Layer-by-layer thinning of two-dimensional materials.

Etching technology - one of the representative modern semiconductor device makers - serves as a broad descriptor for the process of removing material from the surfaces of various materials, whether partially or entirely. Meanwhile, thinning technology represents a novel and highly specialized approach within the realm of etching technology. It indicates the importance of achieving an exceptionally sophisticated and precise removal of material, layer-by-layer, at the nanoscale. Notably, thinning technology has gained substantial momentum, particularly in top-down strategies aimed at pushing the frontiers of nano-worlds. This rapid development in thinning technology has generated substantial interest among researchers from diverse backgrounds, including those in the fields of chemistry, physics, and engineering. Precisely and expertly controlling the layer numbers of 2D materials through the thinning procedure has been considered as a crucial step. This is because the thinning processes lead to variations in the electrical and optical characteristics. In this comprehensive review, the strategies for top-down thinning of representative 2D materials (e.g., graphene, black phosphorus, MoS2, h-BN, WS2, MoSe2, and WSe2) based on conventional plasma-assisted thinning, integrated cyclic plasma-assisted thinning, laser-assisted thinning, metal-assisted splitting, and layer-resolved splitting are covered in detail, along with their mechanisms and benefits. Additionally, this review further explores the latest advancements in terms of the potential advantages of semiconductor devices achieved by top-down 2D material thinning procedures.

Bacteria for Bioplastics: Progress, Applications, and Challenges.

Bioplastics are one of the answers that can point society toward a sustainable future. Under this premise, the synthesis of polymers with competitive properties using low-cost starting materials is a highly desired factor in the industry. Also, tackling environmental issues such as nonbiodegradable waste generation, high carbon footprint, and consumption of nonrenewable resources are some of the current concerns worldwide. The scientific community has been placing efforts into the biosynthesis of polymers using bacteria and other microbes. These microorganisms can be convenient reactors to consume food and agricultural wastes and convert them into biopolymers with inherently attractive properties such as biodegradability, biocompatibility, and appreciable mechanical and chemical properties. Such biopolymers can be applied to several fields such as packing, cosmetics, pharmaceutical, medical, biomedical, and agricultural. Thus, intending to elucidate the science of microbes to produce polymers, this review starts with a brief introduction to bioplastics by describing their importance and the methods for their production. The second section dives into the importance of bacteria regarding the biochemical routes for the synthesis of polymers along with their advantages and disadvantages. The third section covers some of the main parameters that influence biopolymers' production. Some of the main applications of biopolymers along with a comparison between the polymers obtained from microorganisms and the petrochemical-based ones are presented. Finally, some discussion about the future aspects and main challenges in this field is provided to elucidate the main issues that should be tackled for the wide application of microorganisms for the preparation of bioplastics.

Soybean-Based Bio-Adhesives: Role of Diamine on the Adhesive Properties.

One possible approach to achieving sustainable development in the materials sector is to produce polymers from plant oils (POs), which are renewable and environmentally beneficial. Polymers with a high concentration of functional groups can be used as cross-linking agents to enhance the properties of epoxidized POs (epoxidation of plant oil)-based polymers. In this work, a unique resin with novel properties and potential uses was produced by cross-linking epoxidized soybean oil (ESO) with branched and flexible polyamines by ring-opening and amidation polymerizations. This approach is straightforward and ecologically benign. After curing, melamine pentane diamine (MPD) polymer maintained its position as the strongest structural adhesive among the synthesized resins, with a bonding strength of almost 2000 kPa for stainless steel; irrespective of the temperature, stainless steel consistently outperforms melamine ethylene diamine-ESO resin in strength comparisons. At 100 °C, stainless steel has a lap shear strength of about 300 kPa, which is far higher than copper and aluminum; at 180 °C, this value increases by another 750 kPa. While MPD-ESO resin has a shear strength of 1996 kPa at 180 °C, melamine butane diamine-ESO resin has a shear strength of only 1220 kPa.

