Search results for: aerogels

Authors: Tahira Pirzada, Zahra Ashrafi, Saad Khan

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We present a facile and sustainable solid templating approach to fabricate highly porous, flexible and superhydrophobic aerogels of composite nanofibers of cellulose diacetate and silica which are produced through sol gel electrospinning. Scanning electron microscopy, contact angle measurement, and attenuated total reflection-Fourier transform infrared spectrometry are used to understand the structural features of the resultant aerogels while thermogravimetric analysis and differential scanning calorimetry demonstrate their thermal stability. These aerogels exhibit a self-supportive three-dimensional network abundant in large secondary pores surrounded by primary pores resulting in a highly porous structure. Thermal crosslinking of the aerogels has further stabilized their structure and flexibility without compromising on the porosity. Ease of processing, thermal stability, high porosity and oleophilic nature of these aerogels make them promising candidate for a wide variety of applications including acoustic and thermal insulation and oil and water separation.

Keywords: hybrid aerogels, sol-gel electrospinning, oil-water separation, nanofibers

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Authors: Haibo Zhao, Thomas Andre, Katherine Avery, Alper Kiziltas, Deborah Mielewski

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Silica aerogels were fabricated through a modified rapid supercritical extraction (RSCE) process. The silica aerogels were made using a tetramethyl orthosilicate precursor and then placed in a hot press and brought to the supercritical point of the solvent, ethanol. In order to control the pressure release without a pressure controller, a needle valve was used. The resulting aerogels were then characterized for their physical and chemical properties and compared to silica aerogels created using similar methods. The aerogels fabricated using this modified RSCE method were found to have similar properties to those in other papers using the unmodified RSCE method. Silica aerogel infused glass blanket composite, graphene reinforced silica aerogel composite were also successfully fabricated by this new method. The modified RSCE process and system is a prototype for better gas outflow control with a lower cost of equipment setup. Potentially, this process could be evolved to a continuous low-cost high-volume production process to meet automotive requirements.

Keywords: aerogel, automotive, rapid supercritical extraction process, low cost production

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Authors: Y. J. Lin, Y. F. Lin

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CO2 is the primary greenhouse gas which causes global warming in recent years. As the carbon capture and storage (CCS) getting maturing, the reuse of carbon dioxide which made from CCS is the important issue. In this way, the most common method is the synthesis of cyclic carbonate chemicals from the cycloaddition reaction of carbon dioxide and epoxide. The catalyst plays an important role in the CO2/epoxide cycloaddition reactions. The Lewis acid and base sites are both needed on the catalyst surface for the help of epoxide ring opening, leading to the synthesis of cyclic carbonate. Furthermore, the larger specific surface area and more active site of the catalyst are also needed to enhance the efficiency of the CO2/epoxide cycloaddition reactions. Aerogel is a mesoporous nanomaterial (pore size between 2~50 nm) with high specific surface area and porosity (at least 90%) and low density. In this study, the ternary metal oxide aerogels, Mg-doped Al2O3 aerogels, with higher specific surface area and Lewis acid and base sites on the aerogel surface are successfully prepared by using a facile sol-gel reaction. The as-prepared Mg-doped Al2O3 aerogels are also served as heterogenous catalyst for the CO2/propylene- oxide cycloaddition reaction. Compared to the pristine Al2O3 aerogels, the Mg-doped Al2O3 aerogels possessed both Lewis acid and base sites on the surface are able to enhance the efficiency of the CO2/propylene oxide cycloaddition reactions. As a result, the as-prepared Mg-doped Al2O3 aerogels are a promising and novel catalyst for the CO2/epoxide cycloaddition reactions.

