantification in QD radiation detectors requires a large carrier mobility and diffusion lengths in the QD films. Pb chalcogenides-based QDs were synthesized with both traditional oleic acid ligands as well as more weakly binding oleylamine ligands, allowing for in-solution ligand exchange making the deposition of thick films in a single step possible. The PbS and PbSe QDs showed better air stability than PbTe. After precipitation the QDs passivated with the shorter ligand are dispersed in 2,6-difloupyridine resulting in colloidal solutions with concentrations anywhere from 10-100 mg/mL for film processing applications, More concentrated colloidal solutions produce thicker films during spin-coating, while an extremely concentrated solution (100 mg/mL) can be used to produce several micrometer thick films using doctor blading. Film thicknesses of micrometer or even millimeters are needed for radiation detector for high-energy gamma rays, which are of interest for astrophysics or nuclear security, in order to provide sufficient stopping power.

Keywords: colloidal synthesis, lead chalcogenide, radiation detectors, quantum dots

Procedia PDF Downloads 125