Study of Soybean Oil-Based Non-Isocyanate Polyurethane Films via a Solvent and Catalyst-Free Approach.

Synthesizing polymeric materials that are both sustainable and practical has become a priority. Polyurethanes (PUs) are becoming more popular because of their countless applications and exclusive properties in many sectors. While considering the current issue of environmental problems and the excessive use of petroleum products, nonisocyanate PU (NIPU) are favored due to their sustainability and low toxicity compared to conventional PU. In this work, flexible NIPU films were made using a green and facile method. For that, soybean oil (SBO) was used as the starting material and converted into epoxide SBO, followed by its chemical conversion into carbonated SBO (CSBO) using carbon dioxide gas. Following that, the CSBO reacted with three different aliphatic amines, namely, 1,2-ethylenediamine, 1,4-butylenediamine, and 1,6-hexamethylenediamine, in a solventless and catalyst-free system. The films were cast and cured at 85 °C for different curing times. The effects of the aliphatic diamines and curing times on the NIPU films were evaluated. The individual materials were confirmed with Fourier transform infrared, 1H nuclear magnetic resonance, and gel permeation chromatography. To analyze the thermal and mechanical properties, thermogravimetric analysis, dynamic mechanical analysis, and differential scanning calorimetry were performed. Furthermore, mechanical tests such as hardness and tensile strength were also performed along with the degree of swelling, gel content, and contact angle by using several solvents. This study elucidated the structure-property relationship based on the effect of curing time and aliphatic chain size of diamines in the properties of a NIPU film. The satisfactory thermal and mechanical properties, accompanied by a green and facile approach, displayed the potential scalability of the NIPU films.

Eco-friendly mixed metal (Mg-Ni) ferrite nanosheets for efficient electrocatalytic water splitting.

Eco-friendly and cost-effective catalysts with multiple active sites, large surface area, high stability and catalytic activity are highly desired for efficient water splitting as a sustainable green energy source. Within this line, a facile synthetic approach based on solventless thermolysis was employed for the simple and tunable synthesis of Ni1-xMgxFe2O4 (0 ≤ x ≤ 1) nanosheets. The characterization of nanosheets (via p-XRD, EDX, SEM, TEM, HRTEM, and SAED) revealed that the pristine ferrites (NiFe2O4 and MgFe2O4), and their solid solutions maintain the same cubic symmetry throughout the composition regulation. Elucidation of the electrochemical performance of the nanoferrite solid solutions showed that by tuning the local chemical environment of Ni in NiFe2O4 via Mg substitution, the intrinsic catalytic activity was enhanced. Evidently, the optimized Ni0.4Mg0.6Fe2O4 catalyst showed drastically enhanced HER activity with a much lower overpotential of 121 mV compared to the pristine NiFe2O4 catalyst. Moreover, Ni0.2Mg0.8Fe2O4 catalyst exhibited the best OER performance with a low overpotential of 284 mV at 10 mA/cm2 in 1 M KOH. This enhanced electrocatalytic activity could be due to improved electronic conductivity caused by the partial substitution of Ni2+ by Mg2+ in the NiFe2O4 matrix as well as the synergistic effect in the Mg-substituted NiFe2O4. Our results suggest a feasible route for developing earth-abundant metal oxide-based electrocatalysts for future water electrolysis applications.

Optimum iron-pyrophosphate electronic coupling to improve electrochemical water splitting and charge storage.