Keywords: ternary, metal oxide aerogel, CO2 reuse, cycloaddition, propylene oxide

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Authors: Ali Mirtaghavi, Andy Baldwin, Rajendarn Muthuraj, Jack Luo

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Recent advances in biomaterials have led to utilizing biopolymers to develop 3D scaffolds in tissue regeneration. One of the major challenges of designing biomaterials for 3D scaffolds is to mimic the building blocks similar to the extracellular matrix (ECM) of the native tissues. Biopolymer based aerogels obtained by freeze-drying have shown to provide structural similarities to the ECM owing to their 3D format and a highly porous structure with interconnected pores, similar to the ECM. Gelatin (GEL) is known to be a promising biomaterial with inherent regenerative characteristics owing to its chemical similarities to the ECM in native tissue, biocompatibility abundance, cost-effectiveness and accessible functional groups, which makes it facile for chemical modifications with other biomaterials to form biocomposites. Despite such advantages, gelatin offers poor mechanical properties, sensitive enzymatic degradation and high viscosity at room temperature which limits its application and encourages its use to develop biocomposites. Hydrophilic biomass-based cellulose nanofibrous (CNF) has been explored to use as suspension for biocomposite aerogels for the development of 3D porous structures with excellent mechanical properties, biocompatibility and slow enzymatic degradation. In this work, CNF biocomposite aerogels with various ratios of CNF:GEL) (90:10, 70:30 and 50:50) were prepared by freeze-drying technique, and their properties were investigated in terms of physicochemical, mechanical and biological characteristics. Epichlorohydrin (EPH) was used to investigate the effect of chemical crosslinking on the molecular interaction of CNF: GEL, and its effects on physicochemical, mechanical and biological properties of the biocomposite aerogels. Ultimately, chemical crosslinking helped to improve the mechanical resilience of the resulting aerogels. Amongst all the CNF-GEL composites, the crosslinked CNF: GEL (70:30) biocomposite was found to be favourable for cell attachment and viability. It possessed highly porous structure (porosity of ~93%) with pore sizes ranging from 16-110 µm, adequate mechanical properties (compression modulus of ~47 kPa) and optimal biocompatibility both in-vitro and in-vivo, as well as controlled enzymatic biodegradation, high water penetration, which could be considered a suitable option for wound healing application. In-vivo experiments showed improvement on inflammation and foreign giant body cell reaction for the crosslinked CNF: GEL (70:30) compared to the other samples. This could be due to the superior interaction of CNF with gelatin through chemical crosslinking, resulting in more optimal in-vivo improvement. In-vitro cell culture investigation on human dermal fibroblasts showed satisfactory 3D cell attachment over time. Overall, it has been observed that the developed CNF: GEL aerogel can be considered as a potential scaffold for soft tissue regeneration application.

Keywords: 3D scaffolds, aerogels, Biocomposites , tissue engineering

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Authors: Javiera Poblete, Fernando Gajardo, Katherina Fernandez

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Graphene, and its derivatives such as graphene oxide (GO), are emerging nanoscopic materials, with interesting physical and chemical properties. From them, it is possible to develop three-dimensional macrostructures, such as aerogels, which are characterized by a low density, high porosity, and large surface area, having a promising structure for the development of materials. The use of GO as a precursor of these structures provides a wide variety of materials, which can be developed as a result of the functionalization of their oxygenated groups, with specific compounds such as polyethylene glycol (PEG). The synthesis of aerogels of GO-PEG for non-covalent interactions has not yet been widely reported, being of interest due to its feasible escalation and economic viability. Thus, this work aims to develop a non-covalently functionalized GO-PEG aerogels and characterize them physicochemically. In order to get this, the GO was synthesized from the modified hummers method and it was functionalized with the PEG by polymer-assisted GO gelation (crosslinker). The gelation was obtained for GO solutions (10 mg/mL) with the incorporation of PEG in different proportions by weight. The hydrogel resulting from the reaction was subsequently lyophilized, to obtain the respective aerogel. The material obtained was chemically characterized by analysis of Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy and X-ray diffraction (XRD), and its morphology by scanning electron microscopy (SEM) images; as well as water absorption tests. The results obtained showed the formation of a non-covalent aerogel (FTIR), whose structure was highly porous (SEM) and with a water absorption values greater than 50% g/g. Thus, a methodology of synthesis for GO-PEG was developed and validated.

Keywords: aerogel, graphene oxide, polyethylene glycol, synthesis

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Authors: Zulkifli, I. W. Eltara, Anawati

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Understanding the complementary roles of surface energy and roughness on natural nonwetting surfaces has led to the development of a number of biomimetic superhydrophobic surfaces, which exhibit apparent contact angles with water greater than 150 degrees and low contact angle hysteresis. However, superoleophobic surfaces—those that display contact angles greater than 150 degrees with organic liquids having appreciably lower surface tensions than that of water—are extremely rare. In addition to chemical composition and roughened texture, a third parameter is essential to achieve superoleophobicity, namely, re-entrant surface curvature in the form of overhang structures. The overhangs can be realized as fibers. Superoleophobic surfaces are appealing for example, antifouling, since purely superhydrophobic surfaces are easily contaminated by oily substances in practical applications, which in turn will impair the liquid repellency. On the other studied have demonstrate that such aqueous nanofibrillar gels are unexpectedly robust to allow formation of highly porous aerogels by direct water removal by freeze-drying, they are flexible, unlike most aerogels that suffer from brittleness, and they allow flexible hierarchically porous templates for functionalities, e.g. for electrical conductivity. No crosslinking, solvent exchange nor supercritical drying are required to suppress the collapse during the aerogel preparation, unlike in typical aerogel preparations. The aerogel used in current work is an ultralight weight solid material composed of native cellulose nanofibers. The native cellulose nanofibers are cleaved from the self-assembled hierarchy of macroscopic cellulose fibers. They have become highly topical, as they are proposed to show extraordinary mechanical properties due to their parallel and grossly hydrogen bonded polysaccharide chains. We demonstrate that superoleophobic nanocellulose aerogels coating by sol-gel method, the aerogel is capable of supporting a weight nearly 3 orders of magnitude larger than the weight of the aerogel itself. The load support is achieved by surface tension acting at different length scales: at the macroscopic scale along the perimeter of the carrier, and at the microscopic scale along the cellulose nanofibers by preventing soaking of the aerogel thus ensuring buoyancy. Superoleophobic nanocellulose aerogels have recently been achieved using unmodified cellulose nanofibers and using carboxy methylated, negatively charged cellulose nanofibers as starting materials. In this work, the aerogels made from unmodified cellulose nanofibers were subsequently treated with fluorosilanes. To complement previous work on superoleophobic aerogels, we demonstrate their application as cargo carriers on oil, gas permeability, plastrons, and drag reduction, and we show that fluorinated nanocellulose aerogels are high-adhesive superoleophobic surfaces. We foresee applications including buoyant, gas permeable, dirt-repellent coatings for miniature sensors and other devices floating on generic liquid surfaces.

Keywords: superoleophobic, nanocellulose, aerogel, sol-gel

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Authors: Jessica Carolina Hernandez Galeano, Juan Carlos Moreno Pirajan, Liliana Giraldo

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Carbon gels are materials whose structure and porous texture can be designed and controlled on a nanoscale. Among their characteristics it is found their low density, large surface area and high degree of porosity. These materials are produced by a sol-gel polymerization of organic monomers using basic or acid catalysts, followed by drying and controlled carbonization. In this work, the synthesis and characterization of carbon aerogels from resorcinol, phenol and formaldehyde in ethanol is described. The aim of this study is obtaining different carbonaceous materials in the form of spheres using the Stöber method to perform a further evaluation of CO₂ adsorption of each material. In general, the synthesis consisted of a sol-gel polymerization process that generates a cluster (cross-linked organic monomers) from the precursors in the presence of NH₃ as a catalyst. This cluster was subjected to specific conditions of gelling and curing (30°C for 24 hours and 100°C for 24 hours, respectively) and CO₂ supercritical drying. Finally, the dry material was subjected to a process of carbonization or pyrolysis, in N₂ atmosphere at 350°C (1° C / min) for 2 h and 600°C (1°C / min) for 4 hours, to obtain porous solids that retain the structure initially desired. For this work, both the concentrations of the precursors and the proportion of ammonia in the medium where modify to describe the effect of the use of phenol and the amount of catalyst in the resulting material. Carbon aerogels were characterized by Scanning Electron Microscope (SEM), N₂ isotherms, infrared spectroscopy (IR) and X-ray Powder Diffraction (XRD) showing the obtention of carbon spheres in the nanometric scale with BET areas around 500 m2g-1.