Tuning the electronic properties of transition metals using pyrophosphate (P2O7) ligand moieties can be a promising approach to improving the electrochemical performance of water electrolyzers and supercapacitors, although such a material's configuration is rarely exposed. Herein, we grow NiP2O7, CoP2O7, and FeP2O7 nanoparticles on conductive Ni-foam using a hydrothermal procedure. The results indicated that, among all the prepared samples, FeP2O7 exhibited outstanding oxygen evolution reaction and hydrogen evolution reaction with the least overpotential of 220 and 241 mV to draw a current density of 10 mA/cm2. Theoretical studies indicate that the optimal electronic coupling of the Fe site with pyrophosphate enhances the overall electronic properties of FeP2O7, thereby enhancing its electrochemical performance in water splitting. Further investigation of these materials found that NiP2O7 had the highest specific capacitance and remarkable cycle stability due to its high crystallinity as compared to FeP2O7, having a higher percentage composition of Ni on the Ni-foam, which allows more Ni to convert into its oxidation states and come back to its original oxidation state during supercapacitor testing. This work shows how to use pyrophosphate moieties to fabricate non-noble metal-based electrode materials to achieve good performance in electrocatalytic splitting water and supercapacitors.

Fe-phthalocyanine derived highly conjugated 2D covalent organic framework as superior electrocatalyst for oxygen reduction reaction.

Although porphyry systems like metallo-phthalocynine are recognized as promising molecular models for electrocatalytic oxygen reduction reaction (ORR), their poor durability and methanol tolerance are still challenges and need improvement before being considered for practical applications. Herein, we successfully designed and constructed a Fe-phthalocyanine-derived highly conjugated 2D covalent organic framework (2D FePc-COF), using octa-amino-Fe-phthalocyanine (OA-FePc) and cyclohexanone as precursors. The prepared 2D FePc-COF was characterized via multiple analytic techniques. The electrochemical studies indicated that prepared 2D FePc-COF was far more superior to OA-FePc and 20% Pt/C, displaying anodic shift of 100 and 50 mV (vs RHE) in formal potential, respectively. Moreover, this catalyst also demonstrated excellent methanol tolerance and durability (over 10,000 CV cycles). Theoretical investigations revealed that due to extended conjugation and elimination of electron donating groups (-NH2), the shifting of dz2-orbital (Fe) energy took nearer to π*-orbital (O2), allowing optimum coupling of both the orbitals, thereby enhancing 4e- ORR. This work demonstrates the art of molecular design, aiming at improving catalytic activity of macrocyclic molecular systems towards ORR.

Metal-organic frameworks for wastewater treatment: Recent developments, challenges, and future prospects.

Wastewater treatment is critically important for the existence of life on earth; however, this approach involves the removal of toxic metal contaminants and organic pollutants, requiring efficient adsorbent materials. Within this agenda, metal-organic frameworks (MOFs) appear to be potential materials due to their unique properties as efficient adsorbents, effective photocatalysts, and reliable semi-permeable membranes. Therefore, MOFs have undergone various modifications over the years without desirable success to improve adsorption capacity, hydro-stability, reaction kinetics, and reusability. Therefore, scientists around the world got engaged in MOF research for novel modifications, including defect engineering, carbonization, and membrane fabrication, at the laboratory scale. This review focuses on developing MOF-based adsorbents, photocatalysts, and semi-permeable membranes for wastewater treatment since 2015, emphasizing their structural-functional relationships. Finally, the challenges and opportunities with MOFs in wastewater treatment are also underlined for future efforts.

Transition metal-based nanoparticles as potential antimicrobial agents: recent advancements, mechanistic, challenges, and future prospects.

Bacterial transmission is considered one of the potential risks for communicable diseases, requiring promising antibiotics. Traditional drugs possess a limited spectrum of effectiveness, and their frequent administration reduces effectiveness and develops resistivity. In such a situation, we are left with the option of developing novel antibiotics with higher efficiency. In this regard, nanoparticles (NPs) may play a pivotal role in managing such medical situations due to their distinct physiochemical characteristics and impressive biocompatibility. Metallic NPs are found to possess extraordinary antibacterial effects that are useful in vitro as well as in vivo as self-modified therapeutic agents. Due to their wide range of antibacterial efficacy, they have potential therapeutic applications via diverse antibacterial routes. NPs not only restrict the development of bacterial resistance, but they also broaden the scope of antibacterial action without binding the bacterial cell directly to a particular receptor with promising effectiveness against both Gram-positive and Gram-negative microbes. This review aimed at exploring the most relevant types of metal NPs employed as antimicrobial agents, particularly those based on Mn, Fe, Co, Cu, and Zn metals, and their antimicrobial mechanisms. Further, the challenges and future prospects of NPs in biological applications are also discussed.