Keywords: carbon aerogels, carbon spheres, CO₂ adsorption, Stöber method

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Authors: Z. Mazrouei-Sebdani, A. Khoddami, H. Hadadzadeh, M. Zarrebini

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Silica aerogels are well-known meso-porous materials with high specific surface area (500–1000 m2/g), high porosity (80–99.8%), and low density (0.003–0.8 g/cm3). However, the silica aerogels generally are highly brittle due to their nanoporous nature. Physical and mechanical properties of the silica aerogels can be enhanced by compounding with the fibers. Although some reports presented incorporation of the fibers into the sol, followed by further modification and drying stages, no information regarding the aerogel powders as filler in the polymeric fibers is available. In this research, waterglass based aerogel powder was prepared in the following steps: sol–gel process to prepare a gel, followed by subsequent washing with propan-2-ol, n-Hexane, and TMCS, then ambient pressure drying, and ball milling. Inspired by limited dust releasing, aerogel powder was introduced to the PET electrospinning solution in an attempt to create required bulk and surface structure for the nano fibers to improve their hydrophobic and insulation properties. The samples evaluation was carried out by measuring density, porosity, contact angle, sliding angle, heat transfer, FTIR, BET and SEM. According to the results, porous silica aerogel powder was fabricated with mean pore diameter of 24 nm and contact angle of 145.9º. The results indicated the usefulness of the aerogel powder confined into nano fibers to control surface roughness for manipulating superhydrophobic nanowebs with sliding angle of 5˚ and water contact angle of 147º. It can be due to a multi-scale surface roughness which was created by nanowebs structure itself and nano fibers surface irregularity in presence of the aerogels while a laye of fluorocarbon created low surface energy. The wettability of a solid substrate is an important property that is controlled by both the chemical composition and geometry of the surface. Also, a decreasing trend in the heat transfer was observed from 22% for the nano fibers without any aerogel powder to 8% for the nano fibers with 4% aerogel powder. The development of thermal insulating materials has become increasingly more important than ever in view of the fossil energy depletion and global warming that call for more demanding energy-saving practices.

Keywords: Superhydrophobicity, Insulation, Sol-gel, Surface energy, Roughness.

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Authors: Jianzheng Wei, Duo Zhen, Zhihan Yang, Huifeng Tan

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The deployable descent technology is a lightweight entry method using an inflatable heat shield. The heatshield consists of a pressurized core which is covered by different layers of thermal insulation and flexible ablative materials in order to protect against the thermal loads. In this paper, both aluminum and silicon-aluminum aerogels were prepared by freeze-drying method. The latter material has bigger specific surface area and nano-scale pores. Mullite fibers are used as the reinforcing fibers to prepare the aerogel matrix to improve composite flexibility. The flexible composite materials were performed as an insulation layer to an underlying aramid fabric by a thermal shock test at a heat flux density of 120 kW/m² and uniaxial tensile test. These results show that the aramid fabric with untreated mullite fibers as the thermal protective layer is completely carbonized at the heat of about 60 s. The aramid fabric as a thermal resistance layer of the composite material still has good mechanical properties at the same heat condition.

Keywords: aerogel, aramid fabric, flexibility, thermal resistance

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Authors: Deniz Bozoglu, Deniz Deger, Kemal Ulutas, Sahin Yakut

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In recent years, silica aerogels have attracted great attention due to their outstanding properties, and their wide variety of potential applications such as microelectronics, nuclear and high-energy physics, optics and acoustics, superconductivity, space-physics. Hydrophobic silica aerogels were successfully synthesized in one-step by surface modification at ambient pressure. FT-IR result confirmed that Si-OH groups were successfully converted into hydrophobic and non-polar Si-CH3 groups by surface modification using trimethylchloro silane (TMCS) as co-precursor. Using Alpha-A High-Resolution Dielectric, Conductivity and Impedance Analyzer, AC conductivity of samples were examined at temperature range 293-423 K and measured over frequency range between 1-106 Hz. The characteristic relaxation time decreases with increasing temperature. The AC conductivity follows σ_AC (ω)=σ_t-σ_DC=Aω^s relation at frequencies higher than 10 Hz, and the dominant conduction mechanism is found to obey the Correlated Barrier Hopping (CBH) mechanism. At frequencies lower than 10 Hz, the electrical conduction is found to be in accordance with DC conduction mechanism. The activation energies obtained from AC conductivity results and it was observed two relaxation regions.

Keywords: aerogel, synthesis, dielectric constant, dielectric loss, relaxation time

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Authors: Helen L. Hein, Joachim Schwarte

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As a pillar of sustainable development, ecology has become an important milestone in research community, especially due to global challenges like climate change. The ecological performance of products can be scientifically conducted with life cycle assessments. In the construction sector, significant amounts of CO₂ emissions are assigned to the energy used for building heating purposes. Therefore, sustainable construction materials for insulating purposes are substantial, whereby aerogels have been explored intensively in the last years due to their low thermal conductivity. Therefore, the WALL-ACE project aims to develop an aerogel-based thermal insulating plaster that would achieve minor thermal conductivities. But as in the early stage of development phases, a lot of information is still missing or not yet accessible, the ecological performance of innovative products bases increasingly on uncertain data that can lead to significant deviations in the results. To be able to predict realistically how meaningful the results are and how viable the developed products may be with regard to their corresponding respective market, these deviations however have to be considered. Therefore, a classification method is presented in this study, which may allow comparing the ecological performance of modern products with already established and competitive materials. In order to achieve this, an alternative calculation method was used that allows computing with lower and upper bounds to consider all possible values without precise data. The life cycle analysis of the considered products was conducted with an interval arithmetic based calculation method. The results lead to the conclusion that the interval solutions describing the possible environmental impacts are so wide that the result usability is limited. Nevertheless, a further optimization in reducing environmental impacts of aerogels seems to be needed to become more competitive in the future.

Keywords: aerogel-based, insulating material, early development phase, interval arithmetic

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Authors: María Canal-Rodríguez, María Arnaiz, Natalia Rey-Raap, Ana Arenillas, Jon Ajuria

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The constant demand of electrical energy, as well as the increase in environmental concern, lead to the necessity of investing in clean and eco-friendly energy sources that implies the development of enhanced energy storage devices. Li-ion batteries (LIBs) and Electrical double layer capacitors (EDLCs) are the most widespread energy systems. Batteries are able to storage high energy densities contrary to capacitors, which main strength is the high-power density supply and the long cycle life. The combination of both technologies gave rise to Li-ion capacitors (LICs), which offers all these advantages in a single device. This is achieved combining a capacitive, supercapacitor-like positive electrode with a faradaic, battery-like negative electrode. Due to the abundance and affordability, dual carbon-based LICs are nowadays the common technology. Normally, an Active Carbon (AC) is used as the EDLC like electrode, while graphite is the material commonly employed as anode. LICs are potential systems to be used in applications in which high energy and power densities are required, such us kinetic energy recovery systems. Although these devices are already in the market, some drawbacks like the limited power delivered by graphite or the energy limiting nature of AC must be solved to trigger their used. Focusing on the anode, one possibility could be to replace graphite with Hard Carbon (HC). The better rate capability of the latter increases the power performance of the device. Moreover, the disordered carbonaceous structure of HCs enables storage twice the theoretical capacity of graphite. With respect to the cathode, the ACs are characterized for their high volume of micropores, in which the charge is storage. Nevertheless, they normally do not show mesoporous, which are really important mainly at high C-rates as they act as transport channels for the ions to reach the micropores. Usually, the porosity of ACs cannot be tailored, as it strongly depends on the precursor employed to get the final carbon. Moreover, they are not characterized for having a high electrical conductivity, which is an important characteristic to get a good performance in energy storage applications. A possible candidate to substitute ACs are carbon aerogels (CAs). CAs are materials that combine a high porosity with great electrical conductivity, opposite characteristics in carbon materials. Furthermore, its porous properties can be tailored quite accurately according to with the requirements of the application. In the present study, CAs with controlled porosity were obtained from polymerization of resorcinol and formaldehyde by microwave heating. Varying the synthesis conditions, mainly the amount of precursors and pH of the precursor solution, carbons with different textural properties were obtained. The way the porous characteristics affect the performance of the cathode was studied by means of a half-cell configuration. The material with the best performance was evaluated as cathode in a LIC versus a hard carbon as anode. An analogous full LIC made by a high microporous commercial cathode was also assembled for comparison purposes.