Bimetallic Co-Fe sulfide and phosphide as efficient electrode materials for overall water splitting and supercapacitor.

The major center of attraction in renewable energy technology is the designing of an efficient material for both electrocatalytic and supercapacitor (SC) applications. Herein, we report the simple hydrothermal method to synthesize cobalt-iron-based nanocomposites followed by sulfurization and phosphorization. The crystallinity of nanocomposites has been confirmed using X-ray diffraction, where crystalline nature improves from as-prepared to sulfurized to phosphorized. The as-synthesized CoFe-nanocomposite requires 263 mV overpotential for oxygen evolution reaction (OER) to reach a current density of 10 mA/cm2 whereas the phosphorized requires 240 mV to reach 10 mA/cm2. The hydrogen evolution reaction (HER) for CoFe-nanocomposite exhibits 208 mV overpotential at 10 mA/cm2. Moreover, the results improved after phosphorization showing 186 mV to reach 10 mA/cm2. The specific capacitance (Csp) of as-synthesized nanocomposite is 120 F/g at 1 A/g, along with a power density of 3752 W/kg and a maximum energy density of 4.3 Wh/kg. Furthermore, the phosphorized nanocomposite shows the best performance by exhibiting 252 F/g at 1 A/g and the highest power and energy density of 4.2 kW/kg and 10.1 Wh/kg. This shows that the results get improved more than twice. The 97% capacitance retention after 5000 cycles shows cyclic stability of phosphorized CoFe. Our research thus offers cost-effective and highly efficient material for energy production and storage applications.

MXene-Based Nanomaterials for Multifunctional Applications.

MXene is becoming a "rising star" material due to its versatility for a wide portfolio of applications, including electrochemical energy storage devices, electrocatalysis, sensors, biomedical applications, membranes, flexible and wearable devices, etc. As these applications promote increased interest in MXene research, summarizing the latest findings on this family of materials will help inform the scientific community. In this review, we first discuss the rapid evolutionary change in MXenes from the first reported M2XTx structure to the last reported M5X4Tx structure. The use of systematically modified synthesis routes, such as foreign atom intercalation, tuning precursor chemistry, etc., will be further discussed in the next section. Then, we review the applications of MXenes and their composites/hybrids for rapidly growing applications such as batteries, supercapacitors, electrocatalysts, sensors, biomedical, electromagnetic interference shielding, membranes, and flexible and wearable devices. More importantly, we notice that its excellent metallic conductivity with its hydrophilic nature distinguishes MXene from other materials, and its properties and applications can be further modified by surface functionalization. MXene composites/hybrids outperform pristine MXenes in many applications. In addition, a summary of the latest findings using MXene-based materials to overcome application-specific drawbacks is provided in the last few sections. We hope that the information provided in this review will help integrate lab-scale findings into commercially viable products.

MXene: fundamentals to applications in electrochemical energy storage.

A new, sizable family of 2D transition metal carbonitrides, carbides, and nitrides known as MXenes has attracted a lot of attention in recent years. This is because MXenes exhibit a variety of intriguing physical, chemical, mechanical, and electrochemical characteristics that are closely linked to the wide variety of their surface terminations and elemental compositions. Particularly, MXenes are readily converted into composites with materials including oxides, polymers, and CNTs, which makes it possible to modify their characteristics for a variety of uses. MXenes and MXene-based composites have demonstrated tremendous promise in environmental applications due to their excellent reducibility, conductivity, and biocompatibility, in addition to their well-known rise to prominence as electrode materials in the energy storage sector. The remarkable characteristics of 2D MXene, including high conductivity, high specific surface area, and enhanced hydrophilicity, account for the increasing prominence of its use in storage devices. In this review, we highlight the most recent developments in the use of MXenes and MXene-based composites for electrochemical energy storage while summarizing their synthesis and characteristics. Key attention is paid to applications in supercapacitors, batteries, and their flexible components. Future research challenges and perspectives are also described.