Keywords: li-ion capacitors, energy storage, tailored porosity, carbon aerogels

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Authors: A. Bahadoran, M. Zomorodian

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The synthesizer of cobalt oxide nanoballs (length 3−4 μm, width 250−400 nm) was achieved by a simple high-temperature supercritical solution method. Multiwalled carbon aerogels are a step towards high-density nanometer-scale nanostructures. Cobalt oxide nanoballs were prepared by supercritical solution method. Synthesis in an aqueous solution containing cobalt hydroxide at ∼80 °C without any further heat treatment at high temperature. The formation of cobalt oxide nanoballs on carbon aerogel was confirmed by X-ray diffraction and Raman spectroscopy. The FE-SEM images showed the presence of cobalt oxide nanoballs. The reaction mechanism of the ultrasound-assisted synthesis of cobalt oxide nanostructures was proposed on the basis of the XRD, X-ray absorption spectroscopy analysis and FE-SEM observation of the reaction products taken during the course of the synthesis.

Keywords: cobalt oxide nano balls, carbon aerogel, synthesize, nanostructure

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Authors: Amal Maazoun, Abderrazak Mezghani, Ali Ben Moussa

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Aerogel consists of a ramified and inter-connected solid skeleton enclosing a very important number of nano-sized pores filled with air that occupies most of the volume and makes very low density. The thermal conductivity of this material can reach lower values than those of any other material, and it changes with the type of the aerogel and its composition. So, in order to explain the causes of the super-insulation of our material and to determine the factors in which depends on its conductivity we used a numerical simulation. We have developed a numerical code that generates random fractal structure of silica aerogel with pre-defined concentration, properties of the backbone and the gas in the pores as well as the size of the particles. The calculation of the conductivity at any point of domain shows that it is not constant and that it depends on the pore size and the location in the pore. A numerical method based on resolution by inversion of block tridiagonal matrices is used to calculate the equivalent thermal conductivity of the whole fractal structure. The average conductivity calculated for each concentration is in good agreement with those of typical aerogels. And we found that the equivalent thermal conductivity of a silica aerogel depends strongly not only on the porosity but also on the tortuosity of the solid backbone.

Keywords: aerogel, fractal structure, numerical study, porous media, thermal conductivity

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Authors: Pram Abhayawardhana, Ali Reza Nazmi, Hossein Najaf Zadeh

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This study examines the use of additive manufacturing (AM) to develop sustainable and intelligent agricultural formulations that can gradually release fertilisers. AM offers the ability to design customised formulations with precise geometries and controlled release properties while taking into account their mechanical, chemical, and environmental properties. The study specifically investigates the use of an aerogel matrix mixed with a potential fertiliser in agriculture. Highly porous 3D printed aerogel structures were designed to enable the slow release of fertilisers. The performance of the formulated mixture is evaluated against other commonly used materials for slow-release applications. The findings suggest that the 3D printed gel made has great potential for slow-release fertilisers, providing an environmentally friendly solution for agricultural practices. The combination of AM technology and sustainable materials can play a vital role in mitigating the negative environmental impact of traditional fertilisers, as well as improving the efficiency and sustainability of agricultural production.