Phyto-synthesized facile Pd/NiOPdO ternary nanocomposite for electrochemical supercapacitor applications.

Sustainable and effective electrochemical materials for supercapacitors are greatly needed for solving the global problems of energy storage. In this regard, a facile nanocomposite of Pd/NiOPdO was synthesized using foliar phyto eco-friendly agents and examined as an electrochemical electrode active material for supercapacitor application. The nanocomposite showed a mixed phase of a ternary nano metal oxide phase of rhombohedral NiO and tetragonal PdO confirmed by X-ray diffraction (XRD), scanning electron microscopy (SEM) and XPS (X-rays photoelectron spectroscopy). The optical (direct) energy value of the synthesized nanocomposite was 3.14 eV. The phyto-functionalized nanocomposite was studied for electrochemical supercapacitor properties and revealed a specific capacitance of 88 F g-1 and low internal resistance of 0.8 Ω. The nanoscale and phyto organic species functionalized nanocomposite exhibited enhanced electrochemical properties for supercapacitor application.

Waste Citrus reticulata Assisted Preparation of Cobalt Oxide Nanoparticles for Supercapacitors.

The green, sustainable, and inexpensive creation of novel materials, primarily nanoparticles, with effective energy-storing properties, is key to addressing both the rising demand for energy storage and the mounting environmental concerns throughout the world. Here, an orange peel extract is used to make cobalt oxide nanoparticles from cobalt nitrate hexahydrate. The orange peel extract has Citrus reticulata, which is a key biological component that acts as a ligand and a reducing agent during the formation of nanoparticles. Additionally, the same nanoparticles were also obtained from various precursors for phase and electrochemical behavior comparisons. The prepared Co-nanoparticles were also sulfurized and phosphorized to enhance the electrochemical properties. The synthesized samples were characterized using scanning electron microscopic and X-ray diffraction techniques. The cobalt oxide nanoparticle showed a specific capacitance of 90 F/g at 1 A/g, whereas the cobalt sulfide and phosphide samples delivered an improved specific capacitance of 98 F/g and 185 F/g at 1 A/g. The phosphide-based nanoparticles offer more than 85% capacitance retention after 5000 cycles. This study offers a green strategy to prepare nanostructured materials for energy applications.

Sunflower Oil as a Renewable Resource for Polyurethane Foams: Effects of Flame-Retardants.

Currently, polyurethane (PU) manufacturers seek green alternatives for sustainable production. In this work, sunflower oil is studied as a replacement and converted to a reactive form through epoxidation and oxirane opening to produce rigid PU foams. Confirmatory tests such as Fourier-transform infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), and hydroxyl value among others were performed to characterize the synthesized polyol. Despite the versatility of rigid PU foams, they are highly flammable, which makes eco-friendly flame retardants (FRs) desired. Herein, expandable graphite (EG) and dimethyl methyl phosphonate (DMMP), both non-halogenated FR, were incorporated under different concentrations to prepare rigid PU foams. Their effects on the physio-mechanical and fire-quenching properties of the sunflower oil-based PU foams were elucidated. Thermogravimetric and compression analysis showed that these foams presented appreciable compressive strength along with good thermal stability. The closed-cell contents (CCC) were around 90% for the EG-containing foams and suffered a decrease at higher concentrations of DMMP to 72%. The burning test showed a decrease in the foam's flammability as the neat foam had a burning time of 80 s whereas after the addition of 13.6 wt.% of EG and DMMP, separately, there was a decrease to 6 and 2 s, respectively. Hence, our research suggested that EG and DMMP could be a more viable alternative to halogen-based FR for PU foams. Additionally, the adoption of sunflower polyol yielded foams with results comparable to commercial ones.

Effect of Graphene Oxide and Reduced Graphene Oxide on the Properties of Sunflower Oil-Based Polyurethane Films.

Sunflower oil was used for the synthesis of a polyol via an epoxidation reaction followed by a ring-opening reaction. The successful synthesis of the sunflower oil-based polyol (SFO polyol) was demonstrated through structural characterizations and wet-chemistry analysis. Bio-based polyurethane (BPU) films were fabricated using synthesized polyol and diisocyanate. Various amounts of graphene oxide (GO) and reduced graphene oxide (rGO) were added separately to see their effect on the physicomechanical and thermal properties of BPU films. Several tests, such as thermogravimetric analysis, tensile strength, dynamic mechanical analysis, hardness, flexural strength, and the water contact angle, were performed to evaluate the effect of GO and rGO on the properties of the BPU films. Some of the analyses of the BPU films demonstrated an improvement in the mechanical properties, for example, the tensile strength increased from 22.5 to 26 MPa with the addition of only 0.05 wt.% GO. The storage modulus improved from 900 to 1000 and 1700 MPa after the addition of 0.02 and 0.05 wt.% GO, respectively. This study shows that a small amount of GO and rGO could improve the properties of BPU films, making them suitable for use in coating industries.

Biopolymers-Derived Materials for Supercapacitors: Recent Trends, Challenges, and Future Prospects.

Supercapacitors may be able to store more energy while maintaining fast charging times; however, they need low-cost and sophisticated electrode materials. Developing innovative and effective carbon-based electrode materials from naturally occurring chemical components is thus critical for supercapacitor development. In this context, biopolymer-derived porous carbon electrode materials for energy storage applications have gained considerable momentum due to their wide accessibility, high porosity, cost-effectiveness, low weight, biodegradability, and environmental friendliness. Moreover, the carbon structures derived from biopolymeric materials possess unique compositional, morphological, and electrochemical properties. This review aims to emphasize (i) the comprehensive concepts of biopolymers and supercapacitors to approach smart carbon-based materials for supercapacitors, (ii) synthesis strategies for biopolymer derived nanostructured carbons, (iii) recent advancements in biopolymer derived nanostructured carbons for supercapacitors, and (iv) challenges and future prospects from the viewpoint of green chemistry-based energy storage. This study is likely to be useful to the scientific community interested in the design of low-cost, efficient, and green electrode materials for supercapacitors as well as various types of electrocatalysis for energy production.

Tuning composition of CuCo2S4-NiCo2S4 solid solutions via solvent-less pyrolysis of molecular precursors for efficient supercapacitance and water splitting.

Mixed metal sulfides are increasingly being investigated because of their prospective applications for electrochemical energy storage and conversion. Their high electronic conductivity and high density of redox sites result in significant improvement of their electrochemical properties. Herein, the composition-dependent supercapacitive and water splitting performance of a series of Ni(1-x)Cu x Co2S4 (0.2 ≤ x ≤ 0.8) solid solutions prepared via solvent-less pyrolysis of a mixture of respective metal ethyl xanthate precursors is reported. The use of xanthate precursors resulted in the formation of surface clean nanomaterials at low-temperature. Their structural, compositional, and morphological features were examined by p-XRD, SEM, and EDX analyses. Both supercapacitive and electrocatalytic (HER, OER) properties of the synthesized materials significantly vary with composition (Ni/Cu molar content). However, the optimal composition depends on the application. The highest specific capacitance of 770 F g-1 at a current density of 1 A g-1 was achieved for Ni0.6Cu0.4Co2S4 (NCCS-2). This electrode exhibits capacitance retention (C R) of 67% at 30 A g-1, which is higher than that observed for pristine NiCo2S4 (838 F g-1 at 1 A g-1, 47% C R at 30 A g-1). On the contrary, Ni0.4Cu0.6Co2S4 (NCCS-3) exhibits the lowest overpotential of 124 mV to deliver a current density of 10 mA cm-2. Finally, the best OER activity with an overpotential of 268 mV at 10 mA cm-2 was displayed by Ni0.8Cu0.2Co2S4 (NCCS-1). The prepared electrodes exhibit high stability, as well as durability.