Keywords: 3D printing, hydrogel, aerogel, fertiliser, agriculture

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Authors: Alexander Rodríguez-Hernández, Arnulfo Rojas-Perez, Liz Diaz-Vazquez

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The rise in consumerism over the past century has resulted in the creation of higher amounts of plasticizers, personal care products and other chemical substances, which enter and accumulate in water systems. Other sources of pollutants in Neotropical regions experience large inputs of nutrients with these pollutants resulting in eutrophication of water which consume large quantities of oxygen, resulting in high fish mortality. This dilemma has created a need for the development of targeted detection in complex matrices and remediation of emerging contaminants. We have synthesized carbon nanoparticles from macro algae (Ulva fasciata) by oxidizing the graphitic carbon network under extreme acidic conditions. The resulting material was characterized by STEM, yielding a spherical 12 nm average diameter nanoparticles, which can be fixed into a polysaccharide aerogel synthesized from the same macro algae. Spectrophotometer analyses show a pH dependent fluorescent behavior varying from 450-620 nm in aqueous media. Heavily oxidized edges provide for easy functionalization with enzymes for a more targeted analysis and remediation technique. Given the optical properties of the carbon base nanoparticles and the numerous possibilities of functionalization, we have developed a selective and robust targeted bio-detection and bioremediation technique for the treatment of emerging contaminants in complex matrices like estuarine embayment.

Keywords: aerogels, carbon nanoparticles, fluorescent, targeted analysis

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Authors: Sunil P. Lonkar, Vishnu V. Pillai, Saeed Alhassan

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Design and development of highly efficient, inexpensive, and long-term stable earth-abundant electrocatalysts hold tremendous promise for hydrogen evolution reaction (HER) in water electrolysis. The 2D transition metal dichalcogenides, especially molybdenum disulfide attracted a great deal of interests due to its high electrocatalytic activity. However, due to its poor electrical conductivity and limited exposed active sites, the performance of these catalysts is limited. In this context, a facile and scalable synthesis method for fabrication nanostructured electrocatalysts composed 3D graphene porous aerogels supported with MoS₂ and WS₂ is highly desired. Here we developed a highly active and stable electrocatalyst catalyst for the HER by growing it into a 3D porous architecture on conducting graphene. The resulting nanohybrids were thoroughly investigated by means of several characterization techniques to understand structure and properties. Moreover, the HER performance of these 3D catalysts is expected to greatly improve in compared to other, well-known catalysts which mainly benefits from the improved electrical conductivity of the by graphene and porous structures of the support. This technologically scalable process can afford efficient electrocatalysts for hydrogen evolution reactions (HER) and hydrodesulfurization catalysts for sulfur-rich petroleum fuels. Owing to the lower cost and higher performance, the resulting materials holds high potential for various energy and catalysis applications. In typical hydrothermal method, sonicated GO aqueous dispersion (5 mg mL⁻¹) was mixed with ammonium tetrathiomolybdate (ATTM) and tungsten molybdate was treated in a sealed Teflon autoclave at 200 ◦C for 4h. After cooling, a black solid macroporous hydrogel was recovered washed under running de-ionized water to remove any by products and metal ions. The obtained hydrogels were then freeze-dried for 24 h and was further subjected to thermal annealing driven crystallization at 600 ◦C for 2h to ensure complete thermal reduction of RGO into graphene and formation of highly crystalline MoS₂ and WoS₂ phases. The resulting 3D nanohybrids were characterized to understand the structure and properties. The SEM-EDS clearly reveals the formation of highly porous material with a uniform distribution of MoS₂ and WS₂ phases. In conclusion, a novice strategy for fabrication of 3D nanostructured MoS₂-WS₂/graphene is presented. The characterizations revealed that the in-situ formed promoters uniformly dispersed on to few layered MoS₂¬-WS₂ nanosheets that are well-supported on graphene surface. The resulting 3D hybrids hold high promise as potential electrocatalyst and hydrodesulfurization catalyst.

Keywords: electrocatalysts, graphene, transition metal chalcogenide, 3D assembly

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