Sustainable synthesis of organic framework-derived ZnO nanoparticles for fabrication of supercapacitor electrode.

The phytosynthesis of metal oxides nanoparticles (NPs) has been extensively reported; yet mechanism involved and incorporated bioactive compounds in the synthesized NPs are still need to be investigated. In this regard, here an efficient sustainable co-precipitation synthesis of zinc oxide nanoparticles (ZnO NPs) has been developed, employing hydrothermal reactions, using organic compounds of Nasturtium officinale leaves. Pure hexagonal wurtzite ZnO was identified by X-ray diffraction and NPs in the size range of 50-60 nm were observed by field emission scanning electron microscopy. X-ray photoelectron spectroscopy revealed surface modification of ZnO by functional groups associated with the incorporated bio active compounds of Nasturtium officinale. The phyto-functionalized ZnO NPs having anoptical direct band gap of 3.29 eV and optical band gap energy of 2.85 eV were evaluated by cyclic voltammetry at various scan rates, galvanostatic charge-discharge at a range of current densities and electrochemical impedance spectroscopy (Z' vs. Z″ and Z vs. frequency) in aqueous electrolyte. The fabricated ZnO-based electrode revealed a specific capacitance of 86.5 F/g at 2 mV/s with 97% coulombic efficiency for 2000 cycles. The good electrochemical conductivity was demonstrated by lower internal resistance of 1.04 Ω. Therefore, the present study suggested the significant potential of organic compounds incorporated ZnO NPs towards supercapacitor.

Triphenylphosphine-Assisted Transformation of NiS to Ni2P through a Solvent-Less Pyrolysis Route: Synthesis and Electrocatalytic Performance.

Straightforward synthetic routes to the preparation of transition metal phosphides or their chalcogenide analogues are highly desired due to their widespread applications, including catalysis. We report a facile and simple route for the preparation of a pure phase nickel phosphide (Ni2P) and phase transformations in the nickel sulfide (NiS) system through a solvent-less synthetic protocol. Decomposition of different sulfur-based complexes (dithiocarbamate, xanthate, and dithiophosphonate) of nickel(II) was investigated in the presence and absence of triphenylphosphine (TPP). The optimization of reaction parameters (nature of precursor, ratio of TPP, temperature, and time) indicated that phosphorus- and sulfur-containing inorganic dithiophosphonate complexes and TPP (1:1 mole ratio) produced pure nickel phosphide, whereas different phases of nickel sulfide were obtained from dithiocarbamate and xanthate precursors in the presence or absence of TPP. A plausible explanation of the sulfide or phosphide phase formation is suggested, and the performance of Ni2P was investigated as an electrocatalyst for supercapacitance and overall water-splitting reactions. The performance of Ni2P with the surface free of any capping agents is not well explored, as common synthetic methods are solution-based routes; therefore, the electrocatalytic performance was also compared with metal phosphides, prepared by other routes. The highest specific capacitance of 367 F/g was observed at 1 A/g, and the maximum energy and power density of Ni2P were calculated to be 17.9 Wh/kg and 6951 W/kg, respectively. The prepared nickel phosphide required overpotentials of 174 and 316 mV along with Tafel slopes of 115 and 95 mV/dec to achieve a current density of 10 mA/cm2 for the hydrogen evolution reaction (HER) and the oxygen evolution reaction (OER), respectively.